Federal Register, Volume 60 Issue 148 (Wednesday, August 2, 1995)

[Federal Register Volume 60, Number 148 (Wednesday, August 2, 1995)]
[Rules and Regulations]
[Pages 39586-39590]
From the Federal Register Online via the Government Publishing Office [www.gpo.gov]
[FR Doc No: 95-18866]

[[Page 39585]]

_______________________________________________________________________

Part IV

Environmental Protection Agency

_______________________________________________________________________

40 CFR Part 136

Guidelines Establishing Test Procedures for the Analysis of Pollutants;
Chlorinated Pesticides and PCBs by Disk Extraction; Final Rule

Federal Register / Vol. 60, No. 148 / Wednesday, August 2, 1995 /
Rules and Regulations

[[Page 39586]]

ENVIRONMENTAL PROTECTION AGENCY

40 CFR Part 136

[FRL-5267-2]

Guidelines Establishing Test Procedures for the Analysis of
Pollutants; Chlorinated Pesticides and PCBs by Disk Extraction

AGENCY: Environmental Protection Agency (EPA).

ACTION: Final rule.

-----------------------------------------------------------------------

SUMMARY: This amendment to the Guidelines Establishing Test Procedures
approves the use of an additional procedure for the determination of
chlorinated pesticides and polychlorinated biphenyls (PCBs) in
wastewater by adding appropriate citations to Tables IC and ID and by
amending the incorporation by reference section of the regulation
accordingly. The method differs from other approved methods in that it
incorporates a disk of octadecyl-bonded silica enmeshed in a matrix of
inert polytetrafluoroethylene (PTFE) fibrils for extraction of the
analytes. The precision and recovery for the chlorinated pesticides and
PCBs using this technique are not substantially different from those
obtained using the liquid-liquid extraction technique already approved.
Use of approved analytical techniques is required whenever the waste
constituent specified is required to be measured for: an NPDES permit
application; discharge monitoring reports; state certification; and
other requests from the permitting authority for quantitative or
qualitative effluent data. Use of approved test procedures is also
required for the expression of pollutant amounts, characteristics, or
properties in effluent limitations guidelines and standards of
performance and pretreatment standards, unless otherwise specifically
noted or defined.

DATES: This rule shall be effective on September 1, 1995. In accordance
with 40 CFR 23.2 (45 FR 26048), these amendments to the regulation
shall be considered issued for purposes of judicial review at 1 p.m.
eastern time, August 16, 1995.
The incorporation by reference of certain publications listed in
the regulation is approved by the Office of the Federal Register as of
September 1, 1995.
Under section 509(b)(1) of the Clean Water Act, judicial review of
these amendments can be obtained only by filing a petition for review
in the United States Court of Appeals within 120 days after they are
considered issued for purposes of judicial review. Under section
509(b)(2) of the Clean Water Act, these amendments may not be
challenged later in civil or criminal proceedings brought by EPA to
enforce these requirements.

FOR FURTHER INFORMATION CONTACT: Mr. James E. Longbottom, Environmental
Monitoring Systems Laboratory, Office of Research and Development, U.S.
Environmental Protection Agency, Cincinnati, Ohio 45268. Telephone
number: (513) 569-7308.

SUPPLEMENTARY INFORMATION:

I. Authority

This regulation is promulgated under authority of sections 301,
304(h) and 501(a) of the Clean Water Act, 33 U.S.C. 1251 et seq. (the
Federal Water Pollution Control Act Amendments of 1972 as amended) (the
``Act''). Section 301 of the Act prohibits the discharge of any
pollutant into navigable waters unless the discharge complies with a
National Pollutant Discharge Elimination System (NPDES) permit, issued
under section 402. 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 his functions under this
Act''.

