Ul
    REGION m MODIFICATIONS



               TO



NATIONAL FUNCTIONAL GUIDELINES



              FOR



      ORGANIC DATA REVIEW



MULTI-MEDIA, MULTI-CONCENTRATION



        (OLMO1.0-OLMO1.9)
          SEPTEMBER 1994
                 i

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                                                    Region III Modifications
                       FOREWORD
  This document is a modification to the National Functional
 Guidelines for Organic Data Review (Draft, February, 1994).
This document describes those procedures that are to be used for
 Region in Data Validation. It is intended for implementation
      for all  CLP data acquired for use within Region ffl
  but it may  be adapted for use with other similar methods.
 .  All comments and questions pertaining to this document
                "   should be addressed to:
            U.S. Environmental Protection Agency
                         Region ffl
                 Central Regional Laboratory
                  Quality Assurance Branch
                   201 Defense Highway
                         Suite 200
                   Annapolis, MD 21401

                c/o Program Support Section

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                                                                  Region HI Modification*






                               TABLE OF CONTENTS



                                                                             Page



INTRODUCTION	•, . .	  i



PRELIMINARY REVIEW 	,	  ii




DATA QUALIFIER DEFINITIONS		 Hi






VOLATILE DATA REVIEW	 . /	  1




I.    Technical Holding Times	,	  2



H.    GC/MS Instrument Performance Check	  5



m.   Initial Calibration	  g



IV.   Continuing Calibration	   12



V.    Blanks	   15




VI.   System Monitoring Compounds (Surrogate Spikes)	   19



Vfl.   Matrix Spikes/Matrix Spike Duplicates	   23



VBd.  Regional Quality Assurance and Quality Control	   25



IX.   Internal Standards	   27



X. ,   Target Compound Identification	,	   29




XI.   Compound Quantitation and Reported Contract Required Quantitation Limits (CRQLs)  . .   31




XH.   Tentatively Identified Compounds (TICs}	 .   33 -




Xffl.  System Performance	   37



XTV.  Overall Assessment of Data	   38






SEMTVOLATILE DATA REVIEW	   39




I.     Technical Holding Times		   40




H.    GC/MS Instrument Performance Check	   42

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                                                                   Region m Modifications


m.   Initial Calibration	  45
                                 *.
IV.   Continuing Calibration	  49

V.    Blanks			  52

VI.   Surrogate Spikes	  57

VH,  Matrix Spikes/Matrix Spike Duplicates	%	  61

Vm.  Regional Quality Assurance and Quality Control  	  63

DL   Internal Standards	  65

X.    Target Compound Identification'	  67

X.    Compound Quantitation and Reported Contract Required Quantitation Limits (CRQLs)  .  .  69

Xfl.  Tentatively Identified Compounds (TICs)	  71

Xm.  System Performance  .	1	  75

XIV.  Overall Assessment of Data	  76


PESTICIDE DATA REVIEW	  77

I.     Technical  Holding Times	  78

n.    GC/ECD Instrument Performance	 .  80

m.    Initial Calibration		  85

IV.    Continuing Calibration	,-....  88

V.    Blanks		,	  90

VI.    Surrogate  Spikes	 .  94

VI.   Matrix Spike/Matrix Spike Duplicates	  97

VIII.  Regional Quality Assurance and Quality Control	  99

DC.    Pesticide Cleanup Checks	100

X.    Target Compound Identification	 102

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                                                                    Region HI Modifications


XI.   Compound Quantitation and Reported CRQLs	,	105
                                 *i
XD.   Overall Assessment	...,....,...,,	107
APPENDIX A: Contractual Requirements and Equations, Multi-media Multi-concentration  . .   A-l

DRAFT APPENDIX B:  Region ffl Standard Operating Procedure for Data Validation Reports  . B-l

APPENDIX C: Contractual Requirement Comparison Tables	C-l

APPENDIX D: Proposed Guidance for Tentatively Identified Compounds (VOA and SV)  ...   D-l

APPENDIX E: Glossary of Terms  ,	 . E-l

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                                                                             Region Dl Modification*

                                       INTRODUCTION

       This document is designed to offer guidance on EPA Contract Laboratory Program (CLP)
 analytical data evaluation and review.  It has been modified for use within U.S. EPA Region HI.  In some
 applications it may be used as a Standard Operating Procedure (SOP).  In other, more subjective areas,
 only general guidance is offered due to the complexities and uniqueness of data relative to specific
 samples.  For example, areas where the application of specific SOPs are possible are primarily those in
 which definitive performance criteria are established.  These criteria are concerned with specifications
 mat are not sample dependent; they specify performance requirements that  should fully be under a
 laboratory's control.  These specific areas include blanks, calibration standards, performance evaluation
 standard materials, and instrument performance checks (tuning).
                                                                       t
       These Guidelines have been updated to include the requirements in the Statement of Work (SOW)
 for  Organic Analysis  Multi-Media  Multi-Concentration  (SOW  OLM01.0  and  revisions  through
 OLM01.9).

       This update includes changes to instrument performance checks (formerly referred to as tuning)
 and calibration criteria as a result of the Response Factor Workgroup. Regional Modifications to the Data
 Qualifier Definitions from the previous National Functional Guidelines are also included in this document.

       This document is intended to assist in the technical review of analytical data generated through
 the CLP.  Determining  contract  compliance is not the intended objective  of these guidelines or the
 regional data review process. The data review process provides information on analytical limitations of
 data based on specific quality control (QC)  criteria.   In  order  to  provide  more specific usability
 statements, the reviewer must have a  complete understanding of the intended use of the data.  For this
 reason, it is recommended that whenever possible the reviewer obtain usability issues from the user prior
 to reviewing the data. When mis is not possible, the user should  be encouraged to communicate any
 questions to the reviewer. In order to facilitate communication with  the data users in Region ffl, specific
 reporting formats for the data validation report are required. Each report must contain a table of the
 summarized data, sufficient narrative  to inform the user of significant data review issues and adequate
 documentation to support the decisions and  actions of the data reviewer.   The Standard  Operating
 Procedure for preparing the Region in data validation report is presented in  Appendix B.

       At tunes, there may be an urgent need to use data which do not meet all contract requirements
 and technical criteria.  Use of these data does not constitute either a new requirement standard or full
 acceptance of the data.  Any  decision to utilize data for  which performance  criteria have not been met
 is strictly to facilitate the progress of projects requiring the availability of the data. A contract laboratory
 submitting data which are out of specification may  be required to rerun samples or resubmit data even
 if the previously submitted data have been utilized due to urgent program needs; data which do not meet
specified requirements are never fully acceptable.  The only exception to this requirement is in the area
of requirements for individual sample  analysis. If the nature of the sample itself limits the attainment of
specifications, appropriate allowances  must be made. The overriding concern of the Agency is to obtain
data which are technically valid and legally defensible.

       Appendix  A is based  on the Multi-media Multi-concentration SOW and contains appropriate
contractual requirements and equations for verifying various calculations.  Appendix B contains the
Region ID SOP for Data Validation Reports.  Appropriate equations  are presented for easy reference and
to allow the reviewer to verify calculations as needed.   Contractual requirements are provided in
Appendix C to facilitate  comparisons  with the technical  requirements.  Appendix D contains proposed
guidance for Tentatively  Identified Compounds (VOA and SV), and Appendix E contains a glossary of
commonly used terms.

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                                                                             Region III Modifications


                                   PRELIMINARY REVIEW
       In order to use this document effectively, the reviewer should have a general overview of the
 sample delivery group (SDG) or case at hand.  The exact number of samples, their assigned numbers,
 their matrix, and  the number of laboratories involved in their analysis  are  essential information.
 Background information on the site is helpful but often this information may be difficult to locate.  The
 site manager is the best source for answers to questions or further direction.

       Contract Compliance Screening (CCS) is a source of summarized information regarding contract
 compliance. If available, it can be used to alert the reviewer to problems in the SDG data package.

       Sample cases (SDGs) routinely have unique samples which require  special attention by the
 reviewer. These include field blanks, field duplicates, and performance audit samples which need to be
 identified. The sampling records should provide:

       1. Project Officer for site.

       2. Complete list of samples with information on:
            *
         , a. sample matrix,
          b. field blanks,
          c. field duplicates,
          d. field spikes,
          e. QC audit samples,
          f. shipping dates, and
          g. laboratories involved.

      The chain-of-custody record includes sample descriptions and date(s) of sampling.  The reviewer
must take into account lag times between sampling and receipt for  analysis when assessing technical
sample holding times. • • -

      The laboratory's SDG narrative is another source of general information. Notable problems with
matrices, insufficient sample volume for analysis or reanalysis, samples received in broken containers,
and unusual events should be found in the SDG narrative.

      The SDG narrative for the sample data package must include a Laboratory Certification Statement
(exactly as stated  in the SOW), signed by the laboratory manager or designee. This statement authorizes
the validation and release of the sample data results.  In addition, the  laboratory must also provide
comments in the SDG narrative describing in detail any problems encountered in processing the samples
in the data package.

      For every data package, the reviewer must verify that the laboratory certification statement is
present, exactly as in the SOW (i.e., verbatim to the statement in the SOW, and signed by the Laboratory
Manager or designee).  The reviewer must further verify that the data package  is consistent with the
laboratory's certified narrative.  Also, the reviewer should check the comments provided in the narrative
to determine if they are sufficient to describe and explain the associated problem.

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                                                                        Region 111 Modifications
                  GLOSSARY OF DATA QUALIFIER CODES (ORGANIC)
CODES RELATING TO IDENTIFICATION
(CONFIDENCE CONCERNING PRESENCE OR ABSENCE OF COMPOUNDS):

   U =   Not detected. The associated number indicates approximate sample concentration necessary
          to  be detected.

   (NO CODE) = Confirmed identification.

   B =   Not detected substantially above the level reported in laboratory or field blanks.

   R =   Unreliable result.  Analyte may or may not be present in the sample.   Supporting data
          necessary to confirm result.

   N =   Tentative identification. Consider present.  Special methods may be needed to confirm its
          presence or absence in future sampling efforts.
CODES RELATED TO OUANTTTATION
(can be used for both positive results and sample quantitation limits):

   J =  Analyte present.  Reported value may not be accurate or precise.

   K  =  Analyte present.  Reported value may be biased high.  Actual value is expected lower.

   L  =  Analyte present.  Reported value may be biased low.. Actual value is expected to be higher.

  UJ  =  Not detected, quantitation limit may be inaccurate or imprecise.

  UL  = Not detected, quantitation limit is probably higher.



O_THEJI CODES.

   Q  =  No analytical result.

  NJ  =  Qualitative identification questionable due to poor resolution.   Presumptively  present at
         approximate quantity.
                                           in

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                                                                           Region ID Modification!



                                                                                      VGA


                                VOLATILE DATA REVIEW



The volatile data requirements to be checked are listed below

      I.      Technical Holding Times (CCS - Contractual holding times only)

      n.     GC/MS Instrument Performance Check (CCS)

      ffl.     Initial Calibration (CCS)

      IV.     Continuing Calibration (CCS)

      V.     Blanks

      VI.     System Monitoring Compounds (CCS)

      VII.    Matrix Spikes/Matrix Spike Duplicates

      Vin.   Regional Quality Assurance and Quality Control

      DC.     Internal Standards (CCS)

      X.     Target Compound Identification

      XI.     Compound Quantitation and Reported Contract Required Quantitation Limits (CRQLs)

      XII.    Tentatively Identified Compounds

      XIII.   System Performance

      XIV.   Overall Assessment of Data
Note: "CCS" indicates that the contractual requirements for these items will also be checked by CCS;
       CCS requirements are not always the same as the data review criteria.

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                                                                               Ragion III Modification*



                                                                                       VGA
                                 I. Technical Holding Times
 A.   Review Items:  Form I VOA, EPA Sample Traffic Report and/or chain-of-custody, raw data, and
      SDG Narrative.

 B.   Objective

      The objective is to ascertain the validity of results based on the holding time of the sample from
      time of collection to time of analysis.

 C.   Criteria

      Technical requirements for sample holding times have only been established for water matrices.
      The holding times for soils (and other non-aqueous matrices such as sediments, oily wastes, and
      sludge) are currently under investigation.  In Region HI, a 14 day holding time will be applied to
      all non-aqueous samples.   When soil  holding time criteria are established  and  available, the
      procedure for qualifying soil samples will be re-evaluated.

      The holding time criteria for water samples, as stated in the current 40 CFR Part 136 (Clean Water
      Act) is as follows:

            For non-aromatic volatile compounds in cooled (@ 4°Q water samples, the maximum
            holding time is 14 days from sample collection.

            Maximum holding times for purgeable aromatic hydrocarbons in cooled (@ 4°C ± 2°C),
            acid-preserved (pH  2 or below) water samples are 14 days from sample collection.

            Water samples mat have not been maintained at 4°C (± 2°C) and/or preserved to a pH of
            2 or below should be analyzed within 7 days from sample collection. If insufficient ice is
            used to ship samples, the laboratory may  receive samples with no ice left in the cooler.
            Under these circumstances, the temperature of the samples may exceed 4°C.

      It is further required mat volatile compounds in properly preserved non-aqueous  samples be
      analyzed within  14 days of sample collection for all volatile compounds.

      The contractual maximum holding times which differ from the technical maximum holding times
      state mat  water  and soil samples are to be analyzed within 10 days from the validated time of
      sample receipt (VTSR) at the laboratory.

D.    Evaluation

      Technical holding times are established by comparing the sampling dates on the EPA Sample
      Traffic Report with dates of analysis on Form I VOA and the raw data. Information contained in
      the complete  SDG  file (formerly called the purge file) should  also be  considered  in the
      determination  of holding times.  Verify  that the analysis dates on the Form Is and  the  raw
      data/SDG file are identical. Examine me sample records to determine if samples were preserved.

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Technical Holding Times
Region III Modifications

        VOA
      If adequate documentation on sample preservation is not available, contact the sampler.  If the
      sampler cannot be contacted, then it must be assumed mat the samples are unpreserved. If there
      is no indication in the SDG narrative or the sample records that mere was a problem with the
      samples (e.g., samples aot maintained @ 4°C or containing headspace in the samples), then the
      integrity of samples can be assumed to be good. If it is indicated mat there were problems with
      the samples,  men  the integrity of the  sample may have been  compromised  and professional
      judgement should be used to evaluate die effect of the problem on the sample results.

E.    Action

    1.  If technical holding tunes are exceeded, document in the data review narrative that holding times
        were exceeded and qualify the sample results as follows.  (Also see Table 1).

           If there is no evidence mat the aqueous samples were properly preserved and the technical
           holding times exceeded 7 days, qualify positive results with "L" and sample quantitation
           limits with "UL" for all aromatic compounds. Use professional judgement to determine if
           and how non-aromatic volatile compounds should also be qualified.

           If the samples were properly preserved but the technical holding times exceeded 14 days, for
           aqueous and  non-aqueous samples, qualify all positive results with  "L"  and all sample
           quantitation limits with "UL*.
           Table L Qualification of Volatile Analytes Based on Technical Holding Times
Matrix
Water
Non-aqueous
Preserved
No
Yes
No/Yes
> 7 Days
All Aromatics*
None
None
> 14 Days
All Compounds
All Compounds
All Compounds
            * Reviewer should use professional judgement to determine if data for additional
             compounds require qualification.

    2.   If technical holding times are grossly exceeded (e.g., by greater than two tunes the required time
        for volatiles) either on the first analysis or upon re-analysis, the reviewer must use professional
        judgement to determine the reliability of the data and the effects of additional storage on the
        sample results.   Should the reviewer determine mat qualification is necessary, non-detected
        volatile target compounds may be qualified unusable "R".  Positive results are considered bias
        low and are qualified with "L".

    3.   Due to limited  information concerning holding times for  non-aqueous  samples,  it  is
        recommended that a comment in the data review narrative be included to state mat a holding
        time of 14 days was used.

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                                                                              •  Region III Modifications

Technical Holding Times

    4.  Whenever possible, the reviewer should  comment on the effect  of the analysis beyond the
        holding time on the resulting data in the data review narrative.

    5.  He reviewer should also be aware of the scenario in which the laboratory has exceeded the
        technical holding times, but met contractual holding times.  In this case, the data reviewer
        should notify the Regional TPO (where samples were collected) and/or RSCC that shipment
        delays may have occurred so that the field and/or shipping problem can be corrected.  The
        reviewer may pass mis information on to the Regional TPO for that laboratory, but should
        explain mat contractually the laboratory met the requirements,

    6.  When there are other quality control problems to conjunction with exceeded holding times (such
        as suspected laboratory contamination), the reviewer should follow the hierarchy of qualifiers.
        In particular, if  for any reason the reviewer doubts the presence of a compound, the data
        summary form should display only the "B" or "R"  qualifier and not the "L" qualifier.  This is
        because no net direction of bias can be inferred under these  conditions.  When results are
        reported by the laboratory as below the CRQL, the "L" qualifier is used over die "J" qualifier.

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                                                                              Region III Modifications

                                                                                      VGA
                         D- GC/MS Instrument Performance Check


 A. Review Items:  Form V VOA, BFB mass spectra and mass listing.

 B. Objective

    Gas chromatograph/mass spectrometer (GC/MS) instrument performance checks (formerly referred
    to as tuning) are performed to ensure mass resolution, identification, and to some degree, sensitivity.
    These  criteria are  not sample specific.  Conformance  is determined using  standard  materials,
    therefore, these criteria should be met in all circumstances.

 C. Criteria

    Hie analysis of the instrument performance check solution must be performed at the beginning of
    each 12-hour period during which samples or standards are analyzed.  The instrument performance
    check,  bromofluorobenzene (BFB) for volatile analysis, must meet the ion abundance criteria given
    below.                        '

           Bromofluorobenzene (BFB)

           m/z    ION ABUNDANCE CRITERIA

           50     8.0-40.0% of m/z 95
           75     30.0-66.0% of m/z 95
           95     Base peak, 100%  relative abundance
           96     5.0-9.0% of m/z 95
           173    Less man 2.096 of m/z 174
           174    50.0-120.0% of m/z 95
           175    4.0-9.0% of mass  174
           176    93,0 - MM .0% of m/z 174
           177    5.0-9.0% of m/z 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.

D.  Evaluation

    1.   Compare the data presented for each Instrument Performance Check (Form V VOA) with each
        mass listing submitted to ensure the following:

           Form V VOA is present and completed for each 12-hour period during which samples were
           analyzed.

           The laboratory has not made transcription errors between the raw data and the form. If there
           are major differences between the mass listing and the Form Vs, a more in-depth review of
           die data is required. This may include obtaining and reviewing additional information from
           the laboratory.

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                                                                                 Region 111 Modifications

 GC/MS Instrument Performance Check                                                  VGA
           Hie appropriate number of significant figures has been reported (number of significant
           figures given for each ion in the ion abundance criteria column) and mat rounding is correct.
           (See SOW for requirements).

           The laboratory has not made calculation errors.

    2.  Verify from the raw data (mass spectral listing) that the mass assignment is correct and that the
        mass listing is normalized to m/z 95.

    3.  Verify mat the ion abundance criteria was met.  The criteria for m/z 173, 176, and 177 are
        calculated by normalizing to the specified m/z.

    4.  If possible, verify that  spectra were  generated  using  appropriate background subtraction
        techniques. Since the BFB spectrum is obtained from chromatographic peaks that should be free
        from coelution problems, background subtraction should be done in accordance with the
        following procedure. Three scans (the peak apex scan and the scans immediately preceding and
        following the apex) are acquired and averaged and background subtraction must be accomplished
        using a single scan prior to the elution of BFB.

    HQTjg;       All instrument conditions must be identical to those used in the sample analysis.
                  Background subtraction  actions resulting in spectral distortions for the sole purpose
                  of meeting the contract specifications are contrary to the quality assurance objectives
                  and are therefore unacceptable.

E.  Action

    1.  If the laboratory has made minor transcription errors which do not significantly affect the data,
        the data reviewer should make the necessary corrections on a copy of the form.

    2.  If the laboratory has failed to provide the correct forms or has made significant transcription or
        calculation errors, the  Region's designated representative should contact the  laboratory and
        request corrected  data.   If the information is  not  available  then the reviewer must use
        professional judgement to assess the data.

    3.  If mass assignment is in error (such as m/z 96 is indicated as the base peak rather man m/z 95),
        classify all associated data as unusable (R).

    4.  If ion abundance criteria  are not met, professional judgement may be applied to determine to
        what extent the data may be utilized.   Guidelines to aid in the application  of professional
        judgement to mis topic are discussed as follows:

           The most important factors to consider are die empirical results mat are relatively insensitive
           to location on the chromatographic profile  and the type of instrumentation.  Therefore, the
           critical ion abundance criteria for BFB are the m/z 95/96, 174/175, 174/176, and 176/177
           ratios. The relative abundances of m/z 50 and 75 are of lower importance.

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                                                                                Raoion 111 Modifications

GC/MS Instrument Performance Check                                                  VOA
    5.  Decisions to use analytical data associated with BFB instrument performance checks not meeting
        contract requirements should be clearly noted in the data review narrative.

    6.  If the reviewer has reason to believe that instrument performance check criteria were achieved
        using techniques otter than those  described in n.D.4, then additional information on the
        instrument performance checks should be obtained. If the techniques employed are found to be
        at variance with the contract requirements, the performance and procedures of the  laboratory
        may merit evaluation.

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                                                                                  Region 01 Modifications

                                                                                          VGA
                                     III.  Initial Calibration



 A.  Review Items:  Form VI VOA, quantitation reports, and chromatograms.

 B.  Objective

     Compliance requirements for satisfactory instrument calibration are established to ensure that the
     instrument is capable of producing acceptable qualitative and quantitative data for compounds on the
     volatile target compound list (TCL).  Initial calibration demonstrates mat the instrument is capable
     of acceptable performance in the beginning of the analytical run and of producing a linear calibration
     curve.

 C.  Criteria

     1.   Initial calibration standards containing both volatile target compounds and system monitoring
         compounds are analyzed at concentrations of 10, 20, SO, 100, and 200 ug/L at the beginning
         of each analytical sequence or as necessary if the continuing calibration acceptance criteria are
         not met. The initial calibration (and any associated samples and blanks) must be analyzed within
         12 hours of the associated instrument performance check.

     2.   Separate initial calibrations must be performed for water samples (or medium level soil samples)
         and for low level soil samples. The calibration for water samples and medium level soil samples
         is performed with an unheated purge and the calibration for low level soil samples is performed
         with a heated purge.

     3.   Initial calibration standard Relative Response Factors (RRFs) for volatile target compounds and
         system monitoring compounds (surrogates) must be greater than or equal to 0.05.  (Contractual
         initial calibration RRF criteria are listed in Appendix A).

    4.   The Percent Relative Standard Deviation (%RSD) from the initial calibration must be less than
         or equal to 30.0% for all  compounds. (Contractual calibration %RSD criteria are  listed hi
         Appendix A).

D. Evaluation

     1.   Verify that the correct concentration of standards were used for the initial calibration (i.e., 10,
         20, SO, 100, and 200 ug/L for water).

    2.   Verify that the correct initial calibration was used for water and medium level soil samples (i.e.,
         unheated purge) and for low level soil samples (i.e., heated purge).

    3.   If any sample results were calculated using an initial calibration, verify that the correct standard
         (i.e.,  the SO ug/L standard) was used for calculating sample results and that the samples were
         analyzed within  12 hours of the associated instrument performance check.

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                                                                               Region III Modification*

Initial Calibration                                                                      VOA
    4.  Evaluate the initial calibration RRFs and RRF for all volatile target compounds and system
        monitoring compounds (surrogates):
        a.  Check and  recalculate the RRFs and  RRF for at  least one volatile target compound
            associated with each internal standard, verity that the recalculated value(s) agrees with the
            laboratory reported value(s).

        b.  Verify that for all volatile target compounds and system monitoring compounds, the initial
            calibration RRFs are greater than or equal to 0.05.

