[Federal Register Volume 66, Number 10 (Tuesday, January 16, 2001)]
[Rules and Regulations]
[Pages 3466-3497]
From the Federal Register Online via the Government Publishing Office [www.gpo.gov]
[FR Doc No: 01-178]
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ENVIRONMENTAL PROTECTION AGENCY
40 CFR Parts 136, 141, and 143
[FRL-6918-2]
RIN 2040-AD59
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; Methods
Update
AGENCY: Environmental Protection Agency (EPA).
ACTION: Direct Final Rule.
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SUMMARY: EPA is approving the use of updated versions of test
procedures (i.e., analytical methods) for the determination of
chemical, radiological, and microbiological pollutants and contaminants
in wastewater and drinking water. These updated versions of analytical
methods have been published by one or more of the following
organizations: American Society for Testing Materials (ASTM), United
States Geological Survey (USGS), United States Department of Energy
(DOE), American Public Health Association (APHA), American Water Works
Association (AWWA), and Water Environment Federation (WEF). Previously
approved versions of the methods remain approved. Today's action will
give the analytical community a larger selection of analytical methods.
Today's action also corrects typographical errors and updates
references where appropriate.
DATES: This final rule is effective on May 16, 2001 without further
notice, unless EPA receives adverse comment by March 19, 2001. If EPA
receives such comment, EPA will publish a timely withdrawal in the
Federal Register informing the public that this rule (or distinct
amendments, paragraphs, or sections of this rule) will not take effect.
The incorporation by reference of the publications listed in
today's rule is approved by the Director of the Federal Register as of
May 16, 2001.
For judicial review purposes, this final rule is promulgated as of
1:00 p.m. (Eastern time) on January 30, 2001 as provided in 40 CFR 23.2
and 23.7.
ADDRESSES: You may submit written comments either by mail or
electronically. Send comments to the Methods Update Comment Clerk (W-
99-21), U.S. Environmental Protection Agency, Water Docket, MC-4101,
Ariel Rios Bldg., 1200 Pennsylvania Ave., NW., Washington, DC 20460.
Submit electronic comments to OW-Docket @epa.gov. Please submit copies
of any references cited in your comments. EPA would appreciate an
original and 3 copies of your comments and enclosures (including
references).
This Federal Register document is also available on the Internet
at:
http://www.epa.gov/fedrgstr. The record for this rulemaking has been
established under docket number W-99-21. Supporting documents
(including references and methods cited in this notice) are available
for review at the U.S. Environmental Protection Agency, Water Docket,
East Tower Basement, Room EB57, 401 M Street, SW., Washington, DC
20460. For access to the docket materials, call 202/260-3027 on Monday
through Friday, excluding Federal holidays, between 9:00 a.m. and 3:30
p.m. Eastern Daylight Standard Time for an appointment.
Copies of final methods published by ASTM are available for a
nominal cost through American Society for Testing and Materials, 100
Barr Harbor Drive, West Conshohocken, PA 19428-2959. Copies of final
methods published by USGS are available for a nominal cost through the
United States Geological Survey, U.S. Geological Survey Information
Services, Box 25286, Federal Center, Denver, CO 80225-0425. Copies of
final methods published by DOE are available for a nominal cost through
the Environmental Measurements Laboratory, U.S. Department of Energy,
376 Hudson Street, New York, NY 10014-3621. Copies of Standard Methods
are available for a nominal cost from the American Public Health
Association,
[[Page 3467]]
1015 Fifteenth Street, NW., Washington, DC. 20005.
FOR FURTHER INFORMATION CONTACT: For information regarding wastewater
methods contact Dr. Maria Gomez-Taylor, Engineering and Analysis
Division (4303), USEPA Office of Science and Technology, Ariel Rios
Bldg., 1200 Pennsylvania Ave., NW., Washington, DC 20460 (e-mail:
[email protected]). For information regarding the drinking
water methods, contact Dr. Richard Reding, Office of Ground Water and
Drinking Water, U.S. Environmental Protection Agency, Cincinnati, Ohio
45268 (e-mail: [email protected]).
SUPPLEMENTARY INFORMATION:
Potentially Regulated Entities
A. Clean Water Act
EPA Regions, as well as States, Territories, and Tribes, are
authorized to implement the National Pollutant Discharge Elimination
System (NPDES) program and issue permits that comply with the
technology-based and water quality-based requirements of the Clean
Water Act. In doing so, the NPDES permitting authority, including
authorized States, Territories, and Tribes, make a number of
discretionary choices associated with permit writing, including the
selection of pollutants to be measured and, in many cases, limited in
permits. If EPA has ``approved'' (i.e., promulgated through rulemaking)
standardized testing procedures for a given pollutant, the NPDES permit
must specify one of the approved testing procedures or an approved
alternate test procedure. Permitting authorities may, at their
discretion, require the use of any method approved at 40 CFR part 136
in the permits they issue. Therefore, dischargers with NPDES permits
could be affected by the standardization of testing procedures in this
rulemaking, because NPDES permits may incorporate the testing
procedures in today's rulemaking. In addition, when a State, Territory,
or authorized Tribe provides certification of Federal licenses under
Clean Water Act section 401, States, Territories, and Tribes are
directed to use the standardized testing procedures. Categories and
entities that may ultimately be affected include:
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Examples of potentially
Category regulated entities
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Regional, State and Territorial States, Territories, and Tribes
Governments and Indian Tribes. authorized to administer the
NPDES permitting program;
States, Territories, and
Tribes providing certification
under Clean Water Act section
401; Governmental NPDES
permittees
Industry............................... Industrial NPDES permittees
Municipalities......................... Publicly-owned treatment works
with NPDES permits
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B. Safe Drinking Water Act
Public water systems are the regulated entities required to conduct
analyses to measure for contaminants in water samples. However, EPA
Regions, as well as States, local, and tribal governments with primacy
to administer the regulatory program for public water systems under the
Safe Drinking Water Act, sometimes conduct analyses to measure for
contaminants in water samples. If EPA has established a maximum
contaminant level (``MCL'') for a given drinking water contaminant, the
Agency also ``approves'' (i.e., promulgates through rulemaking)
standardized testing procedures for analysis of the contaminant. Once
EPA standardizes such test procedures, analysis using those procedures
(or approved alternate test procedures) is required. Public water
systems required to test water samples must use one of the approved
standardized test procedures. Categories and entities that may
ultimately be regulated include:
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Examples of potentially
Category regulated entities SIC
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State, Local, & Tribal Governments. States, local and tribal 9511
governments that analyze
water samples on behalf
of public water systems
required to conduct such
analysis; States, local,
and tribal governments
that themselves operate
public water systems
required to conduct
analytic monitoring.
Industry........................... Industrial operators of 4941
public water systems.
Municipalities..................... Municipal operators of 9511
public water systems.
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C. These tables are not intended to be exhaustive, but rather
provide a guide for readers regarding entities potentially regulated by
this action. The tables list the types of entities that EPA is now
aware could potentially be regulated by this action. Other types of
entities not listed in the tables 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) and 40 CFR 136.1 (NPDES permits and CWA). 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.
Outline of Notice
I. Legal Authorities
A. Clean Water Act
B. Safe Drinking Water Act
II. Overview of Methods Updates
A. Amendments to Methods at 40 CFR Part 136 for Monitoring
Wastewater
B. Amendments to Methods at 40 CFR Part 141 for Monitoring
Primary Drinking Water Contaminants
C. Amendments to Methods at 40 CFR Part 143 for Monitoring
Secondary Drinking Water Contaminants
III. Reasons for Using Direct Final Rulemaking
IV. Description of the Amendments in Today's Actions
A. Approval of Updated Versions of Analytical Methods
1. ASTM Methods for Analyses of Wastewater and Drinking Water
2. APHA/AWWA/WEF Methods (Standard Methods) for Analyses of
Wastewater and Drinking Water
3. USGS Methods for Analyses of Wastewater
4. DOE Methods for Analysis of Radionuclides in Drinking Water
B. Typographical Errors
C. Performance-based Measurement System
V. Administrative Requirements
A. Executive Order 12866: Regulatory Planning and Review
B. Regulatory Flexibility Act (RFA), as amended by the Small
Business
[[Page 3468]]
Regulatory Enforcement Fairness Act of 1996 (SBREFA), 5 U.S.C. 601
et.seq.
C. Unfunded Mandated Reform Act
D. Paperwork Reduction Act
E. National Technology Transfer and Advancement Act
F. Executive Order 13045: Protection of Children From
Environmental Health Risks and Safety Risks
G. Executive Order 13132: Federalism
H. Executive Order 13084: Consultation and Coordination With
Indian Tribal Governments
I. Congressional Review Act
VI. References
I. Legal Authorities
A. Clean Water Act
This regulation is promulgated under the authority of sections 301,
304(h), and 501(a) of the Clean Water Act (CWA), 33 U.S.C. 1311,
1314(h), 1361(a) (the ``Act''). Section 301 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 EPA Administrator to ``promulgate guidelines establishing
test procedures for the analysis of pollutants that shall include the
factors which must be provided in any certification pursuant to section
401 of this Act or permit applications 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 his
functions under this Act.'' EPA publishes CWA analytical method
regulations at 40 CFR part 136. The Administrator also has made these
test procedures applicable to monitoring and reporting of NPDES permits
(40 CFR part 122, Secs. 122.21, 122.41, 122.44, and 123.25), and
implementation of the pretreatment standards issued under section 307
of the Act (40 CFR part 403, Secs. 403.10 and 403.12).
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)
which 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 section 1401 (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 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 assist in
determining whether persons are acting in compliance with the
requirements of the SDWA (42 U.S.C. 300j-4). EPA's promulgation of
analytical methods 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)).
II. Overview of Methods Updates
EPA has promulgated analytical methods for all currently regulated
wastewater and drinking water pollutants and contaminants. In most
cases, EPA has approved use of more than one analytical method for
measurement of a contaminant, and laboratories may use any approved
method for determining compliance with a monitoring requirement. After
any regulation is published, EPA may amend the regulations to approve
new methods or modifications to approved methods.
Many of the analytical methods already promulgated by EPA have been
published by other organizations, including the American Society for
Testing Materials (ASTM), United States Geological Survey (USGS), and
United States Department of Energy (DOE). In addition, three other
organizations (American Public Health Association, American Water Works
Association and Water Environment Federation) jointly publish Standard
Methods for Examination of Water and Wastewater (referred to as
``Standard Methods''). This rule approves use of updated versions of
currently promulgated ASTM Methods, Standard Methods, and USGS methods
at 40 CFR part 136 for compliance with wastewater standards and
monitoring requirements. This rule also approves updated versions of
currently promulgated methods in the tables of analytical methods
listed at 40 CFR parts 141 and 143 for analyses of drinking water
contaminants. The drinking water methods included in this rule are
published by ASTM, Standard Methods, and DOE. These organizations
publish updated manuals of methods from time to time. Some of the
methods in the updated manuals contain no change from previously
published editions. Other methods contain no significant changes, only
minor technical improvements that make the methods safer and/or easier
to use. Today's amendments contain only methods that have no changes or
only minor technical improvements. No EPA methods are being updated.
This rule does not withdraw from use any currently promulgated
method. For an NPDES permit, the permitting authority should decide the
appropriate method based on the nature of the particular water sample
to be tested and based on the measurement level of concern.
Today's amendments allow use of updated versions of methods, as
outlined below. Each write-up uniquely defined by an identifying method
number is counted as a single updated method, regardless of the nature
of changes. Even if the only change to the method is its inclusion in a
more recent published edition of a methods manual (e.g, 19th Edition of
Standard Methods), it is considered an updated method.
A. Amendments to Methods at 40 CFR Part 136 for Monitoring Wastewater
Today's amendments allow use of 19 updated methods published by the
American Society for Testing and Materials (ASTM) in the 1999 Annual
Book of ASTM Standards, Vols. 11.01 and 11.02 for determinations of
chemical and radionuclide contaminants, and physical parameters.
Previously published versions of these methods, if already promulgated
by EPA, remain approved.
Today's amendments also allow use of 189 updated methods published
by the Standard Methods Committee in Standard Methods for the
Examination of Water and Wastewater, 19th edition, 1995, and 20th
edition, 1998, for determinations of chemical, microbiological and
radionuclide contaminants, and physical parameters.
EPA is also amending 40 CFR Part 136 to update USGS Method I-1472-
85 to Method I-4471-97 for determination of cadmium, and 21 methods
published by USGS in open file reports and method compendiums. The 21
USGS methods are for the determination of one or more analytes . These
methods employ the same analytical procedures and technologies that are
employed in promulgated EPA and VCSB methods. These USGS methods will
give the analytical community a greater selection of methods.
Finally, today's amendments correct typographical errors in the
tables of methods, table footnotes, and sources.
B. Amendments to Methods at 40 CFR Part 141 for Monitoring Primary
Drinking Water Contaminants
Today's amendments allow use of 12 updated methods that are
published in the 1999 Annual Book of ASTM Standards, Vols. 11.01 and
11.02, for determinations of chemical and radionuclide contaminants,
and
[[Page 3469]]
physical parameters. Use of previously promulgated versions of ASTM
methods that are published in these volumes, but have not been revised
from previous editions, is also allowed.
Today's amendments also allow use of 62 updated methods published
by the Standard Methods Committee in Standard Methods for the
Examination of Water and Wastewater, 20th edition, 1998, for
determinations of chemical, microbiological and radionuclide
contaminants, and physical parameters.
Today's amendments allow use of six updated methods published by
DOE in the document ``EML Procedures Manual,'' 28th Edition, Volume 1,
1997, for determinations of radionuclide contaminants.
C. Amendments to Methods at 40 CFR Part 143 for Monitoring Secondary
Drinking Water Contaminants
Today's amendments list an updated version of one chemistry method
(D 4327-97) published in the 1999 Annual Book of ASTM Standards, Vol.
11.01.
Today's amendments also list updated versions of 12 methods
published by the Standard Methods Committee in Standard Methods for the
Examination of Water and Wastewater, 20th edition, 1998, for
determinations of secondary chemical contaminants and physical
parameters.
III. Reasons for Using Direct Final Rulemaking
The Agency is promulgating these amendments as a ``direct final''
rule. EPA is publishing this rule without prior proposal because we
view this as noncontroversial amendments and anticipate no adverse
comment. Today's action approves updated versions of analytical methods
published by several organizations in recent editions of methods
manuals or recent publications. These updated versions contain no
significant changes, only minor technical improvements that make the
methods safer and/or easier to use. However, in the ``Proposed Rules''
section of today's Federal Register, we are publishing a separate
document that will serve as the proposal to update these methods if
adverse comments are filed. This rule will be effective on May 16, 2001
without further notice unless we receive adverse comment by March 19,
2001. If EPA receives adverse comment on one or more distinct
amendments, paragraphs, or sections of this rulemaking, we will publish
a timely withdrawal in the Federal Register indicating which provisions
will become effective and which provisions are being withdrawn due to
adverse comment. Any distinct amendment, paragraph, or section of
today's rulemaking for which we do not receive adverse comment will
become effective on the date set out above, notwithstanding any adverse
comment on any other distinct amendment, paragraph, or section of
today's rule. We will address all public comments in a subsequent final
rule based on the companion proposed rule published elsewhere in
today's Federal Register. We will not institute a second comment period
on the action. Any parties interested in commenting must do so at this
time.
IV. Description of the Amendments in Today's Actions
The Agency is amending the tables of methods at 40 CFR Parts 136,
141 and 143 to include recently updated versions of certain analytical
methods and to correct typographical errors as explained below.
