United States         Office of         Publication 9240.1 -10
          Environmental Protection     Solid Waste and      Dp^54^^^075
          Agency           Emergency Response    SowriSr"994
          Superfund

£EPA     SUPERFUND ANALYTICAL
           METHODS rOR LOW
           CONCENTRATION WATER FOR
           ORGANICS ANALYSIS

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                                                 9240.1-10
                                                 PB95-963505
                                                 EPA540/R-94/075
         SUPERFOND ANALYTICAL METHODS



                     FOR



LOW CONCENTRATION WATER FOR ORGANICS ANALYSIS



                     6/91
  U.S. Environmental Protection Agency
  Region 5, Library (PL-12J)
  77 West Jackson Boulevard,  12th Floor
  Chicago,  IL  60604-3590
                                                      6/91

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               EXHIBIT B
REPORTING AND DELIVERABLES REQUIREMENTS
                  B-l                               6/91

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                              Table of Contents
                                                                         Page


SECTION I:    Contract Reports/Deliverables Distribution 	 B-3

SECTION II:   Report Descriptions and Order of Data
              Deliverables 	B-6

SECTION III:  Foras Instruction Guide 	 B-24

SECTION IV:   Data Reporting Foras 	B-45
                                     B-2                               6/91

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                                   SECTION I

                  CONTRACT REPORTS/DELIVERABLES DISTRIBUTION
The following  table reiterates  the Contract reporting and deliverables
requirements specified  in  the Contract Schedule and specifies the
distribution that is required for each deliverable.  NOTE: Specific recipient
names and addresses are subject to change during the ten of the contract.
SMO will notify the Contractor  in writing of such changes when they occur.
              I ten
  No.
Copies
Delivery
Schedule
  Distribution
(1) (2) (3) (4)
 1.    Updated SOPs
       60 days after
       contract award
       and as required in
       Exhibit E.
                        XXX
*2.    Sample Traffic
        Reports
***3.   Sample Data Summary
        Package
***4.  Sample Data Package
*** 5. Complete SDG File
***6.  Data in Computer-
        Readable Form
       3 days after
       receipt of last
       sample in Sample
       Delivery Group
       (SDG).**

       14 days after
       receipt of last
       sample in SDG.

       14 days after
       receipt of last
       sample in SDG.

       14 days after
       receipt of last
       sample in SDG.

       14 days after
       receipt of last
       sample in SDG.
                    X
                    X
                    X
         X
                            X
                    X
Distribution:
(1)  Sample Management Office (SMO)
(2)  EMSL-LV
(3)  Region-Client (Technical Project Officer)
(4)  NEIC
                                     B-3
                                          6/91

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              Item
                               No.
                             Copies
                  Delivery
                  Schedule
  Distribution
(1)  (2)  (3)  (4)
7.
        GC/MS Tapes
8.
        Extracts
9.***** QA Plan
   Lot     Retain for 365 days        As Directed
           after data submis-
           sion, or submit with-
           in 7 days after
           receipt of written
           request.

   Lot     Retain for 365 days        As Directed
           after data submis-
           sion, or submit with-
           in 7 days after
           receipt of written
           request.

3 Copy     Submit within 60 days       As Directed
           after contract award,
           and as required in
           Exhibit E.
NOTE:


*

**
       Contractor must be prepared to receive the full contract sample
       requirement at the time of contract award.

          Also required in the Sample Data Summary Package.

          Sample Delivery Group (SDG) is a group of  samples within a Case,
          received over a period of 7 days or less and not exceeding 20
          samples. Data for all samples  in the SDG are due concurrently.   The
          date of delivery of the SDG or any samples within the SDG is the
          date that all samples have been delivered.

          Concurrent delivery required.   Delivery shall be made such that all
          designated recipients receive  the item on  the same  calendar day.

          Complete SDG file will contain the original  sample  data package plus
          all of the original documents  described under Complete SDG File
          paragraph 5.

*****     See Exhibit E for a more detailed description.

NOTE:     As specified in the Contract Schedule (Section  G, Government
          Furnished Supplies and Materials),  unless  otherwise instructed by
          the CLP Sample Management Office, the Contractor shall dispose of
          unused sample volume and used  sample bottles/containers no earlier
          than sixty (60) days following submission  of the reconciled complete
          SDG file.   Sample disposal and disposal of unused sample
          bottles/containers is the responsibility of  the Contractor and
                                     B-4
                                                                       6/91

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          should be done in accordance  with all applicable  laws and
          regulations governing disposal  of such materials.

Distribution Addresses :

(1)  USEPA Contract Lab Program
     Sample Management Office (SMO)
     P.  0. Box 818
     Alexandria, VA  22313

     For overnight delivery, service,  use  street address:
     300 North Lee Street, Suite 200
     Alexandria, VA  22314

(2)  USEPA Environmental Monitoring
     Systems Laboratory (EMSL-LV)
     P.  0. Box 15027
     Las Vegas,  NV  89114
     ATTN:  Data Audit Staff

     For overnight delivery service,  use  street address:

     944 E. Harmon, Executive Center
     Las Vegas,  NV  89109
     ATTN:  Data Audit Staff

(3)  USEPA REGIONS:

     The CLP Sample Management Office will provide the Contractor with the
     list of addressees for the ten EPA Regions.   SMO will provide the
     Contractor with updated Regional address/name lists  as necessary
     throughout the period of the contract and identify other client
     recipients on a case-by-case basis.

(4)  USEPA National Enforcement Investigations Center (NEIC)
     ATTN:  CLP Audit Program
     Denver Federal Center Bldg. S3
     P.O. Box 25227
     Denver, CO  80225
                                     B-5                               6/91

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                                  SECTION II


              REPORT DESCRIPTIONS AHD ORDER OF DATA PELI7ERABLBS
The Contractor laboratory shall provide reports and other deliverables as
specified in the Contract Schedule (Performance/Delivery Schedule, Section
F). The required content and form of each deliverable is described in this
Exhibit.

All reports and documentation MOST BE:

o   Legible

o   Clearly labeled and completed in accordance with instructions in this
    Exhibit

o   Arranged in the order specified in this Section

o   Paginated consecutively in ascending order starting from the SDG Narrative

If submitted documentation does not conform to the above criteria, the
Contractor will be required to resubmit such documentation with the
deficiencies corrected, at no additional.''^"-J^ •
                                       «
Whenever the Contractor is required to submit or resubmit data as a result of
an on-site laboratory evaluation, through a SMO action, or through a Regional
Data Reviewer's request, the data must be clearly marked as ADDITIONAL DATA
and must be sent to all three contractual data recipients (SMO, EMSL/LV, and
Region).  A cover letter shall be included which describes what data are
being delivered, to which EPA Case(s)/SDGs it pertains, and who requested the
data.

Whenever the Contractor is required to submit or resubmit data as a. result of
Contract Compliance Screening (CCS) review by SMO, the data must be sent to
all three contractual data recipients (SMO, EMSL/LV, and Region), and in all
three instances must be accompanied by a color-coded COVER SHEET  (Laboratory
Response To Results of Contract Compliance Screening) provided by SMO.

Descriptions of the requirements for each deliverable item cited in the
Contract Performance/Delivery Schedule (Contract Schedule, Section F) are
specified in this Section.  Items submitted concurrently MOST BE arranged in
the order listed.  The components of each item MOST BE arranged in the order
presented in this Section when the item is submitted.

Section III contains the form instructions to assist the Contractor in
providing all the required data.  Section IV of this Exhibit contains copies
of the required data reporting forms in specified formats.
                                     B-6                               6/91

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1     QUALITY ASSURANCE PLAH AND STANDARD OPERATING PROCEDURES

      See contract for specifications.

2.    SAt!?LE TFAg?Tc REPORTS

2.1   Original Sample Traffic Report page narked "Lab Copy for Return to SMO"
      with lab receipt information and signed in original Contractor
      signature, for each sample in the Sample Delivery Group.

2.2   Traffic Reports (TRs) shall be submitted in Sample Delivery Group (SDG)
      sets (i.e., TRs for all samples in an SDG shall be clipped together),
      with an SDG Cover Sheet attached.

2.3   The SDG Cover Sheet shall contain the following items:

          o   Lab name
          o   Contract number
          o   Sample analysis price - full sample price from contract.

          o   Case number
          o   List of EPA Sample Numbers of all samples in the SDG,
             identifying the first and last samples received, and their dates
             of receipt (LRDs).
2.4   When more ttvm one sample is received in the first or last SDG
      shipment, the "first" sample received would be the lowest sample number
      (considering both alpha and numeric designations); the "last" sample
      received would be the highest sample number (considering both alpha and
      numeric designations).

2.5   The EPA Sample Number of the first sample received in the SDG is the
      SDG number.  Each Traffic Report must be clearly marked with the SDG
      Number.  This information should be entered below the Lab Receipt Date
      on the TR.  The TR for the last sample received in the last SDG
      shipment must be clearly marked "SDG - FINAL SAMPLE."

2.6   If samples are received at the laboratory with multi-sample Traffic
      Reports (TRs), all the samples on one multi-sample TR may not
      necessarily be in the same SDG.  In this instance, the laboratory must
      make the appropriate number of photocopies of the TR, and submit one
      copy with each SDG cover sheet.

3.    SAMPLE DATA SUMMARY PACKAGE

3.1   As specified in the Delivery Schedule, one Sample Data Summary Package
      shall be delivered to SMO concurrently with delivery of other required
      sample data.  The Sample Data Summary Package shall be submitted
      separately (i.e., separated by rubber bands, clips or other means)
      directly preceding the Sample Data Package.

3.2   The Sample Data Summary Package consists of specified items from the
      Sample Data Package in the following order:


                                     B-7                               6/91

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          o  SDG Narrative

          o  Organics Analysis Data Sheet for target contpound results  (Form
             I) and  for  tentatively identified compounds  (Form I, TIC) by
             fraction (VOA,  SV, PEST) and by sample within each fraction.
             (No Fora I, TIC for PEST fraction.)
          o  Surrogate Recovery (Font II) by fraction  (VOA, SV, PEST)

          o  Laboratory  Control Sample Recovery  (Fora  III) by fraction (VOA,
             SV, PEST)

          o  Method  Blank Suaaary  (Fora IV), Organics Analysis Data Sheet for
             target  coapound results (Fora I) and for  tentatively identified
             coapounds (Fora I, TIC) by fraction (VOA, SV).
          o  Peak Area and Retention Time Summary of Internal Standards  for
             initial calibration standards (Fora VIII) and saaples (Form
             VIII) by fraction (VOA, SV only).

3.3   Saaple data forms shall be arranged in increasing EPA Saaple Number
      order.

4.    gAifpr.ii; DATA PACKAGE

4.1   The Saaple Data Package shall include data for analyses of all saaples
      in each Saaple Delivery Group, specifically including field saaples,
      reanalyses, dilutions, blanks, Laboratory  Control Saaples, and
      Performance Evaluation Saaples.  The Saaple Data Package is divided
      into the five major units as follows:

          o  SDG Narrative
          o  Sample  Traffic  Reports

          o  Volatiles Data
          o  Seaivolatiles Data
          o  Pestieides/Aroclors Data

4.2   The Volatiles, Semivolatiles, and Pestieides/Aroclors data are each
      specific to an analytical fraction.  If the analysis of that fraction
      is not required, then  that fraction-specific unit is not a required
      deliverable.

      The Contractor shall retain a copy of the  saaple data package for  365
      days after final acceptance of data.  After *h*« time, the Contractor
      may dispose of the package.

4.3.  SDG Narrative

      4.3.1   This document  shall  be clearly labeled "SDG Narrative".   The
              SDG Narrative  shall  contain:  laboratory name;  Case number;  EPA
              Sample Numbers in the Sample Delivery Group (SDG),
              differentiating between  initial analyses,  dilutions and
              reanalysis; SDG number;  Contract number; and detailed
              documentation  of any quality control  sample,  shipment and/or


                                     B-8                               6/91

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               analytical  problems encountered  in processing the samples
               reported in the  data package.

      4.3.2    Whenever data from sample reanalyses are submitted, the
               Contractor  shall state  in the  SDG Narrative for each
               reanalysis,  whether it  considers the reanalysis to be billable,
               and if  so,  why.   A copy of  the narrative should be sent  to SMO
               for their review.  The  Contractor must also include any
               problems encountered; both  technical and administrative, the
               corrective  actions taken, and  resolution.

      4.3.3    The Contractor must also list  the pH determined for each water
               sample  submitted for volatiles analysis.  This information may
               appear  as a simple list or  table in the SDG Narrative.   The
               purpose of  this  pH determination is to ensure that all
               volatiles samples were  acidified in the field.  No pH
               adjustment  is to be performed  by the Contractor on water
               samples for volatiles analysis.

      4.3.4    The SDG Narrative shall contain  the following statement
               varfrafr1"- "I certify that this data package is in compliance
               with the terms and conditions  of the contract, both technically
               and for completeness, for other  than the conditions detailed
               above.   Release  of the  data contained in .this data package and
               in  the  computer-readable data  submitted on diskette has  been
               authorized  by the Laboratory Manager or his designee, as
               verified by the  following signature.*  This statement shall be
               directly followed by signature of the Laboratory Manager or his
               designee with a  typed line  below it containing the signer's
               name and title,  and the date of  signature.

      4.3.5    In  the  event that the Laboratory Manager cannot verify all data
               reported for each saople, the  Laboratory Manager shall provide
               a detailed  description  of the  problems associated with the
               samples in  the SDG Narrative.

      4.3.6    The SDG Narrative itself must  be signed with original signature
               by  the  Laboratory Manager or his designee and dated.

4.4   Sample Traffic Reports

      Copies of the Sample Traffic Reports for all of the samples in the SDG
      are also included in the Sample Data Summary Package.   The Traffic
      Reports shall be arranged in increasing EPA Sample Number order,
      considering both letters and numbers in ordering samples.  Copies of
      the SDG cover sheet are  to be included with the copies of the Traffic
      Reports.

      If samples are received at the laboratory with multi-sample Traffic
      Reports  (TRs), not all samples on one multi-sample TR are necessarily
      in the same SDG.  In this instance,  the laboratory must make the
      appropriate number of photocopies of the TR so that a copy is submitted
      with each data package to which it applies.  In addition, in any
      instance where samples from more than one multi-sample TR are in the

                                     B-9                               6/91

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      sane data package, the laboratory oust submit a copy of the SDG cover
      sheet with copies of the TRs.

4.5   Volatiles Data

      4.5.1   Volatiles QC Summary

              If more than a single fora is necessary, each type of fora oust
              be arranged in chronological order by instrument.

              o   Surrogate Recovery (Fora II LC7)

              o   Laboratory Control Saaple Recovery (Fora III LCV)
              o   Method Blank Suaaary (Fora 17 LCV)

              o   GC/MS Tuning and Mass Calibration - BFB (Fora V LCV)
              o   Internal Standard Area and Retention Tine Suaaary (Fora
                  VIII LCV)

      4.5.2   Volatiles Saaple Data

              Saaple data, including FES, shall be arranged in packets with
              both of the Organic  Analysis Data Sheets (Fora I LCV and Fora I
              LCV-TIC), followed by the raw data for volatile saaples.  These
              saaple packets should then be placed in increasing EPA  Saaple
              Number order.

              4.5.2.1    Organics Analysis Data Sheet for target compound
                         results (Fora I LCV).

              4.5.2.2    Organics Analysis Data Sheet for tentatively
                         identified coapounds (Fora I LCV-TIC).  This fora
                         aust be included even if no TIC's are found.

              4.5.2.3    Reconstructed total ion chroaatograas (RIG)

                         The RIG for each saaple, extract, standard, and
                         blank Bust be normalized to the largest nonsolvent
                         component, and must contain the following header
                         information:

                         o    EPA Saaple Number

                         o    Date and time of analysis

                         o    GC/MS instrument ID

                         o    Lab file ID

                         Internal  standard and surrogate spiking compounds
                         are to be labeled with the names of the compounds,
                         either directly out from the peak, or on  a print-out
                         of retention times if retention times are printed
                         over the peak.

                                     B-10                              6/91

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4.5.2.4    Quantisation Report
           If automated data systems are used for quantisation
           of the target compounds,  the complete data system
           quantitation report must  be included in all sample
           data packages,  in addition to the reconstructed ion
           chromatogram.  The complete data system quantitation
           report shall include all  of the information listed
           below.  For laboratories  which do not use the
           automated data system procedures, a laboratory "raw
           data sheet* quantitation  report containing the
           following information must be included in the sample
           data package in addition  to the chromatogram.

           o    EPA Sample Number

           o    Date and time of analysis

           o    RT or scan number of identified target
                compounds

           o    Ion used for quantitation with measured
           o    Copy of area table from data system

           o    GC/MS instrument ID

           o    Lab file ID

           In all instances where the data system report has
           been edited, or where manual integration or
           quantitation has been performed, the GC/MS operator
           must identify such edits or manual procedures by
           initialing and dating the changes made to the report
           and include the scan range integration.

4.5.2.5    Target Compound Mass Spectra

           For each sample, by each compound identified, copies
           of raw spectra and copies of background-subtracted
           mass spectra of target compounds that are identified
           in the sample and corresponding background-
           subtracted target compound standard mass spectra are
           required.  The raw spectra and die background-
           subtracted spectra must be labeled with EPA Sample
           Number, lab file ID, date and time of analysis, and
           GC/MS instrument ID.  Compound names must be clearly
           marked on all spectra.

4.5.2.6    Tentatively Identified Compound Mass Spectra and
           Library Matches
                       B-ll                              6/91

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                   For each sample, by each compound identified, copies
                   of mass spectra of non-target and non-surrogate
                   organic compounds (Tentatively Identified Compounds)
                   with the associated spectra of the three best
                   library matches are labeled with EPA Sample Number,
                   lab file ID, date and time of analysis, and GC/MS
                   instrument ID.

4.5.3   Volatiles Standards Data

        4.5.3.1    Initial Calibration

                   All initial calibration data must be included for
                   all analyses associated with the SDG.  When more
                   than one initial calibration is performed, the
                   reconstructed ion chromatograms and quantitation
                   reports and each type of form must be put in
                   chronological order, by instrument.

                   Initial Calibration Summary (Form VI LCV).

                   Internal Standard Area and Retention Time Summary
                   (Form VIII LCV)

                   Volatile standard(s) reconstructed ion chromatograms
                   and quantitation reports for the initial (five
                   point) calibration are labeled as in Paragraphs
                   4.5.2.3 and 4.5.2.4.  Spectra are not required.

        4.5.3.2    Continuing Calibration

                   When more than one continuing calibration is
                   performed, the reconstructed ion chromatogram and
                   quantitation reports and each type of form must be
                   in chronological order, and by instrument if more
                   than one instrument is used.

                   Continuing Calibration Summary (Form VII LCV)

                   Internal Standard Area and Retention Time Summary
                   (Form VIII LCV)

                   VGA standard(s) reconstructed ion chromatograms and
                   quantitation reports for all continuing  (12 hour)
                   calibrations are labeled as in Paragraph 4.5.2.3 and
                   4.5.2.4.  Spectra are not required.
                               B-12                              6/91

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      4.5.4    Volatiles QC Data

               4.5.4.1    GC/MS  Tuning Data

                          GC/MS  Turning - BFB data, for  each  12-hour period,
                          shall  be  arranged in chronological order by
                          instrument  for each GC/MS system utilized.

                          GC/MS  Tuning and Mass Calibration  - BFB (Fora V LCV)

                          Bar  graph spectrum, labeled as  in  Paragraph 4.5.2.3.

                          Mass listing, labeled as in Paragraph 4.5.2.3.

               4.5.4.2    Blank  Data

                          Blank  data  shall be arranged  in chronological order
                          by instrument.  NOTE:  This order  is different  from
                          that used for samples.

                          Blank  data  shall be arranged  in packets with  both of
                          the  Organic Analysis Data Sheets (Form I LCV  and
                          Form I LCV-TIC), followed by  the raw data for
                          volatile  samples (see paragraphs 4.5.2.1 to
                          4.5.2.6).

               4.5.4.3    Laboratory  Control Sample Data

                          Organics  Analysis Data Sheet  for target compound
                          results (Form I LCV).  Form I LCV-TIC is not
                          required.

                          Reconstructed icn chromatogram(s)  and qusntitation
                          report(s),  labeled as in Paragraph 4.5.2.3  and
                          4.5.2.4.  Spectra are not required.

4.6   Semivolatiles Data

      4.6.1    Semivolatiles QC  Summary

               If more than a  single  form is necessary, each type of  form must
               be arranged in  chronological order, by instrument.

                          o   Surrogate  Recovery (Form II LCSV)

                          o   Laboratory Control Sample Recovery (Form III
                             LCSV)

                          o   Method Blank  Summary (Form IV LCSV)

                          o   GC/MS  Tuning  and Mass Calibration -  DFTPP (Form
                             V LCSV)

                         o   Internal Standard  Area and Retention Time
                             Summary (Form VIII LCSV-1, LCSV-2)
                                     B-13                              6/91

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4.6.2    Semivolatiles Sample Data

         Sample data,  including FES, shall the arranged in packets with
         both of the Organic Analysis Data* S&eets  (Fora I LCSV and Form
         I LCSV-TIC) ,  followed by the saw dtaea for seaivolatile samples.
         These sample packets should them Bmt gliaced in increasing EPA
         Sample Number order.

         4.6.2.1    Organic Analysis Wmtm il&aet for target compound
                    results (Fora I LOSP-U, M57-2).

         4.6.2.2    Tentatively Idmiftfffrnfl fPimji	!•  (Font I LCSV-TIC).
                    This  fora must be inulhiiftrf even if no TICs are
                    found.

         4.6.2.3    Reconstructed total ion cnromatograas (RICs)
                    The RIC for each mmyBii „ extract, standard,  and
                    blank must be nonm££zBdi to the largest nonsolvent
                    component, and move ffiimmiUfi the following header
                    information:

                    o    EPA Sample BmmBor

                    o    Date  and time oS. aomfflysis

                    o    GO/MS inst

                    o    Lab file ID
                    Internal standard andt smntDgace  spiking compounds
                    are to be labeled w£Q& en« names of the compounds,
                    either directly ostx fennt ttne peak,  or on a print-out
                    of retention fimrj  isE raatetction  times are printed
                    over the peak.
         4.6.2.4    Quantitation
                    If automated data sy»cam» procedures are used for
                    preliminary < adl of  the information listed
                    below.  For laboracmcdtes vhich do not use the
                    automated data sjacumi procedures, a laboratory "raw
                    data sheet" quantfcat&cnc report containing the
                    following infdrmmiLiui nose be  included in the sample
                    data package in a*£Lt=ixinx to  the chromatogram.
                         EPA Sample

                         Date and time aS analysis

                                B-14                             6/91

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                    o    RT  or  scan number of identified target
                         compounds

                    o    Ion used for quantisation with measured
                         area

                    o    Copy of peak area table from data system

                    o    GC/MS  instrument ID

                    o    Lab file ID

                    In all instances where the  data  system report has
                    been edited, or where manual integration  or
                    quantitation has been performed, the GC/HS operator
                    oast Identity such  edits or manual procedures by
                    *q^«?'t«T,
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                   Initial Calibration Data (Form VI LCSV-1, LCSV-2).

                   Internal Standard Area and RT Summary (Form VIII
                   LCSV-1, LCSV-2)

                   Semivolatile standard(s) reconstructed Ion
                   ehroaatograas and quantitation reports for the
                   initial (five point) calibration are labeled as in
                   Paragraphs 4.6.2.3 and 4.6.2.4.  Spectra are not
                   required.

        4.6.3.2    Continuing Calibration

                   When acre than one continuing calibration is
                   performed, the reconstructed ion chroaatogram and
                   quantitation reports and each type of fora must be
                   in chronological order, by instrument.

                   Continuing Calibration Summary(Form VII LCSV-1,
                   LCSV-2).

                   Internal Standard Area and Retention Time Summary
                   (Form VIII LCSV-1, LCSV-2).

                   Semivolatile standard(s) reconstructed ion
                   ehromatograas and quantitation reports for all
                   continuing (12 hour) calibrations are labeled as in
                   Paragraphs 4.6.2.3 and 4.6.2.4.  Spectra are not
                   required.

4.6.4.  Seaivolatiles QC  Data

        4.6.4.1    GC/HS Tuning Data

                   GC/MS Tuning-DFTPP data, for each 12-hour period
                   shall be arranged in chronological order by
                   instrument, for each GC/MS system utilized.

                   GC/MS Tuning and Mass Calibration-BFB (Form V LCSV)

                   Bar graph spectrum, labeled as in Paragraph 4.6.2.3.

                   Mass listing, labeled as in Paragraph 4.6.2.3.

        4.6.4.2    Blank Data

                   Blank data shall be arranged in chronological order
                   by instrument.  NOTE:  This order is different  from
                   that used for samples.

                   Blank data shall be arranged in packets  with both of
                   the Organic Analysis Data  Sheets  (Form I LCSV and
                   Form I LCSV-TIC), followed by  the raw data for
                               B-16                              6/91

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                         semi-volatile samples (see paragraphs 4.6.2.1 to
                         4.6.2.6)

               4.6.4.3    Laboratory Control Sample Data

                         Organic Analysis Data Sheet for target compounds
                         (Fora I LCSV-1, LCSV-2).  Form I LCSV-TIC is saj
                         required.

                         Reconstructed ion chromatogram(s) and quantitation
                         report(s), are labeled as in Paragraphs 4.6.2.3 and
                         4.6.2.4.  Spectra are not required.

4.7   Pesticide/Aroclor Data

      4.7.1    Pesticide/Aroclor QC Summary

               If more  than a  single form  is necessary, forms must be arranged
               in chronological order by instrument.

               o    Surrogate  Percent Recovery Summary (Form II LCP)

               o    Laboratory Control Sample Recovery (Form III LCP)

               o    Method  Blank Summary (Form IV LCP)

                   If  more than a  single method blank summary form is
                   necessary, forms must be arranged in chronological order
                   by  type (method or sulfur blank) by instrument, and by
                   date of analyses.

      4.7.2    Pesticide/Aroclor Sample Data

               Sample data,  including PES, shall be arranged in packets with
               the Organic  Analysis Data Sheet (Form I LCP), followed by  the
               raw data for pesticide samples.  These sample packets should
               then be  placed  in increasing EPA Sample Number order.

               4.7.2.1    Organic Analysis Data Sheet for target compounds
                         (Form I LCP).

               4.7.2.2    Pesticide Identification Summary for Single
                         Component Analytes (Form X LCP-1), only required  for
                         positively identified analytes.

               4.7.2.3    Pesticide Identification Summary for Multicomponent
                         Analytes  (Form X LCP-2) , only required for
                         positively identified analytes.

               4.7.2.4    Pesticide chromatograms

                         All  chromatograms must be labeled with the following
                         information:
                                     B-17                              6/91

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           o    EPA Sample Number

           o    Volume  injected (ul)

           o    Date and time  of analyses

           o    GC  column identification (by stationary
                phase and internal diameter)

           o    GC  instrument  identification

           o    Scaling Factor

           o    Positively identified compounds must be
                labeled with the names of  compounds,
                either  directly out from the peak,  or
                on  a print-out of retention times if
                retention times are printed over the
                peak.

4.7.2.5    Copies of pesticide chromatograms from second GC
           column,  labeled as  in Paragraph 4.7.2.4.

4.7.2.6    Data System  Printouts

           Data system  printouts of retention time  and
           corresponding peak  areas or height must  accompany
           each chromatogram are labeled with the following
           information:

           o    EPA Sample Number

           o    Volume  injected (ul)

           o    Date and time  of analyses

           o    GC  column identification (by stationary
                phase and internal diameter)

           o    GC  instrument  identification

           o    Scaling  Factor

           o    Positively identified compounds must be
                labeled  with the names of  compounds,
                either directly out from the peak,  or
                on  a print-out of retention times if
                retention times are printed over the
                peak.

           In all instances where  the  data system report has
           been edited,  or where manual  integration or
           quantitation has been performed, the GC/EC operator
           must identify such  edits or manual procedures by

                       B-18                              6/91

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                   initialing and dating the change* made to the report
                   and include the integration lime range.

        4.7.2.7    Manual work sheets.

4.7.3   Pesticide/Aroclor Standards Data

        4.7.3.1    Initial Calibration

                   Data oust be included for all calibration analyses
                   pertaining to the SDG.  Uhen more than one initial
                   calibration is performed, the data and each type of
                   form must be put in chronological order, by
                   instrument and GC column.

                   Initial Calibration for Single Component Analytes
                   (Form VI LCP-1, LCP-2).

                   Initial Calibration for Multicomponent Analytes
                   (Form VI LCP-3).

                   Resolution Check Summary (Form VI LCP-4).

                   Analytical Sequence (Form VIII LCP), containing
                   initial calibration standards.

        4.7.3.2    Calibration Verification

                   Calibration Verification Summary (Form VII LCP) for
                   all GC columns.

                   Uhen more than one calibration verification is
                   performed, forms must be in chronological order, by
                   instrument and GC column.

        4.7.3.3    Chromatograms and data system printouts are required
                   for all standards and arranged in chronological
                   order by instrument and each GC column:

                   o    Resolution Check Mixture.

                   o    Performance Evaluation Mixtures, each initial
                        calibration and all those that bracket samples
                        in the SDG.

                   o    Individual Standard Mixture A, at three
                        concentrations, each initial calibration,
                        plus all those that bracket samples in
                        the SDG.

                   o    Individual Standard Mixture B, at three
                        concentrations, each initial calibration,
                        plus all those that bracket samples in
                        the SDG.

                               B-19                              6/91

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                    o    All nultieomponent analytes (Toxaphene
                        and Aroclors), each initial
                        calibration.

                    o    All multieomponent analyte standards
                        analyzed for confiraaeion.

         4.7.3.4    Data system printouts of retention tines and
                    corresponding peak areas or peak heights oust
                    acconpany  each  chromatogram.   In addition, all
                    chromatograms and  data system  printouts are required
                    to be  labeled with the following:

                    o    EPA Sample Number for the standard,
                        i.e.,  INDAl, DJDA2, etc.  (See Forms
                        Instructions for details).

                    o    Label  all standard peaks  for all
                        individual compounds either directly
                        out from the peak or on the printout of
                        retention times if retention times are
                        printed over the peak.

                    o    Total  nanograms injected  for each
                        standard.

                    o    Date and time of injection.

                    o    GC column identification  (by stationary
                        phase  and internal diameter).

                    o    GC instrument identification.

                    o    Scaling factor

                    In all instances where the data system report has
                    been edited, or where manual integration or
                    quantitation has been performed, the GC/EC operator
                    must identity such edits or manual procedures by
                    initialing  and dating the changes made to the report
                    and  include the integration time range.

4.7.4    Festicide/Aroclor QC  Data

         4.7.4.1    Blank  Data

                    Blank  data  instrument - grouped by type of blank
                    (i.e., method and  sulfur) and  arranged in
                    chronological order.  NOTE:  This order is different
                    from that used  for samples.
                   Organics Analysis Data  Sheet for target compounds
                   (Form I LCP).
                               B-20                              6/91

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                          Blank data  shall be arranged in packets with  the
                          Organics Analysis Data Sheet (Form I LCP) followed
                          by  the raw  data (paragraph 4.7.2.2, to 4.7.2.7).

               4.7.4.2    Laboratory  Control Sample

                          Organics Analysis Data Sheet for target compounds
                          (Form I LCF).

                          Chromatograms and data system printouts are labeled
                          as  in Paragraph 4.7.2.4 and  4.7.2.6.

               4.7.4.3    Florisil Cartridge Check

                          Florisil Cartridge Check (Form IX  LCP), for all lots
                          of  cartridges used to process samples  in the  SDG.

                          Each  Form IX LCP shall be followed by  the
                          Chromatograms and data system printouts, labeled as
                          in  4.7.2.4  and 4.7.2.6.

5.    COMPLETE SDG PILE

      As specified in the Delivery Schedule, one Complete SDG File (CSF)
      including the original sample data package shall be delivered to the
      Region concurrently with delivery of copies of  the Sample Data Package
      to SMO and EMSL/LV.  The contents of the CSF will be numbered according
      to the method described  in Section III of Exhibit B.  The Document
      Inventory Sheet, Form DC-2, is contained in Section IV.  The CSF will
      contain all original documents where possible.  No copies will be
      placed in the CSF unless the originals are bound in a logbook which is
      maintained by the laboratory.  The CSF will contain all original
      documents specified in Section III, and Form DC-2 of Exhibit B.

      The CSF will consist of  the following original  documents in the order
      listed in paragraph 5.1  through 5.6 below:

5.1   The original sample data package (see Exhibit B, Section 4).

5.2   A completed and signed Document Inventory Sheet (Form DC-2).

5.3   All original shipping documents, including, but not limited to, the
      following documents:

          o  EPA Chain of Custody Record
          o  Airbills.

          o  EPA Traffic  Reports.
          o  Sample Tags  (if present) sealed in plastic bags.

5.4   All original receiving documents, including, but not limited to, the
      following documents:

          o  Form DC-1

                                     B-21                              6/91

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          o  Other receiving forms or copies of receiving logbooks
          o  SDG Cover Sheet
5.5   All original laboratory records, not already submitted in the Sample
      Data Package, of sample transfer,  preparation and analysis, including,
      but not limited to, the following documents:

          o  Original preparation and analysis forms or copies of preparation
             and analysis logbook pages.

          o  Internal sample and sample extract transfer chain-of-custody
             records.
          o  Screening records.

          o  All instrument output, including strip charts from screening
             activities.
5.6   All other original SDG-related documents in the possession of the
      laboratory, including, but not limited to, the following documents:

          o  Telephone contact logs

          o  Copies of personal logbook pages

          o  All hand written SDG-specific notes
          o  Any other SDG specific documents not covered by the above.

      NOTE:  All SDG-related documentation may be used or admitted as
      evidence in subsequent legal proceedings.  Any other SDG-specific
      documents generated after the CSF is sent to EPA, as well as copies
      that are altered in any fashion, are also deliverables to EPA.
      (Original to the Region and copies to SMO and EMSL/LV).

      If the laboratory does submit SDG-specific documents to EPA after
      submission of the CSF, the documents shall be numbered as an addendum
      to the CSF and a revised DC-2 form shall be submitted, or the documents
      should be numbered as a new CSF and a new DC-2 form should be
      submitted.  The revised DC-2 fora is sent to the Region only.

6.    DATA IN COMfUTmt-BKAP*Rirfi TQPKf

      The Contractor shall provide a computer-readable copy of the data on
      data reporting Forms I-X for all samples in the Sample Delivery Group,
      as specified in the Contract Performance/Delivery Schedule.
      Computer-readable data deliverables shall be submitted on IBM or
      IBM-compatible, 5.25 inch double-sided, double density 360 K-byte or a
      high density 1.2 M-byte diskette or 3.5 inch double-sided double
      density 720 K-byte or 1.44 M-byte diskette.

      When submitted, diskettes shall be packaged and shipped in such a
      manner that the diskette(s) cannot be bent or folded, and will not be
      exposed to extreme heat or cold or any type of electromagnetic
      radiation.  The diskette(s) must be included in the same shipment as
      the hardcopy data and shall, at a minimum, be enclosed in a diskette
      mailer.  The data shall be recorded in ASCII text file format, and
      shall adhere to the file, record and field specifications listed in

                                     B-22                              6/91

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      Exhibit H, Data Dictionary and Format for Data Deliverables in
      Computer-Readable Format.

7.    GC/MS TAPES

      See Exhibit E for requirements.

8.    EXTRACTS

      The Contractor shall store sample extracts at 4*C (±2*C) in
      bottles/vials with Teflon-lined septa.  Extract bottles/vials shall be
      labeled with EPA Sample Number, Case number and Sample Delivery Group
      (SDG) number.  A logbook of stored extracts shall be maintained,
      listing EPA Sample Numbers and associated Case and SDG numbers.

      The Contractor is required to retain extracts for 365 days following
      data submission.  During that time, the Contractor shall submit
      extracts and associated logbook pages within seven days following
      receipt of a written request from the Sample Management Office.
                                     B-23                              6/91

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                                 SECTION III

                            FORK INSTRUCTION GUIDE


This section includes specific instructions for the completion of all
required forms.  Each of the forms is specific to a given fraction (volatile,
semivolatile, pesticide/Aroclor).  The Contractor shall submit only those
forms pertaining to the fractions analyzed for a given sample or samples.
For instance, if a sample is scheduled for volatile analysis only, submit
only VGA forms.  There are two pages relating to the semivolatile fraction
for Forms I, VI, VII, and VIII and four pages relating to the
pesticide/Azoclor fraction for Form VI.  Whenever semivolatiles or
pesticides/Aroclors are analyzed and one of the above named forms is
required, all pages (LCSV-1, LCSV-2, etc.) must be submitted.  These
instructions are arranged in the following order:

     1.    General Information and Header Information

     2.    Organic Analysis  Data Sheet (Form I,  All Fractions)

     3.    Surrogate Recovery (Fora  II,  All Fractions)

     4.    Laboratory Control Sample Recovery (Form III,  All Fractions)

     5.    Method Blank Summary (Form IV, All Fractions)

     6.    GC/MS Tuning and  Mass Calibration (Form V LCV, LCSV)

     7.    Initial Calibration Summary (Form VI, All Fractions)

     8.    Pesticide Resolution Check Summary (Form VI  LCP-4)

     9.    Continuing Calibration Summary (Form VII LCV,  LCSV)

     10.  Calibration Verification  Summary (Form VII LCP)

     11.  Internal Standard Area and Retention Time Summary (Form VIII LCV,
          LCSV)

     12.  Pesticide/Aroclor Analytical Sequence (Form VIII LCP)

     13.  Pesticide/Aroclor Florisil Cartridge Check (Form IX LCP)

     14.  Pesticide/Aroclor Identification (Form X LCP)

     15.  Sample Log-In Sheet (Form DC-1)

     16.  Document Inventory Sheet (Form DC-2)
                                     B-24                              6/91

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1.    GENERAL INFORMATION AND HEADER INFORMATION

1.1   The data reporting forms presented in Section IV have been designed in
      conjunction with the computer-readable data format specified in Exhibit
      H, Data Dictionary and Format for Data Deliverables in
      Computer-Readable Format.  The specific length of each variable for
      computer-readable data transmission purposes is given in the data
      dictionary (Exhibit H).  Information entered on these forms oust not
      exceed the size of the field given on the form, including such
      laboratory-generated items as Lab Name and Lab Sample ID.

1.2   Note that on the hardeopy forms (Section IV), the space provided for
      entries is greater in some instances than the length prescribed for the
      variable as written to diskette (see Exhibit H).  Greater space is
      provided on the hardeopy forms for visual clarity.

1.3   Values must be reported on the hardeopy forms according to the
      individual form instructions in this Section.  For example, results for
      concentrations of VOA target compounds must be reported to two
      significant figures if the value is greater than or equal to 10.
      Values can be written to the diskette file in any format that does not
      exceed the field specification as given in the record specifications
      and discussed in "Record Structure", in Exhibit H.

1.4   For rounding off numbers to the appropriate level of precision, observe
      the following common rules.  If the figure following those to be
      retained is less than 5, drop it (round down).  If the figure is
      greater than 5, drop it and increase the last digit to be retained by 1
      (round up).  If the figure following the last digit to be retained
      equals exactly 5, round up if the digit to be retained is odd, and
      round down if that digit is even.

1.5   All characters which appear on the data reporting forms presented in
      the contract (Exhibit B, Section IV) must be reproduced by the
      Contractor when submitting data, and the format of the forms submitted
      must be identical, to that shown in this Superfund Analytical Method.
      No information may be added, deleted, or moved from its specified
      position without prior written approval by SMO.  The names of the
      various fields and compounds (i.e., "Lab Code", "Coloromethane") on the
      uncompleted forms must appear as they do in the this Superfund
      Analytical Method (Section IV of this exhibit) , except that the use of
      uppercase and lowercase letters is optional.

1.6   Alphabetic entries made onto the forms by the Contractor shall be in
      AL1 UPPERCASE letters.   If an entry does not fill the entire blank
      space provided on the form, null characters shall be used to remove the
      remaining underscores that comprise the blank line.  (See Exhibit H for
      more detailed instructions.)  However, do not remove the underscores or
      vertical bar characters that delineate "boxes" on the forms.  The only
      exception would be those underscores at the bottom of a "box" that are
      intended as a data entry line (for instance, see Form II LCV, line 30.
      If data must be entered on line 30, it will replace the underscores).
                                     B-25                              6/91

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1.7   Forms II, IV, V, VIII, IX, and X contain a field labeled "page _ of _"
      in the bottom left-hand corner.  If the number of entries required on
      any of these forms exceeds the available space, continue entries on
      another copy of the sane fraction-specific form, duplicating all header
      information. If a second page is required, number them consecutively,
      as "page 1 of 2" and "page 2 of 2".  If a second page is not required,
      number the page "page 1 of 1."  NOTE:  These forms are
      fraction-specific.  For example, Form II LCV, Form II LCSV, and'Form II
      LCF are for different data.  Therefore, dp not number the pages of all
      three versions of Form II as "1 of 3, 2 of 3, etc.*  Only number pages
      within a fraction-specific form.

1.8   Six pieces of information are common to the header sections of each
      data reporting form.  They are: Lab Name, Contract, Lab Code, Case No.,
      SAS No.,  and SDG No.  This information, if it applies, must be entered
      on every form and must match on every form.

      1.8.1   The  "Lab Name* shall be the name chosen by the Contractor  to
              identify the laboratory.  It may not exceed 25 characters.

      1.8.2   The  "Lab Code" is  an alphabetical abbreviation of up to 6
              letters, assigned by SMO, to identify the laboratory and aid in
              data processing.  This lab code shall be assigned at the time a
              contract is awarded, and shall not; be modified by the
              Contractor, except at the direction of  SMO.   If a change of
              name or ownership occurs at the laboratory, the lab code will
              remain the same until the Contractor is directed by SMO to use
              another lab code assigned by SMO.

      1.8.3   The  "Case No." is the assigned Case Number (up to 5 digits)
              associated with the sample, and reported on the Traffic Report.

      1.8.4   The  "Contract" is  the number of the SMO contract under which
              the  analyses were performed.

      1.8.5   When more than one sample is received in the  first or  last SDG
              shipment, the "first" sample received would be the lowest
              sample number (considering both alpha and numeric
              designations); the "last* sample received would be the highest
              sample number (considering both alpha and numeric
              designations).

      1.8.6   The  "SAS No." is the EPA-assigned number for  analyses  performed
              under Special Analytical Services.  If  samples are to  be
              analyzed under SAS only, and reported on these forms,  then
              enter SAS No., and leave Case No. blank.  If  samples are
              analyzed according to the "Routine Analytical Services*  (IFB)
              protocols and have additional "SAS" requirements, list both
              Case No. and SAS No. on all forms.  If  the analyses have no  SAS
              requirements, leave "SAS No." blank.  NOTE:   Some samples  in an
              SDG  may have a SAS No. while others do  not.
                                     B-26                              6/91

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1.9   EPA Sample Number

      1.9.1   EPA Sample Number must be entered on several of the forms.
              This field appears either in the upper right-hand corner of the
              form, or as the left column of a table summarizing data from a
              number of samples. When "EPA Sample No." is entered into the
              triple-spaced box in the upper right-hand corner of the form,
              it should be entered on the middle line of the three lines that
              comprise the box.

      1.9.2   All samples, including Laboratory Control Samples and
              Performance Evaluation Samples, blanks, and standards shall be
              identified with an EPA Sample Number.

      1.9.3   For samples, the EPA Sample Number is the unique identifying
              number given in the Traffic Report that accompanied that
              sample.  In order to facilitate data assessment, the following
              identification scheme must be used for samples:

              XXXXX    -  EPA Sample Number assigned
              XJOuumE  -  re-analyzed sample
              XXXXXDL  -  sample analyzed at a dilution
              XXXXXDL2 -  sample analyzed at a secondary dilution (for PEST
                          only)

      1.9.4   The EPA Sample Number must be unique for each Laboratory
              Control Sample within an SDG.  The EPA Sample Number for a
              Laboratory Control Sample must be FLCS##, where:

              F -  fraction (V for volatiles; S for semivolatiles; P for
              pesticides/Aroclors).

              LCS -  indicates a Laboratory Control Sanple.

              ## -  suffix consisting of characters or numbers or both that
              makes the EPA Sample Number for the LCS unique in the SDG.

      1.9.5   The EPA Sample Number must be unique for each blank within an
              SDG.  Within a fraction,  a laboratory must replace the "##"
              terminator of the identifier with one or two characters or
              numbers, or a combination of both.  For example, possible .
              identifiers for volatile blanks would be VBLK1, VBLK2, VBLKAl,
              VBLKB2, VBLK10,  VBLKAB,  etc.

              Volatile method blanks shall be identified as VBLK##.

              Volatile storage blank shall be identified in VSBLK##.

              Volatile instrument blank shall be identified as VTBLK##.

              Semivolatile method blanks shall be identified as SBLK##.

              Pesticide/Axoclor method blanks shall be identified as PBLK##.


                                    B-27                              6/91

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         Pesticide/Aroclor  instrument blanks shall be identified as
         PIBLK**.

         If  a separate  sulfur cleanup blank is required  (e.g., when not
         all Pesticide/Aroclor samples associated with a given method
         blank are  subjected to sulfur cleanup) the PesCicide/Aroclor
         sulfur  cleanup blanks shall be identified as PCBLK##.

1.9.6    The EPA Sample Number must be unique for each standard within
         an  SDG.

         The EPA Sample Numbers for volatile and semivolatile standards
         must be FSTD#**, where:

         F -  fraction  (V  for volatiles; S for semivolatiles).

         STD -  indicates a standard.

         ### -  the concentration in ug/L of volatile standards  (i.e.,
         001,  002, 005, 010) or the amount  injected in  ng for
         semivolatile standards (i.e., 005, 010, 020, 050, and 080).
         These designations will have to be concatenated with other
         information to uniquely identify each standard  in the SDG.

         For pesticide/Aroclor standards, the following  scheme shall be
         used to enter  EPA  Sample Number.
      Name
EPA Sanmle Number
      Individual Mix A (low point)       INDAL*#
      Individual Mix A (mid point)       INDAMtf*
      Individual Mix A (high point)      INDAH##
      Individual Mix B (low point)       INDBLa*
      Individual Mix B (mid point)       INDBM##
      Individual Mix B (high point)      INDBH##
      Resolution Check                   RESC##
      Performance Evaluation Mixture     PEM##
      Toxaphene                          TOXAPH##
      Aroclor 1016                       AR1016**
      Aroclor 1221                       AR1221##
      Aroclor 1232                       AR1232##
      Aroclor 1242                       AR1242##
      Aroclor 1248                       AR1248##
      Aroclor 1254                       AR1254#*
      Aroclor 1260                       AR1260##
      Aroclor 1016/1260                  AR1660##

        The laboratory must  create a unique "EPA Sample No." within an
        SDG by replacing  the two-character "##" terminator of  the
        identifier with one  or  two characters or numbers, or a
        combination of both.

        If the standards  are injected onto both GC  columns on  the  same
        instrument simultaneously,  the  same EPA Sample Number  may  be
                               B-28
                                6/91

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              used  for  reporting data  for the standards for both columns.  If
              simultaneous  Injections  are not made, then the same number may
              not be used.

1.10  Several other pieces of information are common to the header
      information on some of the data reporting forms.  These include: Lab
      Sample ID, Lab File ID, Purge or Sample Volume,  GC Column - ID,
      Instrument ID, Time Analyzed, Date Received, Extracted,  and Date
      Analyzed.

      1.10.1  "Lab  Sample ID" is an optional laboratory-generated internal
              identifier. Up to 12 alpha-numeric  characters may be  reported
              here.

      1.10.2  "Lab  File ID"  is the laboratory-generated name of the GC/MS
              data  system file containing information pertaining to a
              particular analysis.  Up to 14 alpha-numeric characters may be
              used  here.

      1.10.3  "Purge Volume" or "Sample Volume* is  the total volume of water
              that  was  purged or extracted, in milliliters.

      1.10.4  There are two  fields to  be entered  under "GO Column - ID".
              Enter the stationary phase of the GC  column after "GC Column"
              and enter the  internal diameter in  millimeters after  "ID*.

      1.10.5  "Instrument ID" is the identifier that  distinguishes  each
              instrument used for  analysis in the SDG.

      1.10.6  The "Time Analyzed"  shall be in military time.

      1.10.7  "Date Received" is the date of sample receipt at the
              laboratory, as noted on  the Sample  Traffic Report  (i.e., the
              Validated Time of Sample Receipt).  "Date Received" is entered
              as MM/DD/YY.

      1.10.8  Enter the date on which  the extraction  procedure was  started
              for "Date Extracted".  "Date Extracted" is entered as MM/DD/YY.

      1.10.9  For each  fraction, the "Date Analyzed*  is the date of the
              sample analysis.  The date of sample  receipt will be  compared
              with  the  extraction  and  analysis dates  of each fraction to
              ensure that contract holding times  were not exceeded.  "Date
              Analyzed" is entered as  MM/DD/YY.

1.11  For pesticide/Aroclors, analyses on two GC columns are required.  The
      information on the two analyses is differentiated on some of  the forms
      as "Date Analyzed  (1)", "Date Analyzed (2)", etc.   The order  of
      reporting is not  important,  but must be consistent with the information
      reported on Form X.  When simultaneous injection is made on both GC
      columns, the dates (and times)  will be the same.  If simultaneous
      injections are not made,  the (1)  shall refer to the first analysis, and
      (2) the second.    If only one analysis is required, leave blank the
      fields for the second analysis.

                                     B-29                              6/91

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2.    ORGANIC ANALYSIS DATA SHEET fFOBK T\

2.1   Target Compounds.  Fora I LCV,  LCSV-1,  LCSV-2,  and LCP

      This form is used for reporting the detected concentrations of the
      target compounds in the samples,  Laboratory Control Samples,
      Performance Evaluation Samples,  and all blanks  analyzed,  including
      method blanks,  instrument blanks,  sulfur cleanup blanks,  and storage
      blanks.