II. Regulatory Background

The CWA establishes two principal bases for effluent limitations.
First, existing discharges are required to meet technology-based
effluent limitations. New source discharges must meet new source
performance standards based on the best available demonstrated control
technology. Second, where necessary, additional requirements are
imposed to assure attainment and maintenance of water quality standards
established by the States under Section 303 of the CWA. In establishing
or reviewing NPDES permit limits, EPA must ensure that permitted
discharges will not cause or contribute to a violation of water quality
standards, including designated water uses.
For use in permit applications, discharge monitoring reports, and
state certification and to ensure compliance with effluent limitations,
standards of performance, and pretreatment standards, EPA has
promulgated regulations providing nationally-approved testing
procedures at 40 CFR Part 136. Test procedures have previously been
approved for 262 different parameters. Those procedures apply to the
analysis of inorganic (metal, non-metal, mineral) and organic chemical,
radiological, bacteriological, nutrient, demand, residue, and physical
parameters.
Additionally, some particular industries may discharge pollutants
for which test procedures have not been proposed and approved under 40
CFR Part 136. Under 40 CFR Part 122.41 permit writers may impose
monitoring requirements and establish test methods for pollutants for
which no approved Part 136 method exists. 40 CFR 122.41(j) (4). EPA may
also approve additional test procedures when establishing industry-wide
technology-based effluent limitations guidelines and standards as
described at 40 CFR 401.13.
The procedures for approval of alternate test procedures (ATPs) are
described at 40 CFR 136.4 and 136.5. Under these procedures the
Administrator may approve alternate test procedures for nationwide use
which are developed and proposed by any person. 40 CFR 136.4 (a).
Dischargers seeking to use such alternate test procedures on a limited
basis (e.g., for their own discharge), must apply to the State or
Regional EPA permitting office in which the discharge occurs approval
under 136.4 (d). As specified below, today's rule approves an optional
nationwide alternate procedure for determination of chlorinated
pesticides and PCBs in wastewater test samples.

III. The Disk Extraction Test Procedure

The 3M Corporation, in accordance with the regulations published at
40 CFR section 136.5, applied for nationwide approval of their
``Organochlorine Pesticides and PCBs in Wastewater Using Empore Disk''.
3M subsequently presented data to meet the method comparability
criteria set forth in the EPA ``Protocol for Approval of Alternate Test
Procedures for Inorganic and Organic Analytes in National Pollutant
Discharge Elimination System Monitoring'', July 12, 1993.
Extraction and concentration are preparation steps that are
required prior to the determination of many organic analytes that are
found in wastewater. The disk extraction procedure is proposed as an
alternate to the presently approved liquid-liquid extraction procedure.

[[Page 39587]]

A. Scope of the Procedure
Method 3M 0222 is designed as an alternate test procedure for
currently approved EPA Method 608. The Empore^{TM disk is used in
place of liquid-liquid extraction. This method is being promulgated as
an alternative procedure for the determination of nineteen specified
organochlorine pesticides and seven PCBs listed below:

Aldrin
alpha-BHC
beta-BHC
Chlordane
delta-BHC
Dieldrin
Endosulfan I
Endosulfan II
Endosulfan sulfate
Endrin
Endrin aldehyde
gamma-BHC PCB-1254
Heptachlor
Heptachlor epoxide
Methoxychlor
Toxaphene
4,4'-DDD
4,4'-DDE
4,4'-DDT
PCB-1016
PCB-1221
PCB-1232
PCB-1242
PCB-1248
PCB-1254
PCB-1260

The parameters listed in the table can be determined by gas
chromatography using Method 3M 0222. When the method is used to analyze
unfamiliar samples for any or all of the compounds listed, compound
identifications should be supported by at least one additional
qualitative technique. The method describes analytical conditions for a
second gas chromatographic column that can be used to confirm
measurements made with the primary column.

B. Summary of the Methods

A measured volume of sample, approximately 1-L, is extracted using
a 90 mm Empore^{TM disk. The disk is eluted with acetone followed by
methylene chloride. The eluant is dried by pouring through anhydrous
sodium sulfate and exchanged to hexane during concentration to a volume
of 10-mL or less. The eluant is separated by gas chromatography and the
analytes are then measured with an electron capture detector.
The method provides a Florisil column cleanup procedure and an
elemental sulfur removal procedure using activated copper powder to aid
in the elimination of interferences that may be encountered.