A. Approval of Updated Versions of Analytical Methods
The updated versions of methods listed at 40 CFR Parts 136, 141,
and 143 discussed in this section contain updates of currently
promulgated methods that interested parties, such as public water
systems, NPDES permit writers, pretreatment coordinators, laboratory
personnel, certification officials, and regulatory authorities, will
consider to be noncontroversial and generally useful.
1. American Society for Testing and Materials (ASTM) Methods for
Analyses of Wastewater and Drinking Water
In today's rule, EPA is amending 40 CFR Parts 136, 141, and 143 to
include updated ASTM methods that are published in Vols. 11.01 and
11.02 of the ASTM's Annual Book of Standards [ASTM 1999]. The changes,
if any, in the updated ASTM methods that are included in today's rule
are editorial changes or minor technical clarifications. An example of
an editorial change is the replacement of the unit for the measurement
of radioactivity, picocurie, with the unit, Becquerel; 1 Becquerel
equals 27 picocuries. The change to Becquerel conforms the ASTM methods
to the unit of radioactivity measurement that is recommended by the
International Union for Pure and Applied Chemistry (IUPAC), which is an
international organization that recommends standards for units of
measurement.
Examples of minor technical changes are recommendations for the
safe handling of hazardous materials and safer or better ways to
conduct certain hazardous or complicated analytical procedures. Some of
the ASTM methods have been augmented with additional tables of method
performance data. The updated ASTM methods do not contain substantive
changes in procedures or instrumentation. Because EPA is not
withdrawing approval of the currently approved version of any ASTM
method, approval of the revised methods should have no adverse effect
on users.
a. Wastewater Methods
Nineteen ASTM methods that are published in the 1999 Annual Book of
Standards (ASTM 1999) and that have been updated from previous versions
of these methods are approved in today's rule at 40 CFR Part 136 for
wastewater compliance monitoring. Table 1 lists the 19 revised ASTM
wastewater methods.
Table 1--Revised ASTM Wastewater Methods
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Currently Approved Version 1999 Edition Version
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D 858-90............................... D 858-95
D 859-88............................... D 859-94
D 1068-90.............................. D 1068-96
D 1125-91.............................. D 1125-95
D 1126-86(92).......................... D 1126-96
D 1246-82(88).......................... D 1246-95
D 1252-88.............................. D 1252-95
D 1426-93.............................. D 1426-98
D 1688-90.............................. D 1688-95
D 1889-88.............................. D 1889-94
D 2036-91.............................. D 2036-98
D 2972-93.............................. D 2972-97
D 3557-90.............................. D 3557-95
D 3558-90.............................. D 3558-94
D 3559-90.............................. D 3559-96
D 3859-93.............................. D 3859-98
D 3867-90.............................. D 3867-99
D 4190-82(88).......................... D 4190-94
D 4382-91.............................. D 4382-95
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b. Drinking Water Methods for Primary and Secondary Drinking Water
Contaminants
Twelve ASTM methods that are published in the 1999 Annual Book of
Standards (ASTM 1999) and that have been updated from previous versions
of these methods are approved in today's rule at 40 CFR part 141 for
drinking water compliance monitoring. Because one of the updated
methods, D 4327-97, is also applicable to determinations of both
chloride and sulfate, this method is also recommended in the table at
40 CFR part 143 for monitoring of these secondary contaminants. Three
methods, D 3972 for uranium, and D 2460 and D 3454 for radium, have
been updated to describe an optional computation of a total propagated
uncertainty (TPU). EPA is approving these updated radionuclide methods.
Although the TPU computation is technically satisfactory, it requires
more
[[Page 3470]]
effort than the uncertainty computation for radionuclide measurements
specified at 40 CFR 141.25(c) and 141.26(a). EPA does not preclude use
of the TPU computation, but the Agency believes that this computation
is not necessary to obtain an accurate determination of uncertainty.
Therefore, use of the computation specified in the CFR is recommended.
Table 2 lists the 12 revised ASTM drinking water methods.
Table 2.--Revised ASTM Drinking Water Methods
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Currently Approved Version 1999 Edition Version
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D 2036-91.............................. D 2036-98
D 2460-90.............................. D 2460-97
D 2907-91.............................. D 2907-97
D 2972-93.............................. D 2972-97
D 3454-91.............................. D 3454-97
D 3559-95.............................. D 3559-96
D 3645-93.............................. D 3645-97
D 3859-93.............................. D 3859-98
D 3972-90.............................. D 3972-97
D 4327-91.............................. D 4327-97
D 4785-88.............................. D 4785-93
D 5174-91.............................. D 5174-97
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2. APHA/AWWA/WEF Methods (Standard Methods)
a. Wastewater Methods
In today's rule, EPA is amending 40 CFR part 136 to include 189
updated methods that are published in the 19th (APHA 1995) and 20th
(APHA 1998) Editions of Standard Methods. 40 CFR Part 136 currently
includes only methods listed in the 18th Edition (APHA 1992). Because
EPA is not withdrawing approval of the currently promulgated version of
any Standard Method, approval of these methods in this rulemaking
should have no adverse effect on users.
Thirty of the 189 Standard Methods being approved contain minor
technical and/or editorial revisions to the corresponding promulgated
18th Edition versions. The revisions are intended to improve method
usability. Examples of these changes include: better explanations on
conducting a specific step in the method; recommendations for safer
handling or disposal of hazardous reagents; and options to use
alternative procedures, reagents, or equipment (such as the option to
use capillary columns in Method 6200 C, and the merger of Methods 6220
B and 6230 B into one method, 6200 C).
The other 159 methods remain unchanged from the currently
promulgated methods. The only difference is that they are included in a
more recent edition of Standard Methods and in some cases contain a
different identifying method number. Method number changes between the
18th, 19th, and 20th editions occurred in 27 instances. These changes
in numbering are provided in Table 3.
Table 3.--Standard Methods Number Changes
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18th Edition 19th Edition 20th Edition
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3500-Al D...................... 3500-Al D 3500-Al B
3500-As C...................... 3500-As C 3500-As B
3500-Be D...................... 3500-Be D Dropped
3500-Cd D...................... 3500-Cd D Dropped
3500-Ca D...................... 3500-Ca D 3500-Ca B
3500-Cr D...................... 3500-Cr D 3500-Cr B
3500-Cu D...................... 3500-Cu D 3500-Cu B
3500-Cu E...................... 3500-Cu E 3500-Cu C
3500-Fe D...................... 3500-Fe D 3500-Fe B
3500-Pb D...................... 3500-Pb D 3500-Pb B
3500-Mg D...................... 3500-Mg D Dropped
3500-Mn D...................... 3500-Mn D 3500-Mn B
3500-K D....................... 3500-K D 3500-K B
3500-Na D...................... 3500-Na D 3500-Na B
3500-V D....................... 3500-V D 3500-V B
3500-Zn E...................... 3500-Zn E Dropped
3500-Zn F...................... 3500-Zn F 3500-Zn B
4500-NH3 C..................... Dropped Dropped
4500-NH3 E..................... 4500-NH3 C 4500-NH3 C
4500-NH3 F..................... 4500-NH3 D 4500-NH3 D
4500-NH3 G..................... 4500-NH3 E 4500-NH3 E
4500-NH3 H..................... 4500-NH3 G 4500-NH3 G
4500-S-2 E..................... 4500-S-2F 4500-S-2 F
4500-Si D...................... 4500-Si D 4500-SiO2 C
6210 B......................... 6210 B 6200 B
6220 B......................... 6220 B 6220 C
6230 C......................... 6230 B 6230 C
------------------------------------------------------------------------
[[Page 3471]]
Five methods have been dropped from recent editions of Standards
Methods. These methods are not being withdrawn from 40 CFR Part 136
because the methods are technically sound and there may be laboratories
successfully using these methods. The five methods dropped from
Standard Methods are Method 4500-NH3 C, which was not
included in the 19th edition, and Methods 3500-Be D, 3500-Cd D, 3500-Mg
D, and 3500-Zn E, which were not included in the 20th edition.
b. Drinking Water Methods for Primary and Secondary Drinking Water
Contaminants
EPA is also amending 40 CFR Parts 141 and 143 to add 71 methods
that are published in the 20th Edition of Standard Methods. Previous
promulgated versions of these methods, which are published in 18th and
19th Editions of Standard Methods, are listed at 40 CFR Parts 141 and
143. Because EPA is not withdrawing approval of the currently
promulgated version of any Standard Method, approval of the updated
revised methods in this rulemaking should have no adverse effect on
users.
Of the 71 Standard Methods methods included in today's rule, 52
methods are unchanged from previous versions. The remaining 19 methods
contain minor editorial changes or technical clarifications. Some of
these revisions are minor modifications or voluntary but useful
options, such as better explanations on conducting a specific step in
the method; recommendations for safer handling or disposal of hazardous
reagents; and options to use alternative procedures, reagents, or
equipment. The method numbers for five methods changed between the 19th
and 20th editions. These changes in numbering are provided in Table 4.
Table 4.--Standard Methods Number Changes
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19th Edition 20th Edition
------------------------------------------------------------------------
3500-Ca D................................ 3500-Ca B
3500-Mg E................................ 3500-Mg B
4500-Si D................................ 4500-SiO2 C
4500-Si E................................ 4500-SiO2 D
4500-Si F................................ 4500-SiO2 E
------------------------------------------------------------------------
3. USGS Methods for Analyses of Wastewater
In today's rule, EPA is amending 40 CFR Part 136 to update USGS
Method I-1472-85 to Method I-4471-97 for the determination of cadmium,
and to allow use of 21 updated methods published by USGS in open file
reports and method compendiums. At the request of USGS, the 21 methods
are being promulgated for the determination of one or more analytes.
These 21 USGS methods employ the same analytical procedures and
technologies that are employed in approved EPA and voluntary consensus
standards bodies (VCSB) methods. Approval of these USGS methods will
give the analytical community a greater selection of methods.
4. DOE Methods for Analyses of Radionuclides in Drinking Water
In today's rule, EPA is amending 40 CFR Part 141 to add updated
versions of six radionuclide methods that are published by DOE in the
EML Procedures Manual, 28th Edition, Volume 1, 1997 (DOE 1997). The six
methods are Ra-05, Sr-01, Sr-02, U-02, U-04, and Ga-01-R. Two of the
methods in the 1997 DOE manual have been renumbered. Method Ra-05 is
now Ra-04 and the method referred to as Sect. 4.5.4.3 in the 1990
manual has been given the method number Ga-01-R. Four of the methods in
the 1997 DOE manual are unchanged. One method, Method Ga-01-R, has
minor editorial changes. In Method U-02, alpha spectrometry for uranium
determinations, the sample preparation procedure has been revised and
now allows proceeding directly to the microprecipitation step. This
change eliminates the mercury cathode electrolysis isotope separation
step without affecting the sensitivity or selectivity of the analysis.
In the 1990 version of Method U-02, this isotope separation step was
optional for drinking water samples. This previous version of U-02
continues to be approved along with the 1990 versions of the other five
DOE methods. The Agency, however, strongly recommends use of the 1997
version of U-02, because it eliminates the need for radiochemistry
laboratories to handle large quantities of liquid mercury.
B. Typographical Errors
Today's rule corrects typographical errors in the CFR tables at 40
CFR Part 136, and also updates references as appropriate. All of the
amendments to the tables are minor, and do not impose any new
analytical requirements. Today's rule incorporates the following
technical corrections:
(1) Footnote 38 to Table IB at 40 CFR Part 136.3 is corrected and
updated to reference Trichlorotrifluorethane (1,1,2-trichloro-1,2,2-
trifluoroethane; CFC-113) and n-hexane as approved extraction solvents
for the oil and grease Standard Method 5520 B. Previously,
trichlorofluoromethane (CFC-11) was incorrectly listed.
(2) The Standard Methods digestion procedure that precedes Kjeldahl
Nitrogen determination is corrected to reference Standard Methods 4500-
Norg B or C. Previously, Standard Methods 4500 NH3 B or C
were listed, which provide procedures for ammonia distillation and
titrimetric determination (not digestion), respectively.
(3) Footnote 34 and its associated source listing is updated to
reflect a change in method ownership for Direct Current Plasma (DCP)
Method AES0029, developed by Fisons and acquired by Thermo Jarrell Ash.
(4) The reference for the Nickel Colorimetric (Heptoxime) method is
corrected to include Standard Method 3500-Ni D from the 17th Edition
instead of the 18th Edition. Method 3500-Ni D was not included in the
18th Edition of Standard Methods.
(5) Incorrect page number listings for USGS methods were corrected.
(6) The CFR contains two references with the same number. The
second reference (40) in Section 136.3(b) has been renumbered (41) and
reference (41) has been renumbered (42).
C. Performance-based Measurement System
On March 28, 1997, EPA proposed a rule (62 FR 14976) to streamline
approval procedures and use of analytical methods in water programs
through implementation of a performance-based approach to environmental
measurements. On October 6, 1997, EPA published a notice of the
Agency's intent to implement a performance-based measurement system
(PBMS) in all media programs to the extent feasible (62 FR 52098).
EPA's water program offices have developed a plan to implement PBMS.
EPA anticipates that the final rule to implement PBMS in water programs
will be based on the March 28, 1997 proposed rule.
V. Administrative Requirements
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 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
[[Page 3472]]
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. Regulatory Flexibility Act (RFA), as amended by the Small Business
Regulatory Enforcement Fairness Act of 1996 (SBREFA), 5 U.S.C. 601 et
seq.
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 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 today's rule on small
entities, we defined: (1) Small businesses according to SBA size
standards; (2) small governmental jurisdictions as governments of a
city, county, town, school district or special district with a
population less than 50,000; and (3) small organizations as any not-
for-profit enterprise which is independently owned and operated and is
not dominant in its field.
After considering the economic impacts of today's final rule on
small entities, I certify that this action will not have a significant
economic impact on a substantial number of small entities. This final
rule will not impose any requirements on small entities. Today's rule
approves new and revised versions of currently approved ASTM Methods,
Standard Methods, United States Geological Survey (USGS), and United
States Department of Energy (DOE) methods for compliance with
wastewater monitoring and drinking water standards and monitoring
requirements but does not require their use. Previous versions of these
ASTM, Standard Methods, USGS, and DOE methods will not be withdrawn.
Public water systems and laboratories performing analyses on behalf of
these systems may continue to use the previous versions after the
promulgation of today's rule. The final rule merely provides additional
options. Any of the testing procedures currently approved at 40 CFR
parts 136, 141, or 143 can be used if monitoring is otherwise required
for this pollutant under the CWA or SDWA. This rule also makes minor
technical corrections, amendments, and clarifications to the
regulations.
C. 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, local, and tribal
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 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 notifying
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.
Today's rule contains no Federal mandates (under the regulatory
provisions of Title II of the UMRA) for State, local, or tribal
governments or the private sector. This rule imposes no enforceable
duty on any State, local or tribal governments or the private sector.
EPA has determined that this rule contains no regulatory requirements
that might significantly or uniquely affect small governments. Thus,
today's rule is not subject to the requirements of sections 202, 203,
and 205 of the UMRA.
This rule approves the use of analytical methods for conducting
analysis for contaminants in wastewater and drinking water and thus
provides operational flexibility to laboratory analysts. Since the rule
does not withdraw earlier versions of methods, EPA anticipates no
increase in expenditure or burden.
D. 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 action merely provides additional options on the selection of
testing procedures when monitoring is otherwise required under the CWA
or SDWA. Any of the testing procedures approved at 40 CFR parts 136,
141, or 143 can be used if such monitoring is required for a pollutant
or contaminant.