      Complete the header information on each Form I  required,  according to
      the instructions in paragraph 1.

      Enter 1 for the "Dilution Factor",  if a sample  was not diluted or
      concentrated for analysis.   If  a sample has been diluted for analysis,
      enter the "Dilution Factor* as  a single number,  such as 100 when a
      sample is diluted by a factor of 100.   Enter 0.1 when a sample is
      concentrated by a factor of 10.

      For volatiles,  the "Purge Volume"  is  the total  volume (in mL) purged
      for the analysis.

      For semivolatiles and pesticides,  enter the "Concentrated Extract
      Volume" and the "Injection Volume*  in microliters.  The "Concentrated
      Extract Volume* is the actual volume  of the most concentrated sample
      extract.   If a  dilution of the  sample extract is made in a subsequent
      analysis,  this  volume will remain the same, but the dilution factor
      will change.  Enter the *pH" of the sample before extraction, reported
      to 0.1 pH units.   Enter "Y" or  "N"  for  "Yes* or "No" under the "Sulfur
      Cleanup*  for the pesticides.

      In the concentration column,  for positively identified target
      compounds,  the  Contractor shall report  the concentrations as
      uncorrected for blank contaminants.

      For volatile and senu.volati.le results,  report analytical results to one
      significant figure if the value is  less than 10, and to two significant
      figures if greater than or equal to 10.

      Report all pesticide/Aroclor results  to two significant figures.

      If the analytical result is greater than or equal to the quantitation
      limit,  report the result.

      Under the column labeled "Q" for qualifier, flag each result with the
      specific  Data Reporting Qualifiers  listed below.  The Contractor is
      encouraged to use additional flags  (however, see "X" below).  The
      definition of such flags must be explicit and must be included in the
      SDG Narrative.

      For reporting results to the USEPA, the following contract specific
      qualifiers are  to be used.   The nine  qualifiers defined below are not
      subject to modification by the  laboratory.  Up  to five qualifiers may
      be reported on  Form I for each  compound.

                                     B-30                              6/91

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The nine  defined qualifiers to be used are as follows:

U  -      Indicates compound was  analyzed  for  but not detected.   The
         numerical value is the  sample quantitation limit and must be
         corrected for dilution.   For example,  5 U for phenol in water
         if the sample final volume  is the protocol-specified final
         volume.   If a 1 to 10 dilution of the  extract is necessary,  the
         reported limit is SO  U.

J  -      Indicates an estimated  value. This  flag is used either when
         estimating a concentration  for tentatively identified  compounds
         where a 1:1 response  is assumed,  or  when the mass spectral data
         indicate the presence of a  compound  that meets the
         identification criteria but the  result is less than the sample
         quantitation limit but  greater than  zero.   For example,  if the
         sample quantitation limit is 10  ug/L,  but a concentration of 3
         ug/L is  calculated, report  it as 3J.   The sample quantitation
         limit must be adjusted  for  dilution  as  discussed for the U
         flag.

N  -      Indicates presumptive evidence of a  compound.   This flag is
         only used for tentatively identified compounds,  where  the
         identification is based on  a mass spectral library search.  It
         is applied to all TIC results.   For  generic characterization of
         a TIC, such as chlorinated  hydrocarbon,  the M code is  not used.

B  -     This  flag is used on  the sample  Form I  when the  analyte is
         found in the associated blank as  well  as in the  sample.   It
         indicates possible/probable blank contamination and warns the
        data  user to take appropriate action.   This flag must  be used
        for a, TIC as well as  for a  positively  identified target
        compound.

        The combination of flags "BU" or "TIB"  is expressly prohibited.
        Blank contaminants are  flagged "B" only when they are  detected
        in the sample.

E -     This  flag identifies  compounds whose concentrations exceed the
        initial  calibration range of the  instrument for  that specific
        analysis.   If one or  more compounds have a response that exceed
        the initial calibration  range, the sample or extract must be
        diluted  and reanalyzed according  to  the specifications in
        Exhibit  D.  All  such compounds should have the  concentration
        flagged  with an "E" on the  Form  I for the original analysis.
        The dilution of the extract may  cause some compounds identified
        in the first analysis to be below the calibration range in the
        second analysis.   The results of  both  analyses shall be
        reported on separate  Forms  I.  The Form I for  the diluted
        sample shall have the "DL"  (or "DL2")  (for pesticide samples
        only) suffix appended to the EPA  Sample Number.   NOTE:   For
        total xylenes,  where  three  isouers are  quantified as two peaics,
        the calibration range of each peak should be considered
        separately,  e.g.,  a diluted analysis is not required for total
        xylenes  unless  the concentration  of  the peak representing the

                              B-31                               6/91

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              single isomer exceeds 25 ftg/L or the peak representing  the  two
              coeluting isomers on that GC column exceeds 50 /*g/L.

      D -     If a sample or extract is diluted and re-analyzed, as in the
              "E" flag above, all concentration values  reported on that Form
              I are flagged with the "D" flag.  The "DL" or "DL2" (for
              pesticide samples only) suffix is appended to the EPA Sample
              Number on the Form I for the diluted sample.

      A -     This flag is not used under this contract, but; is reserved.

      P -     This flag is used for a pesticide/Aroclor target  analyte when
              there is greater than 25.0% difference between the
              concentration calculated from the two GC  columns  (see Form  X)
              The lower of the two values is reported on Form I and flagged
              with a "P".

      X -     Other specific flags may be required to properly  define the
              results.  If used, they must be fully described and such
              description attached to the Sample Data Summary Package and the
              SDG Narrative.  Begin by using "X".  If more than one flag  is
              required, use "Y" and "Z", as needed.  If more than five
              qualifiers are required for a sample result, use  the "X* flag
              to combine several flags, as needed.  For instance, the "X"
              flag might combine the "A", "B", and "D"  flags for some sample.

2.2   Non-target Compounds.   Form I LCV-TIC and LCSV-TIC

      Fora I LCV-TIC and LCSV-TIC are used for reporting the tentative
      identification and estimated concentration for up to 10 of the non-
      surrogate and non-target organic compounds in the volatile fraction and
      up to 20 of the non-surrogate and non-target organic compounds  in the
      semivolatile fraction.

      Include a Form I LCV-TIC or LCSV-TIC for every volatile and
      semivolatile fraction of every sample, Performance Evaluation Sample,
      and blank analyzed.   Form I LCV-TIC or LCSV-TIC must be provided for
      every analysis (except for the Laboratory Control Samples) that
      requires a Form I for target compounds,  including required dilutions
      and reanalyses,  even if no TICs are found.

      Fill in all header information as section 2.1.

      Report tentatively identified compounds (TICs)  including  CAS number,
      compound name,  retention time,  and the estimated concentration
      (criteria for reporting TICs are given in Exhibit D).  Retention time
      must be reported in minutes and decimal minutes, not seconds or  minutes
      and seconds.

      If in the opinion of the mass spectral interpretation specialist, no
      valid tentative identification can be made, the compound  shall be
      reported as unknown.
                                     B-32                              6/91

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      Total the number of TICs found and enter this number in the "Number
      TICs found." If no TICs were found, enter "0" (zero).

      If the name of a compound exceeds the 28 spaces in the TIC column,
      truncate the name to 28 characters.  If the compound is an unknown,
      restrict description to no more than 28 characters (i.e., unknown
      hydrocarbon, etc.).

      All TIC results, except "generics" (See N flag) are flagged "JN" in  the
      "Q" column to emphasize the quantitative and qualitative uncertainties
      associated with these data.  This includes "unknowns*.

3.    SURROGATE RECOVERY.  POBM II LCV. LCSV. AND LCP

      Form II is used to report the recovery of the surrogate compounds  added
      to each sample, blank, Laboratory Control Sample, and Performance
      Evaluation Sample.

      Complete the header information on each Form II required, according  to
      the instructions in paragraph 1.

      In the table, enter EPA Sample Numbers for each analysis as described
      in paragraph 1.  For each sample, report the percent recovery for  each
      surrogate to the nearest whole number.

      Flag each surrogate recovery outside the QC limits with an asterisk
      (*). The asterisk must be placed in the last space in each appropriate
      column, under the "#" symbol.  In the far right-hand column, total the
      number of surrogate recoveries outside the QC limits for each sample.
      If no surrogates were outside the limits, enter "0".

      If a sample or extract is diluted and the surrogate recovery is below
      the recovery limits in any analysis, enter the calculated recovery or
      "0* (zero) if the surrogate is not detected.  Flag the surrogate
      recovery with a "D* in the column under the "#" symbol.  Do not include
      results flagged "D* in the total number of recoveries for each sample
      outside the QC limits.

      Pesticide/Aroclor samples are analyzed on two GC columns, and
      surrogates recoveries must be reported for both analyses.  Enter the
      information on the stationary phases and internal diameters of the two
      GC columns, as described in paragraph 1.10.4, differentiating the  GC
      columns as "(1)" and "(2)".  Enter the recoveries of the two surrogates
      for each column in a similar fashion.

      Number the Form II pages as described in paragraph 1.7.

4.    LABORATORY CONTROL SAKPTJt BECOVERY.  FORM III LCV. LCSV. AND LCP

      Form III is used to report the recovery of the spiked analytes  in  the
      Laboratory Control Sample (LCS).

      Complete the header information on each Form III required, according to
      the instructions in Sections 1 and 2.

                                     B-33                              6/91

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      The "LCS Lot No. * is an identification number assigned by the Agency to
      the LCS spiking solution, if the solution is provided by the Agency.
      If the LCS solution is purchased by the Contractor from a third party,
      report the identification number used by the laboratory under "LCS Lot
      No.".

      The "LCS Aliquot" is the volume in microliters of LCS spiking solution
      that was added to reagent water before purging or extraction.

      For pesticides, the LCS is reported for both GC columns.  Enter the
      Instrument ID and GC Column - ID for analyses on both GC columns.   The
      order of reporting is not important, but must be consistent with the
      information reported on Form X,  If simultaneous injections are not
      made,  the "Date Analyzed" is the earlier date of the two LCS analyses.

      In the upper box in Form III, under "AMOUNT ADDED", enter the amount in
      nanograms of each analyte added to the sample.  Under "AMOUNT
      RECOVERED",  enter the amount in nanograms of each analyte in the sample
      calculated from analysis.  Calculate the percent recovery of each
      compound in the sample to the nearest whole percent, according to
      Exhibit D, and enter under "% REG".  Enter the limits for each analyte
      in the column for "QC LIMITS*.  The limits should be entered as two
      whole numbers (lower and upper limits) separated by a hyphen.  Flag all
      percent recoveries which do not meet the contract requirements with an
      asterisk (*).  The asterisk must be placed in the last space of the
      percent recovery column, under the •#• symbol.

      Summarize the values outside the QC limits at the bottom of the page.

5.    METHOD BLANK SUMMARY.  FORM IV LCV. LCSV. AND LCP

      Form IV lists the samples including LCS and FES associated with each
      method blank.  A copy of the appropriate Form IV is required for each
      method blank.

      Complete the header information on each Form IV required, according to
      the instructions in Sections 1.

      For semi-volatile and pesticide/Aroclor method blanks, enter the date of
      extraction of the blank.

      For pesticide/Aroclors, enter the "Date Analyzed", "Time Analyzed",
      "Instrument ID",  and "GC Column - ID* for analyses on both GC columns.

      For all three fractions, as appropriate, summarize the samples,
      including LCS and PES associated with a given method blank in the  table
      below the header, entering EPA Sample Number and Lab Sample ID.  For
      volatiles, enter the Lab File ID and Time Analyzed for each sample.
      For seaivolatiles, enter the Lab File ID and Date Analyzed. For
      pesticides/Aroclors, enter the Date Analyzed on each GC column for each
      sample.

      For pesticides/Aroclors, enter "Y" or "N" (for yes or no) under "Sulfur
      Cleanup".  If a separate sulfur cleanup blank is prepared, when not all

                                     B-34                              6/91

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      samples associated with a method blank are subjected to sulfur cleanup,
      then complete & separate Form IV for the sulfur cleanup blank, listed
      the EPA Sample No. of the blank, as described in paragraph 1.9.6, in
      the box in the upper right hand corner of the form.  These samples
      associated with the sulfur cleanup blank will be listed in the lower
      portion of the form, as well as on a copy of Fora IV for their
      associated method blank.  Whenever all the .samples and their associated
      method blank are subjected to sulfur cleanup, no separate sulfur blank
      is required, and only one Form TV needs to be completed.

      Number the Form TV pages as described in paragraph 1.7.

6.    GC/MS TUNING ASP MAS? Cf LT??f TTQK •  FORM V LCV AMD LCSV

      This form is used to report the results of GC/MS tuning for volatiles
      and semivolatiles, and to summarize the date and time of analysis of
      samples, standards, and blanks associated with each GC/MS tune
      (including Laboratory Control and Performance Evaluation Samples).

      Complete the header information on each Form V required, according to
      the instructions in paragraph 1.

      Enter the "Lab File ID" for the injection containing the GC/MS tuning
      compound (BFB for volatiles,  DFTPP for semivolatiles).   Enter the date
      and time of injection of the tuning compound.  Enter injection time as
      military time.

      In the upper table, for each ion listed on the form, enter the %
      Relative Abundance in the right-hand column.  Report relative
      abundances to the number of significant figures given for each ion in
      the ion abundance criteria column.

      Note that for both BFB and DFTPP,  one or more of the high mass ions may
      exceed the abundance of the ion listed on the form as the base peak
      (m/z 95 for BFB,  and m/z 198 for DFTPP).   Despite this  possibility, all
      ion abundances are to be normalized to the nominal base peaks listed on
      Form V (see Exhibit D).

      All relative abundances must be reported as a number.  If zero, enter
      "0",  not a dash or other non-numeric character.   Where  parentheses
      appear, compute the percentage of the ion abundance of the mass given
      in the appropriate footnote,  and enter that value in the parentheses.

      In the lower half of the form,  list all samples, standards, and blanks
      analyzed under that tune in chronological order. by time of analysis
      (in military time).   Refer to paragraph 1 for specific  instructions for
      identifying standards and blanks.   Enter "EPA Sample No.",  "Lab Sample
      ID",  "Lab File ID",  "Date Analyzed",  and "Time Analyzed" for all
      standards,  samples  including LCS and PES,  and blanks.

      Number che  Form V pages  as described in paragraph 1.7.
                                     B-35                              6/91

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7.    INITIAL CALIBRATION SUMMARY.   FORM VI LCV.  LCSV-1.  LCSV-2.  LCP-1.  LCP-2
      AND LCP-3

      For each fraction,  after a GO/MS or GC system has undergone an initial
      calibration,  and after all initial calibration technical criteria  have
      been met, the laboratory must complete and submit all Fora  Vis for
      initial calibrations performed relevant to the samples including LCS
      and FES and blanks  in the SDG,  regardless of when that calibration was
      performed.

      Complete the header information on each Form VI required, according to
      the instructions in paragraph 1.

      Enter the "Case No.* and "SDG No.* for the current  data package,
      regardless of the original Case for which the initial calibration  was
      performed.  Enter "Instrument 10" and "Calibration  Date(s)".   If the
      calendar date changes during  the calibration procedure,  the inclusive
      dates should be given on Form VI.

      For the volatile and semivolatile fractions,  enter  the "Lab File ID"
      for each of the five calibration standards injected.   Complete the
      response factor data for the  five calibration points.  The  relative
      response factor (RRF) is reported for each target compound  and
      surrogate.  The laboratory must report the average  RSLF and  the percent
      relative standard deviation (%RSD) for the RRFs for each target
      compound and surrogate.

      The initial calibration of pesticides and Aroclors  involves the
      determination of retention times, retention time windows, and
      calibration factors.  For single component pesticide  target compounds,
      these data are calculated from the analyses of the  Individual Standard
      Mixtures A and B at three different concentration levels.   For the
      multicomponent target compounds,  these data are calculated  from a
      single point calibration.

      Complete header information on Form VI,  LCP-1 and LCP-2 according  to
      the instructions in paragraph 1.   For the three analyses of Individual
      Standard {fixture A  (low point,  mid point,  and high  point),  and the
      three analyses of Individual  Standard Mixture B performed on each  GC
      column during an initial calibration, complete one  copy of  Form VI for
      each GC column used.  Enter the Instrument ID, GC Column, and ID as
      described previously.  Enter  the dates of analysis  of the first and
      last of the six standards on  each form under "Date(s) Analyzed".  Under
      •Level (x low)", enter the concentration of the low point,  mid point,
      and high point calibration standards as a multiplier  of the low point.
      Therefore, for the  low point,  enter "1.0".   The concentration of the
      mid point standard  is specified in Exhibit D as four  times  the low
      point, therefore, enter "4.0" for "mid".  If the concentration is  not
      exactly 4.0 times the low point,  enter the appropriate multiplier  in a.
      similar format.  The high point standard must be at least 16 times the
      low point, but may  be higher  if that value lies within the  linear  range
      of the instrument,  as specified in Exhibit D.  Therefore, enter the
      appropriate multiplier to the high point standard concentration to one
      decimal place.

                                     B-36                             6/91

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      For the pesticides/Aroclors fraction, one Fora VI (LCP-1 and LCF-2) is
      required for each initial calibration performed on each GC column.  In
      the table, on Form VI LCP-1, enter the retention time of each analyte
      in the low, mid, and high point Standard Mixtures A and B in the
      columns labeled "RT of Standards".  Use the values from Standard
      Mixture A for the surrogates.  Calculate and report in the appropriate
      column the mean retention time and the retention time windows for each
      analyte.  Report the retention time window for each analyte as a range
      of two values, i.e., from 1.44 to 1.54.  Enter the lower value of the
      range in the column under "RT WINDOW" labeled "FROM".  Enter the upper
      value of the range in the column under "TO".  Do not separate the two
      values with a hyphen, and do not enter the retention time window as a
      plus/minus value such as ±0.05.  NOTE: By definition, the center of the
      retention time window must be the mean retention time listed to the
      left of the retention time window.

      On Form VI LCF-2, calculate the calibration factor for each analyte in
      the low, mid, and high point Standard Mixtures A and B.  Use the values
      from Standard Mixture A for the surrogates.  Report the values under
      the columns labeled "CALIBRATION FACTORS".  Calculate the mean of the
      three calibration factors and the percent relative standard deviation
      (%RSD) for the calibration factor values for each analyte.  Report the
      calculated values under the "MEAN" column the "%RSD" columns,
      respectively.

      On Form VI LCP-3, for the initial calibration of multicomponent
      analytes, enter the amount of standard injected in nanograms of each
      analyte, under the "AMOUNT" column.  The number of peaks with an
      asterisk under the "Peak" column indicates the minimum number of peaks
      calibrated for each analyte.  Enter the retention time of each peak
      used to quantitate under the "RT" column.  Data for two additional
      peaks may be reported for each multicomponent analyte.  Calculate and
      report the calibration factor for each peak used under "CALIBRATION
      FACTOR".

8.    PESTICIDE RESOLUTION CHECK SUMMARY.  FORM VI LCP-4

      Pesticide Resolution Check Summary Form VI is used to report the
      resolution of each analyte in the Resolution Check Mixture analyzed at
      the beginning of each initial calibration on each GC column.

      Complete the header information on each Form VI required according to
      the instructions in paragraph 1.

      For each GC column,  enter the "EPA Sample Number" of the Resolution
      Check Mixture, as described in paragraph 1.9.7, for the mixture
      injected on the first GC column.  Enter the Lab Sample ID, Date
      Analyzed (1), and Time Analyzed (1).

      In the table, under "ANALYTE",  enter the name of each analyte as  it
      appears on Form I,  in elution order, starting with the first target
      analyte or surrogate to elute.   Enter the retention time of each  of the
      analytes listed under "RT".
                                     B-37                  .            6/91

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      Calculate the percent resolution between each pair of consecutive peaks
      according to Exhibit D.  Enter the percent resolution of each pair in
      the "RESOLUTION" field of the analyte that elutes earlier (the analyte
      listed first).  The resolution must be calculated for each adjacent
      peaks so that the resolution of peak 1 and peak 2 is calculated, as
      well as peak 2 vs. peak 3, peak 3 vs. peak 4, etc.  The "RESOLUTION"
      field will be left blank for the last analyte in the in the table.  The
      percent resolution must meet the QC limits listed at the bottom 'of the
      page.

      Complete the information for the second GC column in the same fashion.

9.    coNTiNUJj^e CALIBRATION SUMMARY.  FORM vn LCV. LCSV-I AND Lcsv-2

      The Continuing Calibration Summary Form VII is used to verify the
      calibration of the GC/MS system by the analysis of specific calibration
      standards.  Form VII is required for each 12 hour time period for both
      volatile and semivolatile analysis.

      Complete the header information on each Form VII required, according to
      the instructions in paragraph 1.

      Enter date and time of continuing calibration standard analysis, the
      Lab File ID of the continuing calibration standard, and date(s) of
      initial calibration.  Give inclusive dates if initial calibration is
      performed over more than one date.  Enter the average relative response
      factor (RRF) for each target compound that was calculated from the
      initial calibration data (referred to in the initial calibration
      date(s) analyzed field).  Report the relative response factor for each
      target compound and surrogate from the continuing calibration standard
      analysis.

10.   PSSTICIDE/AROCLQH, CALIBRATION VERIFICATION

      Calibration Verification Summary.  Form VII LCP-1 and LCP-2

      The Calibration Verification Summary Form VII is used to report the
      results of the Performance Evaluation Mixtures (PEM), instrument
      blanks, and Individual Standard Mixtures A and B analyzed at the
      beginning and end of a twelve hour sequence.  The laboratory must
      submit this form for each twelve hour sequence analyzed.

      Complete the header information on each Form VII required according to
      the instructions in paragraph 1.

      Enter the initial calibration date(s) analyzed.  Give inclusive dates
      if initial calibration is performed over more than one date.

      On Form VII, LCP-1, enter the EPA Sample No., Lab Sample ID, Date
      Analyzed,  and Time Analyzed for the instrument blank that preceded the
      twelve hour sequence (PIBLK).  For the PEM that initiated or terminated
      the twelve hour sequence (PEM), enter the EPA Sample No., Lab Sample
      ID, Date Analyzed, and Time Analyzed.
                                     B-38                              6/91

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 When reporting data for Che PEM at the beginning of the initial
 calibration sequence,  leave blank the "EPA Sample No.", "Lab Sample
 ID",  and "Date" and "Time Analyzed" fields for the instrument blank
 (PIBLK),  as no instrument blank is analyzed before this PEM.  When
 reporting all other PEM analyses,  the instrument blank fields must be
 completed.

 In the table,  report the retention time for each analyte in the PEM as
 veil  as  the retention time windows.  For each analyte in the PEM,  enter
 the amount of the analyte in nanograms,  to three decimal places,
 calculated to be in the PEM,  under "CALC AMOUNT".   Enter the nominal
 amount of each analyte in the PEM under "NOM AMOUNT".   Calculate the
 relative  percent difference between the calculated amount and nominal
 amount for each analyte according to Exhibit D.   Report the values
 under "%D".

 Calculate the percent  breakdown for endrin and 4,4'-DDT,  and the
 combined  percent breakdown in the  PEM according  to Exhibit D.   Enter
 the values  for the breakdown of endrin and 4,4'-DDT in their respective
 fields immediately under the  table.

 Form  VII  LCP-2 is used to report the dates and times of analysis of the
 instrument  blanks and  the results  of the analyses of the midpoint
 concentrations of Individual  Standard Mixtures A and B that, along with
 the PEM,  bracket each  12-hour period of sample analyses.   One copy of
 Form  VII  LCP-2 must be completed each time the Individual Standard
 Mixtures  are  analyzed,  for each GC column used.   The form is completed
 in a.-  similar  fashion to Form  VII LCP-1,  entering the EPA Sample No.,
 Lab Sample  ID,  Date Analyzed,  and Time Analyzed  for the instrument
 blank immediately preceding the Individual Standard Mixtures A and B,
 and for the standards  themselves.   The upper table on the form contains
 the retention time and amount data for Individual  Standard Mixture A
 compounds.  The lower  table contains the data for  Mixture B.   Enter the
 data  in these  tables in a. fashion  similar to that  for the PEM.
 Complete  copies of Form VII LCP-1  and 2  for each standard reported in
 Form VIII LCP.


 ASP LCSV-2

 Fora VIII is used to summarize  the  peak  areas  and  retention times  of
 the internal standards  added  to  all volatile and semivolatile  samples
 and blanks.  Form VIII  is  also used to check the internal standards in
 the initial calibration sequences.   The  data are used to  determine when
 changes in internal  standard  responses will  adversely affect
 quantisation of target  compounds.   This  form must  be completed each
 time an initial  calibration or  a continuing  calibration is performed,
or when samples  are  analyzed  under  the same  GC/MS  tune  as an initial
calibration.

Complete the header  information on each  Form VIII  required,  according
to the instructions  in  paragraph 1.
                               B-39                              6/91

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      Enter the Lab File ID, Date Analyzed, and Tine Analyzed for the
      continuing calibration standard.  If samples are analyzed immediately
      following an initial calibration, before another GC/MS tune and a
      continuing calibration, Fora VIII shall be completed for the initial
      calibration standard that is the same concentration as the continuing
      calibration standard.  Enter the Lab File ID, the date and time of
      analysis, the areas and retention tines of this initial calibration
      standard in place of those of a continuing calibration standard.-

      From the results of the analysis of the continuing calibration
      standard, enter the area measured for each internal standard and its
      retention time under the appropriate column in the rov labeled "12 HOUR
      STD".  For each volatile internal standard, calculate the area upper
      limit as the area of the particular internal standard plus 40 percent
      of its area, and the area lower limit as the area of the internal
      standard minus 40 percent of its area.  For each semivolatile internal
      standard, calculate the area upper limit as the area of the particular
      standard plus 100% of its area (i.e., two times the area in the 12 HOUR
      STD box), and the area lower limit as the area of the internal standard
      minus 50% of its area (i.e., one half the area in the 12 HOUR STD box).
      Report these values in the boxes labeled "UPPER LIMIT* and "LOVER
      LIMIT* respectively.

      For each volatile and semivolatile internal standard, calculate the
      retention time (RT) upper limit as the RT of the particular internal
      standard plus 0.33 minutes.  The lower limit is the RT of the internal
      standard minus 0.33 minutes.  Report these values in the boxes labeled
      "UPPER LIMIT* and "LOVER LIMIT* respectively.

      For each sample including LCS and PES and blank analyzed under a given
      continuing calibration, enter the EPA Sample Number and the area
      measured for each internal standard and its retention time.  If the
      internal standard area or retention time is outside the upper or lower
      limits calculated above, flag that value with an asterisk (*).  The
      asterisk must be placed in the far right hand space of the box for each
      internal standard area or retention time, directly under the "#"
      symbol.

      If samples are analyzed immediately following an initial calibration as
      described above, enter the EPA Sample Number, internal standard areas,
      and retention times for all five of the initial calibration standards.

      Number the Form VIII pages as described in paragraph 1.7.

12.   PESTICIDE/AROCLOR ANALYTICAL SEQUENCE.  FORM VIII LCP

      Form VIII LCP is required for each analytical sequence for each GC
      system and for each GC column used to analyze pesticide/Aroclors in an
      SDG.

      Complete the header information on each Form VIII required, according
      to the instructions in paragraph 1.
                                     B-40                              6/91

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      Enter the initial calibration date(s).  Give inclusive dates if initial
      calibration is performed over more than one date.

      At the top of the table, report the mean retention time for surrogates
      tetrachloro-m-xylene and decachlorobiphenyl calculated from the initial
      calibration sequence under "TCX" and "DCS", respectively.  For every
      analysis associated with a particular analytical sequence starting with
      the initial calibration, enter the EPA Sample Number, Lab Sample ID,
      Date Analyzed, and Time Analyzed.  Each sample analyzed as part of the
      sequence must be reported on Form VIII LCF even if it is not associated
      with the SDG.  The laboratory may use the EPA Sample No. of "Z2ZZZ" to
      distinguish all samples that are not part of the SDG being reported.
      Report the retention time of the surrogates for each analysis under
      •TCX RT* and "DCS RT".  All sample analyses must be bracketed by
      acceptable analyses of instrument blanks, a FEM, and Individual
      Standard Mixtures A and B.  Given the fact that the initial calibration
      may remain valid for some time (see Exhibit D), it is not necessary to
      report the data from 12-hour periods when no samples in an SDG were
      run.  The laboratory must deliver the Form VIII for the initial
      calibration sequence, and Forms that include the PEMs and Individual
      Standard Mixtures that bracket any and all samples in the SDG.  While
      the data for time periods between the initial calibration and samples
      in the SDG is not a routine deliverable, it must be made available on
      request during on-site evaluations, etc.  Here again, non-EPA samples
      may be indicated with "ZZZZZ".

      Flag all those values which do not meet the contract requirements by
      entering an asterisk (#) in the last column, under the "*".  If the
      retention time cannot be calculated due to interfering peaks, leave the
      RT column blank for that surrogate, enter an asterisk in the last
      (i.e., under "DCS") column, and document the problem In the SDG
      Narrative.

      Number the Form VIII pages as described in paragraph 1.7.

13.   PESTICIDE/AROCLOR FLORISIL CARTRIDGE CHECK.  FORM IX LCP

      Form IX is required for each lot of Florisil cartridges that is used
      with samples associated with the SDG.

      Complete the header information on each Form IX required, according to
      the instructions in paragraph 1.

      Enter the "Case No." and "SDG No." for the current data package,
      regardless of the original Case for which the cartridge check was
      performed.  Enter the "Florisil Cartridge Lot Number".   Enter under the
      "Date Analyzed",  the date the Florisil cartridge check solution was
      analyzed.

      In the upper table,  enter the amount of spike added and spike recovered
      in nancgrams for each analytt.

      Calculate to the nearest whole percent,  and enter the percent recovery
      in the "% REG"  field.   Flag each spike recovery outside the QC limits

                                     B-41                              6/91

-------
      with an asterisk  (*).  The asterisk must be placed in Che last space  in
      the "% Rec* column, under the "#" symbol.

      In the lower table, enter the "EPA Sample No.", the "Lab Sample  ID",
      and "Date Analyzed" for each sample and blank that was cleaned up using
      this lot of Florisil cartridges.

      Number the Form IX pages as described in paragraph 1.7.

14.   PESTICIPg/AROCLOR IDENTIFICATION.  FORM X LCP-1. LCP-2

      Form X summarizes the data used to identify and quantify all
      pesticide/Aroclor target analytes detected in a given sample.  Form X
      LCP-1 is required for each sample (including PES and LCS) or blank in
      which any single  component analytes is detected.  Form X LCP-2 is
      required for each sample (including PES and LCS) or blank in which any
      multicomponent analyte is detected.  If no single component analyte or
      multicomponent analyte is detected in a sample, no copy of the
      applicable Form X is required for that sample.

      Complete the header information on each Form X required, according to
      the instructions  in paragraph 1.

      For each target pesticide or Aroclor detected, enter the name of the
      analyte on Form X in the column labeled "Analyte", spelling the  name  as
      is appears on Form I.  For the multicomponent analytes, there are
      spaces (fields) for up to 5 peaks for each analyte.  The asterisks
      indicate the number of peaks that are required, and data for additional
      peaks may be reported.  The retention time, retention time window, and
      concentration are calculated separately for each peak used for a
      multicomponent analyte.  For each GC column, enter the retention times
      of the analytes detected in the sample next to the appropriate column
      designation (1 or 2).  Enter the retention time windows on each  column
      of the appropriate standard.  The lower value is entered under the
      "FROM" column, the upper value under the "TO* column.  Do not use a
      hyphen.  These data must correspond with those on Form VI, and are
      entered in a similar manner. Calculate the concentration of the  analyte
      using the calibration factors derived from the initial calibration
      sequence.  For the multicomponent analytes, calculate and report the
      mean concentration by averaging the concentration values from the peaks
      used for quantitation.  Calculate and report the percent difference to
      a tenth of a percent between the concentration values (or mean
      concentration values for multicomponent analytes) on the two GC  columns
      under "%D* as described in Exhibit D.

      Number the Form X pages as described in paragraph 1.7.

                   THE FOLLOWING ARE DOCUMENT CONTROL FORMS

                      (To be submitted as hardcopy only)

15.   SAMPT.g LOG-IH SHEET (FORM DC-1^

      This form is used to document the receipt and inspection of samples and
      containers.   One original of Form DC-1 is required for each sample

                                     B-42                              6/91

-------
 shipping container.   If the samples  in a single sample shipping
 container (e.g.,  coolers) must be  assigned to more than one  Sample
 Delivery Group,  the  original  Form  DC-1 shall be placed with  the
 deliverables  for the Sample Delivery Group with the lowest sample
 number  and a  copy of Form DC-1 must  be placed with the deliverables  for
 the  other Sample Delivery Group(s).  The copies should be identified as
 "copy(ies), •  and the location of the original should be noted on the
 copies.

 Sign and date the airbill (if present).  Examine the shipping container
 and  record the presence/absence of custody seals and their condition
 (i.e.,  intact, broken)  in item 1 on  Form DC-1.  Record the custody seal
 numbers  in item  2.

 Open the container,  remove the enclosed sample documentation,  and
 record  the  presence/absence of chain-of-custody record(s), SMO forms
 (i.e., Traffic Reports,  Packing Lists), and airbills or airbill
 stickers in items 3-5 on Form DC-1.  Specify if there is an  airbill
 present  or  an airbill sticker in item 5 on Form DC-1.  Record the
 airbill  or  sticker number in  item  6.

 Remove  the  samples from the shipping container(s), examine the samples
 and  the  sample tags  (if present),  and record the condition of the
 sample bottles (i.e., intact, broken, leaking) and presence  of absence
 of sample tags in items  7 and 8 on Form DC-1.

 Review the  sample shipping documents and complete the header
 information described in Part A.   Compare the information recorded on
 all  the  documents and samples and  mark the appropriate answer in item 9
 on Form  DC-1.

 If there are  no  problems observed  during receipt, sign and date
 (include time) Form  DC-1, the chain-of-custody record, and Traffic
 Report,  and write the sample  numbers on Form DC-1.  Record the
 appropriate sample tags  and assigned laboratory numbers if applicable.
 The  log-in  date  should be recorded at the top of Form DC-1 and the date
 and  time of cooler receipt at the  laboratory should be recorded  in
 items 10 and  11.   Cross  out unused columns and spaces.

 If there are  problems observed during receipt or an answer marked with
 an asterisk (i.e., "absent*") was  marked, contact SMO and document the
 contact  as well  as resolution of the problem on a CLP Communication
 Log.  Following  resolution, sign and date the forms as specified in  the
 preceding paragraph  and  note, where  appropriate, the resolution  of the
 problem.

Record the fraction  designation (if  appropriate) and the specific area
 designation (e.g., refrigerator number) in the. Sample Transfer block
 located  in  the bottom left corner  of Form I.  Sign and date  the  Sample
Transfer block.
                               B-43                              6/91

-------
16.    DOCUMENT IKVKNTORY SHEET (FORM DC-2^

      This form is used to record the inventory of the Complete SDG File
      documents and count of documents in the original Sample Data Package
      which is sent to the Region.

      Organize all complete SDG file documents as described in Exhibit B,
      Section II,  paragraph 5.  Assemble the documents in the order specified
      on Form DC-2,  and stamp each page with a consecutive number.  (Do not
      number the DC-2 form).   Inventory the CSF by reviewing the document
      numbers and recording page number ranges in the columns provided in the
      Form DC-2.  If there are no documents for a specific document type,
      enter an "NA" in the empty space.

      Certain laboratory specific documents related to the CSF may not fit
      into a clearly defined category.  The laboratory should review DC-2 to
      determine if it is most appropriate to place them under No. 7, 8, 9, or
      10.  Category 10 should be used only if there is no appropriate
      previous category.  These types of documents should be described or
      listed in the blanks under each appropriate category.
                                     B-44                              6/91

-------
     SECTION IV
DATA REPORTING FORMS
        B-45                               6/91

-------
                             1LCA
   LOW CONG. WATER VOLATILE ORGANICS ANALYSIS DATA SHEET
                                         EPA SAMPLE NO.
'  b Name:

Lab Code:
Case No.:
Contract:

 SAS No.:
                                    SDG No.:
Lab Sample ID:

Lab File ID:

Purge Volume:


       CAS NO.
                          Date Received:

                          Date Analyzed:
   (mL)


   COMPOUND
         Dilution Factor:
               CONCENTRATION
                  (ug/L)
7 4-87-3 	 Chloromethane


75-01-4 	 Vinvl chloride
75-00-3 	 Chloroethane
75-09-2 	 Methylene chloride
67-64-1 	 Acetone
75-15-0 	 Carbon disulfide
75-35-4 	 1. 1-Dichloroethene
•7 K _ t A _.^ _________ 1 1 _n i r^i ^ m*»n A+-1* ana
/ 3— j*— j— — — x , x— uxcii.Loroci.rm nc
156-59-4 	 cis-1 . 2-Dichloroethene
156-60-5 	 trans-1, 2-Dichloroethene
67-66-3 	 Chloroform
107-06-2 	 1 , 2-Dichloroethane
78-93-3 	 2 -Butanone
74-97 -5 	 Br omochlor omethane
71-55-6 	 1 , 1 , 1-Trichloroethane
56-23-5 	 Carbon tetrachloride
75-27-4 	 Bromodichloromethane
78-87-5 	 1, 2-Dichloropropane
10061-01-5 	 cis-1 , 3-Dichloropropene

/ j»— ux— o— — — AiiciiAoroeiineiie
124-4 8-1 	 D ibr omochlor omethane
79-00-5 	 1 , 1 , 2-Trichloroethane
71-43-2 	 Benzene
10061-02-6 	 trans-l, 3-Dichloropropene


108-10-1 	 4-Methyl-2-pentanone
591-78-6 	 	 — 2-Hexanone
127-18-4 	 Tetrachlor oethene
*7Q_1 A _RM__.______1 1 *} *>_fPn^»— a«-tH 1 n-*-rtn^H a«rt
/y — j* —3— — — x, x, *• i *• — i e ti acn j.or oe unane
106-93-4 	 -1,2-Dibromoethane
108-88-3 	 Toluene
108-90-7 — — — Chlor obenz ene
100-41-4 	 	 Ethylbenzene
100-42-5 	 Styrene


541-73-1 	 1,3-Dichlorobenzene


95-50-1 	 1 , 2-Dichlorobenzene





















































































                                FORM I LCV
                                                  6/91

-------
                             1LCB
 LOW CONG. WATER SEMIVOLATILE ORGANICS ANALYSIS DATA SHEET
                                                      EPA SAMPLE NO.
  i Name:

Lab Code:
Lab Sample ID:

Lab File ID:

Sample Volume:
             Case No.:
Contract:

 SAS No.:
SDG No.:
Concentrated Extract Volume:

Injection Volume:  	 (uL)
                             .(uL)
                                       Date Received:

                                       Date Extracted:

                                       Date Analyzed:
         Dilution Factor:

         pH:
       CAS NO.
                COMPOUND
               CONCENTRATION
                  (ug/L)
                      -Phenol
111-44-4	bis (2-Chloroethyl) ether_
95-57-8-	2-Chlorophenol_
            	2 -Methy Iphenol'
            	2,:
106-44-5	4-Methy Iphenol
       95-48-7
       621-64-7	N-Nitroso-di-n-propylamine
       67-72-1—
       98-95-3—
          ——Nitrobenzene,
          	Isophorone	"
          	2-i
                       •2,4-DimethyIphenol
       111-91-1	
       120-83-2	2,4-Dichlorophenol	
       120-82-1	1,2,4-Trichlorobenzene
106-47-8-
87-68-3—
59-50-7—
91-57-6—
77-47-4—
88-06-2—
95-95-4—
91-58-7—

131-11-3-
208-96-8-
606-20-2-
99-09-2—
83-32-9—
                       4 -Chloroaniline
                     — Hexachlorobutadiene
                    	4-Chloro-3-methylphenol_
                       -2-Methylnaphthalene_
                   ——Hexachlorocyclopentadiene_
                   	2,4,6-Trichlorophenol	~_
                   	2,4,5-Trichlorophenol	
                   	2 -Ch 1 or onaphthalene
                   	2-Nitroaniline
                   •—Dimethylphthalate_
                      -Acenaphthylene
                    	2,6-Dinitrotoluene
                    	3-Nitroaniline	[
                    ——Acenaphthene	
                                FORM I LCSV-1
                                                                6/91

-------
                             1LCC
 LOW CONG. WATER SEMIVOLATILE ORGANICS ANALYSIS DATA  SHEET
                                         EPA SAMPLE NO.
"  b Name:
Lab Code:
Case No.:
Contract:
 SAS No.:
SDG No.:
Lab Sample ID:
Lab File ID:
Sample Volume:
                          Date Received:
                          Date Extracted:
                          Date Analyzed:
Concentrated Extract Volume:
Injection Volume:  	  (uL)
       CAS NO.
   COMPOUND
                          Dilution Factor:
                          PH:  	
               CONCENTRATION
                  (ug/L)

100-02-7—
132-64-9 —


	 4-Nitrophenol
	 Dibenzofuran
121-14-2 	 2 , 4-Dinitrotoluene
84-66-2 	
7005-72-3-
86-73-7 	
100-01-6 —
534-52-1 —
86-30-6—
101-55-3 —
118-74-1 —
87-86-5 	
85-01-8 	
120-12-7—
84-74-2 	
206-44-0 —
129-00-0 —
85-68-7 	
91-94-1 	
56-55-3 	
218-01-9 —
117-81-7 —
117-84-0 —
2Q5-99-2 —
207-08-9 —
50-32-8 	
193-39-5 —
53-70-3 — -
191-24-2 —
	 Diethylphthalate
	 -— 4 -Chlorophenyl-phenyiether
	 Fluorene
	 4-Nitroaniline
	 4 , 6-Dinitro-2-methylphenol
	 — N-Nitrosodipheny lamine ( 1 )
	 4-Bromophenyl-phenylether
	 Hexachlorobenzene
	 Pentachlorophenol
	 Phenanthrene
	 --Anthracene
	 Di-n-butylphthalate
	 Fluoranthene
	 Pyrene
	 Butylbenzylphthalate
	 3 , 3 ' -Dichlorobenzidine
	 — Benzo (a) anthracene
	 cnrysene
	 bis (2-Ethylhexyl) phthalate
	 D±-n-octylphthalate
——Benzo (b) f luoranthene
	 Benzo (Jc) f luoranthene
	 Benzo (a) pyrene
	 indeno (1,2,3 -cd) pyrene
	 Dibenz (a , h) anthracene
	 Benzo (g,h, i) perylene
























































	





     (1)  - Cannot be separated from Diphenylamine
                                FORM I LCSV-2
                                                                      6/91

-------
                             1LCD
   LOW CONC. WATER PESTICIDE ORGANICS ANALYSIS  DATA SHEET
                                                       EPA SAMPLE NO,
T '•> Name:

Lab Code:
             Case No.:
Contract:

 SAS No.:
SDG No.:
Lab Sample ID:

Sample Volume:
Concentrated Extract Volume:

Injection Volume: 	  (uL)

Sulfur Cleanup:  (Y/N) 	
                             .(uL)
         Date Received:

         Date Extracted:

         Date Analyzed:
                                       Dilution Factor:

                                       pH:
       CAS NO.
                 COMPOUND
               CONCENTRATION
                  (ug/L)
       319-85-7
       58-89-9—
       76-44-8-
       309-00-2—
       1024-57-3-
       959-98-8—
       60-57-1-
       72-55-9-
       33213-65-9
       1031-07-8
53494-70-5-
7421-36-3-
5103-71-9	
5103-74-2	
8001-35-2	
12674-11-2—
11104-28-2—
11141-16-5—
53469-21-9—
12672-29-6—
11097-69-1—
11096-82-5—
                beta-BHC
               —gamma-BHC (Lindane)
               —Heptachlor	'm
                -Aldrin
                -Heptachlor epoxo.de_
                -Endosulf an I	~_
                -Dieldrin	
                •4,4' -DDE	
                -Endrin       	
                Endosulf an II
                          :'-
              — Endosulfan sulf ate
                     —Endrin ketone
                       -Endrin aldehyde_
                      —alpha-Chlordane"
                      —gamma-Chlordane~
                      —Toxaphene
                       -Aroclor-1016
                      —Aroclor-1221"
                      —Aroclor-12 3 2"
                      —Aroclor-1242"
                      —Aroclor-1248^
                      —Aroclor-1254~
                      —Aroclor-12 6 o"
                                FORM  I  LCP
                                                                6/91

-------
                             1LCE
   LOW CONG. WATER VOLATILE ORGANICS ANALYSIS DATA SHEET
              TENTATIVELY IDENTIFIED COMPOUNDS
                                         EPA SAMPLE NO.
"  b Name:
Lab Code:
Lab Sample ID:
Lab File ID:
Purge Volume:
Case No.:
Contract:.
 SAS No.:
SDG No.:
                          Date Received:
                          Date Analyzed:
   (mL)
         Dilution Factor:
Number TICs found:
CAS NUMBER
1.
2.
3.
4.
5.
6.
7.
8.
9.
.0.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
21.
22.
23.
24.
25.
26.
27.
28.
29.
30.

COMPOUND NAME































RT






























EST. CONC.
(ug/L)































Q






























                                FORM I LCV-TIC
                                                  6/91

-------
                             1LCF
 LOW CONG. WATER SEMIVOLATILE ORGAHICS ANALYSIS DATA SHEET
               TENTATIVELY IDENTIFIED COMPOUNDS
                                         EPA SAMPLE NO.
  b Name:
Lab Code:
Case No.:
Lab Sample ID:
Lab File ID:
Sample Volume:
Concentrated Extract Volume:
Injection Volume:  	 (uL)
Contract:.
 SAS No.:
SDG No.:
                          Date Received:
                          Date Extracted:
                          Date Analyzed:
                          Dilution Factor:
                          pH:  	
Number TICs found:
CAS NUMBER
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
IS.
16.
17.
18.
19.
20.
21.
22.
23.
24.
25.
26.
27.
28.
29.
30.

COMPOUND NAME































RT






























EST. CONC.
(ug/L)











-



















Q






























                                 FORM I  LCSV-TIC
                                                   6/91

-------
                              2LCA
           LOW CONC. WATER VOLATILE SURROGATE RECOVERY
* b Name:

Lab Code:
Case No.:
Contract:

 SAS No.:
SDG No.
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
EPA
SAMPLE NO.






























BFB
%REC t





























OTHER





























TOT
OUT





























                   BFB = Bromofluorobenzene
                          QC LIMITS
                            %REC
                          (80-120)
                   # Column to be used to flag recovery values.
                   * Values outside of contract required QC limits.
                   D Surrogate diluted out.
page 	 of 	
                                FORM II LCV
                                                  6/91

-------
                             2LCB
          LOW CONG. WATER SEMIVOLATILE SURROGATE RECOVERY
  b Name:

Lab Code:
Case No.:
Contract:

 SAS No.:
SDG NO.

01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
EPA
SAMPLE NO.






























NBZ
%REC #






























FBP
%REC #






























TPH
%REC t






























PEL
%REC #






























2FP
%REC f






























TBP
%REC #






























OTHER






























TOT
OUT






























       NBZ » Nitrobenzene-dS
       FBP = 2-Fluorobiphenyl
       TPH » Terphenyl-dl4
       PHL = Phenol-d5
       2FP = 2-Fluorophenol
       TBP = 2,4,6-Tribromophenol
                QC LIMITS
                  %REC
                (40-112)
                (42-110)
                (24-140)
                (17-113)
                (16-108)
                (18-126)
       # Column to be used to flag recovery values.
       * Values outside of contract required.QC limits.
       D Surrogate diluted out.
page 	 of 	
                                FORM II LCSV
                                                   6/91

-------
                              2LCC
            LOW CONG.  WATER PESTICIDE SURROGATE RECOVERY
* b Name:

Lab Code:
GC Column(1):
   Contract:_

    SAS No.:
SDG No.:
(mm)   GC Column(2):
         ID:
(mm

01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
EPA
SAMPLE NO.






























