[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 EmporeTM 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 EmporeTM 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 EmporeTM 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 EmporeTM 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 EmporeTM 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