E. 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, business practices) that are developed or adopted
by voluntary consensus standard bodies. NTTAA directs EPA to provide
Congress, through the Office of Management and Budget (OMB),
explanations when EPA decides not to use available and applicable
voluntary consensus standards.
In this rulemaking EPA is approving newer versions of voluntary
consensus standards published by ASTM and Standard Methods for many
wastewater and drinking water contaminants. EPA recognizes that other
voluntary consensus standards may also be available for the
contaminants covered by this rule. In order to expedite publication of
this rule as a direct final rule, EPA has chosen not to propose other
voluntary consensus methods at this time. EPA plans to address the
[[Page 3473]]
availability of other voluntary consensus methods in subsequent rules.
F. Executive Order 13045: Protection of Children From Environmental
Health Risks and Safety Risks
Executive Order 13045 (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 rule is
not subject to Executive Order 13045 because it is neither
``economically significant'' as defined under Executive Order 12866,
nor does it concern an environmental health or safety risk that EPA has
reason to believe may have a disproportionate effect on children.
G. 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 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. Today's rule approves the use of
additional analytical methods by laboratories conducting analysis in
wastewater and drinking water. Today's action does not, however,
require use of the alternative methods. The rule provides laboratory
analysts with other options to the list of currently approved testing
procedures under 40 CFR parts 136, 141, and 143 which can be used if
monitoring is otherwise required for these pollutants under the CWA or
SDWA. Thus, Executive Order 13132 does not apply to this rule.
H. Executive Order 13084: Consultation and Coordination With Indian
Tribal Governments
Under Executive Order 13084, EPA may not issue a regulation that is
not required by statute, that significantly or uniquely affects the
communities of Indian tribal governments, and that imposes substantial
direct compliance costs on those communities, unless the Federal
government provides the funds necessary to pay the direct compliance
costs incurred by the tribal governments, or EPA consults with those
governments. If EPA complies by consulting, Executive Order 13084
requires EPA to provide to the Office of Management and Budget, in a
separately identified section of the preamble to the rule, a
description of the extent of EPA's prior consultation with
representatives of affected tribal governments, a summary of the nature
of their concerns, and a statement supporting the need to issue the
regulation. In addition, Executive Order 13084 requires EPA to develop
an effective process permitting elected officials and other
representatives of Indian tribal governments ``to provide meaningful
and timely input in the development of regulatory policies on matters
that significantly or uniquely affect their communities.''
Today's rule does not significantly or uniquely affect the
communities of Indian tribal governments. This rule approves new and
updated analytical methods for drinking water compliance monitoring and
wastewater compliance monitoring. Accordingly, the requirements of
section 3(b) of Executive Order 13084 do not apply to this rule.
I. Congressional Review Act
The Congressional Review Act, 5 U.S.C. 801 et seq., as added by the
Small Business Regulatory Enforcement Fairness Act of 1996 (SBREFA),
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.
804(2). This rule will be effective on May 16, 2001.
VI. References
APHA 1992. Eighteenth edition of Standard Methods for the
Examination of Water and Wastewater, 1992, American Public Health
Association, 1015 Fifteenth Street NW., Washington, DC 20005.
APHA 1995. Nineteenth edition of Standard Methods for the
Examination of Water and Wastewater, 1995, American Public Health
Association, 1015 Fifteenth Street NW., Washington, DC 20005.
APHA 1998. Twentieth edition of Standard Methods for the Examination
of Water and Wastewater, 1998, American Public Health Association,
1015 Fifteenth Street NW., Washington, DC 20005.
ASTM 1999. 1999 Annual Book of ASTM Standards, Vols. 11.01 and
11.02, American Society of Testing and Materials, 100 Barr Harbor
Drive, West Conshohocken, Pennsylvania 19428-2959.
AWWA 1996. ``Standard Methods--A Closer Look,'' Posavec, Steve, in
Opflow, Vol.22, No.2, February 1996, American Water Works
Association, 6666 West Quincy Avenue, Denver, CO 80235.
DOE 1997 ``EML Procedures Manual'', 28th Edition, Volume 1, 1997.
Available at the Environmental Measurements Laboratory, U.S.
Department of Energy (DOE), 376 Hudson Street, New York, NY 10014-
3621.
USGS 1989. 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.
USGS 1992. ``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 of the U.S.
Geological Survey, Denver, CO.
USGS 1993. ``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 of the U.S. Geological Survey, Denver, CO.
USGS 1993. ``Methods of Analysis by the U.S. Geological Survey
National Water Quality Laboratory--Determination of Chromium in
Water by Graphite Furnace Atomic Absorption Spectrometry'', Open
File Report (OFR) 93-449 of the U.S. Geological Survey, Denver, CO.
USGS 1994. ``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'' of the U.S. Geological Survey,
Denver, CO.
USGS 1997. ``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 of the U.S. Geological Survey, Denver, CO.
[[Page 3474]]
USGS 1998 ``Methods of Analysis by the U.S. Geological Survey
National Water Quality Laboratory--Determination of Ammonia Plus
Organic Nitrogen by a Kjeldahl Digestion Method and an Automated
Photometric Finish that Includes Digest Cleanup by Gas Diffusion and
an Automated Photometric Finish That Includes Digest Cleanup by Gas
Diffusion''. Open File Report (OFR) 00-170 of the U.S. Geological
Survey, Denver, CO.
USGS 1998. ``Methods of Analysis by the U.S. Geological Survey
National Water Quality Laboratory--Determination of Arsenic and
Selenium in Water and Sediments by Graphite Furnace-Atomic
Absorption Spectrometry'' Open File Report (OFR) 98-639. Table IB,
Note 49.
USGS 1998. ``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 of the U.S.
Geological Survey, Denver, CO.
List of Subjects
40 CFR Part 136
Environmental protection, Analytical methods, Incorporation by
reference, Reporting and recordkeeping requirements, Water pollution
control.
40 CFR Part 141
Environmental protection, Chemicals, Incorporation by reference,
Indian-lands, Intergovernmental relations, Radiation Protection,
Reporting and recordkeeping requirements, Water supply.
40 CFR Part 143
Environmental protection, Chemicals, Incorporation by reference,
Indian-lands, Water supply.
Dated: December 11, 2000.
Carol M. Browner,
Administrator.
For the reasons set out in the preamble, title 40, chapter I of the
Code of Federal Regulations, is amended as follows:
PART 136--GUIDELINES ESTABLISHING TEST PROCEDURES FOR THE ANALYSIS
OF POLLUTANTS
1. The authority citation for Part 136 continues to read as
follows:
Authority: Secs. 301, 304(h), 307, and 501(a) Pub. L. 95-217, 91
Stat. 1566, et seq. (33 U.S.C. 1251, et seq.) (The Federal Water
Pollution Control Act Amendments of 1972 as amended by the Clean
Water Act of 1977.)
2. Section 136.3 is amended:
a. In paragraph (a) by revising Tables IA, IB, IC, ID, and IE.
b. In paragraph (b) revise references (6) and (10), remove
reference (41), redesignate the second reference (40) as (41),
redesignate reference (43) as (51), and add references (42) through
(50) to read as follows:
Sec. 136.3 Identification of test procedures.
* * * * *
(a) * * *
Table 1A.--List of Approved Biological Methods
--------------------------------------------------------------------------------------------------------------------------------------------------------
Standard Methods 18th,
Parameter and units Method \1\ EPA 19th, 20th Ed. ASTM USGS
--------------------------------------------------------------------------------------------------------------------------------------------------------
Bacteria:
1. Coliform (fecal), number Most Probable p.132 \3\ 9221C E \4\ ....................... .......................
per 100 mL.. Number (MPN), 5 p.124 \3\ 9222D \4\ B-0050-85 \5\
tube.
3 dilution, or
Membrane filter
(MF) \2\, single
step.
2. Coliform (fecal) in MPN, 5 tube, 3 p.132 \3\ 9221C E \3\ ....................... .......................
presence of chlorine, dilution, or. p.124 \3\ 9221D \4\
number per 100 mL.. MF, single step\6\
3. Coliform (total), number MPN, 5 tube, 3 p.114 \3\ 9221B \4\ ....................... .......................
per 100 mL.. dilution, or. p. 108 \3\ 9222B \4\ B-0025-85 \5\
MF \2\, single
step or two step.
4. Coliform (total), in MPN, 5 tube, 3 p. 114 \3\ 9221B \4\ ....................... .......................
presence of chlorine, dilution, or. p. 111 \3\ 9222(B+B.5c) \4\
number per 100 mL.. MF \2\ with
enrichment.
5. Fecal streptococci, MPN, 5 tube, 3 p. 139 \3\ 9230B \4\ ....................... .......................
number per 100 mL.. dilution,. p. 136 \3\ 9230C \4\ B-0055-85 \5\
MF \2\, or........
Plate count....... p.143 \3\ ....................... ....................... .......................
Aquatic Toxicity:
6. Toxicity, acute, fresh Daphnia, Sec. 9 \7\ ....................... ....................... .......................
water organisms, LC50, Ceriodaphnia,
percent effluent.. Fathead Minnow,
Rainbow Trout,
Brook Trout, or
Bannerfish Shiner
mortality.
7. Toxicity, acute, Mysid, Sheepshead Sec. 9 \7\ ....................... ....................... .......................
estuarine and marine Minnow, or
organisms, LC50, percent Menidia spp.
effluent.. mortality.
8. Toxicity, chronic, fresh Fathead minnow 1000.0 \8\ ....................... ....................... .......................
water organisms, NOEC or larval survival 1001.0 \8\
IC25, percent effluent.. and growth. 1002.0 \8\
Fathead minnow 1003.0 \8\
embryo-larval
survival and
teratogenicity.
Ceriodaphnia
survival and
reproduction.
Selenastrum growth
[[Page 3475]]
9. Toxicity, chronic, Sheepshead minnow 1004.0 \9\ ....................... ....................... .......................
estuarine and marine larval survival 1005.0 \9\
organisms,NOEC or IC25, and growth.
percent effluent.. Sheepshead minnow 1006.0 \9\
embryo-larval 1007.0 \9\
survival and 1008.0 \9\
teratogenicity. 1009.0 \9\
Menidia beryllina
larval and growth.
Mysidopsis bahia
survival, growth,
and fecundity.
Arbacia punctulata
fertilization.
Champia parvula
reproduction.
--------------------------------------------------------------------------------------------------------------------------------------------------------
Notes to Table IA:
\1\ The method must be specified when results are reported.
\2\ A 0.45 m membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated and to be free of
extractables which could interfere with their growth.
\3\ USEPA. 1978. Microbiological Methods for Monitoring the Environment, Water, and Wastes. Environmental Monitoring and Support Laboratory, U.S.
Environmental Protection Agency, Cincinnati, Ohio. EPA/600/8-78/017.
\4\ APHA. 1998, 1995, 1992. Standard Methods for the Examination of Water and Wastewater. American Public Health Association. 20th, 19th, and 18th
Editions. Amer. Publ. Hlth. Assoc., Washington, DC.
\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, Virginia.
\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\ USEPA. 1993. Methods for Measuring the Acute Toxicity of Effluents to Freshwater and Marine Organisms. Fourth Edition. Environmental Monitoring
Systems Laboratory, U.S. Environmental Protection Agency, Cincinnati, Ohio. August 1993, EPA/600/4-90/027F.
\8\ USEPA. 1994. Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms. Third Edition.
Environmental Monitoring Systems Laboratory, U.S. Environmental Protection Agency USEPA. 1994, Cincinnati, Ohio. (July 1994, EPA/600/4-91/002).
\9\ Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Marine and Estuarine Organisms. Second Edition.
Environmental Monitoring Systems Laboratory, U.S. Environmental Protection Agency, Cincinnati, Ohio (July 1994, EPA/600/4-91/003). These methods do
not apply to marine waters of the Pacific Ocean.
Table 1B.--List of Approved Inorganic Test Procedures
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
Reference (method number or page)
-----------------------------------------------------------------------------------------------------------------------------------------------------------
Parameter, units and method Standard methods
EPA 1,3,5 [Edition(s)] ASTM USGS 2 Other
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
1. Acidity, as CaCO3, mg/L:
Electrometric endpoint or 305.1 2310 B(4a) [18th, 19th, D1067-92 I-1020-85
phenolphthalein endpoint. 20th].
2. Alkalinity, as CaCO3, mg/L:
Electrometric or Colormetric 310.1 2320 B [18th, 19th, D1067-92 I-1030-85 973.43.3
titration to pH 4.5, manual or 20th].
automatic.
310.2 ....................... ...................................... I-2030-85
3. Aluminum--Total,4 mg/L; Digestion
4 followed by:
AA direct aspiration 36......... 202.1 3111 D [18th, 19th].... ...................................... I-3051-85
AA furnace...................... 202.2 3113 B [18th, 19th]....
Inductively Coupled Plasma/ 5 200.7 3120 B [18th, 19th, ...................................... I-4471-97 50
Atomic Emission Spectrometry 20th].
(ICP/AES) 36.
Direct Current Plasma (DCP) 36.. ........... ....................... D4190-94 ..................................... Note 34.
Colorimetric (Eriochrome cyanine 3500-Al B [
R). 20th] and
3500-Al D
[18th,
19th]
4. Ammonia (as N), mg/L:
[[Page 3476]]
Manual, distillation (at pH 9.5) 350.2 4500-NH3 B [18th, 19th, ...................................... ..................................... 973.49.3
6 followed by: 20th].
Nesserization................... 350.2 4500-NH3 [18th]........ D1426-98(A) I-3520-85 973.49.3
Titration....................... 350.2 4500-NH3C [19th, 20th]
and 4500-NH3 C [18th].
Electrode....................... 350.3 4500-NH3 D or E [19th, D1426-98(B)
20th] and 4500-NH3 F
or G [18th].
Automated phenate, or........... 350.1 4500-NH3 G [19th, 20th] ...................................... I-4523-85
and 4500-NH2 H [18th].
Automated electrode............. ........... ....................... ...................................... ..................................... Note 7.
5. Anitomy--Total,4 mg/L; Digestion
4 followed by:
AA direct aspiration 36......... 204.1 3111 B [18th, 19th]....
AA furnace...................... 204.2 3113 B [18th, 19th]....
ICP/AES 36...................... 200.7 5 3120 B [18th, 19th,
20th].
6. Arsenic--Total,4 mg/L:
Digestion 4 followed by......... 206.5
AA gaseous hydride.............. 206.3 3114 B 4.d [18th, 19th] D2972-97(B) I-3062-85
AA furnace...................... 206.2 3113 B [18th, 19th].... D2972-97(C) I-4063-9849
ICP/AES 36 or................... 200.7 5 3120 B [18th, 19th,
20th].
Colorimetric (SDDC)............. 206.4 3500-As B [20th] and 2972-97(A) I-3060-85
3500-As C [18th, 19th].
7. Barium--Total,\4\ mg/L; Digestion
4 followed by:
AA direct aspiration 14......... 208.1 3111 D [18th, 19th].... ...................................... I-3084-85
AA furnace...................... 208.2 3113 B [18th, 19th].... 4382-95
ICP/AES 14...................... 200.7 5 3120 B [18th, 19th,
20th].
DCP 14.......................... ........... ....................... ...................................... ..................................... Note 34.
8. Beryllium--Total,4 mg/L;
Digestion 4 followed by:
AA direct aspiration............ 210.1 3111 D [18th, 19th].... D3645-93(88)(A) I-3095-85
AA furnace...................... 210.2 3113 B [18th, 19th].... D3645-93(88)(B)
ICP/AES......................... 200.7 5 3120 B [18th, 19th, ...................................... I-4471-97 50
20th].