TCX(l)
%REC t






























TCX(2)
%REC f






























DCB(l)
%REC #






























DCS (2)
%REC #






























OTHER
(1)






























OTHER
(2)






























TOT
OUT






























          TCX «• Tetrachloro-m-xylene
          DCS - Decachlorobiphenyl
    QC LIMITS
      %REC
    (60-150)
    (60-150)
          # Column to be used to flag recovery values.
          * Values outside of contract required QC limits,
          D Surrogate diluted out.
page 	 of 	
                                FORM II LCP
                                    6/91

-------
                             3LCA
   LOW CONG. WATER VOLATILE LAB CONTROL SAMPLE RECOVERY
                                          EPA SAMPLE NO.
T 'i Name:_
Lab Code:
Lab Sample ID:
Lab File ID:
Purge Volume:
LCS Aliquot:
Case No.:
 (uL)
Contract:
 SAS No.:
SDG No.:
                          LCS Lot No.:
                          Date Analyzed:
                          Dilution Factor:
COMPOUND
Vinyl chloride
1 , 2-Dichloroethane
Carbon tetrachloride
1 , 2-Dichloropropane
Trichloroethene
1,1, 2-Trichloroethane
Benzene
cis-1, 3-Dichloropropene
Bromoform
Tetrachloroethene
1, 2-Dibromoethane
1 , 4-Dichlorobenzene

AMOUNT
ADDED
(ng)













AMOUNT
RECOVERED
(ng)













%REC t












QC
LIMITS












   # Column to be used to flag LCS recovery with an asterisk.
   * Values outside of QC limits.
   LCS Recovery:
   outside limits out of
               total.
COMMENTS:
                                FORM III LCV
                                                   6/91

-------
                             3LCB
 LOW CONG. WATER SEMTVOLATILE LAB CONTROL SAMPLE RECOVERY
                                         EPA SAMPLE NO.
T~b Name:
Lab Code:
Lab Sample ID:
Lab File ID:
LCS Aliquot:
Case No.:
  (UL)
Contract:_
 SAS No.:
SDG No.:
Concentrated Extract Volume:
Injection Volume:  	 (uL)
                .(uL)
                          LCS Lot No.:
         Date Extracted:
         Date Analyzed:
         Dilution Factor:
         PH:  	
COMPOUND
Phenol
bis (2-Chloroethyl) ether
2 -Chlorophenol
N-Nitroso-di-n-propylamine
Hexachloroethane
Isophorone
1,2, 4-Trichlorbbenzene
Naphthalene
4 -Chlor oaniline
2,4, 6-Trichlorophenol
2 , 4-Dinitrotoluene
Diethvlphthalate
N-Nitrosodiphenylamine
Hexachlorobenzene
Benzo (a) pyrene

AMOUNT
ADDED
(ng)
















AMOUNT
RECOVERED
(ng)
















%REC #















QC
LIMITS















    # Column to be used to flag LCS recovery with an asterisk.
    * Values outside of QC limits.
    LCS Recovery:
     outside limits out of
                 total.
COMMENTS:
                                FORM III LCSV
                                                  6/91

-------
                             3LCC
   LOW CONG. WATER PESTICIDE LAB CONTROL SAMPLE RECOVERY
                                          EPA SAMPLE NO.
T b Name:
Lab Code:
Case No.:
Lab Sample ID:
LCS Aliquot:
  (uL)
Concentrated Extract Volume:
Injection Volume: 	 (uL)
Sulfur Cleanup:  (Y/N)
Instrument ID(1)
Instrument ID(2) :
Contract:
 SAS No.:
SDG No
                          LCS Lot No.:
         Date Extracted:
         Date Analyzed:
                          Dilution Factor:
                          pH:  	
                 GC Column(1):
                         ID:
                (mm)
COMPOUND
gamma -BHC (Lindane)
Heptachlor epoxide
Dieldrin
4, 4 '-DDE
Endrin
Endosulf an sulf ate
gamma-Chlordane

AMOUNT
ADDED
(ng)








AMOUNT
RECOVERED
(ng)








%REC f







QC
LIMITS







                 GC Column(2):
                         ID:
               (mm)
COMPOUND
gamma-BHC (Lindane)
Heptachlor epoxide
Dieldrin
4. 4 '-DDE
Endrin
Endosulf an sulf ate
gamma-Chlordane

AMOUNT
ADDED
(ng)








AMOUNT
RECOVERED
(ng)








%REC f







QC
LIMITS







  # Column to be used to flag recovery values with  an  asterisk.
  * Values outside of QC limits.
  ~.CS Recovery:	 outside limits out of         total.
COMMENTS:
                                FORM III LCP
                                                   6/91

-------
                             4LCA
       LOW CONG. WATER VOLATILE METHOD BLANK SUMMARY
                                                             EPA  SAMPLE  NO.
T > Name:
Lab Code:
Case No.:
Contract:
 SAS No.:
SDG No.:
Lab Sample ID:
Lab File ID:
Instrument ID:
                          Date Analyzed:
                          Time Analyzed:
         THIS METHOD BLANK APPLIES TO THE FOLLOWING SAMPLES AND LCS:
COMMENTS:
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
EPA
SAMPLE NO.






























LAB
SAMPLE ID





























LAB
FILE ID





























TIME
ANALYZED






























page 	 of 	
                                FORM IV LCV
                                                    6/91

-------
                             4LCB
     LOW CONG. WATER SEMIVOLATILE METHOD BLANK SUMMARY
                                         EPA SAMPLE NO.
7 '•> Name:
Lab Code:
Case No.:
Contract:
 SAS No.:
SOG No.:
Lab Sample ID:
Lab File ID:
Instrument ID:
                          Date Extracted:
                          Date Analyzed:
                          Time Analyzed:
         THIS METHOD BLANK APPLIES TO THE FOLLOWING SAMPLES AND LCS:
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
EPA
SAMPLE NO.






























LAB
SAMPLE ID






























LAB
FILE ID






























DATE
ANALYZED






























COMMENTS:
page 	 of 	
                                FORM IV LCSV
                                                  6/91

-------
                              4LCC
      LOW CONG. WATER PESTICIDE METHOD BLANK SUMMARY
                                         EPA SAMPLE  NO.
7 *•> Name:
Lab Code:
Case No.:
   Contract:
    SAS No.:
                SDG No. :
Date Extracted:
                          Lab Sample ID:
Date Analyzed  (1):
Time Analyzed  (1):
Instrument ID  (1):
GC Column  (l): 	
      ID:
(mm)
      Date Analyzed  (2): 	
      Time Analyzed  (2): 	
      Instrument ID  (2): 	
GC Column (2): 	 ID:
(mm)
Sulfur Cleanup:  (Y/N) 	
            THIS METHOD  BLANK APPLIES TO THE FOLLOWING SAMPLES AND LCS:
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
EPA
SAMPLE NO.


























LAB
SAMPLE ID


























DATE
ANALYZED 1


























DATE
ANALYZED 2


























    COMMENTS:
page 	 of 	
                                FORM IV LCP
                                                  6/91

-------
                             5LCA
       LOW CONC. WATER VOLATILE ORGANIC GC/MS TONING AND MASS
               CALIBRATION - BROMOFLUOROBENZENE  (BFB)
T *i Name:
Lab Code:
Lab File ID:
Instrument ID:
GC Column:
Case No.
  ID:
(am)
      Contract:.
       SAS No.:
SDG No.:
                       BFB Injection Date:
                       BFB Injection Tine:
m/e
50
75
95
96
173
174
175
176
177
ION ABUNDANCE CRITERIA
8.0 - 40.0% of mass 95
30.0 - 66.0% of mass 95
Base peak, 100% relative abundance
5.0 - 9.0% of mass 95
Less than 2.0% of mass i?4
50.0 - 120.0% of mass 95
4.0 - 9.0 % of mass 174
93.0 - 101.0% of mass 174
5.0 - 9.0% of mass 176

% RELATIVE
ABUNDANCE




( )1

( >1
( )1
( )2

        1-Value is % mass 174
                          2-Value is % mass 176
      THIS TUNE APPLIES TO THE FOLLOWING SAMPLES, LCS, BLANKS, AND  STANDARDS:
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
EPA
SAMPLE NO.






















LAB
SAMPLE ID






















LAB
FILE ID






















DATE
ANALYZED






















TIME
ANALYZED






















page
        of
                                FORM V LCV
                                                   6/91

-------
                             5LCB
    LOW CONC. WATER SEMIVOLATILE ORGANIC GC/MS TUNING AND MASS
        CALIBRATION - DECAFLUOROTRIPHENYLPHOSPHINE  (DFTPP)
T h Name:_

Lab Code:
Case No.:
Contract:

 SAS No.:
SDG No.:
Lab File ID:

Instrument ID:
                     DFTPP Injection Date:

                     DFTPP Injection Time:
m/e
51
68
69
70
127
197
198
199
275
365
441
442
443
ION ABUNDANCE CRITERIA
30.0 - 80.0% of mass 198
Less than 2.0% of mass 69
Mass 69 relative abundance
Less than 2.0% of mass 69
25.0 - 75.0% of mass 198
Less than 1.0% of mass 198
Base Peak, 100% relative abundance
5.0 to 9.0% of mass 198
10.0 - 30.0% of mass 198
Greater than 0.75% of mass 198
Present, but less than mass 443
40.0 - 110.0% of mass 198
15.0 - 24.0% of mass 442

% RELATIVE
ABUNDANCE

( )1

( )1








( )2

        1-Value is % mass 69
                          2-Value is % mass 442
      THIS TUNE APPLIES TO THE FOLLOWING SAMPLES, LCS, BLANKS, AND STANDARDS:
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
EPA
SAMPLE NO.






















LAB
SAMPLE ID






















LAB
FILE ID






















DATE
ANALYZED






















TIME
ANALYZED






















page 	 of 	
            FORM V LCSV
                                6/91

-------
                             6LCA
   LOW CONG. WATER VOLATILE ORGANICS INITIAL CALIBRATION  SUMMARY

Lab Name:	   Contract:	

^ .o Code:    '	  Case No.: 	  SAS No.: 	  SDG No.:

Instrument ID:  	  Calibration Date(s) :	    	
LAB FILE ID: RRF1 -
RRF5 » RRF10-

COMPOUND
Chloromethane
Bromomethane '
Vinyl chloride <
Chloroethane
Methylene chloride
Acetone
Carbon disulfide
1,1-Dichloroethene i
1 , 1-Dichloroethane *
cis-1, 2-Dichloroethene
trans-1 , 2-Dichloroethene
Chloroform *
1 , 2-Dichloroethane i
2-Butanone
nromochloromethane i
1 , 1-Trichloroethane i
carbon tetrachloride 3
Bromodichloromethane '
1 , 2-Dichloropropane
cis-1 , 3 -Dichloropropene *
Trichloroethene <
Dibromochloromethane '
1,1, 2-Trichloroethane '
Benzene i
trans- l , 3 -D ichlor opropene <
Bromoform i
4 -Methy 1-2 -pentanone
2-Hexanone
Tetrachloroethene ^
1,1,2,2 -Tetr achlor oethane '
1 , 2 -Dibr omoethane ^
Toluene '
Chlorobenzene '
Ethylbenzene :
Styrene '
Xylenes (total) '
1 , 3-Dichlorobenzene '
1 , 4-Dichlorobenzene '
1,2-Dichlorobenzene '
1, 2-Dibromo-3-chloropropane__



RRF1

k
k




k
k


k
k

k
k
k
k

k
k
k
k
k
k
k


k
k
k
k
k
k
k
k
k
k
k




RRF2








































RRF:
RRF:

RRF5








































i -
25-

RRF10











































RRF25











































RRF








































                                                                          RSD
-romofluorobenzene *
1










* Compounds with required minimum RRF and maximum %RSD values.
  All other compounds must meet a minimum RRF of 0.010,

                              FORM VI LCV
6/91

-------
                             6LCB
 LOW CONG. WATER SEMIVOLATILE ORGANICS INITIAL CALIBRATION  SUMMARY
  •> Name:
Lab Code:
Case No.:
Contract:
 SAS No.:
SDG No.:
Instrument ID:
       Calibration Date(s):
       Calibration Times:
LAB FILE ID: RRF5 -
RRF20- RRF50-

COMPODND
Phenol
bis ( 2-Chloroethyl) ether
2 -Chlorophenol
2 -Methy Iphenol
2,2' -oxybis ( 1 -Chlor opropane)
4 -Methy Iphenol
N-Nitroso-di-n-propylamine
Hexachloroethane
Nitrobenzene
Isophorone
"• -Nitrophenol
, 4-Dimethy Iphenol
bis (2-Chloroethoxy) methane
2 , 4-Dichlorophenol
1,2, 4-Trichlorobenzene
Naphthalene
4 -Chlor oaniline
Hexachlorobutadiene
4 -Chloro-3 -methy Iphenol '
2-Methylnaphthalene '
Hexachlorocyclopentadiene
2,4, 6-Trichlorophenol '
2,4, 5-Trichlorophenol '
2 -Chloronaphthalene
2 -Nitr oaniline
Dimethylphthalate
Acenaphthylene <
2 , 6-Dinitrotoluene '
3 -Nitroaniline
Acenaphthene *
2 , 4-Dinitrophenol
4 -Nitrophenol
Dibenzofuran *
2 , 4 -D ini tr ot o luene i




RRF5


















k
k

k
k



k
k

t


k
k




RRF10



































RRF:
RRFl

RRF20



































L0=
30=

RRF50






































RRF80






































RRF






































RSD



































   'ompounds with required minimum RRF and maximum %RSD values.
  All other compounds must meet a minimum RRF of 0.010.
                                FORM VI LCSV-1
                                                  6/91

-------
                             6LCC
 LOW CONG. WATER SEMIVOLATILE ORGANICS INITIAL CALIBRATION SUMMARY
T "•» Name:
Lab Code:
Instrument ID:
	   Contract:_
 Case  No.: 	  SAS  No.:
	  Calibration Date(s):
        Calibration Times:
SD6 No.:
LAB FILE ID: RRF5 *
RRF20* RRF50*

COMPOUND
Diethylphthalate
4-Chlorophenyl-phenylether <
Fluorene *
4-Nitroaniline
4 , 6-Dinitro-2-methylphenol
N-Nitrosodiphenylamine (1)
4-Bromophenyl-phenylether *
Hexachlorobenzene '
Pentachlorophenol *
Phenanthrene 5
Anthracene <
-n-butylphthalate
Fluoranthene '
Pyrene *
Butylbenzylphthalate
3,3' -Dichlorobenzidiiie
Benzo ( a) anthracene •>
Chrysene 1
bis (2-Ethylhexyl) phthalate
Di-n-octvlphthalate
Benzo (b) f luoranthene
Benzo (k) f luoranthene
Benzo (a) pyrene
Indeno (1,2,3 -cd) pyrene
Dibenz ( a , h) anthracene
Benzo ( g , h , i ) pery lene
Nitrobenzene-d5
2 -Fluor obiphenyl
Terpheny 1-dl 4
Phenol-dS '
2-Fluorophenol '
2,4, 6-Tribromopheribi




RRF5

*
k



»
k
k
k
k

k
k


k
k











k
k





RRF10

































RRF]
RRFi

RRF20

































LO-
JO*

RRF50




































RRF80




































RRF




































%
RSD

:
T



T
:
•:
-
-

r
7


f
•Sc


4
4
•i
i
•i
•i

y
4
r
T


 (1) Cannot be separated from Diphenylamine
 * Compounds with required minimum RRF  and maximum %RSD values.
   11 other compounds must meet  a minimum RRF  of  0.010.
                                 FORM VI LCSV-2
                                                   6/91

-------
                             6LCD
LOW CONG. WATER PESTICIDE INITIAL CALIBRATION OF SINGLE COMPONENT ANALYTES
7 "> Name:

Lab Code:
Case No.:
Contract:

 SAS No.:
SDG No.:
Instrument ID:

GC Column:
 	  Level (x low): low 	 mid

  ID: 	(mm)   Date(s) Analyzed:
                         high
COMPOUND
alpha-BHC
beta-BHC
delta-BHC
gamma-BHC (Lindane)
Heptachlor
Aldrin
Heptachlor epoxide
Endosulfan I
Dieldrin
4, 4 '-DDE
Endrin
Endosulfan II
4,4'-DDD
Endosulfan sulfate
4,4'-DDT
Hethoxychlor
Endrin ketone
Endrin aldehyde
alpha-Chlordane
gamma -Chlordane
Tetrachloro-m-xylene
Decachlorobiphenyl 	
RT 0]
LOW












— : 	





**


? STANDS
MID



















aossa-s


*RDS
HIGH



















=3=


MEAN
RT



















=====


RT W]
FROM






















CNDOW
TO



















:


     * Surrogate retention times are measured from Ind. Mix A analyses.

     Retention time windows are ±0.05 minutes for all compounds that
     elute before Heptachlor epoxide, ±0.07 minutes for all other
     compounds, except ±0.10 minutes for Decachlorobiphenyl.
                                FORM VI LCP-1
                                                  6/91

-------
                             6LCE
LOW CONC. WATER PESTICIDE INITIAL CALIBRATION OF SINGLE COMPONENT ANALYTES
T  •> Name:
Lab Code:
Instrument ID:
GC Column:
Case No.:
Contract:
 SAS No.:
SDG No.:
 	  Level (x low): low 	 mid
  ID: 	(mm)   Date(s) Analyzed:
                         high
COMPOUND
alpha-BHC
beta-BHC
delta-BHC
gamma-BHC (Lindane)
Heptachlor
Aldrin
Heptachlor epoxide
Endosulf an I
Dieldrin
4. 4 '-DDE
Endrin
Endosulf an II
.4/-DDD
Endosulf an sulf ate
4. 4 '-DDT
Methoxychlor
Endrin ketone
Endrin aldehyde
alpha-Chlordane
gamma-Chlordane
Tetrachloro-m-xylene
Decachlorobiphenyl

LOW























CALIBRATIC
MID























>N FACTORS
HIGH























MEAN























%RSD






















* Surrogate calibration factors are measured from Ind. Mix A analyses.
%RSD must be less than or equal to 20.0% for all compounds,  except the
surrogates, where %RSD must be less than or equal to 30.0%.   Up to two
target compounds, but not surrogates, may have %RSD greater  than 20.0%,
but less than  or equal to 30.0%.
                                 FORM VI  LCP-2
                                                   6/91

-------
                             6LCF
LOW CONG. WATER PESTICIDE INITIAL CALIBRATION OF MULTICOMPONENT ANALYTES
T > Name:
Lab Code:
Instrument ID:
GC Column:
Contract:
Case No.: SAS No.: SDG No.:
Date(s) Analyzed:
ID: (mm)
COMPOUND
Toxaphene
Aroclor 1016
Aroclor 1221
Aroclor 1232
Aroclor 1242
Aroclor 1248
Aroclor 1254
Aroclor 1260
AMOUNT
(ng)
















PEAK
*1
*2
*3
4
5
*1
*2
*3
4
5
*1
*2
*3
4
5
*1
*2
*3
4
5
*1
*2
*3
4
5
*1
*2
*3
4
5
*1
*2
*3
4
5
*1
*2
*3
4
5
RT








































RT w:
FROM








































CNDOW
TO








































CALIBRATION
FACTOR








































      * Denotes required peaks
                                FORM VI LCP-3
6/91

-------
                              6LC6
         LOW CONG. WATER PESTICIDE RESOLUTION CHECK SUMMARY
"  •> Name:
Lab Code:
Case No.:
   Contract:
    SAS No.:
SDG No.
GC Column (1):
      ID:
EPA Sample No. (Standard 1):
Date Analyzed (1): 	
GC Column (2):
      ID:
EPA Sample No. (Standard 2):
Date Analyzed (2): 	
 (mm)  Instrument  ID  (1):
	 Lab  Sample  ID  (1):
      Time Analyzed  (1):
01
02
03
04
05
06
07
08
09
ANALYTE









RT








RESOLUTION
(%)









 (mm)  Instrument  ID (2):
	 Lab  Sample  ID (2):
      Time Analyzed (2):
01
02
03
04
05
06
07
08
09
ANALYTE









RT








RESOLUTION
(%)









  Resolution of two adjacent peaks must be calculated as a percentage of the
  height of the smaller peak,  and must be greater than or equal to 60.0%.
                                 FORM VI LCP-4
                                                  6/91

-------
                             7LCA
 LOW CONG. WATER VOLATILE ORGANICS CONTINUING CALIBRATION  SUMMARY
Lab Name:
..—o Code:
Case No.:
Contract:
 SAS No.:
Instrument ID:
Lab File ID:
        Calibration Date:
        Init. Calib. Date(s) :.
SDG No.:
 Time:
      All other compounds must meet a minimum RRF of 0.010.
                                FORM VII LCV
COMPOUND
Chloromethane
Bromomethane
Vinyl chloride
Chloroethane
Methylene chloride
Acetone
Carbon disulfide
1 , 1-Dichloroethene
1 , l-Dichloroethane
cis-1 , 2-Dichloroethene
trans -1 , 2-Dichloroethene
Chloroform
1 , 2-Dichloroethane
2-Butanone
Bromochloromethane
1, 1, 1-Trichloroethane
Carbon tetrachloride
Bromodi Chloromethane
1 , 2-Dichloropropane
cis-1 , 3-Dichloropropene
Tr ichlor oethene
Dibromochloromethane
1,1, 2 -Tr ichlor oethane
Benzene
trans-l , 3-Dichloropropene
Bromoform
4 -Methy 1-2 -pentanone
2-Hexanone
Tetrachloroethene
1,1,2, 2-Tetrachloroethane
1 , 2-Dibromoethane
Toluene
Chlorobenzene
Ethy Ibenz ene
Styrene
Xylenes (total)
1 , 3-Dichlorobenzene
1, 4-Dichlorobenzene
1 , 2-Dichlorobenzene
1 , 2-Dibromo-3-chloroprdpane
Bromofluorobenzene

RRF










































RRF5








































— =

MIN
RRF

0.100
0.100




0.100
0.200
0.100

0.200
0.100

0.050
0.100
0.100
0.200

0.200
0.300
0.100
0.100
0.500
0.100
0.050


0.200
0.100
0.100
0.400
0.500
0.100
0.300
0.300
0.600
0.500
0.400

0.200

%D








































— — "

MAX
%D

30.0
30.0




30.0
30.0


30.0
30.0

30.0
30.0
30.0
30.0

30.0
30.0
30.0
30.0
30.0
30.0
30.0


30.0
30.0
30.0
30.0
30.0
30.0
30.0
30.0
30.0
30.0
30.0

30.0

                                                  6/91

-------
                             7LCB
LOW CONC. WATER SEMIVOLATILE ORGANICS CONTINUING CALIBRATION SUMMARY
"  '•> Name:
Lab Code:
Case No.:
Contract:
 SAS No.:
Instrument ID:
Lab File ID:
        Calibration Date:
        Init. Calib. Date(s).\
        Init. Calib. Times:
SDG No.:
 Time:
COMPOUND
Phenol
bis (2-Chloroethyl) ether
2 -Chlor ophenol
2 -Methy Iphenol
2,2' -oxybis ( l-Chloropropane)
4 -Methy Iphenol
N-Nitroso-di-n-propy'Ia^aine
Hexachloroethane
Nitrobenzene
Isophorone
2 -Nitrophenol
2 , 4 -Dimethy Iphenol
bis ( 2 -Chlor oethoxy ) methane
2 , 4 -Dichlor ophenol
1,2, 4-Trichlorobenzene
Naphthalene
4-Chloroaniline
Hexachlorobutadiene
4 -Chlor o-3 -methy Iphenol
2 -Methy Inaphthalene
Hexachlorocyclopentadlene
2,4, 6-Trichlorophenol
2,4, 5-Trichlorophenol
2 -Chloronaphthalene
2-Nitroaniline
Dimethy Iphthalate
Acenaphthylene
2 , 6-Dinitrotoluene
3 -Nitr oaniline
Acenaphthene
2 , 4-Dinitrophenol
4 -Nitrophenol
Dibenzofuran
2 , 4-Dinitrotoluene

RRF



































RRF20



































MIN
RRF
0.800
0.700
0.700
0.700

0.600
0.500
0.300
0.200
0.400
0.100
0.200
0.300
0.200
0.200
0.700


0.200
0.400

0.200
0.200
0.800


1.300
0.200

0.800


0.800
0.200

%D



































MAX
%D
25.0
25.0
25.0
25.0

25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0


25.0
25.0

25.0
25.0
25.0


25.0
25.0

25.0


25.0
25.0

      All other  compounds must meet  a minumum RRF of 0.010.
                                 FORM VII  LCSV-1
                                                   6/91

-------
                             7LCC
LOW CONG. WATER SEMIVOLATILE ORGANICS CONTINUING CALIBRATION  SUMMARY
T ^ Name:.
Lab Code:
Case No.:
Contract:
 SAS No.:
Instrument ID:
Lab File 10:
        Calibration Date:
        Init. Calib. Date(s) :
        Init. Calib. Tines:
SDG No.:
 Time:
COMPOUND
Diethylphthalate
4-Chlorophenyl-phenylether
Fluorene
4-Nitroaniline
4 , 6-Dinitro-2-methylphenol
N-Nitrosodipheny lamine ( 1 }
4 -Bromopheny 1-pheny lether
Hexachlorobenzene
Pentachlorophenol
Phenanthrene
Anthracene
Di-n-butylphthalate
F luor anthene
Pyrene
Butylbenzylphthalate
3,3' -Dichlorobenzidine
Benzo (a) anthracene
Chrysene
bis (2-Ethylhexyl) phthalate
Di-n-octylphthalate
Benzo (b) f luor anthene
Benzo (k) f luor anthene
Benzo ( a) pyrene
Indeno (1,2,3 -cd) pyrene
Dibenz ( a , h) anthracene
Benzo (g , h , i ) perylene
Nitrobenzene~d5
2 -Fluor obipheny 1
Terphenyl-dl4
Phenol-d5
Fluorophenol
2,4, 6-Tribromophenol

RRF

































RRF20

































MIN
RRF

0.400
0.900



0.100
0.100
0.050
0.700
0.700

0.600
0.600


0.800
0.700


0.700
0.700
0.700
0.500
0.400
0.500
0.010
0.700
0.500
0.800
0.600


%D

































MAX
%D

25.0
25.0



25.0
25.0
25.0
25.0
25.0

25.0
25.0


25.0
25.0


25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0
25.0


    (1) Cannot be separated from Diphenylamine
      All other compounds must meet a minimum RRF of 0.010.
                                FORM VII LCSV-2
                                                  6/91

-------
                             7LCD
  LOW CONC. WATER PESTICIDE CALIBRATION VERIFICATION SUMMARY
' b Name:_
Lab Code:
GC Column:
Contract:
 SAS No.:
Case No.: 	  SAS No.: 	  SDG No.:
  ID: 	(mm) Init. Calib. Date(s):	
EPA Sample No.(PIBLK):
Lab Sample ID (PIBLK) :.
EPA Sample No.(PEM): _
Lab Sample ID (PEM):
         Date Analyzed
         Time Analyzed
         Date Analyzed
         Time Analyzed
PEM
COMPOUND
alpha-BHC
beta-BHC
gamma-BHC (Lindane)
Endrin
4, 4 '-DDT
Methoxychlor

RT






RT W]
FROM






ENDOW
TO






CALC
AMOUNT
(ng)






NOM
AMOUNT
(ng)






%D






4,4'-DDT % breakdown  (1):
Combined % breakdown  (1):
    Endrin % breakdown  (1):
QC LIMITS:
     Absolute values of %D of amounts in PEM must be less than or equal to
     25.0%
     4,4'-DDT breakdown must be less than or equal to 20.0%
     Endrin breakdown must be less than or equal to 20.0%
     Combined breakdown must be less than or equal to 30.0%
                                 FORM VII  LCP-1
                                  6/91

-------
                             7LCE
  LOW CONC. WATER PESTICIDE CALIBRATION VERIFICATION SUMMARY
   ^ Name:_
Lab Code:
GC Column:
                       Contract:
                        SAS No.:
Case No.: 	  SAS No.: 	  SDG No.:
  ID: 	(mm) Init. Calib. Date(s):
EPA Sample No.(PIBLK):
Lab Sample ID (PIBLK):
EPA Sample No.(INDA):
Lab Sample ID (INDA):
                                Date Analyzed :_
                                Time Analyzed :
                                Date Analyzed :.
                                Time Analyzed :
INDIVIDUAL MIX A
COMPOUND
alpha-BHC
gamma-BHC (Lindane)
Heptachlor
Endosulf an I
Dieldrin
Endrin
4. 4 '-ODD
4. 4 '-DDT
iethoxychlor
Tetrachloro-m-xylene
Decachlorobiphenyl

RT











RT W]
FROM











ENDOW
TO











CALC
AMOUNT
(ng)











NOM
AMOUNT
(ng)












%D











EPA Sample No.(INDB):
Lab Sample ID  (INDB):
                                Date Analyzed
                                Time Analyzed
INDIVIDUAL MIX B
COMPOUND
beta-BHC
delta-BHC
Aldrin
Heptachlor epoxide
4. 4 '-DDE
Endosulfan II
Endosulf an sulfate
Endrin ketone
Enrin aldehyde -
alpha-Chlordane
gamma-Chlorodane
Tetrachloro-m-xylene
Decachlorobiphenyl

RT













RT W]
FROM













ENDOW
TO













CALC
AMOUNT
(ng)














NOM
AMOUNT
(ng)














%D













  QC LIMITS:
Absolute value of %D of amounts in the Individual Mixes must b
less than or equal to 25.0%.
                                 FORM VTI LCP-2
                                                        6/91

-------
                             8LCA
   LOW CONG. WATER VOLATILE INTERNAL STANDARD AREA AND  RT SUMMARY
* '•) Name:

Lab Code:
Case No.:
Contract:

 SA5 No.:
SDG No.
Lab File ID (Standard):

Instrument ID:  	

GC Column:            ID:
                            Date Analyzed:

                            Time Analyzed:
           (mm)
 01
 02
 03
 04
 07
 08
 09
 10
 11
 12
 13
 14
 15
 16
 17
 18
 19
 20
 21
 22

12 HOUR STD
UPPER LIMIT
LOWER LIMIT
EPA SAMPLE
NO.






















ISl(CBZ)
AREA t


























RT #


























IS2 (DFB)
AREA #


























RT #


























IS3 (DCB)
AREA #


























RT #


























   IS1 (CBZ) — Chlor obenz ene-d5
   IS2 (DFB) = 1,4-Difluorobenzene
   IS3 (DCB) = l,4-Dichlorobenzene-d4

   AREA UPPER LIMIT - +40% of internal standard area.
   AREA LOWER LIMIT = -40% of internal standard area.
   RT UPPER LIMIT - +0.33 minutes of internal standard RT.
   RT LOWER LIMIT = -0.33 minutes of internal standard RT.

   # Column used to flag internal standard area and RT values with an asteris
   * Values outside of QC limits.
page 	 of 	
                                 FORM VIII LCV
                                                    6/91

-------
                             8LCB
LOW CONC. WATER SEMIVOIATILE INTERNAL STANDARD AREA AND RT SUMMARY
  b Name:

Lab Code:
Case No.:
Contract:

 SAS No.:
                                    SDG No.
Lab File ID (Standard):

Instrument ID:
                            Date Analyzed:

                            Time Analyzed:





01
02
03
04
05
^6
7
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22

12 HOUR STD
UPPER LIMIT
LOWER LIMIT
EPA SAMPLE
NO.






















ISl(DCB)
AREA t


























RT #


























IS2 (NPT)
AREA f


























RT #


























IS3 (ANT)
AREA f


























RT #


























   IS1  (DCS) »  l,4-Dichlorobenzene-d4
   IS2  (NPT) =  Naphthalene-d8
   IS3  (ANT) »  Acenaphthene-dlO

   AREA UPPER LIMIT = +100% of internal  standard area.
   AREA LOWER LIMIT - -50% of internal standard  area.
   RT UPPER LIMIT = +0.33 minutes  of internal  standard  RT.
   RT LOWER LIMIT = -0.33 minutes  of internal  standard  RT.

   # Column used to flag internal  standard area  and RT  values with an asteris]
   * Values outside of QC limits.
page 	 of 	
                                 FORM VIII  LCSV-1
                                                   6/91

-------
                             8LCC
LOW CONG. WATER SEMIVOLATILE INTERNAL STANDARD AREA AND RT  SUMMARY
'  "3 Name:

Lab Code:
     Case No.:
Contract:

 SAS No.:
SDG No.
Lab File ID (Standard):

Instrument ID:  	
                                 Date Analyzed:

                                 Time Analyzed:

12 HOUR STD
UPPER LIMIT
LOWER LIMIT
EPA SAMPLE
NO.






















IS4 (PHN)
AREA f
.

























RT #


























ISS(CRY)
AREA #


























RT #


























IS6(PRY)
AREA #


























RT #


























 01
 02
 03
 04
 05
 "6
  7
 08
 09
 10
 11
 12
 13
 14
 15
 16
 17
 18
 19
 20
 21
 22
   IS4 (PHN)
   IS5 (CRY)
   IS6 (PRY)
Phenanthrene-dl0
Chrysene-dl2
Perylene-dl2
   AREA UPPER LIMIT = +100% of internal standard area.
   AREA LOWER LIMIT = -50% of internal standard area.
   RT UPPER LIMIT = +0.33 minutes of internal standard RT.
   RT LOWER LIMIT = -0.33 minutes of internal standard RT.

   # Column used to flag internal standard area and RT values with an aster is
   * Values outisde of QC limits.
page 	 of
                                FORM VIII LCSV-2
                                                        6/91

-------
Lab Name:_

- .o Code:

GC Column:
                  8LCD
 LOW CONG.  WATER PESTICIDE ANALYTICAL SEQUENCE

	   Contract:	

                           SAS No.:           SDG No.:
                     Case No.:  	           	

                    __ ID:  	(mm)  Init.  Calib.  Date(s):
Instrument ID:
  THE ANALYTICAL  SEQUENCE OF PERFORMANCE EVALUATION MIXTURES,  BLANKS,
               SAMPLES,  AND STANDARDS IS GIVEN BELOW:
      01
      02
      03
      04
      05
      06
      07
      08
      09
      10
      11
      12
      13
      14
      15
      16
      17
      18
      19
      20
      21
      22
      23
      24
      25
      26
      27
      28
      29
      30
      31
      32
MEAN SURRO<
TCX:

EPA
SAMPLE NO.
































3ATE RT FROM :
DCS:

LAB
SAMPLE ID
































CNITIAL CAL:

DATE
ANALYZED
































[BRATION

TIME
ANALYZED


































TCX
RT #


































DCB
RT #
































        TCX = Tetrachloro-m-xylene
        DCB = Decachlorobiphenyl
                                        QC LIMITS
                                     (± 0.05 MINUTES)
                                     (± 0.10 MINUTES)
        # Column used to flag retention time values with an asterisk.
        * Values outside of QC limits.
page 	 of 	
                                FORM VIII LCP
                                                                      6/91

-------
                             9LCA
        LOW CONC. WATER PESTICIDE FLORISIL CARTRIDGE CHECK
Lab Name:
	o Code:
Case No.:
Contract:

 SAS No.:
SDG No.:
Florisil Cartridge Lot Number:

GC Column(l) : 	 ID:
                      Date Analyzed:
              (mm)  GC Column(2):
                            ID:
                   (mm
COMPOUND
alpha-BHC
gamma-BHC
Heptachlor
Endosulfan I
Dieldrin
Endrin
4,4' -ODD
4,4'-DDT
Methoxychlor
Tetrachloro-m-xylene
Decachlorobiphenyl

SPIKE
ADDED
(ng)












SPIKE
RECOVERED
(ng)











%
REC t











QC
LIMITS
80-120
80-120
80-120
80-120
80-120
80-120
80-120
80-120
80-120
80-120
80-120
     f Column to be used to flag recovery with an asterisk
     * Values outside of QC limits

  THIS CARTRIDGE LOT APPLIES TO THE FOLLOWING SAMPLES, BLANKS, AND LCS:
            01
            02
            03
            04
            05
            06
            07
            08
            09
            10
            11
            12
            13
            14
            15
            16
            17
            18
            19
            20
            21
            22
            23
EPA
SAMPLE NO.























LAB
SAMPLE ID
"






















DATE
ANALYZED 1























DATE
ANALYZED 2























page 	 of 	
                                FORM IX LCP
                                                   6/91

-------
                              10LCA
      LOW CONG. WATER PESTICIDE  IDENTIFICATION SUMMARY
                FOR SINGLE  COMPONENT ANALYTES
                                         EPA SAMPLE  NO.
  Y Name:

Lab Code:
Case No.:
   Contract:^

    SAS No.:
SDG No.:
Lab Sample ID  :
Instrument ID  (1):

GC Column (1): 	
     ID:
      Date(s)  Analyzed:

      Instrument ID (2):

(mm)   GC Column(2): 	
         ID:
ANALYTE









COL
1
2
1
2
1
2
1
2
1
2
1
2
1
2
1
2
RT
















RT W]
FROM
















ENDOW
TO
















CONCENTRATION

















%D








page 	 of
                                FORM X LCP-1
                                                  6/91

-------
                             10LCB
      LOW CONC. WATER PESTICIDE IDENTIFICATION SUMMARY
                 FOR MULTICOMPONENT ANALYTES
                                         EPA  SAMPLE NO.
  b Name:_
Lab Code:
Case No.:
   Contract:
    SAS No.:
SDG No.:
Lab Sample ID :
Instrument ID (1)
GC column(1):
     ID:
      Date(s)  Analyzed:
      Instrument ID (2):
(mm)   GC Column(2): 	
         ID:
(mm
ANALYTE

COLUMN 1
COLUMN 2

COLUMN 1
COLUMN 2

COLUMN 1
COLUMN 2
PEAK
*1
*2
*3
4
5
*1
*2
*3
4
5
*1
*2
*3
4
5
*1
*2
*3
4
5
*1
*2
*3
4
5
*1
*2
*3
• 4
5
RT



















"™










RT W]
FROM









"









=










ENDOW
TO









=====









=










CONCENTRATION
































MEAN
CONCENTRATION








%D



   : least 3 peaks are required for  identification  of multicomponent analyses
page 	 of 	
                                 FORM X LCP-2
                                                   6/91

-------
                                         SAMPLE LOG-EN  SHEET
Lab Name:
Received Bv ( Print Name* Log in Dale:
Received By fSipumre^:

Cue Number:
Sample Delivery
Group No^ ,
SAS Number:

REMARKS:
1. Custody Se*l(s) Pnsent/Abseat*
Intact/Broken
2. Cuaodv Sal Not_-

3. Quim-of-Cuaody Present/Absent*
Recoris
4. Tnffic Repoiu or Present/Absent"
Picking List
S. Aiifafll Aiibfll/Sticker
Present/Absent*
. Annul No.:
7. Sample T««J PreseBt/Absenl*
SampfeTag Liaed/Nbt Liaed
Nmnben on Cham-of-
Gttody
8. Sample Coodition: Inuct/Broken*/
Leaking
9. Does infonnation on
icportit JOQ SMDJMC
tags une? Yes/No*
10. Due Received at L«tr

11. TuneReeoved;

Sample Transfer





nn. 	 r. _.

EPA
SAMPLE
#


























CORRESPONDING
SAMPLE
TAG
*

























ASSIGNED
LAB
*


























REMARKS:
CONDITION
OF SAMPLE
SHIPMENT, ETC.

























   • Conua SMO and attach recort of resolution
   Reviewed By: ________________
   Date:	
Logbook No,;  	
Logbook Page  No:
                                               FORM DC-1

-------
          LOW CONCENTRATION  WATER FOR ORGANICS COMPLETE SDO FILE (CSF) INVENTORY SHEET
      LABORATORY NAME 	 CITY/STATE
      CASE NO. _ SOC NO. _ SDG NOS. TO FOLLOW

      NO. _
      CONTRACT NO. _ SOU NO.
     All documents  delivered  in the  complete SDG  file must  be original documents
     where possible.  (REFERENCE EXHIBIT B,  SECTION  II,  PARAGRAPH 5, and SECTION  III,
     PARAGRAPH 16.)
                                                                  PAGE NOs        CHECK
                                                                 FROM   TO     LAB      EPA
1.   Inrentcrr Sheet (Form DC*2)  (Do not number)
2.   SPG case Narrative
3.   Traffic Report
4.   Volatile* Data
     a..  QC  Summary
          Surrogate Percent Recovery Summary (Form II LCV)
          Lab Control Sample Recovery (From III LCV)
          Method Blank Summary (Form IV LCV)
          Tuning and Mass Calibration (Form V LCV)

     b.  Sample  Data
          TCL Results • (Form I LCV)
          Tentatively Identified Compounds (Form I LCV-TIC)
          Reconstructed total ion chromatograms (RIC)
            and Quantitation Reports for each sample
          For each sample:
            Raw spectra and background-subtracted
              mass spectra of target compounds identified
            Mass spectra of all reported TICs with three
              best library matches

     c.  Standards Data (All Instruments)
          Initial Calibration Summary (Form VI LCV)
          RICs and Quan Reports for all Standards
          Continuing Calibration (Form VII LCV)
          RICs and Quant Reports for all Standards
          Internal Standard Area and RT Summary
            (Form VIII LCV)

     d.  QC  Data
          BFB
          Blank Data
          LCS Data
          PES Data

5.   semivola'ti.laa Data
     a.  QC  Summary
          Surrogate Percent Recovery Summary (Form II LCSV)
          Lab Control Sample Recovery (Form III LCSV)
          Method Blank Summary (Form IV LCSV)
          Tuning and Mass Calibration (Form V LCSV)
                                           FORM DC-2-1

                                                                                              6/

-------
    LOW COHCEHTRAXIOX WATER FOR ORGAHICS  COMPLETE SDO FILE (CSF)  INVENTORY SHEET (Coat.)
      CASE NO. 	 SDG MO. 	  SOG NOS. TO FOLLOW 	 	 	 SAS MO.
                                                                 PAGE NOs        CHECK
                                                                FROM  TO      LAB     EPA
5.    8»iH^ol»-tHe» Pa'fca (cont.)

     b.  Sample  Data
          TCL Results (Form I LCSV)
          Tentatively Identified Compounds (Form I LCSV-TIC)
          Reconstructed total ion chromatograms (RIC)
            and  Quantitation Reports for each sample
          For each sample:
            Raw  spectra and background-subtracted
              mass spectra of TCL compounds
            Mass spectra of TICs with three best library matches
              GFC chromatograms (if GPC performed)

     c.  Standards Data (All Instruments)
          Initial Calibration Summary (Form VI LCSV)
          RICs and Quan Reports for all Standards
          Continuing Calibration (Form VII LCSV)
          RICs and Quan Reports for all Standards
          Internal Standard Area and RT Summary
            (Form VIII LCSV)

     d.  QC  Data
          DFTPP
          Blank  Data
          LCS Data
          FES Data

6.    Pesticide*

     a.  QC  Summary
          Surrogate Percent Recovery Summary (Form II LCP)
          Lab Control Sample Recovery (Form III LCP)
          Method Blank Summary (Form IV LCP)

     b.   Sample  Data
          TCL Results - Organic Analysis Data Sheet
            (Form I LCP)
          Chromatograms (Primary Column)
          Chromatograms from second GC column confirmation
          GC Integration report or data system printout and
            calibration plots
          Manual work sheets
          For pesticides/Aroclors confirmed by GC/MS, copies
            of raw spectra and copies of background-subtracted mass
            spectra of target compounds (samples & standards)
                                           FORM DC-2-2

-------
    LOW CONCENTRATION WATER FOR ORGANZCS COMPLETE SCO FILE (CSF) INVENTORY SHEET (Cont.)
      CASE NO.
                     SOG NO.
                                    soc MOS. TO rau.au
                                                                           SAS HO.
                                                                  PAGE NOs
                                                                FROM   TO
                                                                             CHECK
                                                                         IAB    EPA
5.   Pertieidea (cont.)

     c.  Standards  Data
          Initial Calibration Data (Form VI LCP)
          Calibration Verification (Form VII LCP)
          Pesticides Analytical Sequence (Form VIII,
            LCP-1 and -2)
          PesticideFlorisil Cartridge Check (Form IX, LCP)
          Pesticide Identification (Form X LCP)
          Standard chromatograms and data system printout
            for all Standards
          For pesticides/Aroclors confirmed by GC/MS, copies
            of spectra for standards used

     d.  QC  Data
          Blank Data
          LCS Data
          PES Data
      Original preparation and analysis forms or copies of
        preparation and analysis logbook pages
      Internal sample and sample extract transfer
        chain-of-custody records
      Screening records
      All instrument output, including strip charts
        from screening activities  (describe or list)
3.
EPA Shli
         lino/
      Airbills (No. of shipments 	)
      Chain-of-Custody Records
      Sample Tags
      Sample Log-In Sheet (Lab & DC1)
      SDG Cover Sheet
      Miscellaneous Shipping/Receiving Records
        (describe or list)
9.    IntemaJ. I»ab Saaple Transfer1 Records and Tracking Sheet*
    (describe or list)
                                           FORM DC-2-3

-------
    LOW CONCENTRATION WATER FOR ORGANICS COMPLETE SDG FILE  (CSF)  INVENTORY SHEET (Cont.)
      CASE NO.
                      SOG NO.
                                    SOG MOS. TO FOLLOW
.0.  Other Record* (describe or  list)

      Telephone Commmication  Log
1.1.
                                                                           SAS NO.
                                                                  PAGE NOs        CHECK
                                                                FROM   TO      LAB    EPA
Zompleted by:
  (CLP Lab)
(Signature)
(Printed Name/Title)
(Date)
Audited by:
  (EPA)
(Signature)
(Printed Name/Title)
(Date)
                                           FORM DC-2-4

-------
                                   EXHIBIT C
                        TARGET COMPOUND LIST (TCL) AND
                 CONTRACT REQUIRED  QUANTITATION LIMITS  (C&QLs)
NOTE:   The values  in these tables  are quantitation limits,  not absolute
        detection limits.   The  amount of material  necessary  to  produce a
        detector response  that  can  be identified and. reliably quantified is
        greater  than that  needed to simply be  detected above the background
        noise.   Except as  noted,  the quantitation  limits in  these tables are
        set at the  concentrations in the sample  equivalent to the
        concentration of the lowest calibration  standard analyzed for each
        analyte.
                                     C-l                               6/91

-------
       TARGET COMPOUND LIST (TCL) AND
CONTRACT REQUIRED QUANTITATION LIMITS (CRQL)

1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
21.
22.
23.
24.
25.
26.
27.
28.
29.
Volatiles
Chlorone thane
Bromome thane
Vinyl chloride
Chloroethane
Methylene chloride
Acetone
Carbon disulfide
1,1- Dichloroe thene
1 , 1-Dichloroe thane
cis -1,2 -Dichloroe thene
trans -1,2 -Dichloroe thene
Chloroform
1 , 2 - Dichloroe thane
2-Butanone
Bromochlorome thane
1 , 1 , 1-Trichloroethane
Carbon Tetrachloride
Bromodichlorome thane
1 , 2 -Dichloropropane
cis - 1 , 3 - Dichloropropene
Trichloroe thene
Oibroaochlorome thane
1,1, 2 -Trichloroe thane
Benzene
trans - 1 , 3 -Dichloropropene
Brontoform
4-Methyl-2-pentanone
2-Hexanone
Tetrachloroe thene
CAS Number
74-87-3
74-83-9
75-01-4
75-00-3
75-09-2
67-64-1
75-15-0
75-35-4
75-34-3
156-59-4
156-60-5
67-66-3
107-06-2
78-93-3
74-97-5
71-55-6
56-23-5
75-27-4
78-87-5
10061-01-5
79-01-6
124-48-1
79-00-5
71-43-2
10061-02-6
75-25-2
108-10-1
591-78-6
127-18-4
Quantisation Limits
Water
"g/L
1
1
1
1
2
5
1
1
1
1
1
1
1
5
1
1
1
1
1
1
1
1
1
1
1
1
5
5
1
                    C-2
6/91

-------
                        TARGET COMPOUND LIST (TCL) AND
                 CONTRACT REQUIRED QUANTITATION LIMITS (CRQL)
                                   (CONT'D.)
                                                       Quantitation Limits
            Volatiles
CAS Number
Water
ug/L
30.
31.
32.
33.
34.
35.
36.
37.
38.
39.
1,1,2, 2-Tetrachloroethane
1 , 2-Dibromoethane
Toluene
Chlorobenzene
Ethylbenzene
Styrene
Xylenes (total)
1, 3-Dichlorobenzene
1,4- Dichlorobenzene
1 , 2 -Dichlorobenzene
79-34-5
106-93-4
108-88-3
108-90-7
100-41-4
100-42-5
1330-20-7
541-73-1
106-46-7
95-50-1
1
1
1
1
1
1
1
1
1
1
   40. l,2-Dibromo-3-chloropropane
 96-12-8
NOTE:   Except  for Methylene  chloride,  the  quantitation limits  in this  table
        are set at the concentrations  in the  sample  equivalent  to the
        concentration of  the  lowest calibration standard analyzed for each
        analy te.

