[Federal Register Volume 72, Number 57 (Monday, March 26, 2007)]
[Rules and Regulations]
[Pages 14220-14233]
From the Federal Register Online via the Government Publishing Office [www.gpo.gov]
[FR Doc No: 07-1455]
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Part III
Environmental Protection Agency
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40 CFR Parts 136 and 503
Guidelines Establishing Test Procedures for the Analysis of Pollutants;
Analytical Methods for Biological Pollutants in Wastewater and Sewage
Sludge; Final Rule
Federal Register / Vol. 72, No. 57 / Monday, March 26, 2007 / Rules
and Regulations
[[Page 14220]]
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ENVIRONMENTAL PROTECTION AGENCY
40 CFR Parts 136 and 503
[EPA-HQ-OW-2004-0014; FRL-8228-1]
RIN 2040-AE68
Guidelines Establishing Test Procedures for the Analysis of
Pollutants; Analytical Methods for Biological Pollutants in Wastewater
and Sewage Sludge: Final Rule
AGENCY: Environmental Protection Agency (EPA).
ACTION: Final rule.
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SUMMARY: This rule modifies the EPA's Guidelines that establish
approved bacterial testing procedures for analysis and sampling under
the Clean Water Act. EPA proposed these changes for public comment on
August 16, 2005 and April 10, 2006. These changes include approval for
new methods for monitoring microbial pollutants in wastewater and
sewage sludge, including EPA methods, vendor-developed methods and
methods developed by voluntary consensus bodies (VCSB) as well as
updated versions of currently approved methods. The addition of new and
updated methods to the wastewater regulations provides increased
flexibility to the regulated community and laboratories in the
selection of analytical methods. In addition, EPA has made a technical,
non-substantive correction.
DATES: This regulation is effective April 25, 2007. The incorporation
by reference of these methods is approved by the Director of the
Federal Register on April 25, 2007. For judicial review purposes, this
final rule is promulgated as of 1 p.m. (Eastern time) on April 9, 2007
as provided at 40 CFR 23.2 and 23.7.
ADDRESSES: EPA has established a docket for this action under Docket ID
No. EPA-OW-2004-0014. All documents in the docket are listed on the
www.regulations.gov Web site. Although listed in the index, some
information is not publicly available, e.g., CBI or other information
whose disclosure is restricted by statute. Certain other material, such
as copyrighted material, is not placed on the Internet and will be
publicly available only in hard copy form. Publicly available docket
materials are available either electronically through
www.regulations.gov or in hard copy at the HQ Water Docket Center, EPA/
DC, EPA West, Room B102, 1301 Constitution Ave., NW., Washington, DC.
The Public Reading Room is open from 8:30 a.m. to 4:30 p.m., Monday
through Friday, excluding legal holidays. The telephone number for the
Public Reading Room is (202) 566-1744, and the telephone number is
(202) 566-2426.
Note: The EPA Docket Center suffered damage due to flooding
during the last week of June 2006. The Docket Center is continuing
to operate. However, during the cleanup, there will be temporary
changes to Docket Center telephone numbers, addresses, and hours of
operation for people who wish to visit the Public Reading Room to
view documents. Consult EPA's Federal Register notice at 71 FR 38147
(July 5, 2006) or the EPA website at http://www.epa.gov/epahome/dockets.htm for current information on docket status, locations and
telephone numbers.
FOR FURTHER INFORMATION CONTACT: For information regarding the changes
to wastewater regulations, contact Robin K. Oshiro, Engineering and
Analysis Division (4303T), USEPA Office of Science and Technology, 1200
Pennsylvania Ave., NW., Washington, DC 20460, 202-566-1075 (e-mail:
[email protected]).
SUPPLEMENTARY INFORMATION:
A. Potentially Regulated Entities
1. Clean Water Act
EPA Regions, as well as States, Territories and Tribes authorized
to implement the National Pollutant Discharge Elimination System
(NPDES) program, issue permits with conditions designed to ensure
compliance with the technology-based and water quality-based
requirements of the Clean Water Act (CWA). These permits may include
restrictions on the quantity of pollutants that may be discharged as
well as pollutant measurement and reporting requirements. If EPA has
approved test procedures for analysis of a specific pollutant, an NPDES
permittee (or applicant for an NPDES permit) must use an approved test
procedure (or an approved alternate test procedure) for the specific
pollutant when testing for the required waste constituent. Similarly,
if EPA has established permit monitoring requirements, measurements
taken and reported under an NPDES permit must comply with these
requirements. Therefore, entities with NPDES permits will potentially
be regulated by the actions in this rulemaking. Categories and entities
that may potentially be subject to the requirements of today's rule
include:
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Examples of potentially
Category regulated entities
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State, Territorial, and Indian Tribal States, Territories, and Tribes
Governments. authorized to administer the
NPDES permitting program;
States, Territories, and
Tribes providing certification
under Clean Water Act section
401.
Industry............................... Facilities that must conduct
monitoring to comply with
NPDES permits.
Municipalities......................... POTWs that must conduct
monitoring to comply with
NPDES permits.
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This table is not intended to be exhaustive, but rather provides a
guide for readers regarding entities likely to be regulated by this
action. This table lists types of entities that EPA is now aware could
potentially be regulated by this action. Other types of entities not
listed in the table could also be regulated. To determine whether your
facility is regulated by this action, you should carefully examine the
applicability language at 40 CFR 122.1 (NPDES purpose and scope), 40
CFR 136.1 (NPDES permits and CWA), 40 CFR 403.1 (Pretreatment standards
purpose and applicability). If you have questions regarding the
applicability of this action to a particular entity, consult the
appropriate person listed in the preceding FOR FURTHER INFORMATION
CONTACT section.
What process governs judicial review of this rule?
Under Section 509(b)(1) of the Clean Water Act (CWA), judicial
review of today's CWA rule may be obtained by filing a petition for
review in the United States Circuit Court of Appeals within 120 days
from the date of promulgation of this rule. For judicial review
purposes, this final rule is promulgated as of 1 p.m. (Eastern time) on
April 25, 2007 as provided at 40 CFR 23.2. The requirements of this
regulation may also not be challenged later in civil or criminal
proceedings brought by EPA.
Abbreviations and Acronyms Used in the Preamble and Final Rule
AOAC: Association of Official Analytical Chemists International
ASTM: American Society for Testing and Materials International
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CWA: Clean Water Act
EPA: Environmental Protection Agency
VCSB: Voluntary Consensus Standard Body
Table of Contents
I. Statutory Authority
Clean Water Act
II. Summary of Final Rule
A. 40 CFR Part 136
B. 40 CFR Part 503
III. Changes Between the Proposed Rule and the Final Rule
A. Revision to 40 CFR Part 136, Applicability
B. Revision to 40 CFR Part 136, Identification of Test
Procedures
C. Revision to 40 CFR Part 136, Table IA Title
D. Revisions to 40 CFR Part 136, Table II and Footnotes
E. Revisions to 40 CFR Part 503, Sampling and Analysis
IV. Response to Comments
Lack of Connecting Language Between 40 CFR Parts 136 and 503 for
Sewage Sludge Methods
V. Statutory and Executive Order Reviews
A. Executive Order 12866: Regulatory Planning and Review
B. Paperwork Reduction Act
C. Regulatory Flexibility Act
D. Unfunded Mandates Reform Act
E. Executive Order 13132: Federalism
F. Executive Order 13175: Consultation and Coordination with
Indian Tribal Governments
G. Executive Order 13045: Protection of Children from
Environmental Health Risks and Safety Risks
H. Executive Order 13211: Actions that Significantly Affect
Energy Supply, Distribution, or Use
I. National Technology Transfer and Advancement Act
J. Congressional Review Act
I. Statutory Authority
Clean Water Act
EPA is promulgating today's rule pursuant to the authority of
sections 301(a), 304(h), and 501(a) of the Clean Water Act (``CWA'' or
the ``Act''), 33 U.S.C. 1311(a), 1314(h), 1361(a). Section 301(a) of
the Act prohibits the discharge of any pollutant into navigable waters
unless the discharge complies with a National Pollutant Discharge
Elimination System (NPDES) permit issued under section 402 of the Act.
Section 304(h) of the Act requires the Administrator of the EPA to ``*
* * promulgate guidelines establishing test procedures for the analysis
of pollutants that shall include the factors which must be provided in
any certification pursuant to [section 401 of this Act] or permit
application pursuant to [section 402 of this Act].'' Section 501(a) of
the Act authorizes the Administrator to ``* * * prescribe such
regulations as are necessary to carry out this function under [the
Act].'' EPA generally has codified its test procedure regulations
(including analysis and sampling requirements) for CWA programs at 40
CFR Part 136, though some requirements are codified in other Parts
(e.g., 40 CFR Chapter I, Subchapters N and O).
II. Summary of Final Rule
The following sections describe the changes EPA is making in
today's final rule.
A. 40 CFR Part 136
This rule approves new and revised methods for inclusion in 40 CFR
Part 136. These methods include EPA methods, vendor methods submitted
by IDEXX and Hach, and voluntary consensus standards.
The following discussion briefly describes the changes to Part 136
methods approved today.
1. This rule amends the regulations at 40 CFR Part 136 to approve
five E. coli and two enterococci methods for monitoring microbial
pollutants in wastewaters. The E. coli methods include EPA Method 1603
(modified mTEC), and vendor methods Colilert[supreg] and Colilert-
18[supreg], and mColiBlue24[supreg]. The enterococci methods include
EPA Method 1600 (mEI), and vendor method EnterolertTM.
2. The rule approves two fecal coliform and one Salmonella method
for monitoring microbial pollutants in sewage sludge (biosolids). The
fecal coliform methods include EPA Methods 1680 (LT-EC) and 1681 (A-1)
and the Salmonella Method 1682 (Modified MSRV). The methods approved
today are alternative methods to those currently prescribed for
measuring fecal coliform and salmonella in sewage sludge identified in
40 CFR Sec. 503.8(b).
3. The rule amends the regulations by moving the microbial methods
approved for use in ambient waters from Table IA to a new Table IH, and
adding Table IH to section 136.3(a).
4. The rule extends the holding time for fecal coliforms using EPA
Methods 1680 (LTB-EC) or 1681 (A-1) in sewage sludge for Class A
composted, Class B aerobically or anaerobically digested sewage sludge.
5. The rule amends 40 CFR 136.1 to add a new provision that
authorizes the use of the methods identified at 40 CFR 503.8(b) and the
newly approved Part 136 methods for fecal coliform and Salmonella for
permit applications and recordkeeping and reporting required under
EPA's sewage sludge regulations at 40 CFR Part 503.
B. 40 CFR Part 503
This rule amends the regulations at 40 CFR Part 503 by adding a
cross reference to the 40 CFR Part 136 methods in section 503.8(b).
III. Changes Between the Proposed Rule and the Final Rule
Except as noted below, the content of the final rule is the same as
that of the proposed rule. In some instances, EPA revised for clarity
the language of the final rule from that in the proposed rule.
A. Revision to 40 CFR Part 136, Applicability
Based on comment received on the Agency's proposal of methods for
use in sewage sludge, EPA has amended the applicability provision to
clarify that the applicable procedures of Part 136 and Part 503 must be
used for measurements for sewage sludge permit applications and
reporting and recordkeeping requirements under Part 503.