DCP, or......................... ........... ....................... D4190-94 ..................................... Note 34.
Colorimetric (aluminon)......... ........... 3500-Be D [18th, 19th].
9. Biochemical oxygen demand (BOD5),
mg/L:
Dissolved Oxygen Depletion...... 405.1 5210 B [18th, 19th, ...................................... 1-1578-78 8 973.44,3 p. 17.9
20th].
10. Boron 37--Total, mg/L:
Colorimetric (curcumin)......... 212.3 4500-B B [18th, 19th ...................................... I-3112-85
20th].
[[Page 3477]]
ICP/AES, or..................... 200.7 5 3120 B [18th, 19th, ...................................... I-4471-97 50
20th] 20th].
DCP............................. ........... ....................... D4190-94 ..................................... Note 34.
11. Bromide, mg/L:
Titrimetric..................... 320.1 ....................... D1246-95(C) I-1125-85 p. S44.10
12. Cadmium--Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration \36\....... 213.1 3111 B or C [18th, D3557-95 (A or B) I-3135-85 or I-3136-85. 974.27,\3\ p. 37.\9\
19th].
AA furnace...................... 213.2 3113 B [18th, 19th].... D3557-95(D) I-4138-89 \44\
ICP/AES \36\.................... 200.7 5 3120 B [18th, 19th, ...................................... I-4471-97 \50\ .....................................
20th].
DCP \36\........................ ........... ....................... D4190-94 ..................................... Note 34.
Voltametry,\11\ or.............. ........... ....................... D3557-95(C) ..................................... .....................................
Colorimetric (Dithizone)........ ........... 3550-Cd D [18th, 19th]. ...................................... .....................................
13. Calcium--Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration............ 215.1 3111 B [18th, 19th].... D511-93(B) I-3152-85
ICP/AES......................... 200.7 5 3120 B [18th, 19th, ...................................... I-4471-97 \50\
20th].
DCP, or......................... ........... ....................... ...................................... ..................................... Note 34.
Titrimetric (EDTA).............. 215.2 3500-Ca B [20th] and D551-93(A)
3500-Ca D [19th, 20th].
14. Carbonaceous biochemical oxygen
demand (CBOD 5), mg/L: \12\
Dissolved Oxygen Depletion with ........... 521 B [18th, 19th,
nitrification inhibitor. 20th].
15. Chemical oxygen demand (COD), mg/
L;
Titrimetric,................... 410.1 5220 C [18th, 19th, D1252-95(A) I-3560-85 973.46,\3\ p. 17.\9\
20th].
or.............................. 410.2 ....................... ...................................... I-3562-85 .....................................
410.3 ...................................... ..................................... .....................................
Spectrophotometric, manual or 410.4 5220 D [18th, 19th, D1252-95(B) I-3561-85 Notes 13, 14.
automatic. 20th].
16. Chloride, mg/L:
Titrimetric (silver nitrate) or ........... 4500-Cl B [18th, 19th, D512-89(B) I-1183-85 .....................................
20th].
(Mercuric nitrate).............. 325.3 4500-Cl C [18th, 19th, D512-89(A) I-1184-85 973.51.\3\
20th].
Colorimetric, manual or......... ........... ....................... ...................................... I-1187-85 .....................................
Automated (Ferricyanide)........ 325.1 or 4500-Cl E [18th, 19th, ...................................... I-2187-85 .....................................
325.2 20th].
17. Chlorine--Total residual, mg/L;
Titrimetric:
Amperometric direct............. 330.1 4500-Cl D [18th, 19th, D1253-86(92) ..................................... .....................................
20th].
Iodometric direct............... 330.3 4500-Cl B [18th, 19th, ...................................... ..................................... .....................................
20th].
Back titration ether end-point 330.2 4500-Cl C [18th, 19th, ...................................... ..................................... .....................................
\15\ or. 20th].
DPD-FAS......................... 330.4 4500-Cl F [18th, 19th, ...................................... ..................................... .....................................
20th].
[[Page 3478]]
Spectrophotometric, DPD Or 330.5 4500-Cl G [18th, 19th, ...................................... ..................................... Note 16.
Electrode. 20th].
18. Chromium VI dissolved, mg/L;
0.45 micron filtration followed
by:
AA chelaation-extraction or 218.4 3111 C [18th, 19th].... ...................................... I-1232-85 .....................................
Colorimetric (Diphenylcarbazide) ........... 3500-Cr B [20th] and... D1687-92(A) I-1230-85D
3500-Cr D [18th, 19th].
19. Chromium--Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration \36\....... 218.1 3111 B [18th, 19th].... D1687-92(B) I-3236-85 974.27.\3\
AA chelation-extraction......... 218.3 3111 C [18th, 19th].... ...................................... ..................................... .....................................
AA furnace...................... 218.2 3113 B [18th, 19th].... D1687-92(C) I-3233-93 \46\ .....................................
ICP/AES \36\.................... 200.7 5 3120 B [18th, 19th, ...................................... ..................................... .....................................
20th].
DCP,\36\ or..................... ........... ....................... D4190-94 ..................................... Note 34.
Colorimetric (Diphenylcarbazide) 3500-Cr B
[20th and
3500-Cr D
[18th,
19th]
20. Cobalt--Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration............ 219.1 3111 B or C [18th, D3558-94(A or B) I-3239-85 p. 37.\9\
19th].
AA furnace...................... 219.2 3113 B [18th, 19th].... D3558-94(C) I-4243-89 \44\ .....................................
ICP/AES......................... 200.7 5 3120 B [18th, 19th, ...................................... I-4471-97 \50\ .....................................
20th].
DCP............................. ........... ....................... D4190-94 ..................................... Note 34.
21. Color platinum cobalt units or
dominant wavelength, hue, luminance
purity:
Colorimetric (ADMI), or 110.1 2120 E [18th, 19th, ...................................... ..................................... Note 18.
(Platinum cobalt), or 20th].
Spectrophotometric.............. 110.2 2120 B [18th, 19th, ...................................... I-1250-85 .....................................
20th].
110.3 2120 C [18th, 19th, ...................................... ..................................... .....................................
20th].
22. Copper--Total,\4\ mg/L;
Digestion4 followed by:
AA direct aspiration \36\....... 220.1 3111 B or C [18th, D1688-95(A or B) I-3270-85 or I-3271-85 974.27 \3\ p. 37.\9\
19th].
AA furnace...................... 220.2 3113 B [18th, 19th].... D1688-95(C) I-4274-89 \44\
ICP/AES \36\.................... 200.7 5 3120 B [18th, 19th, ...................................... I-4471-97 \44\
20th].
DCP \36\ or..................... ........... ....................... D-4190-94 ..................................... Note 34.
Colorimetric (Neocuproine) or... ........... 3500-Cu B [20th] and ...................................... ..................................... .....................................
3500 Cu D [18th, 19th].
(Bicinchoninate)................ ........... 3500-Cu C [20th] and ...................................... ..................................... Note 19.
3500-As B [18th, 19th].
23. Cyanide--Total, mg/L:
Manual distillation with MgCl22 ........... 4500-CN C [18th, 19th, D2036-98(A) ..................................... .....................................
followed by. 20th].
[[Page 3479]]
Titrimetric, or................. ........... 4500-CN D [18th, 19th, ...................................... ..................................... p. 22.\9\
20th].
Spectrophotometric, manual or... \31\ 335.2 4500-CN E [18th, 19th, D2036-98(A). I-3300-85
20th].
Automated \20\.................. \31\ 335.3 ....................... ...................................... I-4327-85
24. Cyanide amenable to
chlorination, mg/L:
Manual distillation with MgCl2 335.1 4500-CN G [18th, 19th, D2036-98(B)
followed by titrimetric or 20th].
Spectrophotometric.
25. Fluoride--Total, mg/L:
Manual distillation \6\ followed ........... 4500-F B [18th, 19th, ......................................
by. 20th].
Electrode, manual or............ 340.2 4500-F C [18th, 19th, D1179-93(B)
20].
Automated....................... ........... ....................... ...................................... I-4327-85
Colorimetric (SPADNS)........... 340.1 4500-F D [18th, 19th, D1179-93(A)
20th].
Or Automated complexone......... 340.3 4500-F E [18th, 19th,
20th].
26. Gold--Total,\4\ mg/L; Digestion
\4\ followed by:
AA direct aspiration............ 231.1 3111 B [18th, 19th]....
AA furnace, or DCP.............. 231.2
.............................. ........... ....................... ...................................... ..................................... Note 34.
27. Hardness--Total, as CaCO23, mg/L
Automated colorimetric,......... 130.1
Titrimetric (EDTA), or Ca plus 130.2 2340 B or C [18th, D1126-86(92) I-1338-85 973.52B.\3\
Mg as their carbonates, by 19th, 20th].
inductively coupled plasma or
AA direct aspiration. (See
Parameters 13 and 33)..
28. Hydrogen ion (pH), pH units
Electrometric measurement, or 150.1 4500-H+ B [18th, 19th, D1293-84 (90)(A or B) I-1586-85 973.41.\3\
Automated electrode. 20th].
.............................. ........... ....................... ...................................... I-2587-85 Note 21.
29. Iridium--Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration or AA 235.1 3111 B [18th, 19th]....
furnace. 235.2..................
30. Iron--Total,\4\ mg/L; Digestion
\4\ followed by:
AA direct aspiration \36\....... 236.1 3111 B or C [18th, D1068-96(A or B) I-3381-85 974.27.\3\
19th].
AA furnace...................... 236.2 3113 B [18th, 19th].... D1068-96(C) ICP/AES \36\ 200.7 5 I-4471-97 \50\
DCP \36\ or..................... ........... ....................... D4190-94 ..................................... Note 34.
Colorimetric (Phenanthroline)... ........... 3500-Fe B [20th] and D1068-96(D) ..................................... Note 22.
3500-Fe D [18th, 19th].
31. Kjeldahl Nitrogen--Total, (as
N), mg/L:
[[Page 3480]]
Digestion and distillation 351.3 4500-N2org B or C and D3590-89(A)
followed by:. 4500-NH23 B [18th,
19th, 20th].
Titration....................... 351.3 ....................... D3590-89(A) ..................................... 973.48 \3\
Nesslerization.................. 351.3 4500-NH23 C [18th]..... D3590-89(A)
Electrode....................... 351.3 4500-NH23 C [19th, ...................................... .....................................
20th] and 4500-NH3 E
[18th].
Automated phenate colorimetric.. 351.1 4500-NH23 D or E [19th, I-4551-78 \8\
20th] and 4500-NH23 F
or G [18th].
Semi-automated block digestor 351.2 ....................... D3590-89(B) I-4515-91 \45\
colorimetric.
Manual or block digestor 351.4 ....................... D3590-89(A)
potentiometric.
Block Digester, followed by:
Auto distillation and Titration, ........... ....................... ...................................... Note 40.
or Nesslerization.
Flow injection gas diffusion.... 973.483 ....................... ...................................... ..................................... Note 41.
32. Lead--Total,\4\ mg/L; Digestion
\4\ followed by:
AA direct aspiration \36\....... 239.1 3111 B or C [18th, D3559-96(A or B) I-3399-85 974.27.\3\
19th].
AA furnace...................... 239.2 3113 B [18th, 19th].... D3559-96(D) I-4403-89 \44\
ICP/AES \36\.................... 200.7 5 3120 B [18th, 19th, ...................................... I-4471-9750
20th].
DCP \36\........................ ........... ....................... D4190-94 ..................................... Note 34.
Voltametry \11\ or.............. ........... ....................... D3559'96(C)
Colorimetric (Dithizone)........ ........... 3500-Pb B [ 20th] and ...................................... .....................................
3500-Pb D [18th, 19th].
33. Magnesium--Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration............ 242.1 3111 B [18th, 19th].... D511-93(B) I-3447-85 974.27.\3\
ICP/AES......................... 200.7 5 3120 B [18th, 19th, ...................................... I-4471-97 \50\
20th].
DCP or.......................... ........... ....................... ...................................... ..................................... Note 34.
Gravimetric..................... ........... 3500-Mg D [18th, 19th].
34. Manganese--Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration \36\....... 243.1 3111 B [18th, 19th].... D858-95(A or B) I-3454-85 974.27.\3\
AA furnace...................... 243.2 3113 B [18th, 19th].... D858-95(C)
ICP/AES \36\.................... 200.7 5 3120 B [18th, 19th, ...................................... I-4471-97 \50\
20th].
DCP,\36\ or..................... ........... ....................... D4190-94 ..................................... Note 34.
Colorimetric (Persulfate), or... 3500-Mn B [ 3500-Mn D [18th, 19th]. ...................................... ..................................... 920.203.\3\
20th] and
(Periodate)..................... ........... ....................... ...................................... ..................................... Note 23.
35. Mercury--Total,\4\ mg/L:
Cold vapor, manual or........... 245.1 3112 B [18th, 19th].... D3223-91 I-3462-85 977.22.\3\
Automated....................... 245.2
[[Page 3481]]
Oxidation, purge and trap, and \43\ 1631
cold vapor atomic fluorescence
spectrometry (ng/L).
36. Molybdenum--Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration............ 246.1 3111 D [18th, 19th].... ...................................... I-3490-85
AA furnace...................... 246.2 3113 B [18th, 19th].... ...................................... I-3492-96 \47\
ICP/AES......................... 200.7 5 3120 B [18th, 19th, ...................................... I-4471-97 \50\
20th].
DCP............................. ........... ....................... ...................................... ..................................... Note 34.
37. Nickel--Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration \36\....... 249.1 3111 B or C [18th, D1886-90(A or B) I-3499-85
19th].
AA furnace...................... 249.2 3113 B [18th, 19th].... D1886-90(C) I-4503-89 \44\
ICP/AES \36\.................... 200.7 5 3120 B [18th, 19th, ...................................... I-4471-97 \50\
20th].
DCP,\36\ or..................... ........... ....................... D4190-94 ..................................... Note 34.
Colorimetric (heptoxime)........ ........... 3500-Ni D [17th].......
38. Nitrate (as N), mg/L:
Colorimetric (Brucine sulfate), 352.1 ....................... ...................................... ..................................... 973.50,\3\ 419D,\17\ p. 28.\9\
or Nitrate-nitrite N minus
Nitrite N (See parameters 39
and 40).
39. Nitrate-nitrite (as N), mg/L:
Cadmium reduction, Manual or.... 353.3 4500-NO3-E [18th, 19th, D3867-99(B)
20th].
Automated, or................... 353.2 4500-NO3-F [18th, 19th, D3867-99(A) I-4545-85
20th].
Automated hydrazine............. 353.1 4500-NO3-H [18th, 19th,
20th].
40. Nitrite (as N), mg/L;
Spectrophotometric:
Manual or....................... 354.1 4500-NO2-B [18th, 19th, ...................................... ..................................... Note 25.
20th].
Automated (Diazotization)....... ........... ....................... ...................................... I-4540-85
41. Oil and grease--Total
recoverable, mg/L:
Gravimetric (extraction)........ 413.1 5520B [18th, 19th,
20th] \38\.
Oil and grease and non-polar 5520B [18th, 19th,
material, mg/L: Hexane 20th] \39\.
extractable material (HEM): n-
Hexane extraction and
gravimetry \42\. 1664A
Silica gel treated HEM (SGT-
HEM): Silica gel treatment and
gravimetry \42\.