        In the  case of Methylene chloride,  the  CRQL  value in this table is
        based on the lowest level of detection  in samples contaminated  with
        this common laboratory solvent that can be achieved by  reasonable
        means in a production laboratory.
                                     C-3
                               6/91

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       TARGET COMPOUND LIST  (TCI.) AND
CONTRACT REQUIRED OPAMTITATTOM T,TMITS (CROP
                  (CONT'D.)
                                       Quantisation Limits

1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
21.
22.
23.
24.
25.
26.
27.
28.
29.
30.
31.
32.
33.
Sentivo latiles
Phenol
bis- (2-Chloroethyl)ether
2 -Chlorophenol
2-Methylphenol
2,2'- oxyb is ( 1 - caxloropropane )
4-Methylphenol
N- Nitroso - di - n- pr opy lamine
Hexachloroe thane
Nitrobenzene
Isophorone
2-Nitrophenol
2 , 4-Dimechylphenol
bis- (2-Chloroethoxy)me thane
2 , 4-Oichlorophenol
1,2,4-Trichlorobenzene
Naphthalene
4-Chloroaniline
Hexachlorobutadiene
4-Chloro- 3 -methylphenol
2 -Me thy Inaphthalene
Hexachlorocyclopentadiene
2,4,6- Trichloropheno 1
2,4,5- Trichloropheno 1
2 - Chloronaphthalene
2-Nitroaniline
Dime thy Iphthalate
Acenaphthylene
2 , 6 -Dinitro toluene
3-Nitroaniline
Acenaphthene
2 , 4-Dinitrophenol
4 - Ni tropheno 1
Dibenzofuran
CAS Number
108-95-2
111-44-4
95-57-8
95-48-7
108-60-1
106-44-5
621-64-7
67-72-1
98-95-3
78-59-1
88-75-5
105-67-9
11-91-1
120-83-2
120-82-1
91-20-3
106-47-8
87-68-3
59-50-7
91-57-6
77-47-4
88-06-2
95-95-4
91-58-7
88-74-4
131-11-3
208-96-8
606-20-2
99-09-2
83-32-9
51-28-5
100-02-7
132-64-9
Water
US/L
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
20
5
20
5
5
5
20
5
20
20
5
                    C-4
6/91

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       TARGET COMPOUND LIST (TCL) AND
CONTRACT REQUIRED QUANTITATION LIMITS (CRQL)
                  (CONT'D.)
                                      Quancitacion Limits

34.
35.
36.
37.
38.
39.
40.
41.
42.
43.
44.
45.
46.
47.
48.
49.
50.
51.
52.
53.
54.
55.
56.
57.
58.
59.
60.
Semivolaciles
2 , 4-Dinitrotoluene
Oiethylphthalate
4- Chloropheny 1 - pheny le ther
Fluorene
4-Nitroaniline
4, 6-Dinitro-2-methylphenol
N-Nitrosodiphenylamine
4-Bronophenyl-phenylether
Hexachlorobenzene
Pentachlorophenol
Phenanthrene
Anthracene
Di -n-butylphthalate
Fluoranthene
Pyrene
Butylbenzylphthalate
3,3' -Dichlorobenzidine
Benzo(a) anthracene
Chrysene
b is - ( 2 - Ethy Ihexyl ) phthalate
Di -n-octylphthalate
Benzo (b ) fluoranthene
Benzo (k) fluoranthene
Benzo ( a ) pyr ene
Indeno ( 1 , 2 , 3 - cd) pyrene
Dibenz ( a , h) anthracene
Benzo (g,h,i)perylene
CAS Number
121-14-2
84-66-2
7005-72-3
86-73-7
100-01-6
534-52-1
86-30-6
101-55-3
118-74-1
87-86-5
85-01-8
120-12-7
84-74-2
206-44-0
129-00-0
85-68-7
91-94-1
56-55-3
218-01-9
117-81-7
117-84-0
205-99-2 -
207-08-9
50-32-8
193-39-5
53-70-3
191-24-2
Water
ug/L
5
5
5
5
20
20
5
5
5
20
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
5
                    C-5
6/91

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       TARGET COMPOUND LIST (TCL) AND
CONTRACT REQUIRED QUANTITATION LIMITS (CRQL)
                  (CONT'D.)
Quaneitation Limits
Pcsticides/PCBs
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
21.
22.
23.
24.
25.
26.
27.
28.
alpha-BHC
beta-BHC
delta-BHC
gamma-BBC (Lindane)
Heptachlor
Aldrin
Heptachlor epoxide
Endosulfan I
Dieldrin
4, 4' -DDE
Endrin
Endosulfan II
4,4' -ODD
Endosulfan sulfate
4, 4' -DDT
Methoxychlor
Endrin ketone
Endrin aldehyde
alpha- Chlordane
gamna- Chlordane
Toxaphene
Aroclor-1016
Aroclor-1221
Aroclor-1232
Aroclor-1242
Aroclor-1248
Aroclor-1254
Aroclor-1260
CAS Number
319-84-6
319-85-7
319-36-8
58-89-9
76-44-8
309-00-2
1024-57-3
959-98-8
60-57-1
72-55-9
72-20-8
33213-65-9
72-54-8
1031-07-8
50-29-3
72-43-5
53494-70-5
7421-36-3
5103-71-9
5103-74-2
8001-35-2
12674-11-2
11104-28-2
11141-16-5
53469-21-9
12672-29-6
11097-69-1
11096-82-5
Water
ug/L
0.01
0.01
0.01
0.01
0.01
0.01
0.01
0.01
0.02
0.02
0.02
0.02
0.02
0.02
0.02
0.10
0.02
0.02
0.01
0.01
1.0
0.20
0.40
0.20
0.20
0.20
0.20
0.20
                    C-6
6/91

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                       EXHIBIT D
METHOD FOR THE ANALYSIS OF LOW  CONCEIITBATIOH BATES. FOR
        VOLATILE  (FURGEABLE) ORGANIC  COMPOUNDS
                         VOA D-l                            6/91

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                              Table of Contents
                                                                      Page
SECTION I:    Introduction	VOA D- 3

SECTION II:
              Part A - Sample Storage and Holding Tines	VOA D-4
              Part B -  	VOA D-5

SECTION III:  Instrument Quality Control Procedures
                and Requirements
              Part A - Instrument Operating Conditions 	VOA D-15
              Part B - Tuning the Mass Spectrometer	VOA D-17
              Part C - Calibration of the GC/MS System	VOA D-19

SECTION IV:   Sample Analysis and Compound Identification
                and Quantitation	VOA D-26

SECTION V:    Sample Quality Control Procedures and
                Requirements 	VOA D-36
                                     VOA D-2
6/91

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                                   SECTION I

                                 INTRODUCTION
The analytical method that follows is designed to analyze samples containing
low concentrations of the volatile compounds listed in the Target Compound
List  (TCL) in Exhibit C.  The majority of the samples are expected to be from
drinking water and well/ground water sources around Superfund sites.  The
method is based on EPA Method 524.2 and the volatile method contained in the
CLP Statement of Work, "Organic Analysis, Hulti Media, Multi Concentrations
by GO/MS and GC/EC Techniques".  Specific quality control requirements are
incorporated in the method in order to minimize contamination of the samples
from  laboratory sources.

Problems have been associated with the following compounds analyzed by this
method.

o   Chloromethane, vinyl  chloride,  bromomethane,  and chloroethane may display
    peak broadening  if the compounds  are  not delivered to the GC column in a
    tight band.
o   Acetone, hexanone,  2-butanone.  and 4-methyl-2-pentanone have poor purge
    efficiencies.

o   1,1,1-Trichloroethane and all of  the  dichloroethanes  may dehydrohalogenate
    during  storage or analysis.

o   Tetrachloroethane and 1,1-dichloroethane may  be  degraded by contaminated
    transfer lines in purge and trap  systems and/or  active sites in trapping
    materials.

o   Chloromethane may be  lost if the  purge flow is too fast.

o   Bromoform  is one of the compounds most likely to be adversely affected by
    cold spots and/or active sites  in the transfer lines.   Response of its
    quantitation ion (m/z 173)  is directly affected  by the tuning of BFB at
    ions  m/z 174/176.   Increasing the m/z 174/176 ratio within the specified
    QC limits may improve bromoform response.

o   Due  to  the lower quantitation limits  required by this method,  extra
    caution must be  exercised when  identifying compounds.
                                     VOA D-3                           6/91

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                                  SECTION II


PART A - SAMPLE STORAGE AND HOLDING TIMES

1.    PROCEDURES FOR SAMPTg STORAGE

      The samples oust be protected from light and refrigerated at 4*0 (±2*C)
      froa the time of receipt until 60 days after delivery of a complete
      reconciled sample data package.  After 60 days,  the samples may be
      disposed of in a manner that complies with all applicable regulations.

      The samples must be stored in an atmosphere demonstrated to be free of
      all potential contaminants and in a refrigerator used only for storage
      of purgeable samples received under this contract.

      Samples, sample extracts, and standards must be  stored separately.

      Volatiles standards must be stored separately from semivolatile and
      pesticide/Aroclor standards.

2.    CONTRACT REQUIRED HOLDING TIMES

      Analysis of samples must be completed within 10  days of the validated
      time of sample receipt (VTSR).
                                     VGA D-4                           6/91

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FART B

3.    SUMMARY OF METHOD

3.1   An inert gas is bubbled through a 25 mL sample contained in a specially
      designed purging chamber at ambient temperature causing the purgeables
      to be transferred from the aqueous phase to the vapor phase.  The vapor
      is swept through a sorbent column where the purgeables are trapped.
      After purging is completed, the sorbent column is heated and
      backflushed with the inert gas to desorb the purgeables onto a gas
      chromatograph (GO) wide-bore capillary column.  The gas chromatograph
      is temperature programmed to separate the purgeables, which are then
      detected with a mass spectrometer (MS) .

3.2   Target and surrogate compounds are identified in the samples by
      analyzing standards under the same conditions used for samples and
      comparing resultant mass spectra and GC retention times.  Internal
      standards are added to all samples and standards.  A response factor is
      established for each target and surrogate compound during the initial
      and continuing calibrations by comparing the MS response from the
      extracted ion current profile (EICP) for the primary ion produced by
      the target and surrogate compound to the MS response for the primary
      ion produced by an internal standard compound.  Each identified target
      and surrogate compound in a sample is quantified by comparing the
      responses for the target compound and the internal standard, while
      taking into account the response factor from the most recent
      calibration, the sample volume, and any sample dilutions.

3.3   Non- target compounds are identified by comparing the resultant mass
      spectra from the non- target compounds to mass spectra contained in the
      National Institute of Standards and Technology Mass Spectral Library.
      Non- target compounds are quantified by comparing the MS response from
      the reconstructed ion chromatogram (RIG) for the non- target compound
      peaks to the MS response for a peak produced by the nearest internal
      standard compound.  A response factor of 1 is assumed.
4.
4.1   Impurities in the purge gas or methanol, organic compounds out-gassing
      from the plumbing ahead of the trap, and solvent vapors in the
      laboratory account for the majority of contamination problems.  Gas
      lines from the gas tanks to the instrument must be either stainless
      steel or copper tubing.  Non-polytetrafluoroethylene (PTFE) thread
      sealants, or flow controllers with rubber components are not to be
      used.  When potential interfering peaks are noted in laboratory method
      blanks, it may be necessary to reduce solvent contamination in the
      laboratory, purge the methanol used to prepare standard solutions,
      purge the reagent water with helium or nitrogen, change the purge gas
      source, or regenerate the molecular sieve purge gas filter.

4.2   Samples can be contaminated by diffusion of purgeable organics
      (particularly methylene chloride, fluorocarbons , and other common
      laboratory solvents) through the septum seal into the sample during
      storage and handling.  Therefore, these samples must be stored

                                     VGA D-5                           6/91

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      separately from other laboratory samples and standards and must be
      analyzed in a room whose atmosphere is demonstrated to be free of all
      potential contaminants which will interfere with the analysis.  Since
      methylene chloride will permeate through PTFE tubing, all gas
      chromatography carrier gas lines and purge gas plumbing lines are to be
      constructed from stainless steel or copper tubing.
      Non-polytetrafluoroethylene (PTFE) thread sealants, or flow controllers
      with rubber components are not to be used. Laboratory clothing worn by
      the analyst must be clean of solvents since clothing previously exposed
      to methylene chloride and other laboratory solvent fumes during common
      liquid/liquid extraction procedures can contribute to sample
      contamination.

4.3   Contamination by carryover can occur whenever a sample is analyzed
      after a. high level sample which contain high levels of organic
      compounds.  To reduce carryover, the sample purger and sampling syringe
      must be rinsed with reagent water between sample analyses.  Whenever an
      unusually concentrated sample is encountered, it must either be
      followed by analysis of an instrument blank or the next sample must be
      closely monitored to check for cross contamination.  For samples
      containing large amounts of water soluble materials, suspended solids,
      high boiling compounds,  or high purgeable levels, it is necessary to
      wash out the sample purger with a detergent solution between analyses,
      rinse it with distilled water, and then dry it in a 105*C oven.  The
      trap and other parts of the system are also subject to contamination;
      therefore, frequent bakeout and purging of the entire system may be
      required.

5.    APPARATUS AMD MATERIALS

      Brand names,  suppliers and part numbers are for illustrative purposes
      only.  No endorsement is implied.  Equivalent performance may be
      achieved using apparatus and materials other than those specified here,
      but demonstration of equivalent performance meeting the requirements of
      the method is the responsibility of the Contractor.

5.1   Purge and Trap Device -  The purge and trap device consists of three
      separate pieces of equipment;  the sample purger, the trap, and the trap
      heater.  Purge gas plumbing lines are to be constructed from stainless
      steel or copper tubing.   Non-polytetrafluoroethylene (PTFE) thread
      sealants, or flow controllers with rubber components are not to be
      used.

      5.1.1   Sample Purger - The sample purger must be  designed to  accept 25
              mL samples with a water column at least  10  cm deep.  The
              gaseous head space between the water column and the trap must
              have a total volume of less than 15 mL.  The purge  gas must
              pass through the water column as finely  divided bubbles, each
              with a diameter of less than 3 mm at the origin.  The  purge  gas
              must be introduced no more than 5 mm from  the base  of  the water
              column.  Alternate sample purge devices may be utilized
              provided equivalent performance is demonstrated.  A set of
              sample purgers sufficient to meet contract  requirements must be
              reserved for exclusive use in this contract.

                                     VGA D-6                           6/91

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      5.1.2   Trap  Packing

              5.1.2.1    2,6-Diphenylene oxide polymer, 60/80 mesh,
                         chromatographic grade (Tenax GC or equivalent).

              5.1.2.2    Methyl silicone packing, 3 percent OV-1 on
                         Chromosorb V, 60/80 mesh (or equivalent).

              5.1.2.3.   Silica gel (35/60 mesh, Davison, grade 15 or
                         equivalent).

      5.1.3   Trap  - The trap must be at least 25 cm long and have an  inside
              diameter of at least 0.105 inch (0.2667 cm).  Starting from the
              inlet, pack the column in the following order: 0.5 cm silanized
              glass wool, 1 cm methyl silicone coated packing, 15 cm
              2,6-diphenylene oxide polymer, 8 cm silica gel, and 0.5  cm
              silanized glass wool.

      5.1.4   Trap  Heater

              5.1.4.1    The trap heater must be capable of rapidly heating
                         the trap to 180*0.  The polymer section of the trap
                         should not be heated to greater than 180*C and the
                         temperature of the remaining sections should not
                         exceed 220*C during bakeout mode.

              5.1.4.2    The purge and trap device may be assembled as a
                         separate unit or be coupled to a gas chromatograph.

5.2   Gas Chromatograph/Mass Spectrometer

      5.2.1   Gas Chromatograph - The gas chromatograph  (GC) system must be
              capable of temperature programming and have a flow controller
              that  maintains a constant column flow rate throughout
              desorption and temperature program operations.  The system must
              include or be interfaced to a purge and trap system as
              specified in Section 5.1 and have all required accessories
              including syringes, analytical columns, and gases.  All  GC
              carrier gas lines must be constructed from stainless steel or
              copper tubing.  Non-polytetrafluoroethylene (PTFE) thread
              sealants, or flow controllers with rubber components are not to
              be used. The column oven must be cooled to 10*C; therefore, a
              subambient oven controller is required.

              5.2.1.1   Gas  Chromatography Columns

                         Column 1-30 m long x 0.53 mm ID VOCOL (Supelco,
                         Inc.) or equivalent fused silica wide-bore capillary
                         column with 3 um film thickness.

                         Column 2-30 m long x 0.53 mm ID DB-624 fused  silica
                         wide-bore (J&W Scientific, Inc.) or equivalent
                         column with 3 um film thickness.
                                     VOA D-7                           6/91

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      5.2.2   Mass Spectrometer - The mass spectrometer must be capable of
              scanning from 35 to 300 amu every 1 second or less, utilizing
              70 volts (nominal) electron energy in the electron impact
              ionization mode and producing a mass spectrum which meets all
              the tuning acceptance criteria when 50 ng of
              p-bromofluorobenzene (BFB) are injected through the gas
              chromatograph inlet.  To ensure sufficient precision of mass
              spectral data, the MS scan rate must allow acquisition of at
              least five spectra while a sample compound elutes from the GC.
              The purge and trap GO/MS system must be in a room whose
              atmosphere is demonstrated to be free of all potential
              contaminants which will interfere with the analysis.  The
              instrument must be vented to outside the facility or to a
              trapping system which prevents the release of contaminants into
              the instrument room.

      5.2.3   GO/MS Interface - Any gas chromatograph to mass spectrometer
              interface may be used that gives acceptable calibration points
              at 25 ng or less per injection for each of the purgeable target
              and surrogate compounds and achieves all acceptable performance
              criteria.  Gas chromatograph to mass spectrometer interfaces
              constructed of all-glass or glass-lined materials are
              recommended. Glass can be deactivated by silanizing with
              dichlorodimethylsilane.

      5.2.4   Data System - A computer system must be interfaced to the mass
              spectrometer that allows the continuous acquisition and storage
              on inrhln* readable media of all mass spectra obtained
              throughout the duration of the chromatographic program.  The
              computer must have software that allows searching any GC/HS
              data file for ions of a specified mass and plotting such ion
              abundances versus time or scan number.  This type of plot is
              defined as an Extracted Ion Current Profile (EICF).  Software
              must also be available that allows integrating the abundance in
              any EICF between specified time or scan number limits.  Also,
              for the non-target compounds, software must be available that
              allows comparing sample spectra against reference library
              spectra.  The most recent release of the National Institute of
              Standards and Technology Mass Spectral Library shall be used as
              the reference library.

5.3   Magnetic Tape Storage Device -  The magnetic tape storage device must be
      capable of recording data and must be suitable for long-term,  off-line
      storage.

5.4   pH paper - wide range.

5.5   Glassware - A set of glassware sufficient to meet the contract
      requirements must be reserved for exclusive use in this contract.

      5.5.1   Bottles - 15 mL, screw-cap, with Teflon cap liner.

      5.5.2   Volumetric flasks - class A with ground-glass stoppers.
                                     VGA D-8                           6/91

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 5.6   Micro  syringes  -  10 uL  and  larger, 0.006 inch ID needle.

 5.7   Syringe valve  - two-way, with Luer ends (three each), if applicable to
      the purging  device.

 5.8   Syringe -  25 mLt  gas tight  with shut-off valve.

 5.9   Analytical Balance - capable of accurately weighing ±0.0001 g.  The
      balance must be calibrated  with class S weights once per each 12-hour
      workshift.   The balance must also be annually checked by a certified
      technician.

 5.10  Gases  - Heliun, Nitrogen.   Ultra-pure grade.

 5.11  Gas line tubing - polytetrafluoroethylene, stainless steel, or copper
      tubing.

 6.    REAGENTS

 6.1   Reagent water - Reagent water is defined as water in which no purgeable
      target compound is observed at or above the CRQL listed in Exhibit C
      for that compound and in which no non-target compound is observed at or
      above  2.0  ug/L.

      6.1.1   Reagent water may be generated by passing tap water through a.
              carbon filter bed containing about 453 g (1 Ib.) of activated
              carbon (Calgon  Corp., Filtrasorb-300, or equivalent).

      6.1.2   Reagent water may be generated using a water purification
              system (Millipore Super-Q, or equivalent).

      6.1.3   Reagent water may be prepared by boiling water  for 15 minutes.
              Subsequently, while maintaining the temperature at 90*C, bubble
              a  contaminant-free  inert gas through the water  for one hour.
              While still hot, transfer the water to a narrow-mouth screw-cap
              bottle, seal with a Teflon-lined septum, and cap.

6.2   Methanol - HFLC quality or equivalent--Each lot of methanol used for
      analysis under this contract must be purged with nitrogen and must be
      demonstrated to be free of contaminants that interfere with the
      measurement of purgeable compounds listed in the Exhibit C.

7.    STANDARDS

7.1   The Contractor must provide all standards  to be used with this
      contract.   These standards  may be used only after they have been
      certified according to  the  procedure in Exhibit E.   The Contractor oust
      be able to verify that  the  standards are certified.   Manufacturer's
      certificates  of analysis must be retained by the Contractor and
      presented upon request.
                                     VOA D-9                           6/91

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7.2   Stock Standard Solutions

      Stock standard solutions may be purchased or may be prepared in
      methanol from pure standard materials.

      7.2.1   Prepare  stock standard solutions by placing about 9.8 mL of
              methanol into a 10.0 mL ground- glass stoppered volumetric
              flask.   Allow the flask to stand, unstoppered, for about 10
              minutes  or until all alcohol wetted surfaces have dried.  Weigh
              the  flask to the nearest 0.1 mg.

      7.2.2   Add  the  assayed reference material as described below.

              7.2.2.1    If the compound is a liquid,  using a 100. uL syringe,
                         immediately add two or more drops of assayed
                         reference material to the flask, then reweigh.  The
                         liquid must fall directly into the alcohol without
                         contacting the neck of the flask.

              7.2.2.2    If the compound is a gas at room temperature, fill a
                         5 mL valved gas-tight syringe with the reference
                         standard to the 5.0 mL mark.   Lower the needle to 5
                         mm above the methanol meniscus.  Slowly introduce
                         the reference standard above the surface of the
                         liquid.  The gas will rapidly dissolve in the
                         methanol.  This may also be accomplished by using a
                         lecture bottle equipped with a Hamilton Lecture
                         Bottle Septum (#86600).  Attach Teflon tubing to the
                         side-arm relief valve and direct a gentle stream of
                         the reference standard into the methanol meniscus.
      7.2.3   Reweigh, dilute to volume, stopper, then M* by inverting  the
              flask  several times.  For non- gaseous compounds, calculate the
              concentration in micrograms per microliter from the net  gain in
              weight.  When compound purity is assayed to be 97 percent  or
              greater, the weight may be used without correction to calculate
              the concentration of the stock standard.  If the compound
              purity is assayed to be less than 97 percent, the weight must
              be corrected when calculating the concentration of the stock
              solution.  For gaseous compounds, calculate the concentration
              in micrograms per microliter, using the Ideal Gas Law, taking
              into account the temperature and pressure conditions within the
              laboratory .

      7.2.4   Prepare fresh stock standards every two months for gases or for
              reactive compounds such as styrene.  All other stock standards
              for non- gases/non- reactive purgeable compounds must be replaced
              after  six months, or sooner, if standard has degraded or
              evaporated.

7.3   Secondary Dilution Standards

      7.3.1   Using  stock standard solutions, prepare secondary dilution
              standards in methanol that contain the compounds of interest,

                                     VGA D-10                          6/91

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               either  singly  or mixed  together.  Secondary dilution standard
               solutions  should be prepared at concentrations that can be
               easily  diluted to prepare working standard solutions.

      7.3.2    Prepare fresh  secondary dilution standards for gases and for
               reactive compounds, such as styrene, every month or sooner, if
               standard has degraded or evaporated.  Secondary dilution
               standards  for  the other purgeable compounds must be rep-laced
               after six  months, or sooner, if standard has degraded or
               evaporated.

7.4   Working Standards

      7.4.1    Tuning  Solution - p-Bromofluorobenzene (BFB)

               Prepare a  25 ng/uL solution of BFB in methanol.  Prepare fresh
               BFB solution every six months, or sooner, if the solution has
               degraded or evaporated.  Note:  The 25 ng/uL concentration is
               used with  a 2 uL injection volume.  The laboratory may prepare
               a 50 ng/uL solution of BFB if a 1 uL injection volume is used.

      7.4.2    Calibration Standard Solution

               Prepare  the working calibration standard solution containing
               all of  the purgeable target compounds in methanol.  The
               concentration of the non-ketone target compounds and the
               surrogate must be 5.0 ug/mL in the standard (i.e., final
               concentration).  The concentration of the ketones (acetone,
              butanone, 2-hexanone, 4-methyl-2-pentanone) must be 25.0 ug/mL
               in the standard (i.e., final concentration).  Prepare fresh
              working calibration standard solutions weekly, or sooner, if
               solutions have degraded or evaporated.

      7.4.3    Internal Standard Spiking Solution

              Prepare an internal standard spiking solution containing 1,4-
              dichlorobenzene-d4,  chlorobenzene-d5,  and 1,4-difluorobenzene
              in methanol at the concentration of 12.5 ug/mL for each
              internal standard.   Add 10 uL of this  spiking solution into
              25.0 mL of sample or calibration standard for a concentration
              of 5.0 ug/L.   Prepare fresh spiking solution every three
              months.  or sooner,  if the solution has degraded or evaporated.

      7.4.4   Surrogate Compound Spiking Solution

              Prepare  12.5  ng/uL solution of p-bromofluorobenzene in
              methanol.  For samples and blanks,  add 10 uL of the surrogate
              compound solution to 25  mL of sample or reagent water for a
              final  concentration of 5 ug/L.   The surrogate compound is added
              to the working calibration standards so it is not to be added
              again  when aqueous  calibration standards are prepared.   Prepare
              fresh  surrogate compound solution every six months.  or sooner,
              if the solution has  degraded or evaporated.
                                    VGA D-ll                          6/91

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      7.4.5    Laboratory Control  Sample  (LCS)  Spiking.Solution

               Prepare the laboratory  control sample spiking solution
               containing all of the analytes listed below at 12.5 ng/uL in
               methanol.   The laboratory  control sample is prepared by adding
               10  uL of this  solution  into 25.0 mL of reagent water for  a
               concentration  of 5.0 ug/L.  Prepare fresh LCS spiking solution
               every six months, or sooner, if  the solution has degraded or
               evaporated.  The LCS must  contain the following compounds:
              1,2-Dibromoethane
              Benzene
              1,2-Dichloroethane
              1,2-Dichloropropane
              Tetrachoroethene
              Carbon tetrachloride
1,4-Dichlorobenzene
cis-1,3-Dichloropropene
1,1,2-Trichloroethane
Vinyl chloride
Bromoform
Trichloroethene
7.5   Aqueous Calibration Standard Solutions

      7.5.1   Prepare five aqueous initial calibration standard solutions
              containing all of the purgeable target compounds and the
              surrogate compound at the 1.0, 2.0, 5.0, 10, and 25 ug/L
              levels, except the ketones which are at the 5.0, 10, 25, 50,
              and 125 ug/L levels.  It is required that all three xylene
              isomers (o-,p- and m-xylene) be present in the calibration
              standards at concentrations of each isomer equal to that of the
              other target compounds (i.e., 1.0, 2.0, 5.0, 10.0 and 25 ug/L).
              The preparation procedure for the aqueous calibration standard
              solutions is listed in Table 0-1.  The internal standards are
              added to each calibration standard according to the procedures
              in Section 14.3.5.

                               TABLE  D-l

VOL OF
WORKING
STANDARD
(uL added
to 25 mL)
5
10
25
50
125
FINAL
CONG. OF
AQUEOUS
STANDARD FOR
NON-KETONES
(ug/L)
1
2
5
10
25
FINAL
CONG. OF
AQUEOUS
STANDARD FOR
KETONES
(ug/L)
5
10
25
50
125
                                    VOA D-12
                                6/91

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      7.5.2   Aqueous calibration standards may be prepared in a volumetric
              flask or in the syringe used to inject the standard into the
              purging device.

              7.5.2.1    Volumetric flask - Add an appropriate volume of
                         working calibration standard solution to an aliquot
                         of reagent water in a volumetric flask.  Use a
                         microsyringe and rapidly inject the alcohol standard
                         into the expanded area of the filled volumetric
                         flask.  Remove the needle as quickly as possible
                         after injection.  Bring to volume.  Mix by inverting
                         the flask three times only.  Discard the contents
                         contained in the head of the flask.

              7.5.2.2    Syringe - Remove the plunger from a 25 mL syringe
                         and close the syringe valve.  Pour reagent water
                         into the syringe barrel to just short of
                         overflowing.  Replace the syringe plunger and
                         compress the water.  Invert the syringe, open the
                         syringe valve and vent any residual air.  Adjust the
                         water volume to 25.0 mL minus the amount of
                         calibration standard to be added.  Withdraw the
                         plunger slightly and add an appropriate volume of
                         working calibration standard through the valve bore
                         of the syringe.  Close the valve and invert three
                         times.

      7.5.3   The  5 ug/L (25 ug/L for ketones) aqueous calibration  standard
              solution is the continuing calibration standard.

      7.5.4   A  smaller  sample or standard volume  (5 to 25 mL) may  be purged
              but  the CRQL and all QC criteria must be met.  The same purge
              volume must be used for all samples, standards, and blanks  in a.
              single SDG.

      7.5.5   The  methanol contained in each  of the aqueous calibration
              standards  must not exceed 1% by volume.

7.6   Storage of Standards

      7.6.1   Store the  stock standards in Teflon  sealed  screw-cap  bottles
              with zero  headspace at -10'C to -20'C.  Protect the standards
              from light.  Once one  of  the bottles containing the stock
              standard solution has  been opened, it may be used for no longer
              than one week.

      7.6.2   Store secondary dilution  standards in Teflon sealed screw-cap
              bottles with minimal headspace  at -10*C to  -20*C.  Protect the
              standards  from light.  The secondary dilution standards must  be
              checked frequently for signs of degradation or evaporation,
              especially just prior  to  preparing the working calibration
              standards  from them.
                                     VOA D-13                          6/91

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7.6.3   Aqueous standards may be stored up to 24 hours if held in
        Teflon sealed screw-cap vials with zero headspace at 4*C
        (±2*C).  Protect the standards from light. If not so stored,
        they must be discarded after one hour unless they are set up to
        be purged by an autosaopler.  When using an autosampler, the
        standards may be kept up to 12 hours in purge tubes connected
        via the autosampler to the purge and trap device.

7.6.4   Purgeable standards must be stored separately from other
        standards.
                               VOA D-14                          6/91

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                     SECTION III
INSTRUMENT QUALITY CONTROL PROCEDURES AND REQUIREMENTS
                         VOA D-15                          6/91

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FART A - INSTRUMENT OPERATING CONDITIONS

Purge and Trap

      The following are the recommended purge and trap analytical conditions
      except as stated below:
     Purge Conditions:

     Purge Gas:
     Purge Tine:
     Purge Flow Rate:
     Purge Temperature:

     Desorb Conditions:

     Desorb Temperature:
     Desorb Flow Rate:
     Desorb Time:
     Trap Reconditioning Conditions:

     Reconditioning Temperature:
     Reconditioning Time:
                                           Helium or Nitrogen
                                           11.0 ±0.1 min
                                           25-40 mL/min
                                           Ambient
                                           180 *C
                                           15 mL/min
                                           4.0 ±0.1 min
                                           180'C
                                           7.0 min ±0.1 min (minimum).  A
                                           longer time may be required to
                                           bake contamination or water from
                                           the system.

Before initial use, condition the trap overnight at 180*C by backflushing
with at least 20 mL/min flow of inert gas.  Vent the trap effluent to the
hood and not to the analytical column.  Prior to daily use, condition the
trap by heating at 180'C for 10 minutes while backflushing.  The trap may be
vented to the analytical column during daily conditioning; however, the
column must be run through the temperature program prior to analysis of
samples.

Optimize purge and trap conditions for sensitivity and to minimize cross
contamination between samples.  Once optimized, the same purge and trap
conditions must be used for the analysis of all standard, samples, blanks,
Performance Evaluation Samples and Laboratory Control Samples

Gas Chromatograph

     The following are the recommended gas chromatographic analytical
     conditions:
     Carrier Gas:
     Flow Rate:
     Initial Temperature:
     Initial Hold Time:

     Ramp Rate:
     Final Temperature:
     Final Hold  Time:
                                           Helium
                                           15 mL/min
                                           10" C
                                           1.0 - 5.0 min (±0.1 min
                                           precision)
                                           6'C/min
                                           160* C
                                           Until all target compounds elute
                                     VOA D-16
                                                                       6/91

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Optimize GC conditions for compound separation and sensitivity.  Once
optimized, the same GC conditions must be used for the analysis of all
standards, samples, blanks, performance evaluation samples, and laboratory
control samples.

Mass Spectrometer

     The following are the required mass spectrometer conditions:

     Electron Energy:                      70 Volts (nominal)
     lonization Mode:                      El
     Mass Range:                           35-300 amu
     Scan Time:                            To give at least 5  scans per
                                           peak, not to exceed 1 second per
                                           scan.
                                     VGA D-17                          6/91

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PART B  - TUNING THE MASS SPECTROMETER

8.    SUMMARY

      It is necessary to establish that a given GC/MS meets the standard mass
      spectral abundance criteria prior to initiating any on-going data
      collection.  This is accomplished through the analysis of
      p-bromofluorobenzene (BFB).

9.
      Each GC/MS used for volatile analysis must be hardware tuned once per
      twelve (12) hour time period of operation.  Also, whenever the
      Contractor takes corrective action which could change or affect the
      tuning for BFB (e.g., ion source cleaning or repair, column
      replacement, etc.), the tune must be verified before continuing
      analysis irrespective of the twelve-hour daily tuning requirement.  The
      twelve (12) hour time period for GC/MS system tuning and standards
      calibration (initial or continuing calibration criteria) begins at the
      moment of injection of the BFB analysis that the Contractor submits as
      documentation of a compliant tune.  The time period ends after twelve
      (12) hours have elapsed.  In order to meet the tuning requirements, a
      sample, LCS, PES, standard, or blank must be injected within twelve
      hours of the BFB injection.

10.   PROCEDURE

10.1  Inject 50 ng BFB into the GC/MS system.  Alternatively, add 50 ng of
      BFB solution to 25.0 mL of reagent water and analyze according to
      Section 17.  All instrument conditions must be identical to those
      listed in Section III, Part A, except that a different temperature
      program may be used.

10.2  For the tune, BFB may not be analyzed simultaneously with any
      calibration standards or blanks.

11.   TECHNICAL ACCEPTANCE CRITERIA FOR BFB ANALYSIS

11.1  The GC/MS system must be tuned at the frequency described in Section 9.

11.2  The abundance criteria listed in Table D-2 must be met for a 50 ng
      injection of BFB.  The mass spectrum of BFB must be acquired in the
      following manner.  Three scans (the peak apex scan and the scans
      immediately preceding and following the apex) are acquired and
      averaged.  Background subtraction is required, and must be accomplished
      using a single scan prior to the elution of BFB.  Note:   All
      subsequent standards and samples, including LCS, PES and blanks
      associated with a BFB analyses must use identical mass spectrometer
      instrument conditions.

11.3  The criteria listed in Table D-2 are based on adherence to the
      acquisition specifications identified in Section 11.2 and were
      developed for the specific target compound list associated with this
      method.  The criteria are based on performance characteristics of

                                     VOA D-18                          6/91

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      instruments currently utilized in routine support of Program
      activities.  These specifications, in conjunction with relative
      response factor criteria for 28 target compounds (see Table 0-5), are
      designed to control and monitor instrument performance associated with
      the requirements of this method.  As they are performance based
      criteria for these specific analytical requirements, they may not be
      optimal for additional target compounds.

            TABLE D-2  BFB KEY IONS AND ABUNDANCE CRITERIA

            Mass        Ion Abundance Criteria

            SO          8.0-40.0 percent of mass 95
            75          30.0 - 66,0 percent of mass 95
            95          base peak, 100 percent relative abundance
            96          5.0-9.0 percent of mass 95 (see note)
            173         less than 2.0 percent of mass 174
            174         50.0 - 120.0 percent of mass 95
            175         4.0 - 9.0 percent of mass 174
            176         93.0 - 101.0 percent of mass 174
            177         5.0 - 9.0 percent of mass 176


      Note:  All ion abundances must be normalized to m/z 95, the nominal
      base peak,  even though the ion abundance of m/z 174 may be up to 120
      percent that of m/z 95.

12.   CORRECTIVE ACTION

12.1  If the BFB technical acceptance criteria are not met, retune the GC/MS
      system.   It may also be necessary to clean the ion source, clean the
      quadrupole rods, or take other corrective actions to achieve the
      technical acceptance criteria.

12.2  BFB technical acceptance criteria MUST be met before any standards,
      samples or required blanks are analyzed.  Any samples (including LCS
      and FES),  or required blanks analyzed when tuning technical acceptance
      criteria have not been met will require reanalysis at no additional
      cost.
                                     VOA D-19                          6/91

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FART C • CALIBRATION OF THE GO/MS SYSTEM

14.   IHTTIAL CALIBRATION

14.1  Summary - Prior to the analysis of samples  and required blanks and
      after BFB technical acceptance criteria have been net,  each GC/MS
      system must be calibrated at a minimum of five concentrations to
      determine instrument sensitivity and the linearity of GC/MS response
      for the purgeable target and surrogate compounds.

14.2  Frequency

      14.2.1  Each GC/MS system must be calibrated upon award of the
              contract, whenever the Contractor takes corrective action which
              may change or affect the initial calibration criteria (i.e.,
              ion source cleaning or repair, column replacement, etc.), or  if
              the continuing calibration acceptance criteria have not been
              met.

      14.2.2  If time remains in the 12 hour time period after meeting the
              technical acceptance criteria for the initial calibration,
              samples may be analyzed.  It is not necessary to analyze a
              continuing calibration standard, if the initial calibration
              standard that is the same concentration as the continuing
              calibration standard meets the continuing calibration technical
              acceptance criteria.  A method blank is required.  Quantify all
              sample and quality control sample results and quality control
              criteria results, such as internal standard area response
              change and retention time shift, against the initial
              calibration standard that is the same concentration as the
              continuing calibration standard.

14.3  Procedure

      14.3.1  Set-up the purge and trap GC/MS system per the requirements of
              Section III, Part A.

      14.3.2  All samples, required blanks, and standard/spiking solutions
              must be allowed to warm to ambient temperature (approximately 1
              hour) before analysis.

      14.3.3  Tune the GC/MS system to meet the BFB technical acceptance
              criteria in Section 11.

      14.3.4  Prepare a spiking solution containing the internal standards
              using the procedure described in Section 7.4.3.

      14.3.5  Prepare five aqueous calibration standards containing all the
              purgeable target compounds and the surrogate using the
              procedure described in Section 7.5.  Add 10 uL of  the internal
              standard solution to each aqueous standard.  Analyze  each
              calibration standard, according to Section 17.  If a  compound
              saturates at the highest standard concentration  (Section
              7.5.1), and the GC/MS system  is calibrated to achieve a

                                     VOA D-20                          6/91

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              detection sensitivity of no less than 1.0 ug/L. the Contractor
              must document  it in the SDG Narrative and attach a quantitation
              report and RIC.  In this instance, the Contractor must
              calculate the  results based on a four-point initial calibration
              for the specific compound that saturates.  Secondary ion
              quantitation is only allowed when there are sample
              interferences with the primary quantitation ion. If secondary
              ion quantitation is used, calculate a relative response'factor
              using the area response from the most intense secondary ion
              which is free of sample interferences and document the reasons
              for the use of the secondary ion in the SDG Narrative.

14.4  Calculations

      NOTE:  Unless otherwise stated the area response is that of the primary
      quantitation ion.

      Calculating the relative response factor of the xylenes requires
      special attention.   On capillary columns,  the m- and p-xylene isomers
      coelute.  Therefore,  when calculating the relative response factor in
      the equation below,  use the area response (A^) and concentration (C^)
      of the peak from o-xylene.

      14.4.1  Calculate relative response factors (RRF) for each purgeable
              target compound and the surrogate using Equation D.I.  See
              Table D-3 to associate purgeable target compounds with the
              proper internal standard.  See Table D-4 for primary
              quantitation ions to be used for each purgeable target,
              surrogate, and internal standard compounds.

              EQ. D.I           AX      Cis
                        RRF  -  	  x  	
                                Ais      Cx

              Where:

              AX  - Area response (EIC?) for the compound to be measured.

              Ais - Area response (EICF) for the internal standard.

              cis ~ Concentration of the internal standard.

              GX  — Concentration of the compound to be measured.

      14.4.2  Equation D.2 is the general formula for standard deviation  (SD)
              for a statistically small set of values.
              EQ. D.2.
                                 n-1
                                     VOA D-21                          6/91

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         SO - Standard deviation for a  set of values.
         K£ - Value.

         x  - Mean value.
         n  - Number  of values.

14.4.3   Calculate the percent relative standard deviation  (% RSD)  of
         BKF values for each purgeable  target and surrogate compound
         over the  initial  calibration range using Equation  D.3  in
         conjunction  with  Equation D.2.

         EQ-  D.3   %RSD .  SDm*  x loo
                             x

         Where:

         %RSD - Percent relative standard deviation.

         SDssr - Standard deviation of initial calibration response
               factors (per compound).

         From EQ.  0.2:

         X£ - RRF^ -  Relative response  factors  from  initial calibration
                   standard (per compound).
        x - RRF - Mean of  initial calibration response
                  factors  (per compound).

14.4.4  Equation D.4  is the general  formula for  the mean of  a  set  of
        values.

        EQ. D.4
                      n

                x -   	
        Xi - Value.

        x  - Mean value.
        n  — Number of values.

14.4.5  Calculate the mean of the relative retention times  (RRT)  for
        each purgeable target and surrogate compound over the  initial
        calibration range using Equation 0.4  and Equation 0.5.

                  EQ. 0.5                  RTC
                                   RRT -  	
                                           RTis

        RTC - Retention time for the purgeable  target and surrogate
        compound.

                               VOA D-22                          6/91

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               RT^g- Retention time for the internal standard.

               From EQ D.4:

               X£ - RRl£ - Relative retention times  for the  purgeable target
                          or surrogate compound for  each initial calibration
                          standard.
               x - RRT - Mean relative retention time  (per compound) .

               n - Number of values.

      14.4.6   Calculate the area response (Y)  mean for each internal  standard
               over the initial calibration range using Equation D.4.
               Where:
                        — Area responses  for the  internal  standard in each
                        of the calibration standards.
               x - Y - Area response mean.

               n - Number of values.

      14.4.7   Calculate the mean of the  absolute retention  times  (RT)  for
               each  internal standard over  the  initial calibration range  using
               Equation D.4.

               Where:

               xi ~  RTi - Retention  times for the internal standard in  each
                          of the  calibration standards.
              x - RT - Mean absolute  retention  time.

              n — Number of values.

14.5  Technical Acceptance Criteria For Initial Calibration

      14 . 5 . 1  All initial calibration standards must be analyzed  at  the
              concentration levels described  in Section 14.3, and at the
              frequency described in  Section  14.2 on a GC/MS system  meeting
              the BFB technical acceptance criteria.

      14.5.2  The relative response factor (RRF) at each calibration
              concentration for each  purgeable  target and surrogate  compound
              that has a required minimum response factor value must be
              greater than or equal to the compound's minimum acceptable
              response factor listed  in Table D-5.
                                     VOA D-23                          6/91

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      14.S.3   The  %RSD  for  each  target or surrogate compound listed  in Table
               D-5  must  be less than or equal to that value listed.

      14.5.4   Up to  two compounds may fail the criteria listed in paragraphs
               14.5.2 and 14.5.3  and still meet the minimum response  factor
               and  %RSD  requirements.  However, these compounds must  have  a
               M-tpfntiim RRF greater than or equal to 0.010, and the %RSD must
               be less than  or equal to 40.0%.

      14.5.5   The  relative  retention tine (RUT) at each calibration  level
               must be within +0.06 RRT units of mean relative retention time
               (RRT)  over all the calibration levels for each purgeable target
               compound  and  the surrogate.

      14.5.6   The  area  response  (Y) for each internal standard compound in
               each calibration standard must be within the inclusive range of
               +40.0  percent of the mean area response (7) of the internal
               standard  in all of the calibration standards.

      14.5.7   The  retention time (RT) shift for each internal standard at
               each calibration level must be less than or equal to +0.33
               minutes (20.0 seconds) from the mean retention time (RT) over
               all  calibration levels for each internal standard.

14.6  Corrective Action

      14.6.1   If the initial calibration technical acceptance criteria are
               not  met,  inspect the system for problems.  It may be necessary
               to clean  the  ion source, change the column, service the purge
               and  trap  device or take other corrective actions to achieve the
               technical acceptance criteria.

      14.6.2   Initial calibration technical acceptance criteria MUST be met
               before any samples or required blanks are analyzed.  Any
               samples (including LCS and FES) or required blanks analyzed
               when initial  calibration technical acceptance criteria have not
               been met  will require reanalysis at no additional cost.

15.   CONTINUING CALIBRATION

15.1  Summary  - Prior to the analysis of samples and required blanks  and
      after BFB and initial calibration acceptance criteria have been met,
      each GC/MS system must be routinely checked by analyzing a continuing
      calibration standard containing all the purgeable target and surrogate
      compounds to ensure that the instrument continues to meet the
      instrument sensitivity and linearity requirements of the method.

15.2  Frequency

      15.2.1   Each GC/MS used for analysis must be calibrated  once  per each
               twelve (12) hour time period of operation.  The  twelve hour
               time period begins with the injection of BFB.
                                     VOA D-24                          6/91

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       15.2.2   If time remains in the 12 hour time  period after meeting the
               technical acceptance criteria for the  initial  calibration,
               samples may be analyzed.   It is not  necessary  to analyze a
               continuing calibration standard, if  the initial calibration
               standard that is the same concentration as the continuing
               calibration standard meets the continuing calibration technical
               acceptance criteria.  A method blank is required.   Quantify all
               sample results against the initial calibration standard -that is
               the same concentration as the continuing calibration standard
               (5 ug/L for non-ketones,  25 ug/L for ketones).

15.3   Procedure

       15.3.1   Set up the purge and trap GC/MS system per the requirements of
               Section III, Part A.

       15.3.2   All samples, required blanks,  and standard/spiking solutions
               must be allowed to warm to ambient temperature (approximately 1
               hour) before analysis.

       15.3.3   Tune the GC/MS system to  meet the BFB  technical acceptance
               criteria in Section 11.

       15.3.4   Prepare a working continuing calibration standard solution
               containing all the purgeable target  and surrogate compounds
               using the procedure listed in Section  7.4.2.   The concentration
               for the non-ketones and the surrogate  compound will be 5 ug/L.
               The concentration of the  ketones will  be 25 ug/L.

       15.3.5   Prepare the aqueous continuing calibration solution by adding
               25 uL of the working calibration standard to reagent water  as
               described in Paragraph 7.5.

      15.3.6   Add 10 uL of internal standard spiking solution (prepared as
               described in Paragraph 7.4.3)  to the 25 mL syringe or
               volumetric flask containing the continuing calibration
               standard.   Analyze the continuing calibration  standard,
               according to Section 17.

15.4  Calculations

      15.4.1   Calculate a relative response  factor (RRF)  for each target  and
               surrogate compound according to Section 14.4.1.

      15.4.2   Calculate the percent difference between the continuing
               calibration relative response  factor and the most recent
               initial calibration mean  relative response factor for each
               purgeable  target and surrogate compound using  Equation D.6.
                                               RRFj - RRF
                 EQ D. 6   % D RHF  -           	  x 100
                                     VGA D-25                          6/91

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               Where:

               %  DBBF ~ Percent difference between relative
                        response  factors.

               RRF - Relative  response  factor from current continuing
                     calibration  standard.
                   - Mean  relative response  factor froa the most recent
                     initial calibration.

15.5  Technical Acceptance Criteria For Continuing Calibration

      15.5.1  The concentration of the volatile organic target and surrogate
              compounds  in the continuing calibration standard must be 5.0
              ug/L for non-ketones and 25.0  ug/L for ketones.  The continuing
              calibration  standard must be analyzed at the frequency
              described  in Section 15.2 on a GC/MS system meeting the BFB and
              the initial  calibration technical acceptance criteria.

      15.5.2  The relative response factor for each purgeable target and
              surrogate  compound that has a  required Tinlmii response factor
              value must be greater than or  equal to the compound's «ifTri"M"»
              acceptable response factor listed in Table D-5.

      15.5.3  The relative response factor percent difference for each
              purgeable  target and surrogate compound listed in Table D-5
              must be less than or equal to  that value listed.

      15.5.4  Up to two  compounds may fail the requirements-listed in
              paragraph  15.5.2 and 15.5.3 and still meet the minimum response
              factor criteria and percent difference criteria.  However,
              these compounds must have a mf.Mai'^ response factor greater
              than or equal to 0.010 and the percent difference must be
              within the inclusive range of  ±40.0%.

15.6  Corrective Action

      15.6.1  If the continuing calibration  technical acceptance criteria are
              not met, recalibrate the GC/MS instrument according to Section
              14.  It may  be necessary to clean the ion source, change the
              column or  take other corrective actions to achieve the
              continuing calibration technical acceptance criteria.

      15.6.2  Continuing calibration technical acceptance criteria MUST  be
              met before any samples (including LCS and FES) or required
              blanks are analyzed.  Any samples, or required blanks analyzed
              when continuing calibration technical acceptance criteria  have
              not been met will require reanalysis at no additional cost.
                                     VOA D-26                          6/91

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                         SECTION 17
SAMPLE ANALYSIS AND COMPOUND IDENTIFICATION AND QUANTITATION
                             VOA D-27                          6/91

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16.   SUMMARY

16.1  This method is designed for analysis of samples that contain low
      concentrations of the target compounds listed in Exhibit C.   It is
      expected that the samples will come from drinking water and
      well/ground water type sources around Superfund sites.   If,  upon
      inspection of a sample, the Contractor suspects that the sample is
      not amenable to this method, contact SMO for instructions.

16.2  Before samples or required blanks may be analyzed, the purge and
      trap, and the GC/MS instrument must meet the BFB (Section 11),
      initial calibration (Section 14)  and continuing calibration (Section
      15) technical acceptance criteria listed.  Also, before samples may
      be analyzed, a method blank must  be analyzed which meets blank
      technical acceptance criteria listed in Section 26.  All samples,
      required blanks, and calibration  standards must be analyzed under the
      same instrument conditions.  All  samples, required blanks,  and
      standard/spiking solutions must be allowed to warm to ambient
      temperature (approximately 1 hour) before analysis.

17.   PROCEDURE

17.1  Set up the purge and trap GC/MS system per the requirements of
      Section III, Part A.

17.2  Remove the plunger from a 25 mL syringe that has a closed syringe
      valve attached.  Open the sample  or standard container which has been
      allowed to come to ambient temperature (approximately 1 hour), and
      carefully decant the sample into  the syringe barrel to just short of
      overflowing. Replace the syringe  plunger and compress the sample.
      Invert the syringe, open the syringe valve, and vent any residual air
      while adjusting the sample volume to 25.0 mL.  This process of taking
      an aliquot destroys the validity  of the sample for future analysis,
      unless the excess sample is immediately transferred to a smaller vial
      with zero headspace and stored at 4*C (±2*C).

      NOTE:  A smaller sample volume (5 to 25 mL) may be analyzed but the
      CROL and all technical acceptance criteria must oe met.  The same
      sample volume must be used for all standards, samples,  and blanks
      that apply to a single SDG.

17.3  Once the sample allquots have been taken from the VOA vial, the pH of
      the water sample must be determined.  The purpose of the pH
      determination is to ensure that all VOA samples were acidified in the
      field.  Test the pH by placing one or two drops of sample on  the pH
      paper (do not add pH paper to the vial).  Record the pH of each
      sample and report these data in the SDG Narrative, following  the
      instructions in Exhibit B.  No pH adjustment is to be performed by
      the Contractor.

17.4  Add 10.0 uL of the internal standard spiking solution and 10.0 uL of
      the surrogate standard solution through the valve bore of the
      syringe, then close the valve.  Invert the syringe three times.
                                     VOA D-28                          6/91

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17.5  Attach  the valve assembly on the syringe to the valve on the sample
      purger.  Open the valves and inject the sample into the purging
      chamber.