B. Revision to 40 CFR Part 136, Identification of Test Procedures
Section 553 of the Administrative Procedure Act, 5 U.S.C.
553(b)(B), provides that, when an agency for good cause finds that
notice and public procedure are impracticable, unnecessary or contrary
to the public interest, the agency may issue a rule without providing
notice and an opportunity for public comment. EPA has determined that
there is good cause for making today's changes to the rule final
without prior proposal and opportunity for comment. Notice and
opportunity for public comment is not necessary with respect to these
changes because they are not substantive and merely correct errors in
cross-referenced provisions as explained below.
Section 136.3(a) provides that discharge parameter values for which
reports are required must be determined either by the standard
analytical test procedures described in the tables in Part 136 or
approved additional or alternate test procedures. EPA has modified the
language of 40 CFR 136.3(a) to make three corrections. First, EPA has
changed the citation in the last sentence before Table IA from
``paragraphs (b) or (c) of this section or 40 CFR 401.13'' to
``paragraphs (c) of this section, 40 CFR 136.5(a)-(d) and 40 CFR
401.13.'' Paragraph (b) does not describe circumstances in which
alternate procedures may be approved while section 136.5 does.
Second, EPA has deleted the clause at the end of the last sentence
which states that other test procedures may be used
``* * * when such other test procedures have been previously
approved by the Regional Administrator of the Region in which the
discharge will occur, and providing the Director of the State in
which
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the discharge will occur does not object to the use of such
alternate test procedure * * *.''
Only two of the cited provisions require approval by the Regional
Administrator or Director of a State. 40 CFR 401.13 does not because it
pertains to variances of guidelines of national applicability.
The cross-referenced provisions authorize the use of additional or
alternate test procedures in described circumstances. Thus, section
136.3(c) authorizes approval by the Regional Administrator (or Director
of an approved State NPDES Program) for analysis of additional
pollutants or parameters required to be reported for a particular
discharge. Section 136.5(a)-(d) authorizes approval by the Regional
Administrator of alternate procedures for use within a particular EPA
Region. 40 CFR section 401.13 authorizes the use of analytical
procedures that are specifically defined in 40 CFR Parts 402-699. This
last category of analytical procedures that are promulgated for
specific effluent limitations guidelines and pretreatment standards and
not codified in Part 136 do not require the approval of the Director of
a State as the current language erroneously implies.
Third, EPA removed an erroneous reference that was listed as a
source for the methods listed in section 136.3.
EPA has modified the regulation to provide the correct citation and
delete the inaccurate and misleading language. None of the changes EPA
is promulgating today are themselves substantive but rather, as noted,
only either correct an error in citing to the other applicable
provisions of these regulations or correct inaccuracies. The
substantive provisions in question were previously subject to notice
and comment. Thus, notice and public procedures are unnecessary. EPA
finds that this constitutes good cause under 5 U.S.C. 553(b)(B).
C. Revision to 40 CFR Part 136, Table IA Title
The rule revises the title to Table IA from ``List of Approved
Biological Methods'' to ``List of Approved Biological Methods for
Wastewater and Sewage Sludge.'' Today's action updating Table IA at
Sec. 136.3 more clearly defines the removal of approved
microbiological methods for ambient waters from this table. Such
methods have been moved to a new table, Table IH.
D. Revisions to 40 CFR Part 136, Table II and Footnotes
The rule revises Table II (Required Containers, Preservation
Techniques, and Holding Times), and the footnotes to Table II at 40 CFR
136.3(e). Today's action updating Table II at Sec. 136.3(e) more
clearly defines the holding time for bacterial testing as 6 hours
holding time with 2 hours to process samples.
E. Revision to 40 CFR Part 503, Sampling and Analysis
Based on comments received on the Agency's proposal of methods for
use in sewage sludge, EPA is including a cross reference to 40 CFR Part
136 in 40 CFR 503.8(b) which prescribes the methods that must be used
for sampling and analysis of sewage sludge.
IV. Response to Comments
EPA received 39 comments regarding methods included in this final
rule from the August 16, 2005 proposal (70 FR 48256), and 9 comments on
the April 10, 2006 Notice of Data Availability (NODA) (71 FR 18329).
Commentors represented a number of different interests, including
analytical laboratories, water utilities, instrument manufacturers,
State and local governments, trade associations, scientists, and
private citizens. The public docket for this rule includes the Agency's
response to all comments. The majority of the comments were with regard
to method inclusion, method use, and quality control requirements. The
following is a summary of our response to comments about the lack of
connecting language between 40 CFR Parts 136 and 503 for sewage sludge
methods.
EPA proposed to approve methods in 40 CFR Part 136 for sewage
sludge but did not include an appropriate cross reference in 40 CFR
Part 503 to Part 136 so as to allow the use of appropriate 40 CFR 136.3
methods as alternative methods to those listed in 40 CFR 503.8. Based
on comments to the proposal, EPA has amended the language in 40 CFR
503.8(b). In addition, as discussed above, EPA has also amended the
language in 40 CFR 136.1 regarding the applicability of the methods in
this section to 40 CFR Part 503.
V. Statutory and Executive Order Reviews
A. Executive Order 12866: Regulatory Planning and Review
This action is not a ``significant regulatory action'' under the
terms of Executive Order (EO) 12866 (58 FR 51735, October 4, 1993) and
is therefore not subject to review under the EO.
B. Paperwork Reduction Act
This action does not impose an information collection burden under
the provisions of the Paperwork Reduction Act, 44 U.S.C. 3501 et seq.
This rule does not impose any information collection, reporting, or
recordkeeping requirements. This rule merely adds new and updated
versions of testing procedures, withdraws some older testing
procedures, and establishes new sample collection, preservation, and
holding time requirements.
Burden means the total time, effort, or financial resources
expended by persons to generate, maintain, retain, or disclose or
provide information to or for a Federal agency. This includes the time
needed to review instructions; develop, acquire, install, and utilize
technology and systems for the purpose of collecting, validating, and
verifying information, processing and maintaining information, and
disclosing and providing information; adjust the existing ways to
comply with any previously applicable instructions and requirements;
train personnel to be able to respond to a collection of information;
search data sources; complete and review the collection of information;
and transmit or otherwise disclose the information.
An Agency may not conduct or sponsor, and a person is not required
to respond to a collection of information unless it displays a
currently valid OMB control number. The OMB control numbers for EPA's
regulations in 40 CFR are listed in 40 CFR Part 9.
C. Regulatory Flexibility Act
The RFA generally requires an agency to prepare a regulatory
flexibility analysis of any rule subject to notice and comment
rulemaking requirements under the Administrative Procedure Act or any
other statute unless the agency certifies that the rule will not have a
significant economic impact on a substantial number of small entities.
Small entities include small businesses, small organizations, and small
governmental jurisdictions.
For purposes of assessing the impacts of this rule on small
entities for methods under the Clean Water Act, small entity is defined
as: (1) A small business as defined by the Small Business
Administration's (SBA) regulations at 13 CFR 121.201; (2) a small
governmental jurisdiction that is a government of a city, county, town,
school district or special district with a population less than 50,000;
and (3) a small organization that is any not-for-profit enterprise
which is independently owned and operated and is not dominant in its
field.
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.
[[Page 14223]]
This final rule will not impose any requirements on small entities.
This action approves new and updated versions of testing procedures,
withdraws some older testing procedures, and approves new sample
collection, preservation, and holding time requirements. Generally,
these changes will have a positive impact on small entities by
increasing method flexibility, thereby allowing entities to reduce
costs by choosing more cost-effective methods. In some cases,
analytical costs may increase slightly due to the additional QC
requirements included in the methods that are being approved. However,
most laboratories that analyze samples for EPA compliance monitoring
have already instituted QC requirements as part of their laboratory
practices.
D. Unfunded Mandates Reform Act
Title II of the Unfunded Mandates Reform Act of 1995 (UMRA), Public
Law 104-4, establishes requirements for Federal agencies to assess the
effects of their regulatory actions on State, Tribal, and local
governments and the private sector. Under section 202 of the UMRA, EPA
generally must prepare a written statement, including a cost-benefit
analysis, for proposed and final rules with ``Federal mandates'' that
may result in expenditures to State, local, and Tribal governments, in
the aggregate, or to the private sector, of $100 million or more in any
one year. Before promulgating an EPA rule for which a written statement
is needed, section 205 of the UMRA generally requires EPA to identify
and consider a reasonable number of regulatory alternatives and adopt
the least costly, most cost-effective or least burdensome alternative
that achieves the objectives of the rule. The provisions of section 205
do not apply when they are inconsistent with applicable law. Moreover,
section 205 allows EPA to adopt an alternative other than the least
costly, most cost-effective or least burdensome alternative if the
Administrator publishes with the final rule an explanation of why that
alternative was not adopted.
Before EPA establishes any regulatory requirements that may
significantly or uniquely affect small governments, including Tribal
governments, it must have developed under section 203 of the UMRA a
small government agency plan. The plan must provide for the
notification of potentially affected small governments, enabling
officials of affected small governments to have meaningful and timely
input in the development of EPA regulatory proposals with significant
Federal intergovernmental mandates, and informing, educating, and
advising small governments on compliance with the regulatory
requirements.
This rule contains no Federal mandates (under the regulatory
provisions of Title II of UMRA) for State, local, or Tribal governments
or the private sector. The rule imposes no enforceable duty on any
State, local, or Tribal governments or the private sector. In fact,
this rule should (on the whole) save money for governments and the
private sector by increasing method flexibility, and allowing these
entities to reduce monitoring costs by taking advantage of innovations.
Thus, today's rule is not subject to the requirements of Sections 202
and 205 of the UMRA.
EPA has determined that this rule contains no regulatory
requirements that might significantly or uniquely affect small
governments. Generally, this action will have a positive impact by
increasing method flexibility, thereby allowing method users to reduce
costs by choosing more cost effective methods. In some cases,
analytical costs may increase slightly due to changes in methods, but
these increases are neither significant nor unique to small
governments. This rule merely approves new and updated versions of
testing procedures, withdraws some older testing procedures, and
approves new sample collection, preservation, and holding time
requirements. Thus, today's rule is not subject to the requirements of
Section 203 of UMRA.
E. Executive Order 13132: Federalism
Executive Order 13132, entitled ``Federalism'' (64 FR 43255, August
10, 1999), requires EPA to develop an accountable process to ensure
``meaningful and timely input by State and local officials in the
development of regulatory policies that have federalism implications.''
``Policies that have federalism implications'' is defined in the
Executive Order to include regulations that have ``substantial direct
effects on the States, on the relationship between the national
government and the States, or on the distribution of power and
responsibilities among the various levels of government.''
This final rule does not have federalism implications. It will not
have substantial direct effects on the States, on the relationship
between the national government and the States, or on the distribution
of power and responsibilities among the various levels of government,
as specified in Executive Order 13132. This rule merely approves new
and updated versions of testing procedures, withdraws some older
testing procedures, and approves new sample collection, preservation,
and holding time requirements. The costs to State and local governments
will be minimal (in fact, governments may see a cost savings), and the
rule does not preempt State law. Thus, Executive Order 13132 does not
apply to this rule.
In the spirit of Executive Order 13132, and consistent with EPA
policy to promote communications between EPA and State and local
governments, EPA specifically solicited comment on the proposed rule
from State and local officials.