C. Technical Justification for Approved Procedure

The approval of this procedure is based on Agency review of the
supporting information and data submitted by the applicant, 3M
Corporation. EPA is approving the method based on the method
description in EPA's Environmental Monitoring Management Council
format, comparative analyses using the proposed and approved
procedures, and EPA's technical and statistical reviews of each data
package.
3M Corporation provided test data comparing the proposed procedure
with appropriate approved procedure. The results from the proposed
alternate method were compared to the approved EPA Method using liquid-
liquid extraction/gas chromatography procedures. EPA statisticians and
chemists conducted independent reviews of the data. The recovery and
precision of all the submitted data for both the approved and proposed
methods were also compared to the recovery and precision acceptance
criteria derived for EPA Method 608 from Performance Evaluation Studies
WP 18 and 23.
The Agency has judged the currently approved Method 608 method to
be acceptable in the evaluation of the proposed procedure. EPA's
Environmental Monitoring Systems Laboratory in Cincinnati, Ohio (EMSL-
Cincinnati) thoroughly reviewed and evaluated the supporting data
submitted by the 3M Corporation. The comparability reviews indicated
that the analyses afforded comparable recovery and precision in the
recommended concentration ranges for the listed organochlorine
pesticides and PCBs. EPA proposed approval of the Empore^{TM disk
procedure and sought public comment on the suitability of this method
as an alternate procedure for use in the determination of the
parameters listed in 59 FR 65878 (December 21, 1994). The
administrative record is on file at EMSL-Cincinnati, 26 W. Martin
Luther King Dr., Cincinnati, Ohio 45268. The record is available for
public inspection. The approved procedure is also available from 3M
Corporation, 3M Center Building 220-9E-10, St. Paul, MN 55144-1000.
Based on EMSL-Cincinnati's review, and pursuant to 40 CFR Section
136.5, EPA has approved the 3M Corporation's ``Organochlorine
Pesticides and PCBs in Wastewater Using Empore^{TM Disk'' method as
an acceptable alternative procedure for nationwide use. Specifically,
the method exhibits sufficient precision and recovery to establish (1)
its acceptability under Part 136 and (2) its comparability to the
approved procedure for analysis of the specified organochlorine
pesticides and PCBs. As an approved alternate test procedure, this
procedure is acceptable for use by any person required to test for
these parameters.

IV. Public Comments and Response to Most Significant Comments

The Agency requested comments on the proposal to approve the 3M
method for pesticides and PCB's. Comments were received from 5
individuals/organizations. All commenters favored approval of disk
extraction as an acceptable alternate procedure (ATP). The most
significant comments were as follows:
Comment: Other companies produce extraction disks on inert
surfaces, so all references in the method to the disk in the 3M method
should be generic in nature so that other commercial products can be
used by the analyst. Commenter supports feasibility of generic approach
by noting the method includes initial quality control demonstrations
that can demonstrate applicability of the alternative vender's product,
and that EPA used general product description language in the
comparable method approved in 40 CFR 141 for drinking water analyses.
Response: EPA's limited resources are not sufficient to fully
evaluate all new technologies that may be applicable to monitoring
programs under the Clean Water Act. The nationwide alternate test
procedure (ATP) program was established 40 CFR Part 136.4 to allow
developers of new commercial instruments, product or supplies to
demonstrate the efficacy of the measurement technology to measure
pollutant concentration levels. The ATP program is expensive for the
applicant as applicability to a broad variety of wastewaters must be
demonstrated. The Agency does not require this applicant to demonstrate
that the extraction technology can be made to work using competitor's
products. The use of a competitive product in this method would require
additional method development to optimize solvents, flow rates, and
other features of the method. After these procedures have been
standardized, a suitable demonstration of applicability is required.
Because of the diverse nature of wastewaters under this regulation, a
general statement of applicability could be made only if a number of
different wastewaters are tested. Limited use approval could be
obtained on a case-by-case basis by demonstrating applicability to an
individual discharger's wastestream.

[[Page 39588]]
The quality control tests in the 3M method referenced by the commenter
are performed using reagent water and will not demonstrate
applicability to wastewater. The Agency actions in Part 141 were based
on research on drinking water with commercial products from multiple
suppliers. Since drinking waters do not contain the high organic loads
and suspended solids that challenge the solid-phase extraction
procedures, it is easier to establish general applicability to the
matrix.
Comment: Commenter has tried these disks and has encountered some
problems with plugging and finds no mention of what to do when this
happens. Suggests method be limited to samples with less than 2-5%
solids.
Response: In the comparison study performed by 3M, both the
approved EPA Method 608 and the alternate 3M method produced lower
results for wastewaters with very high suspended solids and the 3M
method contains an appropriate caution in this regard. A sample with 2-
5% solids is generally classified as a sludge and is beyond the scope
of this rulemaking.
Comment: Commenter provided a series of questions for EPA to use in
its evalation of the 3M method. The questions addressed technical
specifications for the inert and active components of the disk, and
possible limitations of the method caused by absorptive capacity,
selective absorption or sample pH.
Response: The applicant voluntarily provided EPA with detailed
responses to each of the questions, although much of this information
would normally be treated by EPA as confidential business information.
The applicant's response has been incorporated into the administrative
record for this rulemaking. Alternate test procedures are evaluated
primarily on the basis of method performance characteristics including
accuracy, precision, and sensitivity data quality.