17.6  Close both valves and purge the sample for 11.0 (±0.1) minutes at
      ambient temperature.

17.7  Sample Desorption

      After the 11 minute purge, attach the trap to the gas chromatograph,
      adjust the purge and trap system to the desorb mode, initiate the
      temperature program sequence of the gas chromatograph and start data
      acquisition.  Introduce the trapped material to the GC column by
      rapidly heating the trap to 180*C while backflushing the trap with
      inert gas at 15 mL/oin for 4.0 +0.1 min.  While the trapped material
      is being introduced into the gas chromatograph, empty the sample
      purger and rinse it with reagent water. For samples containing large
      amounts of water soluble materials, suspended solids, high boiling
      compounds or high purgeable levels, it may be necessary to wash out
      the sample purger with a detergent solution, rinse it with reagent
      water, and then dry it in a 105*C oven between analyses.

17.8  Trap Reconditioning — After desorbing the sample, recondition the
      trap for a minimum of 7.0 ±0.1 min at 180*C by returning the purge
      and trap system to purge mode.

17.9  Gas Chromatography - Hold the column temperature at 10*C for 1.0 to
      5.0 min, then program at 6C*/min to 160*C and hold until all target
      compounds have eluted.  Note:  Once an initial hold time has been
      chosen and the GC operating conditions optimized, the same GC
      condition must be used for the analysis.

18.   TERMINATION OP DATA ACQUISITION

      When all purgeable target compounds have eluted from the GC,
      terminate the MS data acquisition and store data files on the data
      system storage device.  Use appropriate data output software to
      display full range mass spectra and appropriate extracted ion current
      profiles (EICPs).

19.   DILUTIONS

19.1  If the initial analysis of a sample indicates the sample must be
      reanalyzed at a dilution,  the dilution must be made just prior to
      GC/MS analysis of the sample.  Until the diluted sample is in a gas
      tight syringe,  all steps in the dilution procedure must be performed
      without delay.   Secondary ion quantitation is only allowed when there
      are sample interferences with the primary quantitation ion, not when
      saturation occurs.   If secondary ion quantitation is used, calculate
      a relative response factor using the area response (EICP) from the
      most intense secondary ion which is free of sample interferences, and
      document the reasons in the SOG Narrative.
                                     VOA D-29                          6/91

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19.2  All dilutions must keep the response of the target compounds that
      required dilution in the upper half of the initial calibration range.

19.3  Dilutions are made in volumetric flasks or in a 25 mL "Luerlock"
      syringe.

      19.3.1  To dilute the sample in a volumetric flask, use the following
              procedure:

              19.3.1.1   Select the volumetric flask that will allow for
                         the necessary dilution (25 mL to 100 mL).

              19.3.1.2   Calculate the approximate volume of reagent water
                         which will be added to the volumetric flask
                         selected and add slightly less than this quantity
                         of reagent water to the flask.

              19.3.1.3   Inject the proper sample aliquot from a syringe
                         into the volumetric flask.  Aliquots of less than
                         1 mL are prohibited.  Dilute the flask to the mark
                         with reagent water.  Cap the flask, invert, and
                         shake three times.

              19.3.1.4   Fill a 25.0 mL syringe with the diluted sample and
                         analyze according to Section 17.

      19.3.2  To dilute the sample in a 25 mL syringe, use the following
              procedure:

              19.3.2.1   Calculate the volume of the reagent water
                         necessary for the dilution.  The final volume of
                         the diluted sample should be 25 mL.

              19.3.2.2   Close the syringe valve, remove the plunger from
                         the syringe barrel, and pour reagent water into
                         the syringe barrel to just short of overflowing.

              19.3.2.3   Replace the syringe plunger and compress the
                         water.

              19.3.2.4   Invert the syringe, open the syringe valve, and
                         vent any residual air.  Adjust the water volume to
                         the desired amount.

              19.3.2.5   Adjust the plunger to the 25 mL mark to
                         accommodate the sample aliquot.  Inject the proper
                         aliquot of sample from another syringe through the
                         valve bore of the 25 mL syringe.  Close the valve
                         and invert three times.

              19.3.2.6   Analyze according to Sections 17.4 to 18.
                                    VOA D-30                          6/91

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20.   IDENTIFICATION OP TARGET COMPOUNDS

20.1  The compounds listed in the Target Compound List (TCL),  Exhibit C,
      shall be identified by an analyst competent in the interpretation of
      mass spectra by comparison of the sample mass spectrum to the mass
      spectrum of a standard of the suspected compound.   Two criteria must
      be satisfied to verify the identifications:  (1) elution of the
      sample compound at the same GC relative retention time as the
      standard compound, and (2) correspondence of the sample compound and
      standard compound mass spectra.

20.2  For establishing correspondence of the GC relative retention time
      (RRT), the sample compound RRT must be within ±0.06 RRT units of the
      RRT of the standard compound in the continuing calibration analysis.
      If co-elution of interfering compounds prohibits accurate assignment
      of the sample compound RRT from the extracted ion current profile for
      the primary ion, the RRT must be assigned by using the total ion
      chromatogram.

20.3  For comparison of standard and sample compound mass spectra, mass
      spectra obtained on the Contractor's GC/MS are required. Once
      obtained, these standard spectra may be used for identification
      purposes, only if the Contractor's GC/MS meets the BFB technical
      acceptance criteria.  These standard spectra may be obtained from the
      continuing calibration analysis that was also used to obtain the
      reference relative retention times.

20.4  The guidelines for qualitative verification by comparison of mass
      spectra are as follows:

      20.4.1  All  ions present  in the standard mass spectra at a  relative
              intensity greater than 25 percent  (most abundant ion in  the
              spectrum equals 100 percent) should be present  in the  sample
              spectrum.

      20.4.2  The  relative intensities of ions specified in Section  20.4.1
              must agree within ±20  percent between the standard  and sample
              spectra.  (Example:  For an ion with an abundance of 50
              percent in the standard spectra, the corresponding  sample
              abundance must be between 30 and 70 percent).

      20.4.3  Ions greater than 25 percent in the sample spectrum but  not
              present in the standard spectrum must be considered and
              accounted for by  the analyst making the comparison.  The
              verification process should FAVOR  FALSE POSITIVES.  All
              compounds meeting the  identification criteria must  be
              reported with their spectra.

      20.4.4  If a compound cannot be verified by all of the  spectral
              identification criteria listed in  Sections 20.4.1 - 20.4.3,
              but  in  the technical judgment of the mass spectral
              interpretation specialist, the identification is correct,
              then the Contractor shall report that identification and
              proceed with quantitation.
                                     VGA D-31                          6/91

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21.   IDEKTIPICATION OP NON-TARGET COMPOUNDS

21.1  A library search shall be executed for non-target sample compounds
      for the purpose of tentative identification.   For this purpose,  the
      most recent release of the National Institute of Standards and
      Technology Mass Spectral Library shall be used.

21.2  Up to ten (10) non-internal standard and non-surrogate organic  '
      compounds of greatest apparent concentration not listed in Exhibit C
      for the purgeable organic fraction shall be tentatively identified
      via a forward search of the NIST Mass Spectral Library. (Compounds
      with a peak area response less than 40 percent of the peak area
      response of the best matched internal standard are not required to be
      searched in this fashion).   Only after visual comparison of sample
      spectra with the nearest library searches will the mass spectral
      interpretation specialist assign a tentative identification.
      Computer generated library search must not use normalization routines
      if those routines would misrepresent the library or unknown spectra
      when compared to each other.

21.3  Guidelines for making tentative identification:

      21.3.1  All ions present in the standard mass spectra at a relative
              intensity greater than 25 percent  (most abundant ion in the
              spectrum equals 100 percent) must be present in the sample
              spectrum.

      21.3.2  The relative intensities of the major ions specified in
              Section 20.4.1 must agree within ±20 percent between the
              standard and sample spectra.   (Example: For an ion with an
              abundance of SO percent in the standard spectra, the
              corresponding sample ion abundance must be between 30 and 70
              percent.)

      21.3.3  Molecular ions present in reference spectrum should be
              present in sample spectrum.

      21.3.4  Ions present in the sample spectrum but not in the reference
              spectrum should be  reviewed for possible background
              contamination or presence of co-eluting compounds.

      21.3.5  Ions present in the reference spectrum but not in the sample
              spectrum should be  reviewed for possible subtraction from the
              sample spectrum because of background contamination or
              co-eluting compounds.  Data system library reduction programs
              can sometimes create these discrepancies.

      21.3.6  Ions greater than 25 percent in the sample spectrum but not
              present in the standard spectrum must be considered and
              accounted for by the analyst making the comparison.  The
              verification process should FAVOR  FALSE POSITIVES.  All
              compounds meeting the identification criteria  must be
              reported with their spectra.
                                     VOA

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      21.3.6   If  in  the technical Judgment of the mass spectral
               interpretation specialist, no valid tentative identification
               can be made, the compound should be reported as unknown.  The
               mass spectral specialist should give additional
               classification of the unknown compound, if possible (e.g.,
               unknown aromatic, unknown hydrocarbon, unknown chlorinated
               compound).  If a probable molecular weight can be
               distinguished, include it.

22.   CALCULATIONS

      NOTE:   Unless otherwise stated the area response is that of the
      extracted ion current profile (EICF)  of the primary quantitation ion.

22.1  Target Compounds

      22.1.1   Calculate target compound and surrogate concentrations using
               Equation D.7.

                   EQ.  D.7  Concentration in ug/L -   (Ax)(Is)(Df)
                                                     (Aia)(RRF)(V0)

              Where:

              AX  - Area response (EICF) for the compound to be measured.
                    The primary quantitation ions for the target, internal
                    standards, and the surrogate compounds are listed in
                    Table D-4.

              A£S - Area response (EICF) for the internal standard.
                    The target compounds are listed with their associated
                    internal standards in Table D-3.

              Is  - Amount of internal standard added in nanograms (ng).

              RRF - The relative response factor from the continuing
                    calibration standard.

              V0  - Total volume of water purged, in milliliters (mL).

              Df  - Dilution factor.  The dilution factor for analysis of
                    water samples for volatiles by this method is defined
                    as the ratio of the number of milliliters (mL) of water
                    purged (i.e.,  V0 above) to the number of mL of the
                    original water sample used for purging.  For example,
                    if 12.5 mL of sample is diluted to 25.0 mL with reagent
                    water and purged, Df-25.0 mL/12.5 mL-2.0.  If no
                    dilution is performed,  Df-1.0.

      22.1.2   When target compounds are below contract required
              quantitation limits (CRQL) but the spectra meet the
              identification criteria,  report the concentration wirh a "J".
              For example, if the CRQL is 1.0 ug/L and a concentration of
                                    VQA D-33                          6/91

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               0.5 ug/L is calculated,  report as "0.5 J".   Report ALL sample
               concentration data as UNCORRECTED for blanks.

       22.1.3   Xylenes (o-,  a-,  and p-  isomers)  are to be  reported as
               xylenes (total).   Because m-  and p-xylene isomers coelute on
               capillary columns, special attention must be given to the
               quantitation of the xylenes.   The relative  response factor
               (RRF) is based on the peak that represents  the single isomer
               on the GC column using o-xylene on capillary columns.  In
               quantitating sample concentrations,  use the areas on both
               peaks and the RRF.  The  areas of the two peaks may be summed
               and the concentration determined, or the concentration
               represented by each of the two peaks may be determined
               separately, and then summed.

       22.1.4   The stereoisomers, trans-l,2-dichloroethene and cis-
               1,2-dichloroethene,  are  to be reported separately.

22.2   Non-Target  Compounds

       Equation D.7  is also used  for calculating non-target compound
       concentrations.  Total  area counts  (or peak heights) from the total
       ion chroma to grams  (RIG) are to be used for both  the non-target
       compound to be measured (Ax) and the  internal standard (A^s).
      Associate the nearest internal standard free of  interferences with
       the non-target compound to be measured.   A relative response  factor
       (RRF) of 1.0  is to  be assumed.  The value from this quantitation
       shall be qualified  as estimated  ("J").  This estimated concentration
      must be calculated  for  all tentatively identified compounds as well
       as those identified as  unknowns.  Do  not  report  any non-target
       compound whose concentration is less  than 2.0 ug/L  (peak area
       response is less than 40%  of the peak area response of the nearest
       internal standard).

22.3   Surrogates

      Calculate the surrogate percent recovery  using Equation  D.8.

                                             Qd
      EQ. D.8  Surrogate  Percent Recovery - 	  x  100
                                             Qa

      Where:

      Q(l - Quantity determined by analysis.

      Qa - Quantity added to  sample/blank.

22.4  Internal Standards

      22.4.1  Calculate  the  percent area response change  (%ARC) between the
              sample/blank analysis and the most recent continuing
              calibration standard analysis for each of the internal
              standards  using Equation D.9.
                                     VOA D-34                          6/91

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              EQ. D.9  % ARC  -  AS  ' ^   x 100
                                    AC

              Where:

              % ARC - Percent area response  change.

                  As - Area response of  the internal  standard (EICF)  in the
                       sample/blank analysis.

                  AC - Area response of  the internal  standard (EICP)  in the
                       most recent  continuing calibration standard.

      22.4.2  Calculate  the retention time shift  (RTS)  between the
              sample/blank analysis and the  most  recent continuing
              calibration standard analysis  for each of the  internal
              standards  using Equation  D.IO.

                     EQ. D.IO       RTS - RTS - RTC

              Where:

              RTS - Retention time shift.

              RTS - Retention time of the internal standard  in a
                    sample/blank.

              RTe - Retention time of the internal standard  in
                    the  most recent continuing calibration standard.

23.   TECHNICAL ACCEPTANCE CRITERIA FOR SAMPLE ANALYSIS

23.1  The sample must be analyzed on a GC/MS system meeting the BFB,
      initial calibration, continuing calibration, and blank technical
      acceptance criteria.

23.2  The sample must be analyzed within the contract holding times.  The
      sample must have an LCS associated with it meeting the LCS technical
      acceptance criteria.  The sample must have a FES associated with ic
      meeting the FES technical acceptance criteria.

23.3  The surrogate compound percent recovery must be between 80 and 120
      percent inclusive.

23.4  The difference of the area response between the sample and the most
      recent continuing calibration standard analysis for each of the
      internal standards must be within the inclusive range of +40.0
      percent of the continuing calibration standard.

23.5  The retention time shift between the sample and the most recent
      continuing calibration standard analysis for each of the internal
      standards  must be within ±0.33 minutes (20.0 seconds).
                                     VOA D-35                          6/91

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 23.6   Excluding  those  ions  in the solvent front, no ion may saturate the
       detector.  No  target  compound concentration may exceed the upper
       limit of the initial  calibration range unless a more dilute aliquot
       of the sample  is also analyzed according to the procedures in Section
       19.

 23.7   The Contractor must demonstrate that there is no carryover from a
       contaminated sample before data from subsequent analyses may be
       submitted.  After a sample that contains a target compound at a level
       exceeding  the  initial calibration range, or a non-target compound at
       a concentration greater than 100 ug/L, or saturated ions from a
       compound (excluding the compound peaks in the solvent front), the
       Contractor must either:

       23.7.1  Analyze  an instrument blank immediately after  the
              contaminated  sample.  If an autosampler is used, an
              instrument blank must also  be  analyzed using the same purge
              inlet  that was  used for the contaminated sample.  The
              instrument blanks must meet the  technical acceptance criteria
              for blank  analysis  (Section 26.4), or

       23.7.2  Monitor  the sample analyzed immediately after  the
              contaminated  sample for all compounds that were in the
              contaminated  sample and that exceeded the limits above.   The
              maximum  contamination criteria are as follows:  the sample
              must not contain a concentration above the CRQL for the
              target compounds or above 2 ug/L for the non- target compounds
              that exceeded the limits in the  contaminated sample.  If  an
              autosampler is  used, the next  sample analyzed  using the same
              purge  inlet that was used for  the contaminated sample also
              must meet  the maximum contamination criteria.

24.   COMtgUTlVH ACTION

24.1  If the technical acceptance criteria for the internal standards and
      surrogate compound are not met,  check calculations,  internal standard
      solutions and  instrument performance.   It may be necessary to bake-
      out the system to remove the water from the purge and trap transfer
      lines of the trap,  to recalibrate the instrument,  or take other
      corrective action procedures to meet the technical acceptance
      criteria.

24.2  If the Contractor needs to analyze more than one (1)  sample dilution
      other than the original analysis to have all the target compounds
      within the initial calibration range (excluding the compound peaks in
      the solvent front), contact SMO.   SMO will contact the Region for
      instructions.

24.3  All samples to be reported must meet the maximum contamination
      criteria in Section 23.7.  If any sample fails to meet these
      criteria,  each subsequent analysis must be checked for cross
      contamination.   The analytical system is considered contaminated
      until a sample has been analyzed that meets the maximum contamination
                                     W)A n.Tfi                          A/01

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      criteria or an instrument blank has been analyzed that meets the
      technical acceptance criteria for blanks.

24.4  Sample technical acceptance criteria MUST be met before data are
      reported.  Samples contaminated from laboratory sources or any
      samples not meeting the sample technical acceptance criteria will
      require reanalysis at no additional cost.

24.5  Sample reruns performed as a result of suspected matrix interference
      beyond the scope of the method will be evaluated on a case-by-case
      basis for payment purposes by SMO.

25.   [This paragraph has been intentionally left blank and has been
      reserved.]
                                     VOA D-37                          6/91

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                    SECTION V
SAMPLE QUALITY CONTROL PROCEDURES AND REQUIREMENTS
                        VOA D-38                          6/91

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26.   BLANK ANALYSIS

26.1  Summary

      There are three different types of blanks required by this method.

      26.1.1  Method Blank -  25 mL of reagent water spiked with 10.0 ul
              internal  standard and  10.0 ul surrogate solution, and carried
              through the  entire analytical scheme.  The method blank is
              analyzed  Immediately following the continuing calibration
              standard  and before  any samples are analyzed.  The method
              blank  must be analyzed immediately after the initial
              calibration  sequence if samples are analyzed before the 12
              hour time period expires.  The method blank measures reagent
              and system contamination.

      26.1.2  Storage Blank - Upon receipt of the first samples from a
              Sample Delivery Group, two-40 mL screw cap VOA vials with a
              FIFE-faced silicon septum are filled with reagent water (80
              mL  total).   The vials  are stored under the same conditions as
              the samples  in  the Sample Delivery Group.  A 25.0 mL aliquot
              of  this reagent water  is spiked with a 10.0 uL internal
              standard  and 10.0 uL of surrogate solution and analyzed after
              all samples  in  the Sample Delivery Group have been analyzed.
              The storage  blank indicates whether contamination may have
              occurred  during storage of samples.

      26.1.3  Instrument Blank - 25  mL of reagent water spiked with 10.0 uL
              of  internal  and 10.0 uL of surrogate solution carried through
              the entire analytical  scheme.  Instrument blanks are analyzed
              after  a sample/dilution which contains a target compound at a
              concentration greater  than 25 ug/L (ketones 125 ug/L) or a
              non-target compound  at a concentration greater than 100 ug/L
              or  saturated ions from a compound (excluding the compound
              peaks  in  the solvent front).  The results from instrument
              blank  analysis  indicate whether there is contamination from a
              previous  sample.

26.2  Frequency

      26.2.1  The method blank must  be analyzed after the continuing
              calibration  standard and before any samples or storage blanks
              are analyzed.   The method blank must be analyzed after the
              initial calibration  sequence if samples are analyzed before
              the 12 hour  time period expires.  A method blank must be
              analyzed  in  each 12-hour time period in which samples,
              including LCS,  FES and storage blanks from an SDG are
              analyzed.

      26.2.2  Storage blanks  must  be analyzed once per Sample Delivery
              Group, after all of  the samples have been analyzed.

      26.2.3  The Contractor must  demonstrate that there is no carryover
              from contaminated samples before data from subsequent
                                     VOA D-39                          6/91

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               analyses may be  used.  Samples may contain target compounds
               at  levels  exceeding  the  initial calibration range (25 ug/L
               for non-ketones,  125 ug/L  for ketones) or non-target
               compounds  at concentrations greater than 100 ug/L. or ions
               from a compound  that saturate the detector (excluding the
               compound peaks in the solvent front).  An instrument blank
               must be analyzed immediately after the contaminated sample
               (also in the same injection port if an autosampler is used)
               or  a sample  that meets the m^»^i««» contamination criteria in
               Section 23.7 must be analyzed.  For these purposes, if the
               instrument blank meets the technical acceptance criteria for
               blank analysis or the sample meets the MX*™"!! contamination
               criteria,  the system is  considered to be uncontaminated.  If
               the instrument blank or  sample does not meet the criteria
               (i.e.,  is  contaminated), the system must be decontaminated.
               Until an instrument  blank  meets the blank technical
               acceptance criteria  or a sample meets the matimm
               contamination criteria (Section 23.7), any samples analyzed
               since the  original contaminated sample will require
               reanalysis at no additional expense.

26.3  Procedure

      Prepare and analyze the blanks and calculate results  according to
      Sections 17 through 22.

26.4  Technical Acceptance Criteria For Blank Analysis

      26.4.1   All blanks must be analyzed on a GC/MS system meeting the
               BFB,  initial calibration,  and continuing calibration
               technical  acceptance criteria and at the frequency described
               in  Section 26.2.

      26.4.2   The storage  blank must be  analyzed on a GC/MS system chat
               also  meets the technical acceptance criteria for the method
               blank.

      26.4.3   Surrogate  compound recovery in the blank must be between 80
               and 120 percent  inclusive.

      26.4.4   The difference of the area response between the blank and the
               most  recent  continuing calibration standard analysis for each
               of  the  internal  standards  must be within the inclusive range
               of  ±40.0 percent  of  the  response in the continuing
               calibration  standard.

      26.4.5   The retention time shift between the blank and the most
               recent continuing calibration standard analysis for each of
               the internal standards must be less than or equal to ±0.33
              minutes (20.0 seconds).

      26.4.6  The concentration of the target compounds in the blank must
              be  less than the  CRQL for  each target compound. The
                                         n./.n

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               concentration  of non- target compounds  in  the blank must be
               less  than 2.0  ug/L.

26.5  Corrective Action

      26.5.1   It  is the Contractor's responsibility  to  ensure  that method
               interferences  caused by contaminants in solvents, reagents,
               glassware,  laboratory air and other sample storage and '
               processing hardware  that lead to discrete artifacts and/or
               elevated baselines in gas chromatograns be eliminated.  If a
               Contractor's blanks  exceed the criteria in Paragraph 26.4.6,
               the Contractor must  consider the analytical system to be out
               of  control.  The source of the contamination must be
               investigated and appropriate corrective measures MUST be
               taken and documented before further sample analysis proceeds.

      26.5.2   Any method blank or  instrument blank that fails  to meet the
               technical acceptance criteria must be  reanalyzed at no
               additional cost.  Further, all samples processed within the
               same  12-hour time period with a method blank or  instrument
               blank that does  not  meet the blank technical acceptance
               criteria will  require reanalysis at no additional cost.
               Mote:   Storage blank data must be retained by  the Contractor
               and be made available for inspection during the  on- site
               laboratory evaluation.

27.   LABORATORY CONTROL
27 . 1  Summary
      The LCS is an internal laboratory quality control sample designed to
      assess (on an SDG-by-SDG basis) the capability of the contractor to
      perform the analytical method listed in this Exhibit.
27 . 2  Frequency
      The LCS must be prepared, analyzed, and reported once per Sample
      Delivery Group.  The LCS must be prepared and analyzed concurrently
      with the samples in the SDG using the same instrumentation as the
      samples in the SDG.
27 . 3  Procedure
      27.3.1  Prepare  the LCS using  the procedure described in Section 17 .
              Spike 25 mL of reagent water with 10.0 uL of  LCS spiking
              solution (see Paragraph 7.4.5), 10.0 uL of internal  standard,
              and 10.0 uL of surrogate solution.

      27.3.2  Analyze  the LCS as described in Sections  17 to 22.
                                     VOA D-41                          6/91

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27.4  Calculations

      27.4.1  Calculate  individual compound recoveries of the LCS using
              Equation D.8, substicuting LCS percent recovery for surrogate
              percent recovery.

      27.4.2  See Section 22 for equations necessary for other
              calculations.

27.5  Technical Acceptance Criteria For Laboratory Control Sample Analysis

      27.5.1  The LCS oust be analyzed on a GC/MS system meeting the BFB,
              initial calibration, continuing calibration, and blank
              technical  acceptance criteria at the frequency described in
              Section 27.2.

      27.5.2  The LCS oust be prepared as described in Paragraph 27.3.

      27.5.3  The LCS must be prepared and analyzed with a method blank
              that meets the blank technical acceptance criteria.

      27.5.4  Surrogate compound recovery in the LCS must be between 80 and
              120 percent inclusive.

      27.5.5  The area response change between the LCS and .the most recent
              continuing calibration standard analysis for each of the
              internal standards must be within the inclusive range of
              ±40.0 percent.

      27.5.6  The retention time shift between the LCS and the most recent
              continuing calibration standard analysis for each of the
              internal standards must be within ±0.33 minutes (20.0
              seconds).

      27.5.7  The percent recovery for each of the compounds in the LCS
              must be within the recovery limits listed in Table D-6.

                              TABLE 0-6

                                                     Percent
            Compound                              Recovery Limits

            Vinyl chloride60-140
            1,2-Dichloroethane                         60-140
            Carbon tetrachloride                       60-140
            1,2-Dichloropropane          '              60-140
            Trichloroethene                             60-140
            1,1,2-Trichloroethane                      60-140
            Benzene                                    60-140
            cis-l,3-Dichloropropene                    60-140
            Bromoform                                  60-140
            Tetrachloroethene                          60-140
            1,2-Dibromoethane                          60-140
            1,4-Dichlorobenzene                        60-140
                                     wu

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      NOTE:  The recovery limits for any of the compounds listed above may
      be expanded ac any time during the period of performance if SMO
      determines that the limits are too restrictive.

27.6  Corrective Action

      27.6.1  If the LCS technical  acceptance criteria for the  internal
              standards and  surrogate are not met, check calculations,
              internal standard and surrogate solutions, and  instrument
              performance.   It  may  be necessary to recalibrate  the
              instrument or  take other corrective action procedures  to meet
              the internal standard and surrogate criteria.

      27.6.2  The laboratory may not submit data from an SDG  until the LCS
              technical acceptance  criteria are met.  LCS contamination
              from  laboratory sources or any LCS not meeting  the  criteria
              will  require reanalysis of the LCS at  no additional cost.

      27.6.3  Further, all samples  in the SDG prepared and analyzed  with  an
              LCS that does  not meet the LCS technical acceptance criteria
              will  also require reanalysis at no additional cost.  Any LCS
              failing to meet these technical acceptance criteria must be
              reanalyzed at  no  additional cost.

28.    PERFORMANCE EVALUATION SAMPT.g (PES^

28.1  Summary

      The PES is an external laboratory quality control  sample prepared and
      designed to assess (on an SDG-by-SDG basis) the capability of  the
      Contractor to perform the analytical method listed in this Exhibit.

28.2  Frequency

      The Contractor must analyze and report the PES once per SDG, if
      available.  The PES must be prepared and analyzed  concurrently with
      the samples in the SDG using  the same instrumentation as  the samples
      in the SDG.

28.3  Procedure

      28.3.1  The PES will be received  either as an  ampulated extract or  as
              a full volume  sample. If received as  an ampulated extract,
              the Contractor will receive instructions concerning the
              dilution procedure to bring the extract to full volume prior
              to preparation and analysis of the PES.

      28.3.2  Prepare the PES for analysis using the procedure described in
              Section 17.  Add  10.0 uL  of internal standard  and 10.0 uL of
              surrogate solution to the aqueous PES. Analyze the PES as
              described in Sections 17  to 22.

28.4  Calculations
                                     VOA D-43                          6/91

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      See Section 22 for equations necessary for calculations.

28.5  Technical Acceptance Criteria for the FES

      28.5.1   The  FES  must be  analyzed on a GC/MS system meeting the BFB,
               initial  calibration, continuing calibration, and blanks
               technical acceptance criteria at a frequency described in
               Section  28.2.

      28.5.2   The  FES  must be  prepared according to the procedure in
               Section  28.3.

      28.5.3   The  surrogate  compound percent recovery in the  FES must be
               between  80 and 120 percent inclusive.

      28.5.4   The  difference of the area response between the FES and the
               most  recent  continuing calibration standard analysis for each
               of the internal  standards must be within the inclusive range
               of ±40.0 percent.

      28.5.5   The  retention  time shift between the FES and the most recent
               continuing calibration standard analysis for each of the
               internal standards must be within ±0.33 minutes (20.0
               seconds).

28.6  Corrective Action

      28.6.1   If the FES technical acceptance criteria for the internal
               standards and  the surrogate are not met, check  calculations,
               standard solutions and instrument performance.  It may be
               necessary to recalibrate the instrument or take other
               corrective action procedures to meet the internal standard
               criteria.  Any FES failing to meet these technical acceptance
               criteria must  be reanalyzed at no additional cost.  If
               insufficient FES spiking extract remains or if  insufficient
               full  volume PES  remains, document this in the SDG Narrative
               by stating that  the FES could not be reanalyzed because
               insufficient volume remains.

      28.6.2   In addition  to complying with the PES technical acceptance
               criteria, the  Contractor will be responsible for correctly
               identifying  and  quantifying the compounds included in the
               PES.  SMO will notify the Contractor of unacceptable
               performance.

               Note:  Unacceptable performance for identification and
               quantitation of  compounds is defined as a score less than 75
               percent.

      28.6.3   The PES  technical acceptance criteria MUST be met before
               sample data  are  reported.  Also, the Contractor must
               demonstrate  acceptable performance for compound
               identification and quantitation.
                                     VOA n-4£                          fi/QI

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                                    TABLE D-3
            VOLATILE TARGET COMPOUNDS  AND SURROGATE WITH CORRESPONDING
                       INTERNAL STANDARDS FOR QUANTITATION
 1.4-DIFLUOROBENZENE
CHLOROBENZENE-d5
Acetone
Bromochloromethane
Brooome thane
2-Butanone
Carbon dlsulfide
Chloroe thane
Chloroform
Chloromethane
1,1-Dichloroethane
1,2-Dichloroethane
1,1-Dichloroethene
cis-1,2-Dichloroethene
trans-1,2-Dichloroethene
Methylene chloride
Vinyl chloride
4-Bromo£luorobenzene
Benzene
Bromodichloromethane
Carbon tetrachloride
Chlorobenzene
Dibromochloromethane
1,2-Dibromoethane
1,2-Dichloropropane
cis-1,3-Dichloropropene
trans-1,3-Dichloropropene
Ethylbenzene
2-Hexanone
4-Methy1-2-pentanone
Styrene
1,1,2,2-Tetrachloroethane
Tetrachloroethene
Toluene
1,1,1-Trichloroethane
1,1,2-Trichloroethane
Trichloroethene
Xylenes (total)
1.4-DICHLOROBENZENE-d4
Br onto form
1,2-Dibromo-3-chloropropane
1,2-Dichlorobenzene
1,3-Dichlorobenzene
1,4-Dichlorobenzene
                                       VOA D-45
                            6/91

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                               TABLE  0-4
              PRIHARY QUANTITATION  IONS  (M/Z) AND SECONDARY
                   IONS FOR VOLATILE ORGANIC COMPOUNDS
Volatile
Target
Conroounds
Acetone
Benzene
Bromochlorome thane
Broaodiehlorome thane
Bromoform
Bromome thane
2-Butanone
Carbon dlsulfide
Carbon tetrachloride
Chlorobenzcne
Chloroethane
Chloroform
Chlorome thane
Dlbromochlorome thane
1 , 2 -Dibromo- 3 - chloropropane
1 , 2 -Dibromoe thane
1 , 2 -Dichlorobenzene
1 , 3 -Dichlorobenzene
1 , 4-Dichlorobenzexie
1 , 1-Dichloroe thane
1 , 2-Dichloroethane
1,1- Dichloroethene
cis - 1 , 2 -Dichloroethene
trans -1,2- Dichloroethene
1 , 2-Dichloropropane
cis-1 , 3-Dichloropropene
trans -1,3- Dichloropropene
Ethylbenzene
2-Hexanone
Methylene chloride
4 - Methyl - 2 - pentanone
Styrene
1,1,2, 2 -Tetrachloroechane
Tetrachloroethene
Toluene
1,1, 1-Trichloroe thane
1,1, 2 -Trichloroe thane
Trichloroe thene
Vinyl chloride
Xylenes (total)
SURROGATE COMPOUND AND INTERNAL
4 - Bromo fluorobenzene
Chlorobenzene - d$
l,4-Dichlorobenzene-d4
1 , 4-Difluorobenzene
Primary
Quant i tat ion
Ion
43
78
128
83
173
94
43
76
117
112
64
83
50
129
75
107
146
146
146
63
62
96
96
96
63
75
75
91
43
84
43
104
83
166
91
97
97
95
62
106
STANDARDS :
174
117
152
114
Secondary
Ions
58
_
49,130
85 , 127
175,254
96
72*
78
119
77 , 114
66
85
52
127
155,157
109,188
111,148
111,148
111,148
65,83
98
61,63
61,98
61,98
112
77
77
106
58,57,100
86,49
58 , 100
78
131,85
168,129
92
99,61
83,85,99,132,134
130,132
64
91

95,176
82,119
115,150
63,88
Quantitation of this analyte is based on m/z 43 but m/z 72
must be present in the spectrum.
                                  VOA D-46
6/91

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                                  TABLE D-5
           TECHNICAL ACCEPTANCE CRITERIA FOR INITIAL AND CONTINUING
                  CALIBRATION FOR VOLATILE ORGANIC COMPOUNDS

Volatile                       Minimum               Maximum             Maximum
Compound	RRF	%RSD	%Dlf E

Benzene                           0.500                 30.0              +30.0
Bromochloromethane                0.05                  30.0              +30.0
Bromodichloromethane              0.200                 30.0              +30.0
Bromoform                         0.05                  30.0              +30.0
Bromomethane                      0.100                 30.0              +30.0
Carbon cecrachloride              0.100                 30.0              +30.0
Chlorobenzene                     0.500                 30.0              +30.0
Chloroform                        0.200                 30.0              +30.0
Dibromochloromechane              0.100                 30.0              +30.0
1,2-Dibromoechane                 0.100                 30.0              +30.0
1,2-Dichlorobenzene               0.400                 30.0              +30.0
1,3-Dichlorobenzene               0.600                 30.0              +30.0
1,4-Dichlorobenzene               0.500                 30.0              +30.0
1,1-Dichloroechane                0.200                 30.0              +30.0
1,2-Dichloroechane                0.100                 30.0           _   +30.0
1,1-Dichloroechene                0.100                 30.0              +30.0
cis-1,3-Dichloropropene           0.200                 30.0              +30.0
crans-1,3-Dichloropropene         0.100                 30.0              +30.0
Ethylbenzene                      0.100                 30.0              +30.0
Scyrene                           0.300                 30.0              +30.0
1,1,2,2-Tetrachloroethane         0.100                 30.0              ±30.0
Tetrachloroechene                 0.200                 30.0              +30.0
Toluene                           0.400                 30.0              +30.0
1,1,1-Trichloroethane             0.100                 30.0              +30.0
1,1,2-Trichloroethane             0.100                 30.0              +30.0
Trichloroethene                   0.300                 30.0              +30.0
Vinyl chloride                    0.100                 30.0              +30.0
Xylenes (total)                   0.300                 30.0              +30.0
4-Bromofluorobenzene              0.200                 30.0              +30.0
The following compounds have no maximum %RSD or maximum % Difference
criteria, but must meet a minimum RRF criterion of 0.010:

Carbon disulfide                  trans-1,2-Dichloroethene
Choroethane                       1,2-Dichloropropane
Chloromethane                     Methylene  Chloride
cis-1,2 -Dichloroethene

Note:  At the present time,  the Agency has not set minimum RRF or %RSD
criteria for Acetone, 2-Butanone, 1,2-Dibromo-3-chloropropane, 2-Hexanone and
4-Methyl- 2-pentanone.
                                     VOA D-47                          6/91

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                                 EXHIBIT D
METHOD FOR THE ANALYSIS OF LOW CONCENTRATION WATER FOR SEHT70LATILE ORGANIC
                                 COMPOUNDS
                                    SV D-l                            6/91

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                              Table of Contents
                                                                      Page
SECTION I:    Introduction	SV D-3

SECTION II:
              Part A - Sample/Sample Extract Storage and
                         Holding Times 	SV D-4
              Part B - Equipment and Standards 	SV D-5

SECTION III:  Instrument Quality Control Procedures
                and Requirements
              Part A - Instrument Operating Conditions 	SV D-13
              Part B - Tuning the Mass Spectrometer	SV D-14
              Part C - Calibration of the GC/MS System	SV D-16

SECTION IV:   Sample Preparation, Analysis, and Compound
                Identification and Quantitation	SV D-23

SECTION V:    Sample Quality Control Procedures and
                Requirements 	SV D-33
                                     SV D-2
6/91

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                                   SECTION I
                                 INTRODUCTION
The analytical method that follows is designed to analyze samples containing
low concentrations of the semivolatile compounds listed on the Target
Compound List (TCL) in Exhibit C.  The majority of the samples are expected
to be from drinking water and well/ground water sources around Superfund
sites.  The method is based upon the semivolatile method contained in the CLP
Statement Of Work, "Organic Analysis, Multi-Media, Multi-Concentration by
GO/MS and GC/EC Techniques*, except that a single extraction at a pH 2.0 is
used.  Incorporated in the method are specific requirements to minimize
contamination of the samples from laboratory sources.

Problems have been associated with the following compounds covered by this
method:

o   Oichlorobenzidine  and 4-chloroaniline may be  subject to  oxidative losses
    during solvent concentration.
o   Hexachlorocyclopentadiene is  subject to thermal decomposition in the inlet
    of the gas chromatograph,  chemical  reactions  in acetone  solution, and
    photochemical  decomposition.

o   N-nitrosodiphenylamine decomposes in the gas  chroma to graphic inlet forming
    diphenylamine  and,  consequently, may be detected as diphenylamine.

o   Due to the lower quantitation limits required by this method,  extra
    caution must be exercised when identifying compounds.
                                     SV D-3                            6/91

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                                  SECTION II


PART A - SAMPLE/SAMPLE EXTRACT STORAGE AND HOLDING TIMES

1.    PROCEDURES FOR SAMPT-3 STORAGE

      The samples must be protected from light and refrigerated at 4*C (±2*C)
      from the tine of receipt until 60 days after delivery of a complete
      reconciled data package.  After 60 days the samples may be disposed of
      in a. manner that complies with all applicable regulations.

      Samples must be stored in an atmosphere demonstrated to be free of all
      potential contaminants.

      Samples, sample extracts, and standards must be stored separately.

2.    PROCEDURE FOR SAMPLE EXTRACT STORAGE

      Sample extracts must be protected from light and stored at 4'C (±2*0)
      until 365 days after delivery of a complete data package.

      Sample extracts must be stored in an atmosphere demonstrated to be free
      of all potential contaminants.

      Samples, sample extracts, and standards must be stored separately.

3.    CONTRACT REQUIRED HOLDING TIMES

      The extraction shall be started within 5 days of the Validated Time of
      Sample Receipt (VTSR).

      Extracts must be analyzed within 40 days following the start of the
      extraction.
                                     SV D-4                            6/91

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 PART B  -  EQUIPMENT AND  STANDARDS

 4.    SUMMARY OP METHOD

 4.1   A one  liter aliquot of sample is acidified to pH 2.0 and extracted with
      methylene chloride using a continuous liquid-liquid extractor.  The
      methylene chloride extract is dried and concentrated to a volume of 1.0
      mL.  The extract  is injected onto a gas chromatograph (GC) capillary
      column.  The gas  chromatograph is temperature programmed to separate
      the seaivolatile  compounds, which are then detected with a mass
      spectrometer (MS).

 4.2   Target and surrogate compounds are identified in the samples by
      analyzing standards under the same conditions used for samples and
      comparing resultant mass spectra and GC retention times.  Internal
      standards are added to all samples and standards.  A response factor is
      established for each target and surrogate compound during the initial
      and continuing calibrations by comparing the MS response for the
      primary ion produced by the compound extracted ion current profile
      (EICP) to the MS  response for the primary ion produced by an internal
      standard.  Each identified target and surrogate compound in a sample is
      quantified by comparing the responses for the target compound and the
      internal standard, while taking into account the response factor from
      the most recent calibration, the sample volume, and any sample
      dilutions.

4.3   Non-target compounds are identified by comparing the resultant mass
      spectra from the non-target compounds to mass spectra contained in the
      National Institute of Standards and Technology Mass Spectral Library.
      Non-target compounds are quantified by comparing the MS response from
      the reconstructed ion chromatogram (RIG) for the non-target compound
      peaks  to the MS response produced by the nearest internal standard.  A
      response factor of 1 is assumed.

5.    INTERFERENCES

      Contaminants in solvents, reagents,  glassware and other sample
      processing hardware, may cause method interferences such as discrete
      artifacts and/or elevated baselines in the reconstructed ion current
      (RIC) profiles (TICPs).  All of these materials must be routinely
      demonstrated to be free from interferences under the conditions of the
      analysis by running laboratory method blanks.  Matrix interferences may
      be caused by contaminants that are coextracted from the sample.  The
      extent of matrix interferences will vary considerably from source to
      source.

6.    APPARATUS AND MATERIALS

      Brand names,  suppliers and part numbers are for illustrative purposes
      only.   No endorsement is implied.   Equivalent performance may be
      achieved using apparatus and materials other than those specified here,
      but demonstration of equivalent performance meeting the requirements of
      the method is the responsibility of the Contractor.
                                     SV D-5                            6/91

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6.1   Gas Chromatograph/Mass Spectrometer

      6.1.1    Gas  Chromatograph  - The gas chromatograph (GC) system must be
               capable  of temperature programming and have a flow controller
               that maintains a constant column flow rate throughout the
               temperature program .  The system must be suitable for
               splitless  injection and have all required accessories including
               syringes,  analytical columns, and gases.  All GC carrier gas
               lines must be constructed from stainless steel or copper
               tubing.  Non-polytetrafluoroethylene (PTFE) thread sealants, or
               flow controllers with rubber components are not to be used.

               Gas  Chromatography Column - A 30 m x 0.25 mm ID (or 0.32 am)
               bonded-phase silicone coated fused silica capillary column (J&W
               Scientific OB-5 or equivalent).  A film thickness of 0.25 to
               1.0  urn may be used.

      6.1.2    Mass Spectrometer  - The mass spectrometer must be capable of
               scanning from 35 to 500 amu every 1 second or less, utilizing
               70 volts (nominal) electron energy in the electron impact
               ionization mode and producing a mass spectrum which meets all
               die  tuning acceptance criteria when 50 ng of
               decafluorotriphenylphosphine (DFTPP) is injected through the
               gas  chromatograph  inlet.  To ensure sufficient precision of
               mass spectral data, the MS scan rate must allow acquisition of
               at least five spectra while a sample compound elutes from the
               GC.  The GC/MS system must be in a room whose atmosphere is
               demonstrated to be free of all potential contaminants which
               will interfere with the analysis.  The instrument must be
               vented outside the facility or to a trapping system which
               prevents the release of contaminants into the instrument room.

      6.1.3    Data System - A computer system must be interfaced to the mass
               spectrometer that  allows the continuous acquisition and storage
               on machine readable media of all mass spectra obtained
               throughout the duration of the chromatographic program.  The
               computer must have software that allows searching any GC/MS
               data file  for ions of a specified mass and plotting such ion
               abundances versus  time or scan number.  This type of plot is
               defined  as an Extracted Ion Current Profile (EIC?).  Software
               must also  be available that allows integrating the abundance in
               any  EICP between specified time or scan number limits.  Also,
               for  the  non-target compounds, software must be available that
               allows comparing sample spectra against reference library
               spectra.   The most recent release of the National Institute of
               Standards  and Technology Mass Spectral Library shall be used as
               the  reference library.

6.2   Magnetic Tape Storage Device - The magnetic tape storage device must be
      capable of recording data and suitable for long-term,  off-line storage.
                                     SV D-6                            6/91

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 6.3    Glassware:   A set of glassware  sufficient  to meet  contract requirements
       must be reserved for exclusive  use  in this contract.

       6.3.1   Continuous liquid-liquid extractors -  Equipped with Teflon or
               glass connecting joints and stopcocks  requiring no lubrication
               (Hershberg-Wolf Extractor-Ace Glass Company,  Vineland,  NJ, P/N
               6841-10 or equivalent.)

       6.3.2   Drying column - 19 mm ID chromatographic column with coarse
               frit. (Substitution of a small pad of  Pyrex pre-extracted glass
               wool for the frit will prevent cross contamination of sample
               extracts.)

       6.3.3   Concentrator tube - Kuderna-Danish, 10 mL, graduated (Kontes,
               Vineland, NJ, K-570050-1025 or equivalent).

       6.3.4   Evaporation flask - Kuderna-Danish, 500 mL (Kontes K-570001 -
               0500 or equivalent).   Attach to concentrator tube with springs.

       6.3.5   Snyder column - Kuderna-Danish, Three-ball macro (Kontes
               K-50300-0121 or equivalent).

       6.3.6   Snyder column - Kuderna-Danish, Two-ball micro (Kontes  K-
               569001-0219 or equivalent).

       6.3.7   Vials -  Amber glass,  2  mL capacity with Teflon-lined screw-cap.

       6.3.8   Syringes - 0.2 mL,  0.5  mL,  and 5 mL volumes.

6.4    Gases - Helium, Nitrogen, ultra pure  grade.

6.5    Gas-line tubing  -  stainless steel, or copper tubing.

6.6    Silicon carbide boiling chips - approximately 10/40 mesh.  Heat to
       400*C for 30 minutes  or Soxhlet extract with methylene chloride.

6.7   Water bath - Heated,  with concentric  ring  cover, capable of temperature
       control.  To prevent  the release of solvent fumes  into the laboratory,
       the bath must be used in a hood.

6.8   Balance - Analytical, capable of accurately weighing +0.0001 g.  The
      balances must be calibrated with class S weights once per each 12-hour
      workshift.  The balances must also be annually checked by a certified
       technician.

6.9   Nitrogen evaporation device equipped with  a water bath that can be
      maintained at 30*C to 35*C.  To prevent the release of solvent fumes
      into  the laboratory,  the nitrogen evaporation device must be used  in a
      hood.  The N-Evap by Organomation Associates, Inc. South Berlin, MA  (or
      equivalent)  is suitable.
                                     SV D-7                            6/91

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 6.10  Micro-syringes  -  10 uL and larger, 0.006 inch ID needle.

 6.11  pH meter  - Calibrate according to manufacturer's instructions.  pH
      meter must be calibrated before each use.

 7.    REAGZNTg

 7.1   Reagent water - Reagent water is defined as water in which no
      semivolatile target compound is observed at or above the CRQL listed in
      Exhibit C for that compound and in which no non-target compound is
      observed at or above 10 ug/L.

      7.1.1   Reagent water may be generated by passing tap water  through  a
              carbon  filter bed containing about 453  g (1 Ib) of activated
              carbon  (Calgon Corp., Filtrasorb-300 or equivalent).

      7.1.2   Reagent water may be generated using a  water purification
              system  (Millipore Super-Q or equivalent).

 7.2   Solvents - Acetone, methanol, methylene chloride.   Pesticide quality or
      equivalent.

 7.3   Sodium sulfate -  (ACS) Granular, anhydrous (J.T. Baker anhydrous
      powder, catalog #73898,  or equivalent).  Purify by heating at 400*C for
      four hours in a shallow tray, cool in a desiccator,  and store in a
      glass bottle.

 7.4   Sulfuric acid solution (1:1) - slowly add 50 mL of concentrated 0*2804
      (Sp. Gr. 1.84) to 50 mL of reagent water.

 8.

 8.1   The Contractor must provide all standard solutions to be used with this
      contract.   These  standards may be used only after they have been
      certified according to the procedure in Exhibit E.   The Contractor must
      be able to verify that the standards are certified.   Manufacturer's
      certificates of analysis must be retained by the Contractor and
      presented upon request.

8.2   Stock Standard Solutions

      Stock standard solutions may be purchased or prepared using the
      following procedure.

      8.2.1   Accurately weigh about 0.0100  g of pure material.  Dissolve  the
              material  in methylene chloride or another suitable solvent and
              dilute  to volume in a 10 mL volumetric  flask.  Larger volumes
              may be used at the convenience of the analyst.
                                     SV D-8                            6/91

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      8.2.2    When compound purity  is  assayed to be 97 percent or greater,
               the weight may be used without correction to calculate the
               concentration of the  stock solution.  If the compound purity  is
               assayed to be less  than  97 percent, the weight must be
               corrected when calculating the concentration of the stock
               solution.

      8.2.3    Fresh stock standards must be prepared once every twelve'
               months,  or sooner,  if standards have degraded or concentrated.
               Stock standards  must  be  checked for signs of degradation or
               concentration just  prior to preparing secondary dilution and
               working standards from them.

8.3   Secondary Dilution Standards

      8.3.1    Using stock standards, prepare secondary dilution standards in
               methylene  chloride  that  contain the compounds of interest
               either singly or mixed together.

      8.3.2    Fresh secondary  dilution standards must be prepared once every
               twelve months, or sooner, if standards have degraded or
               concentrated.  Secondary dilution standards must be checked for
               signs of degradation  or  concentration just prior to preparing
               working standards from them.

8.4   Working Standards

      8.4.1    Tuning Solution  - Decafluorotriphenylphosphine (DFTPP)

               Prepare a  50 ng/uL  solution of DFTPP in methylene chloride.
               The DFTPP  solution  must  be prepared fresh once every twelve
               months,  or  sooner,  if the solution has degraded or
               concentrated.