F. Executive Order 13175: Consultation and Coordination With Indian
Tribal Governments
Executive Order 13175, entitled ``Consultation and Coordination
with Indian Tribal Governments'' (65 FR 67249, November 9, 2000),
requires EPA to develop an accountable process to ensure ``meaningful
and timely input by tribal officials in the development of regulatory
policies that have tribal implications.''
This final rule does not have tribal implications, as specified in
Executive Order 13175. It will not have substantial direct effects on
Tribal governments, on the relationship between the Federal government
and Indian tribes, or on the distribution of power and responsibilities
between the Federal government and Indian tribes. This rule merely
approves new and updated versions of testing procedures, withdraws some
older testing procedures, and approves new sample collection,
preservation, and holding time requirements. The costs to Tribal
governments will be minimal (in fact, governments may see a cost
savings), and the rule does not preempt State law. Thus, Executive
Order 13175 does not apply to this rule.
G. Executive Order 13045: Protection of Children From Environmental
Health Risks and Safety Risks
Executive Order 13045: ``Protection of Children from Environmental
Health Risks and Safety Risks'' (62 FR 19885, April 23, 1997) applies
to any rule that: (1) Is determined to be ``economically significant''
as defined under Executive Order 12866, and (2) concerns an
environmental health or safety risk that EPA has reason to believe may
have a disproportionate effect on children. If the regulatory action
meets both criteria, the Agency must evaluate the environmental health
or safety effects of the planned rule on children, and explain why the
planned regulation is preferable to other potentially effective and
reasonably feasible alternatives
[[Page 14224]]
considered by the Agency. This final rule is not subject to the
Executive Order 13045 because it is not economically significant as
defined in Executive Order 12866. Further it does not concern an
environmental health or safety risk that EPA has reason to believe may
have a disproportionate effect on children. This action approves new
and updated versions of testing procedures, withdraws some older
testing procedures, and approves new sample collection, preservation,
and holding time requirements.
H. Executive Order 13211: Actions That Significantly Affect Energy
Supply, Distribution, or Use
This rule is not subject to Executive Order 13211, ``Actions
Concerning Regulations That Significantly Affect Energy Supply,
Distribution, or Use'' (66 FR 28355 (May 22, 2001)) because it is not a
significant regulatory action under Executive Order 12866.
I. National Technology Transfer and Advancement Act
As noted in the proposed rule, Section 12(d) of the National
Technology Transfer and Advancement Act of 1995, (NTTAA), Public Law
104-113, section 12(d) (15 U.S.C. 272 note), directs EPA to use
voluntary consensus standards in its regulatory activities unless to do
so would be inconsistent with applicable law or otherwise impractical.
Voluntary consensus standards are technical standards (e.g., material
specifications, test methods, sampling procedures, and business
practices) that are developed or adopted by voluntary consensus
standard bodies. The NTTAA directs EPA to provide Congress, through the
OMB, explanations when the Agency decides not to use available and
applicable voluntary consensus standards. This rulemaking involves
technical standards. EPA has decided to use E. coli, enterococci and
fecal coliform methods published in Standard Methods and ASTM
International.
The E. coli methods from Standard Methods are method 9223B
(Standard Methods 18th, 19th and 20th Editions) and method 9223 B-97
(Standard Methods Online Edition), as well as AOAC method 991.15. The
enterococci method from ASTM is method D6503-99. The fecal coliform
methods from Standard Methods are methods 9221 C E (Standard Methods
18th, 19th and 20th Editions) and method 9221 C E-99 (Standard Methods
Online Edition). Standard Methods can be obtained from American Public
Health Association, 1015 15th Street, NW., Washington DC 20005, AOAC
methods can be obtained from Association of Official Analytical
Chemists International, 481 North Frederick Avenue, Suite 500,
Gaithersburg, MD 20877-2417, and ASTM methods can be obtained from ASTM
International, 100 Barr Harbor Drive, West Conshohocken, PA 19428.
These newly approved procedures reflect improvements in science and
technology. EPA believes that the addition of these methods offer a
wider variety of options that may be more cost effective to conduct
compliance monitoring of bacterial pollutants.
J. Congressional Review Act
The Congressional Review Act, 5 U.S.C. 801 et seq., as added by the
Small Business Regulatory Enforcement Fairness Act of 1996, generally
provides that before a rule may take effect, the agency promulgating
the rule must submit a rule report, which includes a copy of the rule,
to each House of the Congress and to the Comptroller General of the
United States. EPA will submit a report containing this rule and other
required information to the U.S. Senate, the U.S. House of
Representatives, and the Comptroller General of the United States prior
to publication of the rule in the Federal Register. 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 April 25, 2007.
List of Subjects
40 CFR Part 136
Environmental protection, Incorporation by reference, Reporting and
recordkeeping requirements, Water pollution control.
40 CFR Part 503
Environmental protection, Reporting and recordkeeping requirements,
Waste treatment and disposal, Water pollution control.
Dated: September 28, 2006.
Stephen L. Johnson,
Administrator.
Editorial Note: The Office of the Federal Register received this
document on March 8, 2007.
0
For the reasons set out in the preamble, title 40, chapter I of the
Code of Federal Regulations, is amended as follows:
PART 136--GUIDELINES ESTABLISHING TEST PROCEDURES FOR THE ANALYSIS
OF POLLUTANTS
0
1. The authority citation for Part 136 continues to read as follows:
Authority: Secs. 301, 304(h), 307, and 501(a) Pub. L. 95-217, 91
Stat. 1566, et seq. (33 U.S.C. 1251, et seq.) (The Federal Water
Pollution Control Act Amendments of 1972 as amended by the Clean
Water Act of 1977.)
0
2. Section 136.1 is revised to read as follows:
Sec. 136.1 Applicability.
(a) The procedures prescribed herein shall, except as noted in
Sec. 136.5, be used to perform the measurements indicated whenever the
waste constituent specified is required to be measured for:
(1) An application submitted to the Administrator, or to a State
having an approved NPDES program for a permit under section 402 of the
Clean Water Act of 1977, as amended (CWA), and/or to reports required
to be submitted under NPDES permits or other requests for quantitative
or qualitative effluent data under parts 122 to 125 of title 40, and,
(2) Reports required to be submitted by dischargers under the NPDES
established by parts 124 and 125 of this chapter, and,
(3) Certifications issued by States pursuant to section 401 of the
CWA, as amended.
(b) The procedure prescribed herein and in part 503 of title 40
shall be used to perform the measurements required for an application
submitted to the Administrator or to a State for a sewage sludge permit
under section 405(f) of the Clean Water Act and for recordkeeping and
reporting requirements under part 503 of title 40.
0
3. Section 136.3 is amended as follows:
0
a. By revising paragraph (a) introductory text and Table IA.
0
b. In paragraph (a) by adding Table IH after the notes of Table IG.
0
c. In paragraph (b) by revising the introductory text and by revising
references 2, 6, 10, 11, 34, 38, 39, and 52 through 62; and by adding
references 70 through 72.
0
d. By revising paragraph (e).
Sec. 136.3 Identification of test procedures.
(a) Parameters or pollutants, for which methods are approved, are
listed together with test procedure descriptions and references in
Tables IA, IB, IC, ID, IE, IF, IG, and IH. In the event of a conflict
between the reporting requirements of 40 CFR Parts 122 and 125 and any
reporting requirements associated with the methods listed in these
tables, the provisions of 40 CFR Parts 122 and 125 are controlling and
will determine a permittee's reporting requirements. The full text of
the referenced test procedures are incorporated by reference into
Tables
[[Page 14225]]
IA, IB, IC, ID, IE, IF, IG, and IH. The incorporation by reference of
these documents, as specified in paragraph (b) of this section, was
approved by the Director of the Federal Register in accordance with 5
U.S.C. 552(a) and 1 CFR Part 51. Copies of the documents may be
obtained from the sources listed in paragraph (b) of this section.
Documents may be inspected at EPA's Water Docket, EPA West, 1301
Constitution Avenue, NW., Room B102, Washington, DC (Telephone: 202-
566-2426); or at the National Archives and Records Administration
(NARA). For information on the availability of this material at NARA,
call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html. These test
procedures are incorporated as they exist on the day of approval and a
notice of any change in these test procedures will be published in the
Federal Register. The discharge parameter values for which reports are
required must be determined by one of the standard analytical test
procedures incorporated by reference and described in Tables IA, IB,
IC, ID, IE, IF, IG, and IH or by any alternate test procedure which has
been approved by the Administrator under the provisions of paragraph
(d) of this section and Sec. Sec. 136.4 and 136.5. Under certain
circumstances paragraph (c) of this section, Sec. 136.5(a) through (d)
or 40 CFR 401.13, other additional or alternate test procedures may be
used.
Table IA.--List of Approved Biological Methods for Wastewater and Sewage Sludge
--------------------------------------------------------------------------------------------------------------------------------------------------------
Standard methods
Parameter and units Method \1\ EPA 18th, 19th, 20th Standard methods AOAC, ASTM, USGS Other
ed. online
--------------------------------------------------------------------------------------------------------------------------------------------------------
Bacteria:
1. Coliform (fecal), number Most Probable p. 132 \3\........ 9221 C E.......... 9221 C E-99.......
per 100 mL or number per Number (MPN),\5\ 1680 \12,14\......
gram dry weight. tube 3 dilution, 1681 \12,19\......
or
Membrane filter p. 124 \3\........ 9222 D............ 9222 D-97......... B-0050-85 \5\.....
(MF) \2\, single
step.
2. Coliform (fecal) in MPN, 5 tube, 3 p. 132 \3\........ 9221 C E.......... 9221 C E-99.......
presence of chlorine, dilution, or
number per 100 mL.
MF \2\, single p. 124 \3\........ 9222 D............ 9222 D-97.........
step.
3. Coliform (total), number MPN, 5 tube, 3 p. 114 \3\........ 9221 B............ 9221 B-99.........
per 100 mL. dilution, or
MF \2\, single p. 108 \3\........ 9222 B............ 9222 B-97......... B-0025-8 \5\......
step or two step.
4. Coliform (total), in MPN, 5 tube, 3 p. 114 \3\........ 9221 B............ 9221 B-99.........
presence of chlorine, dilution, or
number per 100 mL.
MF \2\ with p. 111 \3\........ 9222 (B+B.5c)..... 9222 (B+B.5c)-97..
enrichment.
5. E. coli, number per 100 MPN \7,9,15\ .................. 9223 B \13\....... 9223 B-97 \13\.... 991.15 \11\....... Colilert[supreg]\1
mL \20\. multiple tube/ 3,17\
multiple well. Colilert-
18[supreg]\13,16,
17\
MF \2,6,7,8,9\ 1603 \21\......... .................. .................. .................. mColiBlue-
single step. 24[supreg]\18\
6. Fecal streptococci, MPN, 5 tube 3 p. 139 \3\........ 9230 B............ 9230 B-93.........
number per 100 mL. dilution,.
MF \2\, or........ p. 136 \3\........ 9230 C............ 9230 C-93......... B-0055-85 \5\.....
Plate count....... p. 143 \3\........
7. Enterococci, number per MPN \7,9\, .................. .................. .................. D6503-99 \10\..... Enterolert[supreg]
100 mL \20\. multiple tube/ \13,23\
multiple well.