1664A
42. Organic carbon--Total (TOC), mg/
L:
Combustion or oxidation......... 415.1 5310 B, C, or D [18th, D2579-93 (A or B) ..................................... 973.47,\3\ p. 14.\24\
19th, 20th].
43. Organic nitrogen (as N), mg/L:
[[Page 3482]]
Total Kjeldahl N (Parameter 31)
minus ammonia N (Parameter 4).
44. Orthophosphate (as P), mg/L;
Ascorbic acid method:
Automated, or................... 365.1 4500-P F [18th, 19th, ...................................... I-4601-85 973.56.\3\
20th].
Manual single reagent........... 365.2 4500'P E [18th, 19th, D515-88(A) ..................................... 973.55.\3\
20th].
Manual two reagent.............. 365.3 .......................
45. Osmium--Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration, or........ 252.1 3111 D [18th, 19th]....
AA furnace...................... 252.2 .......................
46. Oxygen, dissolved, mg/L:
Winkler (Azide modification), or 360.2 4500-O C [18th, 19th, D888-92(A) I-1575-78 \8\ 973.45B.\3\
20th].
Electrode....................... 360.1 4500-O G [18th, 19th, D888-92(B) I-1576-78 \8\
20th].
47. Palladium--Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration, or........ 253.1 3111 B [18th, 19th].... ...................................... ..................................... p. S27.\10\
AA furnace...................... 253.2 ....................... ...................................... ..................................... p. S28.\10\
DCP............................. ........... ....................... ...................................... ..................................... Note 34.
48. Phenols, mg/L:
Manual distillation \26\........ 420.1 ....................... ...................................... ..................................... Note 27.
Followed by:
Colorimetric (4AAP) manual, or.. 420.1 ....................... ...................................... ..................................... Note 27.
Automated \19\.................. 420.2 ....................... ......................................
49. Phosphorus (elemental), mg/L:
Gas-liquid chromatography....... ........... ....................... ...................................... ..................................... Note 28.
50. Phosphorus--Total, mg/L:
Persulfate digestion followed by 365.2 4500-P B, 5 [18th, ...................................... ..................................... 973.55.\3\
19th, 20th].
Manual or....................... 365.2 or 4500-P E [18th, 19th, D515-88(A)
365.3 20th].
Automated ascorbic acid 365.1 4500-P F [18th, 19th, ...................................... 1--4600-85 973.56.\3\
reduction. 20th].
Semi-automated block digestor... 365.4 ....................... D515-88(B) I-4610-91 \48\
51. Platinum--Total,\4\ mg/L:
Digestion \4\ followed by:
AA direct aspiration............ 255.1 3111 B [18th, 19th]....
AA furnace...................... 255.2
DCP............................. ........... ....................... ...................................... ..................................... Note 34.
52. Potassium--Total,\4\ mg/L:
Digestion \4\ followed by:
AA direct aspiration............ 258.1 3111 B [18th, 19th].... ...................................... I-3630-85 973.53.3.\3\
ICP/AES......................... 200.7 5 3120 B [18th, 19th,
20th].
[[Page 3483]]
Flame photometric, or........... ........... 3500-K B [20th] and
3500-K D [18th, 19th].
Colorimetric.................... ........... ....................... ...................................... ..................................... 317 B.\17\
53. Residue--Total, mg/L:
Gravimetric, 103-105 deg........ 160.3 2540 B [18th, 19th, ...................................... I-3750-85
20th].
54. Residue--filterable, mg/L:
Gravimetric, 180 deg............ 160.1 2540 C [18th, 19th, ...................................... I-1750-85
20th].
55. Residue--nonfilterable (TSS), mg/
L:
Gravimetric, 103-105 deg. post 160.2 2540 D [18th, 19th, ...................................... I-3765-85
washing of residue. 20th].
56. Residue--settleable, mg/L:
Volumetric, (Imhoff cone), or 160.5 2540 F [18th, 19th,
gravimetric. 20th].
57. Residue--Volatile, mg/L:
Gravimetric, 550 deg............ 160.4 ....................... ...................................... I-3753-85
58. Rhodium--Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration, or........ 265.1 3111 B [18th, 19th]....
AA furnace...................... 265.2
59. Ruthenium--Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration, or........ 267.1 3111 B [18th, 19th]....
AA furnace...................... 267.2
60. Selenium--Total,\4\ mg/L;
Digestion \4\ followed by:
AA furnace...................... 270.2 3113 B [18th, 19th].... D3859-98(B) I-4668-98 \49\
ICP/AES,\36\ or................. 200.7 5 3120 B [18th, 19th,
20th].
AA gaseous hydride.............. ........... 3114 B [18th, 19th].... D3859-98(A) I--3667-85
61. Silica \37\--Dissolved, mg/L;
0.45 micron filtration followed by:
Colorimetric, Manual or......... 370.1 4500-SiO2 C [20th] and D859-94 I-1700-85
4500-SiD [18th, 19th].
Automated (Molybdosilicate), or. ........... ....................... ...................................... I-2700-85
ICP............................. 200.7 5 3120 B [18th, 19th, ...................................... I-4471-97 \50\
20th].
62. Silver--Total,\4\ mg/L:
Digestion 4, 29 followed by:
AA direct aspiration............ 272.1 3111 B or C [18th, ...................................... I-3720-85 974.27,\3\ p. 37.\9\
19th].
AA furnace...................... 272.2 3113 B [18th, 19th].... ...................................... I-4724-89 \44\
ICP/AES......................... 200.7 5 3120 B [18th, 19th, ...................................... I-4471-97 \50\
20th].
DCP............................. ........... ....................... ...................................... ..................................... Note 34.
63. Sodium--Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration............ 273.1 3111 B [18th, 19th].... ...................................... I-3735-85 973.54.\3\
ICP/AES......................... 200.7 5 3120 B [18th, 19th, ...................................... I-4471-97\50\
20th].
DCP, or......................... ........... ....................... ...................................... ..................................... Note 34.
[[Page 3484]]
Flame photometric............... ........... 3500 Na B [20th] and
3500 Na D [18th, 19th].
64. Specific conductance, micromhos/
cm at 25 deg. C:
Wheatstone bridge............... 120.1 2510 B [18th, 19th, D1125-95(A) I-2781-85 973.40.\3\
20th].
65. Sulfate (as SO4), mg/L:
Automated colorimetric (barium 375.1
chloranilate).
Gravimetric..................... 375.3 4500-SO4 -2C or D ...................................... ..................................... 925.54.\3\
[18th, 19th, 20th].
Turbidimetric................... 375.4 ....................... D516-90 ..................................... 426C.\30\
66. Sulfide (as S), mg/L:
Titrimetric (iodine), or........ 376.1 4500-S-2F [19th, 20th] ...................................... I-3840-85
or 4500-S-2 E [18th].
Colorimetric (methylene blue)... 376.2 4500-S-2D..............
67. Sulfite (as SO3), mg/L:
Titrimetric (iodine-iodate)..... 377.1 4500-SO3 -2B [18th,
19th, 20th].
68. Surfactants, mg/L:
Colorimetric (methylene blue)... 425.1 5540 C [18th, 19th, D2330-88
20th].
69. Temperature, deg.C:
Thermometric.................... 170.1 2550 B [18th, 19th, ...................................... ..................................... Note 32.
20th].
70. Thallium--Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration............ 279.1 3111 B [18th, 19th.....
AA furnace...................... 279.2
ICP/AES......................... 200.7 5 3120 B [18th, 19th,
20th].
71. Tin--Total,\4\ mg/L; Digestion
\4\ followed by:
AA direct aspiration............ 282.1 3111 B [18th, 19th].... ...................................... I-3850-78 \8\
AA furnace, or.................. 282.2 3113 B [18th, 19th]....
ICP/AES......................... 200.7 5
72. Titanium--Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration............ 283.1 3111 D [18th, 19th]....
AA furnace...................... 283.2
DCP............................. ........... ....................... ...................................... ..................................... Note 34.
73. Turbidity, NTU:
Nephelometric................... 180.1 2130 B [18th, 19th, D1889-94(A) I-3860-85
20th].
74. Vanadium--Total,\4\ mg/L;
Digestion \4\ followed by:
AA direct aspiration............ 286.1 3111 D [18th, 19th]....
AA furnace...................... 286.2 ....................... D3373-93
ICP/AES......................... 200.7 5 3120 B[18th, 19th, ...................................... I-4471-97 \50\
20th].
DCP, or......................... ........... ....................... D4190-94 ..................................... Note 34.
Colorimetric (Gallic Acid)...... ........... 3500-V B [20th] and
3500-V D [18th, 19th].
[[Page 3485]]
75. Zinc--Total,\4\, mg/L; Digestion
\4\ followed by:
AA direct aspiration \36\....... 289.1 3111 B or C [18th, D1691-95(A or B) I-3900-85 974.27,\3\ p. 37.\9\
19th].
AA furnace...................... 289.2
ICP/AES \36\.................... 200.7 5 3120 B [18th, 19th, 20 ...................................... I-4471-97 \50\
\th\].
DCP,\36\ or..................... ........... ....................... D4190-94 ..................................... Note 34.
Colorimetric (Dithizone) or..... ........... 3500-Zn E [18th, 19th].
(Zincon)........................ ........... 3500-Zn B [20th] and ...................................... ..................................... Note 33.
3500-Zn F [18th, 19th].
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
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, 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, 15th ed. (1990).
\4\ For the determination of total metals the sample is not filtered before processing. A digestion procedure is required to solubilize suspended material and to destroy possible organic-metal
complexes. Two digestion procedures are given in ``Methods for Chemical Analysis of Water and Wastes, 1979 and 1983''. One (Section 4.1.3), is a vigorous digestion using nitric acid. A less
vigorous digestion using nitric and hydrochloric acids (Section 4.1.4) is preferred; however, the analyst should be cautioned that this mild digestion may not suffice for all samples types.
Particularly, if a colorimetric procedure is to be employed, it is necessary to ensure that all organo-metallic bonds be broken so that the metal is in a reactive state. In those situations,
the vigorous digestion is to be preferred making certain that at no time does the sample go to dryness. Samples containing large amounts of organic materials may also benefit by this
vigorous digestion, however, vigorous digestion with concentrated nitric acid will convert antimony and tin to insoluble oxides and render them unavailable for analysis. Use of ICP/AES as
well as determinations for certain elements such as antimony, arsenic, the noble metals, mercury, selenium, silver, tin, and titanium require a modified sample digestion procedure and in all
cases the method write-up should be consulted for specific instructions and/or cautions.
NOTE TO TABLE 1B NOTE 4: If the digestion procedure for direct aspiration AA included in one of the other approved references is different than the above, the EPA procedure must be used.
Dissolved metals are defined as those constituents which will pass through a 0.45 micron membrane filter. Following filtration of the sample, the referenced procedure for total metals must be
followed. Sample digestion of the filtrate for dissolved metals (or digestion of the original sample solution for total metals) may be omitted for AA (direct aspiration or graphite furnace)
and ICP analyses, provided the sample solution to be analyzed meets the following criteria:
a. has a low COD (20)
b. is visibly transparent with a turbidity measurement of 1 NTU or less
c. is colorless with no perceptible odor, and
d. is of one liquid phase and free of particulate or suspended matter following acidification.
\5\ The full text of Method 200.7, ``Inductively Coupled Plasma Atomic Emission Spectrometric Method for Trace Element Analysis of Water and Wastes,'' is given at Appendix C of this Part 136.
\6\ Manual distillation is not required if comparability data on representative effluent samples are on company 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, N.Y. 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, Apr. 2, 1975. Available from ANSI, 1430 Broadway, New York, NY 10018.
\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.
\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\ After the manual distillation is completed, the autoanalyzer manifolds in EPA Methods 335.3 (cyanide) or 420.2 (phenols) are simplified by connecting the re-sample line directly to the
sampler. When using the manifold setup shown in Method 335.3, the buffer 6.2 should be replaced with the buffer 7.6 found in Method 335.2.
\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.
[[Page 3486]]
\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\ EPA Methods 335.2 and 335.3 require the NaOH absorber solution final concentration to be adjusted to 0.25 N before colorimetric determination of total cyanide.
\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\ ``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 the Trichlorotrifluorethane (1,1,2-trichloro-1,2,2-trifluoroethane; CFC-113) and n-hexane extraction solvents are approved.
\39\ Nitrogen, Total Kjeldahl, Method PAI-DK01 (Block Digestion, Steam Distillation, Titrimetric Detection), revised 12/22/94, OI Analytical/ALPKEM, PO 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, PO 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, PO 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, Virginia 22161.
\43\ 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\ ``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.
\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) 98-xxx.
\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.
Table 1C.--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)] ASTM Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Acenaphthene.................... 610 625, 1625 610 6440 B, 6410 B [18th, D4657-92 Note 9, p. 27.
19th, 20th].
2. Acenaphthylene.................. 610 625, 1625 610 6440 B, 6410 B [18th, D4657-92 Note 9, p. 27.
19th, 20th].
3. Acrolein........................ 603 604, 1624 \4\ .......... ..................... ...........................
4. Acrylonitrile................... 603 624, 1624 \4\ 610 ..................... ...........................
5. Anthracene...................... 610 625, 1625 610 6410 B 6440 B [18th, D4657-92 Note 9, p. 27.
19th, 20th].
6. Benzene......................... 602 624, 1624 .......... 6200 B [20th] and ...........................
6210 B [18th, 19th],
6200 C [20th] and
6220 B [18th, 19th].
7. Benzidine....................... .......... 625, 1625 \5\ 605 ..................... ..................... Note 3, p.1.
8. Benzo(a)anthracene.............. 610 625, 1625 610 6410 B, 6440 B [18th, D4657-92 Note 9, p. 27.
19th, 20th].
9. Benzo(a)pyrene.................. 610 625, 1625 610 6410 B, 6440 B [18th, D4657-92 Note 9, p. 27.
19th, 20th].
10. Benzo(b)fluoranthene........... 610 625, 1625 610 6410 B 6440 B [18th, D4657-92 Note 9, p. 27.
19th, 20th].
11. Benzo(g, h, i)perylene......... 610 625, 1625 610 6410 B 6440 B [18th, D4657-92 Note 9, p. 27.
19th, 20th].
12. Benzo(k)fluoranthene........... 610 625, 1625 610 6410 B 6440 B [18th, D4657-92 Note 9, p. 27.
19th, 20th].
[[Page 3487]]
13. Benzyl chloride................ .......... ................ .......... ..................... Note 3, p. 130: Note 6, p.
S102.
14. Benzyl butyl phthalate......... 606 625, 1625 .......... 6410 B [18th, 19th, ..................... Note 9, p. 27.
20th].
15. Bis(2-chloroethoxy)methane..... 611 625, 1625 .......... 6410 B [18th, 19th, ..................... Note 9, p. 27.
20th].
16. Bis(2-chloroethyl)ether........ 611 625, 1625 .......... 6410 B [18th, 19th, ..................... Note 9, p. 27.
20th].
17. Bis(2-ethylhexyl)phthalate..... 606 625, 1625 .......... 6200 C [20th] and ..................... Note 9, p. 27
6230 B [18th, 19th],
6410 B [18th, 19th,
20th].
18. Bromodichloromethane........... 601 624, 1624 .......... 6200 C [20th] and ..................... ...........................
6230 B [18th, 19th],
6200 B [20th] and
6210 B [18th, 19th].
19. Bromoform...................... 601 624, 1624 .......... 6200 C [20th] and ..................... ...........................
6230 B [18th, 19th],
6200 B [20th] and
6210 B [18th, 19th].
20. Bromomethane................... 601 624, 1624 .......... 6200 C [20th] and ..................... ...........................