      8.4.2    Initial  and Continuing Calibration Solutions

               8.4.2.1    Five  initial calibration standard solutions are
                         required- for all target and surrogate compounds.
                         Standard concentrations of 5, 10, 20, 50, and 80
                         ng/uL are required for five of the surrogates and
                         all but eight of the target compounds.  Nine
                         compounds:   2,4-dinitrophenol, 2,4,5-
                         trichlorophenol,  2-nitroaniline,  3-nitroaniline, 4-
                         nitroaniline,  4-nitrophenol, 4,6-dinitro-2-
                         methylphenol and pentachlorophenol,  2,4,6
                         tribromophenol (surrogate),  require calibration at
                         20, 50,  80, 100,  and 120 ng/uL.

               8.4.2.2    To prepare a calibration standard solution, add an
                         appropriate volume of secondary dilution standard  to
                         methylene chloride in a volumetric flask.  Dilute  to
                         volume with methylene chloride.
                                     SV D-9                            6/91

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              8.4.2.3    Add 10.0 uL of internal standard spiking solution
                         (Paragraph 8.6.1) to 1.0 mL of each calibration
                         standard for a concentration of 20 ng/uL for each
                         internal standard.

              8.4.2.4    The 20 ng/uL initial calibration solution (80 ng/uL
                         for the nine compounds listed in 8.4.2.1) is the
                         continuing calibration solution.

              8.4.2.5    The five initial calibration solutions must be
                         prepared fresh before use.  The continuing
                         calibration standard solution must be prepared
                         weekly, or sooner, if the solution has degraded or
                         concentrated.

8.5   Surrogate Standard Spiking Solution

      8.5.1   Prepare a surrogate standard spiking solution in methanol that
              contains, 2,4,6-tribromophenol (an acid surrogate compound), at
              a concentration of 120 ug/aL.  The other acid surrogate
              compounds:  phenol-dg and 2-fluorophenol, and the base/neutral
              compounds:  nitrobenzene-ds, terphenyl-d^, and 2-
              fluorobiphenyl are at a concentration of 40 ug/mL.

      8.5.2   The surrogate standard spiking solution must be prepared every
              twelve months, or sooner, if the solution has degraded or
              concentrated.

8.6   Internal Standard Spiking Solution

      8.6.1   Prepare an internal standard spiking solution in methylene
              chloride or another suitable solvent that contains  1,4
              dichlorobenzene-d^, naphthalene•dg, acenaphthene-d^g,
              phenanthrene-diQ, chrysene-dj^, and perylene-di2 at 2000 ng/uL.
              It may be necessary to use  5 to 10 percent benzene  or toluene
              in this solution and a few  minutes of ultrasonic mixing in
              order to dissolve all the constituents.

      8.6.2   The internal standard spiking solution must be prepared every
              six months, or sooner, if the solution has degraded or
              concentrated.

8.7   Laboratory Control Sample (LCS)  Spiking Solution

      8.7.1   Prepare a laboratory control sample spiking solution that
              contains each of the compounds at the concentrations listed
              below in methanol.
                                     SV D-10                           6/91

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                                                     Concentration
              Compounds                                 (ug/nL)

              Phenol                                      40.0
              2-Chlorophenol                              40.0
              4-Chloroaniline                             40.0
              2,4,6-Trichlorophenol                       40.0
              bis(2-Chloroethyl)ether                     20.0
              N-Nitroso-di-n-propylamine                  20.0
              Hexachloroe thane                            20.0
              Isophorone                                  20.0
              1,2,4-Trichlorobenzene                      20.0
              Naphthalene                                 20.0
              2,4-Dinitrotoluene                          20.0
              Diethylphthalate                            20.0
              N-Nitrosodiphenylamine                      20.0
              Hexachlorobenzene                           20.0
              Benzo(a)pyrene                              20.0


      8.7.2   The laboratory control sample solution must be prepared every
              twelve months, or sooner, if the solution has degraded or
              concentrated.

8.8   Storage of Standard Solutions

      8.8.1   Store the stock and secondary standard solutions at  -10*C to
              -20*0 in Teflon-lined screw-cap amber  bottles.

      8.8.2   Store the working standard solutions at 4*C (+2*C) in Teflon-
              lined screw-cap amber bottles.

      8.8.3   Protect all standards from light.

      8.8.4   Samples, sample extracts, and standards must be stored
              separately.
                                     SV D-ll                           6/91

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                     SECTION III
INSTRUMENT QUALITY CONTROL PROCEDURES AND REQUIREMENTS
                         SV D-12                           6/91

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 PART A  -  INSTRUMENT OPERATING CONDITIONS

 Gas Chromacograph

      The following are  the recommended gas chromatographic analytical
 conditions.
Carrier Gas:
Linear Velocity:
Injector Temperature:
Injector:
Initial Temperature:
Initial Hold Time:
Ramp Rate:
Final Temperature:
Final Hold Time:
Helium
25-30 cm/sec
250-300*C
Grob-type, splitless
40* C
4.0 ±0.1 min
10*C/min
290-C
10 min or until all compounds of interest
have eluted.
Optimize GC conditions for compound separation and sensitivity.  Once
optimized, the same GC conditions must be used for the analysis of all
standards, samples, blanks, performance evaluation samples, and laboratory
control samples.

Mass Spectrometer

      The following are the required mass spectrometer conditions:
Transfer Line Temperature:
Source Temperature:

Electron Energy:
lonization Mode:
Mass Range:
Scan Time:
250-300*C
According to manufacturer's
specifications.
70 volts (nominal)
El
35 to 500 amu
At least 5 scans per peak, not to exceed
1 second per scan.
                                     SV D-13
                                   6/91

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PART B - TUNING THE MASS SPECTROMETER

9.    SUMMARY

      It is necessary to establish that a given GC/MS meets the standard mass
      spectral abundance criteria prior to initiating any on-going data
      collection. This is accomplished through the analysis of
      decafluorotriphenylphosphine (DFTPP).

10.   FREQUENCY

      Each GC/MS system used must be hardware tuned once per twelve (12) hour
      time period of operation.  Also, whenever the Contractor takes
      corrective action which may change or affect the tuning criteria for
      DFTPP (e.g., ion source cleaning or repair, column replacement,  etc.).
      the tune must be verified irrespective of the twelve-hour tuning
      requirement.  The twelve (12) hour time period for GC/MS system tuning
      and standards calibration (initial or continuing calibration criteria)
      begins at the moment of injection of the DFTPP analysis that the
      Contractor submits as documentation of a compliant tune.  The time
      period ends after twelve (12) hours have elapsed.  In order to meet
      tuning requirements, samples, PES, LCS, blanks, and standards must be
      injected within twelve hours of the DFTPP injection.

11.   PROCEDURE

11.1  Inject 50 ng of DFTPP into the GC/MS system.  All instrument conditions
      must be identical to those listed in Section III, Part A, except that a
      different temperature program may be used.

11.2  DFTPP may be analyzed separately or as part of the calibration
      standard.

12.   TECHNICAL ACCEPTANCE CRITERIA FOR DFTPP ANALYSIS

12.1  The GC/MS system must be tuned at the frequency described in Section
      10.

12.2  The abundance criteria listed in Table D-7 must be met for a 50 ng
      injection of DFTPP.  The mass spectrum of DFTPP must be acquired in the
      following manner.  Three scans (the peak apex scan and the scans
      immediately preceding and following the apex) are acquired and
      averaged.  Background subtraction is required, and must be accomplished
      using a single scan prior to the elution of DFTPP.  Note:  All
      subsequent standards samples, including LCS, PES, and blanks, must use
      identical mass spectrometer instrument conditions.
                                     SV D-14                           6/91

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                                   Table D-7

               DFTPP KEY IONS AND  ION ABUNDANCE CRITERIA
   Mass          Ion Abundance Criteria

    51       30.0-80.0 percent of mass 198
    68       Less than 2.0 percent of mass 69
    69       Present
    70       Lass than 2.0 percent of mass 69
   127       25.0 - 75.0 percent of mass 198
   197       Less than 1.0 percent of mass 198
   198  .     Base peak, 100 percent relative abundance (see note)
   199       5.0 - 9.0 percent of mass 198
   275       10.0 - 30.0 percent of mass 198
   365       Greater than 0.75 percent of mass 198
   441       Present but less than mass 443
   442       40.0 - 110.0 percent of mass 198
   443       15.0 - 24.0 percent of mass 442

Note:  All ion abundance MUST be normalized to m/z 198, the nominal base
       peak, even though the ion abundances of m/z 442 may be up to 110
       percent that of m/z 198.
12.3  The criteria above are based on adherence to the acquisition
      specifications identified in paragraph 12.2.  The criteria are based on
      performance characteristics of instruments currently utilized in
      routine support of Program activities.  These specifications, in
      conjunction with relative response factor criteria for 51 target
      compounds (see Table D-10), are designed to control and monitor
      instrument performance associated with the requirements of this method.

13.   CORRECTIVE ACTION

13.1  If the DFTPP acceptance criteria are not met, retime the GC/MS system.
      It may be necessary to clean the ion source, clean quadrupoles, or take
      other actions to achieve the acceptance criteria.

13.2  DFTPP acceptance criteria MUST be met before any standards, samples
      (including LCS and PES),  or required blanks are analyzed.  Any samples
      or required blanks analyzed when tuning criteria have not been met will
      require reanalysis at no additional cost.

14.   [This paragraph has been intentionally left blank and has been
      reserved.]
                                     SV D-15                           6/91

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PART C - CALIBRATION OF THE GC/MS SYSTEM

15.   INITIAL CALIBRATION

15.1  Summary - Prior co Che analysis of samples and required blanks and
      after tuning criteria have been met, each GC/MS system must be
      initially calibrated at a minimum of five concentrations to determine
      instrument sensitivity and the linearity of GC/MS response for the
      semivolatile target and surrogate compounds.

15.2  Frequency

      15.2.1  Each GC/MS system must be initially calibrated upon award of
              the contract, whenever the Contractor takes corrective action
              which may change or affect the initial calibration criteria
              (e.g., ion source cleaning or repair, column replacement,
              etc.), or if the continuing calibration technical acceptance
              criteria have not been met.

      15.2.2  If time still remains in the 12 hour time period after meeting
              the technical acceptance criteria for the initial calibration,
              samples may be analyzed.  It is not necessary to analyze a
              continuing calibration standard within this 12 hour time
              period, if the initial calibration standard that is the same
              concentration as the continuing calibration standard meets the
              continuing calibration technical acceptance criteria.  Quantify
              all sample and quality control sample results and quality
              control criteria results, such as internal standard area
              response change and retention time shift, against the initial
              calibration standard that is the same concentration as the
              continuing calibration standard.

15.3  Procedure

      15.3.1  Set-up the GC/MS system per the requirements of Section III,
              Part A.

      15.3.2  All standard/spiking solutions and blanks must be allowed to
              warm to ambient temperature (approximately 1 hour) before
              preparation or analysis.

      15.3.3  Prepare five calibration standards containing all the
              semivolatile target and surrogate compounds at the
              concentrations described in Paragraph 8.4.2.

      15.3.4  Prepare an internal standard spiking solution using the
              procedure described in Section 8.6.

      15.3.5  Tune the GC/MS system to meet the technical acceptance criteria
              in Section 12 for DFTPP.

      15.3.6  Analyze each calibration standard by injecting  1.0 uL of
              standard.  If a compound saturates when the 80 ng/uL  standard
              is injected (120 ng/uL for the nine compounds listed  in

                                     SV D-16                            6/91

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              Paragraph 8.4.2), and the GC/MS system is calibrated to achieve
              a detection sensitivity of no less than the CRQL for each
              compound,' the Contractor must document it in the SOG Narrative,
              and attach a quantitation report and RIG.  In this instance,
              the Contractor must calculate the results based on a four-point
              initial calibration for the specific compound that saturates.
              Secondary ion quantitation is only allowed when there are
              sample interferences with the primary quantitation ion.  If
              secondary ion quantitation is used, calculate a relative
              response factor using the area response from the most intense
              secondary ion which is free of interferences, and document the
              reasons for the use of the secondary ion in the SDG Narrative.

15.4  Calculations

      NOTE:  Unless  otherwise stated the area response is  that of the primary
      quantitation ion.

      15.4.1  Calculate relative response factors (RRF) for each semivolatile
              target and surrogate compounds using Equation D.ll.  See Table
              D-8 to associate semivolatile target and surrogates compounds
              with the proper internal standard.  See Table D-9 for primary
              quantitation ions to be used for each semivolatile target
              compound, surrogate, and internal standard.

              EQ. D.ll        AX    Cls
                       RRF -	 X -p	
                              Ais   °x

              Where:

              AX  - Area of the primary quantitation ion response (EICP) for
                    the compound to be measured.

              A£S - Area of the primary quantitation ion response (EICP) for
                    the internal standard.

              cis ~ Concentration of the internal standard.

              GX  - Concentration of the compound to be measured.

      15.4.2  Equation D.12 is the general formula for standard deviation
              (SD) for a statistically small set of values.
              EQ. D.12
                      »-
                                    SV  D-17                           6/91

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         Where:

         SD - Standard deviation for  set of values.

         x^ - Value.

         x - Mean value.

         n - Number of values.

15.4.3   Calculate the percent relative standard deviation (%RSD)  of RRP
         values  for each  semivolatile target and surrogate compound over
         the initial  calibration range using Equation D.13 in
         conjunction  with Equation D.12.

         EQ.  D.13          SDBBF
                  %RSD -  —7-   x 100
                            x

         Where:

         %RSD -  Percent relative standard deviation.

         SDRRT -  Standard  deviation of initial  calibration response
                factors (per compound).

         From EQ. D.12

         *i - RRF - Relative response factors  from  initial calibration
                   standard (per compound).
        x - RRF - Mean value of  initial calibration  response  factors
                  (per compound).

15.4.4  Equation D.14  is  the general formula for the mean of  a set of
        values.
        EQ.  D.14        x -  	
                                n

        X£ - Value.


        x -  Mean value.

        n —  Number of values.

15.4.5  Calculate the mean of  the  relative  retention times (RRT)  for
        each semivolatile target and surrogate compound over the
        initial calibration  range  using Equation D.14 and Equation
        D.15.
                               SV D-18                           6/91

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                         EQ.  D.15                 RTC
                                          RRT -
               RTC - Retention time for the scmivolatile target and surrogate
                     compound.

                   - Retention time for the internal standard.
                  From EQ. D.14:

                         - Relative retention times for the semivolatile
                           target or surrogate compound for each initial
                           calibration standard.
               x - RRT - Mean relative retention time.

      15.4.6   Calculate the area response (Y)  mean for each internal standard
               compound over the initial calibration range using Equation
               D.14.

               Where:

               Xi - Y  - Area responses of the primary quantitation ion (EICF)
                        for  the internal standard for each initial calibration
                        standard.
              x - Y - Area response  mean.

      15.4.7  Calculate  the mean of  the  absolute  retention times  (RT)  for
              each  internal standard over  the initial calibration range  using
              Equation D.14.

              Where:

              X£ —  RT -  Retention time for the internal  standard  for each
                         initial  calibration standard.
              x - RT - Mean retention  time.

              n - Number of values.

15.5  Technical Acceptance Criteria For Initial Calibration

      15.5.1  All initial calibration  standards must  be  analyzed at the
              concentration levels described  in paragraph  8.4.2  and at the
              frequency described in Section  15.2 on  a GC/MS  system meeting
              the DFTPP technical acceptance  criteria.

      15.5.2  The relative response factor  (RRF) at each calibration
              concentration for each semivolatile target and  surrogate

                                     SV D-19                           6/91

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               compound must be greater  than or  equal  to  the  compound's
               minimum acceptable relative  response  factor  listed  in Table  D-
               10.

      15.5.3   The  %RSD over the initial calibration range  for relative
               response factor for each  semivolatile and  surrogate compound
               that has a required %RSD  must be  less than or  equal to the %RSD
               listed in Table D-10.

      15.5.4   Up to four compounds may  fail the criteria listed in paragraph
               15.5.2 and 15.5.3 and  still  meet  the  minimum RRF and %RSD
               requirements.   However, these four compounds must have a
               minimum RRF greater than  0.010 and %RSD less than or equal to
               40.0%.

      15.5.5   The  relative retention time  (RRT) for each of  the semivolatile
               target and surrogates  compounds at each calibration level must
               be within ±0.06 relative  retention time units  of the mean
               relative retention time (RRT)  for each  compound.

      15.5.6   The  area response (Y)  for each internal standard compound in
               each calibration standard must be within the inclusive r_ange of
               -50  percent to +100 percent  of the mean area response (Y) of
               the  internal standard  in  all of the calibration standards.

      15.5.7   The  retention time (RT) shift for each  of  the  internal
               standards at each calibration level must be  within ±0.33     	
               minutes (20.0 seconds) compared to the  mean  retention time (RT)
               over the initial calibration range for  each  internal standard.

15.6  Corrective Action

      15.6.1   If the technical acceptance  criteria  for initial calibration
               are  not met,  inspect the  system for problems.  It may be
               necessary to clean the ion source, change  the  column, or take
               other corrective actions  to  achieve the acceptance  criteria.

      15.6.2   Initial calibration technical acceptance criteria MUST be met
               before any samples (including the LCS and  FES) or required
               blanks are analyzed.  Any samples or  required  blanks analyzed
               when initial calibration  criteria have  not been met will
               require reanalysis at no  additional cost.

16.   CONTINUING CALIBRATION

16.1  Summary

      Prior to the analysis of samples and required blanks and after tuning
      criteria and initial calibration criteria have been met,  each GC/MS
      system must be routinely checked by analyzing a continuing calibration
      standard to ensure that the instrument continues to meet the instrument
      sensitivity and linearity requirements of the method.  The continuing
      calibration standard contains all  the semivolatile target compounds,
      surrogates, and internal standards.

                                     SV D-20                           6/91

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16.2  Frequency
      16.2.1   Each GC/HS used for analysis must be calibrated once every
               twelve (12) hour time period of operation.   The 12 -hour time
               period begins with the injection of DFTPP.

      16.2.2   If time still remains in the 12 hour time period after meeting
               the technical acceptance criteria for the initial calibration,
               samples may be analyzed.  It is not necessary to analyze a
               continuing calibration standard within this  12 hour time
               period, if the initial calibration standard  that is the same
               concentration as the continuing calibration  standard meets the
               continuing calibration technical acceptance  criteria.  Quantify
               all sample results against the 20 ng/uL (80  ng/uL for the nine
               compounds listed in Section 8.4.2.1) calibration standard.

16 . 3  Procedure

      16.3.1   Set up GC/MS system per the requirements of  Section III,  Part
               A.

      16.3.2   Prepare a continuing calibration standard solution containing
               all the semivolatile target and surrogate compounds using the
               procedure listed in Section 8.4.2.

      16.3.3   All standard/ spiking solutions and blanks must be allowed to
               warm to ambient temperature (approximately 1 hour) before
               preparation or analysis.

      16.3.4   Tune the GC/MS system to meet the DFTPP technical acceptance
               criteria in Section 12.

      16.3.5   Start the analysis of the continuing calibration standard by
               injecting 1.0 uL of standard.

16 . 4  Calculations

      16.4.1   Calculate a relative response factor (RRF) for each
               semivolatile target and surrogate compound using Equation D.ll.

      16.4.2   Calculate the percent difference between the mean relative
               response factor from the most recent initial calibration and
               the continuing calibration relative response factor for each
               semivolatile target and surrogate compound using Equation D.17.
                                                 - RRFC
              EQ D.17   % Difference R» - - — — -   x 100
                                               RRFj.
                                     SV D-21                           6/91

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               Where:
               RRFj[ - Average  relative response factor from  the most
                      recent initial calibration.

               RRFC - Relative response  factor from continuing calibration
                      standard.

16.5  Technical Acceptance Criteria For Continuing Calibration

      16.5.1   The  continuing  calibration standard oust be analyzed at  the 20
               ng/uL (80 ng/uL for  the nine compounds listed in 8.4.2.1)
               concentration level  at the frequency described in  Section 16.2
               on a GC/MS  system meeting the DFTPP tuning and the initial
               calibration technical acceptance criteria.

      16.5.2   The  relative response factor for each semivolatile target and
               surrogate compound must be greater than or equal to the
               compound's  «
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                                SECTION IV
SAMPLE PREPARATION, ANALYSIS, AND COMPOUND IDENTIFICATION AND QUANTITATION
                                   SV D-23                           6/91

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17.   SUMMARY
      This method is designed for analysis of samples that contain low
      concentrations of the semivolatile compounds listed in Exhibit C.  The
      majority of the samples are expected to come from drinking water
      sources and well/ground water around Superfund sices.  If, upon
      inspection of a sample, the Contractor suspects that the sample is not
      amenable to this method, contact SMO for instructions.

18.   PROCZPT3S2

18.1  Extraction

      Continuous liquid-liquid extraction is required for the extraction of
      the samples.

      18.1.1  Add methylene chloride to the bottom of the  extractor  and fill
              it to a depth of at least 1 inch above the bottom side arm.

      18.1.2  Using a 1 liter graduated cylinder, measure  out a 1.0  liter
              sample aliquot.  Transfer the 1 liter sample aliquot to  the
              continuous extractor.  Pipet 1.0 mL of surrogate  standard
              spiking solution into the sample and mix well.  Check  the pH of
              the sample with a pH meter and adjust the pH to 2.0 with 1:1
              H2S04.

      18.1.3  Add sufficient methylene chloride to the distilling flask to
              ensure proper solvent cycling during operation.   Extract for 18
              hours.  Allow to cool, then detach the distilling flask  and
              label.

      18.1.4  If the sample was received in a 1 liter container, rinse the
              empty container with 60 mL of methylene chloride  after taking
              the sample aliquot.  Add the rinsate to the  continuous
              extractor.

18.2  Concentrating the Extracts

      18.2.1  Assemble a Kuderna-Danish (K-D) concentrator by attaching a  10
              mL concentrator tube to a SOO mL evaporative flask.  Other
              concentration devices or techniques may be used in place of  the
              K-D, if equivalency is demonstrated for all  the semivolatile
              target compounds listed in Exhibit C.

      18.2.2  Transfer  the extract by pouring the extract  through a  drying
              column containing about 10 cm of anhydrous granular sodium
              sulfate, and collect the extract in a K-D concentrator.   Rinse
              the distilling  flask and column with 20 to 30 mL  of methylene
              chloride to complete the quantitative transfer.

      18.2.3  Add one or two clean boiling chips and attach a three-ball
              Snyder column to the evaporative flask.  Pre-wet  the Snyder
              column by adding about 1 mL methylene chloride to the  top of
              the column.  Place the K-D apparatus on a hot water bath (60*C


                                     SV D-24                           6/91

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         co  80*C)  so  thac  Che  concentrator Cube  is partially immersed in
         Che hot water, and  the  entire  lover rounded surface of the
         flask is  bathed with  hot vapor-:  Adjust the vertical posicion
         of  the apparatus  and  the water temperature as required to
         complete  Che concentration in  10 to 15  minutes.  At the proper
         rate of distillation, the balls of Che  column will accively
         chatter but  the chambers will  not flood with condensed solvent.
         When Che  apparent volume of liquid reaches 1 mL, remove the K-D
         apparatus from Che waCer bath  and allow ic Co drain and cool
         for ac least 10 minutes.  Remove the Snyder column and rinse
         the flask and its lower joint  into the  concentrator tube with 1
         to  2 mL of mechylene  chloride.  A 5 mL  syringe is recommended
         for this  operation.

18.2.4   Two different types of concentration techniques are permitted
         to  obtain Che final 1.0 mL volume:  micro Snyder column and
         nitrogen  evaporation  techniques.

         18.2.4.1   Micro Snyder Column Technique

                   Add another one or two clean boiling chips to the
                   concentrator cube and attach a two-ball micro Snyder
                   column. Pre-wec Che Snyder column by adding abouc
                   0.5 mL of mechylene chloride Co Che cop of Che
                   column.  Place Che K-D apparatus in a hoc water bath
                   (60*C to 80*C)  so that che concentrator Cube is
                   partially immersed in che hoc water.   Adjust the
                   vertical posicion of Che apparatus and che water
                   temperature as required to complete che
                   concentration in 5 to 10 minutes.   At che proper
                   race of distillation che balls of che column will
                   accively chatter but Che chambers will noC flood
                   with condensed solvent.  When Che apparent volume of
                   liquid reaches about 0.5 mL,  remove che K-D
                   apparatus from Che water bath and allow it to drain
                   for at least 10 minutes while cooling.   Do not let
                   che extract go to dryness.   Remove che Snyder column
                   and rinse its flask and its lower joint into che
                   concencrator tube with 0.2 mL of methylene chloride.
                   Adjust Che final volume Co 1.0 mL with mechylene
                   chloride.   Transfer Che excracc Co a  Teflon-sealed
                   screw-cap bottle,  label che bottle and store at 4*C
                   (±2'C).

        18.2.4.2    Nitrogen Evaporation Technique (taken from ASTM
                   Method D3086)

                   Place  the concentrator tube with an open micro
                   Snyder column attached in a warm water bach (30*C to
                   35*C)  and evaporate  che  solvenc volume co just below
                   1  mL by blowing a  gentle  stream of clean,  dry
                   nitrogen (filtered chrough a column of activated
                   carbon) above the  extract.   Caution:  Gas lines from
                   the  gas source  to  the  evaporation apparatus must be


                              SV D-25                           6/91

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                          stainless steel, copper, -or Teflon tubing.  The
                          internal vail of the concentrator tube must be
                          rinsed down several times with methylene chloride
                          during the operation and the final volume brought to
                          1.0 mL with methylene chloride.  During evaporation,
                          the tube solvent level must be kept below the water
                          level of the bath.  The extract must never be
                          allowed to become dry.  Transfer the extract to a
                          Teflon-sealed screw-cap bottle, label the bottle and
                          store at 4*C (±2*C).

18.3  Instrumental Analysis

      18.3.1   Set up  the  GC/MS system per the requirements of Section III,
               Part A.   Before samples or required blanks can be analyzed, the
               instrument  must meet the DFTPP, initial calibration, and
               continuing  calibration technical acceptance criteria.  All
               samples,  required blanks,  extracts, and standard/spiking
               solutions must be allowed  to warm to ambient temperature
             .  (approximately 1 hour) before preparation/analysis.  All sample
               extracts  and required blanks must be analyzed under the same
               instrumental conditions as the calibration standards.

      18.3.2   Add 10.0  uL of the internal standard spiking solution  (2000
               ng/uL)  to the 1.0 mL extract.  For sample dilutions, add an
               appropriate amount of the  internal standard spiking solution to
               maintain  a  20 ng/uL concentration of the internal standards in
               the diluted extract.

      18.3.3   Inject  1.0  uL of sample extract into the GC/MS, and start data
               acquisition.

      18.3.4   When all  semivolatile target compounds have eluted from the GC,
               terminate the MS data acquisition and store data files on the
               data system storage device.  Use appropriate data output
               software  to display full range mass spectra and EICPs.

19.   DILUTIONS

19.1  When a sample extract is analyzed that has a semivolatile target
      compound concentration greater than the upper limit of the initial
      calibration range or in which ions from a compound saturate the
      detector (excluding the compound peaks in the solvent front), the
      extract must be diluted and reanalyzed.   Secondary ion quantitation is
      only allowed when there are sample interferences with the primary
      quantitation ion,  not when saturation occurs.  If secondary ion
      quantitation is used, calculate a relative response factor using the
      area response (EICP) from the most intense secondary ion which is free
      of sample interferences,  and document the reasons for the use of the
      secondary ion in the SDG Narrative.
                                     SV D-26                           6/91

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 19.2   Dilute  the sample using  the following procedure:

       19.2.1   Calculate the sample  dilution necessary to keep the
               semi-volatile target compounds that required dilution within the
               upper half of the initial calibration range and so  that no
               compound has ions which saturate the  detector (excluding the
               compound peaks in the solvent front).   Note:   Do not dilute
               sample solely to get  2,4,6 tribromophenol value within the
               initial calibration range.

       19.2.2   Dilute the sample extract with methylene chloride in a
               volumetric flask.

       19.2.3   Analyze the sample dilution per Section 18.3,  including the
               addition of internal  standards to maintain a 20 ng/uL
               concentration of the  internal standards (see 18.3.2).

 20.    IDENTIFICATION OF TARGET COMPOUNDS

 20.1   The compounds listed  in  the Target Compound List  (TCL), Exhibit C,
       shall be identified by an analyst competent in  the interpretation  of
       mass spectra by comparison of the sample mass spectrum  to the mass
       spectrum of a standard of the suspected compound.  Two  criteria must be
       satisfied to verify the  identifications:   (1) elution of the sample
       compound at the same  GO  relative retention time as the  standard
       compound, and  (2) correspondence of the sample compound and standard
       compound mass spectra.

 20.2   For establishing correspondence of the GC  relative retention time
       (RRT),  the sample compound RRT must be within ±0.06 BRT units of the
      RRT of  the standard compound.   For reference, the standard must be run
       on the  same shift as  the sample.  If co-elution of interfering
       compounds prohibits accurate assignment of the sample compound RRT from
       the extracted ion current profile for the  primary ion,  the RRT must be
       assigned by using the total ion chromatogram.

20.3   For comparison of standard and sample compound mass spectra, mass
       spectra obtained on the  Contractor's GC/MS are required. These standard
       spectra may be used for  identification purposes, only if the
      Contractor's GC/MS meets  the DFTPP daily tuning technical acceptance
      criteria.  These standard spectra may be obtained from  the analysis
      used to obtain reference  relative retention times.

20.4  The guidelines for qualitative verification by comparison of mass
      spectra are as follows:

      20.4.1  All ions present in the  standard mass spectra at a  relative
               intensity greater than 25  percent (most abundant ion in the
              spectrum equals  100 percent)  must be  present in the sample
              spectrum.

      20.4.2  The relative  intensities  of  the major ions specified in Section
              20.4.1 must agree within +20  percent  between the standard and
              sample spectra.   (Example: For an ion with an abundance of 50


                                     SV D-27                           6/91

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              percent: in the standard spectra, the corresponding sample ion
              abundance must be between 30 and 70 percent.)

      20.4.3  Ions  greater  than 25 percent in the sample spectrum but not
              present in the standard spectrum must be considered and
              accounted for by the analyst making the comparison.  The
              verification  process should FAVOR FALSE POSITIVES.  All
              compounds meeting the identification criteria must be reported
              with  their spectra.

      20.4.4  If  a  compound cannot be verified by all of Che criteria in
              Sections 20.4.1 • 20.4.3, but in the technical Judgment of the
              mass  spectral interpretation specialist, the identification is
              correct, then the Contractor shall report that identification
              and proceed with quantitation.

21.   IDENTIFICATION OF SON-TARGET COMPOUNDS

21.1  A library search shall be executed for non-target compounds for the
      purpose of tentative identification.   The most recent release of the
      National Institute of Standards and Technology Mass Spectral Library
      shall be used as the reference library.

21.2  Up to 20 non-surrogate/non-internal standard organic compounds of
      greatest apparent concentration not listed in Exhibit C for the
      semivolatiles shall be tentatively identified via a forward search of
      the National Institute of Standards and Technology Mass Spectral
      Library.  (Compounds with a peak area response less than 50 percent of
      the area response for the nearest internal standard and compounds which
      elute before the first semivolatile target compound elutes are not
      required to be searched in this fashion.)   Only after visual comparison
      of sample spectra with the nearest library searches will the mass
      spectral interpretation specialist assign a tentative identification.
      Computer generated library search must not use normalization routines
      if those routines would misrepresent the library or unknown spectra
      when compared to each other.

21.3  Guidelines for making tentative identification

      21.3.1  Relative intensities of major ions in the reference spectrum
              (ions greater than  25 percent of the most abundant ion) should
              be  present in the sample spectrum.

      21.3.2  The relative  intensities of the major ions should agree within
              ±20 percent.  (Example: For an ion with an abundance of 50
              percent in the standard spectra, the corresponding sample  ion
              abundance should be between 30 and 70 percent.

      21.3.3  Molecular ions present in reference spectrum should be present
              in  sample spectrum.

      21.3.4  Ions  present  in the sample spectrum but not  in the reference
              spectrum should be  reviewed for possible background
              contamination or presence of co-eluting compounds.


                                     SV D-28                           6/91

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      21.3.5   Ions present in the  reference  spectrum but not in the sample
               spectrum should be reviewed for possible subtraction from  the
               sample  spectrum because of  background contamination or
               coeluting compounds.   Data  system  library reduction programs
               can sometimes create these  discrepancies.

      21.3.6   If  in the technical  judgment of the mass interpretation
               spectral specialist,  no valid  tentative identification  can be
               made, the compound should be reported as unknown.  The  mass
               spectral specialist  should  give additional classification  of
               the unknown  compound,  if possible  (e.g., unknown phthalate,
               unknown hydrocarbon,  unknown acid  type, unknown  chlorinated
               compound). If a probable molecular weight can be distinguished,
               include it.

22.   CALCULATIONS

      NOTE:  Unless otherwise stated, the area response is from the extracted
      ion current profile  (EICP) of the primary quantitation ion.

22.1  Target Compounds

      22.1.1   Calculate target compound concentrations using Equation D.18.

               EQ. D.18                           (A,)(Is)(Vc)(Df)
                         Concentration in ug/L -
                                                  (Ais)(RRF)(V0)(Vi)

              Where:

              AX  - Area response (EICF) for the  compound to be measured.
                    The primary quantitation ions for the target compounds,
                    internal standards, and surrogates are listed  in
                    Table D-9.

              Ais ~ Area response (EICF) for the  internal standard.  The
                    target compounds are listed with their associated
                    internal standard in Table D-8.

              Is  - Amount of internal standard inj ected in nanograins  (ng).

              RRF - The RRF from the most recent  continuing calibration as
                    determined in Section 15.4.1.

              V0  - Volume of water extracted in milliliters (mL).

              V^  - Volume of extract injected in microliters  (uL).

              Vt  - Volume of final extract in microliters (uL).

              Df  - Dilution Factor.  The dilution factor for  analysis of
                    water samples  for semivolatiles  by this  method is defined
                    as follows:
                                     SV D-29                           6/91

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              u^ mo^t:  cone .  extract used to make dilution •+• ul^ clean  solvent
              uL most  cone,  extract used to make dilution

              If no dilution is performed, Df - 1.0.

      22.1.2  When target compounds are below contract required quantisation
              limits (CRQL), but the spectra meet the identification
              criteria., report the concentration with a "J".  For example,  if
              the CRQL is 5  ug/L and a concentration of 3.0 ug/L is
              calculated, report as "3.0 J*.  Report ALL saf|*ple concentration
                      PNCORRECTED for
22.2  Hen-Target Compounds

      Equation D.18 is used for calculating the concentrations of the non-
      target compounds.  Total area counts (or peak heights) from the
      reconstructed ion chromatograms (RIG) are to be used for both the non-
      target compound to be measured (A^) and the internal standard (A^s) .
      Associate the nearest internal standard free of interferences with  the
      non- target compound to be measured.  A relative response factor (KEIF)
      of one (1) is to be assumed.  The value from this quantitation shall be
      qualified as estimated ("J").  This estimated concentration must be
      calculated for all tentatively identified compounds as well as those
      identified as unknowns.

22 . 3  Surrogates

      Calculate the surrogate percent recovery using Equation D.19.

                                               Qd
      EQ. D.19   Surrogate Percent Recovery -  = —  x  100

      Where:

      Qd - Quantity determined by analysis.

      Qa - Quantity added to sample/blank.

22.4  Internal Standards

      22.4.1   Calculate  the  percent area response change  (% ARC)  for  the
               sample/blank analysis compared  to  the most  recent continuing
               calibration standard analysis for  each  of  the internal  standard
               compounds  using Equation  D.20.

                                 A« - A-
             EQ. D.20  % ARC -      »      x 100
                                     SV D-30                           6/91

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               Where:

               % ARC - Percent area response change.

               As    - Area response of the internal  standard in
                       the sample/blank analysis.

               AC    - Area response of the internal  standard in the most
                       recent continuing calibration  standard.

      22.4.2   Calculate the retention time shift  (RTS)  between the
               sample/blank analysis and the most  recent continuing
               calibration standard analysis for each of the internal
               standards using Equation D.21.

               EQ.  D.21  RTS - RTS - RTC

               Where:

               RTS  - Retention time shift.

               RTS  - Retention time of the  internal standard in a
                     sample/blank.

               RTC  - Retention time of the  internal standard in the
                     most recent continuing calibration standard.

23.   TECHNICAL ACCEPTARCE  CRITERIA FOR SAMPLE ANALYSIS

23.1  The sample must be analyzed on  a  GC/HS system meeting the DFTPP,
      initial calibration,  and  continuing  calibration technical acceptance
      criteria.

23.2  The sample must be extracted and  analyzed within the contract holding
      times.

23.3  The sample must have  an associated method blank meeting  the blank
      technical acceptance  criteria.  The  sample must have a Laboratory
      Control Sample associated with  it meeting the LCS  technical acceptance
      criteria.  The sample must  also have a PES associated with it meeting
      the PES techncial acceptance  criteria.

23.4  The percent recovery  for  each of  the surrogates in the sample must be
      within the acceptance windows listed in Table D-ll.

23.5  The difference of the area  response  change for each of the internal
      standards for the sample  must be  within the  inclusive range of  -50
      percent and +100 percent  of the response of  the internal standards in
      the most recent continuing  calibration analysis.

23.6  The retention time shift  for  each of the internal  standards must be
      within ±0.33 minutes  (20.0  seconds)  between  the sample and the  most
      recent continuing calibration standard analysis.
                                     SV D-31                           6/91

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23.7  Excluding those ions in the solvent front, no ion may saturate the
      detector.  No target compound concentration may exceed the upper limit
      of the initial calibration range unless a more dilute aliquot of the
      sample extract is also analyzed according to the procedures in Section
      19.

                         Table 0-11

      CONTRACT REQUIRED SURROGATE SPIKE RECOVERY LIMITS
        Surrogate Compound      % Recovery


         Nitrobenzene-d$          40-112
         2-Fluorobiphenyl         42-110
         Terphenyl-d14            24-140
         Phenol-d5                17-113
         2-Fluorophenol           16-110
         2,4,6-Tribromophenol     18-126


24.   CORggCTTvE ACTION

24.1  If the sample technical acceptance criteria for the surrogates and
      internal standards are not net, check calculations, surrogate and
      internal standard solutions, and instrument performance.  It may be
      necessary to recalibrate the instrument or take other corrective action
      procedures to meet the surrogate and internal standard technical
      acceptance criteria.

24.2  If the Contractor needs to analyze more than one (1) sample dilution
      other than the original analysis to have all the target compounds
      within the initial calibration range and to have no ions saturating the
      detector (excluding the peaks in the solvent front), contact SMO.  SMO
      will contact the Region for instructions.

24.3  Sample analysis technical acceptance criteria MUST be met before data
      are reported.  Samples contaminated from laboratory sources, or
      associated with a contaminated method blank or any samples analyzed not
      meeting the technical acceptance criteria will require reextraction
      and/or reanalysis at no additional cost.

24.4  Sample reruns performed as a result of suspected matrix interferences
      beyond the scope of the method will be reviewed on a case-by-case basis
      for payment purposes by SMO.

25.   [This paragraph has been intentionally left blank and has been
      reserved.]
                                     SV D-32                           6/91

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                     SECTION V
SAMPLE QUALITY CONTROL PROCEDURES AND REQUIREMENTS
                       SV D-33                           6/91

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26.   BLANK ANALYSIS

26.1  Summary - A method blank is 1.0 liter of reagent water carried through
      the entire analytical scheme.

26.2  Frequency

      26.2.1  A method blank must be extracted at least once:

              o   every 20 samples,  AND
              o   whenever samples are extracted.

      26.2.2  Each method blank must be analyzed on each GC/MS used to
              analyze the samples prepared with the method blank.

26.3  Procedure for Method Blank Preparation

      26.3.1  Prepare the method blank at the frequency listed in Section
              26.2.  Measure out 1.0 liter of reagent water for each method
              blank aliquot.  Extract and concentrate the method blank at the
              sane time as the samples associated with the blank according to
              Sections 18.1.1 and 18.2.

      26.3.2  Analyze the method blank and calculate the results according to
              Sections 18-22.

26.4  Technical Acceptance Criteria For Blank Analysis

      26.4.1  All blanks must be analyzed at the frequency described in
              Section 26.2 on a GC/MS system meeting the DFTPP, initial
              calibration, and continuing calibration technical acceptance
              criteria.

      26.4.2  The percent recovery  for each of the surrogates in the blank
              must be within the acceptance windows listed in Table D-ll.

      26.4.3  The area response change for each of the internal standards for
              the blank must be within the inclusive range of -50 percent and
              +100 percent compared to the internal standards in the most
              recent continuing calibration analysis.

      26.4.4  The retention time shift for each of the internal standards
              must be within ±0.33  minutes (20.0 seconds) between the blank
              and the most recent continuing calibration analysis.

      26.4.5  The concentration of  the target compounds in the blanks must be
              less than or equal to the CRQL for each target compound.   The
              concentration of non-target compounds in the blanks must not
              exceed 10 ug/L.

26.5  Corrective Action

      26.5.1  If a Contractor's blanks do not meet the technical acceptance
              criteria, the Contractor must consider  the analytical  system  to


                                     SV D-34                           6/91

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              be out of control.  It is the Contractor's responsibility to
              ensure that method interferences caused by contaminants in
              solvents, reagents, glassware, and sample storage and
              processing hardware that lead to discrete artifacts and/or
              elevated baselines in gas chromatograms be eliminated.  If
              contamination is a problem, the source of the contamination
              must be investigated and appropriate corrective measures MUST
              be taken and documented before further sample analysis
              proceeds .

      26.5.2  Any method blank that fails to meet the technical acceptance
              criteria must be reextracted and reanalyzed at no additional
              cost.  Further, all samples processed with a method blank that
              is out of control (i.e., contaminated) will require
              reextraction and reanalysis at no additional cost.

27.   LABORATORY CONTROL
27.1  Summary
      The LCS is an internal laboratory quality control sample designed to
      assess (on an SDG-by-SDG basis) the capability of the contractor to
      perform the analytical method listed in this Exhibit.
27 . 2  Frequency
      The LCS must be prepared, extracted, analyzed, and reported once per
      Sample Delivery Group.  The LCS must be extracted and analyzed
      concurrently with the samples in the SDG using the same instrumentation
      as the samples in the SDG.

27 . 3  Procedure

      27.3.1  Measure  a  1.0 liter  aliquot of reagent water in a  1 liter
              graduated  cylinder and  transfer  the water to a continuous
              extractor.  Pipet 1.0 mL of the  LCS spiking solution  (Paragraph
              8.7.1) and 1.0 mL of the surrogate standard spiking solution
              into  the water and mix  well.  Extract and concentrate the
              sample according to  Sections 18.1 and 18.2.

      27.3.2  Analyze  the LCS  per  Sections 18-21.

27 . 4  Calculations

      27.4.1  Calculate  individual compound recoveries of the LCS using
              Equation D.19, substituting LCS  percent recovery for  surrogate
              percent  recovery.

      27.4.2  See Section 22 for equations necessary for other calculations.
                                     SV D-35                           6/91

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27.5  Technical Acceptance Criteria For Laboratory Control Sample Analysis

      27.5.1  The LCS must be analyzed at the frequency described in Section
              27.2 on a GC/MS system meeting the DFTPP, initial calibration,
              and continuing calibration technical acceptance criteria.

      27.5.2  The LCS must be prepared as described in Paragraph 27.3.

      27.5.3  The LCS must be prepared and analyzed with a method blank that
              met the blank technical acceptance criteria.

      27.5.4  The percent recovery for each of the surrogates in the LCS must
              be within the acceptance windows listed in Table D-ll.

      27.5.6  The area response change for each internal standard for the LCS
              must be within the inclusive range of -50 percent and +100
              percent compared to the internal standard in the most recent
              continuing calibration analysis.

      27.5.7  The retention time shift for each of the internal standards
              within ±0.33 minutes (20.0 seconds) between the LCS and the
              continuing calibration standard analysis.

      27.5.8  The percent recovery for each of the compounds in the LCS must
              be within the recovery limits listed in Table D-12.

                                    Table D-12

                 LABORATORY CONTROL SAMPLE PERCENT RECOVERY LIMITS
                COMPOUND                           % RECOVERY
                Phenol                             44 - 120
                2-Chlorophenol                     58 - 110
                4-Chloroaniline                    35 - 98
                2,4,6-Trichlorophenol              65 - 110
                bis(2-Chloroethyl)ether            64 - 110
                N-Nitroso-di-n-propylamine         34 - 102
                Hexachloroethane                   32 - 77
                Isophorone                         49 - 110
                1,2,4-Trichlorobenzene             44-96
                Naphthalene                        56 - 160
                2,4-Dinitrotoluene                 61 - 140
                Diethylphthalate                   76 - 104
                N-Nitrosodiphenylamine             35 - 120
                Hexachlorobenzene                  30 - 95
                Benzo(a)pyrene                     55 - 92

     NOTE:  The recovery limits for any of the compounds  in  the  LCS  may be
     expanded at any time during the period of performance if SMO determines
     that the limits are too restrictive.
                                    SV D-36                           6/91

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 27.6  Corrective Action

       27.6.1  If the LCS technical acceptance criteria for the surrogates and
               internal standards are not met, check calculations, surrogate
               and internal standard solutions, and instrument performance.
               It may be necessary to recalibrate the instrument or take other
               corrective action procedures to meet the surrogate and internal
               standard criteria.

       27.6.2  The laboratory may not submit data from an SDG until the LCS
               technical acceptance criteria are met.  LCS contamination from
               laboratory sources or any LCS not meeting the criteria will
               require reanalysis and reextraction of the LCS at no additional
               cost.

       27.6.3  Further,  all samples in the SDG prepared and analyzed with an
               LCS that does not meet the LCS technical acceptance criteria
               will also require reanalysis at no additional cost.  Any LCS
               failing to meet these technical acceptance criteria must be
               reanalyzed and reextracted at no additional cost.

 28.    PERFORMANCE EVALUATION  SAMPLE  fPES^

 28.1   Summary

       The FES is an external  laboratory quality  control sample  prepared and
       designed to assess  (on  an  SDG-by-SDG basis) the capability  of the
       Contractor to perform the  analytical method listed  in this  Exhibit.

 28.2   Frequency

       The Contractor must extract, analyze, and  report the  results of  the PE
       sample  once per SDG, if available.  The  FES must be extracted and
       analyzed concurrently with the samples in  the SDG using the same
       instrumentation as the  samples in the SDG.

 28.3   Procedure

       28.3.1   The PES will  be received either as an ampulated extract or as  a
               full volume sample.  If  received as an ampulated extract, the
               Contractor  will receive  instructions  concerning the dilution
               procedure to  bring the extract  to  full volume prior to
               preparation and analysis of the  PES.

       28.3.2   Extract and concentrate  the PES  using the  procedure described
               in Section  18.  Add  1.0  mL  of surrogate solution to 1 liter of
               reagent water spiked with the PES  solution.  Analyze the PES as
               described in  Sections  18 to 21.

28.4  Calculations

      See Section 22 for equations necessary for calculations.

28.5  Technical Acceptance Criteria for the PES


                                     SV D-37                           6/91

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      28.5.1  The PES must be analyzed on a GC/MS system meeting the DFTPP
              tuning, initial calibration, and continuing calibration
              technical acceptance criteria at the frequency described in
              Section 28.2.

      28.5.2  The PES must be extracted and concentrated according to Section
              28.3.

      28.5.3  The PES must be prepared and analyzed with a method blank that
              met the blank technical acceptance criteria.

      28.5.4  The percent recovery for each of the surrogates in the PES must
              be within the acceptance windows listed in Table D-ll.

      28.5.5  The area response change between the PES and. the most recent
              continuing calibration standard analysis for each of the
              internal standards must be within the inclusive range of -50
              percent and +100 percent.

      28.5.6  The retention tine shift between the PES and the most recent
              continuing calibration standard analysis for each of the
              internal standards must be within ±0.33 minutes (20.0 seconds).

28.6  Corrective Action

      28.6.1  If the PES technical acceptance criteria for the internal
              standards and the surrogate are not met, check calculations,
              standard solutions and instrument performance.  It may be
              necessary to recalibrate the instrument or take other
              corrective action procedures to meet the internal standard
              criteria.  Any PES failing to meet these technical acceptance
              criteria must be reextracted and reanalyzed at no additional
              cost.  If insufficient PES spiking extract remains or if
              insufficient full volume PES remains, document this in the SDG
              Narrative by stating that the PSS could not be reextracted and
              reanalyzed because insufficient volume remained.

      28.6.2  In addition to complying with the PES technical acceptance
              criteria, the Contractor will be responsible for correctly
              identifying and quantitating the compounds included in the PES.
              SMO will notify the Contractor of unacceptable performance.

              Note:  Unacceptable performance for identification and
              quantitation of compounds is defined as a score less than 75
              percent.