    NOTE:  Because  historical performance data indicate poor response and/or erratic behavior, the
            volatile compounds in Table 2 have no contractual maximum %RSD criteria. Contractually
            they must meet a minimum RRF criterion of 0.01; however, for data review purposes, the
            "greater than or equal to 0.05" criterion is applied to all volatile compounds.

                  Table 2.  Volatile Target Compounds Exhibiting Poor Response

                            Acetone                      1,2-Dichloropropane
                            2-Butanone                  2-Hexanone
                            Carbon disulfide             Methylene chloride
                            Chloroethane                4-Methyl-2-pentanone
                            Chloromethane               Toluene-d8
                            1,2-Dichloroethene (total)    l,2-Dichloroethane-d4

                  NOTE:  Compounds in bold are  system monitoring compounds.
    5.   Evaluate the %RSD for all volatile target compounds and system monitoring compounds:

        a.  Check and recalculate the %RSD for one or more volatile target compound(s) associated
           with each internal standard; verity that the recalculated value(s) agrees with the laboratory
           reported value(s).

        b.  Verity that all volatile target compounds have a % RSD of less man or equal to 30.0%. The
           contractual criteria for an acceptable initial calibration specifies mat up to any 2 volatile
           target compounds may fail to meet minimum RRF or maximum %RSD as long as they have
           RRFs that are greater than or equal to 0.010, and %RSD of less man or equal to 40.0%.
           For data review purposes, however, alt compounds must be considered for qualification
           when the %RSD exceeds the ± 30.0% criterion.

        c.  If the %RSD is greater than 30.0%, then the reviewer should use professional judgement
           to determine the need to  check the points  on the curve for the cause of the non-linearity.
           This is checked by eliminating either the high point or the low point and recalculating the
           %RSD.

    6.   If errors are detected in the calculations of the initial calibration for either RRF or %RSD,
        perform a more comprehensive evaluation.

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                                                                                 Region 111 Modifications

Initial Calibration                                                                        VOA

E.  Action

    1.  All volatile target  compounds, including the 9 "poor performers"  (see Table 2, system
        monitoring compounds are excluded) will be qualified using the following criteria:

        a.  If the %RSD is greater than 30.0% and all initial calibration RRFs greater than or equal to
            0.05, quality positive results with "I". Non-detects are not qualified. When the %RSD is
            grossly exceeded (i.e., >  50%) use professional judgement for qualifying non-detects as
            "UJ".
        b.  If any initial calibration RRF is less than 0.05, qualify positive results that have acceptable
          *  mass spectral identification with "L", and non-detected analytes as unusable, "R".

    2.   At the reviewer's discretion, a more in-depth review to minimize the qualification of data can
        be accomplished by considering the following:

        a.  If any  of the required volatile compounds have  a %RSD greater man 30.0%, and  if
            eliminating either the high or the low point of the curve does not restore the %RSD to less
            than or equal to 30.0%:

            i.     Qualify positive results for mat compound(s) with "J".

            ii.     No qualifiers are needed for volatile target compounds mat were not detected. If the
                  %RSD is grossly exceeded (i.e.,  >50%), professional judgement is used to qualify
                  iron-detects with "UJ".

        b.  If the high point of the curve is outside of the linearity criteria (e.g., due to saturation):

            i.     No qualifiers are required for positive results in the linear portion of the curve.

            ii.     Qualify positive results outside of the linear portion of the curve with a "J".

            iii.    No qualifiers are needed for volatile target compounds that were not detected. If the
                  %RSD is grossly exceeded (i.e.,  > 50%), professional judgement is used to qualify
                  non-detects with "UJ".

        c.   If the low end of the curve is outside of the linearity criteria:

            i.     No qualifiers are required for positive results hi the linear portion of the curve.

            ii.     Qualify low level positive results in the area of non-linearity with "J".

            iii.    No qualifiers are needed for volatile target compounds that were not detected. If the
                  %RSD is grossly exceeded (i.e.,  >50%), professional judgement is used to qualify
                  non-detects with "UJ").
        NOTE:    If a, b, or c options are used, a description of the process must be dearly stated in
                  the data review narrative.

                                              10

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                                                                                  Region 111 Modifications

Initial Calibration                                                                         VOA
    3.  If the laboratory has  failed to provide  adequate calibration information,  the designated
        representative should contact the laboratory and request the necessary  Information.  If the
        information is not available, the reviewer must use professional judgement to assess the data.

    4,  The potential effects on the data due to unacceptable calibration criteria should be noted in the
        data review narrative.

    5,  When there are other quality control problems in conjunction with exceeding initial calibration
        criteria, the reviewer should follow die hierarchy of qualifiers. In particular, if for any reason
        the reviewer doubts the presence of a compound, die data summary form should display only
        the *B" or "R" qualifier and not the  "L" or "J" qualifier.
                                              11

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                                                                                 Roflion HI Modifications

                                                                                         VOA
                                  IV. Continuing Calibration



A.  Review Items:  Form VII VOA, quantitation reports, and chromatograms

B.  Objective

     Compliance requirements for satisfactory instrument calibration are established to ensure mat the
     instrument is capable of producing  acceptable qualitative  and quantitative  data.   Continuing
     calibration establishes the 12-hour relative response factors on which the quantitations are based and
     checks satisfactory performance of the instrument on a day-to-day basis.

C,  Criteria

     1.  Continuing  calibration standards  containing bom target compounds and  system monitoring
        compounds are analyzed at the beginning of each 12-hour analysis period following the analysis
        of the instrument performance check and prior to the analysis of the method blank and samples.
        The continuing calibration may either be a part of the initial calibration or run independently on
        another 12-hour analysis period.

    2.  The continuing calibration ERF for volatile target compounds and system monitoring compounds
        must be greater man or equal to 0.05.


    3.  The percent difference (%D) between the initial calibration RRF and die continuing calibration
        RRF must be within ±. 25.0%.

D. Evaluation

    1.  Verify that the continuing calibration was run at die required frequency and that the continuing
        calibration was compared to the correct initial calibration.

    2.  Evaluate the continuing calibration RRF for all volatile target compounds and system monitoring
        compounds:

        a.  Check and recalculate  die continuing calibration RRF  for at least one  volatile target
            compound associated with each internal standard; verify oat the recalculated value(s) agrees
            with the laboratory reported value(s),

        b.  Verify mat  all  volatile compounds and  system  monitoring  compounds  meet die RRF
            specifications.

            Because historical performance  data indicate poor response and/or erratic behavior, die
            compounds listed in Table 2 (Section HLD.4) have no contractual maximum %D criteria.
            Contractually they must meet a minimum RRF criterion of 0.01, however, for data review
            purposes, the  "greater  than or equal  to 0.05"  criterion is applied to all volatile
            compounds.

                                              12

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                                                                                Region ill Modifications

Continuing Calibration                                                                  VOA


    3.  Evaluate the %D between initial calibration RRF and continuing calibration RRF for one or
        more compounds).

        a.  Check and recalculate the %D for one or more volatile target compound(s) associated with
            each internal standard; verify that die recalculated value(s) agrees with the laboratory
            reported value(s).

        b.  Verify that the %D  is within ± 25.0%  for all volatile  target compounds and system
            monitoring compounds.  Note those compounds which have a  %D outside the +. 25.0%
            criterion. The contractual criteria for an acceptable continuing calibration specifies that up
            to any 2 volatile target compounds may fail to meet minimum  RRF or maximum %D as
            long as they have RRFs that are greater than or equal to 0.010, and %D of less than or
            equal to 40.0%. For data review purposes, however, all compounds must be considered for
            qualification when the %D exceeds the ±_ 25.0% criterion.

    4.  If errors are detected in the calculations of either the continuing calibration RRF or the %D,
        perform a more comprehensive recalculation.

E.  Action

    1.  The reviewer should use professional judgement to determine if it is necessary to qualify the data
        for any volatile target compound.  If qualification of data is required, it should be performed
        using the following guidelines:

        a.  If the %D is outside the +. 25.0% criterion and the continuing  calibration RRF is greater
            man or equal to 0.05, qualify positive results with "1".

        b.  If the %D is outside the +, 25.0% criterion and the continuing  calibration RRF is greater
            man  or equal  to 0.05, no qualification  of  non-detected volatile target compounds is
            necessary. If the %D is grossly exceeded (>50%), professional judgement may be used
            to qualify non-detects with *UJ".

        c.  If the continuing calibration RRF is less man 0.05, qualify  positive results  that have
            acceptable mass spectral identifications with "L".

        d.  If the continuing calibration RRF is less than 0.05,  qualify non-detected volatile target
            compounds as unusable, "R".

    2.  If the laboratory has  failed to  provide adequate calibration information,  the designated
        representative should contact the  laboratory and  request the necessary information.   If the
        information is not available, the reviewer must use professional judgement to assess the data.

    3.   The potential effects on the data due to unacceptable calibration criteria should be noted in the
        data review narrative.
                                              13

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                                                                                Region 111 Modifications

Continiuing Calibration                                                                 VGA


    4.  When there are otter quality control  problems in conjunction  with  exceeding continuing
        calibration criteria, the reviewer should follow the hierarchy of qualifiers.  In particular, if for
        any reason the reviewer doubts the presence of a compound, the  data summary form should
        display only the "B* or "R* qualifier and not the "L" or "I" qualifier.
                                             14

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                                                                                 Region III Modifications

                                                                                         VOA
                                          v.
A,  Review Items:  Form I VOA, Form IV VOA, chromatograms, and quantitation reports.

B.  Objective

     The purpose of laboratory (or field) blank analysis is to determine the existence and magnitude of
     contamination resulting from laboratory (or field) activities.  The criteria for evaluation of blanks
     apply to any blank associated with the samples (e.g., methods blanks, instrument blanks, trip blanks,
     and equipment blanks).  If problems  with any blank exist, all associated data must be carefully
     evaluated to determine whether or not there is an inherent variability in the data, or if the problem
     is an isolated occurrence not affecting  other data.

C.  Criteria

     1.   No contaminants should be found  in the blanks.

     2.   A method blank analysis must be  performed after the calibration standards and once for every
         12-hour time period beginning with the injection of BFB.

     3.   Hie method blank must be analyzed on each GC/MS system used to analyze samples for each
         type of analysis, i.e., unheated purge (water and medium level soil) and heated purge (low level
         soil).

     4.   An instrument blank should be analyzed after any sample that has saturated ions from a given
         compound to check mat the blank is free of interference and the system is not contaminated.

D.  Evaluation

     1.   Review the results of all associated blanks on the forms and raw data (chromatograms and
         quantitation reports) to evaluate the presence of target and non-target compounds in the blanks.

     2.   Verify that a method blank analysis has been reported per matrix,  per concentration level for
         each  12-hour time period on each GC/MS system used to  analyze volatile samples.  The
         reviewer can use the Method Blank Summary (Form IV VOA) to identify the samples associated
         with each method blank.

     3.   Verify mat the instrument blank analysis has been performed following any sample analysis
         where a target analyte(s)  is reported at high concentration^).

E.   Action

     If the appropriate blanks were not analyzed with the frequency described in Criteria 2,3, and 4, then
    die data reviewer should use professional judgement to determine if the associated sample data should
    be qualified. The reviewer may need to obtain additional information from the laboratory.
                                              15

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                                                                                 Region III Modifications


Blanks                                                                                   VGA
    Action regarding unsuitable blank results depends on the circumstances and origin of the blank.
    Positive sample results should be reported and qualified "B", if the concentration of the compound
    in the sample is less than or equal to 10 times (lOx) the amount in any blank for the common volatile
    laboratory contaminants (methylene chloride, acetone, and 2-butanone), or 5 times (5x) the amount
    for other volatile target compounds. In situations where more than one blank is associated with a
    given sample, qualification should be based upon a comparison with the blank having the highest
    concentration of a contaminant.  The results must not be corrected by subtracting any blank value.

    For qualification purposes, consider all blanks in a case associated with all samples.

    Field blanks measure contamination introduced not only in the field but also from the laboratory.
    In general, evaluation of the impact on specific sample results is handled the same as with laboratory
    blanks.  The reviewer should use caution in attributing contamination to the field as opposed to
    laboratory sources. However, when field-introduced contamination is suspected, it is helpful for the
    reviewer to consult the sampling group to identify possible sources and prevent future reoccurrences.
    Verified field sources of contamination should be noted in the data review narrative.  If a field blank
    has the highest concentration of a contaminant, then all samples in the associated case are qualified
    "B", using the 5x and lOx rule.  Other field blanks associated with  the case are not qualified.
    Specific actions are as follows:

    1.   If a volatile compound is found in a blank but not found in the  sample, no action is taken.

    2.   Any volatile compound detected in the  sample (other than the common  volatile laboratory
        contaminants), mat was also detected in any associated blank, is qualified "B", when the sample
        concentration is  less than five times  (5x) the  blank concentration.  For common volatile
        laboratory contaminants, the results are qualified "B*, when the sample concentration is less man
        10 times (lOx) the blank concentration.

    3.   The reviewer should note mat blanks may not involve the same weights, volumes, or dilution
        factors as the associated samples. These factors must be taken into consideration when applying
        the "Sx"  and "10x"  criteria, such that a comparison of the total  amount of contamination is
        actually made.

        Additionally, mere may be  instances  where little or  no contamination was present in the
        associated blanks, but  qualification of the sample  is deemed necessary.   If the reviewer
       determines that the contamination is from a source other man the sample, he/she should qualify
       the data.  Contamination introduced through dilution water is one example.   Although it is not
       always possible to determine, instances of this occurring it can  be detected when contaminants
       are found in the diluted sample result but are absent in the undiluted sample result.  Since both
       results are not routinely reported, it may  be impossible to verify mis source of contamination.
                                              16

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                                                                                Region 111 Modifications

                                                                                         VOA
                              ¥1. System Monitoring Compounds
                                      (Surrogate Spikes)


A: Review Items: Form II VOA quantitation reports and chromatograms.

B: Objective

    Laboratory performance on individual samples is established by means of spiking activities.  All
    samples are spiked with system monitoring compounds (formerly referred to as surrogates) prior to
    sample purging.   Hie evaluation of the results of these system monitoring  compounds is  not
    necessarily straightforward.   Hie sample itself may  produce effects due to  such factors  as
    interferences  and high concentrations of analytes.   Since the effects  of the sample matrix  are
    frequently outside the control  of the laboratory and may  present relatively unique problems,  the
    evaluation and review of data based on specific sample results is frequently subjective and demands
    analytical experience and professional judgement.  Accordingly, this section consists primarily of
    guidelines, in some cases with  several optional approaches suggested.

C. Criteria

    I.  Three system monitoring compounds (1,2-dichloroethane-d4, bromofluorobenzene, and toluene-
        d8) are added to all samples and blanks to measure their recovery hi environmental samples and
        blank matrices.
   m

    2.  Recoveries for system monitoring compounds in volatile samples and blanks must be within the
        limits specified in Appendix A and the SOW.

D. Evaluation

    1.  Check raw data (e.g., chromatograms and quantitation reports) to verify the recoveries on  the
        System Monitoring Compound Recovery Form ~ Form n VOA.  Check for any calculation or
        transcription errors.

    2.   Check that the system monitoring compound recoveries were calculated correctly.  The equation
        can be found  in Appendix  A.

    3.   The following should be determined from the System Monitoring Compound Recovery form(s):

        a. If any system monitoring compound(s) in the volatile fraction is out of specification, there
           should be a reanalysis to confirm that the non-compliance is due to sample matrix  effects
           rather than laboratory deficiencies.


    NOTE: When there are unacceptable system monitoring compound recoveries followed by successful
        analyses, the laboratories are required to report only the successful run.

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                                                                                 Region III Modifications

System Monitoring Compounds                                                          VOA


        b. Hie laboratory failed to perform acceptably if system monitoring compounds are outside
           criteria with DO evidence of re-analysis. Medium soils must first be re-extracted prior to re-
           analysis when this occurs.

        c. Verify that no blanks have system monitoring compounds outside the criteria,

    4.  Any time there are two or more analyses for a particular sample, the reviewer must determine
        which are the best data to report.  Considerations should include but are not limited to:

        a. System monitoring compound recovery (marginal versus gross deviation).

        b. Technical holding times.

        c. Comparison of the values of the target compounds reported in each sample analysis.

        d. Other QC information, such as performance of internal standards.

E.  Action

    Data are qualified based  on  system monitoring compounds results if the  recovery of any volatile
    system monitoring compound is out of specification. For system monitoring compound recoveries
    out of specification, the following approaches are suggested based on a review of all data from the
    package, especially considering the apparent complexity of the sample matrix.  (Also, see Table 3.)

    1.  If a system monitoring compound in the volatile sample has a recovery greater man the upper
        acceptance limit:

        a. Detected volatile target compounds are qualified "J".

        b. Results for non-detected volatile target compounds should be qualified  "UJ".

    2.  If a system monitoring compound in the volatile sample has a recovery greater than or equal to
        10% but less than the lower acceptance  limit:

        a. Detected volatile target compounds are qualified "J".

        b. For non-detected  volatile target compounds, the sample quantitation limit  is  qualified as
           approximated, "UJ".

    3.  If a system monitoring compound in a volatile sample shows less than 10% recovery:

        a. Detected volatile compounds are qualified "L".

        b. Non-detected  volatile target compounds are qualified as unusable, "R".
                                             20

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                                                                                  Region 111 Modifications

 Blanks                                                                                    VGA
     4.   If gross contamination exists (i.e., saturated peaks by GC/MS), all affected compounds in the
        . associated samples should be qualified as unusable "R" due to interference.

     5.   If inordinate numbers of other target compounds are found at low levels in the blank(s), it may
         be indicative of a problem and should be noted in the report narrative.

     6.   The same consideration given to the  target  compounds should also be given to Tentatively
         Identified Compounds (TlCs), which are found in both the sample and associated blank(s).  (See
         VGA Section Xffl for TIC guidance.)

     7.   If an instrument blank  was not analyzed following a sample analysis which contained an
         analyte(s) at high concentration^), sample analysis results after the high concentration sample
         must be evaluated for carryover.   Professional judgement  should be used to determine if
         instrument  cross-contamination has affected any  positive  compound identifications).   If
         instrument cross-contamination is suggested, then this should be noted for TPO action if the
         cross-contamination is suspected of having an effect on the sample results. Sample results which
         are possible artifacts of carry-over should be  flagged as unusable "R".

     8.   When there is convincing evidence that contamination  is restricted to a particular instrument,
         matrix, or concentration level, the Sx/lOx rule will only be applied to compare contaminated
         blanks to certain associated samples (as opposed to all samples in the case). Some examples are
         as follows:

         Column bleed (siloxanes) may be localized to a particular instrument.

         Methanol extractions in the medium soil volatile analysis protocol can give rise to contaminants
         that are not seen  in the low-level aqueous  analyses.

         Common laboratory contaminants, such as methylene chloride, are generally too unpredictable
         to safely assume contamination is restricted to a particular instrument, matrix, or concentration
         level.

    9.   For  benzene  and/or  toluene,  the reviewer  may identify that  the observed  laboratory
         contamination is attributable to a specific, regular, and predictable process (such as trap bleed),
         which results in a constant 1 or 2 ppb  instrument level concentration in all runs (bom samples
         and blanks).  In this situation, the reviewer may want to consider flaging certain  results as
        tentatively identified,  "N", as opposed  to "B", if the sample instrument level is clearly greater
        man the consistent level of contamination detected in blanks and other samples.  (This particular
        situation supercedes the 5x/10x rule.)
Blanks                                                                                   VOA

                                               17

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                                                                            Rogion HI Modifications

10. The  following  are examples of  applying  the blank  qualification guidelines.   Certain
    circumstances may warrant deviations from these guidelines.  Any deviations must be clearly
    stated in the data review narrative.

    3gx ample ....... |;  Sample result is greater than the Contract Required Quantitation Limit (CRQL),
                but is less man the 5x or lOx multiple of the blank result.

                                                          Rule
                                                       10*    5%

                    Blank Result                        7     7
                    CRQL                              5     5
                    Sample Result                      60    30
                    Final Sample Result                60B    30B

      In the example for the "lOx" rule, sample results less man 70 (or 10 x 7) would be qualified
      "B".  In the case of the "5x" rule, sample results less than 35 (or 5x7) would be qualified
    Example 2:  Sample result is less than the CRQL, and is also less man the 5x or lOx multiple
                of the blank result.

                                                          Rule
                                                       lOx   5x

                    Blank Result                         6     6
                    CRQL                              5     5
                    Sample Result                       4J    4J
                    Final Sample Result                  4B    4B

      Note that data are reported as 4B, indicating that the qualitative presence is not confirmed.

    fa ample j:  Sample result is greater man the 5x or lOx multiple of the blank result.

                                                          Bills
                                                       10%   5%

                    Blank Result                        10     10
                    CRQL                              5     5
                    Sample Result                      12O    60
                    Final Sample Result                 12O    60

      For both the "lOx" and "5x* rules, sample results exceeded the adjusted blank result of 100
      (or 10 x 10) and 50 (or 5 x 10), respectively.

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System Monitoring Compounds
Region III Modifications

        VGA
    4.  If two or three system monitoring compounds in the volatile sample have recoveries outside
        acceptance limits, refer to Table 3.

                       Table 3.  Qualification of Volatile Analytes Based on
                              System Monitoring Compound Recoveries



Detected
Analytes
Non-
Detected
Analytes
1 or more
< 10%

L

R


1
High/Low

J

UJ


2 or 3
High/Low

J

UJ


2 or 3
All Low

L

UL


2 or 3
All
High
K

None

"
    5.   In the special case of a blank analysis with system monitoring  compounds out of specification,
        the reviewer must give special consideration to the validity of associated sample data. The basic
        concern is whether the blank problems represent an isolated problem with the blank alone, or
        whether there is a fundamental problem with the analytical process.  For example, if one or
        more  samples  in the batch  show acceptable  system monitoring compound recoveries,  the
        reviewer may choose to consider the blank problem to be an isolated occurrence.

    6.   Whenever possible, potential effects of the data resulting from system monitoring recoveries not
        meeting the advisory limits should be noted in  the data review narrative.

    7.   Positive results for compounds already flagged for blank contamination,  "B", will not need a
        separate flag for system monitoring compound recoveries. However, these situations should be
        addressed hi the data review narrative and the support documentation.

    8.   When dilutions are performed which prevent detection of system monitoring compounds, the
        data   review  narrative  and   support  documentation should   indicate  that   extraction
        efficiency/method accuracy cannot be verified.

    9.   When both the initial analysis and the reanalysis have system monitoring compound recoveries
        outside of criteria, the data summary form should normally contain the highest concentration
        obtained for each compound detected, provided mat system monitoring compound recoveries in
        the analysis being reported do not suggest a high bias. However, if a demonstrated laboratory
        contaminant  is detected  in one analysis but not in the other, the negative result may be more
        appropriate to report.
                                             21

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                                                                                Region III Modifications

System Monitoring Compounds                                                          VOA
        When the reanalysis of a sample is within the system monitoring compound recovery criteria,
        the laboratory is required to provide only data far the acceptable analysis.  If both sets of data
        are provided, and if a compound was detected in die initial analysis but not in the reanalysis,
        then the  positive  result should be reported (provided the compound  is not a demonstrated
        laboratory contaminant). He reported result should be flagged as estimated "J", due to possible
        sample inhomogeneity.
                                             22

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                                                                               Rayon til Modifications

                                                                                       VOA
                          VH. Matrix Spike/Matrix Spike Duplicate
 A.  Review Items: Form in VOA-I and VOA-2, chromatograms, and quantitation reports.

 B.  Objective

     Data for matrix spike/matrix spike duplicates  (MS/MSD) are generated to determine  long-term
     precision and accuracy of the analytical method on various matrices and to demonstrate acceptable
     compound recovery by the laboratory at the time of sample analysis.  These data alone cannot be
     used to evaluate the precision and accuracy of individual samples.  However, when exercising
     professional judgement, this data should be used in conjunction with other available QC information.