MF \2,6,7,8,9\ 1600 \24\.........
single step.
8. Salmonella, number per MPN multiple tube. 1682 \22\.........
gram dry weight \12\.
Aquatic Toxicity:
9. Toxicity, acute, fresh Ceriodaphnia dubia 2002.0 \25\.......
water organisms, LC 50, acute.
percent effluent.
Daphnia puplex and 2021.0 \25\.......
Daphnia magna
acute.
Fathead Minnow, 2000.0 \25\.......
Pimephales
promelas, and
Bannerfin shiner,
Cyprinella
leedsi, acute.
[[Page 14226]]
Rainbow Trout, 2019.0 \25\.......
Oncorhynchus
mykiss, and brook
trout, Salvelinus
fontinalis, acute.
10. Toxicity, acute, Mysid, Mysidopsis 2007.0 \25\.......
estuarine and marine bahia, acute.
organisms of the Atlantic
Ocean and Gulf of Mexico,
LC50, percent effluent.
Sheepshead Minnow, 2004.0 \25\.......
Cyprinodon
variegatus, acute.
Silverside, 2006.0 \25\.......
Menidia
beryllina,
Menidia menidia,
and Menidia
peninsulae, acute.
11. Toxicity, chronic, fresh Fathead minnow, 1000.0 \26\.......
water organisms, NOEC or Pimephales
IC25, percent effluent. promelas, larval
survival and
growth.
Fathead minnow, 1001.0 \26\.......
Pimephales
promelas, embryo-
larval survival
and
teratogenicity.
Daphnia, 1002.0 \26\.......
Ceriodaphnia
dubia, survival
and reproduction.
Green alga, 1003.0 \26\.......
Selenastrum
capricornutum,
growth.
12. Toxicity, chronic, Sheepshead minnow, 1004.0 \27\.......
estuarine and marine Cyprinodon
organisms of the Atlantic variegatus,
Ocean and Gulf of Mexico, larval survival
NOEC or IC25, percent and growth.
effluent.
Sheepshed minnow, 1005.0 \27\.......
Cyprinodon
variegatus,
embryo-larval
survival and
teratogenicity.
Inland silverside, 1006.0 \27\.......
Menidia
beryllina, larval
survival and
growth.
Mysid, Mysidopsis 1007.0 \27\.......
bahia, survival,
growth, and
fecundity.
Sea urchin, 1008.0 \27\.......
Arbacia
punctulata,
fertilization.
--------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ The method must be specified when results are reported.
\2\ A 0.45 [mu]m membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated and to be free of
extractables which could interfere with their growth.
\3\ USEPA. 1978. Microbiological Methods for Monitoring the Environment, Water, and Wastes. Environmental Monitoring and Support Laboratory, U.S.
Environmental Protection Agency, Cincinnati, OH, EPA/600/8-78/017.
\4\ [Reserved].
\5\ USGS. 1989. U.S. Geological Survey Techniques of Water-Resource Investigations, Book 5, Laboratory Analysis, Chapter A4, Methods for Collection and
Analysis of Aquatic Biological and Microbiological Samples, U.S. Geological Survey, U.S. Department of the Interior, Reston, VA.
\6\ Because the MF technique usually yields low and variable recovery from chlorinated wastewaters, the Most Probable Number method will be required to
resolve any controversies.
\7\ Tests must be conducted to provide organism enumeration (density). Select the appropriate configuration of tubes/filtrations and dilutions/volumes
to account for the quality, character, consistency, and anticipated organism density of the water sample.
[[Page 14227]]
\8\ When the MF method has been used previously to test waters with high turbidity, large numbers of noncoliform bacteria, or samples that may contain
organisms stressed by chlorine, a parallel test should be conducted with a multiple-tube technique to demonstrate applicability and comparability of
results.
\9\ To assess the comparability of results obtained with individual methods, it is suggested that side-by-side tests be conducted across seasons of the
year with the water samples routinely tested in accordance with the most current Standard Methods for the Examination of Water and Wastewater or EPA
alternate test procedure (ATP) guidelines.
\10\ ASTM. 2000, 1999, 1996. Annual Book of ASTM Standards--Water and Environmental Technology. Section 11.02. ASTM International. 100 Barr Harbor
Drive, West Conshohocken, PA 19428.
\11\ AOAC. 1995. Official Methods of Analysis of AOAC International, 16th Edition, Volume I, Chapter 17. Association of Official Analytical Chemists
International. 481 North Frederick Avenue, Suite 500, Gaithersburg, MD 20877-2417.
\12\ Recommended for enumeration of target organism in sewage sludge.
\13\ These tests are collectively known as defined enzyme substrate tests, where, for example, a substrate is used to detect the enzyme [beta]-
glucuronidase produced by E. coli.
\14\ USEPA. July 2006. Method 1680: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation Using Lauryl-Tryptose Broth (LTB) and EC
Medium. US Environmental Protection Agency, Office of Water, Washington, DC EPA-821-R-06-012.
\15\ Samples shall be enumerated by the multiple-tube or multiple-well procedure. Using multiple-tube procedures, employ an appropriate tube and
dilution configuration of the sample as needed and report the Most Probable Number (MPN). Samples tested with Colilert[supreg] may be enumerated with
the multiple-well procedures, Quanti-Tray[supreg] Quanti-Tray[supreg] 2000, and the MPN calculated from the table provided by the manufacturer.
\16\ Colilert-18[supreg] is an optimized formulation of the Colilert[supreg] for the determination of total coliforms and E. coli that provides results
within 18 h of incubation at 35 [deg]C rather than the 24 h required for the Colilert[supreg] test and is recommended for marine water samples.
\17\ Descriptions of the Colilert[supreg], Colilert-18[supreg], Quanti-Tray[supreg], and Quanti-Tray[supreg]/2000 may be obtained from IDEXX
Laboratories, Inc., 1 IDEXX Drive, Westbrook, ME 04092.
\18\ A description of the mColiBlue24[supreg] test, Total Coliforms and E. coli, is available from Hach Company, 100 Dayton Ave., Ames, IA 50010.
\19\ USEPA. July 2006. Method 1681: Fecal Coliforms in Sewage Sludge (Biosolids) by Multiple-Tube Fermentation using A-1 Medium. U.S. Environmental
Protection Agency, Office of Water, Washington, DC EPA-821-R-06-013.
\20\ Recommended for enumeration of target organism in wastewater effluent.
\21\ USEPA. July 2006. Method 1603: Escherichia coli (E. coli) in Water by Membrane Filtration Using Modified membrane-Thermotolerant Escherichia coli
Agar (modified mTEC). U.S. Environmental Protection Agency, Office of Water, Washington, DC EPA-821-R-06-011.
\22\ USEPA. July 2006. Method 1682: Salmonella in Sewage Sludge (Biosolids) by Modified Semisolid Rappaport-Vassiliadis (MSRV) Medium. U.S.
Environmental Protection Agency, Office of Water, Washington, DC EPA-821-R-06-014.
\23\ A description of the Enterolert[supreg] test may be obtained from IDEXX Laboratories, Inc., 1 IDEXX Drive, Westbrook, ME 04092.
\24\ USEPA. July 2006. Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-[beta]-D-Glucoside Agar (mEI). U.S.
Environmental Protection Agency, Office of Water, Washington, DC EPA-821-R-06-009.
\25\ USEPA. October 2002. Methods for Measuring the Acute Toxicity of Effluents and Receiving Waters to Freshwater and Marine Organisms. Fifth Edition.
U.S. Environmental Protection Agency, Office of Water, Washington, DC EPA/821/R-02/012.
\26\ USEPA. October 2002. Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Freshwater Organisms. Fourth
Edition, U.S. Environmental Protection Agency, Office of Water, Washington, DC EPA/821/R-02/013.
\27\ USEPA. October 2002. Short-term Methods for Estimating the Chronic Toxicity of Effluents and Receiving Waters to Marine and Estuarine Organisms.
Third Edition. U.S. Environmental Protection Agency, Office of Water, Washington, DC EPA/821/R-02/014.
* * * * *
Table IH.--List of Approved Microbiological Methods for Ambient Water
--------------------------------------------------------------------------------------------------------------------------------------------------------
Standard methods
Parameter and units Method \1\ EPA 18th, 19th, 20th Standard methods AOAC, ASTM, USGS Other
Ed. online
--------------------------------------------------------------------------------------------------------------------------------------------------------
Bacteria:
1. E. coli, number per 100 MPN \6,8,14\ .................. 9221 B.1/9221 F 9221 B.1-99/9221 F
mL. multiple tube, \11,13\. \11,13\.
Multiple tube/ .................. 9223 B \12\....... 9223 B-97 \12\.... 991.15 \10\....... Colilert[supreg]
multiple well, \12,16\ Colilert-
18[supreg]
\12,15,16\.
MF \2,5,6,7,8\ two 1103.1 \19\....... 9222 B/9222 G 9222 B-97/9222 G D5392-93 \9\......
step, or \18\, 9213 D. \18\.
Single step....... 1603 \20\, 1604 .................. .................. .................. mColiBlue-
\21\. 24[supreg] \17\.
2. Enterococci, number per MPN \6,8\ multiple .................. 9230 B............ 9230 B-93.........
100 mL. tube,
Multiple tube/ .................. .................. .................. D6503-99 \9\...... Enterolert[supreg]
multiple well. \12,22\.
MF \2,5,6,7,8\ two 1106.1 \23\....... 9230 C............ 9230 C-93......... D5259-92 \9\......
step.
Single step, or... 1600 \24\.........
Plate count....... p. 143 \3\........
Protozoa:
3. Cryptosporidium.......... Filtration/IMS/FA. 1622 \25,\1623
\26\.
4. Giardia.................. Filtration/IMS/FA. 1623 \26\.........
--------------------------------------------------------------------------------------------------------------------------------------------------------
\1\ The method must be specified when results are reported.
\2\ A 0.45 [mu]m membrane filter (MF) or other pore size certified by the manufacturer to fully retain organisms to be cultivated and to be free of
extractables which could interfere with their growth.
\3\ USEPA. 1978. Microbiological Methods for Monitoring the Environment, Water, and Wastes. Environmental Monitoring and Support Laboratory, U.S.
Environmental Protection Agency, Cincinnati, OH. EPA/600/8-78/017.
\4\ [Reserved]
\5\ Because the MF technique usually yields low and variable recovery from chlorinated wastewaters, the Most Probable Number method will be required to
resolve any controversies.
\6\ Tests must be conducted to provide organism enumeration (density). Select the appropriate configuration of tubes/filtrations and dilutions/volumes
to account for the quality, character, consistency, and anticipated organism density of the water sample.
[[Page 14228]]
\7\ When the MF method has not been used previously to test waters with high turbidity, large number of noncoliform bacteria, or samples that may
contain organisms stressed by chlorine, a parallel test should be conducted with a multiple-tube technique to demonstrate applicability and
comparability of results.
\8\ To assess the comparability of results obtained with individual methods, it is suggested that side-by-side tests be conducted across seasons of the
year with the water samples routinely tested in accordance with the most current Standard Methods for the Examination of Water and Wastewater or EPA
alternate test procedure (ATP) guidelines.