      28.6.3  The PES technical acceptance criteria MUST be met before sample
              data are reported.  Also, the Contractor must demonstrate
              acceptable performance for compound identification and
              quantitation.
                                     SV D-38                           6/91

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                                                                                   TABLE D-B

                                                                     SEHIVOLATILE  INTERNAL STANDARDS UITH
                                                            CORRESPONDING TARGET ANALVTES ASSIGNED FOR QUANTITATION
1,4-Dfchlorobenzene-d4
Naphthaitne-da
Actnaphthcna-djO
Phenanthrene-dio
Chrysene-d)2
Perylene-di2
Phenol
bis(2-Chloroethyl)ether
2-Chlorophenol
2-Hethylphenol
bls(2-Chloroisopropyl)ether
4-Hethylphenol
N-Nitroso-dl-n-propytamlne
2-fluorophenol (surr)
Phenol-d6 (surr)
     C/l

     o
     UJ
Nitrobenzene
Isophorona
2-Mltrophenol
2,4-Dimethylphenol
bi*(2-Chloroethoxy)methane
2,4-Oichlorophenol
4-ChloroanHlne
Hexachlorobutadlene
4-Chloro-3-methylphenol
2-Hethylnaphthalene
N1trobenien«-dS (turr)
Hexachlorocyclopent adIene
2,4,6-Trichlorophenol
2,4,5-Trlchlorophenol
2-Chloronaphthalene
2-Nltroaniline
Dimethyl phthalate
Acenaphthylene
3-Mltroanlline
Acenaphthene
2,4-Dinltrophenol
4-Nltrophenol
Dlbcntofuran
2,4-Dlnltrotoluene
2,6-D < nl t rotoluene
DUthylphthalate
A-Chlorophenyl phenyl ether
Fluorine
4-Nltroanlline
2-Fluorobiphenyl  (surr)
2,4,6-Trlbromophenol  (surr)
4,6-Dlnltro-2-methylphenol
M-Mitrosodlphenylamlne
4-Bromophenyl phenyl ether
Hexachlorobenzene
PentachIorophenoI
Phenanthrene
Anthracene
DI-n-Butyl phthalate
Fluoranthene
Pyrene
ButylbenzylphthaUte
3,3-Dichlorobenzldlne
Benzo(a)Anthracene
bis(2-Ethylhexyl)phthalate
Chrysene
Terphenyl-dU (surr)
Dl-n-octylphthalate
Benzo(b)fIuoranthene
Benzo(k)fIuoranthene
Benio(a)pyrene
lndeno(1,2,3-cd)Pyrene
Dibeni(a,h)anthracene
Benzo(g,h,I)perylene
                 Surr =• surrogate compound

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                                  Table D-9

              Primary Quantitation Ions (m/z)  and Secondary Ions
                      for Semivolatile Organic Compounds
PaTame tei*
   Ion
Phenol
bis(2-Chloroethyl)ether
2-Chlorophenol
1,3-Dichlorobenzene
1,4-Dtchlorobenzene
1,2-Dichlorobenzene
2-Methylpheno1
2,2'-oxybis(l-Chloropropane)
4-Methylphenol
N-nitroso-di-n-propylamine
Hexachloroethane
Nitrobenzene
Isophorone
2-Nitrophenol
2,4-Dimethylphenol
bis(-2-Chloroethoxy)methane
2,4-Oichlorophenol
1,2,4-Trichlorobenzene
Naphthalene
4-Chloroaniline
Hexachlorobutadiene
4-Chloro-3-methylphenol
2-Me thylnaphthalene
Hexachlorocyclopentadiene
2,4,6-Trichlorophenol
2,4,5-Trichlorophenol
2-Chloronaphthalene
2-Nitroaniline
Dimethyl phthalate
Acenaphthylene
3-Nitroaniline
Acenaphthene
2,4-Dinitrophenol
4-Nitrophenol
Dibenzofuran
2,4-Oinitrotoluene
2,6-Dinitrotoluene
 94
93
128
146
146
146
108
 45
108
 70
117
 77
 82
139
107
 93
162
180
128
127
225
107
142
237
196
196
162
 65
163
152
138
153
184
109
168
165
165
    65, 66
   63, 95
    64, 130
   148, 113
   148, 113
   148, 113
     107
    77, 79
     107
42, 101, 130
   201, 199
    123, 65
    95, 138
    65, 109
   121, 122
    95, 123
    164, 98
   182, 145
   129, 127
     129
   223, 227
   144, 142
     141
   235, 272
   198. 200
   198, 200
   164, 127
    92, 138
   194, 164
   151, 153
   108, 92
   152, 154
    63, 154
   139, 65
      139
    63, 182
    89, 121
                                     SV D-40
                           6/91

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                            Table D-9 (continued)




Parameter                               Primary Ton        Secondary lonf
Oiethylphthalate
4 • Chlorophenyl • phenyle ther
Fluorene
4-Nitroaniline
4, 6-Dinitro-2-methylphenol
N-Nitrosodiphenylamine
4 - Bromophenyl - phenyle ther
Hexachlorobenzene
Pentachloropheno 1
Phenanthrene
Anthracene
Di - n- butylphthalate
Fluoranthene
Pyrene
Butylbenzylphthalate
3,3' -Dichlorobenzidine
Benzo (a) anthracene
b is ( 2 - Ethylhexyl ) phthalate
Chrysene
Di-n-octyl phthalate
Benzo (b ) fluoranthene
Benzo (k) fluoranthene
Benzo (a) pyr one
Zndeno ( 1 , 2 , 3 - cd) pyrene
Oibenz ( a , h) anthracene
Benzo ( g , h , i ) perylene
Surrogates
Phenol -d5
2 - Fluor ophenol
2,4, 6 -Tribromophenol
Nitrobenzene £5
2 - Fluor ob ipheny 1
Terphenyl
Internal Standards
1 , 4-Dichlorobenzene - 04.
Naphthalene - dg
Acenapthene -d^Q
Phenanthrene - d^Q
Chrysene -dj^2
Perylene -d^2
149
204
166
138
198
169
248
284
266
178
178
149
202
202
149
252
228
149
228
149
252
252
252
276
278
276

99
112
330
82
172
244

152
136
164
188
240
264
177, 150
206, 141
165, 167
92, 108
182. 77
168, 167
250, 141
142, 249
264, 268
179, 176
179, 176
150, 104
101, 100
101, 100
91, 206
254, 126
229, 226
167, 279
226, 229
-
253, 125
253, 125
253, 125
138, 227
139, 279
138, 277

42, 71
64
332, 141
128, 54
171
122, 212

115
68
162, 160
94,80
120,236
260, 265
                                    SV D-41                           6/91

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                                  TABLE D-10
                ACCEPTANCE CRITERIA FOR INITIAL AND CONTINUING
                CALIBRATION FOR SEMIVOLATILE ORGANIC COMPOUNDS
Semlvolatile
Compounds
Phenol
bis (2 -Chloroethyl) ether
2 - Chlorophenol
2-Methylphenol
4-Methylphenol
N-Nitroso-dl-n-propylamine
Hexachloroe thane
Nitrobenzene
Isophorone
2-Nitrophenol
2 , 4-Dinethylphenol
bis (2-Chloroethoxy)me thane
2 , 4-Dichlorophenol
1,2, 4-Trichlorobenzene
Naphthalene
4 -Chloro - 3 -me thylphenol
2 -Methylnaphthalene
2,4, 6-Trichlorophenol
2,4, 5-Trichlorophenol
2 - Chloronaphthalene
Acenaphthylene
Acenaphthene
Dibenzofuran
2 , 4 -Dinitro toluene
2 , 6-Dinitrotoluene
4 - Chloropheny 1 - pheny le Cher
Fluorene
4 - Bromopheny 1 - pheny lether
Hexachlorobenzene
Pentachloropheno 1
Phenanthrene
Anthracene
Fluoranthene
Pyrene
Benzo (a) anthracene
Chrysene
Benzo (b ) fluoranthene
Benzo (k) fluoranthene
Benzo(a)pyrene
Indeno (1,2,3-cd) pyr ene
Dibenzo (a, h) anthracene
Benzo ( g , h , i ) perylene
Minimum
RRF
0.800
0.700
0.700
0.700
0.600
0.500
0.300
0.200
0.400
0.100
0.200
0.300
0.200
0.200
0.700
0.200
0.400
0.200
0.200
0.800
1.300
0.800
0.800
0.200
0.200
0.400
0.900
0.100
0.100
0.050
0.700
0.700
0.600
0.600
0.800
0.700
0.700
0.700
0.700
0.500
0.400
0.500
Ma-vtimmi
%RSD
20.5
20.5
20.5
20.5
20.5
20.5
20.5
20.5
20.5
30.0
30.0
20.5
20.5
20.5
20.5
20.5
20.5
20.5
20.5
20.5
20.5
20.5
20.5
30.0
20.5
20.5
20.5
20.5
20.5
20.5
20.5
20.5
20.5
20.5
20.5
20.5
20.5
20.5
20.5
20.5
20.5
20.5
Maximum
%Diff
±25.0
+25.0
±25.0
±25.0
+25.0
±25.0
±25.0
±25.0
±25.0
±30.0
±30.0
±25.0
+25.0
±25.0
±25.0
±25.0
±25.0
±25.0
+25.0
±25.0
±25.0
+25.0
±25.0
±30.0
±25.0
±25.0
+25.0
+25.0
±25.0
+25.0
+25.0
±25.0
±25.0
+25.0
+25.0
±25.0
+25.0
±25.0
±25.0
+25.0
±25.0
±25.0
(continued)


                                     SV D-42                           6/91

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                                  TABLE D-10
                ACCEPTANCE CRITERIA FOR INITIAL AND CONTINUING
                CALIBRATION FOR SEMIVOLATILE ORGANIC COMPOUNDS
Semivolatile
Compounds	
 RRF
Maximum
 %RSD
Maximum
 %Dlff
Phenol -d5
2 - Fluorophenol
2 - Fluorobipheny 1
0.800
0.600
0.500
0.700
 20.5
 20.5
 20.5
 20.5
  ±25.0
  ±25.0
  +25.0
  +25.0
The following compounds have no maximum %RSD or maximum %D criteria, but must
meet a minimum RRF criterion of 0.010:
2,2'-oxybis(1-Chloropropane)
4-Chloroaniline
Hexachlorobutadiene
Hexachlorocyclopentadiene
2-Nitroaniline
DimethyIphthalate
3-Nitroaniline
2,4-Dinitrophenol
4-Nitrophenol
Diethylphthalate
  4-Nitroaniline
  4,6-Dinitro-2-methyIpheno 1
  N-Nitrosodiphenylamine
  01-n-butyIphthalate
  ButylbenzyIphthalate
  3,3'-Dichlorobenzidine
  bis(2-Ethylhexyl)phthalate
  Di-n-octyIphthalate
  2,4,6-Tribromopheno1
  Nitrobenzene-d
                                     SV D-43
                               6/91

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                       EXHIBIT D
METHOD FOR THE ANALYSIS OF LOW CONCENTRATION WATER FOR
                PESTICIDES AND AROCLORS
                         PEST D-l                          6/91

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                              Table of Contents
                                                                   Page
SECTION I:    Introduction	PEST D-3

SECTION II:
              Part A - Sample Storage and Holding
                         Tines 	PEST D-4
              Part B - Equipment and Standards 	PEST D-5

SECTION III:  Instrument Quality Control Procedures
                and Requirements
              Part A - Instrument Operating Conditions 	PEST 0-15
              Part B - Calibration of the GC/ECD System	PEST D-15

SECTION IV:   Sample Preparation, Extraction and
                Cleanup 	PEST D-27

SECTION V:    Sample Analysis and Compound
                Identification and Quantitation	PEST D-35

SECTION VI:   Sample Quality Control Procedures
                and Requirements 	PEST D-44
                                     PEST D-2
6/91

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                                   SECTION  I
                                 INTRODUCTION
The analytical method that follows is designed to analyze water in order to
determine the presence and concentration of the chlorinated pesticides and
Aroclors found in the Target Compound List (Exhibit C).  The majority of the
samples are expected to be from drinking water and well/ground water sources
around Superfund sites.  The method can be used for determining analyte
concentrations as low as ten parts per trillion.  The method is based on EPA
Method 608.  Quality control requirements are incorporated in the method in
order to maximize GC/ECD sensitivity and column resolution and to minimize
contamination of the samples from laboratory sources.

Resolution difficulties have been associated with the following pairs of
compounds using this method:

o   On a DB-608  or equivalent column,  ODE and dieldrin;  Methoxychlor and
    Endrin ketone;  and Endosulfan I and gamma-Chlordane.

o   On a DB-1701 or equivalent column,  Endosulfan I  and gamma - Chlor dane;  and
    Methoxychlor and Endosulfan sulfate.
                                     PEST D-3                          6/91

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                                  SECTION II


FART A - SAMPLE STORAGE AND HOLDING TIMES.

1.    PROCEDURES FOR SAMyrfl STORAGE
      The samples mist be protected from light and refrigerated at 4'C (±2*C)
      from the tine of receipt until 60 days after delivery of a complete
      reconciled sample data package.  After 60 days the samples may be
      disposed of in a manner that complies with all applicable regulations.

      The samples must be stored in an atmosphere demonstrated to be free of
      all potential contaminants and in a refrigerator used only for storage
      of samples received under this contract.

      Samples, sample extracts, and standards must be stored separately.

2.    PROCEDURE TOR gAU^TJ; ETfBACf STORAGE
      Sample extracts must be protected from light and stored at 4*0 (±2'C)
      until 365 days after delivery of a complete data package.

      Sample extracts must be stored in an atmosphere demonstrated to be free
      of all potential contaminants.

      Samples, sample extracts,  and standards must be stored separately.

      CONTRACT REOUTBifl* HOLDING  TIMES

      The extraction of all samples must be started within 5 days of the
      Validated Time of Sample Receipt (VTSR) .

      Analysis of samples must be completed within 40 days following the
      stare of extraction.
                                     PEST D-4                          6/91

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 PART B - ffinil'PMENT AND STANDARDS

 3.    SUMMARY OF METHOD

 3.1   A one liter aliquot of sample is spiked with the surrogate solution and
       extracted with methylene chloride by using a continuous liquid- liquid
       extractor.  The methylene chloride extract is dried and concentrated,
       exchanged to hexane,  cleaned up to remove interferences, and adjusted
       to a final volume of 2.0 mL.

 3.2   The hexane extract is injected onto two wide-bore capillary columns in
       a gas chromatograph (GC) .  The gas chromatograph is temperature
       programmed to separate the pesticides and Aroclors which are then
       detected with an electron capture detector (ECD) .   Calibration and run
       sequence specifications of the GC/ECD method apply independently to
       both GC columns.

 3.3   A single component pesticide  is identified if a peak is detected within
       its appropriate retention time window on each of two GC columns.
       Quantitative analysis of pesticides/Aroclors must be accomplished by
       the external standard method.   Single component analytes and the
       surrogates must be analyzed at three concentrations during the initial
       calibration.

 3.4   Toxaphene and Aroclors are identified primarily by pattern recognition,
       but retention times of three  to five major peaks must also be taken
       into consideration.   Single-point calibrations for multicomponent
       analytes  are  sufficient for quantitation by this method.   Standards for
       identified Aroclors and Toxaphene must be run within 72 hours of the
       sample  analysis in which they  were observed.   These standards are used
       to  verify identification only;  quantitation is based on the standards
       analyzed  during initial calibration.
4.1   Method interferences may be caused by contaminants in solvents,
      reagents, glassware, and sample processing hardware.  These
      contaminants lead to discrete artifacts or to elevated baselines  in  gas
      chroma to grams.  These materials must be routinely demonstrated to be
      free from interferences under the sample preparation and analysis
      conditions by analyzing instrument blanks and method blanks.
      Interferences caused by phthalate esters can pose a major problem in
      pesticide analysis.  Because common flexible plastics contain varying
      amounts of phthalates which are easily extracted during laboratory
      operations, cross -contamination of glassware frequently occurs when
      plastics are handled.  Interferences from phthalates can best be
      minimized by avoiding the use of such plastics in the laboratory.

4.2   Matrix interferences may be caused by contaminants that are co-
      extracted from the sample.   The extent of matrix interferences will
      vary considerably from source to source, depending upon the nature of
      the site being sampled.  The cleanup procedures in Section 12 must be
      used to remove such interferences in order to achieve the Contract
      Required Quantitation Limits (CRQL).

                                     PEST D-5                          6/91

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5.    APPARATUS AND

      Brand names, suppliers, and part numbers are for illustrative purposes
      only.  No endorsement is implied.  Equivalent performance may be
      achieved using apparatus and materials other than those specified here,
      but demonstration of equivalent performance meeting the requirements of
      method is the responsibility of the Contractor.

5.1   Gas Chromatograph/Electron Capture Detector (GC/ECD)

      5.1.1   Gas Chromatograph

              5.1.1.1    The gas chromatograph (GO) system must regulate
                         temperature in order to give a reproducible
                         temperature program and have a flow controller that
                         maintains a constant column flow rate throughout the
                         temperature program.  The system must be suitable
                         for splitless injection and have all required
                         accessories including syringes, analytical columns,
                         and gases.

              5.1.1.2    Gas chromatographs that are available from some
                         manufacturers may have difficulty in meeting certain
                         method QC requirements because of Endrin and DDT
                         breakdown in the injector.  This problem can be
                         minimized by operating the injector at 200-205'C,
                         using a Pvrex (not quartz) methyl silicone
                         deactivated injector liner, and deactivating any
                         metal parts in the injector with dichlorodimethyl
                         silane.  In some cases, using a 0.25-inch packed
                         column injector converted for use with 0.53 mm
                         capillary columns works better than a Grob-type
                         injector.  If a Grob-type injector is used, a 4 mm
                         liner may be required to meet breakdown criteria.

      5.1.2   Gas Chromatograph Columns

              5.1.2.1    Two wide-bore (0.53 mm ID) fused silica GC columns
                         are required.  A separate detector is required for
                         each column.  The specified analytical columns are a
                         DB-1701, 30 m x 0.53 mm ID, 1.0 urn film thickness,
                         Jfiff Scientific, Folsom, CA, and a DB-608, 30 m x
                         0.53 mm ID, 0.5 to 1.0 urn film thickness from J&tf
                         Scientific.  Equivalent columns may be employed if
                         they meet the requirements in Section III.

              5.1.2.2    Columns are mounted in 0.25-inch injector ports by
                         using glass adapters available from a variety of
                         commercial sources (J&W Scientific, Supelco, Inc.,
                         Hewlett-Packard, Varian, Inc., Perkin Elmer, or
                         equivalent).  The two columns may be mounted into a
                         single injection port with a tee adapter,  (Supelco,
                         Inc., Beliefonte, PA, Catalog No. 2-3660, or
                         equivalent).  Use of this adapter allows

                                     PEST D-6                          6/91

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                         simultaneous injection onto both columns.
                         Laboratories should follow the manufacturer's
                         recommendation on mounting 0.53 mm capillaries into
                         injection ports.

      S.I.3   The carrier gas for routine applications is helium.
              Laboratories may choose to use hydrogen as a carrier gas, but
              they must  clearly identify its use in the SDG Narrative and on
              all divider pages preceding raw chromatographic data in
              submissions to SMO.  Laboratories that choose to use hydrogen
              are advised to exercise caution in its use.  Use of a hydrogen
              leak detector is highly recommended if hydrogen is  used as a
              carrier gas.  All GO carrier gas lines must be constructed from
              stainless  steel or copper tubing.  Non-polytetrafluoroethylene
              (PTFE) thread sealants, or flow controllers with rubber
              components are not to be used.

      5.1.4   Electron Capture Detector - The makeup gas must be  P-5, P-10
              (argon/methane) or nitrogen according to the instrument
              specification.  The GC/ECD system must be in a room in which
              the atmosphere has been demonstrated to be free of  all
              contaminants which may interfere with the analysis.  The
              instrument must be vented to outside the facility or to a
              trapping system which prevents the release of contaminants into
              the instrument room.

      5.1.5   Data System - A data system must be interfaced to the GC/ECD.
              The data system must allow the continuous acquisition of data
              throughout the duration of the chromatographic program and must
              permit, at the minimum, the output of time vs. intensity  (peak
              height or  peak area) data.  Also, the data system must be able
              to rescale chromatographic data in order to report
              chromatograms meeting the requirements listed within this
              method.

5.2   Glassware - A set of glassware sufficient to meet contract  requirements
      must be reserved for exclusive use in this contract.

      5:2.1   Continuous liquid-liquid extractors equipped with Teflon or
              glass connecting lines for use with methylene chloride
              (Hershberg-Wolf Extractor, Ace Glass Company, Vineland, NJ, P/N
              6841-10, or equivalent).

      5.2.2   Concentrator tube - Kude ma-Danish, 10 mL, graduated  (Kontes,
              Vineland,  NJ K-570050-1025, or equivalent).

      5.2.3   Evaporative flask - Kuderna-Danish, 500 mL  (Kontes  K-570001  -
              0500, or equivalent).  Attach to concentrator tube  with
              springs.

      5.2.4   Snyder column - Kuderna-Danish, three-ball macro  (Kontes
              K-50300-0121, or equivalent).
                                     PEST D-7                          6/91

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      5.2.5    Drying column,  chromatographic  column approximately 400 mm  long
               x 19 mm ID.  with coarse  frit.   (Substitution of a small pad of
               disposable Pyrex glass wool for the  frit will help prevent
               cross-contamination of sample extracts.)

      5.2.6    Pipet,  Volumetric 1.00 mL or 2.00 mL (optional).

      5.2.7    Microsyringe, 1.0 uL and larger, 0.006  inch ID needle.

      5.2.8    Syringe,  1.00 mL or 2.00 mL (optional).

      5.2.9    Flask,  Volumetric 10.00  mL.

      5.2.10   Flask,  Volumetric 1.00 mL or 2.00 mL (optional).

      5.2.11   Snyder column,  micro two or three ball  with a 19 mm ground
               glass joint.

      5.2.12   Glass vials, minimum of  20  mL,  with  screw cap and Teflon  or
               aluminum foil liner.

      5.2.13   Vials,  10 mL, with screw cap and Teflon liner (optional).

      5.2.14   Vials and caps,  1 or 2 mL for GC auto sampler.

      5.2.15   Bottle or test  tube,  50  mL with Teflon-lined screw cap for
               sulfur removal.

      5.2.16   Centrifuge tubes,  calibrated, 12 mL, for sulfur removal.

      5.2.17   Micropipet,  250 uL,  with disposable  tips.

5.3   pH Paper, wide range.

5.4   Boiling chips.

      5.4.1    Silicon carbide boiling  chips,  approximately 10 to 40 mesh.
               Heat the chips  to 400*0  for 30  minutes  or solvent rinse before
               use.

      5.4.2    Teflon boiling  chips (optional).  Solvent rinse the chips
               before  use.

5.5   Water bath, heated, with concentric ring cover,  capable of temperature
      control.  NOTE:  To prevent the release of solvent fumes into the
      laboratory, the water bath must be used in a hood.

5.6   Balance.  Analytical, capable of accurately weighing ±0.0001 g.  The
      balances must be calibrated with class S weights once per each 12-hour
      workshift.  The balances must also be annually checked by a certified
      technician.
                                     PEST D-8                          6/91

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5.7   Nitrogen evaporation device equipped with a heated bath that can be
      maintained at 30 to 35*C (N-Evap by Organomation Associates,  Inc.,
      South Berlin, HA, or equivalent).  To prevent the release of solvent
      fumes into the laboratory,  the nitrogen evaporation device must be  used
      in a hood.

5.8   Florisil Cleanup Equipment

      5.8.1   Florisil bonded silica.  1-g cartridges with stainless steel or
              Teflon frits, Catalog No. 694-313  (Analytichem, 24201 Frampton
              Ave., Harbor City, CA, or equivalent).

      5.8.2   Vacuum system for  eluting multiple cleanup cartridges.  Vac
              Elute Manifold, Analytichem International  (J.T. Baker, or
              Supelco) or equivalent.

      5.8.3   Vacuum trap made from a  500 mL sidearm flask fitted with a one-
              hole stopper and glass tubing.

      5.8.4   Vacuum pressure gauge.

      5.8.5   Rack for holding 10 mL volumetric  flasks  in the manifold.

5.9   Mechanical shaker or mixer, for sulfur removal.

6.
6.1   Sodium sulfate, granular-anhydrous reagent grade, heated at 400"C for 4
      hours, or at 120*C for 16 hours, cooled in a desiccator, and stored in
      a glass bottle.  Each lot must be extracted with hexane and analyzed by
      GC/ECD to demonstrate that it is free of interference before use (J.T.
      Baker anhydrous granular, Catalog No. 3375, or equivalent).

6.2   Methylene chloride, hexane, acetone, toluene, iso-octane, and methanol
      (optional), pesticide quality, or equivalent.  It is recommended that
      each lot of solvent be analyzed to demonstrate that it is free of
      interference before it is used.  Methylene chloride must be certified
      as acid free or must be tested to demonstrate that it is free of
      hydrochloric acid.  Acidic methylene chloride must be passed through
      basic alumina and then demonstrated to be free of hydrochloric acid.

6.3   Mercury, triple distilled, for sulfur clean-up.

6.4   Copper powder (optional), fine, granular (Mallinckrodt 4649 or
      equivalent).  Copper may be used instead of mercury for sulfur clean-
      up.  Remove oxides by treating with dilute nitric acid, rinse with
      distilled water to remove all traces of acid, rinse with acetone, and
      dry under a stream of nitrogen.

6.5   Sodium hydroxide solution (10 N) .  Carefully dissolve 40 g of NaOH  in
      reagent water and dilute the solution to 100 mL.

6.6   Concentrated sulfuric acid, (Sp. Gr. 1.84).


                                     PEST D-9                          6/91

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6.7   Nitric acid, dilute, for sulfur removal with copper.

6.8   Reagent water.  Reagent water is defined as a water in which no target
      analyte is observed at the CRQL for that compound.

      6.8.1   Reagent water nay be generated by passing tap water through a
              carbon filter bed containing about 453 g (1 Ib.) of activated
              carbon (Calgon Corp., Filtrasorb-300, or equivalent).

      6.8.2   Reagent water may be generated using a water purification
              system (Millipore Super -Q or equivalent) .
6 . 9   Ten percent acetone in hexane (v/v) .  Prepare by f*«M»ig 10 . 0 mL of
      acetone to 90.0 mL of hexane.  NOTE:  Prepare this mixture accurately
      or the results from the Florisil cartridge cleanup will be adversely
      affected.  Vater in the acetone will also adversely affect Florisil
      performance.

7.    STANDARDS

7.1   The Contractor must provide all standards to be used with this
      contract.  These standards may be used only after they have been
      certified according to the procedure in Exhibit E.  The Contractor must
      be able to verify that the standards are certified.  Manufacturer's
      certificates of analysis must be retained by the Contractor and
      presented upon request.

7.2   Stock standard solutions (1.00 ug/uL) - Stock standard solutions may be
      purchased as certified solutions or prepared from pure standard
      materials.

      7.2.1   Prepare stock  standard solutions by accurately weighing about
              0.0100 g of pure material.  Dissolve the material in  toluene,
              dilute to volume in  a 10 mL volumetric flask with toluene  or
              acetone.  Larger volumes may be used at the convenience of the
              analyst.

      7.2.2   When compound  purity is assayed to be 97 percent or greater,
              the weight may be used without correction  to calculate  the
              concentration  of the stock solution.  If the compound purity is
              assayed to be  less than 97 percent, the weight must be
              corrected when calculating the concentration of the stock
              solution.

      7.2.3   Fresh stock standards must be prepared once every twelve
              months, or sooner, if standards have degraded or concentrated.
              Stock standards must be checked for signs  of degradation or
              concentration  just prior to preparing working standards from
              them.
                                     PEST D-10                         6/91

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7.3   Working Standards

      7.3.1   Surrogate Standard Spiking Solution

              The surrogates, tetrachloro-m-xylene and decachlorobiphenyl,
              are added to all standards, samples, and blanks.  Prepare a
              surrogate spiking solution of 0.20 ug/mL of each of the two
              compounds in acetone.  The solution should be checked
              frequently for stability.  The solution oust be replaced after
              six months or at an earlier time, if the solution has degraded
              or concentrated.

      7.3.2   Resolution Check Mixture

              The Resolution Check Mixture is composed of the pesticides and
              surrogates at the concentrations listed below in hexane or iso-
              octane.  The mixture must be prepared every six months or
              sooner, if the solution has degraded or concentrated.

                         Compounds          Concentration fng/mL)

                         gamma-Chlordane              10.0
                         Endosulfan I                 10.0
                         p,p'-DDE                     20.0
                         Dieldrin                     20.0
                         Endosulfan sulfate           20.0
                         Endrin ketone                20.0
                         Methoxychlor                100.0
                         Tetrachloro-m-xylene         20.0
                         Decachlorobiphenyl           20.0

      7.3.3   Performance Evaluation Mixture

              The Performance Evaluation Mixture is prepared in hexane or
              iso-octane as listed below.  The PEM must be prepared weekly or
              more often, if the solution has degraded or concentrated.

                         ComDounds          Concentration (tip /m1L)
                         gamma-BHC                    10.0
                         alpha-BHC                    10.0
                         4,4'-DDT                    100.0
                         beta-BHC                     10.0
                         Endrin                       50.0
                         Methoxychlor                250.0
                         Tetrachloro-m-xylene         20.0
                         Decachlorob iphenyl           20.0

      7.3.4   Single Component Pesticides

              The Individual Standard Mixture solutions must be prepared in
              either hexane or iso-octane.  The concentrations of the
              pesticides in the low point standard mixtures are given  below.
              The midpoint concentration must be 4 times the low  point

                                     PEST D-ll                         6/91

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         concentration  for each analyte, including the surrogates.  The
         high concentration must be at least 16 times the low point
         concentration  for each analyte, including the surrogates, but a
         higher concentration may be chosen by the Contractor.  The high
         point concentration defines the upper end of the concentration
         range for which the calibration is valid.  The solution oust be
         prepared every 6 months or sooner, if the solution has degraded
         or concentrated.
                 Low Point
               Concentration
                 (ng/aLl
    Individual
  Standard Mix A

alpha-BHC                5.0
Heptachlor               5.0
gamma-BBC                5.0
Endosulfan I             5.0
Dieldrin                10.0
Endrin                  10.0
p.p'-DDD                10.0
p.p'-DDT                10.0
Methoxychlor            50.0
Tetrachloro-m-xylene     5.0
Decachlorob ipheny1      10.0
  Individual
Standard Mix B

beta-BHC
delta- BHC
Aldrin
Heptachlor epoxide
alpha-Chlordane
gamna-Chlordane
p.p'-DDE
Endosulfan sulfate
Endrin aldehyde
Endrin ketone
Endosulfan II
Tetrachloro-m-xylene
Decachlorobiphenyl
  Low Point
Concentration
    (ng/mL)
                                                            .0
                                                            .0
                                                            .0
                                                            .0
                                                            .0
                                                            .0
     5.
     5.
     5.
     5.
     5.
     5.
    10.0
    10.0
    10.0
    10.0
    10.0
     5.0
    10.0
7.3.5   Multicomponent Standards
        Toxaphene and Aroclor standards must be prepared individually
        except for Aroclor 1260 and Aroclor 1016 which nay be combined
        in one standard mixture.  The calibration standards for the
        Aroclors must be prepared at concentrations of 100 ng/mL,
        except for Aroclor 1221 which must be prepared at 200 ng/mL.
        Toxaphene must be prepared at 500 ng/mL.  All multicomponent
        standards must contain the surrogates at 20.0 ng/mL.  The
        Aroclor and Toxaphene solutions must be prepared in hexane or
        iso-octane.  Each solution must be prepared every 6 months, or
        sooner, if the solution has degraded or concentrated.

7.3.6   Florisil Cartridge Check Solution

        Prepare a 0.10 ug/mL solution of 2,4,5-trichlorophenol in
        acetone.  The solution must be prepared every 6 months, or
        sooner, if the solution has degraded or concentrated.

7.3.7   Laboratory Control Sample (LCS) Spiking Solution

        Prepare a laboratory control sample (LCS) spiking solution  that
        contains each of the analytes at the concentrations listed
        below in methanol or acetone.  The LCS solution must be
        prepared every six months or sooner, if the solution has
        degraded or concentrated.
                               PEST D-12
                                                                       6/91

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               Compounds                 Concentration f*'g/"'Tr)
               gamma-BHC                            0.10
               Heptachlor epoxide                  0.10
               Dieldrin                            0.20
               4,4'-DDE                            0.20
               Endrin                               0.20
               Endosulfan sulfate                  0.20
               gamna-Chlordane                     0.10

7.4   Storage of Standards

      7.4.1    Store the  stock and secondary standard solutions  at -10*C to -
               20*C in Teflon-lined screw-cap amber bottles.

      7.4.2    Store the  working standard solutions at 4*C (±2'C)  in Teflon-
               lined screw-cap amber bottles.  The working standards must be
               checked frequently for signs  of degradation or evaporation.

      7.4.3    Protect all standards from light.

      7.4.4    Samples, sample extracts,  and standards must be stored
               separately.
                                     PEST D-13                         6/91

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                     SECTION in
mSTBIJMEHT QUALITY COHTROL PROCEDURES AHD REQUIREMEHTS
                         PEST D-14                         6/91

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PART A - INSTRUMENT OPERATING CONDITIONS

8.    GAS CHROMATOGRAPH / ELECTRON CAPTURE DETECTOR

      The following are the gas chromatographic analytical conditions.   The
conditions are recommended unless otherwise noted.


      Carrier Gas:                  Helium
      Column Flow:                  5 aL/min

      Make-up Gas:                  Argon/Methane (P-5 or P-10)  or N2
                                    (required)

      Injector Temperature:         > 200*C (required)

      Injection Technique:          On-column

      Injection Volume:             1 or 2 ul (see note below)

      Injector:                     Grob-type, splitless

      Initial Temperature:          150*C

      Initial Hold Time:            1/2 min
      Temperature Ramp:             S"C to 6'C/ain

      Final Temperature:            275*C

      Final Hold Time:              After Decachlorobiphenyl has eluted
                                    (approximately 10 minutes)

      Optimize GC conditions for analyte separation and sensitivity.   Once
      optimized, the same GC conditions must be used for the analysis of all
      standards, samples, blanks, performance evaluation samples and
      laboratory control samples.  NOTE:  Manual injections must be 2.0 uL.
      Auto injectors may use 1.0 uL volumes.  The same injection volume must
      be used for all standards, blanks, and samples.

      The linearity of the ECD may be greatly dependent on the  flow rate of
      the make-up gas.  Care must be taken to maintain stable and appropriate
      flow of make-up gas to the detector.

      Cold (ambient temperature) on-column injectors that allow injection
      directly onto a 0.53 mm ID column may be used as long as  the acceptance
      criteria for resolution, calibration, and analyte breakdown are met.
                                     PEST D-15                        6/91

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PART B - CALIBRATION OF THE GC/ECD SYSTEM

9.    INITIAL CALIBRATION

9.1   Summary

      Prior to sample analysis,  each GC/ECD system oust be initially
      calibrated at a minimum of three concentrations for single component
      analytes in order to determine instrument sensitivity and the linearity
      of GC response.  Each multicomponent analyte is analyzed at one
      concentration.

9.2   Frequency

      Each GC/ECD system must be initially calibrated upon award of the
      contract, whenever major instrument maintenance or modification is
      performed (e.g., column replacement or repair,  cleaning or replacement
      of ECD,  etc.) , or if the calibration verification technical acceptance
      criteria have not been met.

9.3   Procedure

      9.3.1    Set up  the GC/ECD  system as described in Section 8.

      9.3.2    Prepare the initial calibration standards using the procedures,
               the analytes, and  the concentrations according to Section 7.

      9.3.3   All standards, samples, and blanks must be allowed to warm  to
               ambient temperature before preparation or analysis.

      9.3.4   Analyze the initial calibration sequence as given below.  NOTE:
               Steps 16 and 17 are used as part of the calibration
              verification as well  (see Section 10).

                         INITIAL CALIBRATION SEQUENCE

                              1.  Resolution Check
                              2.  Performance Evaluation Mixture
                              3.  Aroclor 1016/1260
                              4.  Aroclor 1221
                              5.  Aroclor 1232
                              6.  Aroclor 1242
                              7.  Aroclor 1248
                              8.  Aroclor 1254
                              9.  Toxaphene
                             10.  Low Point Standard A
                             11.  Low Point Standard B
                             12.  Midpoint Standard A
                             13.  Midpoint Standard B
                             14.  High Point Standard A
                             15.  High Point Standard B
                             16.  Instrument Blank
                             17.  Performance Evaluation Mixture
                                     PEST D-16                         6/91

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9.4   Calculations

      9.4.1   For each single component pesticide and surrogate, a retention
              time (RT) is measured in each of three of the calibration
              standards analyses (low point, midpoint, high point) during the
              initial calibration for Individual Standard Mixture A and
              Individual Standard Mixture B.  The RT for the surrogates is
              measured from the Individual Standard Mixture A analyses.  The
              mean RT is calculated as the average of the three values.
              Calculate a mean absolute retention time (RT) for each single
              component pesticide and surrogate using Equation D.22.

                         	    n
              EQ. D.22.  RT  - Z
                              1-1
              RT  - Mean absolute retention time of analyte.

              RTi - Absolute retention time of analyte.

              n   - Number of measurements (3).

      9.4.2    A retention time window is calculated for each single component
              analyte and surrogate and for the major peaks (3 to 5) of each
              multicomponent analyte by using Table D.13.  Windows are
              centered around the average absolute retention time for the
              analyte established during the initial calibration.

                                         TABLE D.13

                         RETENTION TIME WINDOWS  FOR SINGLE AND MULTICOMPONENT
                                   ANALYTES AND  SURROGATES.
                                                 Compound Identification
                           Compound                Window (minutes)

                         alpha-BHC                        ±0.05
                         beta-BHC                         ±0.05
                         gamma-BBC                        ±0.05
                         delta-BHC                        ±0.05
                         Heptachlor                       ±0.05
                         Aldrin                            ±0.05
                         alpha-Chlordane                  ±0.07
                         gamma-Chlordane                  ±0.07
                         Heptachlor epoxide               ±0.07
                         Dieldrin                         ±0.07
                         Endrin                            ±0.07
                         Endrin  aldehyde                  ±0.07
                         Endrin  ketone                    ±0.07
                         DDD                              ±0.07
                         DDE                              ±0.07
                         DDT                              ±0.07

                                    PEST D-17                         6/91

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                                   TABLE D.13 (continued)

                   RETENTION TIME WINDOWS FOR SINGLE AND MULTICOMPONENT
                             ANAIYTES AND SURROGATES.
                                           Compound Identification
                     Compound                Window (minutes)

                   Endosulfan I                     ±0.07
                   Endosulfan II                    ±0.07
                   Endosulfan sulfate               ±0.07
                   Hethoxychlor                     ±0.07
                   Aroclors                         ±0.07
                   Toxaphene                        ±0.07
                   Tetrachloro-m-xylene             ±0.OS
                   Decachlorobiphenyl               ±0.10

9.4.3   The linearity of the instrument is determined by calculating a.
        percent relative standard deviation  (%RSD) of the calibration
        factors from a three-point calibration curve for each of the
        single component pesticide and surrogates.  Either peak area or
        peak height may be used to calculate calibration factors used
        in the %RSD equation.  For example,  it is permitted  to
        calculate linearity for endrin based on peak area and to
        calculate linearity for aldrin based on peak height.  It is not
        permitted within a %RSD calculation  for an analyte to use
        calibration factors calculated from both peak area and peak
        height.  For example, it is not permitted to calculate the
        calibration factor for the low point standard for endrin using
        peak height and calculate the midpoint and high point standard
        calibration factors for endrin using peak area.

        9.4.3.1    Calculate the calibration factor for each single
                   component pesticide and surrogate over the initial
                   calibration range using Equation D.23.

        9.4.3.2    Calculate the mean and the %RSD of the calibration
                   factors for each single component pesticide and
                   surrogate over the initial calibration range using
                   Equation D.24 and Equation D.25.

        EQ. D.23  CF —  Peak Area (or Height) of the Standard
                                  Mass Injected (ng)

                        n
                  —    2  CF*
        EQ. D.24  CF - i-1
        EQ. D.25  % RSD -  SDcF
                               PEST D-18                         6/91

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               %D     -  Percent Difference
                     ~  nominal concentration of each analyte
               ccalc  ~ Calculated concentration of each analyte from the
                       analyses of the standard

      9.4.7    Calculate the resolution between the analytea in the Resolution
               Check Mixture and the midpoint concentrations of individual
               standard mixtures A and B using Equation D.31.

               EQ. D.31   % Resolution - jj  * 100%


               V - Depth of the valley between the two peaks.  The depth of
                  the valley is measured along a vertical line from the level
                  of the apex of the shorter peak to the floor of the valley
                  between the two peaks.
               H - Height of the shorter of the adjacent peaks

9.5   Technical Acceptance Criteria For Initial Calibration

      All initial calibration technical acceptance criteria apply
      independently to both GC columns.

      9.5.1    The initial calibration sequence must be analyzed according to
               the procedure and in the order listed in Section 9.3, at the
               concentrations listed in Section 7, and at the frequency listed
               in Section 9.2.  The GC/ECD operating conditions optimized in
               Section 8 must be followed.

      9.5.2    The resolution between two adjacent peaks in the Resolution
               Check Mixture must be greater than or equal to 60.0%.  On the
               DB-1701 GC column, resolution difficulties are most likely
               between Endosulfan I and gamma- Chlordane and between
               Methoxychlor and endosulfan sulfate.  On the DB-608 GC column,
               the poorest resolution will probably be between p.p'-DDE and
               Dieldrin; Methoxychlor and Endrin ketone; and Endosulfan I and
               gamna- Chlordane .

      9.5.3    All single component pesticides and surrogates in both runs of
               the Performance Evaluation Mixture (PEM) must be 100 percent
               resolved.

      9.5.4    The absolute retention times of each of the single component
               pesticides and surrogates in both runs of the PEM must be
               within the retention time window determined from the three -
               point initial calibration in paragraph 9.4.2.
                                     PEST D-20                         6/91

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9.S.5    The  absolute value of the percent difference of the calculated
         amount and the  true amount for each of the single component
         pesticides and  surrogates in both of the PEM runs must be less
         than or equal to 25.0 percent, using Equation D.30.

9.5.6    The  percent breakdown of DOT and endrin in each of the PEM runs
         must be less than or equal to 20.0 percent.  The combined
         breakdown of DDT and endrin must be less than or equal to 30.0
         percent.

9.5.7    The  %RSD of the calibration factors for each single component
         target compound must be less than or equal to 20.0 percent,
         except as noted.  The %RSD of the calibration factors for the
         two  surrogates  must be less than or equal to 30.0 percent.  Up
         to two single component target compounds (but not surrogates)
         may  exceed the  20.0 percent limit for %RSD, but those compounds
         must have a %RSD of less than or equal to 30.0 percent.

9.5.8    The  resolution  between any two adjacent peaks in the midpoint
         concentrations  of Individual Standard Mixtures A and B in the
         initial calibration must be greater than or equal to 90.0
         percent.

9.5.9    All  instrument  blanks must meet the technical acceptance
         criteria in Paragraph 20.3.4.

9.5.10   The  identification of single component pesticides by gas
         chromatographic methods is based primarily on retention time
         data.   The retention time of the apex of a peak can only be
         verified from an on-scale chromatogram.  The identification of
         multicomponent  analytes by gas chromatographic methods is based
         primarily on recognition of patterns of retention times
         displayed on a  chromatogram.  Therefore, the following
         requirements apply to all data presented for single component
         and  multicomponent analytes.

         9.5.10.1   The chromatograms that result from the analyses of
                   the Resolution Check Mixture, the Performance
                   Evaluation Mixture, and Individual Standard Mixtures
                   A and B during the initial calibration sequence must
                   display the single component analytes present in
                   each standard at greater than 10 percent of full
                   scale but less than 100 percent of full scale.

         9.5.10.2   The chromatograms for at least one of the three
                   analyses each of Individual Standard Mixtures A and
                   B from the initial calibration sequence must display
                   the single component analytes at greater than 50
                   percent and less than 100 percent of full scale.
                               PEST D-21                         6/91

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              9.5.10.3   The ehromatograms of the standards for the
                         multieomponent analytes analyzed during the initial
                         calibration sequence must display the peaks chosen
                         for identification of each analyte at greater than
                         25 percent and less than 100 percent of full scale.

              9.5.10.4   For all Resolution Check Mixtures, Performance
                         Evaluation Mixtures, Individual Standard Mixtures,
                         and blanks, the baseline of the chromatogram must
                         return to below 50 percent of full scale before the
                         elution time of alpha-BHC, and return to below 25
                         percent of full scale after the elution time of
                         alpha-BHC and before Che elution time of
                         decachlorobiphenyl.

              9.5.10.5   If a chromatogram is replotted electronically to
                         meet requirements, the scaling factor used must be
                         displayed on the chromatogram.

              9.5.10.6   If the chromatogram of any standard needs to be
                         replotted electronically to meet these requirements,
                         both the initial chromatogram and the replotted
                         chromatogram must be submitted in the data package.

9.6   Corrective Action

      9.6.1   If the technical acceptance criteria for the initial
              calibration are not met, inspect the system for problems.  It
              may be necessary to change the column, bake out the detector,
              clean the injection port, or take other corrective actions to
              achieve the acceptance criteria.

      9.6.2   Contamination should be suspected as a cause if the detector
              cannot achieve acceptable linearity using this method.  In the
              case of low level contamination, baking out the detector at
              elevated temperature  (350*C) should be sufficient to achieve
              acceptable performance.  In the case of heavy contamination,
              passing hydrogen through the detector for 1-2 hours at elevated
              temperature may correct the problem.  In the case of severe
              contamination, the detector may require servicing by the ECO
              manufacturer.  DO NOT OPEN THE DETECTOR.  THE ECD CONTAINS
              RADIOCHEMICAL SOURCES.

      9.6.3   If a laboratory decontaminates a detector using elevated
              temperature, the ECD electronics must be turned off during the
              bake out procedure.

      9.6.4   After bake out or hydrogen reduction, the detector must be
              recalibrated using the initial calibration sequence.
                                     PEST D-22                         6/91

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      9.6.5   Initial calibration technical acceptance criteria MOST be met
              before any samples (including the LCS and PES) or required
              blanks are analyzed.  Any samples (including the LCS and PES)
              or required blanks analyzed after the initial calibration
              criteria have not been met will require reanalysis at no
              additional cost.
10.   CAVpfltftTIOH VERIFICATION

10 . 1  Summary

      Three types of analyses are used to verify the calibration and evaluate
      instrument performance.  The analyses  of instrument blanks,  Performance
      Evaluation Mixtures (PEM) ,  and the mid point concentration of
      Individual Standard Mixtures A and B constitute the continuing
      calibration.  Sample data are not acceptable unless bracketed by
      acceptable analyses of instrument blanks,  PEM, and both Individual
      Standard Mixtures A and B.

10.2  Frequency

      10.2.1  An  instrument blank and the Performance Evaluation Mixture must
              bracket one end  of a 12 -hour period during which sample data
              are collected, and a second instrument blank and the mid point
              concentration  of Individual Standard Mixtures A and B must
              bracket the other end of the 12 -hour period.

      10.2.2  For the 12 -hour  period immediately following the initial
              calibration sequence, the  instrument blank and the PEM that are
              the last  two steps in the  initial calibration sequence bracket
              the front end  of that 12 -hour period.  The injection of the
              instrument blank starts the beginning of that 12 -hour period
              (see Section 13.3).  Samples may be injected for 12 hours from
              the injection  of the instrument blank.  The first three
              injections ^imnad^fltelY after that 12 -hour period must be an
              instrument blank, Individual Standard Mixture A, and Individual
              Standard  Mixture B.  The instrument blank must be analyzed
              first, before  either standard.  The Individual Standard
              Mixtures  may be  analyzed in either order  (A,B or B,A).

      10.2.3  The analyses of  the instrument blank  and Individual Standard
              Mixtures  A and B immediately following one 12 -hour period may
              be  used to begin the subsequent 12 -hour period, provided that
              they meet the  acceptance criteria  in  Section 10.5.  In that
              instance ,  the  subsequent 12 -hour period must be bracketed by
              the acceptable analyses of an instrument blank and a PEM, in
              that order.  Those two analyses may in turn be used to bracket
              the front end  of yet another 12 -hour  period.  This progression
              may continue every 12 hours until  such time as any of  the
              instrument blanks, PEMs, or Individual Standard Mixtures  fails
              to  meet the acceptance criteria in Section 10.5.  The  12 -hour
              time period begins with the injection of  the instrument blank.
              Standards (PEM or  Individual Standard Mixtures) ,  samples  and
                                     PEST D-23                         6/91

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              required blanks may be injected for 12:00 hours from the time
              of injection of the instrument blank.

      10.2.4  If more than 12 hours have elapsed since the injection of the
              instrument blank that bracketed a previous 12-hour period, an
              acceptable instrument blank and PEM must be analyzed in order
              to start a new sequence.  This requirement applies even if no
              analyses were performed since that standard(s) was injected.

      10.2.5  After a break in sample analyses, the laboratory may only
              resume the analysis of samples using the current initial
              calibration for quantitation by analyzing an acceptable
              instrument blank and a PEM.

      10.2.6  If the entire 12-hour period is not required for the analyses
              of all samples to be reported and all data collection is to be
              stopped, the incomplete sequence must be ended with either the
              instrument blank/PEM combination or the instrument
              blank/Individual Standard Mixtures A and B combination,
              whichever was due to be performed at the end of 12-hour period.

10.3  Procedure

      10.3.1  Set up the GC/ECD system as described in Section 8.

      10.3.2  Prepare the PEM standard and the mid point concentration of
              Individual Standard Mixtures A and B as in Section 7, and the
              instrument blank as in Section 20.3.

      10.3.3  The PEM, the Individual Standard Mixtures, and the instrument
              blank must be at ambient temperature at the time of preparation
              and analysis.

      10.3.4  Analyze the PEM, instrument blank, and the mid point
              concentration of Individual Standard Mixtures A and B at the
              required frequencies (Sections 10.2 and 13.3).

10.4  Calculations

      10.4.1  For each analysis of the Performance Evaluation Mixture used to
              demonstrate continuing calibration, calculate the percent
              difference between the amount of each analyte (including the
              surrogates) found in the PEM and the nominal amount, using
              Equations D.26 and D.30.

      10.4.2  For each analysis of the Performance Evaluation Mixture used to
              demonstrate continuing calibration, calculate the percent
              breakdown of Endrin and DDT, and the combined breakdown, using
              Equations D.26, D.27, D.28, and D.29.