 C.  Criteria

     1.   Matrix spike (MS) and matrix spike duplicate (MSD) samples are analyzed at a frequency of one
         MS and MSD per 20 samples of similar matrix.

     2.   Spike recoveries should be within the advisory limits provided on Form m VOA-1 and VOA-2
         and SOW.

     3.  Relative percent difference (RPD) between MS and MSD recoveries must be within the advisory
        limits provided on Form  ffl VOA-1 and VOA-2 and SOW.

D. Evaluation

     1.   Verify that MS and MSD samples were*analyzed at the required frequency and that results are
        provided for each sample matrix.

    2.   Inspect results for the MS/MSD Recovery on Form in VOA-1 and VOA-2 and verify that the
        results for recovery and RPD are within the advisory limits.

    3.   Verify transcriptions from raw data and verify calculations.

    4.   Check that the matrix spike recoveries and RPDs were calculated correctly.

    5.   Compare %RSD results of non-spiked compounds between the original result, MS, and MSD.

E.  Action

    1.   No action is taken on MS/MSD data alone.  However, using informed professional judgement,
        the data reviewer may use the MS and  MSD results in conjunction with other QC criteria to
        determine the need for some qualification of the data.

    2.   The data reviewer should first try to determine to what extent the results of the MS/MSD affect
        the associated data.  This determination should be made with regard to the MS/MSD sample
        itself as well as specific analytes for all samples associated with the MS/MSD.

                                            23

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                                                                               Region HI Modifications

Matrix Spike/Matrix Spike Duplicate                                                    VOA


    3.   In those instances where it can be determined that the results of the MS/MSD affect only the
        sample spiked, then qualification should be limited to this sample alone.  However,  it may be
        determined through die MS/MSD results that a laboratory is having a systematic problem in the
        analysis of one or more analytes, which affects all associated samples.

    4.   The reviewer must use professional judgement to determine the need for qualification of positive
        results of non-spiked compounds.

    5.   When non-spiked compounds are present in either the MS or MSD results, a table in the data
        review  narrative is constructed showing original (unspiked) sample results for non-spiked
        compounds, non-spiked compounds present in the MS and MSD and the calculated %RSD.
                                            24

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                                                                                Region IK Modification*


                                                                                         VOA
                     Vin.  Regional Quality Assurance and Quality Control
A. Review Items: Form I VOA, cbromatograms, and quantitation reports, and QAPjP,

B. Objective

    Regional Quality Assurance and Quality Control (QA/QC) refer to any  QA and/or QC samples
    initiated by die Region, including field duplicates, Performance Evaluation (PE) samples, blind
    spikes, and blind blanks.

C. Criteria

    Criteria are dependent on the type of QC sample. Frequency may vary,

    1.  The analytes present in the PE sample must be correctly identified and quant Stated.

D. Evaluation

    1.  Evaluation of Performance Evaluation (PE) Samples are not to be presented as part of the data
        review. All Form Is associated with the Performance Evaluation Samples are to be sent (with
        a cover memo stating the case number and laboratory information) directly to  the Quality
        Assurance Branch in Region EQ.

        U.S. Environmental Protection Agency
        Region M, Central Regional Laboratory
        Quality Assurance Branch
        201 Defense Highway, Suite 200
        Annapolis, MD  21401

        Attn: Program Support Section

    2.  Percent difference between target compounds present in  the field duplicate samples shall be
        determined.  Evaluation of the percent difference compared to those specified in the site QAPjP
        may be presented in the data review narrative.

£.  Action

    1.  Field duplicate results are to be presented in a table format in the data review narrative.  If
        target compounds were not present in either of the field duplicate samples, then a table is not
        required.  The percent difference is to be  calculated and presented in  the table. (If one of the
        field duplicates was also used as a matrix spike/matrix spike duplicate sample, men the table
        should include any non-spiked compounds  detected, along with the relative standard deviation.)

        No action is taken based on percent difference of field duplicate sample data alone. However
        using informed professional judgement the data reviewer may use the field duplicate results in
        conjunction with other QC criteria to determine the need for  some qualification of the data.

                                             25

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                                                                               . Region III Modifications

Regional Quality Assurance and Quality Control                             •             VOA


    2.  Other types of Regional QC Samples

        Professional judgement  is needed for evaluating other types of QC samples that may be
        associated with a particular case of samples. This information may be used in conjunction with
        other QC criteria to determine the need for qualification of data,
                                             26

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                                                                                 Region 111 Modifications

                                                                                          VGA
                                    IX.  Internal Standards



 A.  Review Items:  Form VH VOA, quantitation reports, and chromatograms.

 B.  Objective

     Internal Standards (IS) performance criteria ensures that GC/MS sensitivity and response are stable
     during each analysis.

 C.  Criteria

     1.   Internal standard area counts must not vary by  more than a factor of two (-50% to  +100%)
         from the associated calibration standard.

     2.   The retention time of the internal standard must not vary more than .±.30 seconds from the
         retention time of the associated calibration standard.

 D.  Evaluation

     1.   Check raw  data (e.g., chromatograms and quantitation lists) to verify the internal  standard
         retention times and areas reported on the Internal Standard Area Summary (Form Vm VOA).

     2.   Verify that all retention times and IS areas are within criteria.

     3.   If there are  two analyses for a particular fraction, the reviewer must determine which are the
         best data to  report. Considerations should include:

         a.  Magnitude and direction of the IS area shift.

         b.  Magnitude and direction of the IS retention time shift.

         c. Technical holding times.

         d. Comparison of the values of the target compounds reported in each fraction,

         c. Other QC,

E.  Action

     1.  If an IS area count for a sample or blank is outside -50% or +100% of the area for associated
        standard, then:

        a. Positive results for compounds quantitated using mat IS should be qualified as estimated, "J".

        b. Non-detected compounds quantitated using an IS area count greater man +100% or less that
           50% should be qualified "UF.

                                              27

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                                                                                 Region 111 Modifications

Internal Standards                                                                       VOA
        c. If extremely low area counts are reported, or if performance exhibits a major abrupt drop-off
           then a severe loss of sensitivity is indicated.  Non-detected target compounds should then be
           qualified as unusable, "R".

    2.  If an IS retention time varies by more than 30 seconds:

        The  chromatographic profile for mat sample  must be examined to determine if any  false
        positives  or negatives exist. For shifts of a large magnitude, the reviewer may consider partial
        or total rejection of the data lor  mat sample fraction.  Positive results should not need to be
        qualified  as "R", if the mass spectral criteria are met
                                             28

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                                                                                 Region ill Modifications

                                                                                         VGA
                              X.  Target Compound Identification
A. Review Items: Form I VOA, quantitation reports, mass spectra, and chromatograms.

B. Objective

    The objective of die criteria for GC/MS qualitative analysis is to minimize the number of erroneous
    identifications of compounds.  An erroneous identification can either be a false positive (reporting
    a compound present when it is not) or a false negative (not reporting a compound mat is present),

C. Criteria

    1.  The relative retention times (RRTs) must be within ± 0.06 RRT units of the standard RRT.

    2.  Mass spectra of the sample compound and a current laboratory-generated standard (i.e., the mass
        spectrum from the associated calibration standard) must match  according to the following
        criteria:

        a. All ions present in the standard mass spectrum at a relative intensity greater man 10% must
           be present in the sample spectrum.

        b. The relative intensities of these ions must agree within _+ 20% between the standard and
           sample spectra. (Example:  For an ion with an abundance of 50% in the standard spectrum,
           the corresponding sample ion abundance must be between 30% and 70%.)

        c. Ions present at greater wan 10% in the sample mass spectrum but not present in the standard
           spectrum must be considered and accounted for.

D.  Evaluation

    1.   Check that the RRT of reported compounds is within ± 0.06 RRT units of the standard RRT.

    2.   Check the sample compound spectra against the laboratory standard spectra to see mat it meets
        the specified criteria.

    3.   The reviewer should be aware of situations (e.g.,  high concentration samples preceding low
        concentration samples ) when sample carry-over is a possibility and should use professional
        judgement to determine if instrument cross-contamination has affected any positive compound
        identification.  The SOW specifies that an instrument blank must be run after samples in which
        a target analyte ion(s) saturates the detector.

    4.   Check the chromatogram to verify that peaks are accounted for; i.e., major peaks are either
        identified as target compounds, TICs, system monitoring compounds, or internal standards.
                                             29

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                                                                                 Region III Modifications

Target Compound Identification                                                          VOA


E.  Action

    1,  Hie application of qualitative  criteria for GC/MS analysis  of target compounds requires
        professional judgement. It is up to the reviewer's discretion to  obtain additional information
        tram the laboratory.  If it is determined that incorrect identifications were made, all such data
        should be qualified as not detected "U". Hie data review narrative and support documentation
        would verify that the misidentified peak was library searched as a TIC, if appropriate.

    2,  Professional judgement must be used to qualify  the  data  if  it  is  determined that cross-
        contamination has occurred,

    3.  If the presence of a target compound is strongly suggested by raw data, but its mass spectrum
        contains  minor  inadequacies, the compound may be added to the data summary form and
        qualified as a tentative identification, "N".  The reviewer should address corroborating evidence
        in the narrative, such as the presence of the compound in closely related compounds in the same
        sample.

    4.  If the laboratory did not report a compound of acceptable matching quality, the reviewer should
        add this compound  to the  sample data summary form.  The narrative  and  the support
        documentation should indicate this action.  The reviewer should request the laboratory to
        reexamine and resubmit the result, particularly if the value is greater man the CRQL.

    5.  Any changes made  to the reported  compounds or  concerns  regarding target compound
        identifications should be clearly  indicated in the data review narrative.  .
                                             30

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                                                                                 Region 111 Modifications

                                                                                         VGA
                       XI. Compound Ouantitation and Reported CROLs
 A.  Review Items:  Form 1 VOA, sample preparation sheets, SDG narrative, quantitation reports, and
     chromatograms.

 B.  Objective

     The objective is to ensure that the reported quantitation results and Contract Required Quantitation
     Limits (CRQLs) are accurate.

 C.  Criteria

     1.   Compound quantitation, as well as the adjustment of the CRQLs, must be calculated according
         to the correct equation.

     2.   Compound RRFs must be calculated based oa the internal standard (IS) associated with mat
         compound, as listed in Appendix A (also as specified in the SOW) for packed column analyses.
         For analyses performed by capillary column method (EPA Method 524.2),the target compounds
         will  not necessarily be associated with the same internal standard as in the packed column,
         depending on the compound elution order. Quantitation must be based on the quantitation ton
         (m/z) specified in the SOW for both the  IS and target analytes.  The compound quantitation
         must be based on the RRF from the appropriate daily standard.

D.  Evaluation

     1.   For all  fractions, raw data should be examined to verify the correct calculation of ail sample
         results reported by the laboratory. Quantitation lists and chromatograms should be compared
         to the reported positive sample results and quantitation limits.  Check the reported values.

     2.  Verify that the correct internal standard, quantitation ton, and RRF were used to quantitate the
         compound.   Verify  that  the same internal standard, quantitation ion, and RRF  are  used
         consistently through out, in bom the calibration as well as the quantitation process. For analyses
        performed by capillary column, the reviewer should use professional judgement to determine mat
        the laboratory has selected the appropriate internal standard.

     3.  Verify that the CRQLs have been adjusted to reflect all sample dilutions and dry weight factors
        that are not accounted for by the method.

E.  Action

     1.  If any discrepancies are found, the laboratory may be contacted by the designated representative
        to obtain additional information mat could resolve any differences.  If a discrepancy remains
        unresolved, the reviewer must use professional judgement to  decide which value is the best
        value.  Under these circumstances, the reviewer may  determine qualification of data is
        warranted.   A description of the reasons for data qualification and the qualification mat is
        applied  to the data should be documented in the data review narrative and in the document
        support.

                                             31

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                                                                              • Region III Modifications

Compound Quantitation and Reported CRQLs                                           VOA


    2.   Calculation errors can sometimes be revealed by abnormally high system monitoring compound
        recoveries, matrix spike recoveries, or inappropriately high results for certain compounds.

    3.   The reviewer must assure mat any results in error by more man 10 percent are identified and
        corrected on the sample data summary.   If laboratory resubmission is not performed, the
        reviewer should document  his/her  changes to  the data  in  the  narrative and support
        documentation.

    4.   If a sample concentration is above the highest standard and contract required dilutions were not
        performed, the chromatogram and mass spectrum should be examined for signs of a saturated
        signal.  If the ion used for quantitation was saturated, then the result should be flagged as biased
        low,  "L".  If the ion used  for quantitation was not saturated, the result should be flagged as
        estimated, "J".
                                            32

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                                                                                 Region til Modifications

                                                                                         VGA
                            XD.  Tentatively Identified Compounds
A.  Review Items:  Form I VOA-TIC chromatograms, and library search printout and spectra for
     three tentatively identified compounds (TIC) candidates.

B.  Objective

     Chromatographic peaks in volatile fraction analyses that are not target analytes, system monitoring
     compounds or internal standards are potential Tentatively Identified Compounds (TICs). TICs must
     be qualitatively identified by a National Institute of Standards and Technology (NIST) mass spectral
     library search and the identifications assessed by the data reviewer.

C.  Criteria

     For each sample, the laboratory must conduct a mass spectral search of the NIST library and report
     the possible identity for the 10 largest volatile fraction peaks which are not system monitoring
     compounds, internal standards, or target compounds, but which have an area or height greater than
     10 percent of the area or height of the nearest internal standard.  TIC results are reported for each
     sample on the Organic Analyses Data Sheet (Form I VOA-TIC).

     NOTE:    Since the SOW revision  of October 1986, the CLP does not allow the laboratory to
               report as Tentatively  Identified Compounds any  target compound which is properly
               reported in another fraction. For example, late eluting volatile target compounds should
               not be reported as semivolatile TICs.

D.  Evaluation

     1.  Guidelines for tentative identification are as follows:

        a. Major ions (greater than 10%  relative intensity) in the reference spectrum should be present
           in the sample spectrum.

        b. The relative intensities of the major ions should agree within ±_ 20% between the sample and
           the reference spectra.

        c. Molecular ions present in the  reference spectrum should be present in the sample spectrum.

        d. Ions present in the sample spectrum but not in the reference spectrum should be reviewed
           for possible background  contamination, interference or coelution of additional TIC or target
           compounds.

        e. When the above criteria  are not met, but in the technical judgement of the data reviewer or
           mass spectral interpretation specialist the identification is correct, the data reviewer may
           report the identification.
                                              33

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                                                                                 Region 111 Modifications

Tentatively Identified Compounds                                                        VGA


        f.  If in the data reviewer's judgement the identification is uncertain or there are extenuating
           factors affecting compound identifications, the TIC result may be reported as "unknown".

    2.  Check the raw data to verify that the laboratory has generated a library search for all required
        peaks in the chromatograms for samples and blanks.

    3,  Blank chromatograms should be examined to verify that TIC peaks present in samples  are not
        found in blanks.  When a low-level non-target compound that is a common artifact or laboratory
        contaminant is detected in a sample, a thorough check of blank chromatograms  may  require
        looking for peaks which are less man 10 percent of the internal standard height, but present in
        the blank chromatogram at a similar relative retention time.

    4.  All mass spectra for every sample and  blank must be examined.

    5.  Since TIC library searches often yield several candidate compounds having a dose  matching
        score, all reasonable choices must be considered.

    6.  Hie reviewer should be aware of common laboratory artifacts/contaminants and their sources
        (e.g., aldol condensation products, solvent preservatives, and reagent contaminants). These may
        be present in blanks and not reported as sample TICs.

        Examples:

        a.  Common laboratory contaminants: COj (m/z 44), siloxanes (m/z 73), diethyl ether, hexane,
           certain freons (1, l,2-trichloro-l ,2,2-trifluoroethaneorfluorotrichJorometbane), andphthalates
           at levels less man 100 ug/L or 4000 ug/Kg.

        b.  Solvent preservatives such as cyclohexene which  is a methylene  chloride preservative.
           Related by-products include cydohexanone, cydohexenone,  cydohexanol, cyclohexenol,
           chlorocyclohexene, and chlorocyclohexanol.

        c.  Aldol condensation reaction products of acetone include: 4-hydroxy-4-methyl-2-pentanone,
           4-methyl-2-penten-2-one, and 5,5-dimethyl-2(5H)-furanone.

    7.  Occasionally, a target compound may be identified in the proper analytical fraction by non-target
        library search procedures, even {hough  it was not found on the quantitation list.  If the total area
        quantitation method was used, the reviewer should request that the laboratory  recalculate the
        result using the proper quantitation ion. In addition, the reviewer should evaluate other  sample
        chromatograms and check library reference retention times on quantitation lists to determine
        whether the false negative result is an  isolated occurrence or whether additional  data may be
        affected.                                                                         .   .

    8.   Target compounds could be identified  in more man one fraction.  Verify mat quantitation is
        made from the proper fraction.
                                             34

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                                                                                  Region 111 Modifications

Tentatively Identified Compounds                                                         VOA


    9.  Library  searches  should not be performed  on  internal  standards  or system  monitoring
        compounds.

    10. TIC concentration should be estimated assuming a RRF of 1.0.

    11. See Appendix B for additional guidance.

E.  Action

    1.  All TIC results should be qualified "J", estimated concentration, on the laboratory Form I-TICs.

    2.  General actions related to the review of TIC results are as follows:

        a. If it is determined that a tentative identification of a non-target compound is not acceptable,
           the tentative identification should be changed to "unknown" or an appropriate identification.

        b. If all contractually required peaks were not library searched and quantitated, the designated
           representative could request these data from the laboratory.

    3.   Blank Results

        Form I-TIC which contain sample results that are questioned by laboratory results, should be
        flagged "B" and a line drawn through these data for emphasis (initialed and dated), on the Form
        I-TIC that is included in the validation report.

        To  be considered  questionable,  a sample TIC concentration must be  within  10 times the
        concentration of one of  the blank results. If different volumes/weights are used, the total
        amount of compound in the extract must be compared for sample versus blank.  For VOA data,
        an instrument level comparison is used unless the contamination is proven to originate during
        sample storage (before preparation/analysis). In general, blanks analyzed within the same case,
        by the same lab, may be  cross-applied to either soil or water samples extracted or analyzed on
        other days.

        To question a sample result, only presumptive evidence for the presence of the compound in the
        blank is necessary. The presence of the TIC in the blank is suggested in any of the following
        situations:

        a.  Relative retention times (RRTs) match for sample versus blank, and the sample library search
           result matches the same compound 01 compound class as the library search result for the
           blank.

        b.  RRTs match, but library search results do not list the same compound or class  for sample
           versus blank. However, some of the largest ions in the sample are also in the blank, and a
           direct comparison of sample versus blank spectra suggests that the TIC in the sample is quite
           possibly the same compound as that in the blank.
                                              35

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                                                                                 Region III Modifications

Tentatively Identified Compounds                                                         VOA
        c. A peak at the same RRT as the sample TIC is present in the chromatogram of die blank, but
           no library search was performed or included in the data.  (The labs do not have to library
           search peaks less than 10% of the height of the nearest internal standard,  although these
           peaks may still be important to identify low-level  blank contaminants that can question
           sample results at levels above 10% of the nearest internal standard height.)

        All blank results must be attached in the support documentation section of the data review.

    4.  When a compound is not found in any blanks, but is a suspected artifact of common laboratory
        contaminant, the result may be qualified as unusable, "R",  and a line drawn through the result
        (initialed and dated) on a copy of the Form I-TIC that is included in the validation report.

    5.  In deciding  whether a library search  result for a TIC represents a reasonable identification,
        professional judgment must be exercised. If mere is more than one possible match, the result
        may be reported as "either compound  X or compound Y".  If there  is a lack of isomer
        specificity, the TIC result may be changed to a non-specific isomer result (e.g., 1,3,5-trimethyl
        benzene to trimethyl benzene isomer)  or to  a compound class (e.g., 2-methyl,3-ethyl benzene
        to substituted aromatic compound).  These changes may be made directly on a copy of the Form
        I-TIC, as long as changes are initialed and dated.

    6.  Other case factors may influence TIC judgments.  If a sample TIC match is poor but other
        samples have a TIC with a good library match., similar relative retention time, and the same
        ions, identification information may be inferred from the other sample TIC result.

    7.  Physical constants, such as boiling point, may be factored into professional judgment of TIC
        results.

    8.  Any changes made to the reported data or any concerns regarding TIC identifications should be
        indicated in  the data review narrative.  Any changes  made regarding TIC identifications or
        qualifications are to be made on copies of the laboratory generated Form I-TIC and not the
        originals.
                                              36

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                                                                                 Region 111 Modifications

                                                                                          VGA
                                       .  System Performance
A.  Review Items:  Form Vm VOA, Form IH VOA-1 and VOA-2, and chromatogfams.

B.  Objective

     During the period following instrument Performance QC checks (e.g., blanks, tuning, calibration),
     changes may occur in the system that degrade the quality of the data. While this degradation would
     not be directly shown by QC checks until the next required series of analytical QC runs, a thorough
     review of the ongoing data acquisition can yield indicators of instrument performance.

C.  Criteria

     There are no specific criteria for system performance.  Professional judgement should be applied to
     assess the system performance.

D.  Evaluation

     1.  Abrupt,  discrete shifts in the reconstructed ion chromatogram  (R1C) baseline may indicate a
        change in the instrument's sensitivity  or the zero  setting.  A baseline "shift" could indicate a
        decrease in sensitivity in the instrument or an increase in the instrument zero, possibly causing
        target compounds, at or near the detection limit,  to miss detection.  A baseline "rise" could
        indicate problems such  as a change in the instrument zero, a leak, or degradation of the column.

     2.  Poor chromatographic performance affects both qualitative and quantitative results, indications
        of substandard performance include:

        a. High RIC background levels or shifts in absolute retention times of internal standards.

        b. Excessive baseline rise at elevated temperature.

        c. Extraneous peaks.

        d. Loss  of resolution.

        e. Peak  tailing or peak splitting that may result in inaccurate quantitation.

E.  Action

    Professional judgement must be used to qualify the data if it is determined that system performance
    has degraded during  sample analyses.
                                                                                         VOA

                                              37

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                                                                                   Region HI Modification*

                                XIV. Overall Assessment of Data
 A.  Review items: Entire data package, data review results, and (if available) Quality Assurance Project
     Plan (QAPjP), and Sampling and Analysis Plan (SAP),

 B.  Objective

     The overall assessment of a data package is a brief narrative in which the data reviewer expresses
     concerns and comments on the quality and where necessary, the useability of die data.

 C.  Criteria

     Assess the overall quality of the data.

     Review all available materials to assess the overall quality of the data, keeping in mind the additive
     nature of analytical problems.

D.  Evaluation

     1.   Evaluate any technical problems which have not been previously addressed.

    2.   If appropriate information is available, the reviewer may assess the useability of the data to assist
         the data user in avoiding inappropriate use of the data.  Review all available information,
         including the QAPjP (specifically the Data Quality Objectives), SAP, and communication with
         data user that concerns the intended use and desired quality of these data.

£.  Action

     1.   Use professional judgement to determine if mere is any need to  qualify data which were not
         qualified based on the QC criteria previously discussed.

    2.  Write a  brief narrative to give the user an indication of the analytical limitations of the data.
      *  If sufficient information on the intended use and required quality of the data are available, the •
        reviewer should include his/her assessment of the useability of the data within the given context.