\9\ ASTM. 2000, 1999, 1996. Annual Book of ASTM Standards--Water and Environmental Technology. Section 11.02. ASTM International. 100 Barr Harbor Drive,
West Conshohocken, PA 19428.
\10\ AOAC. 1995. Official Methods of Analysis of AOAC International, 16th Edition, Volume I, Chapter 17. Association of Official Analytical Chemists
International. 481 North Frederick Avenue, Suite 500, Gaithersburg, MD 20877-2417.
\11\ The multiple-tube fermentation test is used in 9221B.1. Lactose broth may be used in lieu of lauryl tryptose broth (LTB), if at least 25 parallel
tests are conducted between this broth and LTB using the water samples normally tested, and this comparison demonstrates that the false-positive rate
and false-negative rate for total coliform using lactose broth is less than 10 percent. No requirement exists to run the completed phase on 10 percent
of all total coliform-positive tubes on a seasonal basis.
\12\ These tests are collectively known as defined enzyme substrate tests, where, for example, a substrate is used to detect the enzyme [beta]-
glucuronidase produced by E. coli.
\13\ After prior enrichment in a presumptive medium for total coliform using 9221B.1, all presumptive tubes or bottles showing any amount of gas, growth
or acidity within 48 h 3 h of incubation shall be submitted to 9221F. Commercially available EC-MUG media or EC media supplemented in the
laboratory with 50 [mu]g/mL of MUG may be used.
\14\ Samples shall be enumerated by the multiple-tube or multiple-well procedure. Using multiple-tube procedures, employ an appropriate tube and
dilution configuration of the sample as needed and report the Most Probable Number (MPN). Samples tested with Colilert[supreg] may be enumerated with
the multiple-well procedures, Quanti-Tray[supreg] or Quanti-Tray[supreg] 2000, and the MPN calculated from the table provided by the manufacturer.
\15\ Colilert-18[supreg] is an optimized formulation of the Colilert[supreg] for the determination of total coliforms and E. coli that provides results
within 18 h of incubation at 35 [deg]C rather than the 24 h required for the Colilert[supreg] test and is recommended for marine water samples.
\16\ Descriptions of the Colilert[supreg], Colilert-18[supreg], Quanti-Tray[supreg], and Quanti-Tray[supreg]/2000 may be obtained from IDEXX
Laboratories, Inc., 1 IDEXX Drive, Westbrook, ME 04092.
\17\ A description of the mColiBlue24[supreg] test, Total Coliforms and E. coli, is available from Hach Company, 100 Dayton Ave., Ames, IA 50010.
\18\ Subject total coliform positive samples determined by 9222B or other membrane filter procedure to 9222G using NA-MUG media.
\19\ USEPA. July 2006. Method 1103.1: Escherichia coli (E. coli) in Water by Membrane Filtration Using membrane-Thermotolerant Escherichia coli Agar
(mTEC). U.S. Environmental Protection Agency, Office of Water, Washington, DC EPA-821-R-06-010.
\20\ USEPA. July 2006. Method 1603: Escherichia coli (E. coli) in Water by Membrane Filtration Using Modified membrane-Thermotolerant Escherichia coli
Agar (Modified mTEC). U.S. Environmental Protection Agency, Office of Water, Washington, DC EPA-821-R-06-011.
\21\ Preparation and use of MI agar with a standard membrane filter procedure is set forth in the article, Brenner et al. 1993. ``New Medium for the
Simultaneous Detection of Total Coliform and Escherichia coli in Water.'' Appl. Environ. Microbiol. 59:3534-3544 and in USEPA. September 2002.: Method
1604: Total Coliforms and Escherichia coli (E. coli) in Water by Membrane Filtration by Using a Simultaneous Detection Technique (MI Medium). U.S.
Environmental Protection Agency, Office of Water, Washington, DC EPA 821-R-02-024.
\22\ A description of the Enterolert[supreg] test may be obtained from IDEXX Laboratories, Inc., 1 IDEXX Drive, Westbrook, ME 04092.
\23\ USEPA. July 2006. Method 1106.1: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus-Esculin Iron Agar (mE-EIA). U.S.
Environmental Protection Agency, Office of Water, Washington, DC EPA-821-R-06-008.
\24\ USEPA. July 2006. Method 1600: Enterococci in Water by Membrane Filtration Using membrane-Enterococcus Indoxyl-[beta]-D-Glucoside Agar (mEI). U.S.
Environmental Protection Agency, Office of Water, Washington, DC EPA-821-R-06-009.
\25\ Method 1622 uses filtration, concentration, immunomagnetic separation of oocysts from captured material, immunofluorescence assay to determine
concentrations, and confirmation through vital dye staining and differential interference contrast microscopy for the detection of Cryptosporidium.
USEPA. 2001. Method 1622: Cryptosporidium in Water by Filtration/IMS/FA. U.S. Environmental Protection Agency, Office of Water, Washington, DC EPA-821-
R-01-026.
\26\ Method 1623 uses filtration, concentration, immunomagnetic separation of oocysts and cysts from captured material, immunofluorescence assay to
determine concentrations, and confirmation through vital dye staining and differential interference contrast microscopy for the simultaneous detection
of Cryptosporidium and Giardia oocysts and cysts. USEPA. 2001. Method 1623. Cryptosporidium and Giardia in Water by Filtration/IMS/FA. U.S.
Environmental Protection Agency, Office of Water, Washington, DC EPA-821-R-01-025.
(b) The full texts of the methods from the following references
which are cited in Tables IA, IB, IC, ID, IE, IF, IG and IH are
incorporated by reference into this regulation and may be obtained from
the source identified. All costs cited are subject to change and must
be verified from the indicated source. The full texts of all the test
procedures cited are available for inspection at the National Archives
and Records Administration (NARA). For information on the availability
of this material at NARA, call 202-741-6030, or go to: http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html.
References, Sources, Costs, and Table Citations
* * * * *
(2) 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. Available at http://www.epa.gov/clariton/srch.htm or
from: National Technical Information Service, 5285 Port Royal Road,
Springfield, Virginia 22161, Pub. No. PB-290329/A.S. Table IA, Note 3;
Table IH, Note 3.
* * * * *
(6) American Public Health Association. 1992, 1995, and 1998.
Standard Methods for the Examination of Water and Wastewater. 18th,
19th, and 20th Edition (respectively). Available from: American Public
Health Association, 1015 15th Street, NW., Washington, DC 20005.
Standard Methods Online is available through the Standard Methods Web
site (http://www.standardmethods.org). Tables IA, IB, IC, ID, IE, and
IH.
* * * * *
(10) ASTM International. Annual Book of ASTM Standards, Water, and
Environmental Technology, Section 11, Volumes 11.01 and 11.02, 1994,
1996, 1999, Volume 11.02, 2000, and individual standards published
after 2000. Available from: ASTM International, 100 Barr Harbor Drive,
P.O. Box C700, West Conshohocken, PA 19428-2959, or http://www.astm.org. Tables IA, IB, IC, ID, IE, and IH.
* * * * *
(11) USGS. 1989. U.S. Geological Survey Techniques of Water-
Resources Investigations, Book 5, Laboratory Analysis, Chapter A4,
Methods for Collection and Analysis of Aquatic Biological and
Microbiological Samples, U.S. Geological Survey, U.S. Department of the
Interior, Reston, Virginia. Available from USGS Books and Open-File
Reports Section, Federal Center, Box 25425, Denver, Colorado 80225.
Table IA, Note 5; Table IH.
* * * * *
(34) USEPA. October 2002. Methods for Measuring the Acute Toxicity
of Effluents and Receiving Waters to Freshwater and Marine Organisms.
Fifth Edition. U.S. Environmental Protection Agency, Office of Water,
Washington, DC EPA 821-R-02-012. Available at http://www.epa.gov/
epahome/index/
[[Page 14229]]
sources.htm or from National Technical Information Service, 5285 Port
Royal Road, Springfield, Virginia 22161, Pub. No. PB2002-108488. Table
IA, Note 25.
* * * * *
(38) USEPA. October 2002. Short-Term Methods for Measuring the
Chronic Toxicity of Effluents and Receiving Waters to Freshwater
Organisms. Fourth Edition. U.S. Environmental Protection Agency, Office
of Water, Washington, DC EPA 821-R-02-013. Available at http://www.epa.gov/epahome/index/sources.htm or from National Technical
Information Service, 5285 Port Royal Road, Springfield, Virginia 22161,
Pub. No. PB2002-108489. Table IA, Note 26.
(39) USEPA. October 2002. Short-Term Methods for Measuring the
Chronic Toxicity of Effluents and Receiving Waters to Marine and
Estuarine Organisms. Third Edition. U.S. Environmental Protection
Agency, Office of Water, Washington, DC EPA 821-R-02-014. Available at
http://www.epa.gov/epahome/index/sources.htm or from National Technical
Information Service, 5285 Port Royal Road, Springfield, Virginia 22161,
Pub. No. PB2002-108490. Table IA, Note 27.
* * * * *
(52) IDEXX Laboratories, Inc. 2002. Description of Colilert[reg],
Colilert-18[reg], Quanti-Tray[reg], Quanti-Tray[reg]/2000,
Enterolert[reg] methods are available from IDEXX Laboratories, Inc.,
One Idexx Drive, Westbrook, Maine 04092. Table IA, Notes 17 and 23;
Table IH, Notes 16 and 22.
(53) Hach Company, Inc. Revision 2, 1999. Description of m-
ColiBlue24[reg] Method, Total Coliforms and E. coli, is available from
Hach Company, 100 Dayton Ave, Ames IA 50010. Table IA, Note 18; Table
IH, Note 17.
(54) USEPA. July 2006. Method 1103.1: Escherichia coli (E. coli) in
Water by Membrane Filtration Using membrane-Thermotolerant Escherichia
coli Agar (mTEC). U.S. Environmental Protection Agency, Office of
Water, Washington DC EPA-621-R-06-010. Available at http://www.epa.gov/waterscience/methods/. Table IH, Note 19.
(55) USEPA. July 2006. Method 1106.1: Enterococci in Water by
Membrane Filtration Using membrane-Enterococcus-Esculin Iron Agar (mE-
EIA). U.S. Environmental Protection Agency, Office of Water, Washington
DC EPA-621-R-06-008. Available at http://www.epa.gov/waterscience/methods/. Table IH, Note 23
(56) USEPA. July 2006. Method 1603: Escherichia coli (E. coli) in
Water by Membrane Filtration Using Modified membrane-Thermotolerant
Escherichia coli Agar (Modified mTEC). U.S. Environmental Protection
Agency, Office of Water, Washington DC EPA-821-R-06-011. Available at
http://www.epa.gov/waterscience/methods/. Table IH, Note 19; Table IH,
Note 20.
(57) Brenner et al. 1993. New Medium for the Simultaneous Detection
of Total Coliforms and Escherichia coli in Water. Appl. Environ.
Microbiol. 59:3534-3544. Available from the American Society for
Microbiology, 1752 N Street NW., Washington DC 20036. Table IH, Note
21.
(58) USEPA. September 2002. Method 1604: Total Coliforms and
Escherichia coli (E. coli) in Water by Membrane Filtration Using a
Simultaneous Detection Technique (MI Medium). U.S. Environmental
Protection Agency, Office of Water, Washington DC EPA-821-R-02-024.
Available at http://www.epa.gov/waterscience/methods/. Table IH, Note
20.