V. Regulatory Requirements

A. Executive Order 12866

Under Executive Order 12866, EPA must judge whether a regulation is
``major'' and, therefore, requires a regulatory impact analysis. EPA
has determined that this regulation is not major as it will not result
in an effect on the economy of $100 million or more, a significant
increase in cost or prices, or any of the effects described in the
Executive Order. This final rule would simply specify an alternative
analytical procedure which may be used by laboratories in measuring
concentrations of organochlorine pesticides and PCBs using EPA Method
608 and, therefore, would have no adverse economic impacts. This rule
is not considered significant under the Executive Order.

B. Regulatory Flexibility Act

This amendment is consistent with the objectives of the Regulatory
Flexibility Act (5 U.S.C. 602 et seq.) because it will not have a
significant economic impact on a substantial number of small entities.
The procedure included in this final rule would give all laboratories
the flexibility to use this alternate procedure or not to use it.

C. Paperwork Reduction Act

This rule contains no requests for information activities and,
therefore, no information collection request (ICR) was submitted to the
Office of Management and Budget (OMB) for review in compliance with the
Paperwork Reduction Act, (44 U.S.C. 3501 et seq.).

D. Unfunded Mandates

Under Section 202 of the Unfunded Mandates Reform Act of 1995,
signed into law on March 22, 1995, EPA must prepare a written statement
to accompany rules where the estimated costs to State, local, or tribal
governments, or to the private sector will be Sec. 100 million or more
in any one year. Under Section 205, EPA must select the most cost-
effective and least burdensome alternative that achieves the objective
of such a rule and that is consistent with statutory requirements.
Section 203 requires EPA to establish a plan for informing and advising
any small governments that may be significantly and uniquely affected
by the rule.
EPA estimates that the costs to State, local or tribal governments,
or the private sector, from this rule will be far less than Sec. 100
million. This rule should have minimal impact, if any, on the existing
regulatory burden imposed on NPDES permittees required to monitor for
regulated pollutants because the rule would merely make additional
options available to the laboratory analyst conducting an existing
approved test method. EPA has determined that an unfunded mandates
statement therefore is unnecessary. Similarly, the method approved
today does not establish any regulatory requirements that might
significantly or uniquely affect small governments.
List of Subjects in 40 CFR Part 136
Environmental protection, Incorporation by reference, Water
pollution control.

Dated: July 25, 1995.
Carol M. Browner,
Administrator.

In consideration of the preceding, EPA amends part 136 of title 40
Chapter I of the Code of Federal Regulations as follows:
PART 136--AMENDED
1. The authority citation for 40 CFR part 136 continues to read as
follows:

Authority: Secs. 301, 304(h), 307, and 501(a) Public Law 95-217,
Stat. 1566, et seq. (33 U.S.C. 1251 et seq.)(the Federal Water
Pollution Control Act Amendments of 1972 as amended by the Clean
Water Act of 1977).

2. Section 136.3 is amended as follows:
a. In Table 1C of paragraph (a) by revising entries 76. PCB-1016,
77. PCB-1221, 78. PCB-1232, 79. PCB-1242, 80. PCB-1248, 81. PCB-1254,
82. PCB-1260; and by adding footnote 8.
b. In Table ID of paragraph (a) by revising entries 1. Aldrin, 8.
-BHC, 9. -BHC, 10. -BHC, 11. -BHC
(Lindane), 15. Chlordane, 18. 4,4'-DDD, 19. 4,4'-DDE, 20. 4,4'-DDT, 28.
Dieldrin, 32. Endosulfan I, 33. Endosulfan II, 34. Endosulfan sulfate,
35. Endrin, 36. Endrin aldehyde, 40. Heptachlor, 41. Heptachlor
epoxide, 46. Methoxychlor, and 69. Toxaphene; and by adding footnote 8.
Sec. 136.3 Identification of test procedures.

(a) * * *

Table IC.--List of Approved Test Procedures for Non-Pesticide Organic Compounds
--------------------------------------------------------------------------------------------------------------------------------------------------------
EPA method number \2\ \7\
Parameter \1\ --------------------------------------- Standard methods 18th ed. ASTM Other
GC GC/MS HPLC
--------------------------------------------------------------------------------------------------------------------------------------------------------

* * * * * * *
76. PCB-1016............................ 608 625 ........... 6410 B ........... Note 3, p. 43; note 8.
77. PCB-1221............................ 608 625 ........... 6410 B ........... Note 3, p. 43; note 8.
78. PCB-1232............................ 608 625 ........... 6410 B ........... Note 3, p. 43; note 8.