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                                                                                      sv

                              SEMTVOLATILE DATA REVIEW



The semivoiatile data requirements to be checked are listed below:

      I.      Technical Holding Times (CCS - Contractual holding times only)

      D.     GC/MS Instrument Performance Check (CCS)

      ni.     Initial Calibration (CCS)

      IV.     Continuing Calibration (CCS)

      V.     Blanks (CCS)

      VI.     Surrogate Spikes (CCS)

      VH.    Matrix Spikes/Matrix Spike Duplicates

      VDL   Regional Quality Assurance and Quality Control

      DC.     Internal Standards (CCS)

      X.     Target Compound Identification

      XI.     Compound Quantitation and Reported Contract Required Quantitation Limits (CRQLs)

      Xn.    Tentatively Identified Compounds

      XIH.   System Performance (CCS)

      XTV.   Overall Assessment of Data
Note: "CCS" indicates that the contractual requirements for these items will also be checked by CCS;
      CCS requirements are not always the same as the data review criteria.
                                           39

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                                                                              Region Ht Modifications


                                                                                           sv
                                  I.  Technical Holding Times
 A.   Review Items: Form I SV-1 and SV-2, EPA Sample Traffic Report ami/or chain-of-custody, raw
      data, and sample extraction sheets.

 B.   Objective

      The objective is to ascertain the validity of .results based on the holding time of the sample from
      time of collection to time of sample extraction and analysis.

 C.   Criteria

      Technical requirements for sample holding times have only been established for water matrices.
      The holding times for soils (and other non-aqueous matrices such as sediments, oily wastes, and
      sludge) are currently under investigation. When the results are available they will be incorporated
      into the data evaluation process. Additionally, results of holding tune studies will be incorporated
      into the data review criteria as the studies are conducted and approved.

      The holding time criteria for water samples, as stated in the current 40 CFR Part 136 (Clean Water
      Act) is as follows:

            For semivolatile compounds in cooled (@ 4°C) water samples the maximum holding
            time  is 7 days from sample  collection to extraction and 40 days from  sample
            extraction to analysis.

      It is further required that semivolatile compounds in properly preserved non-aqueous samples be
      extracted within 7 days  from sample collection  and the extracts analyzed within 40 days from
      sample extraction.

      The contractual holding times, which differ from the technical holding times,  state that water
      samples are to be extracted within 5 days from the validated time of sample receipt (VTSR) at the
      laboratory,  and  soil  samples  are to be extracted within 10 days from  the  VTSR.   Also,
      contractually  both water  and  soil sample extracts must be analyzed within 40  days  of sample
      extraction.  However, the contractual delivery due date is 35 days from the VTSR.

D.    Evaluation

      Technical holding times for sample extraction are established by comparing the sampling date on
      the EPA Sample Traffic Report with the dates of extraction on Form I SV-1 and  SV-2 and the
      sample extraction sheets.  To determine if the samples were analyzed within the holding time after
      extraction,  compare the dates of extraction on  the sample extraction sheets with the dates of
      analysis on Form I SV-1 and SV-2.
                                              40

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                                                                               Region ffl Modification!


Technical Holding Times                                                                    SV
      Verify that the traffic report indicates that the samples were received intact and iced.   If the
      samples  were not  iced  or there were  any problems with the samples upon receipt, then
      discrepancies in the sample condition could effect die data.

E.    Action

      1.    a.   If technical holding times are exceeded, flag all positive results as estimated "I* and
                sample quantitation limits as estimated "UJ" and document that holding times were
                exceeded.   However,  please note that some  extractable  compounds are extremely
                persistent in the environment (e.g., PAHs) in non-aqueous matrices and would  not be
                expected to degrade significantly during sample storage.   The reviewer must use
                professional judgement in the application of data qualifiers to those compounds in non-
                aqueous matrices.

            b.   If in the professional judgement of the data reviewer a loss of semivolatile compound(s)
                is evident due to exceeding the holding time criteria, the affected positive results or the
                associated quantitation limits may be qualified as biased low, "L" or "UL" respectively.
                The narrative must contain the reviewer's justification for qualification of the compound
                results as biased low.

      2.    If technical holding times are grossly exceeded (greater than 2 times the required technical
            holding  time),  either on the first  analysis or upon  re-analysis, the reviewer must use
            professional judgement to determine the reliability of the data and the effects of additional
            storage on  the sample results.  The reviewer may determine that positive results or the
            associated  quantitation limits are approximates and  should  be qualified with "J" or  "UJ",
            respectively. The reviewer may determine mat non-detect data are unusable (R).

      3.    Because of limited information concerning  holding times for  non-aqueous samples, it is
            recommended that a comment in the data review narrative be included to state that aqueous
            holding times were applied.

      4.    Whenever possible, the reviewer should comment on the effect of exceeding the holding time
            on the resulting data in die data review narrative.

      5.    The reviewer should also be aware of die scenario in which  the laboratory has exceeded the
            technical holding times, but met contractual  holding tunes.  In mis case, the date reviewer
            should notify the Regional TPO (where samples were collected) and/or RSCC that shipment
            delays may have occurred so that the field problem  can be corrected.

      6.    When there are other quality control problems in conjunction with exceeded holding times
            (such as suspected laboratory  contamination), the reviewer should follow the hierarchy of
            qualifiers.  In particular, if for any reason the reviewer doubts the presence of a compound,
            the data summary should display only the "B" or "R" qualifier, and not the "L" qualifier.
            This is because  no net direction of bias can be inferred under these conditions.
                                              41

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                                                                          Region 01 ModiGcatkm*


                                                                                       sv
                         n. GC/MS Instrument Performance Cheek


 A.   Review Items:  Form V SV, and DFTPP mass spectra and mass listing.

 B.   Objective

      Gas chromatograph/mass spectrometer (GC/MS) instrument performance checks (formerly referred
      to as tuning) are performed to  ensure mass resolution, identification and, to some degree,
      sensitivity.  These criteria are not sample specific. Conformance is determined using standard
      materials, therefore, these criteria should be met in all circumstances.

 C.   Criteria

      The analysis of the instrument performance check solution must be performed at the beginning of
      each 12-hour period during which samples or standards are analyzed. The instrument performance
      check,  decafluorotriphenylphosphine (DFTPP)  for semivolatile  analysis, must meet the ion
      abundance criteria given below.

                  Decafluorotriphenylphosphine (DFTPP)

                  m/z          ION ABUNDANCE CRITERIA

                  51           30.0-80.0% of m/z 198
                  68           Less than 2.0% of m/z 69
                  69           Present
                  70           Less than 2.0% of m/z 69
                  127          25.0-75.0% of m/z 198
                  197          Less than 1.0% of m/z 198
                  198          Base peak, 100%  relative abundance
                  199          5.0-9.0% of m/z 198
                  275          10.0-30.0% of m/z 198
                  365          Greater man 0.75% of m/z 198
                  441          Present, but less than m/z 443
                  442          40.0 - 110.0% of m/z  198
                  443          15.0 -24.0% of m/z 442

    Note:    All ion abundances 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 mat of m/z 198.

D.  Evaluation

      1.    Compare the data presented on each GC/MS Instrument Performance Check (Form V SV)
           with each mass listing submitted and ensure the following:

           a.  Form V 5V is present and completed for each 12-hour period during which samples
               were analyzed.

                                           42

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 GC/MS Instrument Performance Check                                                     SV
            b.   The laboratory -has not made any transcription errors between the data and the form.
                 If mere are major differences between the mass listing and the Form Vs, a more in-
                 depth  review of the  data is required.  This may  include obtaining  and reviewing
                 additional information from the laboratory.

            c.   The appropriate number of significant figures has been reported (number of significant
                 figures given for each ion in the ion abundance criteria column) and that rounding is
                 correct.

            d.   The laboratory has not made  any calculation errors.

      2.    Verify from the raw data (mass spectral listing) that the mass assignment is correct and that
            the mass is normalized to m/z 198.

      3.    Verify mat the ion abundance criteria was met. The criteria for m/z 68, 70, 441, and 443
            are calculated by normalizing to the specified m/z.

      4.    If possible, verify mat spectra were generated using appropriate background subtraction
            techniques. Since the DFTPP spectrum is obtained from chromatographic peaks that should
            be free from coelution problems, background subtraction should be done in accordance with
            the following procedure.   Three  scans (the peak apex  scan  and the  scans  immediately
            preceding and following the apex) are acquired and  averaged  and background subtraction
            must be accomplished using a single scan prior to the elution of DFTPP.

      Note:      All instrument conditions must be identical to those used  in the sample  analysis.
                 Background subtraction actions resulting in spectral distortions for the sole purpose of
                 meeting the contract specifications are contrary to the quality assurance objectives and
                 are therefore unacceptable.

E.    Action

      1.    If the laboratory has made minor transcription errors which do not significantly affect the
            data, the data reviewer should make the necessary corrections on a copy of the form.

      2.    If the laboratory has failed to provide the correct forms or  has made significant transcription
            or calculation errors, the Region's designated representative should contact the laboratory
            and request corrected data.  If the information is not available, men the reviewer must use
            professional judgement to assess the data.

      3.    If mass assignment is in error (such as m/z 199 is indicated as the base peak rather man m/z
            198), classify all associated data as unusable, "R".

      4.    If ion abundance criteria are not met, professional judgement may be applied to determine
            to what extent the data may be utilized. Guidelines to aid in the application of professional
            judgement in evaluating ion abundance criteria are discussed as follows:
                                              43

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                                                                              Region m Modifications


GC/MS Instrument Performance Check                                                     SV
           a.   Some of the most critical factors in the DFTPP criteria are the non-instrument specific
                requirements that are also not unduly affected by the location of the spectrum on the
                chromatographic profile.  The m/z ratios for 198/199 and 442/443 are critical. These
                ratios are based  on the natural abundances of carbon 12 and carbon 13 and should
                always be met.  Similarly, the relative abundances for m/z 68, 70,  197, and  441
                indicate the condition of the instrument and the suitability of the resolution adjustment
                and are very important.  Note that all  of the foregoing abundances relate to adjacent
                ions; they are relatively insensitive to differences in instrument design and position of
                the spectrum on the chromatographic profile.

           b.   For the ions at m/z 51, 127, and 275,  the actual relative abundance is not as critical.
                For instance, if m/z 275 has 40% relative abundance (criteria: 10.0-30.0%) and other
                criteria are met, then the deficiency is minor.

           c.   The  relative abundance of  m/z  365  is an indicator  of  suitable instrument  zero
                adjustment. If relative abundance for m/z 365 is zero, minimum detection limits may
                be affected.   On the other hand, if m/z  365  is present,  but less man the  0.75%
                minimum abundance criteria, the deficiency is not as serious.

     5.    Decisions to use analytical data associated with DFTPP instrument performance checks not
           meeting contract requirements should be clearly noted in the data review narrative.

     6.    If the  reviewer  has reason  to believe that instrument performance check criteria were
           achieved using techniques other than those specified  in the SOW and n.D.4  above,
           additional information on the DFTPP instrument performance checks should be obtained.
           If the  techniques employed  are found to be at variance with contract  requirements, the
           procedures of the laboratory may merit evaluation.  For example, if the reviewer has reason
           to believe that an inappropriate technique was used to obtain background subtraction (such
           as  background  subtracting  from the solvent front or  from  another region of  the
           chromatogram rather man the DFTPP peak),  men  this should be noted  in the report
           narrative.
                                              44

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                                                                               Region ffl Modification*


                                                                                             sv
                                          Initial Calibration
A.   Review Items:  Form VI SV-1 and SV-2, quantitation reports, and chromatograms.

B.   Objective

      Compliance requirements for satisfactory instrument calibration are established to ensure that die
      instrument is capable of producing acceptable qualitative and quantitative data for compounds on
      the semivolatile Target Compound List (TCL).  Initial calibration demonstrates that the instrument
      is capable of acceptable  performance in the beginning of the analytical  run and of producing a
      linear calibration curve.

C.   Criteria

      1.    Initial calibration standards containing both semivolatile target compounds and surrogates are
            analyzed at concentrations of 20,  SO, 80,  120, and 160 ug/L at the beginning of each
            analytical sequence or as necessary if the continuing calibration acceptance criteria are not
            met. The initial calibration (and any associated samples and blanks) must be analyzed within
            12 hours of the associated instrument performance check.

      2.    Minimum Relative Response Factor (RRF) criteria must be greater than or equal to 0.05.
            Contractual RRF criteria are listed  in Appendix A.

      3.    The Percent Relative Standard Deviations (%RSD) for the  RRFs  in the initial calibration
            must be less than or equal to 30%.

D.   Evaluation

      1.    Verify that the correct concentration of standards were used  for the initial calibration (i.e.,
            20, 50, 80,120, and 160 ug/L). For the eight compounds with higher CRQLs, only a four-
            point initial calibration is required-(i.e., 50, 80, 120, and 160 ug/L).  (See Appendix A for
            list).

      2.    If any sample results were calculated using  an initial calibration, verify  that the correct
            standard  (i.e., the  50 ppb standard) was used  for calculating sample results and that the
            samples were analyzed within 12 hours of the associated instrument performance check.

      3.    Evaluate the RRFs for all semivolatile target  compounds and surrogates:

            a.   Check and recalculate the RRF and RRF for at least one semivolatile target compound
                associated with each internal standard. Verify that the recalculated value(s) agrees with
                the laboratory reported value(s).
                                              45

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                                                                             Region HI ModificatiocM


Initial Calibration                                                                         SV
           b.   Verify that all semivolatile target compounds and surrogates have RRFs that are greater
                than or equal to 0.05. If problems are suspected with low response factor or compound
                identification, also check elution order.

      NOTE:    Because historical performance data indicate poor response and/or erratic behavior, the
                semivolatile compounds to Table 4 have  no contractual  maximum  %RSD  criteria.
                Contractually  they must meet a minimum ERF criteria of 0.01, however, for data
                review purposes,  the "greater than  or equal to 0.05" criterion is applied to all
                semivolatile compounds.

                Table 4. Semivolatile Target Compounds Exhibiting Poor Response

                      2,2'-oxybis(l-Chloropropane)        Diethylphthalate
                      4-Chloroaniline~                   4-Nitroaniline
                      Hexachlorobutadiene                4,6-Dinitro-2-methylphenol
                      Hexachlorocyclopentadiene          N-Nitrosodipbenylamine
                      2-Nitroaniline                      Di-n-butylphthalate
                      Dimethylphthalate                  Butylbenzylphthalate
                      3-NitroaniIine                      3-3'-Dichlorobenzidine
                      2,4-Dinitrophenol                  bis(2-Ethylhexyl)phthalate
                      4-Nitrophenol                      Di-n-octylphthalate
                      Carbazole
    4.   Evaluate the %RSD for all semivolatile target compounds and surrogates.

        a.  Check and recalculate the %RSD for one or more semivolatile target compound(s); verify
           that the recalculated value(s) agrees with the laboratory reported value(s).

        b.  Verify that all semivolatile target compounds have a %RSD of less man or equal to 30%.
           The contractual criteria  for an  acceptable initial calibration specifies that  up to any 4
           semivoiatile target compounds may fail to meet minimum RRF or maximum %RSD as long
           as they have RRFs mat are greater man or equal to 0.010, and %RSD of less man or equal
           to 40,0%.  For data review purposes, however, all compounds must be considered  for
           qualification when the %RSD exceeds the ±_ 30.0% criterion.

        c.  If the %RSD is greater man 30.0%, men the reviewer should use professional judgement to
           determine the need to check the points on the curve for the cause of the non-linearity. This
           is checked by eliminating either the high point or the low point and recalculating the %RSD-

    5.   If errors are detected in the calculations of either  the RRF or the %RSD, perform a more
        comprehensive recalculation.
                                             46

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                                                                                Region III Modification!


Initial Calibration                                                                           SV


E.  Action

    I.  All semivolatile target compounds, including the 19 "poor performers" (see Table 4) will be
        qualified using the following criteria:
        a. If die %RSD is greater than 30.0% and the RRF is greater than or equal to O.OS, qualify
           positive results with "J", and non-detected semivolatile target compounds using professional
           judgement.
        b. If the RRF is  less than O.OS, qualify positive results that have acceptable mass spectral
           identification with "J" using professional judgement, and non-detects as unusable "R".

    2.  At the reviewer's discretion, a more in-depth review to minimize the qualification of data can
        be accomplished by considering the following:

        a. If any of the required semivolatile compounds have a %RSD greater than 30.0%, and if
           eliminating either the high or the low point of the curve does not restore the %RSD to less
           than or  equal to 30.0%:

           i.       Qualify positive results for that compound(s) with "J".

           ii.      Qualify non-detected semivolatile target compounds based on professional judgement.

        b. If the high point of the curve is outside of the linearity criteria (e.g. due to saturation):

           i.       No qualifiers are required for positive results in the linear portion of the curve.

           ii.      Qualify positive results outside of the linear portion of the curve with "I".

           tii.      No qualifiers are needed for non-detected target compounds.

        c.  If the low end of the curve is outside of the  linearity criteria:

           i.       No qualifiers are required for positive results in the linear portion of the curve.

           ii.      Qualify low level positive results in the area of non-linearity with "J".

           iii.      Qualify non-detected semivolatile target compounds using professional judgement.

   3.   If the  laboratory  has  failed to provide adequate calibration information, the designated
        representative should  contact the  laboratory and request the necessary information.  If the
        information is not available, the reviewer must use professional judgement to assess the data.

   4.   Whenever possible, the potential effects on the data resulting from a failure to meet calibration
        criteria should be noted in the data review narrative.
                                              4?

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                                                                              Region QI Modification!


Initial Calibration                                                                          SV
    5.  When it is suspected that relative response factors were incorrectly generated from misidentified
        peaks or incorrect area measurements, the laboratory should be contacted to requantitate these
        RRFs and associated sample results.  Hie report narrative should identify affected results and
        document the cause of the reviewer's suspicions.  In addition, a  CLP telephone log must be
        completed.

    6.  Positive results for compounds flagged for blank contamination *B" will not need a separate flag
        "J" in the data summary form for minimum RRF,  %RSD, or %D outside criteria.  However,
        these situations should be addressed in the data review narrative.
                                             48

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                                                                              Region in Modification*


                                  IV.  Continuing Calibration                              SV



A.  Review Items:  Form VH SV-1 and SV-2, quantitation reports, and chromatograms.

B.  Objective

     Compliance requirements for satisfactory instrument calibration are established to ensure that the
     instrument is capable of producing acceptable qualitative and quantitative data for semivolatile target
     compounds.  Continuing calibration establishes the 12-hour relative response factors on which the
     quantitations are based and checks satisfactory performance of the instrument on a day-to-day basis.

C.  Criteria

     1.  Continuing calibration standards containing both target compounds and surrogates are analyzed
        at the beginning of each 12-hour analysis period following the  analysis of die  instrument
        performance check and prior to the analysis of blanks and samples.

     2.  The  minimum Relative Response  Factors  (RRF)  for  semivolatile target compounds  and
        surrogates must be greater than or equal to 0.05.
    3.  The percent difference (%D) between the initial calibration RRF and the continuing calibration
        RRF must be within ± 25.0% for all target compounds.

D.  Evaluation

    1.  Verify that the continuing calibration was run at the required frequency and mat the continuing
        calibration was compared to the correct initial calibration.

    2.  Evaluate the continuing calibration RRF for all semivolatile target compounds and surrogates.

        a. Check and recalculate the continuing calibration RRF for at least one semivolatile target
           compound for each internal standard; verify that the recalculated value(s) agrees with the
           laboratory reported value(s).

        b. Verify that all semivolatile target compounds and surrogates have RRFs within specifications.

    Note:  Because historical  performance data indicate poor response and/or erratic behavior, the
           compounds  in  Table 4 (Section m.D.3)  have no  contractual  maximum %D criteria.
           Contractually they  must meet a minimum RRF criterion of 0.01, however, for data review
           purposes, the  "greater than  or equal to 0.05" criterion is applied to all  semivolatile
           compounds.
                                              49

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                                                                             Region ID Modifications


Continuing Calibration                                                                    SV
    3,  Evaluate the %D between initial calibration RRF and continuing calibration RRF for one or
        more semivolatile compounds.

        a. Check and recalculate the %D for at least one semivolatile target compound for each internal
           standard; verify that the recalculated value agrees with die laboratory reported value(s).

        b. Verify that the  %D is within the +. 25.0% criterion, for all semivolatile target compounds
           and surrogates.  Note those compounds which have a %D outside the +. 25.0% criterion.
           Hie  contractual criteria for an acceptable continuing calibration specifies that up to any 4
           semivolatile target compounds may fail to meet minimum RRF or maximum %D as long as
           they have RRFs mat are greater than or equal to 0.010, and %D of less than or equal to
           40.0%.  For data  review purposes,  however, all  compounds must  be  considered  for
           qualification when the %D exceeds the  ± 25.0% criterion.

    4.  If errors are detected in the calculations of either the continuing calibration RRF or the %D»
        perform a more comprehensive recalculation.

E.  Action
                           *

    1.  The reviewer should use professional judgement to determine if it is necessary to qualify the data
        for  any semivolatile target compound.   If qualification  of data  is required,  it should be
        performed using the following guidelines:

        a. If the %D is outside the +. 25.0% criterion and the continuing calibration RRF is greater
           man or equal to 0.05, qualify positive results "I*.

        b. If the %D is outside the ±_ 25.0% criterion and the continuing calibration RRF is greater
           than  or  equal  to 0.05,  qualify non-detected  semivolatile target compounds  based  on
           professional judgement.

        c. If the  continuing calibration  RRF is  less than 0.05,  qualify positive results  mat have
           acceptable mass spectral identification with "I" or use professional judgement.

        d. If the continuing calibration RRF is less man 0.05, qualify non-detected semivolatile target
           compounds as unusable "R".

    2.  If the laboratory has  railed  to provide adequate calibration information,  the designated
        representative should contact  the laboratory and request the necessary information.  If  the
        information is not available, the reviewer must use professional judgement to assess the data.

    3.  Whenever possible, the potential effects on die data resulting from a failure to meet calibration
        criteria should be noted in the data review narrative.
                                             50

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                                                                             Region m ModiGulicmx


Continuing Calibration                                                                     SV
    4.  When it is suspected that relative-response factors were incorrectly generated from misidentified
        peaks or incorrect area measurements, the laboratory should be contacted to requantitate these
        RRFs and associated sample results.  The report narrative should identity affected results and
        document the cause of the reviewer's suspicions.  In addition, a CLP telephone log must be
     ,   completed.

    5.  Positive results for compounds flagged for blank contamination "B" will not need a separate flag
        "3" in the data summary form for minimum RRF,  %RSD, or %D outside criteria.  However,
        these situations should be addressed in the data review narrative.
                                             51

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                                                                              Region 01 Modification*


                                                                                           sv
                                          V.  Blanks
A. Review Items: Form I SV-1 and SV-2, Form IV SV, chromatograms, and quantitation reports.

B. Objective.

    The purpose of laboratory (or field) blank analyses is to determine the existence and magnitude of
    contamination problems resulting from laboratory (or field) activities.  The criteria for evaluation of
    blanks apply to any blank associated with the samples (e.g., method blanks, instrument blanks, trip
    blanks, and equipment  blanks).   If problems with any blank exist, all associated  data must be
    carefully evaluated to determine whether or not there is an inherent variability in the  data, or if the
    problem is an  isolated occurrence not affecting other data.

C. Criteria

    1.   No contaminants should be found  in the blanks.

    2.   The method blank must be analyzed on each GC/MS system used to analyze that specific group
         or set of samples.

D. Evaluation

    1.   Review the results of all associated blank, Form I SV-1 and SV-2, and raw data (chromatograms
         and quantitation reports) to evaluate the presence of target and non-target compounds in the
         blanks.

    2.   Verify that a method blank analysis has been reported per matrix, per  concentration level, for
         each extraction batch and for each GC/MS system used to analyze semivolatile samples.  The
         reviewer can use the Method Blank Summary  (Form  IV SV) to assist in identifying samples
        associated with each method blank.

E.  Action

    If the appropriate blanks were not analyzed  with the frequency described above,  men the data
    reviewer should use professional judgement to determine  if the associated sample data should be
    qualified.  The reviewer may  need to obtain additional information from the laboratory.