(59) USEPA. July 2006. Method 1600: Enterococci in Water by
Membrane Filtration Using membrane-Enterococcus Indoxyl-[beta]-D-
Glucoside Agar (mEI). U.S. Environmental Protection Agency, Office of
Water, Washington DC EPA-821-R-06-009. Available at http://www.epa.gov/waterscience/methods/. Table IA, Note 24; Table IH, Note 24.
(60) USEPA. April 2001. Method 1622: Cryptosporidium in Water by
Filtration/IMS/FA. U.S. Environmental Protection Agency, Office of
Water, Washington DC EPA-821-R-01-026. Available at http://www.epa.gov/waterscience/methods/. Table IH, Note 25.
(61) USEPA. April 2001. Method 1623: Cryptosporidium and Giardia in
Water by Filtration/IMS/FA. U.S. Environmental Protection Agency,
Office of Water, Washington DC. EPA-821-R-01-025. Available at http://www.epa.gov/waterscience/methods/. Table IH, Note 26.
(62) AOAC. 1995. Official Methods of Analysis of AOAC
International, 16th Edition, Volume I, Chapter 17. AOAC International,
481 North Frederick Avenue, Suite 500, Gaithersburg, Maryland 20877-
2417. Table IA, Note 11; Table IH.
* * * * *
(70) USEPA. July 2006. Method 1680: Fecal Coliforms in Sewage
Sludge (Biosolids) by Multiple-Tube Fermentation using Lauryl Tryptose
Broth (LTB) and EC Medium. U.S. Environmental Protection Agency, Office
of Water, Washington DC. EPA 821-R-06-012. Available at http://www.epa.gov/waterscience/methods/.
(71) USEPA. July 2006. Method 1681: Fecal Coliforms in Sewage
Sludge (Biosolids) by Multiple-Tube Fermentation using A-1 Medium. U.S.
Environmental Protection Agency, Office of Water, Washington DC. EPA
821-R-06-013. Available at http://www.epa.gov/waterscience/methods/.
(72) USEPA. July 2006. Method 1682: Salmonella in Sewage Sludge
(Biosolids) by Modified Semisolid Rappaport-Vassiliadis (MSRV) Medium.
U.S. Environmental Protection Agency, Office of Water, Washington DC.
EPA 821-R-06-014. Available at http://www.epa.gov/waterscience/methods/
.
* * * * *
(e) Sample preservation procedures, container materials, and
maximum allowable holding times for parameters are cited in Tables IA,
IB, IC, ID, IE, IF, IG and IH are prescribed in Table II. Information
in the table takes precedence over information in specific methods or
elsewhere. Any person may apply for a variance from the prescribed
preservation techniques, container materials, and maximum holding times
applicable to samples taken from a specific discharge. Applications for
variances may be made by letters to the Regional Administrator in the
Region in which the discharge will occur. Sufficient data should be
provided to assure such variance does not adversely affect the
integrity of the sample. Such data will be forwarded by the Regional
Administrator, to the Alternate Test Procedure Program Coordinator,
Washington, DC, for technical review and recommendations for action on
the variance application. Upon receipt of the recommendations from the
Alternate Test Procedure Program Coordinator, the Regional
Administrator may grant a variance applicable to the specific discharge
to the applicant. A decision to approve or deny a variance will be made
within 90 days of receipt of the application by the Regional
Administrator.
[[Page 14230]]
Table II.--Required Containers, Preservation Techniques, and Holding Times
----------------------------------------------------------------------------------------------------------------
Maximum holding time
Parameter No./name Container \1\ Preservation \2,3\ \4\
----------------------------------------------------------------------------------------------------------------
Table IA--Bacterial Tests:
1-5. Coliform, total, fecal, and PA, G.................. Cool, <10 [deg]C, 6 hours.\22,23\
E. coli. 0.0008% Na2S2O3 \5\.
6. Fecal streptococci............ PA, G.................. Cool, <10 [deg]C, 6 hours.\22\
0.0008% Na2S2O3 \5\.
7. Enterococci................... PA, G.................. Cool, <10 [deg]C, 6 hours.\22\
0.0008% Na2S2O3 \5\.
8. Salmonella.................... PA, G.................. Cool, <10 [deg]C, 6 hours.\22\
0.0008% Na2S2O3 \5\.
Table IA--Aquatic Toxicity Tests:
9-11. Toxicity, acute and chronic P, FP, G............... Cool, <=6 [deg]C \16\.. 36 hours.
Table lB--Inorganic Tests:
1. Acidity....................... P, FP, G............... Cool, <=6 [deg]C \18\.. 14 days.
2. Alkalinity.................... P, FP, G............... Cool, <=6 [deg]C \18\.. 14 days.
4. Ammonia....................... P, FP, G............... Cool, <=6 [deg]C \18\, 28 days.
H2SO4 to pH<2.
9. Biochemical oxygen demand..... P, FP, G............... Cool, <=6 [deg]C \18\.. 48 hours.
10. Boron........................ P, FP, or Quartz....... HNO3 to pH<2........... 6 months.
11. Bromide...................... P, FP, G............... None required.......... 28 days.
14. Biochemical oxygen demand, P, FP G................ Cool, <=6 [deg]C \18\.. 48 hours.
carbonaceous.
15. Chemical oxygen demand....... P, FP, G............... Cool, <=6 [deg]C \18\, 28 days.
H2SO4 to pH<2.
16. Chloride..................... P, FP, G............... None required.......... 28 days.
17. Chlorine, total residual..... P, G................... None required.......... Analyze within 15
minutes.
21. Color........................ P, FP, G............... Cool, <=6 [deg]C \18\.. 48 hours.
23-24. Cyanide, total or P, FP, G............... Cool, <=6 [deg]C \18\, 14 days.
available (or CATC). NaOH to pH>12 \6\,
reducing agent \5\.
25. Fluoride..................... P...................... None required.......... 28 days.
27. Hardness..................... P, FP, G............... HNO3 or H2SO4 to pH<2.. 6 months.
28. Hydrogen ion (pH)............ P, FP, G............... None required.......... Analyze within 15
minutes.
31, 43. Kjeldahl and organic N... P, FP, G............... Cool, <=6 [deg]C \18\, 28 days.
H2SO4 to pH<2.
Table IB--Metals: \7\
18. Chromium VI.................. P, FP, G............... Cool, <=6 [deg]C \18\, 28 days.
pH = 9.3-9.7 \20\.
35. Mercury (CVAA)............... P, FP, G............... HNO3 to pH<2........... 28 days.
35. Mercury (CVAFS).............. FP, G; and FP-lined cap 5 mL/L 12N HCl or 5 mL/ 90 days.\17\
\17\. L BrCl \17\.
3, 5-8, 12, 13, 19, 20, 22, 26, P, FP, G............... HNO3 to pH<2, or at 6 months.
29, 30, 32-34, 36, 37, 45, 47, least 24 hours prior
51, 52, 58-60, 62, 63, 70-72, to analysis \19\.
74, 75.
Metals, except boron, chromium
VI, and mercury.
38. Nitrate...................... P, FP, G............... Cool, <=6 [deg]C \18\.. 48 hours.
39. Nitrate-nitrite.............. P, FP, G............... Cool, <=6 [deg]C \18\, 28 days.
H2SO4 to pH<2.
40. Nitrite...................... P, FP, G............... Cool, <=6 [deg]C \18\.. 48 hours.
41. Oil and grease............... G...................... Cool to <=6 [deg]C 28 days.
\18\, HCl or H2SO4 to
pH<2.
42. Organic Carbon............... P, FP, G............... Cool to <=6 [deg]C 28 days.
\18\, HCl, H2SO4, or
H3PO4 to pH<2.
44. Orthophosphate............... P, FP, G............... Cool, <=6 [deg]C \18\.. Filter within 15
minutes; Analyze
within 48 hours.
46. Oxygen, Dissolved Probe...... G, Bottle and top...... None required.......... Analyze within 15
minutes.
47. Winkler...................... G, Bottle and top...... Fix on site and store 8 hours.
in dark.
48. Phenols...................... G...................... Cool, <=6 [deg]C \18\, 28 days.
H2SO4 to pH<2.
49. Phosphorous (elemental)...... G...................... Cool, <=6 [deg]C \18\.. 48 hours.
50. Phosphorous, total........... P, FP, G............... Cool, <=6 [deg]C \18\, 28 days.
H2SO4 to pH<2.
53. Residue, total............... P, FP, G............... Cool, <=6 [deg]C \18\.. 7 days.
54. Residue, Filterable.......... P, FP, G............... Cool, <=6 [deg]C \18\.. 7 days.
55. Residue, Nonfilterable (TSS). P, FP, G............... Cool, <=6 [deg]C \18\.. 7 days.
56. Residue, Settleable.......... P, FP, G............... Cool, <=6 [deg]C \18\.. 48 hours.
57. Residue, Volatile............ P, FP, G............... Cool, <=6 [deg]C \18\.. 7 days.
61. Silica....................... P or Quartz............ Cool, <=6 [deg]C \18\.. 28 days.
64. Specific conductance......... P, FP, G............... Cool, <=6 [deg]C \18\.. 28 days.
65. Sulfate...................... P, FP, G............... Cool, <=6 [deg]C \18\.. 28 days.
66. Sulfide...................... P, FP, G............... Cool, <=6 [deg]C \18\, 7 days.
add zinc acetate plus
sodium hydroxide to
pH>9.
67. Sulfite...................... P, FP, G............... None required.......... Analyze within 15
minutes.
68. Surfactants.................. P, FP, G............... Cool, <=6 [deg]C \18\.. 48 hours.
69. Temperature.................. P, FP, G............... None required.......... Analyze.
73. Turbidity.................... P, FP, G............... Cool, <=6 [deg]C \18\.. 48 hours.
Table lC--Organic Tests \8\
[[Page 14231]]
13, 18-20, 22, 24-28, 34-37, 39- G, FP-lined septum..... Cool, <=6 [deg]C \18\, 14 days.
43, 45-47, 56, 76, 104, 105, 108- 0.008% Na2S2O3 \5\.
111, 113. Purgeable Halocarbons.
6, 57, 106. Purgeable aromatic G, FP-lined septum..... Cool, <=6 [deg]C \18\, 14 days.\9\
hydrocarbons. 0.008% Na2S2O3 \5\,
HCl to pH 2 \9\.
3, 4. Acrolein and acrylonitrile. G, FP-lined septum..... Cool, <=6 [deg]C \18\, 14 days.\10\
0.008% Na2S2O3 \5\, pH
to 4-5 \10\.
23, 30, 44, 49, 53, 77, 80, 81, G, FP-lined cap........ Cool, <=6 [deg]C \18\, 7 days until
98, 100, 112. Phenols \11\. 0.008% Na2S2O3 \5\. extraction, 40 days
after extraction.
7, 38. Benzidines \11,\ \12\..... G, FP-lined cap........ Cool, <=6 [deg]C \18\, 7 days until
0.008% Na2S2O3 \5\. extraction.\13\
14, 17, 48, 50-52. Phthalate G, FP-lined cap........ Cool, <=6 [deg]C \18\.. 7 days until
esters \11\. extraction, 40 days
after extraction.