6230 B [18th, 19th],
6200 B [20th] and
6210 B [18th, 19th].
21. 4-Bromophenylphenyl ether...... 611 625, 1625 .......... 6410 B [18th, 19th, ..................... Note 9, p. 27.
20th].
22. Carbon tetrachloride........... 601 624, 1624 .......... 6200 C [20th] and ..................... Note 3, p. 130.
6230 B [18th, 19th],
6410 B [18th, 19th,
20th].
23. 4-Chloro-3-methylphenol........ 604 625, 1625 .......... 6410 B, 6420 B [18th, ..................... Note 9, p. 27.
19th, 20th].
24. Chlorobenzene.................. 601, 602 624, 1624 .......... 6200 B [20th] and ..................... Note 3, p. 130.
6210 B [18th, 19th],
6200 C [20th] and
6220 B [18th, 19th],
6200 C [20th] and
6230 B [18th, 19th].
25. Chloroethane................... 601 624, 1624 .......... 6200 B [20th] and ..................... ...........................
6210 B [18th, 19th],
6200 C [20th] and
6230 B [18th, 19th].
26. 2-Chloroethylvinyl ether....... 601 624, 1624 .......... 6200 B [20th] and ..................... ...........................
6210 B [18th, 19th],
6200 C [20th] and
6230 B [18th 19th].
27. Chloroform..................... 601 624, 1624 .......... 6200 B [20th] and ..................... Note 3, p. 130.
6210 B [18th, 19th],
6200 C [20th] and
6230 B [18th 19th].
28. Chloromethane.................. 601 624, 1624 .......... 6200 B [20th] and ..................... ...........................
6210 B [18th, 19th],
6200 C [20th] and
6230 B [18th 19th].
29. 2-Chloronaphthalene............ 612 625, 1625 .......... 6410 B [18th, 19th, ..................... Note 9, p. 27.
20th].
30. 2-Chlorophenol................. 604 625, 1625 .......... 6410 B [18th, 19th, ..................... Note 9, p. 27.
20th].
31. 4-Chlorophenylphenl ether...... 611 625, 1625 .......... 6410 B [18th, 19th, ..................... Note 9, p. 27.
20th].
32. Chrysene....................... 610 625, 1625 610 6410 B [18th, 19th, D4657-92 Note 9, p. 27.
20th].
33. Dibenzo(a,h)anthracene......... 610 625, 1625 610 6410 B, 6440 B [18th, D4657-92 Note 9, p. 27.
19th, 20th].
34. Dibromochloromethane........... 601 624, 1624 .......... 6200 B [20th] and ..................... ...........................
6210 B [18th, 19th],
6200 C [20th] and
6230 B [18th 19th].
35. 1,2-Dichlorobenzene............ 601, 602, 624, 625, 1625 .......... 6200 B [20th] and ..................... Note 9, p. 27.
612 6220 B [18th, 19th],
6200 C [20th] and
6230 B [18th 19th],
6410 B [18th, 19th,
20th].
36. 1,3-Dichlorobenzene............ 601, 602, 624,625, 1625 .......... 6200 B [20th] and ..................... Note 9, p. 27.
612 6220 B [18th, 19th],
6200 C [20th] and
6230 B [18th 19th],
6410 B [18th, 19th,
20th].
37. 1,4-Dichlorobenzene............ 601, 602, 624, 625, 1625 .......... 6200 B [20th] and ..................... Note 9, p. 27.
612 6220 B [18th, 19th],
6200 C [20th] and
6230 B [18th 19th],
6410 B [18th, 19th,
20th].
38. 3,3-Dichlorobenzidine.......... .......... 625, 1625 605 6410 B [18th, 19th, ..................... ...........................
20th].
39. Dichlorodifuoromethane......... 601 ................ .......... 6200 B [20th] and ..................... ...........................
6230 B [18th, 19th].
40. 1,1-Dichloroethane............. 601 624, 1624 .......... 6200 B [20th] and ..................... ...........................
6210 B [18th, 19th].
[[Page 3488]]
41. 1,2-Dichloroethane............. 601 624, 1624 .......... 6200 B [20th] and ..................... ...........................
6210 B [18th, 19th],
6200 C [20th] and
6230 B [18th, 19th].
42. 1,1-Dichloroethene............. 601 624, 1624 .......... 6200 B [20th] and ..................... ...........................
6210 B [18th, 19th],
6200 C [20th] and
6230 B [18th, 19th].
43. trans 1,2-Dichloroethene....... 601 624, 1624 .......... 6200 B [20th] and ..................... ...........................
6210 B [18th, 19th],
6200 C [20th] and
6230 B [18th, 19th].
44. 2,4-Dichlorophenol............. 604 625, 1625 .......... 6410 B [18th, 19th, ..................... Note 9, p. 27.
20th].
45. 1,2-Dichloropropane............ 601 624, 1624 .......... 6200 B [20th] and ..................... ...........................
6210 B [18th, 19th],
6200 C [20th] and
6230 B [18th, 19th].
46. cis-1,3-Dichloropropene........ 601 624, 1624 .......... 6200 B [20th] and ..................... ...........................
6210 B [18th, 19th],
6200 C [20th] and
6230 B [18th, 19th].
47. trans-1,3-Dichloropropene...... 601 624, 1624 .......... 6200 B [20th] and ..................... ...........................
6210 B [18th, 19th],
6200 C [20th] and
6230 B [18th, 19th].
48. Diethyl phthalate.............. 606 625, 1625 .......... 6410 B [18th, 19th, ..................... Note 9, p. 27.
20th].
49. 2,4-Dimethylphenol............. 604 625, 1625 .......... 6410 B, 6420 B [18th, ..................... Note 9, p. 27.
19th, 20th].
50. Dimethyl phthalate............. 606 625, 1625 .......... 6410 B [18th, 19th, ..................... Note 9, p. 27.
20th].
51. Di-n-butyl phthalate........... 606 625, 1625 .......... 6410 B [18th, ..................... Note 9, p. 27.
phthalate 19th,
20th].
52 Di-n-octyl phthalate............ 606 625, 1625 .......... 6410 B [18th, ..................... Note 9, p. 27.
phthalate 19th,
20th].
53. 2,3-Dinitrophenol.............. 604 625, 1625 .......... 6410 B, 6420 B [18th, .....................
19th, 20th].
54. 2,4-Dinitrotoluene............. 609 625, 1625 .......... 6410 B [18th, 19th, ..................... Note 9, p. 27.
20th].
55. 2,6-Dinitrotoluene............. 609 625, 1625 .......... 6410 B [18th, 19th, ..................... Note 9, p. 27.
20th].
56. Epichlorohydrin................ .......... ................ .......... ..................... ..................... Note 3, p. 130; Note 6, p.
S102.
57. Ethylbenzene................... 602 624, 1624 .......... 6200 B [20th] and
6210 B [18th, 19th],
6200 C [20th] and
6220 B [18th, 19th].
58. Fluoranthene................... 610 625, 1625 610 6410 B, 6440 B [18th, D4657-92 Note 9, p. 27.
19th, 20th].
59. Fluorene....................... 610 625, 1625 610 6410 B, 6440 B [18th, D4657-92 Note 9, p. 27.
19th, 20th].
60. 1,2,3,4,6,7,8- .......... 1613
Heptachlorodibenzofuran.
61. 1,2,3,4,7,8,9- .......... 1613
Heptachlorodibenzofuran.
62. 1,2,3,4,6,7,8- .......... 1613
Heptachlorodibenzo-p-dioxin.
63. Hexachlorobenzene.............. 612 625, 1625 .......... 6410 B [18th, 19th, ..................... Note 9, p. 27.
20th].
64. Hexachlorobutadiene............ 612 625, 1625 .......... 6410 B [18th, 19th, ..................... Note 9, p. 27.
20th].
65. Hexachlorocyclo- pentadiene.... 612 625, 1625B \5\ .......... 6410 B [18th, 19th, ..................... Note 9, p. 27.
20th].
66. 1,2,3,4,7,8- .......... 1613
Hexachlorodibenzofuran.
67. 1,2,3,6,7,8- .......... 1613
Hexachlorodibenzofuran.
68. 1,2,3,7,8,9- .......... 1613
Hexachlorodibenzofuran.
69. 2,3,4,6,7,8- .......... 1613
Hexachlorodibenzofuran.
70. 1,2,3,4,7,8-Hexachlorodibenzo-p- .......... 1613
dioxin.
71. 1,2,3,6,7,8-Hexachlorodibenzo-p- .......... 1613
dioxin.
72. 1,2,3,7,8,9-Hexachlorodibenzo-p- .......... 1613
dioxin.
73. Hexachloroethane............... 616 625, 1625 .......... 6410 B [18th, 19th, ..................... Note 9, p. 27.
20th].
[[Page 3489]]
74. Ideno(1,2,3-cd)pyrene.......... 610 625, 1625 610 6410 B, 6440 B [18th, D4657-92 Note 9, p. 27.
19th, 20th].
75. Isophorone..................... 609 625, 1625 .......... 6410 B [18th, 19th, ..................... Note 9, p. 27.
20th].
76. Methylene chloride............. 601 624, 1624 .......... 6200 C [18th, 19th, ..................... Note 3, p. 130.
20th].
77. 2-Methyl-4,6-dinitrophenol..... 604 625, 1625 .......... 6420 B, 6410 B [18th, ..................... Note 9, p. 27.
19th, 20th].
78. Naphthalene.................... 610 625, 1625 610 6440 B, 6410 B [18th, ..................... Note 9, p. 27.
19th, 20th].
79. Nitrobenzene................... 609 625, 1625 .......... 6410 B [18th, 19th, D4657-92 Note 9, p. 27.
20th].
80. 2-Nitrophenol.................. 604 625, 1625 .......... 6410 B, 6420 B [18th, ..................... Note 9, p. 27.
19th, 20th].
81. 4-Nitrophenol.................. 604 625, 1625 .......... 6410 B, 6420 B [18th, ..................... Note 9, p. 27.
19th, 20th].
82. N-Nitrosodimethylamine......... 607 625, 1625 .......... 6410 B [18th, 19th, ..................... Note 9, p. 27.
20th].
83. N-Nitrosodi-n-propylamine...... 607 625, 1625 \5\ .......... 6410 B [18th, 19th, ..................... Note 9, p. 27.
20th].
84. N-Nitrosodiphenylamine......... 607 625, 1625 \5\ .......... 6410 B [18th, 19th, ..................... Note 9, p. 27.
20th].
85. Octachlorodibenzofuran......... .......... 1613
86. Octachlorodibenzo-p-dioxin..... .......... 1613
87. 2,2-Oxybis(1-chloropropane).... 611 625, 1625 .......... 6410 B [18th, 19th,
20th].
88. PCB-1016....................... 608 625 .......... 6410 B [18th, 19th, ..................... Note 3, p. 43.
20th].
89. PCB-1221....................... 608 625 .......... 6410 B [18th, 19th, ..................... Note 3, p. 43.
20th].
90. PCB-1232....................... 608 625 .......... 6410 B [18th, 19th, ..................... Note 3, p. 43.
20th].
91. PCB-1242....................... 608 625 .......... 6410 B [18th, 19th, ..................... Note 3, p. 43.
20th].
92. PCB-1248....................... 608 625 .......... .....................
93. PCB-1254....................... 608 625 .......... 6410 B [18th, 19th, ..................... Note 3, p. 43.
20th].
94. PCB-1260....................... 608 625 .......... 6410 B, 6630 B [18th, ..................... Note 3, p. 43.
19th, 20th].
95. 1,2,3,7,8- .......... 1613
Pentachlorodibenzofuran.
96. 2,3,4,7,8- .......... 1613
Pentachlorodibenzofuran.
97. 1,2,3,7,8,-Pentachlorodibenzo-p- .......... 1613
dioxin.
98. Pentachlorophenol.............. 604 625, 1625 .......... 6410 B, 6630 B [18th, ..................... Note 3, p. 140; Note 9, p.
19th, 20th]. 27.
99. Phenanthrene................... 610 625, 1625 610 6410 B, 6440 B [18th, D4657-92 Note 9, p. 27.
19th, 20th].
100. Phenol........................ 604 625, 1625 .......... 6420 B, 6410 B [18th, ..................... Note 9, p. 27.
19th, 20th].
101. Pyrene........................ 610 625, 1625 610 6440 B, 6410 B [18th, D4675-92 Note 9, p. 27.
19th, 20th].
102. 2,3,7,8- .......... 1613
Tetrachlorodibenzofuran.
103. 2,3,7,8-Tetrachlorodibenzo-p- .......... 613, 1613 \5\
dioxin.
104. 1,1,2,2- Tetrachlooethane..... 601 624, 1624 .......... 6200 B [20th] and ..................... Note 3, p. 130.
6210 B [18th, 19th],
6200 C [20th] and
6230 B [18th, 19th].
105. Tetrachloroethene............. 601 624, 1624 .......... 6200 C [20th] and ..................... Note 3, p. 130.
6230 B [18th, 19th],
6410 B [18th, 19th,
20th].
106. Toluene....................... 602 624. 1624 .......... 6200 B [20th] and
6210 B [18th, 19th],
6200 C [20th] and
6220 B [18th, 19th].
107. 1,2,4-Trichlorobenzene........ 612 625, 1625 .......... 6410 B [18th, 19th, ..................... Note 3, p. 130; Note 9, p.
20th]. 27.
108. 1,1,1-Trichloroethane......... 601 624, 1624 .......... 6200 B [20th] and
6210 B [18th, 19th],
6200 C [20th] and
6230 B [18th, 19th].
109. 1,1,2-Trichloroethane......... 601 624, 1624 .......... 6200 B [20th] and ..................... Note 3, p. 130.
6210 B [18th, 19th],
6200 C [20th] and
6230 B [18th, 19th].
[[Page 3490]]
110. Trichloroethene............... 601 624, 1624 .......... 6200 B [20th] and
6210 B [18th, 19th],
6200 C [20th] and
6230 B [18th, 19th].
111. Trichlorofluoro- 601 624 .......... 6200 B [20th] and
methane........................ 6210 B [18th, 19th],
6200 C [20th] and
6230 B [18th, 19th].
112. 2,4,6-Trichlorophenol......... 604 625, 1625 .......... 6420 B, 6410 B [18th, ..................... Note 9, p. 27.
19th, 20th].
113. Vinyl chloride................ 601 624, 1624 .......... 6200 B [20th] and
6210 B [18th, 19th],
6200 C [20th] and
6230 B [18th, 19th] .
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table IC notes:
\1\ All parameters are expressed in micrograms per liter (g/L) except for Method 1613 in which the parameters are expressed in picograms per
liter (pg/L).
\2\ The full text of Methods 601-613, 624, 625, 1624, and 1625, are given at Appendix A, ``Test Procedures for Analysis of Organic Pollutants,'' of this
Part 136. The full text of Method 1613 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 1624.
\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 1625, 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, 1624, and 1625 (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 1624 and 1625) 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 and cannot be reported to demonstrate regulatory
compliance.
Note: These warning limits are promulgated as an ``interim final action with a request for comments.''
\8\ ``Organochlorine Pesticides and PCBs in Wastewater Using Empore TM Disk'' 3M Corporation Revised 10/28/94.
\9\ USGS Method 0-3116-87 from ``Methods of Analysis by U.S. Geological Survey National Water Quality Laboratory--Determination of Inorganic and Organic
Constituents in Water and Fluvial Sediments'' U.S. Geological Survey, Open File Report 93-125.