    Action in the case of unsuitable blank results depends on the circumstances  and origin of the blank.
    Positive sample results should be reported unless the concentration of the compound in the sample
    is less than or equal to 10  times (lOx) the amount in  any blank for the  common  phthalate
    contaminants, or 5 times the amount for other compounds.  In instances where more than one blank
                                              52

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                                                                               Region m Modification!


 Blanks                                                                                      SV
     is associated with a given sample, qualification should be based upon comparison with the associated
     blank* having the highest concentration of a  contaminant.  Toe results must not be corrected by
     subtracting any blank value.

     Field blanks measure contamination introduced not only in the field but also from the laboratory.
     In general, evaluation of the impact on specific sample results is handled as with laboratory blanks.
     The reviewer should use caution in attributing contamination to the field as  opposed to laboratory
     sources.  However, when field-introduced contamination is suspected, it is helpful for the reviewer
     to consult the sampling group to identify possible sources and prevent future reoccurrences. Verified
     field sources of contamination should be noted in the data review narrative.  If a field blank has a
     highest concentration of a contaminant, then all samples in the associated case are qualified "B",
     using the 5x and lOx rule. Other field blanks associated with the case are not qualified.

     Specific actions are as follows:

     1.   If a semivolatile compound is found in a blank but not found in the sample, no action is taken.
         If the contaminants found are volatile target compounds (or interfering non-target compounds)
         at significant concentrations above the CRQL, men this should be noted in the report narrative.

     2.   Any semivolatile compound detected in the  sample (other man  the common  phthalate
         contaminants), that was  also detected  in any associated blank, is qualified "B"  if the sample
         concentration is less than five times (5x) the blank concentration.  For phthalate contaminants,
         the results are qualified IB* when the sample result is less than lOx the blank concentration.

         In using the 5x/10x rule Jo  compare blank results to sample  results which were calculated using
         different weights, volumes, or dilution factors, the reviewer must choose between comparing the
         levels detected with die instrument, the total amount of compound (ug of contamination) present
         in the extracts, or the final concentration of the contaminant in the sample aliquots. Often, more
         than one approach will be acceptable and will yield the equivalent flagging of sample results.

         a.  Comparisons involving sample dry weight correction factors, but with all other calculation
            factors the same for sample versus blank:

            o   In this case, the reviewer can compare the wet weight concentrations, instrument levels,
                or the total amount of compound (ug  of contaminant) in the extracts.  All of these
                approaches will be acceptable and will yield equivalent flagging of sample results.

         b.  When the sample  has  a smaller initial aliquot  size than the blank (purge or  extraction
            weight/volume), but all other calculation factors beyond this analytical step are identical (i.e.,
* For qualification purposes, to determine the highest concentration of a contaminant, consider all blanks
in a case associated with all samples.
                                               53

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                                                                              Region ffl Modification!


Blanks                                                                                     SV
           same final extract volumes, injection volumes, and extract dilution factors for sample versus
           blank):

           o    In this case, it is acceptable and equivalent to compare either instrument levels, the total
                amount  of compound (ug of contaminant) in the  extracts, or the concentration of
                contaminant in the extracts.

           o    Final concentrations of sample versus blank should not be compared.

        c.  When the sample has a larger final extract volume or a greater dilution factor than the blank:

           o    If the laboratory contaminant may have been introduced after or during the sample
                dilution  step, then  a  direct comparison of instrument levels  is appropriate.   For
                example, comparing the instrument level result for a water sample mat was diluted
                1:100 prior to injection would take into account possible laboratory contamination of
                the syringe, instrument, or dilution solvent.

           o    On the other hand, if it is highly probable that the contamination originated before the
                dilution step, then it is more appropriate to calculate and compare the total amount of
                compound (ug of contaminant) present in the undiluted extract of the sample versus the
                blank. For example, a BNA extract diluted 1:100 prior to injection may only be subject
                to   phthalate   contamination   prior   to   the   dilution   step   (i.e.,   during
                extraction/concentration).

           o    If the results of a dilution run are to be flagged "B" because of blank contamination,
                the reviewer should attempt to determine whether an undiluted run was also performed.
                If so, the undiluted run may be used to verify the presence of a compound detected at
                levels too high to be questioned or, conversely, to prove that a compound was actually
                not present at levels  multiplied by a dilution factor.

        The reviewer should note that blanks may not involve  the same weights, volumes, or dilution
        factors as the associated samples.  These factors must be taken into consideration when applying
        the "5x" and " lOx" criteria, such that a comparison of the total amount of contamination is
        actually  made.

        Additionally, mere may  be  instances where  little  or  no contamination was  present in the
        associated blanks, but qualification of the sample was deemed necessary.   Contamination
        introduced through dilution is one example. Although it is not always possible to determine,
        instances of this occurring can be detected when contaminants are found in die diluted sample
        result, but are absent in the undiluted sample result.  Since both results are not routinely
        reported, it may be impossible to verify mis source of contamination. However, if the
        reviewer determines that the contamination is from a source other man the sample, he/she
        should qualify the data.  An  explanation of the rationale used for this determination should be
        provided in the narrative accompanying the Regional Data Assessment Summary.
                                              54

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                                                                              Region M Modifications


Blanks                                                                                     SV

    3.  If gross contamination exists (i.e., saturated peaks by GC/MS), all affected compounds in the
        associated samples should be qualified as unusable "R", due to interference.  This should be
        noted for TPO action if the contamination is suspected of having an effect on the sample results.

    4.  If inordinate amounts of other target compounds are found at low levels in the blank(s), it may
        be indicative of a problem and should be noted for TPO action.
    5.  The same consideration given to the target compounds should also be given to Tentatively
        Identified Compounds (TICs) which are found in both the sample and associated blank(s).  (See
        SV Section XII for TIC guidance.)                               •

    6.  If an instrument  blank was not analyzed following a sample  analysis which contained an
        analyte(s) at high concentration^), sample analysis results after the high concentration sample
        must be evaluated for carryover.   Professional judgement  should be used to determine if
        instrument  cross-contamination has  affected any positive  compound identification(s).   If
        instrument cross-contamination is suggested, then mis should be noted for TPO action if the
        cross-contamination is suspected of having an effect on the sample results.

    7.  Blanks or samples  run after a matrix spike or  standard should  be carefully examined to
        determine the occurrence of instrument or syringe carry-over. Since the efficiency of sample
        transfer can vary dramatically according to apparatus and operator techniques, professional
        judgment should  be used in each case to determine whether  sample or blank results  are
        attributable to carry-over.  Some common examples are as follows:

        o  Zero to .one percent syringe carry-over occasionally in BNA runs.

        o  Higher percentages of carry-over following BNA  runs that are saturated.

        Sample results which are possible artifacts of carry-over should be flagged as unusable, "R".

    8.   When there is convincing evidence mat contamination is restricted to a particular instrument,
        matrix, or concentration level, the 5X/10X rule will  only be applied to compare contaminated
        blanks to certain associated samples (as opposed to all samples in the case).  Some examples are
        as follows:

        o  Column bleed (siloxanes) may be localized to a particular  instrument.

        o  Common laboratory contaminants, such as methylene chloride and phthalates, are generally
           too unpredictable to safely assume contamination is restricted to a particular instrument,
           matrix, or concentration level.
                                              55

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                                                                             Region ID Modifications


Blanks                                                                                    SV

    Hie following are examples of applying the blank qualification guidelines. Certain circumstances
    may warrant deviations from these guidelines.
    Example 1:  Sample result is greater than the Contract Required Quantitation Limit (CRQL), but is
                less than the 5x or lOx multiple of the blank result.

                                                           Rule
                        Blank Result                      7     7
                        CRQL                            5     5
                        Sample Result                    60    30
                        Qualified Sample Result           60S  30B

                  In the example for the "10x" rule, sample results less than 70 (or 10 x 7) would be
                  qualified "B". In the case of the *5x* rule, sample results less than 35 (or 5x7)
                  would be qualified "B".
    Example 2:    Sample result is less than CRQL, and is also less than the 5x or lOx multiple of
                  the blank result.
                                                          Rule
                                                        JO*  &

                        Blank Result                      6     6
                        CRQL                            5     5
                        Sample Result                     4J    4J
                        Qualified Sample Result            4B    4B

                  Note that data are reported as 4B, indicating that the qualitative presence is not
                  confirmed.

        Example 3:  Sample result is greater man the 5x or lOx multiple of the blank result.

                                                          Rule
                        Blank Result                     10    10
                        CRQL                            5     5
                        Sample Result                    120   60
                        Qualified Sample Result           120   60

                  For both the * IQx" and "5x" rules, sample results exceeded the adjusted blank results
                  of 100 (or 10x10) and 50 (or 5x10), respectively.
                                             56

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                                                                               Region m ModiGcAliooi
                                                                                            sv
                                     VI.  Surrogate Spikes
A. Review Items:  Form n SV-1 and SV-2, chromatograms, and quantitation reports.

B. Objective

    Laboratory performance on individual samples is established by means of spiking activities.  All
    samples are spiked with surrogate compounds prior to sample preparation.  The evaluation of the
    results of these surrogate spikes is not necessarily straightforward. The sample itself may produce
    effects because of such factors as interferences and high concentrations of analytes.  Since the effects
    of the sample matrix are frequently outside the control of the laboratory and may present relatively
    unique problems, the evaluation and review of data based on specific sample results is frequently
    subjective and demands  analytical experience and professional judgment.  Accordingly, this section
    consists primarily of guidelines, in some cases with several optional approaches suggested.

C. Criteria

    1.  Surrogate spikes, 4  acid compounds (3 required and  1 advisory) and 4 base/neutral compounds
        (3 required  and 1 advisory)  are added to all samples and blanks to measure their recovery in
        sample and blank matrices.   .

    2.  Surrogate spike recoveries for semivolatile  samples and  blanks  must  be within the limits
        specified in Appendix A and on Form n SV-1 and SV-2 or SOW.

D. Evaluation

    1.  Check raw data (e.g., chromatograms and quantitation reports) to  verify the surrogate spike
        recoveries on the Surrogate Recovery Form tt-SV-1 and SV-2-.  Check for any transcription or
        calculation errors.

    2.  Check that the surrogate spike recoveries were calculated correctly. The equation can be found
        in Appendix A.

    3.  The following should be determined from the Surrogate Recovery form(s):

        a. If any two base/neutral oj acid surrogates are out of specification, or if any one base/neutral
           or acid extractable surrogate has  a recovery of less than  10%,  then  there should be a
           reanalysis to confirm mat the non-compliance is because of sample matrix effects rather man
           laboratory deficiencies.

    ]No|e:  When there are  unacceptable surrogate recoveries followed by successful re-analyses,  the
           laboratories are required to report only the successful run.
                                              57

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                                                                               Region m Modification*


 Surrogate Spikes                                                                           SV

         b.  Hie  laboratory has failed  to  perform satisfactorily if surrogate recoveries  are out of
            specification and there is no evidence of re-injection of the extract, or re-extraction and
            reanalysis (if re-injection fails to resolve the problem).

         c.  Verify that no blanks have surrogates recoveries outside the criteria.

    4.   Any time there are two or more analyses for a particular traction the reviewer must determine
         which are the best data to report.  Considerations should include but are not limited to:

         a.  Surrogate recovery (marginal versus gross deviation).

         b.  Technical holding times.

         c.  Comparison of the values of the target compounds reported in each fraction.

         d.  Other QC information, such as performance of internal standards.

    5.   When both the initial analysis and the reanalysis have surrogate recoveries outside of criteria,
         the data summary should normally contain the highest concentration obtained for each compound
         detected, provided that surrogate recoveries in the analysis being reported do not suggest a high
         bias.  However, if a demonstrated laboratory contaminant is detected in one analysis but not the
         other, the negative result may be more appropriate to report.

         When the reanalysis of a fraction is within surrogate recovery criteria, the laboratory is required
         to provide only data for the acceptable analysis. If both  sets of data are provided, and  if a
         compound  was detected in the  initial analysis but not the reanalysis, then the positive result
         should be reported (provided the compound is not a demonstrated laboratory contaminant). The
         reported result should be flagged as estimated "J", due to possible sample inhomogeneity.

    6    If advisory surrogates are outside established criteria, professional  judgement will be used in
         qualifying the sample results. If the results are outside the criteria, then qualification would only
         affect similar target compounds.

E.  Action

    Data are not qualified with respect to surrogate recovery unless two or more semivolatile surrogates,
    within the same traction (base/neutral or acid fraction), are out of specification. For surrogate spike
    recoveries out of specification, the following approaches are suggested based on a review of all data
    from me case, especially considering the apparent complexity of the sample matrix.

    fstote:  These actions apply to  all  surrogates, except for  "advisory*  surrogates.  Professional
           judgement should be used in qualifying sample results based on  advisory surrogate
           recoveries. Qualification based on advisory surrogate recoveries should be applied to similar
           compounds in the sample only.  Specify in the narrative any actions taken based on advisory
          • surrogate  recovery.
                                              58

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                                                                              Region IB Modifications
Surrogate Spikes
SV
    1.  If two or more surrogates in either semivolatile fraction (base/neutral or acid fraction) have a
        recovery greater than the upper acceptance limit (UL):

        a. Specify the fraction that is being qualified, i.e. acid, base/neutral, or both.

        b. Detected semivolatile target compounds are qualified biased high, "K".

        c. Results for non-detected semivolatile target compounds should not be qualified.

    2.  If two or more surrogates in either semivolatile fraction have a recovery greater man or equal
        to 10% but less than the lower acceptance limit (LL):

        a. Specify the fraction mat is being qualified, i.e. acid, base/neutral, or bom.

        b. Detected semivolatile target compounds are qualified biased low, "L".

        c. For non-detected semivolatile target compounds, the sample quantitation limit is qualified as
           biased low, "UL".

    3.   If any surrogate in either semivolatile fraction show less man 10% recovery:

        a. Specify the fraction mat  is  being qualified, i.e. acid, base/neutral, or both,

        b. Detected  semivolatile target compounds are qualified biased low, "L*.

        c. Non-detected semivolatile target compounds may be qualified as unusable "R". (If advisory
          surrogate limits are not met, use professional judgement to qualify non-detected compounds).

                     Table 5. Qualification of Semivolatile Anal vies Based on
                                     Surrogate Recoveries

                                 SURROGATE RECOVERY

Detected analytes
Non-detected analytes
2 or 3
all high
K
i
none
2 or 3
all low
L
UL
2 or 3
mixed high/low
J
UJ
1 or more
< 10% rec.
L
R
   4.  If two or more surrogate recoveries in either semivolatile fraction (base/neutral or acid fraction)
       are outside surrogate recovery limits, and one of the recoveries is below the lower limit (but
       > 10%) and the other recovery is above the upper limit:

       a. Specify the fraction that is being qualified, i.e., acid, base/neutral, or bom.
                                             59

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                                                                               Region ID Modifications


Surrogate Spikes                                                                            SV

                                                            *•
        b. Detected semivolatile target compounds are qualified as estimated, "J".

        c. Non-detected semivolatile target compounds are qualified as estimated, "UJ".

    5.  In the special case of a blank analysis with surrogates out of specification, the reviewer must
        give special  consideration to the validity of associated sample data.  The basic concern is
        whether the blank problems represent an isolated problem with the blank alone, or whether mere
        is a fundamental problem with the analytical process.  For example, if one or more samples in
        the batch show acceptable surrogate recoveries, the reviewer may choose to consider the blank
        problem  to be an isolated occurrence.  However, even if this judgement allows some use of the
        affected  data, analytical problems should be noted for TPO action.  Also note if there  are
        potential contractual problems associated with the lack of re-analysis of samples that were  out
        of specification.

    6.  Whenever possible, the potential effects of the data resulting from surrogate recoveries  not
        meeting the advisory limits should be noted in the data review narrative.

    7.  Positive results for compounds already flagged for blank contamination will not need a separate
        flag for surrogate recoveries.  However, these situations should be addressed in die narrative
        or the support documentation.

    8.  When dilutions are performed which prevent  detection of BNA  surrogate compounds,  the
        narrative or support documentation should indicate that extraction efficiency/method accuracy
        cannot be verified.

    9.  Although semivolatile surrogate recoveries cannot usually be correlated with specific analytes,
        in the following cases specific action will be allowed based upon a particular surrogate:

        a. When a semivolatile surrogate is the deuterated analog of a TCL analyte (for example,  d3-
           phenol and phenol), a low recovery for the surrogate can be used to flag positive results and
           quantitation limits as biased low for the undeuterated analog. (This applies even if no other
           surrogates are outside criteria or if other surrogates are biased high instead of low.)

        b. When d12-terphenyl is biased low, positive results and quantitation limits for the heavier
           polyaromatic hydrocarbons (those which elute starting with fluorathene) can be considered
           as biased  low.  (This applies even if no other surrogates are  outside criteria  or  if other
        •   surrogates are biased high instead of low.)

        c. When 2,4,6-tribromophenol is  biased  low,positive  results and  quantitation limits  for
           trichlorophenols and pentachlorophenol can be considered as biased low.  (mis applies even
           if no other surrogates are outside criteria or  if other surrogates are biased high instead of
           low.)
                                              60

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                                                                            Region HI Modification*


                                                                                         sv
                         VH.  Matrix Spikes/Matrix Spike Duplicates
 A. Review Items: Form in SV-1 and SV-2, chromatograms, and quantitation reports.

 B. Objective

    Data for matrix spikes/matrix spike duplicates (MS/MSD) are generated to determine long-term
    precision and accuracy of die analytical method on various matrices and to demonstrate acceptable
    compound recovery by the laboratory at the tune of sample analysis.  These data alone cannot be
    used to evaluate the precision and accuracy of individual samples.   However, when exercising
    professional judgement, this data should be used in conjunction with other available QC information.

 C. Criteria

    1.  Matrix spike and matrix spike duplicate samples are analyzed at frequency of one MS and MSD
        per 20 samples of similar matrix.

    2.  Matrix spike and matrix spike duplicate recoveries should be  within the advisory limits
        established on Form in SV-1 and SV-2 and in the SOW..

    3.  Hie Relative Percent Differences (RPDs) between matrix spike  and matrix spike duplicate
        recoveries should be within the advisory limits listed on Form in SV-1 and SV-2 and in the
        SOW.

D. Evaluation

    1.  Verify that MS and MSD samples were analyzed at the required frequency and that results are
        provided for each sample matrix.

    2.   Inspect results for the MS/MSD Recovery on Form HI SV-1 and SV-2 and verify mat the results
        for recovery and RPD are within the advisory limits.

    3.   Verify transcriptions from raw data and verify calculations.

    4.   Check that the recoveries and RPDs were calculated correctly.

    5,   Compare results (%RSD) of non-spiked compounds between the original result, MS, and MSD.

E.  Action

    1.   No action  is taken on MS/MSD  data alone. However, using informed professional judgment
        the data reviewer may use the matrix spike and matrix spike duplicate results in conjunction with
        other QC criteria and determine the need for some qualification of the data.
                                             61

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                                                                            Region m Modi6cttioiu


Matrix Spikes/Matrix Spike Duplicates                                                     SV


    2.  The data reviewer should first try to determine to what extent the results of the MS/MSD effect
        the associated data.  This determination should be made with regard to the MS/MSD sample
        itself as well as specific analytes for all samples  associated with the MS/MSD.

    3.  In those instances where it can be determined that the results of the MS/MSD effect only the
        sample spiked, then qualification should be limited to this sample alone. However, it may be
        determined through the MS/MSD results that a laboratory is having a systematic problem in the
        analysis of one or more analytes, which affects all associated samples.

    4.  The reviewer must use professional judgement to determine the need for qualification of positive
        results of non-spiked compounds.
    5.   When extremely low % recoveries are noted, qualify data for all affected  compounds using
        professional judgement.

    6.   When non-spiked compounds are present in either the MS or MSD results, a table in the data
        review narrative  is  constructed showing original (unspiked)  sample results for  non-spiked
        compounds, non-spiked compounds present in the MS and MSD and the calculated %RSD.

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                                                                              Region m Modi fuatioiu


                                                                                            sv
                     VBi. Regional Quality Assurance and Quality Control



 A.  Review Items:  Form I SV, Chromatograms, and Quantitation reports.

 B.  Objective

     Regional  Quality Assurance and  Quality Control (QA/QC) refer to any QA  and/or QC samples
     initiated by die Region, including field duplicates, Performance Evaluation (PE) samples, blind
     spikes, and blind blanks.

 C.  Criteria

     Criteria are dependent on the type of QC sample.  Frequency may vary.

     1.  The analytes present in the PE sample must be correctly identified and quantitated.

 D.  Evaluation

     1.  Evaluation of Performance Evaluation (PE) Samples are not to be presented as part of the data
        review.  All forms associated .with the Performance Evaluation Samples are to be sent (with a
        cover memo stating the  case number  and  laboratory information)  directly to the Quality
        Assurance Branch in Region M.

        U.S.  Environmental Protection Agency
        Region III, Central Regional Laboratory
        Quality Assurance Branch
        201 Defense Highway, Suite 200
        Annapolis, MD  21401

        Attn:  Program Support Section

    2.  Percent difference between target compounds present in the field duplicate samples shall be
        determined. Evaluation of the percent difference compared to those specified in the site Quality
        Assurance Project Plan may be presented in the data review narrative.

E.  Action

     1.  Field duplicate results are to be presented in a table form in the data review narrative.  If target
        compounds were not present in either of the field duplicate samples, men a table is not required.
        The percent difference is to  be calculated and presented  in the table,   (if  one of the field
        duplicates was also used as a  matrix spike/matrix spike duplicate sample, then the table should
        include any non-spiked compounds detected,  along with the % relative standard deviation.)
                                              63

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                                                                             Regton ID ModiDcationi


Regional Quality Assurance and Quality Control                                            SV
        No action is taken based on percent difference of field duplicate sample data alone.  However,
        using informed professional judgement, the data reviewer may use the field duplicate results in
        conjunction with other QC criteria and determine the need for some qualification of the data.

    2.  Other types of Regional QC Samples

        Professional judgement is  needed for evaluating  other  types  of QC samples that may be
        associated with a particular case of samples.  This information may be used in conjunction with
        other QC criteria to determine the need for qualification of data.
                                             64

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                                                                              Region HI Modification!


                                                                                           sv
                                    IX. Internal Standards
A. Review Items: Form Vffl SV-1 and SV-2 , quantitation reports, and chromatograms.

B. Objective

    Internal Standards (IS) performance criteria ensure that GC/MS sensitivity and response are stable
    during every analytical run.

C. Criteria

    1 .  Internal standard area counts for samples and blanks must not vary by more than a factor of two
        (- 50% to +  100%) from the associated calibration standard.

    2.  Hie retention time of the internal standards in samples and blanks must not vary by more than
        +_ 30 seconds from the retention time of the associated calibration standard.

D. Evaluation

    1 .  Check raw data (e.g. , chromatograms and quantitation lists) for samples and blanks to verify the
        internal standard retention times and areas reported on the Internal Standard Area Summary
        (Forms Vm SV-1, Vffl SV-2).
    2.  Verify that all retention times and IS areas are within the required criteria.

    3.  If there are two analyses for a particular fraction, the reviewer must determine which ate the
        best data to report.  Considerations should include:

        a. Magnitude and direction of the IS area shift.

        b. Magnitude and direction of the IS retention time shift.

        c. Technical holding times.

        d. Comparison of the values of the target compounds reported in each fraction.

E.  Action

    1.  If an  IS area count for a sample or blank is outside - 50% or  + 100% of the area for the
        associated standard:

        a. Positive results for compounds quantitated using that IS should be qualified with "1*.

        b. Non-detected compounds quantitated using an IS area count greater than + 100% or less man
           50% should be qualified with "UF.

                                              65

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                                                                              Region IQ Modification!


Internal Standards                                                                          SV
        c. If extremely low area counts are reported, or if performance exhibits a major abrupt drop-
           off, men a severe loss of sensitivity is indicated, Non-detected target compounds should men
           be qualified as unusable "R".