82-84. Nitrosamines \11,\ \14\... G, FP-lined cap........ Cool, <=6 [deg]C \18\, 7 days until
store in dark, 0.008% extraction, 40 days
Na2S2O3 \5\. after extraction.
88-94. PCBs \11\................. G, FP-lined cap........ Cool, <=6 [deg]C \18\.. 1 year until
extraction, 1 year
after extraction.
54, 55, 75, 79. Nitroaromatics G, FP-lined cap........ Cool, <=6 [deg]C \18\, 7 days until
and isophorone \11\. store in dark, 0.008% extraction, 40 days
Na2S2O3 \5\. after extraction.
1, 2, 5, 8-12, 32, 33, 58, 59, G, FP-lined cap........ Cool, <=6 [deg]C \18\, 7 days until
74, 78, 99, 101. Polynuclear store in dark, 0.008% extraction, 40 days
aromatic hydrocarbons \11\. Na2S2O3 \5\. after extraction.
15, 16, 21, 31, 87. Haloethers G, FP-lined cap........ Cool, <=6 [deg]C \18\, 7 days until
\11\. 0.008% Na2S2O3 \5\. extraction, 40 days
after extraction.
29, 35-37, 63-65, 107. G, FP-lined cap........ Cool, <=6 [deg]C \18\.. 7 days until
Chlorinated hydrocarbons \11\. extraction, 40 days
after extraction.
60-62, 66-72, 85, 86, 95-97, 102,
103. CDDs/CDFs \11\.
Aqueous Samples: Field and Lab G...................... Cool, <=6 [deg]C \18\, 1 year.
Preservation. 0.008% Na2S2O3 \5\,
pH<9.
Solids and Mixed-Phase Samples: G...................... Cool, <=6 [deg]C \18\.. 7 days.
Field Preservation.
Tissue Samples: Field G...................... Cool, <=6 [deg]C \18\.. 24 hours.
Preservation.
Solids, Mixed-Phase, and Tissue G...................... Freeze, <=-10 [deg]C... 1 year.
Samples: Lab Preservation.
Table lD--Pesticides Tests:
1-70. Pesticides \11\............ G, FP-lined cap........ Cool, <=6 [deg]C \18\, 7 days until
pH 5-9 \15\. extraction, 40 days
after extraction.
Table IE--Radiological Tests:
1-5. Alpha, beta, and radium..... P, FP, G............... HNO3 to pH<2........... 6 months.
Table IH--Bacterial Tests:
1. E. coli....................... PA, G.................. Cool, <10 [deg]C, 6 hours.\22\
0.0008% Na2S2O3 \5\.
2. Enterococci................... PA, G.................. Cool, <10 [deg]C, 6 hours.\22\
0.0008% Na2S2O3 \5\.
Table IH--Protozoan Tests:
8. Cryptosporidium............... LDPE; field filtration. 0-8 [deg]C............. 96 hours.\21\
9. Giardia....................... LDPE; field filtration. 0-8 [deg]C............. 96 hours.\21\
----------------------------------------------------------------------------------------------------------------
\1\ ``P'' is polyethylene; ``FP'' is fluoropolymer (polytetrafluoroethylene (PTFE; Teflon[supreg]), or other
fluoropolymer, unless stated otherwise in this Table II; ``G'' is glass; ``PA'' is any plastic that is made of
a sterlizable material (polypropylene or other autoclavable plastic); ``LDPE'' is low density polyethylene.
\2\ Except where noted in this Table II and the method for the parameter, preserve each grab sample within 15
minutes of collection. For a composite sample collected with an automated sampler (e.g., using a 24-hour
composite sampler; see 40 CFR 122.21(g)(7)(i) or 40 CFR Part 403, Appendix E), refrigerate the sample at <=6
[deg]C during collection unless specified otherwise in this Table II or in the method(s). For a composite
sample to be split into separate aliquots for preservation and/or analysis, maintain the sample at <=6 [deg]C,
unless specified otherwise in this Table II or in the method(s), until collection, splitting, and preservation
is completed. Add the preservative to the sample container prior to sample collection when the preservative
will not compromise the integrity of a grab sample, a composite sample, or an aliquot split from a composite
sample; otherwise, preserve the grab sample, composite sample, or aliquot split from a composite sample within
15 minutes of collection. If a composite measurement is required but a composite sample would compromise
sample integrity, individual grab samples must be collected at prescribed time intervals (e.g., 4 samples over
the course of a day, at 6-hour intervals). Grab samples must be analyzed separately and the concentrations
averaged. Alternatively, grab samples may be collected in the field and composited in the laboratory if the
compositing procedure produces results equivalent to results produced by arithmetic averaging of the results
of analysis of individual grab samples. For examples of laboratory compositing procedures, see EPA Method
1664A (oil and grease) and the procedures at 40 CFR 141.34(f)(14)(iv) and (v) (volatile organics).
[[Page 14232]]
\3\ When any sample is to be shipped by common carrier or sent via the U.S. Postal Service, it must comply with
the Department of Transportation Hazardous Materials Regulations (49 CFR Part 172). The person offering such
material for transportation is responsible for ensuring such compliance. For the preservation requirements of
Table II, the Office of Hazardous Materials, Materials Transportation Bureau, Department of Transportation has
determined that the Hazardous Materials Regulations do not apply to the following materials: Hydrochloric acid
(HCl) in water solutions at concentrations of 0.04% by weight or less (pH about 1.96 or greater); Nitric acid
(HNO3) in water solutions at concentrations of 0.15% by weight or less (pH about 1.62 or greater); Sulfuric
acid (H2SO4) in water solutions at concentrations of 0.35% by weight or less (pH about 1.15 or greater); and
Sodium hydroxide (NaOH) in water solutions at concentrations of 0.080% by weight or less (pH about 12.30 or
less).
\4\ Samples should be analyzed as soon as possible after collection. The times listed are the maximum times that
samples may be held before the start of analysis and still be considered valid (e.g., samples analyzed for
fecal coliforms may be held up to 6 hours prior to commencing analysis). Samples may be held for longer
periods only if the permittee or monitoring laboratory has data on file to show that, for the specific types
of samples under study, the analytes are stable for the longer time, and has received a variance from the
Regional Administrator under Sec. 136.3(e). For a grab sample, the holding time begins at the time of
collection. For a composite sample collected with an automated sampler (e.g., using a 24-hour composite
sampler; see 40 CFR 122.21(g)(7)(i) or 40 CFR Part 403, Appendix E), the holding time begins at the time of
the end of collection of the composite sample. For a set of grab samples composited in the field or
laboratory, the holding time begins at the time of collection of the last grab sample in the set. Some samples
may not be stable for the maximum time period given in the table. A permittee or monitoring laboratory is
obligated to hold the sample for a shorter time if it knows that a shorter time is necessary to maintain
sample stability. See Sec. 136.3(e) for details. The date and time of collection of an individual grab
sample is the date and time at which the sample is collected. For a set of grab samples to be composited, and
that are all collected on the same calendar date, the date of collection is the date on which the samples are
collected. For a set of grab samples to be composited, and that are collected across two calendar dates, the
date of collection is the dates of the two days; e.g., November 14-15. For a composite sample collected
automatically on a given date, the date of collection is the date on which the sample is collected. For a
composite sample collected automatically, and that is collected across two calendar dates, the date of
collection is the dates of the two days; e.g., November 14-15.
\5\ Add a reducing agent only if an oxidant (e.g., chlorine) is present. Reducing agents shown to be effective
are sodium thiosulfate (Na2S2O3), ascorbic acid, sodium arsenite (NaAsO2), or sodium borohydride (NaBH4).
However, some of these agents have been shown to produce a positive or negative cyanide bias, depending on
other substances in the sample and the analytical method used. Therefore, do not add an excess of reducing
agent. Methods recommending ascorbic acid (e.g., EPA Method 335.4) specify adding ascorbic acid crystals, 0.1-
0.6 g, until a drop of sample produces no color on potassium iodide (KI) starch paper, then adding 0.06 g (60
mg) for each liter of sample volume. If NaBH4 or NaAsO2 is used, 25 mg/L NaBH4 or 100 mg/L NaAsO2 will reduce
more than 50 mg/L of chlorine (see method ``Kelada-01'' and/or Standard Method 4500-CN- for more information).
After adding reducing agent, test the sample using KI paper, a test strip (e.g. for chlorine, SenSafeTM Total
Chlorine Water Check 480010) moistened with acetate buffer solution (see Standard Method 4500-Cl.C.3e), or a
chlorine/oxidant test method (e.g., EPA Method 330.4 or 330.5), to make sure all oxidant is removed. If
oxidant remains, add more reducing agent. Whatever agent is used, it should be tested to assure that cyanide
results are not affected adversely.
\6\ Sample collection and preservation: Collect a volume of sample appropriate to the analytical method in a
bottle of the material specified. If the sample can be analyzed within 48 hours and sulfide is not present,
adjust the pH to > 12 with sodium hydroxide solution (e.g., 5% w/v), refrigerate as specified, and analyze
within 48 hours. Otherwise, to extend the holding time to 14 days and mitigate interferences, treat the sample
immediately using any or all of the following techniques, as necessary, followed by adjustment of the sample
pH to > 12 and refrigeration as specified. There may be interferences that are not mitigated by approved
procedures. Any procedure for removal or suppression of an interference may be employed, provided the
laboratory demonstrates that it more accurately measures cyanide. Particulate cyanide (e.g., ferric
ferrocyanide) or a strong cyanide complex (e.g., cobalt cyanide) are more accurately measured if the
laboratory holds the sample at room temperature and pH > 12 for a minimum of 4 hours prior to analysis, and
performs UV digestion or dissolution under alkaline (pH=12) conditions, if necessary.
(1) Sulfur: To remove elemental sulfur (S8), filter the sample immediately. If the filtration time will exceed
15 minutes, use a larger filter or a method that requires a smaller sample volume (e.g., EPA Method 335.4 or
Lachat Method 01). Adjust the pH of the filtrate to > 12 with NaOH, refrigerate the filter and filtrate, and
ship or transport to the laboratory. In the laboratory, extract the filter with 100 mL of 5% NaOH solution for
a minimum of 2 hours. Filter the extract and discard the solids. Combine the 5% NaOH-extracted filtrate with
the initial filtrate, lower the pH to approximately 12 with concentrated hydrochloric or sulfuric acid, and
analyze the combined filtrate. Because the detection limit for cyanide will be increased by dilution by the
filtrate from the solids, test the sample with and without the solids procedure if a low detection limit for
cyanide is necessary. Do not use the solids procedure if a higher cyanide concentration is obtained without
it. Alternatively, analyze the filtrates from the sample and the solids separately, add the amounts determined
(in [mu]g or mg), and divide by the original sample volume to obtain the cyanide concentration.