[[Page 39589]]

79. PCB-1242............................ 608 625 ........... 6410 B ........... Note 3, p. 43; note 8.
80. PCB-1248............................ 608 625 ........... .......................... ........... Note 3, p. 43; note 8.
81. PCB-1254............................ 608 625 ........... 6410 B ........... Note 3, p. 43; note 8.
82. PCB-1260............................ 608 625 ........... 6410 B, 6630 B ........... Note 3, p. 43; note 8.

* * * * * * *
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table IC Notes
\1\ All parameters are expressed in micrograms per liter (g/L).
\2\ The full text of Methods 601-613, 624, 625, 1624 and 1625, are given at appendix A, ``Test Procedures for Analysis of Organic Pollutants,'' of this
part 136. The standardized test procedure to be used to determine the method detection limit (MDL) for these test procedures is given at appendix B,
``Definition and Procedure for the Determination of the Method Detection Limit'' of this part 136.
\3\ ``Methods for Benzidine: Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater,'' U.S. Environmental Protection
Agency, September, 1978.
* * * * * * *
\7\ Each analyst must make an initial, one-time demonstration of their ability to generate acceptable precision and accuracy with Methods 601-613, 624,
625, 1624 and 1625 (See appendix A of the part 136) in accordance with procedures each in section 8.2 of each of these Methods. Additionally, each
laboratory, on and on-going basis must spike and analyze 10% (5% for Methods 624 and 625 and 100% for Methods 1624 land 1625) of all samples to
monitor and evaluate laboratory data quality in accordance with sections 8.3 and 8.4 of these Methods. When the recovery of any parameter falls
outside the warning limits, the analytical results for that parameter in the unspiked sample are suspect and cannot be reported to demonstrate
regulatory compliance.
\8\ ``Organochlorine Pesticides and PCBs in Wastewater Using Empore TM Disk'', 3M Corporation Revised 10/28/94.

Table ID.--List of Approved Test Procedures for Pesticides \1\
--------------------------------------------------------------------------------------------------------------------------------------------------------
Standard methods
Parameter g/L Method EPA \2\ \7\ 18th ed. ASTM Other
--------------------------------------------------------------------------------------------------------------------------------------------------------
1. Aldrin....................................... GC 608 6630 B & C D3086-90 Note 3, p. 7; note 4, p. 30; note
8.
GC/MS 625 6410 B ................ .................................

* * * * * * *
8. -BHC................................ GC 608 6630 B & C D3086-90 Note 3, p. 7; note 8.
GC/MS \5\ 625 6410 B ................ .................................
9. -BHC................................ GC 608 6630 C D3086-90 Note 8.
GC/MS \5\ 625 6410 B ................ .................................
10. -BHC............................... GC 608 6630 C D3086-90 Note 8.
GC/MS \5\ 625 6410 B ................ .................................
11. -BHC (Lindane)..................... GC 608 6630 B & C D3086-90 Note 3, p. 7; note 4, p. 30; note
8.
GC/MS 625 6410 B ................ .................................

* * * * * * *
15. Chlordane................................... GC 608 6630 B & C D3086-90 Note 3, p. 7; note 8.
GC/MS 625 6410 B ................ .................................

* * * * * * *
18. 4,4'-DDD.................................... GC 608 6630 B & C D3086-90 Note 3, p. 7; note 4, p. 30; note
8.
GC/MS 625 6410 B ................ .................................
19. 4,4'-DDE.................................... GC 608 6630 B & C D3086-90 Note 3, p. 7; note 4, p. 30; note
8.
GC/MS 625 6410 B ................ .................................
20. 4,4'-DDT.................................... GC 608 6630 B & C D3086-90 Note 3, p. 7; note 4, p. 30; note
8.
GC/MS 625 6410 B ................ .................................

* * * * * * *
28. Dieldrin.................................... GC 608 6630 B & C ................ Note 3, p. 7; note 4, p. 30; note
8.
GC/MS 625 6410 B ................ .................................