    2.  If an IS retention time varies by more man 30 seconds:

        The  chromatograpbic profile for mat  sample must  be examined to  determine if any false
        positives or negatives  exist.  For shifts of a large magnitude, the reviewer may consider partial
        or total rejection (R) of the data for that sample fraction. Positive results should not need to be
        qualified with "R* if the mass spectral criteria are met.

    3.  If the internal standards performance criteria are grossly exceeded, then this should be noted for
        TPO action.   Potential effects on the data resulting from unacceptable  internal standard
        performance should be noted in the data review narrative.

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                                                                              Region ID Modification!


                                                                                           sv
                              X.  Target Compound Identification
A* Review Items:  Form I SV-1 and SV-2  quantitation reports, mass spectra, and chromatograms.

B. Objective

    Qualitative criteria for compound identification have been established to minimize the number of
    erroneous identifications of compounds. An erroneous identification can either be a false positive
    (reporting a compound present when it is not) or a false negative (not reporting a compound that is
    present).

    The identification criteria can be applied much more easily in detecting false positives than false
    negatives.  More information is available due to the requirement for submittal of data supporting
    positive identifications. Negatives,  or non-detected compounds,  on the other hand  represent an
    absence of data and are, therefore, much more difficult to assess.  One  example  of detecting false
    negatives is the reporting of a Target Compound as a TIC.

C. Criteria

    1.  Compound must be within ± 0.06 relative retention time (RRT) units of the  standard RRT.

    2.  Mass spectra of the sample compound and a current laboratory-generated standard must match
        according to the following criteria:

        a. All ions present in the standard mass spectrum at a relative intensity greater than 10% must
           be present in the sample spectrum.

        b. The relative intensities of these ions must agree within ± 20%  between the standard and
           sample spectra.  (Example: For an ion with an abundance of 50% in the standard spectrum,
           the corresponding sample ion abundance must be between 30% and 70%.)

        c. Ions present at greater than 10% in the, sample mass spectrum but not present in the standard
           spectrum must be considered and accounted for.

D.  Evaluation

    1.  Check that the RRT of reported  compounds is within ± 0.06 RRT units of the standard relative
        retention time.

    2.  Check the sample compound spectra against the laboratory standard spectra to verify that its
        meets the specified criteria.

    3.  The reviewer should be  aware  of situations (e.g.,  high concentration samples preceding low
        concentration samples) when sample carryover is  a possibility and should  use judgment to
        determine if instrument cross-contamination has affected any positive compound identification.
                                              67

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                                                                              Region ID Modification*


Target Compound Identification                                                             SV
    4.  Check the chromatograra to verify that peaks are accounted for, i.e., major peaks are either
        identified as target compounds, TICs, surrogates, or internal standards.

E.  Action

    1.  The application of qualitative criteria for  GC/MS  analysis of target compounds requires
        professional judgement.  It is up to the reviewer's discretion to obtain additional information
        from the laboratory.  If it is determined .that incorrect identifications were made, all such data
        should be qualified as not detected "U" or unusable "R".

    2.  Professional judgement must  be used to  qualify the data if it is determined that cross-
        contamination has occurred.

    3.  Any changes  made  to the reported  compounds  or concerns regarding  target compound
        identifications should be clearly indicated  in the data review narrative.  The necessity for
        numerous or significant changes should be noted for TPO action.

    4.  If it is determined mat incorrect identifications were made, all such data should be reported as
        not-detected, and the narrative and the support documentation should indicate this action. In
        addition, the reviewer should verify that the misidentified peak was library searched as a TIC,
        if appropriate.

    5.  If the presence of a target compound is strongly suggested by raw data, but its mass spectrum
        contains minor inadequacies, the compound may be added to the data summary and qualified as
        a tentative identification "N".  The reviewer  should address corroborating evidence in the
        narrative, such as the presence of the compound in closely related compounds in the same
        sample.

    6.  If the laboratory did not report a compound of acceptable matching quality, the reviewer should
        add this compound to the sample data summary. The narrative and the support documentation
        should  indicate this action, as well as the ORDA. The reviewer should request the laboratory
        to re-examine and resubmit the result, particularly if the value is greater than the CRQL.

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                                                                               Region in Modification*


                                                                                            sv
                       XI. Compound Ouantitation and Reported CROLS
 A.  Review Items:  Form I SV-1 and SV-2, sample preparation sheets, case narrative, sample clean-up
     sheets, quantitation reports, and chromatograms.

 B.  Objective

     The objective is to ensure that the reported quantitation results and Contract Required Quantitation
     Limits (CRQLs) for semivolatUe target compounds are accurate.

 C.  Criteria

     1.   Compound quantitation, as well as the adjustment of the CRQL, must be calculated according
         to the correct equation.

     2.   Compound area responses must be calculated based on the internal standard (IS) associated with
         that compound, as listed in Appendix (also as specified in the Statement of Work).  Quantitation
         must be based on the quantitation ion (m/z) specified in the SOW for bom  the IS and target
         analytes.  The compound quantitation must be based on the RRF from the  appropriate daily
         calibration standard.

D.  Evaluation

     1.   For all fractions, raw data should be examined to verify the correct calculation of all sample
         results reported  by the laboratory. Quantitation lists, chromatograms, and sample preparation
         log sheets should be compared  to the reported positive sample results and quantitation limits.
         Check the reported values.  Calculation errors can sometimes be revealed by abnormally high
         surrogate recoveries, matrix spike  recoveries, or  inappropriately high results  for certain
         compounds.

     2.   Verify that the correct internal standard, quantitation ion, and RRF were used to quantitate the
         compound.   Verify that  the same  internal standard, quantitation ion, and RRF  are used
         consistently throughout the calibration and quantitation processes.

     3.   Verify that the CRQLs have been adjusted to reflect all sample dilutions, concentrations, splits,
         clean-up activities, and dry weight factors that are not accounted for by the method.

E.  Action

     1.  If there are  any discrepancies  found,  the laboratory  may be contacted  by the designated
         representative to obtain additional  information that could resolve  any differences.   If a
        discrepancy remains unresolved, the reviewer must use professional judgement to decide which
        value is the best value.  Under these circumstances,  the reviewer may determine
         qualification of data is warranted. Decisions made on data quality should be included in the data
        review narrative. A description of the reasons for data qualification and the qualification that
         is applied to the data should be  documented in the data review narrative.

                                              69

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                                                                            Region O Modifications


Compound Quantitation and Reported CRQLS                                             SV
    2.   Numerous or significant failures to accurately quantify the target compound or to properly
        evaluate and adjust CRQLs should be noted for TPO action.

    3.   The reviewer must assure that any results in error by more than 10 percent are identified and
        corrected on  the sample data summary.  If laboratory resubmission is not performed, the
        reviewer should document his/her changes to the data in the narrative or support documentation.
        Calculation errors should also be noted on the ORDA.

    4.   If a sample concentration is above the highest standard and  contract required dilutions were not
        performed, the TPO should be informed on the ORDA. The chromatogram and mass spectrum
        should  be examined for signs of a saturated signal.  If the ion used  for  quantitation was
        saturated, then the result should be flagged as biased low, "L". If the ion used for quantitation
        was not saturated, the result should be flagged as estimated, "I*.

    5.   When sample results were quantitated  using RRFs from the wrong calibration standard, the
        laboratory should resubmit these results.   The ORDA should  identify affected results and
        document the error. In addition, a CLP telephone log must be completed.
                                             70

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                                                                               Region m Modification


                                                                                            sv
                            XII.  Tentatively Identified Compounds
A. Review Items:  Form ISV-TIC, chromatograms, and library search printout with spectra for three
    TIC candidates.

B. Objective

    Chromatographic peaks in semivolatile fraction analyses that are not target analytes, surrogates, or
    internal standards are potential tentatively identified compounds (TICs).  TICs must be qualitatively
    identified by a National Institute of Standards and Technology (HIST) mass spectral library search
    and the identifications assessed by the data reviewer.

C. Criteria

    For each sample, the laboratory must conduct a mass spectral search of the MIST library and report
    the possible identity for the 20 largest semivolatile fraction peaks which are not surrogate, internal
    standard,  or target compounds, but which have area or height greater than 10 percent of the area or
    height of  the nearest internal standard.  TIC results are reported for each sample on the Organic
    Analyses Data Sheet (Form I SV-TIC).

    Note:  Since the SOW revision of October 1986, the CLP does not allow the laboratory to report
           as tentatively identified compounds any target compound  which is properly  reported in
           another fraction.  For example, late eluting volatile target compounds should not be reported
           as semivolatile TICs.

D. Evaluation

    1.  Guidelines for tentative identification are as follows:

        a. Major ions (greater than 10% relative intensity) in the reference spectrum should be present
           in the sample spectrum.

        b. The relative intensities of the major ions should agree within .±20% between the sample and
           the reference spectra.

        c. Molecular ions present in the reference spectrum should be present in the sample spectrum.

        d. Ions present in the sample spectrum but not in the reference spectrum should be reviewed
           for possible background contamination, interference, or coelution of additional TIC or target
           compounds.

        e. When the above criteria are not met, but in the technical judgment of the data reviewer or
           mass spectra! interpretation specialist the identification is correct, the data reviewer may
           report the identification.
                                              71

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                                                                              Region ID Modi6c*tioa»


Tentatively Identified Compounds                                                           SV
        f. If in the data reviewer's judgment the identification is uncertain or there are extenuating
           factors affecting compound identifications, the TIC result may be reported as "unknown",

    2.  Check the raw data to verify that the laboratory has generated a library search for all required
        peaks in the chromatograms for samples and blanks.

    3.  Blank chromatograms should be examined to verify mat TIC peaks present in samples are not
        found in blanks. When a low-level non-target compound that is a common artifact or laboratory
        contaminant is detected in  a sample, a thorough check of blank chromatograms  may require
        looking for peaks which are less than 10 percent of the internal standard height, but present in
        the blank chromatogram at a similar relative retention time.

    4.  All mass spectra for each sample and blank must be examined.

    5.  Since TIC library searches often yield several candidate compounds having a close matching
        score, all reasonable choices should be considered.

    6.  The reviewer should be aware of common laboratory artifacts/contaminants and their sources
        (e.g., aldol condensation products, solvent preservatives, and reagent contaminants). These may
        be present in blanks and not reported as sample TICs.

        Examples:

        a. Common laboratory contaminants:  CC^ (m/z 44), siloxanes (m/z 73), diethyl ether, hexane,
           certain ft eons (1,1,2-trichloro-1,2,2-trifluoroethaneor fluorotrichloromethane), and phthalates
           at levels less man 100 ug/L or 4000 ug/Kg.

        b. Solvent preservatives, such  as cyclohexene which  is a methylene chloride preservative.
           Related by-products include  cyclohexanone, cyclohexenone,  cyclohexanol, cyclohexenol,
           chlorocyclohexene, and  chlorocyclohexanol.

        c. Aldol reaction products of acetone include:  4-hydroxy-4-methyl-2-pentanone, 4-methyl-2-
           penten-2-one, and 5,5-dimethyl-2(5H)-ruranone.

    7.  Occasionally, a target compound may be identified as  a TIC in the proper analytical fraction by
        non-target library search procedures, even though it was not  found on the quantitation list. If
        the total area  quantitation method was used, die reviewer should request that the laboratory
        recalculate the result using the proper quantitation ion. In addition, the reviewer should evaluate
        other sample chromatograms and check library reference retention tunes on quantitation lists to
        determine whether the false negative result is an isolated occurrence or whether additional data
        may be affected.

    8.  Target compounds may be identified in more man one fraction. Verify that quantitation is made
        from the proper fraction.
                                              72

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                                                                              Region in Modification*


Tentatively Identified Compounds                                                           SV


    9.  Library searches should not be performed on internal standards or surrogates.

    10. TIC concentration should be estimated assuming a RRF of 1.0.

E.  Action

    1.  All TIC results should be qualified "J", estimated concentration on the Laboratory
        Form I-TlCs.

    2.  General actions related to the review of TIC results are as follows:

        a. If it is determined that a tentative identification of a non-target compound is not acceptable,
           the tentative identification should be changed to "unknown" or an appropriate identification.

        b. If all contractually required peaks were not library searched and quantitated, the designated
           representative could request these data from the laboratory.

    3.  Blank Results

        Form I-TIC which contain sample results that are questioned by blank results, should be flagged
        "B" and a line drawn through these data for emphasis (initialed and dated).

        To  be considered questionable, a sample  TIC concentration must be within 10 times  the
        concentration of one of the blank results.  If different volumes/weights are used, the total
        amount of compound  in the extract must be compared for sample versus blank.  In general,
        blanks analyzed within the same case, by the same lab, may be cross-applied to either soil or
        water samples extracted or analyzed on other days.

        To question a sample result, only presumptive evidence for the presence of the compound in the
        blank is necessary.  The presence of the TIC in the blank is suggested in any  of the following
        situations:

        a. Relative retention times (RRTs) match for sample versus blank, and the sample library search
           result matches the  same compound oj compound class as the library search result for the
           blank.

        b. RRTs match, but library search results do not list the same compound or  class for sample
           versus blank. However, some of the largest ions in the sample are also in  the blank, and a
           direct comparison of sample versus blank spectra suggests mat the TIC in the sample is quite
           possibly the same compound as that in the blank.

        c. A peak at the same RRT as the sample TIC is present in the chromatogram of the blank, but
           no library search was performed  or included in the data.  (The labs do  not have to library
                                              73

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                                                                              Region ffl Modification*


Tentatively Identified Compounds                                                           SV

        search peaks less than 10% of the height of the nearest internal standard, although these peaks
        may still be important to identify low-level blank contaminants that can question sample results
        at levels above  10% of the nearest internal standard height.)

        All blank results must be attached in the support documentation section of the data review.

    4.  When a compound is not found in any blanks, but is a suspected artifact of common laboratory
        contamination, the reviewer should cross off the reported TIC result on the copy of the Form
        I-TIC and note the reason(s) hi the narrative.

    5.  In deciding whether a library search result for  a TIC represents a reasonable identification,
        professional judgment must be exercised.  If there is more than one possible match, the result
        may  be reported as  "either compound X or compound Y".  If there is a lack of isomer
        specificity, the TIC result may be changed to a non-specific isomer result (e.g., 1,3,5-trimethyl
        benzene to trimethyl benzene isomer) or to a compound class (e.g., 2-methyl, 3-ethyl benzene
        to substituted aromatic compound). These changes may be made directly on a copy of the Form
        I-TIC,  as long as changes are initialed and dated.

    6.  Other case factors may influence TIC judgments.  If a sample TIC match is poor but other
        samples have a  TIC with a good library match, similar relative retention time, and the same
        ions, identification information may be inferred from the other sample TIC results.

    7.  Physical constants, such as boiling point, may be factored into professional judgment of TIC
        results.

    8.  Any changes made to the reported data or any concerns regarding TIC identifications should be
        indicated in the data review narrative.  Any changes made regarding TIC identifications or
        qualifications are to be made on copies of the laboratory generated Form I-TIC and not the
        originals.

    9.   Failure to properly evaluate and report TICs should be noted for TPO action.
                                             74

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                                                                                            sv
                                  Xin.  System Performance
 A.  Review Items:  Form in SV-1 and SV-2, Form Vffl SV-I ami SV-2, and ehromatograms.

 B.  Objective

     During the period following Instrument Performance QC checks (e.g. blanks, tuning, calibration),
     changes may occur in the system that degrade the quality of the data.  While mis degradation would
     not be directly shown by QC checks until the next required series of analytical QC runs, a through
     review of the ongoing data acquisition can yield indicators  of instrument performance.

 C.  Criteria

     There are no specific criteria for system performance.  Professional judgement should be used to
     assess the system performance.

 D.  Evaluation

     1.  Abrupt, discrete shifts in the reconstructed ion chromatogram (RIC) baseline may indicate a
        change  in the instrument's sensitivity or the zero setting.  A baseline  shift could indicate a
        decrease in sensitivity in the instrument or an increase  in the instrument zero, possibly causing
        target compounds at or  near the detection limit to be non-delects.   A baseline "rise* could
        indicate problems such as a change in the instrument zero, a leak, or degradation of the column.

     2.  Poor  chromatographic performance affects both qualitative and quantitative results.  Indications
        of substandard performance include:

        a.  High RIC background levels or shifts m absolute retention times of internal standards.

        b.  Excessive baseline rise at elevated temperature.

        c.  Extraneous peaks.

        d.  Loss  of resolution as  suggested  by  factors such as non-resolution of 2,4- and 2,5-
            dinitrotoluene.

        e.  Peak tailing or peak splitting that may result in inaccurate quantitation,

E.  Action

    Professional judgement must be used to qualify the data if it is determined that system performance
    has degraded during sample analyses.  Any degradation of system performance which significantly
    affected the data should be documented for TPO action.
                                              75

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                                                                                Region HI Modifications


                                                                                             sv
                                XIV.  Overall Assessment of Data
A.  Review Items: Entire data package, data review results, ami (if available) Quality Assurance Project
     Plan (QAPjP), and Sampling and Analysis Plan (SAP).

B.  Objective

     Hie overall assessment of a data package is a brief narrative in which the data reviewer expresses
     concerns and comments on the quality and, if possible, the useability of the data.

C.  Criteria

     Assess the overall quality of the data.

     Review all available materials to assess the overall quality of the data, keeping in mind the additive
     nature of analytical problems.

D.  Evaluation

     1.   Evaluate any technical problems which have not been previously addressed.

    2.   Review all available  materials to  assess the overall quality of the data, keeping in mind the
         additive nature of analytical problems.

    3.   If appropriate information is available, the reviewer may assess the useability of the data to assist
         the data user in avoiding inappropriate use of the data.  Review all available information,
         including the QAPjP (specifically the Data Quality Objectives), SAP, and communication with
         data user that concerns the intended use and desired quality of the data.

E.  Action

     1.   Use professional judgement to determine if there is any need to  qualify data which were not
         qualified based on the QC criteria previously discussed.

    2.  Write a brief narrative to give the user an indication of die analytical limitations of the data.
         Any inconsistency  of mat data with the SDG Narrative should be noted for TPO  action.  If
        sufficient  information on  the intended use and required  quality of die data are available, the
        reviewer should include his/her assessment of the useability of the data within the given context.
                                               76

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                                                                         Region m Modi fic*tion»


                                                                                   PEST



                         PESHCIDE/AROCLOR DATA REVIEW



Hie pesticide/Aroclor data requirements to be checked are listed below.


     I.     Technical Holding Times (CCS-Contractual holding times only)

     H.     GC/ECD Instrument Performance Check

     m.    Initial Calibration (CSS)

     IV.    Continuing Calibration (CCS)

     V.     Blanks

     VI.    Surrogate Spikes (CCS)

     VII.   Matrix Spikes/Matrix Spike Duplicates

     Vm.   Regional Quality Assurance and Quality Control

     IX.    Pesticide Cleanup decks

     X.     Target Compound Identification

     XI.    Compound Quantitation and Reported Contract Required Quantitation Limits (CRQLs)

     XIL   Overall Assessment  of Data
Nofe:    "CCS* indicated mat the contractual requirements for these items will also be checked by CCS:
        CCS requirements are not always the same as the data review criteria.
                                           77

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                                                                              Region m Modification!

                                                                                         PEST
                                  I. Technical Holding Times
 A. Review Items; Form I PEST, EPA Sample Traffic Report, and/or chain-of-custody, raw data, SDG
    Narrative, and sample extraction sheets.

 B. Objective

    The objective is to ascertain the validity of results based on the holding time of the sample from time
    of collection to time of sample extraction and analysis.

 C. Criteria

    Technical requirements for sample holding times have only been established for water matrices.  The
    holding times for soils (and other non-aqueous matrices such as sediment, oily wastes, and sludge)
    are currently under  investigation.  When the results are available they will be incorporated into die
    date evaluation process. Additionally, results of holding time studies will be incorporated into the
    data review criteria  as die studies are conducted and approved.

    The holding time criteria for water samples, as stated in the current 40 CFR Part 136 (Clean Water
    Act) is as follows:

        For pesticides and Aroclors in cooled (@ 4°C) water samples, the technical holding time is 7 days
        from sample  collection to extraction and 40 days from sample extraction to  analysis.

    It is recommended that pesticides and Aroclors in soil samples in properly preserved non-aqueous
    samples be extracted within 7 days of sample collection and extracts analyzed within 40 days from
    sample extraction.

    The contractual holding times, which differ from the technical holding times, state that extraction of
    water  samples by separatory funnel must be completed within 5 days of validated time of sample
    receipt (VTSR),  extraction of water samples by continuous liquid-liquid extraction procedures must
    be started within 5 days of VTSR, and soil/sediment samples are to be extracted within 10 days of
    VTSR,  Also,  contractually both water and soil sample extracts must be analyzed within 40 days of
    sample extraction.  However, the contractual delivery due date is either  14 days or 35 days after
    receipt in the laboratory of the last sample in the SDG, depending on die contract.

D. Evaluation

    Technical holding times for sample extraction are established by comparing the sample collection date
    on the EPA Sample Traffic  Report with the dates of extraction on  Form I PEST and the sample
    extraction sheets.  To determine if the samples were analyzed within die holding time after extraction,
    compare the dates of extraction on the sample extraction sheets with the dates of analysis on Form
    I PEST.
                                              78

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                                                                              Region ID Modification*

Technical Holding Times                                                                 PEST
    Verify that the traffic report indicates that the samples were received intact and iced.  If the samples
    were not iced or there were any problems with the samples upon receipt, the discrepancies in the
    sample condition could affect die data,

E,  Action

    1.  If technical holding times are exceeded, qualify all detected compound results as estimated "J"
       and sample quantitation limits as estimated "UJ", and document in the data review narrative mat
       holding times were exceeded.   However,  please note that some extractable compounds are
       extremely persistent in the environment (e.g., PCBs) in non-aqueous  matrices and would not be
       expected to degrade significantly during sample storage.  The reviewer must use professional
       judgement in the application of data qualifiers to those compounds in non-aqueous matrices.

    2.  If technical holding times are grossly exceeded, either on the first analysis or upon re-analysis,
       the reviewer must use professional judgement to determine the reliability of the data and the effect
       of additional storage on the sample results. The reviewer may determine that detected compound
       results or the associated quantitation limits are approximates and should be qualified with "J" or
       "UJ", respectively.  The reviewer may determine that non-detected  target compound data are
       unusable (R).

    3.  Whenever possible, the reviewer should comment on the effect of exceeding the holding time on
       the resulting data in the data review narrative.

    4.  When contractual and/or technical holding times are exceeded, mis should be noted as an action
       item for the TPO.

    5.  The reviewer should also be aware of the scenario in which the laboratory has exceeded the
       technical holding times, but met contractual holding times.  In mis case, the data reviewer should
       notify the Regional TPO  (where samples were collected) and/or RSCC indicating mat shipment
       delays have occurred so mat the field and/or shipping problems can be corrected.  The  reviewer
       may  pass this information on to the laboratory's TPO, but should explain mat contractually the
       laboratory met the requirements.

    6.  When there are other quality control problems in conjunction with exceeded holding times (such
       as suspected laboratory contamination), the reviewer should follow the hierarchy of qualifiers.
       In particular, if for any reason the reviewer  doubts the  presence  of a compound,  die  data
       summary should display only the "B" or "R" qualifier, and not the "J" qualifier.

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                                                                            Region ID Modificitioni


                                                                                       PEST
                         II.  GC/ECP Instrument Performance Check
A.  Review Items:  Form VI PEST-4, Form VD PEST-1, Form Vm PEST, chromatograms, and data
    system printouts.

B.  Objective

    Performance checks on the gas chromatograph with electron capture detector (GC/ECD) system are
    performed to ensure adequate resolution and instrument sensitivity. These criteria are not sample
    specific. Conformance is determined using standard materials, therefore, these criteria should be met
    in all circumstances.