(2) Sulfide: If the sample contains sulfide as determined by lead acetate paper, or if sulfide is known or
suspected to be present, immediately conduct one of the volatilization treatments or the precipitation
treatment as follows: Volatilization--Headspace expelling. In a fume hood or well-ventilated area, transfer
0.75 liter of sample to a 4.4 L collapsible container (e.g., CubitainerTM). Acidify with concentrated
hydrochloric acid to pH < 2. Cap the container and shake vigorously for 30 seconds. Remove the cap and expel
the headspace into the fume hood or open area by collapsing the container without expelling the sample. Refill
the headspace by expanding the container. Repeat expelling a total of five headspace volumes. Adjust the pH to
> 12, refrigerate, and ship or transport to the laboratory. Scaling to a smaller or larger sample volume must
maintain the air to sample volume ratio. A larger volume of air will result in too great a loss of cyanide (>
10%). Dynamic stripping: In a fume hood or well-ventilated area, transfer 0.75 liter of sample to a container
of the material specified and acidify with concentrated hydrochloric acid to pH < 2. Using a calibrated air
sampling pump or flowmeter, purge the acidified sample into the fume hood or open area through a fritted glass
aerator at a flow rate of 2.25 L/min for 4 minutes. Adjust the pH to > 12, refrigerate, and ship or transport
to the laboratory. Scaling to a smaller or larger sample volume must maintain the air to sample volume ratio.
A larger volume of air will result in too great a loss of cyanide (> 10%). Precipitation: If the sample
contains particulate matter that would be removed by filtration, filter the sample prior to treatment to
assure that cyanide associated with the particulate matter is included in the measurement. Ship or transport
the filter to the laboratory. In the laboratory, extract the filter with 100 mL of 5% NaOH solution for a
minimum of 2 hours. Filter the extract and discard the solids. Combine the 5% NaOH-extracted filtrate with the
initial filtrate, lower the pH to approximately 12 with concentrated hydrochloric or sulfuric acid, and
analyze the combined filtrate. Because the detection limit for cyanide will be increased by dilution by the
filtrate from the solids, test the sample with and without the solids procedure if a low detection limit for
cyanide is necessary. Do not use the solids procedure if a higher cyanide concentration is obtained without
it. Alternatively, analyze the filtrates from the sample and the solids separately, add the amounts determined
(in [mu]g or mg), and divide by the original sample volume to obtain the cyanide concentration. For removal of
sulfide by precipitation, raise the pH of the sample to > 12 with NaOH solution, then add approximately 1 mg
of powdered cadmium chloride for each mL of sample. For example, add approximately 500 mg to a 500-mL sample.
Cap and shake the container to mix. Allow the precipitate to settle and test the sample with lead acetate
paper. If necessary, add cadmium chloride but avoid adding an excess. Finally, filter through 0.45 micron
filter. Cool the sample as specified and ship or transport the filtrate and filter to the laboratory. In the
laboratory, extract the filter with 100 mL of 5% NaOH solution for a minimum of 2 hours. Filter the extract
and discard the solids. Combine the 5% NaOH-extracted filtrate with the initial filtrate, lower the pH to
approximately 12 with concentrated hydrochloric or sulfuric acid, and analyze the combined filtrate. Because
the detection limit for cyanide will be increased by dilution by the filtrate from the solids, test the sample
with and without the solids procedure if a low detection limit for cyanide is necessary. Do not use the solids
procedure if a higher cyanide concentration is obtained without it. Alternatively, analyze the filtrates from
the sample and the solids separately, add the amounts determined (in [mu]g or mg), and divide by the original
sample volume to obtain the cyanide concentration. If a ligand-exchange method is used (e.g., ASTM D6888), it
may be necessary to increase the ligand-exchange reagent to offset any excess of cadmium chloride.
(3) Sulfite, thiosulfate, or thiocyanate: If sulfite, thiosulfate, or thiocyanate is known or suspected to be
present, use UV digestion with a glass coil (Method Kelada-01) or ligand exchange (Method OIA-1677) to
preclude cyanide loss or positive interference.
(4) Aldehyde: If formaldehyde, acetaldehyde, or another water-soluble aldehyde is known or suspected to be
present, treat the sample with 20 mL of 3.5% ethylenediamine solution per liter of sample.
[[Page 14233]]
(5) Carbonate: Carbonate interference is evidenced by noticeable effervescence upon acidification in the
distillation flask, a reduction in the pH of the absorber solution, and incomplete cyanide spike recovery.
When significant carbonate is present, adjust the pH to >=12 using calcium hydroxide instead of sodium
hydroxide. Allow the precipitate to settle and decant or filter the sample prior to analysis (also see
Standard Method 4500-CN.B.3.d).
(6) Chlorine, hypochlorite, or other oxidant: Treat a sample known or suspected to contain chlorine,
hypochlorite, or other oxidant as directed in footnote 5.
\7\ For dissolved metals, filter grab samples within 15 minutes of collection and before adding preservatives.
For a composite sample collected with an automated sampler (e.g., using a 24-hour composite sampler; see 40
CFR 122.21(g)(7)(i) or 40 CFR Part 403, Appendix E), filter the sample within 15 minutes after completion of
collection and before adding preservatives. If it is known or suspected that dissolved sample integrity will
be compromised during collection of a composite sample collected automatically over time (e.g., by interchange
of a metal between dissolved and suspended forms), collect and filter grab samples to be composited (footnote
2) in place of a composite sample collected automatically.
\8\ Guidance applies to samples to be analyzed by GC, LC, or GC/MS for specific compounds.
\9\ If the sample is not adjusted to pH 2, then the sample must be analyzed within seven days of sampling.
\10\ The pH adjustment is not required if acrolein will not be measured. Samples for acrolein receiving no pH
adjustment must be analyzed within 3 days of sampling.
\11\ When the extractable analytes of concern fall within a single chemical category, the specified preservative
and maximum holding times should be observed for optimum safeguard of sample integrity (i.e., use all
necessary preservatives and hold for the shortest time listed). When the analytes of concern fall within two
or more chemical categories, the sample may be preserved by cooling to <=6 [deg]C, reducing residual chlorine
with 0.008% sodium thiosulfate, storing in the dark, and adjusting the pH to 6-9; samples preserved in this
manner may be held for seven days before extraction and for forty days after extraction. Exceptions to this
optional preservation and holding time procedure are noted in footnote 5 (regarding the requirement for
thiosulfate reduction), and footnotes 12, 13 (regarding the analysis of benzidine).
\12\ If 1,2-diphenylhydrazine is likely to be present, adjust the pH of the sample to 4.0 0.2 to
prevent rearrangement to benzidine.
\13\ Extracts may be stored up to 30 days at < 0 [deg]C.
\14\ For the analysis of diphenylnitrosamine, add 0.008% Na2S2O3 and adjust pH to 7-10 with NaOH within 24 hours
of sampling.
\15\ The pH adjustment may be performed upon receipt at the laboratory and may be omitted if the samples are
extracted within 72 hours of collection. For the analysis of aldrin, add 0.008% Na2S2O3.
\16\ Sufficient ice should be placed with the samples in the shipping container to ensure that ice is still
present when the samples arrive at the laboratory. However, even if ice is present when the samples arrive, it
is necessary to immediately measure the temperature of the samples and confirm that the preservation
temperature maximum has not been exceeded. In the isolated cases where it can be documented that this holding
temperature cannot be met, the permittee can be given the option of on-site testing or can request a variance.
The request for a variance should include supportive data which show that the toxicity of the effluent samples
is not reduced because of the increased holding temperature.
\17\ Samples collected for the determination of trace level mercury (<100 ng/L) using EPA Method 1631 must be
collected in tightly-capped fluoropolymer or glass bottles and preserved with BrCl or HCl solution within 48
hours of sample collection. The time to preservation may be extended to 28 days if a sample is oxidized in the
sample bottle. A sample collected for dissolved trace level mercury should be filtered in the laboratory
within 24 hours of the time of collection. However, if circumstances preclude overnight shipment, the sample
should be filtered in a designated clean area in the field in accordance with procedures given in Method 1669.
If sample integrity will not be maintained by shipment to and filtration in the laboratory, the sample must be
filtered in a designated clean area in the field within the time period necessary to maintain sample
integrity. A sample that has been collected for determination of total or dissolved trace level mercury must
be analyzed within 90 days of sample collection.
\18\ Aqueous samples must be preserved at <=6 [deg]C, and should not be frozen unless data demonstrating that
sample freezing does not adversely impact sample integrity is maintained on file and accepted as valid by the
regulatory authority. Also, for purposes of NPDES monitoring, the specification of ``<=[deg]C'' is used in
place of the ``4 [deg]C'' and ``< 4 [deg]C'' sample temperature requirements listed in some methods. It is not
necessary to measure the sample temperature to three significant figures (\1/100\th of 1 degree); rather,
three significant figures are specified so that rounding down to 6 [deg]C may not be used to meet the <=6
[deg]C requirement. The preservation temperature does not apply to samples that are analyzed immediately (less
than 15 minutes).
\19\ An aqueous sample may be collected and shipped without acid preservation. However, acid must be added at
least 24 hours before analysis to dissolve any metals that adsorb to the container walls. If the sample must
be analyzed within 24 hours of collection, add the acid immediately (see footnote 2). Soil and sediment
samples do not need to be preserved with acid. The allowances in this footnote supersede the preservation and
holding time requirements in the approved metals methods.
\20\ To achieve the 28-day holding time, use the ammonium sulfate buffer solution specified in EPA Method 218.6.
The allowance in this footnote supersedes preservation and holding time requirements in the approved
hexavalent chromium methods, unless this supersession would compromise the measurement, in which case
requirements in the method must be followed.
\21\ Holding time is calculated from time of sample collection to elution for samples shipped to the laboratory
in bulk and calculated from the time of sample filtration to elution for samples filtered in the field.
\22\ Samples analysis should begin immediately, preferably within 2 hours of collection. The maximum transport
time to the laboratory is 6 hours, and samples should be processed within 2 hours of receipt at the
laboratory.
\23\ For fecal coliform samples for sewage sludge (biosolids) only, the holding time is extended to 24 hours for
the following sample types using either EPA Method 1680 (LTB-EC) or 1681 (A-1): Class A composted, Class B
aerobically digested, and Class B anaerobically digested.
PART 503--STANDARDS FOR THE USE OR DISPOSAL OF SEWAGE SLUDGE
0
3. The authority citation for Part 503 continues to read as follows:
Authority: Secs. 405(d) and (e) of the Clean Water Act, as
amended by Pub. L. 95-217, sec. 54(d), 91 Stat. 1591 (33 U.S.C.
1345(d) and (e)); and Pub. L. 100-4, title IV, sec. 406(a), (b), 101
Stat., 71, 72 (33 U.S.C. 1251 et seq.).
0
4. Section 503.8 is amended by revising paragraph (b) introductory text
to read as follows:
Sec. 503.8 Sampling and analysis.
* * * * *
(b) Methods. The materials listed below are incorporated by
reference in this part. These incorporations by reference were approved
by the Director of the Federal Register in accordance with 5 U.S.C.
552(a) and 1 CFR part 51. The materials are incorporated as they exist
on the date of approval, and notice of any change in these materials
will be published in the Federal Register. They are available for
inspection at the HQ Water Docket Center, EPA/DC, EPA West, Room B102,
1301 Constitution Ave., NW., Washington, DC, and at the National
Archives and Records Administration (NARA). For information on the
availability of this material at NARA, call 202-741-6030, or go to:
http://www.archives.gov/federal_register/code_of_federal_regulations/ibr_locations.html.
Copies may be obtained from the standard producer or publisher
listed in the regulation. The methods in the materials listed below (or
in 40 CFR Part 136) shall be used to analyze samples of sewage sludge.
* * * * *
[FR Doc. 07-1455 Filed 3-23-07; 8:45 am]
BILLING CODE 6560-50-P