Table 1D.--List of Approved Test Procedures for Pesticides \1\
--------------------------------------------------------------------------------------------------------------------------------------------------------
Standard methods 18th,
Parameter Method EPA 2 7 19th, 20th Ed. ASTM Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Aldrin........................... GC 608 6630 B & C D3086-90 Note 3, p. 7; Note 4,
p. 27; note 8.
GC/MS 625 6410 B ........................... ......................
2. Ametryn.......................... GC ........... ........................... ........................... Note 3, p. 83; Note 6,
p S68.
3. Aminocarb........................ TLC ........... ........................... ........................... Note 3, p. 94; Note 6,
p. S16.
4. Atraton.......................... GC ........... ........................... ........................... Note 3, p. 83; Note 6,
p. S68.
5. Atrazine......................... GC ........... ........................... ........................... Note 3, p. 83; Note 6,
p. S68; Note 9.
6. Azinphos methyl.................. GC ........... ........................... ........................... Note 3, p. 25; Note 6,
p. S51.
7. Barban........................... TLC ........... ........................... ........................... Note 3, p. 104; Note
6, p. S64.
8. -BHC.................... GC 608 6630 B & C 3086-90 Note 3, p. 7; Note 8.
GC/MS 625 \5\ 6410 B ........................... ......................
9. -BHC.................... GC 608 6630 C D3086-90 Note 8.
GC/MS 625 \5\ 6410 B ........................... ......................
10. -BHC................... GC 608 6630 C D3086-90 Note 8.
GC/MS 625 \5\ 6410 B ........................... ......................
11. -BHC (Lindane)......... GC 608 6630 B & C D3086-90 Note 3, p. 7; Note 4,
p. 27; Note 8.
GC/MS 625 6410 B ........................... ......................
12. Captan.......................... GC ........... 6630 B D3086-90 Note 3, p. 7.
13. Carbaryl........................ TLC ........... ........................... ........................... Note 3, p. 94, Note 6,
p. S60.
14. Carbophenothion................. GC ........... ........................... ........................... Note 4, p. 27; Note 6,
p. S73.
15. Chlordane....................... GC 608 6630 B & C D3086-90 Note 3, p. 7; Note 4,
p. 27; Note 8.
GC/MS 625 6410 B ........................... ......................
16. Chloropropham................... TLC ........... ........................... ........................... Note 3, p. 104; Note
6, p. S64.
17. 2,4-D........................... GC ........... 6640 B ........................... Note 3, p. 115; Note
4, p. 40.
18. 4,4'-DDD........................ GC 608 6630 B & C D3086-90 Note 3, p. 7; Note 4,
p. 27; Note 8.
GC/MS 625 6410 B ........................... ......................
19. 4,4'-DDE........................ GC 608 6630 B & C D3086-90 Note 3, p. 7; Note 4,
p. 27; Note 8.
GC/MS 625 6410 B ........................... ......................
20. 4,4'-DDT........................ GC 608 6630 B & C D3086-90 Note 3, p. 7; Note 4,
p. 27; Note 8.
[[Page 3491]]
GC/MS 625 6410 B ........................... ......................
21. Demeton-O....................... GC ........... ........................... ........................... Note 3, p. 25; Note 6,
p. S51.
22. Demeton-S....................... GC ........... ........................... ........................... Note 3, p. 25; Note 6,
p. S51.
23. Diazinon........................ GC ........... ........................... ........................... Note 3, p. 25; Note 4,
p. 27; Note 6, p.
S51.
24. Dicamba......................... GC ........... ........................... ........................... Note 3, p. 115.
25. Dichlofenthion.................. GC ........... ........................... ........................... Note 4, p. 27; Note 6,
p. S73.
26. Dichloran....................... GC ........... 6630 B & C ........................... Note 3, p. 7.
27. Dicofol......................... GC ........... ........................... D3086-90
28. Dieldrin........................ GC 608 6630 B & C ........................... Note 3, p. 7; Note 4,
p. 27; Note 8.
GC/MS 625 6410 B
29. Dioxathion...................... GC ........... ........................... ........................... Note 4, p. 27; Note 6,
p. S73.
30. Disulfoton...................... GC ........... ........................... ........................... Note 3, p. 25; Note 6
p. S51.
31. Diuron.......................... TLC ........... ........................... ........................... Note 3, p. 104; Note
6, p. S64.
32. Endosulfan I.................... GC 608 6630 B & C D3086-90 Note 3, p. 7; Note 4,
p. 27; Note 8.
GC/MS 625 \5\ 6410 B
33. Endosulfan II................... GC 608 6630 B & C D3086-90 Note 3, p. 7; Note 8.
GC/MS 625 \5\ 6410 B
34. Endosulfan Sulfate.............. GC 608 6630 C ........................... Note 8.
GC/MS 625 6410 B
35. Endrin.......................... GC 608 6630 B & C D3086-90 Note 3, p. 7; Note 4,
p. 27; Note 8.
GC/MS 625 \5\ 6410 B
36. Endrin aldehyde................. GC 608 ........................... ........................... Note 8.
GC/MS 625
37. Ethion.......................... GC ........... ........................... ........................... Note 4, p. 27; Note 6,
p. S73.
38. Fenuron......................... TLC ........... ........................... ........................... Note 3, p. 104; Note
6, p. S64.
39. Fenuron-TCA..................... TLC ........... ........................... ........................... Note 3, p. 104; Note
6, p. S64.
40. Heptachlor...................... GC 608 6630 B & C D3086-90 Note 3, p. 7; Note 4,
p. 27; Note 8.
GC/MS 625 6410 B
41. Heptachlor epoxide.............. GC 608 6630 B & C D3086-90 Note 3, p. 7; Note 4,
p. 27; Note 6, p.
S73; Note 8.
GC/MS 625 6410 B
42. Isodrin......................... GC ........... ........................... ........................... Note 4, p. 27; Note 6,
p. S73.
43. Linuron......................... GC ........... ........................... ........................... Note 3, p. 104; Note
6, p. S64.
44. Malathion....................... GC ........... 6630 C ........................... Note 3, p. 25; Note 4,
p. 27; Note 6, p.
S51.
45. Methiocarb...................... TLC ........... ........................... ........................... Note 3, p. 94; Note 6,
p. S60.
46. Methoxychlor.................... GC ........... 6630 B &C D3086-90 Note 3, p. 7; Note 4,
p. 27; Note 8.
47. Mexacarbate..................... TLC ........... ........................... ........................... Note 3, p. 94; Note 6,
p.S60.
48. Mirex........................... GC ........... 6630 B & C ........................... Note 3, p. 7; Note 4,
p. 27.
49. Monuron......................... TLC ........... ........................... ........................... Note 3, p. 104; Note
6, p. S64.
50. Monuron......................... TLC ........... ........................... ........................... Note 3, p. 104; Note
6, p. S64.
51. Nuburon......................... TLC ........... ........................... ........................... Note 3, p. 104; Note
6, p. S64.
52. Parathion methyl................ GC ........... 6630 C ........................... Note 3, p. 25; Note 4,
p. 27.
53. Parathion ethyl................. GC ........... 6630 C ........................... Note 3, p. 25; Note 4,
p. 27.
54. PCNB............................ GC ........... 6630 B & C ........................... Note 3, p. 7.
55. Perthane........................ GC ........... ........................... D3086-90 Note 4, p. 27.
56. Prometron....................... GC ........... ........................... ........................... Note 3, p. 83; Note 6,
p. S68; Note 9.
57. Prometryn....................... GC ........... ........................... ........................... Note 3, p. 83; Note 6,
p. S68; Note 9.
58. Propazine....................... GC ........... ........................... ........................... Note 3, p. 83; Note 6,
p. S68; Note 9.
59. Propham......................... TLC ........... ........................... ........................... Note 3, p. 104; Note
6, p. S64.
60. Propoxur........................ TLC ........... ........................... ........................... Note 3, p. 94; Note 6,
p. S60.
61. Secbumeton...................... TLC ........... ........................... ........................... Note 3, p. 83; Note 6,
p. S68.
62. Siduron......................... TLC ........... ........................... ........................... Note 3, p. 104; Note
6, p. S64.
63. Simazine........................ GC ........... ........................... ........................... Note 3, p. 83; Note 6,
p. S68; Note 9.
64. Strobane........................ GC ........... 6630 B & C ........................... Note 3, p. 7.
65. Swep............................ TLC ........... ........................... ........................... Note 3, p. 104; Note
6, p. S64.
66. 2,4,5-T......................... GC ........... 6640 B ........................... Note 3, p. 115; Note
4, p. 40.
67. 2,4,5-TP (Silvex)............... GC ........... 6640 B ........................... Note 3, p. 115; Note
4, p. 40.
68. Terbuthylazine.................. GC ........... ........................... ........................... Note 3, p. 83; Note 6,
p. S68.
69. Toxaphene....................... GC 608 6630 B & C D3086-90 Note 3, p. 7; Note 4,
p. 27; Note 8.
GC/MS 625 6410B
70. Trifluralin..................... GC ........... 6630 B ........................... Note 3, p. 7; Note 9.
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table ID notes:
\1\ Pesticides are listed in this table by common name for the convenience of the reader. Additional pesticides may be found under Table 1C, 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).
[[Page 3492]]
\5\ The method may be extended to include -BHC, -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 and cannot be reported to demonstrate regulatory compliance. These
quality control requirements also apply to the Standard Methods, ASTM Methods, and other Methods cited.
Note: These warning limits are promulgated as an ``Interim final action with a request for comments.''
\8\ ``Organochlorine Pesticides and PCBs in Wastewater Using Empore\TM\ 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 1E.--List of Approved Radiologic Test Procedures
--------------------------------------------------------------------------------------------------------------------------------------------------------
Reference (method number or page)
----------------------------------------------------------------------------------------------------
Parameter and units Method Standard methods 18th,
EPA \1\ 19th, 20th Ed. ASTM USGS \2\
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Alpha-Total, pCi per liter.. Proportional or 900 7110 B................ D1943-90. pp. 75 and 78.\3\
scintillation
counter.
2. Alpha-Counting error, pCi Proportional or Appendix B 7110 B................ D1943-90 p. 79.
per liter. scintillation
counter.
3. Beta-Total, pCi per liter... Proportional 900.0 7110 B................ D1890-90 pp. 75 and 78.\3\
counter.
4. Beta-Counting error, pCi.... Proportional Appendix B 7110 B................ D1890-90 p. 79.
counter.
5. (a) Radium Total pCi per Proportional 903.0 7500Ra B.............. D2460-90 ..............................
liter. counter.
(b) Ra, pCi per liter.......... Scintillation 903.1 7500Ra C.............. D3454-91 p. 81.
counter.
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table 1E notes:
\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''.
* * * * *
(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). Amer. Publ. Hlth. Assoc.,
1015 15th Street NW., Washington, DC 20005. Table IA, Note 4. Tables
IB, IC, ID, IE.
* * * * *
(10) Annual Book of ASTM Standards, Water, and Environmental
Technology, Section 11, Volumes 11.01 and 11.02, 1994 and 1999 in 40
CFR 136.3, Tables IB, IC, ID, and IE.
* * * * *
(42) USEPA, January 1999 Errata for the Effluent and Receiving
Water Testing Manuals: Acute Toxicity of Effluents and Receiving
Waters to Freshwater and Marine Organisms; Short-Term Methods for
Estimating the Chronic Toxicity of Effluents and Receiving Waters to
Marine and Estuarine Organisms. U.S. Environmental Protection
Agency, Office of Research and Development, Duluth, MN. EPA-600/R-
98-182.
(43) ``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. Available from: U.S. Geological Survey, Denver
Federal Center, Box 25425, Denver, CO 80225. Table IB, Note 44;
Table IC, Note 9.
(44) ``Methods of Analysis by the U.S. Geological Survey
National Water Quality Laboratory--Determination of Ammonium Plus
Organic Nitrogen by a Kjeldahl Digestion Method and an Automated
Photmetric Finish that Includes Digest Cleanup by Gas Diffusion'',
Open File Report (OFR) 00-170. Available from: U.S. Geological
Survey, Denver Federal Center, Box 25425, Denver, CO 80225. Table
IB, Note 45.
(45) ``Methods of Analysis by the U.S. Geological Survey
National Water Quality Laboratory--Determination of Chromium in
Water by Graphite Furnace Atomic Absorption Spectrometry'', Open
File Report (OFR) 93-449. Available from: U.S. Geological Survey,
Denver Federal Center, Box 25425, Denver, CO 80225. Table IB, Note
46.
(46) ``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. Available from: U.S. Geological Survey, Denver
Federal Center, Box 25425, Denver, CO 80225. Table IB, Note 47.
(47) ``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. Available
from: U.S. Geological Survey, Denver Federal Center, Box 25425,
Denver, CO 80225. Table IB, Note 48.
(48) ``Methods of Analysis by the U.S. Geological Survey
National Water Quality Laboratory--Determination of Arsenic and
Selenium in Water and Sediments by Graphite Furnace-Atomic
Absorption Spectrometry'' Open File Report (OFR) 98-639. Table IB,
Note 49.
(49) ``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. Available from: U.S.
Geological Survey, Denver Federal Center, Box 25425, Denver, CO
80225. Table IB, Note 50.
(50) ``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. Available from: U.S. Geological Survey, Denver Federal
[[Page 3493]]
Center, Box 25425, Denver, CO 80225. Table ID, Note 9.
(c) * * *
(d) * * *
(e) * * *
PART 141--NATIONAL PRIMARY DRINKING WATER REGULATIONS
1. 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.
2. Section 141.21 is amended by revising footnote 1 to the table in
paragraph (f)(3) to read as follows:
Sec. 141.21 Coliform sampling.
* * * * *
(f) * * *
(3) * * *
1 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.
* * * * *
3. Section 141.23 is amended by revising the table to read as
follows:
Sec. 141.23 Inorganic chemical sampling and analytical requirements.
* * * * *
(k) * * *
(1) * * *
--------------------------------------------------------------------------------------------------------------------------------------------------------
Contaminant Methodology 1,3 EPA ASTM 3 SM 4 (18th, 19th ed.) SM 4 (20th, ed.) Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Alkalinity................. Titrimetric..... ........ D1067-92B 2320 B 2320 B .....................
Electrometric ........ ................. .......................... ...................... I-1030-85 \5\
titration.
2. Antimony................... Inductively 200.8 \2 ................. .......................... ...................... .....................
Coupled Plasma \
(ICP)-Mass.
Spectrometry.... ........ ................. .......................... ...................... .....................
Hydride-Atomic ........ D3697-92 .......................... ...................... .....................
Absorption.
Atomic 200.9 \2 ................. .......................... ...................... .....................
Absorption; \
Platform.
Atomic ........ ................. 3113 B ...................... .....................
Absorption;
Furnance.
3. Arsenic 4.................. Inductively 200.7 \2 ................. 3120 B 3120 B .....................
Coupled Plasma. \
ICP-Mass 200.8 \2 ................. .......................... ...................... .....................
Spectrometry. \
Atomic 200.9 \2 ................. .......................... ...................... .....................
Absorption; \
Platform.
Atomic ........ D2972-97C 3113 B ...................... .....................
Absorption;
Furnace.
Hydride Atomic ........ D2972-97B 3114 B ...................... .....................
Absorption.
4. Asbestos................... Transmission 100.1 \9 ................. .......................... ...................... .....................
Electron \
Microscopy.
Transmission 100.2 \1 ................. .......................... ...................... .....................
Electron 0\
Microscopy.