C.  Criteria

    1.  Resolution Check Mixture

       a. The Resolution Check Mixture must be analyzed at the beginning of every initial calibration
         sequence, on  each GC column and instrument used for analysis.  The Resolution Check
         Mixture contains the following pesticides and surrogates:

               gamma-Chlordane         Endrin ketone
               Endosulfan I              Methoxychlor
               4,4'-DDE                Tetrachloro-m-xylene
               Dieldrin                 Decachlorobiphenyl
               Endosulfan sulfate

       b. The depth of the valley between two adjacent peaks in the Resolution Check Mixture must be
         greater man or equal to 60.0 percent of the height of the shorter peak.

   2.  Performance Evaluation Mixture

       a. The Performance Evaluation Mixture (PEM) must be analyzed at the beginning (following the
         resolution check mixture) and at the end of the initial calibration sequence. The PEM must
         also be analyzed at the beginning of every other 12-hour analytical period. The PEM contains
         the following pesticides and surrogates:

               gamma-BHC              Endrin
               alpha-BHC                Methoxychlor
               4,4*-DDT                Tetrachloro-m-xylene
               beta-BHC                 Decachlorobiphenyl

       b. The  resolution of adjacent peaks for the  PEM injections in'  each calibration (initial and
         continuing) must be 100 percent for both GC columns.

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                                                                            Region QI Modifications

 GC/ECD Instrument Performance Check                                               PEST
       c. The absolute retention times of each of the single component pesticides and surrogates in all
          PEM analyses mtist be within the specific retention time windows centered around the mean
          retention times determined from the three-point initial calibrations
          using the Individual Standard Mixtures.  A list of the retention time windows is included in
          Appendix A.

          For example, for a given pesticide the mean retention time is first determined from the initial
          calibration and found to be 12.69 minutes.  The retention time window for mis pesticide is ±
          0.05 minutes.  Therefore, the calculated retention time window would range from 12.64 to
          12.74

       d. The relative percent difference (RPD) between the calculated amount and the true amount for
          each of the single component pesticides and surrogates in the PEM analyses must be less than
          or equal to 25.0 percent.

       e. The percent breakdown is the amount of decomposition that 4,4'-DDT and Endrin undergo
          when analyzed on the GC column.  For Endrin, the percent breakdown is determined by the
          presence of Endrin aldehyde and/or Endrin ketone in the GC chromatogram. For 4,4'-DDT,
          the percent breakdown is determined from the presence of 4,4'-DDD and/or 4,4'-DDE in the
          GC chromatogram.  The equations used to verify these calculations are provided in Appendix
          A.

          i. The individual percent breakdown for both 4,4'-DDT and Endrin in each PEM must be less
            than or equal to 20.0 percent for both GC columns.

          ti. The combined percent breakdown for 4,4'-DDT and Endrin hi each PEM must be less man
            or equal to 30.0 percent for both GC columns.

D.  Evaluation

    1.  Resolution Check Mixture

       a. Verify from the Form Vffl PEST that the resolution check mixture was analyzed at the
          beginning of the initial calibration  sequence on each GC column and instrument used for
          analysis.

       b. Check tfie  resolution check mixture data and Form VI PEST-4 to verify that the resolution
          criterion between two adjacent peaks for the required  compounds is less than or equal to 60%.
          The resolution criteria requires that  the depth of the valley between two adjacent peaks in the
          resolution check mixture must be greater than or equal to 60% of the height of the shorter
          peak.

    2.  Performance Evaluation Mixture

       a. Verify from the Form Vm PEST mat the Performance Evaluation  Mixture (PEM)  was
          analyzed at the proper frequency and position  sequence.

                                            81

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                               '                                              Region ID Modifications

GC/ECD Instrument Performance Check                                                PEST
       b. Check the PEM data from the initial and continuing calibrations to verify that the resolution
          between adjacent peaks is 100 percent on both GC columns.

       c. Check the PEM data from the initial and continuing calibrations and Form VII PEST-1 to
          verify that the absolute retention times for the pesticides in each analysis are
          within the calculated retention time windows based on the mean RT from the three-point initial
          calibration using equations and examples found in Appendix A.

       d. Verity that the relative percent difference (RPD) between the calculated amount and the true
          amount for each of the pesticides and surrogates is less man or equal to 25,0 percent.

       e. Verity that the individual breakdown on each GC column for 4,4'-DDT and Endrin is less than
          or equal to 20.0 percent, and  that the combined breakdown is less man or equal to 30.0
          percent.

E.  Action

    1.  Resolution Check Mixture: If resolution criteria are not met, the quantitative results may not be
       accurate due to  inadequate resolution.  Detected target compounds that were not adequately
       resolved should be qualified  with  "J".  Qualitative identifications may also be questionable if
       coelution exists.  Non-detects with retention times in die region of coelution may not be valid,
       depending on the extent of the problem.  Professional judgement should be used to determine the
       need to qualify data as unusable (R).

    2.  Performance Evaluation  Mixture Retention  Times:   Retention tune  windows  are  used in
       qualitative identification.  If the retention times of the pesticides in the PEM do not fall  within
       the retention time windows,  the associated sample results should  be  carefully evaluated.  All
       samples injected after the last in-control standard are potentially affected.

       a.  For the affected samples, check to see if the sample chromatograms contain any peaks that are
          close to die expected retention time window of the pesticide of interest.   If no peaks are
          present either within or close to the retention time  window of the deviant target  pesticide
          compound, then there is  usually no affect on the data (i.e.,  non-detected values can be
          considered valid).   Sample data mat are potentially affected by standards  not meeting the
          retention time windows should be noted in the data review narrative.

       b.  If the affected  sample chromatograms contain peaks which may be of concern (i.e., above the
          CRQL and either dose to  or within the expected retention time window of the analyte
          of interest), then the reviewer should determine the extent of the effect on the data and may
          choose to qualify detected target compound "Ml" and non-detected target compounds "R". In
          some cases, additional effort by the reviewer may be necessary to determine if sample peaks
          represent the compounds of interest, for example:
                                             82

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                                                                              Region M Modification*

GC/ECD Instrument Performance Check                                                 PEST
          i.  The reviewer can examine the data package for the presence of three or more standards
             containing the pesticide of interest that were run within a 72-hour period during which the
             sample was analyzed.

          ii.  If three or more such standards are present,  the mean and standard deviation of the
             retention time window can be re-evaluated.

          iii.   If all standards and matrix spikes fall within the revised window, the valid positive or
               negative sample results can be determined using this window.

          iv.   The narrative should  identify the additional efforts taken by the reviewer and the
               resultant impact on data usability.  In addition, the support documentation should contain
               all calculations and comparisons generated by the reviewer.

       c.  If the reviewer can not resolve the problem of concern with the available data, all positive
          results and quantitation limits should be qualified "R".

   3.  If PEM resolution criteria are not met, quantitative results for compounds in the region where the
       criteria is not met may not be accurate due to inadequate resolution. Positive sample results for
       compounds that were not adequately resolved should be qualified "J".  If in the professional
       judgement of the reviewer, qualitative identifications are questionable due to poor resolution,
       positive sample results should be qualified "NJ". Non-detected target compounds that would elute
       in the region of coelution may not be valid depending on the extent of the coelution problem.
       Professional judgement should be used to qualify detection limits unusable  "R".

   4.  If RPD criteria are not met, qualify all associated positive results generated during the analytical
       sequence with "J" and  the sample  quantitation limits for non-detected target compounds with
       "UJ".

   5.  4,4'-DDT/Endrin Breakdown:

       a. If 4,4'-DDT breakdown is greater than 20.0 percent:

         i. Qualify all positive results for DDT with "L" (biased low). If DDT was not detected, but
            DDD and DDE are detected,  then qualify the quantitation limit for DDT as unusable (R).

         ii. Qualify positive results for DDD and/or DDE as presumptively present at an approximated
            quantity (NJ).

       b. If Endrin breakdown is greater than 20.0 percent:

         i. Qualify all positive results for Endrin with "L" biased low. If Endrin was not detected, but
            Endrin  aldehyde and Endrin  ketone  are detected, then qualify the quantitation limit for
            Endrin as unusable (R).
                                             83

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                                                                            Region ID Modific*tioos

GC/ECD Instrument Performance Check                                                PEST
          ii. Qualify positive results for Endrin ketone and Endrin aldehyde as presumptively present
            at an approximated quantity (NJ).

       c.  If the combined 4,4*-DDT ami Endrin breakdown is greater man 30.0 percent:

          i. Qualify ill positive results for DDT and Endrin, "J* estimated. If Endrin was not detected,
            but Endrin aldehyde and Endrin ketone are detected, then qualify the quantitation limit for
            Endrin as unusable (R).  If DDT was not detected, but DDD and DDE are detected, then
            qualify the quantitation limit for DDT as unusable (R).
          ii. Qualify positive results for Endrin ketone and Endrin aldehyde as presumptively present
            at an approximated quantity (HI).  Quality  positive results for DDD and/or DDE as
            presumptively present at an approximated quantity (NJ),

   6.  Potential effects on the sample data resulting from the initial calibration problems should be noted
       in the data review narrative.
                                            84

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                                                                              Region ID Modification*

                                                                                         PEST
                                    III.  Initial Calibration
A.  Review Items:  Form VI PEST-1,2,3, and 4, Form VH PEST-I, Form VHI PEST, chromatograms,
    and data system printouts.

B.  Objective

    Compliance  requirements for  satisfactory initial  calibration  are  established  to ensure that  the
    instrument is capable of producing  acceptable qualitative and quantitative data for pesticide and
    Aroclor target compounds.   Initial  calibration demonstrates that the instrument  is capable of
    acceptable performance at the beginning of the analytical sequence  and  of producing a linear
    calibration curve.

C.  Criteria

    1.  Individual Standard  Mixtures

       a.  Individual Standard Mixtures A and B (containing all of the single component pesticides and
          surrogates)  must  be analyzed at low, midpoint, and high levels during the initial calibration,
          on each GC column and instrument used for analysis.

       b.  The resolution between any two adjacent peaks in the midpoint concentration of Individual
          Standard  Mixtures A and B in the initial calibration must be greater than or equal to 90.0
          percent on both columns.

       c.  The absolute retention times of each of the single component pesticides and surrogates are
          determined  from  three-point initial calibration using the Individual Standard Mixtures.  A list
          of the retention time windows and an example for calculating retention tune windows is given
          in section m in Appendix A.   •     ~      -

       d.  At least one chromatogram from each of the Individual Standard Mixtures A and B must yield
          peaks  that give recorder deflections between SO to 100 percent of full scale.

       e.  The concentrations of the low, medium, and high level standards containing all of the single
          component pesticides and surrogates (Individual Standard Mixtures A and B) must meet the
          following criteria on bom GC  columns.

          The low point corresponds to the CRQL for each analyte.  The midpoint concentration must
          be 4 times the low point. The high point must be at least 16 times the low point, but a higher
          concentration may be chosen.

       f.  The Percent Relative Standard Deviation (%RSD)  of the calibration  factors for each  of the
          single component pesticides and  surrogates in the initial calibration on both columns for
          Individual Standard Mixtures A and B must be less than or equal to 20.0 percent, except as
          noted below.  For the two surrogates, the %RSD must be less than or equal to 30.0 percent.
                                             85

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                                                                              Region m Modifications

 Initial Calibration                                                                       PEST
          Up to two single component target pesticides (other than the surrogates) per column may
          exceed die 20.0 percent limit but the %RSD must be less than or equal to 30.0 percent,

      Note:  Either peak area or peak height may be used to calculate die calibration factors that are,
             in turn, used to  calculate  %RSD.  However,  the type of peak  measurement used  to
             calculate each calibration factor for a given compound must be consistent.  For example,
             if peak area is used to calculate the low point calibration factor for endrin, men the mid and
             high point calibration factors for endrin must also be calculated using peak area.

    2. Multi-component Target Compounds

       a. The multi-component target compounds (the 7 Aroclors and Toxaphene) must each be analyzed
          separately at a single concentration level during the initial calibration sequence. The analysis
          of the multi-component target compounds must also contain the pesticide surrogates.

       b. For each multi-component analyte, the retention times are determined for three to five peaks.
          A retention time window of ±  0.07 minutes is used to determine retention time windows for
          all multi-component analyte peaks.

       c. Calibration factor data must be determined for each peak selected from the multi-component
          analytes.

D.     Evaluation

    1.  Individual Standard Mixtures

       a. Verify from the Form VTD PEST mat the Individual Standard Mixtures A and B  were analyzed
          at the proper frequency on each GC column and instrument used for analysis.  Check the raw
          data (chromatograms and data system print outs) for each standard to verify that each of the
          standards was analyzed at the required concentration levels.

       b. Check the raw data and determine that  the midpoint standard's  concentration  is 4 times the
          concentration of the tow point standard's concentration and verify mat resolution is greater
          than 90%.

       c. Check the Individual Standard  Mixtures A  and B data and Form VI PEST-1 and review the
          calculated retention time windows for calculation and transcription errors.

       d. Check the Individual Standard Mixtures  A and B data and Form VI PEST-2 to  verify mat the
          %RSD for the calibration factors in each of the single component pesticides and surrogates in
          the initial calibration analyses on both columns are in compliance with the criteria in Section
          m.C. Check and recalculate the calibration factors and %RSD for  one or more pesticides;
          verify mat the recalculated values agree with the reported values. If errors are detected,  more
          comprehensive recalculation should be performed.
                                              86

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                                                                               Region m Modifciliom

Initial Calibration                                                                        PEST


    2.  Multi-component Target Compounds

       a. Verify from the Form VIII PEST that each of the multi-component target compounds were
          analyzed at the required frequency. Check the raw data for the standards to verify that the
          multi-component analytes were analyzed at the required concentration.

       b. Check the data for the multi-component target compounds and Form PEST VI-3 to verify that
          at least three peaks were used for calibration and that retention time and calibration factor data
          are available for each peak.

E.  Action

    1.  If the initial calibration sequence was not followed as required, then professional judgement must
       be used to evaluate the effect of the non-compliance on the sample data. If the requirements for
       the initial calibration sequence \vere_ not met, then mis should be noted for TPO action on the
       ORDAS.   If the non-compliance has a potential effect on the data,  then the data should  be
       qualified according to the professional judgement of the reviewer and this should be noted in the
       data review narrative.

    2.  If resolution criteria are not met, then the quantitative results may not be  accurate due to peak
       overlap and lack of adequate resolution.  Positive sample results for compounds that were not
       adequately resolved should be qualified with "J". Qualitative identifications may be questionable
       if coelution exists. Non-detected target compounds that elute in the region of coelution may not
       be valid depending on the extent of the coelution problem.  Professional judgement should  be
       used to qualify data as unusable (R).

    3.  If the  %RSD linearity  criteria are not met for the compound(s) being quantified, qualify all
       associated positive quantitative results with "I".   When the %RSD is grossly exceeded (i.e.,
       > 50%), use professional judgement for qualifying non-detects as "UJ".

    4.  Potential effects on the sample data due to problems with calibration should be noted in the data
       review narrative.  If the data reviewer has knowledge that the laboratory has repeatedly failed to
       comply with the requirements for frequency, linearity,  retention time, or resolution, mis
       information should be documented in the report narrative.
                                              87

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                                                                              Region ID Modification

                                                                                         PEST
                                  IV.  Continuing Calibration
 A. Review Items:  Form VH  PEST-I and 2,  Form Vffl PEST, chTOmatograms, and data system
    printouts.

 B. Objective

    Compliance requirements for satisfactory instrument calibration are established to ensure that the
    instrument is capable of producing acceptable qualitative and quantitative data. Continuing calibration
    checks and documents satisfactory performance of the instrument over specific time periods during
    sample  analysis.   To verify  the  calibration and evaluate  instrument performance, continuing
    calibration is performed, consisting of the analyses of instrument blanks, the PEM, and the midpoint
    concentration of Individual Standard Mixtures A and B.

 C. Criteria

    1. An instrument  blank and the PEM must bracket one end of a 12-hour period  during which
       samples are analyzed, and a second instrument blank and the midpoint concentration of Individual
       Standard Mixtures A and B must bracket the other end of the 12-hour period.

    2. The resolution  between any  two  adjacent peaks in the midpoint concentration of Individual
       Standard Mixtures A and B must be greater than or equal to 90.0 percent.

    3. The absolute retention time for each single component pesticide and surrogate in the midpoint
       concentration of Individual Standard Mixtures A and B must be within the retention time windows
       determined from the initial calibration.

    4. The RPD between the calculated  amount and the true amount for each of the pesticides and
       surrogates in the midpoint concentration of the Individual Standard Mixtures A and B must not
       exceed 25.0 percent.

D.  Evaluation

    1. Check the Form VHI PEST to verify that die instrument blanks, PEMs, and Individual Standard
       Mixtures were analyzed at the proper frequency and that no more than 12 hours elapsed between
       continuing calibration brackets in an ongoing analytical sequence.

    2. Check the data for the midpoint concentration of Individual Standard Mixtures A and B to verify
       that the resolution between any two adjacent peaks is greater than or equal  to 90.0 percent.

    3. Check the  data for each of the single component pesticides and surrogates in the  midpoint
       concentration of Individual Standard Mixtures A and  B and Form VH PEST-2 to verify that the
       absolute retention times are within the appropriate retention time windows.

    4. Check that the data from the midpoint concentration of Individual Standard Mixtures A and B and
       Form VII PEST-2 between the calculated amount and the true amount for each of the pesticides
       and surrogates is less than or equal to 25.0%.

                                              88

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                                                                              Region M ModiCcilioai

Continuing Calibration                                                                   PEST


E.  Action

    1.  If die continuing calibration sequence was not followed as required, then professional judgement
       must be used to evaluate the effect of the non-compliance on the sample data.  If the requirements
       for the continuing calibration sequence were not met, men this should be noted in the report
       narrative.  If the non-compliance has a potential effect on the data, then the data should be
       qualified according to the professional judgement of the reviewer and mis should be noted in the
       data review narrative.

    2,  If resolution criteria are not met then the quantitative results may not be  accurate due to
       inadequate resolution. Positive sample results for compounds that were not adequately resolved
       should be qualified with T. Qualitative identifications may be questionable if coelution exists.
       Non-detected target compounds mat elute in the region of coelution may not be valid depending
       on the extent of the coelution problem.  Professional judgement should  be used to qualify data
       as unusable (R).
    %
    3.  Retention time windows are used in qualitative identification.  If the standards do not fall within
       the retention time windows, the associated sample results should be carefully evaluated.  All
       samples injected after the last in-control standard are potentially affected.

       a.  For the affected samples, check to see if the sample chromatograms contain any peaks that are
          close to the expected retention time window of the pesticide of interest.  If no peaks are
          present either within or close  to the retention time window of the deviant target pesticide
          compound, then non-detected values can be considered valid.  Sample data that is potentially
          affected by the standards not meeting the retention time windows should be noted in the data
          review narrative.
       b.  If the affected sample chromatograms contain peaks which may be of concern (i.e., above the
          CRQL and either  dose to or within the expected retention time window  of the pesticide of
          interest), then the reviewer should follow the guidelines provided in  Section Q.E.2 to
          determine the extent of the effect on the data.

   4,  If the RPD is  greater man 25% for the  compound(s) being quantified, qualify all associated
       positive quantitative results with "J" and the sample quantitation limits for non-detects with "UJ"
       when the RPD is grossly exceeded (i.e., >50%).

   5.  Potential effects on the sample data due to problems with calibration should be noted in the data
       review narrative. If the data reviewer has knowledge mat the laboratory has repeatedly failed to
       comply with the requirements for frequency, linearity, retention time, resolution, or DDT/Endrin
       breakdown, the data reviewer should note this in the report narrative.
                                              89

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                                                                              Region ID Modifications

                                                                                         PEST
                                           V. Blanks
 A. Review Items: Form I PEST, Form IV PEST, chromatograms, and data system printouts.

 B. Objective

    The purpose of laboratory (or field) blank analyses is to determine the existence and magnitude of
    contamination problems resulting from laboratory (or field) activities. The criteria for evaluation of
    laboratory blanks apply to any blank associated with the samples (e.g., method blanks, instrument
    blanks, field generated blanks, and sulfur cleanup blanks).  If problems with any blank exist, all
    associated data must be carefully evaluated to determine whether or not mere is an inherent variability
    in the data, or if the problem is an isolated occurrence not affecting other data.

 C. Criteria

    1.  No contaminants should be present in the blanks.

    2.  Frequency:

        a. Method Blanks - A method blank analysis must be performed for each 20 samples of similar
          matrix in each sample delivery group (SDG) or whenever a sample extraction procedure is
          performed.

       b. Instrument Blanks - An acceptable instrument blank must be run at least once every 12 hours
          and immediately prior to  the analysis of either the performance evaluation mixture or
          Individual Standard Mixtures, A  and B, depending on the place in the analysis sequence.

       c. Sulfur Cleanup Blanks - A  sulfur cleanup blank must be analyzed whenever part of a set of
          samples extracted together requires sulfur cleanup.  If the entire set of samples associated with
          a method blank requires sulfur cleanup, men the method blank also serves the purpose of a
          sulfur blank and  no separate sulfur blank is required.

       d. Field Generated Blanks - Equipment rinsate blanks and/or field blanks may be collected and
          analyzed with each set of samples collected. The QAPjP will specify the type and frequency
          for the collection of these blanks.

D.  Evaluation

    1.  Review the results of all associated blanks.. Form I PEST and  Form IV PEST, and raw data
       (chromatograms and data system printouts) to evaluate the presence of target pesticides/PCBs.

    2.  Verify mat method blank analysis has been reported per SDG, per matrix, per concentration level,
       for each GC system used to analyze samples, and for each extraction batch.

    3.  Verify that the method blank analyses do not contain any target pesticide or Aroclor/Toxaphene
       at greater man its Contract Required Quantitation Limits (CRQL).

                                              90

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                                                                               Region ID ModiGc*tions

Blanks                                                                                   PEST

    4. For the surrogates in each method blank, verify that the observed retention times are within the
       appropriate retention time windows calculated from the initial calibration.

    5, Verify that the instrument blank analysis has been performed  every 12 hours as part of the
       continuing calibration and following a sample analysis which contains an analyte(s) at high
       concentration(s), and that the instrument blanks do not contain any target analytes above one-half
       the CRQL, assuming that die material in the instrument resulted from the extraction of a 1-L
       water sample.

    6. Verify that the sulfur cleanup blanks were analyzed at the required frequency and that they do not
       contain any target compound  above  the  CRQL, assuming that the material in  the instrument
       resulted from the extraction of a 1-L water sample.   If a separate sulfur  cleanup blank  was
       prepared, one version of Form IV PEST should be completed associating all the samples with the
       method blank, and a second version  of Form IV PEST should be completed listing only those
       samples associated with the separate sulfur cleanup blank.

E.  Action

    If the appropriate blanks were not analyzed with die frequency described in Section V.C.2, then the
    data reviewer should use professional judgement to determine if the associated sample data should
    be qualified. The reviewer may need to  obtain additional  information from the laboratory.

    Action in the case of unsuitable blank results depends on the circumstances and the origin of the
    blank.  Detected  compound results should be reported and qualified "B" if the concentration of the
    compound in the sample is less than or equal to 5 times (Sx) die amount in the blank.  In instances
    where more man one blank is associated  with a given sample,  qualification should be based upon a
    comparison with the associated blank having  the highest concentration  of a  contaminant.   For
    qualification purposes, to determine the highest concentration of a contaminant,  consider all blanks
    in a case associated  with all samples, except for instrument blanks, which only affect the samples
    bracketed by the contaminated instrument blank.  The results must not be corrected by subtracting
    the blank value.

    Specific actions are as follows:

    1.  If a target pesticide or Aroclor/Toxaphene is found in  die blank but not found in the samples),
       no qualification is required.  If the contaminants) is found at level(s) significantly greater than
       the CRQL, then this should be noted  in the  report narrative.