* * * * * * *
32. Endosulfan I................................ GC 608 6630 B & C D3086-90 Note 3, p. 7; note 8.
GC/MS \5\ 625 6410 B ................ .................................
33. Endosulfan II............................... GC 608 6630 B & C D3086-90 Note 3, p. 7; note 8.
GC/MS \5\ 625 6410 B ................ .................................
34. Endosulfan Sulfate.......................... GC 608 6630 C ................ Note 8.
GC/MS 625 6410 B ................ .................................
35. Endrin...................................... GC 608 6630 B & C D3086-90 Note 3, p. 7; note 4, p. 30; note
8.

[[Page 39590]]

GC/MS \5\ 625 6410 B ................ .................................
36. Endrin aldehyde............................. GC 608 .................. ................ Note 8.
GC/MS 625 .................. ................ .................................

* * * * * * *
40. Heptachlor.................................. GC 608 6630 B & C D3086-90 Note 3, p. 7; note 4, p. 30; note
8.
GC/MS 625 6410 B ................ .................................
41. Heptachlor epoxide.......................... GC 608 6630 B & C D3086-90 Note 3, p. 7; note 4, p. 30; note
6, p. S73; note 8.
GC/MS 625 6410 B ................ .................................

* * * * * * *
46. Methoxychlor................................ GC ........... 6630 B & C D3086-90 Note 3, p. 7; note 4, p. 30; note
8.

* * * * * * *
69. Toxaphene................................... GC 608 6630 B & C D3086-90 Note 3, p. 7; note 4, p. 30; note
8.
GC/MS 625 6410 B ................ .................................

* * * * * * *
--------------------------------------------------------------------------------------------------------------------------------------------------------
Table ID Notes:
\1\ Pesticides are listed in this table by common name for the convenience of the reader. Additional pesticides may be found under Table 1C, where
entries are listed by chemical name.
\2\ The full text of Methods 608 and 625 are given at Appendix A. ``Test Procedures for Analysis of Organic Pollutants'', of this Part 136. The
standardized test procedure to be used to determine the method detection limit (MDL) for these test procedures is given at Appendix B. ``Definition
and Procedure for the Determination of the Method Detection Limit'', of this Part 136.
\3\ ``Methods for Benzidine, Chlorinated Organic Compounds, Pentachlorophenol and Pesticides in Water and Wastewater'', U. S. Environmental Protection
Agency, September, 1978. This EPA publication includes thin-layer chromatography (TLC) methods.
\4\ ``Methods for Analysis of Organic Substances in Water and Fluvial Sediments'', Techniques of Water-Resources Investigations of the U.S. Geological
Survey, Book 5, Chapter A3 (1987).
\5\ The method may be extended to include -BHC, 11-BHC, endosulfan I, endosulfan II, and endrin. However, when they are known
to exist in the sample, Method 608 is the preferred method.
\6\ ``Selected Analytical Methods Approved and Cited by the United States Environmental Protection Agency''. Supplement to the Fifteenth Edition of
Standard Methods for the Examination of Water and Wastewater (1981).
\7\ Each analyst must make an initial, one-time, demonstration of their ability to generate acceptable precision and accuracy with Methods 608 and 625
(See Appendix A of this Part 136) in accordance with procedures given in section 8.2 of each of these methods. Additionally, each laboratory, on an on-
going basis, must spike and analyze 10% of all samples analyzed with Method 608 or 5% of all samples analyzed with Method 625 to monitor and evaluate
laboratory data quality in accordance with Sections 8.3 and 8.4 of these methods. When the recovery of any parameter falls outside the warning limits,
the analytical results for that parameter in the unspiked sample are suspect and cannot be reported to demonstrate regulatory compliance. These
quality control requirements also apply to the Standard Methods, ASTM Methods, and other Methods cited.
\8\ ``Organochlorine Pesticides and PCBs in Wastewater Using Empore^{TM Disk'', 3M Corporation, Revised 10/28/94.

3. In 136.3(b) the list entitled ``References, Sources, Costs, and
Table Citations'' is amended by adding paragraph (33) to read as
follows:

Sec. 136.3 Identification of test procedures.

* * * * *
(b) * * *
References, Sources, Costs, and Table citations:
* * * * *
(33) ``Organochlorine Pesticides and PCBs in Wastewater Using
Empore ^{TM Disk'' Test Method 3M 0222, Revised 10/28/94. 3M
Corporation, 3M Center Building 220-9E-10, St. Paul, MN 55144-1000.
Method available from 3M Corporation. Table IC, Note 8 and Table ID,
Note 8.

[FR Doc. 95-18866 Filed 8-1-95; 8:45 am]
BILLING CODE 6560-50-P}}}}}}