95-18866. Guidelines Establishing Test Procedures for the Analysis of Pollutants; Chlorinated Pesticides and PCBs by Disk Extraction  

  • [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
    
    

Document Information

Effective Date:
9/1/1995
Published:
08/02/1995
Department:
Environmental Protection Agency
Entry Type:
Rule
Action:
Final rule.
Document Number:
95-18866
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.
Pages:
39586-39590 (5 pages)
Docket Numbers:
FRL-5267-2
PDF File:
95-18866.pdf
CFR: (1)
40 CFR 136.3