5. Barium..................... Inductively 200.7 \2 ................. 3120 B 3120B .....................
Coupled Plasma. \
ICP-Mass 200.8 \2 ................. .......................... ...................... .....................
Spectrometry. \
Atomic ........ ................. 3111 D ...................... .....................
Absorption;
Direct.
Atomic ........ ................. 3113 B ...................... .....................
Absorption;
Furnace.
6. Berylium................... Inductively 200.7 \2 ................. 3120 B 3120B .....................
Coupled Plasma. \
ICP-Mass 200.8 \2 ................. .......................... ...................... .....................
Spectrometry. \
Atomic 200.9 \2 ................. .......................... ...................... .....................
Absorption; \
Platform.
Atomic ........ D3645-97B 3113 B ...................... .....................
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 ...................... .....................
Absorption;
Furnace.
8. Calcium.................... EDTA titrimetric ........ D511-93A 3500-Ca D 3500-Ca .....................
Atomic ........ D511-93B 3111 B ...................... .....................
Absorption;
Direct
Aspiration.
Inductively 200.7 \2 ................. 3120 B 3120 B .....................
Coupled Plasma. \
9. Chromium................... Inductively 200.7 \2 ................. 3120 B 3120 B .....................
Coupled. \
ICP-Mass 200.8 \2 ................. .......................... ...................... .....................
Spectrometry. \
Atomic 200.9 \2 ................. .......................... ...................... .....................
Absorption; \
Platform.
Atomic ........ ................. 3113 B ...................... .....................
Absorption;
Furnace.
10. Copper.................... Atomic ........ D1688-95C 3113 B ...................... .....................
Absorption;
Furnace.
Atomic ........ D1688-95A 3111 B ...................... .....................
Absorption;
Direct
Aspiration.
Inductively 200.7 \2 ................. 3120 B 3120 B .....................
Coupled Plasma. \
ICP-Mass 200.8 \2 ................. .......................... ...................... .....................
spectrometry. \
Atomic 200.9 \2 ................. .......................... ...................... .....................
Absorption; \
Platform.
11. Conductance............... Conductivity.... ........ D1125-95A 2510 B 2510 B
12. Cyanide................... Manual ........ D2036-98A 4500-CN- C 4500-CN- C
Distillation
followed by.
Spectrophotometr ........ D2036-98B 4500-CN- G 4500-CN- G
ic, Amenable.
Spectrophotometr ........ D2036-98A 4500-CN- E 4500-CN- E I-3300-85 \5\
ic Manual.
Spectrophotometr 335.4 \6
ic Semi- \
automated.
Selective Electrode ................ 4500-CN- D4500-CN- F ..........................
F
13. Fluoride.................. Ion 300.0 \6 D4327-97 4110 B 4110 B
Chromatography. \
Manual Distill.; ........ ................. 4500-F- B,D 4500-F- B,D
Color. SPADNS.
Manual Electrode ........ D1179-93B 4500-F- C 4500-F- C
Automated ........ ................. .......................... ...................... 380-75WE \11\
Electrode.
Automated ........ ................. 4500-F - E 4500-F- 129-71W \11\
Alizarin.
14. Lead...................... Atomic ........ D3559-96D 3113 B
Absorption;
Furnace.
[[Page 3494]]
ICP-Mass 200.8 \2
spectrometry. \
Atomic 200.9 \2
Absorption; \
Platform.
Differential ........ ................. .......................... ...................... Method 1001 \15\
Pulse Anodic
Stripping
Voltammetry.
15. Magnesium................. Atomic ........ D511-93 B 3111 B
Absorption.
ICP............. 200.7 \2 ................. 3120 B 3120 B
\
Complexation ........ D511-93 A 3500-Mg E 3500-Mg B
Titrimetric
Methods.
16. Mercury................... Manual, Cold 245.1 \2 D3223-97 3112 B
Vapor. \
Automated, Cold 245.2 \1
Vapor. \
ICP-Mass 200.8 \2
Spectrometry. \
17. Nickel.................... Inductively 200.7 \2 ................. 3120 B 3120 B
Coupled Plasma. \
ICP-Mass 200.8 \2
Spectrometry. \
Atomic 200.9 \2
Absorption; \
Platform.
Atomic ........ ................. 3111 B
Absorption;
Direct.
Atomic ........ ................. 3113 B
Absorption;
Furnace.
18. Nitrate................... Ion 300.0 \6 D4327-97 4110 B 4110 B B-1011 \8\
Chromatography. \
Automated 353.2 \6 D3867-90A 4500-NO3-F 4500-NO3- F
Cadmium \
Reduction.
Ion Selective ........ ................. 4500-NO3- D 4500-NO3- D 601 \7\
Electrode.
Manual Cadmium ........ D3867-90B 4500-NO3- E 4500-NO3- E
Reduction.
19. Nitrite................... Ion 300.0 \6 D4327-97 4110 B 4110 B B-1011 \8\
Chromatography. \
Automated 353.2 \6 D3867-90A 4500-NO3- F 4500- NO3- F
Cadmium \
Reduction.
Manual Cadmium ........ D3867-90B 4500-NO3- E 4500-NO3- E
Reduction.
Spectrophotometr ........ ................. 4500-NO2- B 4500-NO2- B
ic.
20. Ortho-phosphate \12\...... Colorimetric, 365.1 \6 ................. 4500-P F 4500-P F
Automated, \
Ascorbic Acid.
Colorimetric, ........ D515-88A 4500-P E 4500-P E
ascorbic acid,
single reagent.
Colorimetric ........ ................. .......................... ...................... \5\ I-1601-85
Phosphomolybdat
e.
Automated- ........ ................. .......................... ...................... \5\ I-2601-90
segmented Flow.
Automated ........ ................. .......................... ...................... \5\ I-2598-85
Discrete.
Ion 300.0 \6 D4327-97 4110 B 4110 B .....................
Chromatography. \
21. pH........................ Electrometric... 150.1 \1 D1293-95 4500-H\+\ B 4500-H+ B
\
................ 150.2 \1
\
22. Selenium.................. Hydride-Atomic ........ D3859-98A 3114 B
Absorption.
ICP-Mass 200.8 \2
Spectrometry. \
Atomic 200.9 \2
Absorption; \
Platform.
Atomic ........ D3859-98B 3113 B
Absorption;
Furnace.
23. Silica.................... Colorimetric, ........ ................. .......................... ...................... \5\ I-1700-85
Molybdate Blue;.
Automated- ........ ................. .......................... ...................... \5\ I-2700-85
segmented Flow.
Colorimetric.... ........ D859-94
Molybdosilicate. ........ ................. 4500-Si D 4500-SiO2 C
Heteropoly blue. ........ ................. 4500-Si E 4500-SiO2 D
Automated for ........ ................. 4500-Si F 4500-SiO2 E
Molybdate-
reactive Silica.
Inductively 200.7 \2 ................. 3120 B 3120 B
Coupled Plasma. \
24. Sodium.................... Inductively 200.7 \2
Coupled Plasma. \
Atomic ........ ................. 3111 B
Absorption;
Direct
Aspiration.
25. Temperature............... Thermometric.... ........ ................. 2550 2550
26. Thallium.................. ICP-Mass 200.8 \2
Spectrometry. \
Atomic 200.9 \2
Absorption; \
Platform.
--------------------------------------------------------------------------------------------------------------------------------------------------------
\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, or 1999, Vols. 11.01 and 11.02, American Society for Testing and Materials; 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 the American Society for Testing and Materials, 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 Sediments, 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 ed., 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.
[[Page 3495]]
\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\ 10 Method 100.2, ``Determination of Asbestos Structure Over 10-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 L of 30% hydrogen peroxide per 100ml of solution. For direct analysis
of arsenic with method 200.8 using ultrasonic nebulization, samples and standards must contain one mg/L of sodium hypochlorite.
\15\ 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 8053.
4. Section 141.24 is amended by revising the 11th, 12th and last
sentences in paragraph (e)(1), before the Table, to read as follows:
Sec. 141.24 Organic chemicals, sampling and analytical requirements.
* * * * *
(e) * * *
(1) * * * 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 three editions may be used. * * * ASTM Method D 5317-93 is
available in the Annual Book of ASTM Standards (1999), Vol. 11.02,
American Society for Testing and Materials, 100 Barr Harbor Drive, West
Conshohocken, PA 19428, or in any edition published after 1993.
* * * * *
5. 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 or page number)
Contaminant Methodology ------------------------------------------------------------------------------------------------------------------------------------------
EPA \1\ EPA \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 ..............
Gross alpha\11\............... Co-precipitation... ....... .......... 00-02 .......... 7110 C ...................
Radium 226.................... Radon emanation,... 903.1 p 16 Ra-04 p 19 7500-Ra C D 3454-97 R-1141-76 Ra-04 N.Y.\9\
Radiochemical...... 903.0 p 13 Ra-03 .......... 304, 305, 7500-Ra B D 2460-97 R-1140-76 ..............
Radium 228.................... Radiochemical...... 904.0 p 24 Ra-05 p 19 7500-Ra D ................... R-1142-76 .............. N.Y.\9\
................... ....... .......... .......... .......... .................... ................... .................. .............. N.J.\10\
Uranium\12\................... Radiochemical...... 908.0 .......... .......... .......... 7500-U B ...................
Fluorometric....... 908.1 .......... .......... .......... 7500-U C (17th Ed.) D2907-97 R-1180-76 U-04
................... ....... .......... .......... .......... .................... ................... R-1181-76
Alpha spectrometry. ....... .......... 00-07 p 33 7500-U C (18th, 19th D 3972-97 R-1182-76 U-02
or 20th Ed
Laser ....... .......... .......... .......... .................... D 5174-97
Phosphorimetry.
Man-made:
Radioactive cesium............ Radiochemical...... 901.0 p 4 .......... .......... 7500-Cs B D 2459-72 R-1111-76 ..............
Gamma ray 901.1 .......... .......... p 92 7120 D 3649-91 R-1110-76 4.5.2.3
spectrometry.
Radioactive iodine............ Radiochemical...... 902.0 p 6 .......... .......... 7500-I B
................... ....... p 9 .......... .......... 7500-I C
Gamma ray.......... ....... .......... .......... .......... 7500-I D D 3649-91
spectrometry....... 901.1 .......... .......... p 92 7120 D 4785-93 .................. 4.5.2.3
Radioactive................... Radiochemical...... 905.0 p 29 Sr-04 p. 65 303, 7500-Sr B ................... R-1160-76 Sr-01
Strontium 89, 90.............. ................... ....... .......... .......... .......... .................... ................... .................. Sr-02
[[Page 3496]]
Tritium....................... Liquid 906.0 p 34 H-02 p. 87 306, 7500-3H B D 4107-91 R-1171-76 ..............
scintillation.
Gamma emitters................ Gamma ray.......... 901.1 .......... .......... p 92 7120 D 3649-91 R-1110-76 Ga-01-R
Spectrometry....... 902.0 .......... .......... .......... 7500-Cs B D 4785-93
................... 901.0 .......... .......... .......... 7500-I B
------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------
The procedures shall be done in accordance with the documents listed below. The incorporation by reference of documents 1 through 10 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, 401 M Street, SW., Washington, DC 20460 (Telephone: 202-260-3027); or at the
Office of the Federal Register, 800 North Capitol Street, NW., Suite 700, Washington, DC.
\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. PB 253258.
\3\ ``Radiochemistry Procedures Manual'', EPA 520/5-84-006, December, 1987. Available NTIS, ibid. PB 84-215581.
\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 Editions, 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, 7110C, 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, 7500-3H B are in the 17th, 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. Methods 302, 303, 304, 305 and 306 are only in the 13th edition.
\6\ Annual Book of ASTM Standards, Vol. 11.02, 1999; American Society for Testing and Materials; any year containing the cited version of the method may be used. Copies may be obtained from
the American Society for Testing and Materials, 100 Barr Harbor Drive, West Conshohocken, PA 19428.
\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, Volume I and Volume II; 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. 4.5.4.3. 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\ In uranium (U) is determined by mass, a 0.67 pCi/g of uranium conversion factor must be used. This conversion factor is based on the 1:1 activity ration of U-234 and U-238 that
is characteristic of naturally occurring uranium..
6. Section 141.74 is amended by revising the footnote 1 to the
Table in paragraph (a)(1) and by revising the first three sentences of
paragraph (a)(2) to read as follows:
Sec. 141.74 Analytical and monitoring requirements.
(a) * * *
(1) * * *
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.
* * * * *
(2) Public water systems must measure residual disinfectant
concentrations with one of the analytical methods in the following
table. Except for the method for ozone residuals, the disinfectant
residual 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. The ozone method, 4500-O 3 B, is
contained in both the 18th and 19th editions of Standard Methods for
the Examination of Water and Wastewater, 1992, 1995; either edition may
be used. * * *
* * * * *
PART 143--NATIONAL SECONDARY DRINKING WATER REGULATIONS
1. The authority citation for Part 143 continues to read as
follows:
Authority: 42 U.S.C. 300f et seq.
2. Section 143.4 is amended by revising the Table in paragraph (b)
to read as follows:
Sec. 143.4 Monitoring.
* * * * *
(b) * * *
--------------------------------------------------------------------------------------------------------------------------------------------------------
Contaminant EPA ASTM \3\ SM \4\ 18th and 19th ed. SM\4\ 20th ed. Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Aluminum....................... \2\ 200. ..................... 3120 B 3120 B .....................
7
\2\ 200. ..................... 3113 B ............................. .....................
8
\2\ 200. ..................... 3111 D ............................. .....................
9
2. Chloride....................... \1\ 300. D4327-97 4110 B 4110 B .....................
0
........ ..................... 4500-Cl- D 4500-Cl- D .....................
........ D512-89B 4500-Cl- B 4500-Cl- B .....................
3. Color.......................... ........ ..................... 2120 B 2120 B .....................
4. Foaming Agents................. ........ ..................... 5540 C 5540 C .....................
5. Iron........................... \2\ 200. ..................... 3120 B 3120 B .....................
7
[[Page 3497]]
\2\ 200. ..................... 3111 B ............................. .....................
9
........ ..................... 3113 B ............................. .....................
6. Manganese...................... \2\ 200. ..................... 3120 B 3120 B .....................
7
\2\ 200. ..................... 3111 B ............................. .....................
8
\2\200.9 ..................... 3113 B ............................. .....................
7. Odor........................... ........ ..................... 2150 B 2150 B .....................
8. Silver......................... \2\200.7 ..................... 3120 B 3120 B \5\ I-3720-85
\2\ 200. ..................... 3111 B ............................. .....................
8
\2\ 200. ..................... 3113 B ............................. .....................
9
9. Sulfate........................ \1\ 300. D4327-97 4110 B 4110 B .....................
0
\1\ 375. ..................... 4500-SO4\2\- F 4500-SO4\2\- F .....................
2
........ ..................... 4500-SO4\2\- C, D 4500-SO4\2\- C, D .....................
........ D516-90 4500-SO4\2\- E 4500-SO4\2\- E .....................
10. Total Dissolved Solids........ ........ ..................... 2540 C 2540 C .....................
11. Zinc.......................... \2\ 200. ..................... 3120 B 3120 B .....................
7
\2\ 200. ..................... 3111 B ............................. .....................
8
--------------------------------------------------------------------------------------------------------------------------------------------------------
\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, or 1999, Vols. 11.01 and 11.02, American Society for Testing and Materials; any year containing the cited
version of the method may be used. Copies may be obtained from the American Society for Testing and Materials, 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.
[FR Doc. 01-178 Filed 1-12-01; 8:45 am]
BILLING CODE 6560-50-P