      10.4.3  For each analysis of the mid point concentration of  Individual
              Standard Mixtures A and B used to demonstrate continuing
              calibration, calculate the percent difference between  the
              amount of each analyte  (including the surrogates)  found in the

                                     PEST D-24                         6/91

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              standard mixture and the nominal amount, using Equations D.26
              and D.30.  Do not attempt to calculate the breakdown of Endrin
              and DDT in the Individual Standard Mixtures, as these standards
              contain the breakdown products as well as the parent compounds.

10.5  Technical Accepcance Criteria For Calibration Verification

      All calibration verification technical acceptance criteria apply
      independently to both columns.

      10.5.1  The PEMs, Individual Standard Mixtures, and instrument blanks
              must be analyzed at the required frequency (paragraph 10.2),
              using the procedure in paragraph 10.3, on a GC/ECD system that
              has met the initial calibration technical acceptance criteria.

      10.5.2  All single component pesticides and surrogates in the
              Performance Evaluation Mixtures used to demonstrate continuing
              calibration must be 100 percent resolved.  The resolution
              between any two adjacent peaks in the midpoint concentrations
              of Individual Standard Mixtures A and B in the initial
              calibration must be greater than or equal to 90.0 percent.

      10.5.3  The absolute retention time for each of the single component
              pesticides and surrogates in the PEMs and mid point
              concentration of the Individual Standard Mixtures used to
              demonstrate continuing calibration must be within the retention
              time windows determined from the three-point initial
              calibration in paragraph 9.4.2.

      10.5.4  The absolute value of the percent difference of the calculated
              amount and the true amount for each of the single component
              pesticides and surrogates in the PEM and mid point
              concentration of the Individual Standard Mixtures used to
              demonstrate continuing calibration must be less than or equal
              to 25.0 percent, using Equation D.30.

      10.5.5  The percent breakdown of DDT and endrin in the PEM must be less
              than or equal to 20.0 percent each on both columns.  The
              combined breakdown of DDT and endrin must be less than or equal
              to 30.0 percent on both columns.

      10.5.6  All instrument blanks must meet the technical acceptance
              criteria in Paragraph 20.3.4.

      10.5.7  The identification of single component pesticides by gas
              chromatographic methods  is based primarily on retention time
              data.  The retention time of the apex of a peak can only be
              verified from an on-scale chromatogram.  The identification of
              multicomponent analyses by gas chromatographic methods  is based
              primarily on recognition of patterns  of  retention times
              displayed on a chromatogram.  Therefore, the following
              requirements apply to all data presented for single component
              and multicomponent analytes.
                                     PEST D-25                         6/91

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               10.5.7.1   The chromatograas that result from the analyses of
                         the Performance Evaluation Mixture and the
                         Individual Standard Mixtures must display the single
                         component analytes present in each standard at
                         greater than 10 percent of full scale but less than
                         100 percent of full scale.

               10.5.7.2   For any PEM, Individual Standard Mixture, or blank,
                         the baseline of the chrooatogram must return to
                         below 50 percent of full scale before the elution
                         time of alpha-BHC, and return to below 25 percent of
                         full scale after the elution time of alpha-BHC and
                         before the elution time of decachlorobiphenyl.

               10.5.7.3   If a chromatogram is replotted electronically to
                         meet these requirements, the scaling factor used
                         must be displayed on the chromatogram.

               10.5.7.4   If the chromatogram of any standard or blank needs
                         to be replotted electronically to meet these
                         requirements, both the initial chromatogram and the
                         replotted chronatogram(s) must be submitted in the
                         data package.

10.6  Corrective Action.

      10.6.1   If the technical acceptance criteria for the calibration
               verification are not met, inspect the system for problems and
               take corrective action to achieve the acceptance criteria.

      10.6.2   Major corrective actions such as replacing the GC column or
               baking out the detector will require that a new initial
               calibration be performed and meets the technical acceptance
               criteria.

      10.6.3   Minor corrective actions may not require performing a new
               initial calibration, provided that a new analysis of the
               standard  (PEM or Individual Mixtures) that originally failed
               the criteria and an associated instrument blank immediately
               after the corrective action do meet all the acceptance
               criteria.

      10.6.4   If a Performance Evaluation Mixture or Individual Standard
               Mixture does not meet the technical acceptance criteria listed
               above, it must be reinjected immediately.  If the second
               injection of the FEM or Individual Standard Mixture meets the
               criteria, sample analysis may continue.  If the second
               injection does not meet the criteria, all data collection must
               be stopped.  Appropriate corrective action must be  taken, and a
               new initial calibration sequence must be run before more sample
               data are collected.
                                     PEST D-26                         6/91

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10.6.5  If an  instrument blank does not meet the technical acceptance
        criteria  listed in Paragraph 20.3.4, all data collection must
        be stopped.  Appropriate corrective action must be taken to
        clean  out the system, and an acceptable instrument blank must
        be analyzed before more sample data are collected.

10.6.6  Analysts  are cautioned that running an instrument blank and a
        Performance Evaluation Mixture or Individual Standard Mixtures
        once every 12 hours are the minimum contract requirements.
        Late eluting peaks may carry over from one injection to the
        next if highly complex samples are analyzed or if the GC
        conditions are unstable.  Such carryover is unacceptable.
        Therefore, it may be necessary to run instrument blanks and
        standards more often to avoid discarding data.

10.6.7  If a successful instrument blank and FEM cannot be run after an
        interruption in analysis (Paragraph 10.2.5), an acceptable
        initial calibration must be run before sample data may be
        collected.  All acceptable sample analyses must be preceded and
        followed  by acceptable standards and instrument blanks, as
        described in Section 10.2.

10.6.8  Calibration verification technical acceptance criteria must be
        met before any samples (including LCS, PES) and required blanks
        are reported.  Any samples, including LCS and PES required with
        a calibration verification which did not meet the technical
        acceptance criteria will require reanalysis at no additional
        cost.
                               PEST D-27                         6/91

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                SECTION IV
SAMPLE FHEPABATION, EXTRACTION,  AHD CLEAHDF
                    PEST D-28                         6/91

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11.   SUMMARY

11.1  This method is designed for analysis of samples that contain low
      concentrations of the pesticides and Aroclors listed in Exhibit C.  The
      majority of the samples are expected to come from drinking water
      sources and well/ground water around Superfund sites.  If, upon
      inspection of a sample, the Contractor suspects that the sample is not
      amenable to this method, contact SMO for instructions.

12.   PROCEDURE

12.1  Extraction

      Continuous Liquid-Liquid Extraction is required for the extraction of
      the samples.

      12.1.1  Add methylene  chloride  (100 to 250 mL) to  the bottom of  the
              extractor and  fill  it to a depth of at least one  inch  above  the
              bottom sidearm.

      12.1.2  Measure out each 1.0 liter sample aliquot  in a separate  1 liter
              graduated cylinder.  Measure and record the  pH of the  sample
              with wide range pH  paper and adjust the pH to between  5  and  9
              with 10 N sodium hydroxide or concentrated sulfuric acid,  if
              required.  Samples  requiring pH adjustment must be noted in  the
              SDG Narrative.  Transfer the sample aliquot  into  the continuous
              extractor.

      12.1.3  Using-a micropipet  with disposable tip, add  200 uL of  the
              surrogate solution  to all samples and method blanks.

      12.1.4  Adjust the level of methylene chloride in  the extractor  so that
              the bottom sidearm  is half filled with solvent.

      12.1.5  If  the sample  was received in a 1 liter container, rinse the
              empty container with 60 mL of methylene chloride  after taking
              the sample aliquot.  Add the rinsate to the  continuous
              extractor.

      12.1.6  Add sufficient methylene chloride to the distilling flask to
              ensure proper  solvent cycling during operation.   Extract the
              solution for 18 hours.  Allow to cool, then  detach the
              distillation flask  and  label.

12.2  Extract Drying and Concentration

      12.2.1  Assemble a Kuderna-Danish (K-D) concentrator by attaching a  10
              mL  concentrator tube to a 500 mL evaporative flask.  Other
              concentration  devices or techniques may be used in place of  the
              K-D, if equivalency is  demonstrated for all  the target
              pesticides and Aroclors listed in Exhibit  C.
                                     PEST D-29                         6/91

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      12.2.2   Pour the  extract  through a drying column containing about 10 cm
               of anhydrous  granular sodium sulfate and collect the extract in
               the K-D concentrator.  Rinse the Erlenneyer flask and the
               sodium sulfate with at least two additional 20 to 30 mL
               portions  of methylene chloride to complete the quantitative
               transfer.

      12.2.3   Add one or two clean boiling chips to the evaporative flask and
               attach a  three-ball Snyder column. Pre-wet the Snyder column by
               adding about  1 mL of methylene chloride to the top of the
               column.   Place the K-D apparatus on a hot water bath (60-80*0)
               so that the concentrator tube is partially immersed in the hot
               water and the entire lower rounded surface of the flask  is
               bathed with hot vapor.  Adjust the vertical position of  the
               apparatus and the water temperature as required to complete the
               concentration in  15 to 30 minutes.  At the proper rate of
               distillation, the balls of the column will actively chatter,
               but the chambers  will not flood with condensed solvent.  When
               the apparent  volume of liquid reaches 3 to 5 mL, remove  the K-D
               apparatus.  Allow it to drain and cool for at least 10 minutes.
               DO NOT ALLOW  THE  EVAPORATOR TO GO DRY.

      12.2.4   Proceed with  the  solvent exchange to hexane.

12.3  Solvent Exchange To Hexane

      12.3.1   Momentarily remove the three-ball Snyder column, add 50  mL of
               hexane and a  new  boiling chip, and reattach the Snyder column.
               Pre-wet the column by adding about 1 mL of hexane to the top.
               Concentrate the solvent extract as before.  When the apparent
               volume of liquid  reaches 1 mL, remove the K-D apparatus  and
               allow it  to drain and cool for at least 10 minutes.  DO  NOT
               ALLOW THE EVAPORATOR TO GO DRY.

      12.3.2   Remove the Snyder column; using 1 to 2 mL of hexane, rinse the
               flask and its lower joint into the concentrator tube.

      12.3.3   Use the micro Snyder column or the nitrogen blowdown technique
               (Section  12.5) to concentrate the hexane extract to 1.0  mL.

12.4  Extract Cleanup

      12.4.1   The two cleanup procedures specified in this method are
               Florisil  cartridge and sulfur cleanup.   Florisil cartridge
               cleanup is required for all extracts.  Sulfur cleanup must be
               performed on  all  extracts containing sulfur at levels that
               interfere with GC/ECD analysis.  Sulfur contamination in a
               sample analysis is unacceptable.  Method blanks must be
               subjected to  the  same cleanup procedures as the samples.
                                     PEST D-30                         6/91

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12.4.2  Florisil Cartridge Procedure

        Florisil cartridge cleanup significantly reduces matrix
        interferences caused by polar compounds and is required for all
        extracts.

        12.4.2.1   Cartridge Performance Check.   Every lot number of
                   Florisil cartridges must be tested by the following
                   procedure before they are used for sample cleanup.
                   Add 0.50 mL of 2,4,5•triehlorophenol solution (0.1
                   ug/mL in acetone)  and 0.50 mL of Standard Mixture A,
                   midpoint concentration (Section 7.3.4) to 4 mL of
                   hexane.   Reduce the final volume to 1.0 mL using the
                   extract concentration techniques in paragraph 12.5.
                   Place the mixture onto the top of a washed Florisil
                   cartridge, and elute it with 9 mL of hexane/acetone
                   [(90:10)(V/V)].  Use two additional 1 mL hexane
                   rinses to ensure quantitative transfer of standard
                   from the cartridge.  Reduce the final volume to 1.0
                   mL using micro Snyder column or nitrogen evaporation
                   techniques (Section 12.5).  Analyze the solution by
                   GC/ECD.   This solution must be analyzed on a GC/ECD
                   meeting the initial and calibration verification
                   technical acceptance criteria.  The recovery of each
                   analyte must be determined for evaluation and
                   reporting purposes.  The lot of Florisil cartridges
                   is acceptable if all pesticides and surrogates are
                   recovered at 80 to 120 percent, if the recovery of
                   triehlorophenol is less than 5%, and no peaks
                   interfering with the target analytes are detected.

        12.4.2.2   Florisil cartridge cleanup procedure

                   12.4.2.2.1   Attach the vacuum manifold to a water
                                aspirator or to  a vacuum pump with a
                                trap  installed between the manifold and
                                the vacuum source.   Adjust the vacuum
                                pressure in the  manifold to between 5
                                and 10 pounds of vacuum.

                   12.4.2.2.2   Place a 1 g Florisil cartridge into the
                                vacuum manifold  for each sample
                                extract.

                   12.4.2.2.3   Prior to cleanup of samples, the
                                cartridges must  be washed with
                                hexane/acetone (90:10).   This is
                                accomplished by  placing the cartridge
                                in the vacuum manifold,  by pulling a
                                vacuum,  and by passing at least 5 mL of
                                the hexane/acetone solution through the
                                cartridge.   While the cartridges are
                                being washed,  adjust the vacuum applied
                                to each cartridge so that the flow rate

                              PEST D-31                          6/91

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             through each cartridge is approximately
             equal.  DO NOT ALLOW THE CARTRIDGES TO
             GO DRY AFTER THEY HAVE BEEN WASHED.

12.4.2.2.4   After the cartridges in the manifold
             are washed, the vacuum is released, and
             a rack containing labeled 10 mL
             volumetric flasks is placed inside the
             manifold.  Care must be taken to ensure
             that the solvent line from each
             cartridge is placed inside of the
             appropriate volumetric flask as the
             manifold top is replaced.

12.4.2.2.5   Transfer the 1 mL extract to the top
             frit of the appropriate Florisil
             cartridge.  Rinse the concentrator tube
             twice with 0.5 mL of hexane/acetone
             (90:10) and transfer each rinse to the
             top frit of the cartridge.

12.4.2.2.6   The pescieides/Aroclors in the extract
             concentrates are then eluted through
             the column with 8.0 mL of
             hexane/acetone (90:10) and are
             collected into die 10 mL volumetric
             flasks held in the rack inside the
             vacuum manifold.

12.4.2.2.7   Transfer the eluate in each volumetric
             flask to a clean centrifuge tube or 10
             mL vial.  Use two additional 1 mL
             hexane rinses to ensure quantitative
             transfer of the cartridge eluate.

12.4.2.2.8   Concentrate the extract to 2.0 mL using
             either a micro Snyder column or
             nitrogen evaporation (Section 12.5).
             Measure the final volume with a syringe
             or by transferring the extract to a
             volumetric flask.

12.4.2.2.9   If crystals of sulfur are evident or if
             the presence of sulfur is suspected,
             proceed to Section 12.4.3.  Sample
             analyses with interference caused by
             sulfur are not acceptable and the
             extracts must be cleaned up and
             reanalyzed.

12.4.2.2.10  If the extract is not contaminated with
             sulfur, transfer the sample to a. GC
             vial and label the vial.  The extract
             is ready for GC/ECD analysis.  Proceed

            PEST D-32                         6/91

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                                to Section 13.   Store the extracts at
                                4*C in the dark until analyses are
                                completed.
12.4.3  Sulfur Removal
        Sulfur can be removed by one of two methods, according to
        laboratory preference.  Interference which is due to sulfur is
        not acceptable.  If the sulfur concentration ia such that
        crystallization occurs in the concentrated extract, centrifuge
        the extract to settle the crystals, and remove the sample
        extract with a disposable pipette, leaving the excess sulfur in
        the centrifuge tube.  Transfer the extract to a clean
        centrifuge tube or clean concentrator tube before proceeding
        with further sulfur cleanup.

        12.4.3.1   If only part of a set of samples requires sulfur
                   cleanup, then two blanks are required for that set:
                   one that is shaken with mercury or copper, and one
                   that is not.   If only part of a set of samples
                   requires sulfur cleanup, do not subject the
                   associated method blank to sulfur cleanup, but
                   prepare a separate sulfur cleanup blank as described
                   below.   If all the samples are subjected to sulfur
                   cleanup, process the method blank along with the
                   samples.  In this ease, no additional sulfur cleanup
                   blank is required.

                   Sulfur cleanup blank.   Add 200 uL of surrogate to 10
                   mL of hexane in a clean centrifuge tube or 10 mL
                   vial.   Concentrate the solution to 2.0 mL by using
                   either nitrogen blowdown or a micro Snyder column.
                   The concentrated volume of the blank must be the
                   same as the final volume of the samples associated
                   with the blank.  Measure the volume with a syringe
                   or by transferring the solution to a volumetric
                   flask.   Proceed with the sulfur removal using the
                   same technique (mercury or copper) as the samples
                   associated with the blank.

        12.4.3.2   Mercury technique

                   Add one to three drops of mercury to each hexane
                   extract in a clean vial.  Tighten the top on the
                   vial and agitate the sample for 30 seconds.  Filter
                   or centrifuge the extract.  Fipet the extract to
                   another vial and leave all solid precipitate and
                   liquid mercury.  If the mercury appears shiny,
                   proceed to Section 13  and analyze the extract.  If
                   the mercury turns black, repeat sulfur removal as
                   necessary.   CAUTION:   Waste containing mercury
                   should be segregated and disposed of properly.
                               PEST D-33
6/91

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                         NOTE:  Mercury is a highly toxic metal and
                         therefore, mist be used with great care.  Prior to
                         using mercury, it is recommended that the analyst
                         become acquainted with proper hand!ing and cleanup
                         techniques associated with this metal.
               12.4.3.3   Copper technique

                         Add approximately 2 g of cleaned copper powder to
                         the extract in the centrifuge or concentrator tube.
                         (2 g will fill the tube to about the 0.5 mL mark).
                         Mix the copper and extract for at least 1 minute on
                         a mechanical shaker.  Separate the extract from the
                         copper powder by drawing off the extract with a
                         disposable pipet, and transfer the extract to a
                         clean vial.  The extract transferred to the vial
                         still represents the 2.0 mL final volume.  The
                         separation of the extract from the copper powder is
                         necessary to prevent degradation of the pesticides.
                         If the copper appears bright, proceed to Section 13
                         and analyze the extract.  If the copper changes
                         color, repeat the sulfur removal procedure as
                         necessary.

12.5. Extract Concentration

      Two different techniques are permitted to concentrate the extract to
      1.0 nL (volume before Florisil cleanup) or 2.0 mL (extract volume
      before instrumental analysis).  They are the micro Snyder column and
      nitrogen evaporation techniques.

      12.5.1   Micro Snyder Column Technique

               Add another one or two clean boiling chips to the concentrator
               tube and attach a two-ball micro Snyder column. Pre-wet the
               Snyder column by adding about 0.5 mL of hexane to the top of
               the column.  Place the K-D apparatus in a hot water bath  (60*C
               to 65 *C) so that the concentrator tube is partially immersed  in
               the hot water.  Adjust the vertical position of the apparatus
               and the water temperature as required to complete the
               concentration in 5 to 10 minutes.  At the proper rate of
               distillation the balls of the column will actively chatter but
               the chambers will not flood with condensed solvent. When the
               apparent volume of liquid reaches about 0.5 mL, remove the K-D
               apparatus from the water bath and allow it to drain for at
               least 10 minutes while cooling.  Remove the Snyder column and
               rinse its flask and lower joint into the concentrator tube with
               0.2 mL of hexane.  Adjust the final volume with hexane to 1.0
               mL (Florisil) or 2.0 mL (analysis).
                                     PEST D-34                         6/91

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12.5.2   Nitrogen Evaporation Technique  (taken from ASTM Method  D  3086).

         12.5.2.1  Place the concentrator tube with an open micro
                   Snyder column attached in a warm water bath  (30*C to
                   35*C) and evaporate the solvent volume to Just below
                   1 or 2 mL by blowing a gentle stream of clean, dry
                   nitrogen filtered through a column of activated
                   carbon above the solvent.  Adjust the final volume
                   with hexane to 1.0 mL (Florisil) or 2.0 mL
                   (analysis).

         12.5.2.2  CAUTION:  Gas lines from the gas source to the
                   evaporation apparatus must be stainless steel,
                   copper, or Teflon tubing.  The internal wall of new
                   tubing must be rinsed several times with hexane and
                   then dried prior to use.  During evaporation, the
                   tube solvent level must be kept below the water
                   level of the bath.  DO NOT ALLOW THE EXTRACT TO GO
                   TO DRYNESS.

12.5.3   If the extract has not been put through Florisil yet, proceed
         to Section 12.4 for extract cleanup.  Otherwise, transfer the
         extract  to a Teflon-lined screw-cap bottle and label the
         bottle.   Store at 4*C (±2»C).
                               PEST D-35                          6/91

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                         SECTIOH V






SAMPLE AHALYSIS AHD COMPOUND IDENTIFICATION AND QUANTITAXION
                             PEST D-36                        6/91

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13.   INSTRUMENTAL ANALYSIS

      Before samples or required blanks can be analyzed, the instrument must
      meet the initial calibration and calibration verification technical
      acceptance criteria.  All sample extracts, including LCS and FES,
      required blanks, and calibration standards must be analyzed under the
      same instrumental conditions.  All samples (Including the LCS and FES),
      required blanks, extracts, and standard/spiking solutions must be
      allowed to warm to ambient temperature (approximately 1 hour) before
      preparation/analysis.

13.1  Set up the GC/ECD system per the requirements in Section III.  Unless
      ambient temperature on-column injection is used (see Section 8), the
      injector must be heated to at least 200*C.  The optimized gas
      chromatographic conditions from Section 8 must be used.

13.2  The injection must be made on-column by using either automatic or
      manual injection.  If autoinjectors are used, 1.0 uL injection volumes
      may be used.  Mnmial injections must use at least 2.0 uL injection
      volumes.  The same injection volume must be used for all standards,
      samples, and blanks associated with the same initial calibration.  If a
      single injection is used for two GO columns attached to a single
      injection port, it may be necessary to use an injection volume greater
      than 2 uL.   However, the same injection volume must be used for all
      analyses.
                                     PEST D-37                          6/91

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13.3
      All acceptable samples must be analyzed within a valid analysis
      sequence as given below.
Tii
      0 hr.
      12 hr.
Another 12 hr.
Another 12 hr.
                 Infection #
                 1 -  15

                 16

                 17

                 18
                 o
                 o
                 o
                 o
                 1st  injection
                   past 12:00 hr.
                 2nd  and 3rd
                   injections
                   past 12:00 hr.
                 o
                 o
                 o
                 o
                 o
                 o
                 1st  injection
                   past 12:00 hr.
                 2nd  injection
                 o
                 o
                 o
                 o
                 o
                 o
                 1st  injection
                   past 12:00 hr.
                 2nd  and 3rd
                   inj actions
                   past 12 hr.
                 o
                 o
                 o
                 o
                 o
                 etc.
                                       Material Iniected
                                 First 15 steps of the
                                   Initial Calibration
                                 Instrument Blank at end of
                                 PEM at end of
                                   Initial Calibration
                                 First Sample

                                 Subsequent Samples

                                 Last sample
                                 Instrument Blank

                                 Individual Standard Mixtures A and B
                                        Sample

                                        Subsequent Samples
                                 Last Sample
                                 Instrument Blank

                                 Performance Evaluation Mixture
                                 Sample

                                 Subsequent Samples
                                 Last Sample
                                 Instrument Blank

                                 Individual Standard Mixtures A and B
                                        Sample

                                        Subsequent Samples
      NOTE:  The first 12 hours are counted from the injection #16 (the
      Instrument Blank at the end of the initial calibration sequence),  not
      from injection #1.  Samples may be injected until 12:00 hours have
      elapsed.  All subsequent 12-hour periods are timed from the injection
      of the instrument blank that brackets the front end of the samples.
      Because the 12-hour time period is timed from injection of the
                                     PEST D-38
                                                                      6/91

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       instrument blank until the in1action of the last sample, each 12-hour
       period nay be separated by the length of one chronatographic run, that
       of  the analysis of the last sample.  While the 12-hour period may not
       be  exceeded, the laboratory may run instrument blanks and standards
       more frequently, for instance, to accomodate staff working on 8-hour
       shifts.

13.4   Included with the subsequent samples in the analysis sequence are all
       of  the required method blanks and sulfur cleanup blanks.  The
       Contractor may decide at what point in the sequence the method blanks
       and sulfur cleanup blanks are to be analyzed.

13.5   Termination of Data Acquisition

       After decachlorooiphenyl has eluted from the GO column, the data
       acquisition may be terminated for that analysis.

14.    DILUTIONS

14.1   The sample or blank must first be analyzed at the most concentrated
       level (injection taken from the 2.0 mL final extract after the clean-up
       steps).

       14.1.1   If the response  of any single component pesticide  is  greater
               than the response  of  that analyte  in the  initial calibration
               high point standard,  then the extract must be  diluted to have
               the  response of  that  analyte between the  initial calibration
               low  point and high point standard.

       14.1.2   If the response  of the largest peak in a  multicomponent analyte
               is greater than  the most intense single component  analyte
               response in the  initial calibration high  point standard, then
               the  response of  the largest peak in a multicomponent  analyte
              must be diluted  to have its response between the responses  of
               the  initial calibration midpoint and high point standard of
               that single component pesticide.

       14.1.3   If a greater than  10  times dilution is needed  (for example, 50
               to 1 dilution),  then  a 10 times more concentrated  dilution  (5
               to 1 dilution) also must be analyzed.

14.2  When diluted, the chromatographic data for the single component
      pesticide must be able to be reported at greater than 10 percent of
      full scale but less than 100 percent of full scale.

14.3  When diluted, multicomponent analytes must be able to be reported at
      greater than 25 percent of full scale but less than 100 percent of full
      scale.

14.4  If a chromatogram is  replotted electronically to meet these
      requirements, the scaling factor used must be displayed on the
      chromatogram.  If the chromatogram of any sample needs to be replotted
      electronically to meet these requirements,  both the initial
                                     PEST D-39                         6/91

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      chromatogram and the replotted cfarooatogram(s) must be submitted in the
      data package.

14.5  Dilute the sample using the following procedure:

      14.5.1   Calculate  the extract dilution in order for the single
               component  pesticides to meet the requirement listed in
               paragraph  14.2.

      14.5.2   Calculate  the extract dilution in order for the multicomponent
               analytes to meet  the requirement listed in 14.3.

      14.5.3   Dilute  the sample extract with hexane in a volumetric flask.

15.   IDENTIFICATION OF TARGET AHALTTSS

15.1  The laboratory will identify single component analyte peaks based on
      the retention time windows established during the initial calibration
      sequence.  Single component analytes are identified when peaks are
      observed in the RT window for the analyte on both GC columns.

15.2  A set of three to five major peaks is selected for each multicomponent
      analyte.  Retention time windows for each peak are determined from the
      initial calibration analysis.   Identification of a multicomponent
      analyte in the sample is based on pattern recognition in conjunction
      with the elution of three to five sample peaks within the retention
      time window of the corresponding peaks of the standard on both GC
      columns.  The number of potential quantitation peaks is listed in Table
      D.14.

                                  TABLE D-14

      MulticonrDonenC Analvte        No  of Potential Ouantitatiem Peaks
      Aroclor 1016/1260                       5/5
      Aroclor 1221                            3
      Aroclor 1232                            4
      Aroclor 1242                            5
      Aroclor 1243                            5
      Aroclor 1254                            5
      Toxaphene                               4

15.3  A standard of any identified multicomponent analyte must be run within
      72 hours of its detection in a sample chromatogram within a valid 12
      hour sequence.

15.4  The choice of the peaks used for multicomponent analyte identification
      and the recognition of those peaks may be complicated by the
      environmental alteration of the Toxaphene or Aroclors, and by the
      presence of coeluting analytes, or matrix interferences, or both.
      Because of the alteration of these materials in the environment,
      multicomponent analytes in samples may give patterns similar to, but
      not identical with, those of the standards.

                                     PEST D-40                         6/91

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15.5  Toxaphene and Aroclors require only a single-point calibration.
      Identification requires visual inspection of an on-scale pattern.

16.   OTJAMTITATION OF AHALYTES

16.1  Quantitation for all analytes and surrogates oust be performed and
      reported on both columns.

16.2  Manual integration of peaks (e.g., measuring peak height with a ruler)
      is only permitted when accurate electronic integration of peaks cannot
      be done.  If manual integration of peaks is required, it must be
      documented in the SDG Narrative.

16.3  The Contractor must quantitate each single component analyte and
      surrogate based on the calibration factor from the most recent initial
      calibration midpoint standard mixture analyses.  Do not use the
      analyses of the Individual Standard Mixtures used to demonstrate
      continuing calibration for quantitation of samples.

16.4  The Contractor must quantitate each multicomponent analyte based on the
      calibration factor from the most recent initial calibration standard.

16.5  If more than one multicomponent analyte Is present, the Contractor must
      choose separate peaks to quantitate the different multicomponent
      analytes.  A peak common to both analytes present in the sample must
      not be used to quantitate either analyte.

16.6  Before reporting data, it is required that the Contractor check for
      flags generated by the data system that indicate improper quantitation
      of analytes.

16.7  The chromatograms of all samples, standards, and blanks must be
      reviewed by a qualified pesticide analyst before they are reported.

16.8  Calculations.

      16.8.1  Calculate the concentration of the  single  component pesticides
              and surrogates by using  the following  equation:

              EQ  D 32  Concentration  ug/L -   (^  
                                               (CF) (Vj.) (Vx)

         Where:


         AX - Response (peak area or height).

         CF - Calibration factor for the external standard (Paragraph 9.4.3)
              (per ng).

         Vt - Volume of total extract (uL).   (This volume is 2000 uL.)
                                     PEST D-41                         6/91

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   V^ - Volume of extract injected (uL) .   (If a single injection is
        made onto two columns, use one -half the volume of the syringe
        as the volume injected onto each column.)

   Vx - Volume of water extracted (mL) .  (NOTE:  for instrument blanks
        and sulfur cleanup blanks, assume a 1,000 mL volume).

   Df - Dilution factor.  The dilution factor for analysis of water
        samples by this method is defined as follows:

"L Tost cone, extract "ged to make dilution + **i- clean solvent
         uL most cone, extract used to make dilution

If no dilution is performed, Of - 1.0.

        The  calibration factors used  in Equation D.32 are those from
        the  most recent Initial calibration.   If the calibration
        factors used to determine the linearity  of  the initial
        calibration  were based on peak area,  then the response  of the
        analyte in the  sample must be based on peak area.   Similarly,
        if peak height  was  used to determine  linearity, use peak height
        to determine the concentration in the sample.

16.8.2  During initial  calibration, a set of  three  to five  quantitation
        peaks was chosen for each multicomponent analyte.   Calculate
        the  concentration of each of  the selected Aroclor or Toxaphene
        peaks individually  using Equation D.32.  Determine  the  mean
        concentration for all of the  selected peaks.  The mean  value is
        reported on  Form X  (Exhibit B) for  both  GC  columns.

16.8.3  For  the single  component pesticides,  report the lover of the
        two  values quantitated from the two columns of Form I.   For the
        multicomponent  analytes, report the lower of the  two mean
        values from  the two columns on Form I.

16.8.4  The  recoveries  of the surrogates are  calculated according to
        Equation D.33.

      EQ.  D.33                                qd
                Surrogate Percent Recovery -  jr—  x  100


      Where:

      Qd - Quantity determined by analysis.

      Qa - Quantity added to sample/blank.

16.8.5  The  percent  difference is calculated  according to Equation
        D.34.

       EQ. D.34                Concfl  - Conc^
                        %D -                  x  100
                               PEST D-42                         6/91

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            Where,

            Concg - The higher  of  the  two concentrations  for  the target
                    compound  in question.

            ConcL - The lower of the two concentrations for the target
                    compound  in question.

               Note that using this equation will result in percent difference
               values  that are always positive.   The value will also be
               greater than a value calculated using the higher concentration
               in the  denominator,  however,  given the likelihood of a positive
               interference raising the concentration determined on one GC
               column, this is a conservative approach to comparing the two
               concentrations.

17.   TECHNICAL ACCEPTANCE CRITERIA FOR SA*?TtB ANALYSIS

      All requirements listed below apply independently to both GC  columns
      and to all instruments  used  for  these analyses.

17.1  Samples must be analyzed under the GC/ECD operating conditions  in
      Section 8.  The instrument must  have met all initial calibration and
      calibration verification technical acceptance criteria.  Sample data
      must be bracketed at 12-hour intervals (or less) by acceptable  analyses
      of instrument blanks, Performance Evaluation Mixtures,  and Individual
      Standard Mixtures A and B, as described in Section  10.2.

17.2  The sample must be extracted and analyzed within the contract holding
      times.

17.3  The LCS associated with the samples must meet the LCS technical
      acceptance criteria.  The FES associated with the samples must  meet the
      FES technical acceptance criteria.  The method blank extracted  with the
      samples must meet the method blank technical acceptance criteria.  If a
      sulfur cleanup blank is associated with the samples, that blank must
      meet the sulfur cleanup blank technical acceptance  criteria.

17.4  The retention time for each of the surrogates must  be within  the
      retention time window as calculated in Section 9.

17.5  The percent recovery for the surrogates must be between 60.0  and 150
      percent, inclusive.

17.6  No target analyte concentrations may exceed the upper limit of  the
      initial calibration (See paragraph 14.1.1 and 14.1.2) or else extracts
      must be diluted and reanalyzed.

17.7  A standard for any identified multicomponent analyte must be  analyzed
      on the same instrument within 72 hours of its detection in a  sample
      within a valid 12 hour sequence.
                                     PEST D-43                         6/91

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17.8  The identification of single component pesticides by gas
      chronatographic methods is based primarily on retention time data.  The
      retention time of the apex of a peak can only be verified from an on-
      scale chromatogram.  The identification of multicomponant analytes by
      gas chromatographic methods is based primarily on recognition of
      patterns of retention times displayed on a chromatogram.  Therefore,
      the following requirements apply to all data presented for single
      component and multicomponent analytes.

      17.8.1  When no analytes are identified in a sample, the chromatograms
              from the analyses of the sample extract must use the same
              scaling factor as was used for the low point standard of the
              initial calibration associated with those analyses.

      17.8.2  Chromatograms must display single component pesticides detected
              in the sample at less than full scale.

      17.8.3  Chromatograms must display the largest peak of  any
              multicomponent analyte detected in the sample at less than full
              scale.

      17.8.4  If an extract must be diluted, chromatograms must display
              single component pesticides between 10 and 100  percent of  full
              scale.

      17.8.5  If an extract must be diluted, ehromatograms must display
              multicomponent analytes between 25 and 100 percent  of full
              scale.

      17.8.6  For any sample or blank, the baseline of the chromatogram  must
              return to below 50 percent of full scale before the elution
              time of alpha-BHC, and return to below 25 percent of full  scale
              after the elution time of  alpha-BHC and before  the  elution time
              of decachlorobiphenyl.

      17.8.7  If a chromatogram is replotted electronically to meet these
              requirements, the scaling  factor used must be displayed on the
              chromatogram.

      17.8.8  If the chromatogram of any sample needs to be replotted
              electronically to meet these requirements, both the initial
              chromatogram and the replotted chromatogram(s)  must be
              submitted in the data package.

18.   COPBgCTIVg ACTION

18.1  If the sample technical acceptance criteria are not met, check
      calculations,  surrogate solutions,  and instrument performance.  It may
      be necessary to recalibrate the instrument or take other corrective
      action procedures to meet the technical acceptance criteria, in which
      case,  the  affected samples must be reanalyzed at no additional cost
      after the  corrective action.
                                     PEST D-44                         6/91

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18.2  If the Contractor needs to analyze more than the most concentrated
      extract and two (2) sample dilutions to have all the pesticide/Aroclor
      compounds within the calibration range of the instrument, contact SMO.
      SMO will contact the Region for instructions.

18.3  Sample analysis technical acceptance criteria MUST be met before data
      are reported.  Samples contaminated from laboratory sources or
      associated with a contaminated method blank or sulfur cleanup blank
      will require reextraction and reanalysis at no additional cost.  Any
      samples analyzed that do not meet the technical acceptance criteria
      will require reextraction and\or reanalysis at no additional cost.

18.4  Sample reextraction/reanalyses performed as a result of suspected
      matrix interferences beyond the scope of the method will be reviewed on
      a case-by-case basis for payment purposes by SMO.
                                     PEST D-45                         6/91

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                    SECTIOH 71






SAMPLE QUALITY CONTROL PROCEDURES AND REQUIREMENTS
                       PEST D-46                         6/91

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20.

      Summary

      There are two types of blanks required by this  method:  the method blank
      and the Instrument blank.  A separate sulfur cleanup blank may also be
      required If some, but not all of the samples are subjected to sulfur
      cleanup.  Samples that are associated with a sulfur cleanup blank are
      also associated with the method blank with which they were extracted.
      Both the method and sulfur cleanup blanks must  meet the respective
      technical acceptance criteria for the sample analysis technical
      acceptance criteria to be met.

20.1  Method Blanks

      20.1.1  Summary

              A method blank is 1.0 liter of reagent water carried through
              the entire analytical scheme.

      20.1.2  Frequency

              A method blank must be extracted and analyzed:

                     o   once every 20 samples, AND

                     o   every time samples are extracted.
      20.1.3  Procedure

              20.1.3.1   Measure 1.0 liter of reagent water for each method
                         blank aliquot.  Add 200 uL of the surrogate
                         solution.  Extract and concentrate the method blank
                         according to Section 12.

              20.1.3.2   Analyze the method blank according to Section 13.
                         Calculate the results according to Section 16.

      20.1.4  Technical Acceptance Criteria for Method Blanks

              20.1.4.1   All method blanks must be prepared and analyzed at
                         the frequency described in Paragraph 20.1.2 using
                         the procedure in Paragraph 20.1.3 on a GC/ECD system
                         meeting the initial calibration and  calibration
                         verification technical acceptance criteria.

              20.1.4.2   The concentration in the method blank of the target
                         compounds in Exhibit C must  be less  than or equal to
                         the CRQL for each target compound.

              20.1.4.3   The method blank must meet all sample technical
                         acceptance criteria in Section 17.
                                     PEST  D-47                         6/91

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      20.1.5   Corrective Action

               20.1.5.1   If a method blank does not meet the technical
                         acceptance criteria, the Contractor must consider
                         the analytical system to be out of control.  It is
                         the Contractor's responsibility to ensure that
                         method interferences caused by contaminants in
                         solvents, reagents, glassware, and sample storage
                         and processing hardware that lead to discrete
                         artifacts and/or elevated baselines in gas
                         chromatograms be eliminated.  If contamination is a
                         problem, the source of the contamination must be
                         investigated and appropriate corrective measures
                         MUST be taken and documented before further sample
                         analysis proceeds.

               20.1.5.2   Any method blank that fails to meet the technical
                         acceptance criteria must be reextraeted and
                         reanalyzed at no additional cost.  Further, all
                         samples (including LCS and PES) processed with a
                         method blank that does not meet the blank technical
                         acceptance criteria (i.e., contaminated) will
                         require reextraetion and reanalysis at no additional
                         cost.

20.2  Sulfur Cleanup Blank

      20.2.1   Summary

               The sulfur cleanup blank is a modified form of the method
               blank.  The sulfur cleanup blank is hexane spiked with the
               surrogates and passed through the sulfur cleanup procedure
               (Section 12.4.3).

      20.2.2   Frequency

               The sulfur cleanup blank is prepared when only part of a set of
               samples extracted together requires sulfur removal.  A method
               blank is associated with the entire set of samples.  The sulfur
               cleanup blank is associated with the part of the set which
               required sulfur cleanup.  If all the samples associated with a
               given method blank are subjected to sulfur cleanup, then no
               separate sulfur cleanup blank is required.

      20.2.3   Procedure

               20.2.3.1   Prepare the sulfur cleanup blank per Paragraph
                         12.4.3.1 at the frequency listed in Paragraph
                         20.2.2.

               20.2.3.2   Analyze the sulfur cleanup blank according to
                         Section 13.  Calculate the results according to
                         Section 16.
                                     PEST D-48                         6/91

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      20.2.4   Technical Acceptance Criteria for Sulfur  Cleanup  Blanks

               20.2.4.1  All  sulfur cleanup blanks must be prepared and
                         analyzed  at  the frequency described in Paragraph
                         20.2.2 using the procedure in Paragraph 20.2.3 on a
                         GC/ECD system meeting  the initial calibration and
                         calibration  verification technical acceptance
                         criteria.

               20.2.4.2  The  concentration  in the sulfur cleanup blank of the
                         target compounds in Exhibit C must be  less than or
                         equal to  the CBQL  for  each target compound.

               20.2.4.3  The  sulfur cleanup blank must meet all sample
                         technical  acceptance criteria in Section 17.

      20.2.5   Corrective Action

               20.2.5.1  If a sulfur  blank does not meet the technical
                         acceptance criteria, the Contractor must consider
                         the  analytical system  to be out of control.  It is
                         the  Contractor's responsibility to ensure that
                         interferences caused by contaminants in solvents,
                         reagents,  glassware, and sample storage and
                         processing hardware that lead to discrete artifacts
                         and/or elevated baselines in gas chromatograms be
                         eliminated.  If contamination is a problem, the
                         source of  the contamination must be investigated and
                         appropriate  corrective measures MUST be taken and
                         documented before further sample analysis proceeds.

               20.2.5.2   Any  sulfur blank that fails to meet the technical
                         acceptance criteria must be reextracted and
                         reanalyzed at no additional cost.  Further, all
                         samples (including LCS and PES) processed with a
                         sulfur blank that does not meet the blank technical
                         acceptance criteria (i.e., contaminated) will
                         require reextraction and reanalysis at no additional
                         cost.

20.3  Instrument Blanks

      20.3.1   Summary

              An instrument blank is  a volume of clean solvent  containing the
               surrogates that is analyzed to determine the extent of
              contamination in the  GC/ECD system.

      20.3.2  Frequency

              The first analysis after a 12-hour analysis sequence (see
              Section 10.2) must be an instrument blank..  All groups of
              acceptable sample analyses are to be preceded and followed by
              acceptable instrument blanks.   If more than 12 hours have

                                    PEST D-49                         6/91

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         elapsed  since the injection of the instrument blank  that
         bracketed a previous 12-hour period, an instrument blank must
         be  analyzed to initiate a new 12-hour sequence (see Section
         10.2).

20.3.3   Procedure

         20.3.3.1  Prepare the instrument blank by spiking the
                   surrogates into hexane or iso-octane for a
                   concentration of 20.0 ng/mL of Tetrachloro-m-xylene
                   and Decachlorobiphenyl.

         20.3.3.2  Analyze the instrument blank according to Section 13
                   at the frequency listed in paragraph 20.3.2.
                   Calculate the results according to Section 16.

20.3.4   Technical Acceptance Criteria for Instrument Blanks

         20.3.4.1  All instrument blanks must be prepared and analyzed
                   at the frequency described in Paragraph 20.3.2 using
                   the procedure in Paragraph 20.3.3 on a GC/ECD system
                   meeting the initial calibration and calibration
                   verification technical acceptance criteria.

         20.3.4.2  The concentration in the instrument blank of each
                   target analyte in Exhibit C must be less than or
                   equal to the CRQL for that analyte.

         20.3.4.3  The instrument blank must meet all sample technical
                   acceptance criteria in Section 17.

20.3.5   Corrective Action

         20.3.5.1  If analytes are detected at greater than the CRQL or
                   the surrogate RTs are outside the RT windows, all
                   data collection must be stopped, and corrective
                   action must be taken.  Data for samples which were
                   run between the last acceptable instrument blank and
                   the unacceptable blank are considered suspect.  An
                   acceptable instrument blank must be run before
                   additional data are collected.  All samples which
                   were run after the last acceptable instrument blank
                   must be reinjected during a valid run sequence and
                   must be reported at no additional cost.

         20.3.S.2  Analysts are cautioned that running an instrument
                   blank once every 12 hours (see Section 10) is the
                   minimum contract requirement.  Late eluting peaks
                   may carry over from one injection to the next if
                   highly complex samples are analyzed or if the GC
                               PEST D-50                         6/91

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                         conditions are unstable.  Such carryover is
                         unacceptable.  Therefore, it may be necessary to run
                         instrument blanks more often to avoid discarding
                         data.

21.   LABORATORY COOTROL SAMPLES (LCS)

21.1  Summary

      The laboratory control sample (LCS) is an internal laboratory quality
      control sample designed to assess (on an SDG-by-SDG basis) the
      capability of the contractor to perform the analytical method listed in
      this Exhibit.

21.2  Frequency

      The LCS must be prepared, extracted, analyzed,  and reported once per
      Sample Delivery Group.  The LCS must be extracted and analyzed
      concurrently with the samples in the SDG using the same instrumentation
      as the samples in the SDG.

21.3  Procedure

      21.3.1  Measure a 1  liter aliquot of  reagent water  in a 1 liter
              graduated cylinder and  transfer  the water to  a continuous
              extractor.   Pipet 1.0 mL of the  LCS spiking solution  (Paragraph
              7.3.7) and 200 uL of the surrogate standard spiking solution
              into  the water and mix  well.   Extract and concentrate the
              sample according to  Section 12.

      21.3.2  Analyze the  LCS  per  Section 13.

21.4  Calculations

      21.4.1  Calculate the results according  to Section  16.

      21.4.2  Calculate individual compound recoveries of the LCS using
              Equation D.33, substituting LCS  percent recovery  for  surrogate
              percent recovery.

21.5  Technical Acceptance Criteria For Laboratory Control Sample Analysis

      21.5.1  The LCS must be  analyzed at the  frequency described in Section
              21.2  on a GC/ECD system meeting  the initial calibration  and
              calibration  verification technical acceptance criteria.

      21.5.2  The LCS must be  prepared as described in Paragraph 21.3.

      21.5.3  The LCS must meet all sample  technical acceptance criteria in
              Section 17.

      21.5.4  The percent  recovery for each of the compounds  in the LCS  mist
              be within the recovery  limits listed in Table D-15.
                                     PEST D-51                         6/91

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                                     Table D-15

                      LABORATORY CONTROL SAMPLE RECOVERY LIMITS
                 COMPOUND                           % RECOVERY
                    •BHC                            56-123
               Heptaehlor epoxide                   74-150
               Dieldrin                             33-130
               4, 4 '-ODE                             50-150
               Endrln                               56-121
               Endosulfan sulfate                   50-100
               gamma- Chlordane                      33-130

               NOTE:   The recovery limits  for any of the  compounds  in the LCS
               may be expanded at any time during the period of performance if
               SMO determines  that the limits are too restrictive.

21.6  Corrective Action

      21.6.1   If the LCS technical acceptance criteria for  the surrogates or
               the LCS compound recovery are  not  met, check  calculations, the
               surrogate and LCS solutions, and instrument performance.   It
               may be necessary to recalibrate the instrument or  take other
               corrective action procedures to meet the surrogate and LCS
               recovery criteria.

      21.6.2   LCS technical acceptance criteria  MUST be  met before data are
               reported.   LCS  contamination from  laboratory  sources or any LCS
               analyzed not meeting the technical acceptance criteria will
               require reextraction and reanalysis of the LCS at  no additional
               cost.

      21.6.3   All samples prepared and analyzed  in an SDG with an  LCS that
               does not meet the technical acceptance criteria will also
               require reextraction and reanalysis at no  additional cost.

22.
22 . 1  Summary
      The PES is an external laboratory quality control sample prepared and
      designed to assess (on an SDG-by-SDG basis) the capability of the
      contractor to perform the analytical method listed in this Exhibit.
                                     PEST D-52                         6/91

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22.2  Frequency
      The Contractor must extract, analyze, and report the PES once per SDG,
      if available.  The PES must be extracted and analyzed concurrently with
      the samples in the SDG using the same instrumentation as the samples in
      the SDG.

22.3  Procedure

      22.3.1   The PES will be received either as an aapulated extract or  as  a
               full volume sample.  If received as an ampulated extract, the
               Contractor will receive instructions concerning the  dilution
               procedure to bring the extract to full volume prior  to
               preparation and analysis of  the PES.

      22.3.2   Add 200 uL of  surrogate solution to 1 liter of  reagent  water
               spiked with the PES solution.  Extract and concentrate  the  FES
               using the procedure described in Section 12.  Analyze the PES
               as  described in Section 13.

22.4  Calculations

      See paragraph 16 for all equations necessary for calculations.

22.5  Technical Acceptance Criteria for Performance Evaluation Sample

      22.5.1   The PES must be analyzed on  a GC/ECD system meeting  the initial
               calibration and calibration  verification technical acceptance
               criteria at the frequency described in Section  22.2.

      22.5.2   The PES must be extracted and concentrated according to Section
               22.3.

      22.5.3   The PES must meet  all sample technical acceptance criteria  in
               Section 17.

22.6  Corrective Action

      22.6.1   If  the PES technical acceptance criteria for the surrogates are
               not met, check calculations, standard solutions and  instrument
               performance.   It may be necessary to recalibrate the instrument
               or  take other  corrective action procedures to meet the
               technical acceptance criteria.  Any PES failing to meet these
               technical acceptance criteria must be reextracted and
               reanalyzed at  no additional  cost.  If insufficient PES  extract
               remains or if  an insufficient volume of the PES remains,
               document this  in the SDG Narrative by stating that the  PES
               could not be reextracted and reanalyzed because insufficient
               volume remained.

      22.6.2   In  addition to complying with the PES technical acceptance
               criteria, the  Contractor will be responsible for correctly
               identifying and quantifying  the compounds included in the
                                     PEST D-53                         6/91

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                 Performance Evaluation Sample.   SMO will notify the Contractor
                 of unacceptable performance.

                 Note:   Unacceptable performance for identification and
                 quantitation of compounds is  defined as a score less than 75
                 percent.

        22.6.3   The FES technical acceptance  criteria HOST be met before sample
                 data are  reported.  Also, the Contractor must demonstrate
                 acceptable performance for compound identification and
                 quantitation.
U S. Environmental Protection Agency
Region 5.Library (PL-12J)
77 West Jackson Boulevard, 12th Moor
Chicago, IL  60604-3590

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