    2.  Any pesticide or Aroclor/Toxaphene detected in the  sample, that was  also detected  in  any
       associated blank, is qualified "B" if the sample concentration is less than five times (5x) the blank
       concentration.

       The reviewer should note mat analyte concentrations calculated for  method blanks may not
       involve the same weights, volumes or dilution factors as the associated samples.  These factors
       must be taken into consideration when applying the "Sx" criteria, such that a comparison of the
       total amount of contamination is actually made.
                                              91

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                                                                               Region m Modification!

Blanks                                                                                   PEST

       Additionally, there may be instances when little or no contamination was present in die associated
       blanks, but qualification of die sample was deemed necessary. Contamination introduced through
       dilution is one example.  Although it is not always possible to determine, instances of mis
       occurring can be detected when contaminants are found in the diluted sample result, but absent
       in the undiluted sample result.  Since both results are not routinely reported, it may be impossible
       to verify this source of contamination.   However,  if  the  reviewer determines  mat die
       contamination is from a source other man die sample, he/she should qualify die data.  In this
       case, die "Sx" rule does not apply, die sample value should be reported and qualified "B" and a
       note should be added to die  narrative.

    3.  If gross contamination exists (i.e.,  saturated peaks), all affected  compounds in the associated
       samples should be qualified as unusable (R), due to interference. This should be noted in die data
       review narrative if die contamination is suspected of having an effect  on me sample results.

    4.  If inordinate amounts of other target pesticides or Aroclors/Toxaphene are found at low levels  in
       die blank(s), it may be indicative of a problem at the laboratory and should be noted in the data
       revie6w narrative.

    5.  If an instrument blank was not analyzed following a sample analysis which contained an analyte(s)
       at high concentration^),  sample analysis results after  the high concentration sample  must be
       evaluated for carryover. Professional judgement should be used to determine if instrument cross-
       contamination has affected any positive compound identification(s), and if so, detected compound
       results should be qualified.  If instrument cross-contamination is suggested, dien diis should be
       noted in die data review narrative if die cross-contamination is suspected of having an effect on
       die sample results.

    The following are examples of applying die blank qualification guidelines.  Certain circumstances
    may warrant deviations from these guidelines.

       Example I:   Sample result is greater than die CRQL, but is less dian die 5x multiple of me
                    blank result.
                                                           Sx
                         Blank Result                       1.0
                         CRQL                            0.5
                         Sample Result                     4.0
                         Qualified Sample Result            4.0B

                    In diis case, sample results less man 5.0 (or 5 x 1.0) would be qualified as a blank
                    contaminant, "B".

       Example 2:   Sample result is less man die CRQL, and is also less man me 5x multiple of me
                    blank result.
                                                           22.
                         Blank Result                       1.0
                         CRQL                            0.5
                         Sample Result                     0.4J
                         Qualified Sample Result            0.4B

                                              92

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Blanks
                    Region HI Modification*

                               PEST
       Example 3:    Sample result is greater than the 5x multiple of the blank result,
                         Blank Result
                         CRQL
                         Sample Result
                         Final Sample Result
1.0
0.5
10.0
10.0
               In this case, die sample result exceeded the adjusted blank result (5 x 11) and the sample
               result is not qualified.
   6,  In pesticide analyses by GC/EC, contractually compliant laboratory blanks can sometimes contain
       interferences  which  obscure detection of target pesticide compounds (since the interfering
       compound may not actually be a pesticide).  If sample quantitation limits are flagged as biased
       low  (UL)  or  unreliable  (R)  due to  interferences  attributable to such  laboratory  blank
       contamination, men mis issue should be addressed in the narrative.

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                                                                              Region m Modifications

                                     VI.  Surrogate Spikes                               PEST


 A. Review Items: Form 0 PEST, Form VE PEST, chromatograms, and data system printouts.

 B. Objective

    Laboratory performance on individual samples is established by means of spiking samples prior to
    extraction and  analysis to determine surrogate spike recoveries.  All samples are spiked with
    surrogate compounds prior to sample extraction to measure extraction efficiency. The evaluation of
    the recovery results of these surrogate spikes is not necessarily straightforward. The sample itself
    may produce effects due to such factors as interferences and high concentrations of target and/or non-
    target analytes.  Since the effects of the sample matrix are frequently outside the control of the
    laboratory and may present relatively unique problems, the evaluation and review of data based on
    specific sample results is frequently subjective and demands analytical experience and professional
    judgment.  Accordingly, this section consists primarily of guidelines, in some cases with several
    optional approaches suggested.
                                                                *

 C. Criteria

    1.  Two surrogate spikes, tetrachloro-m-xylene and decachlorobiphenyl, are added to all samples,
       Individual Standard Matures, PEMs, blanks, and matrix spikes to measure their recovery  in
       sample and blank matrices.

   2.  The advisory  limits  for  recovery of  the  surrogates  tetrachloro-m-xylene (TCX)  and
       decachlorobiphenyl (DCB) are 60-150 percent for both water and soil samples.

   3.  The retention times of both of the surrogates in the PEM, Individual Standard Mixtures, and
       samples must be within the calculated retention time windows.  TCX must be within ± 0.05
       minutes, and DCB must be within ± 0.10 minutes of the mean retention time determined from
       the initial calibration.

D. Evaluation

   1.  Check raw data (e.g., chromatograms and data system printouts) to verify that the recoveries on
       the Surrogate Recovery Form II PEST are accurate and within die advisory limits and mat die
       retention times on the Pesticide Analytical Sequence Form vm PEST are accurate and within the
       retention time limits.

   2.  Check that the surrogate spike recoveries were calculated correctly and free from transcription
       errors.

   3.  If surrogate spike recoveries are not within limits, check the raw data for possible interferences
       which may have affected surrogate recoveries.

   4.  If retention time limits were not met, check the raw data for possible misidentificauon of GC
       peaks.  Non-recovery of surrogates may be due to shite in  RT.
                                              94

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Surrogate Spikes
Region CO Modi6c*lioai

           PEST
   5.  If low surrogate recoveries  are  observed, the reviewer  should  investigate  whether the low
       recoveries were a result of sample dilution.

   6.  In the special case of a blank analysis with surrogates out of specification, the reviewer must give
       special consideration to the validity of associated sample data. Hie basic concern is whether the
       blank problems represent an isolated problem with the  blank alone, or whether there is a
       fundamental problem with the analytical process.  For example, if one or more samples in die
       batch show acceptable surrogate recoveries,  the  reviewer may choose to  consider the blank
       problem to be an isolated occurrence.

E. Action

   1.  If surrogate spike recoveries are outside of advisory limits (60-150%), the  following guidance is
       suggested. Professional judgement must be used in applying these criteria.

   TABLE X - Guidance for qualifying data based on surrogate recoveries outside the advisory limits
               (60-150%)  but greater  than 10%.   In  instances where detection  limits require
               qualification, the qualifier begins with a U and is  listed hi the  column titled "Value
               reported from the column with non-conformance".
#of
outliers
1 out
2 out
3 out
4 out
Recovery
High
Low
2 high same column
2 low same column
Mixed same column -
2 high different column
2 low different column
Mixed different column
All high
All low
2 high 1 low
2 low 1 high
Other mix of
high and low
All high
All low
Mixed
Value reported from
the column with
non-conformance
No action
No action
K
L, UL
J,UJ
J
J,UJ
Prof, judgement
K
L, UL
K (2 high)
L, UJ (2 low)
J, UJ
K
L, UL
J,UJ
Value reported from
the column without
non-conformance
No action
No action
No action
No action
No action
Not applicable
Not applicable
Not applicable
Not applicable
Not applicable
J (1 low 2nd column)
J (1 high 2nd column)
Not applicable
Not applicable
Not applicable
Not applicable
                                              95

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                                                                               Regioa ID Modificitiotu

Surrogate Spikes                                                                         PEST
       a. If either pesticide surrogate recovery is reported >0% but  <10%,  the reviewer should
          examine the sample chromatogram to assess the qualitative validity of the analysis.  If low
          surrogate  recoveries are found to be due to sample dilution, then professional judgement
          should be used to determine if the resulting data should be qualified.  If sample dilution is not
          a factor, then detected target compounds  may  be qualified "L", and non-detected target
          compound results should be qualified unusable (R).

       b. If zero  pesticide surrogate recovery is reported, the reviewer should  examine the sample
          chromatogram to determine if the surrogate may  be present, but slightly outside its retention
          time window.  If this is the case, in addition to assessing surrogate recovery for quantitative
          bias, the overriding consideration is to investigate the qualitative validity of the analysis.  If
          the surrogate is not present, qualify all non detected target compounds as unusable (R).

   2.  If surrogate retention times in PEMs,  individual standards, and samples are outside of the
       retention time limits, qualification of the data is left up to the professional judgement of the
       reviewer.  Refer to section n E.2 for more guidance.

   3.  Potential effects of the data resulting from surrogate recoveries not meeting the advisory limits
       should be noted in the data review narrative.

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                                                                            Region m Modificalioai

                                                                                       PEST
                          VII.  Matrix Spikes/Matrix Snike Duplicates
A. Review Items: Form in PEST-i and PEST-2, chromatograms, and data system printouts.

B. Objective

    Data for Matrix spikes (MS) and Matrix spike duplicates (MSD) are generated to determine long-term
    precision and accuracy of the analytical method on various matrices. These data alone cannot be used
    to evaluate the precision and accuracy of individual samples.  However, when exercising professional
    judgement, MS/MSD data should be used in conjunction with other available QC information.

C. Criteria

    1.  Matrix spikes (MS) and matrix spike duplicate (MSD) samples are analyzed at a frequency of at
       least one MS and MSD per 20 samples of each matrix.

    2.  Matrix spike recoveries should be within die advisory limits provided on Form III PEST-1 and
       PEST-2 and in Appendix A.

    3.  Relative percent difference (RPD) between MS and MSD recoveries must be within the advisory
       limits provided on Form HI PEST-1 and PEST-2 and in Appendix A.

D. Evaluation

    1.  Verify  that MS and MSD samples were analyzed at the required frequency and that results are
       provided for each sample matrix.

    2.  Inspect results for the MS/MSD  Recovery on Form M PEST-1 and PEST-2 and verify  that die
       results  for recovery and RPD are within the advisory limits-.

    3.   Verify  transcriptions from raw data and verify calculations.

    4.   Check that the matrix spike recoveries and RPD were calculated correctly.

    5.   Compare %RSD results of non-spiked compounds between the original result, MS, and  MSD.

E.  Action

    1.   No action is taken on MS/MSD data alone. However, using informed professional judgement the
       data reviewer may use the MS  and MSD  results in conjunction with other  QC criteria and
       determine the need for some qualification of the data.

   2.   The data reviewer should first try to determine to what extent  die results of die MS/MSD affect
       die associated sample data. The determination should  be made with  regard to die MS/MSD
       sample itself, as well as specific  analytes for all samples associated with the MS/MSD.
                                             97

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                                                                            Region HI Modification!

Matrix Spikes/Matrix Spike Duplicates                                                  PEST
   3.  In some instances where it can be determined that the results of the MS/MSD affect only the
       sample spiked, then qualification should be limited to this sample alone.  However, it may be
       determined through the MS/MSD results that a laboratory is having a systematic problem in the
       analysis of one or more analytes, which affects all associated samples.  For example, if die
       recoveries for MS and MSD are consistently low for bom water and soil samples, mis could be
       indicative of a systematic problem in the laboratory and recoveries should be examined in all
       associated samples.

   4.  The reviewer must use professional judgement to determine the need for qualification of positive
       results of non-spiked compounds.

   5.  When extremely  low  %  recoveries  are noted,  qualify data for all affected compounds using
       professional judgement.

   6.  When non-spiked compounds are present in either the MS or MSD results, a table in the data
       review  narrative  is constructed showing original (unspiked) sample results for  non-spiked
       compounds, non-spiked compounds present in the MS and MSD and the calculated % RSD.
                                            98

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                                                                              Region ffl Modificuiam

                     Vin.  Regional Quality Assurance and Quality Control               PEST
 A. Review Items:  Form I PEST, chromatograms, Data system printouts, traffic reports and raw data
    for Regional QC samples.

 B. Objective

    Regional Quality Assurance and Quality Control (QA/QC) refers to any QA and/or QC initiated by
    the Region, including field duplicates, Regional Performance Evaluation (PE) samples, blind spikes,
    and blind blanks. It is highly recommended that Regions adopt the use of these,

 C. Criteria

    Criteria are dependent on the type of QC sample.  Frequency may vary.

    1.  The analytes present in the PE sample must be correctly identified and quantified.

D. Evaluation

    1.  Evaluation of Performance Evaluation (PE) Samples are not to be presented as part of the data
       review.  All forms associated with the Performance Evaluation Samples are to be sent (with a
       cover memo stating the case number and laboratory information) directly to the Quality Assurance
       Branch in Region HI:

                     U.S. Environmental Protection Agency
                     Region HI, Central Regional Laboratory
                     Quality Assurance Branch
                     201 Defense Highway, Suite 200
                     Annapolis, MD 21401

                     Attn: Program Support Section—
E,  Action

    1.  Field duplicate results are to be presented in a table form in the data review narrative.  If target
       compounds were not present in either of the field duplicate samples, then a table is not required.
       The percent difference is  to be calculated  and presented in the table.   (If  one of the  field
       duplicates was also used as a matrix spike/matrix spike duplicate sample, men the table should
       include any non-spiked compounds detected, along with the % relative standard deviation.)

   2.  No action is taken based on percent difference of field duplicate sample data alone. However,
       using  informed professional judgement, the data reviewer may use the field duplicate results in
       conjunction with other QC criteria and determine the need  for some qualification of the data.

   3.  Other types of Regional QC Samples

       Professional judgement is needed for evaluating other types of QC samples that may be associated
       with a particular case of samples. This information may be used in conjunction with other QC
       criteria to determine the need for qualification of data.

                                             99

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                                                                              Region m Modification*

                                                                                         PEST
                              IX. Pesticide Cleanup Checks
A. Review Items: Form DC PEST-1 and 2, chromatograms, and data system printouts.

B. Objective

   Pesticide cleanup procedures are utilized to remove matrix  interferences from sample extracts prior
   to analysis.   The use  of  the  Florisil cartridge  cleanup  procedure significantly reduces matrix
   interferences caused by polar compounds. Gel permeation ehroraatography (GPC) is used to remove
   high molecular weight contaminants mat can interfere with the analysis of target analytes.  Pesticide
   cleanup procedures are checked by spiking the cleanup columns and cartridges and verifying the
   recovery of pesticides through the cleanup procedure.

C. Criteria

   1.  Florisil Cartridge Cleanup

       a.  Florisil cartridges must be used for the cleanup of all sample extracts.

       b.  Every lot number of Florisil cartridges used for sample cleanup must be checked by spiking
          with 2,4,5-trichlorophenol and the midpoint concentration of Individual Standard Mixture A.
          These compounds are listed in Appendix A.

       c.  The lot of Florisil cartridges is acceptable if the recoveries for all of the pesticides  and
          surrogates in Individual Standard Mixture A are within 80 and 120 percent, if the recovery
          of 2,4,5-trichlorophenol  is less than 5. percent, and if no peaks interfering with the  target
          analytes are detected.

   2.  Gel Permeation Chromatography (GPC)

       a.  GPC is used for the cleanup of all SOU sample extracts and for water  sample extracts mat
          contain high molecular  weight components that interfere  with  the analysis  of  the  target
          analytes.

       b.  At least once every 7 days, die calibration of the GPC unit must be checked by spiking with
          two check mixtures: the matrix spiking solution and a mixture of 0.2 ug/mL Aroclors 1016
          and  1260.  The matrix spiking solution compounds for the GPC Check are:

               Pesticide                    Ug/mL
               gamma-BHC(Lindane)        0.5
               4,4'-DDT                    1.0
               Endrin                       1.0
               Heptachlor                   0.5
               Aldrin                       0.5
               Dieldrb                      1.0
                                             100

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                                                                               Region m Modification*

Pesticide Cleanup Checks                                                                 PEST
        c. The GPC calibration is  acceptable if the recovery of the pesticides in the matrix spiking
          solution are within 80 to 110 percent, and the Aroclor patterns should match those generated
          for previously run standards.

        d. A GPC blank must be analyzed after each GPC calibration and is acceptable if the blank does
          not exceed one-half the CRQL for any target analytes.

D.     Evaluation

    1.   Florisil Cartridge Check

        Check the data from the Florisil cartridge solution  analyses and  the Form DC-PEST-1  and
        recalculate some of the percent recoveries to verify mat the percent recoveries of the pesticides
        and  surrogates in Individual Standard Mixture A are within 80-120%, the recovery of 2,4,5-
        trichloropheno! is less than 5%, and no interfering peaks are present. Compare the raw data to
        the reported results and verify that no calculation or transcription errors have occurred.

   2.   Gel  Permeation Chromatography (GPC)

        Check the data from the GPC calibration check analyses and the Form DC PEST-2 and recalculate
        some of the percent recoveries to verify that the percent recoveries of the pesticides in the matrix
        spike solution are within 80-110% and that the Aroclor patterns are similar to  those of previous
       standards.  Check to make sure that no transcription errors have occurred.

£, Action

   1.  If Florisil Cartridge Check criteria are not met,  the raw data should be examined for the presence
       of polar  interferences and professional judgement  should be used in qualifying the data.  If a
       laboratory chooses to analyze samples under an unacceptable Florisil Cartridge Check, then this
       should be noted in the data review narrative.

   2.  If Gel Permeation Criteria are not met, the raw data should be examined for the presence of high
       molecular weight contaminants and professional judgement should be used in qualifying the data.
       If a laboratory chooses to analyze samples under an unacceptable Gel Permeation Criteria, then
       8th is should be noted in the data review narrative.

   3.  If zero recovery was obtained for the pesticide compounds and surrogates during either check,
       then the non-detected target  compounds may be suspect and the data may be qualified unusable
       (R).

   4.  If high recoveries (i.e., greater than 120%) were obtained for the pesticides and surrogates during
       either check, use professional judgement to qualify detected target compounds as biased high (K).
       Non-detected target compounds do not require  qualification.

   5,  Potential effects on the sample data resulting from the pesticide cleanup analyses not yielding
       acceptable results should be noted in the data review narrative.

                                             101

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                                                                            Region ID Modific*tkmi

                                                                                       PEST
                             X. Target Compound Identification
 A. Review Items:  Form I PEST, Form X PEST-1  and PEST-2, chromatograms, and data system
    printouts,

 B. Objective

    Qualitative criteria for compound identification have been established to minimize the number of false
    positives (reporting a compound present when it is not) and false negatives (not reporting a compound
    mat is present).

 C. Criteria

    1.  The retention times of both of the surrogates, matrix spikes, and reported compounds in each
       sample must be within the calculated retention time windows on bom columns.  TCX must be
       within ± 0.05 minutes of the mean  retention time determined from the initial calibration and
       DCS must  be within ± 0.10 minutes of the mean retention time determined from the initial
       calibration.

    2.  GC/MS confirmation is required if the concentration of a compound exceeds 10 ng/uL in the final
       sample extract.  Pesticides mat are confirmed by GC/MS should be identified with a *C" in the
       Q column on Form I PEST.

    3.  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,

    4.  Chromatograms must display single component pesticides detected in the sample and the largest
       peak of any multicomponent analyte detected in the sample at less than full scale.

   5.  If an extract must be diluted, chromatograms must display single component pesticides between
       10 and 100 percent of full scale, and multicomponent analytes between 25 and 100 percent of full
       scale.

   6.  For any sample, the baseline of the chromatogram must return to below 50 percent of full scale
       before the elution time of alpha-BHC, and also return to below 25 percent of full scale after the
       elution time of alpha-BHC and before the elution time of decachlorobiphenyl.

   7.  If a chromatogram is replotted electronically to meet these requirements, the scaling factor used
       must be displayed on die chromatogram, and both the initial chromatogram and the replotted
       chromatogram must be submitted in the data package.

D. Evaluation

    1.  Review Form I PEST, the associated raw data  (chromatograms and data system printouts) and
       Form X PEST-1 and PEST-2.  Confirm reported detected analytes by comparing the sample

                                            102

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                                                                               Region m Modification

Target Compound Identification                                                          PEST
       chromatograms to the tabulated results and verifying peak measurements  and retention times.
       Confirm reported non-detected  analytes by a review of the sample chromatograms.  Check the
       associated blank data for potential interferences (to evaluate sample data for false positives) and
       check the calibration data for adequate retention time windows (to evaluate sample data for false
       positives and false negatives).

   2.  For multi-component target compounds (Toxaphene and Aroclors), the retention times and relative
       peak heights ratios of major component peaks should be compared against the  appropriate
       standard chromatograms.

   3.  Verify that GC/MS confirmation was performed for pesticide concentrations in the final sample
       extract which exceeded 10 ng/uL.

E. Action

   1,  If the qualitative criteria for both columns were not met, all target compounds that are reported
       detected should be considered non-detected.  The reviewer may use professional judgement to
       qualify reported compounds "N", tentatively identified, or "R", rejected.  In the case of multi-
       component compounds,  the reviewer  can accept the reported compound based on pattern
       recognition and relative peak height ratios.  The reviewer should use professional judgement to
       assign an appropriate quantitation limit  using the following guidance:

       a. If the misidentified peak  was sufficiently outside the target pesticide retention time window,
          then the reported values may be a false positive and should be replaced with the sample CRQL
          value.

       b. If the misidentified peak poses an interference with potential detection of a target peak, then
          the reported value should be considered and qualified as unusable (R),

   2.  If the data reviewer identifies a peak in both GC column analyses that falls within the appropriate
       retention time windows, but was reported as a non-detect, then die compound may be a false
       negative. Professional judgement should be used to decide if the compound should be included.
       All  conclusions made regarding target  compound  identification should be included in the data
       review narrative.

   3.  If multi-component target compounds  exhibit marginal pattern-matching quality, professional
       judgement should  be  used  to  establish whether  die differences  are due to environmental
       "weathering" (i.e., degradation  of die earlier eluting peaks relative to die later eluting peaks).
       If die presence of a multi-component pesticide is strongly suggested, results should be reported
       as presumptively present  (N).   If an observed pattern closely matches more than one Aroclor,
       professional judgement should be used to decide  whether die  neighboring Aroclor is a better
       match,  or if multiple Aroclors are present.

   4.  If it is determined that qualitative criteria for two-column confirmation were not met, all such data
       should be reported as not detected and it should be clearly noted in die narrative.
                                             103

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                                                                              Region III Modification

Target Compound Identification                                                          PEST
   5,  When all qualitative criteria for identification have been met, single-peak pesticides which are not
       confirmed by GC/MS should be noted in the narrative, indicating that supporting data may be
       necessary to rely upon these results.  If supporting data exist (site-related records, GC/MS
       confirmations of other samples,  etc.), the reviewer should discuss the type of supporting data in
       the narrative. Whenever single-peak pesticides are confirmed by an acceptable GC/MS spectrum
       and retention time match against standards, confirmation should be noted in the narrative.
                                             104

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                                                                               Region DI Modifiutioai

                                                                                          PEST
                         . CompOTnd QuanfMtUiQn and ReporteJ C
A. Review Items:  Form I PEST, Form X PEST-i and  PEST-2,  sample preparation  log  sheets,
    chromatograms, case narrative, and data system printouts.

B.    Objective

    The objective is to ensure that the reported quantitative results and contract required quantitation limits
    (CRQLs) are accurate.

C. Criteria

    Compound quantitation, as well as the adjustment of the CRQL, must be calculated according to the
    equations provided in Appendix A (also found in Section D/Pest of the Statement of Work).

D. Evaluation

    1.  Raw data should be examined to verify the correct calculation of all sample results reported by
       the laboratory.  Data system printouts, chromatograms, and sample preparation log sheets should
       be  compared to the reported positive sample results and  quantitation limits.  Verify that die
       sample  values  are reported  correctly.    Calculation errors  can sometimes be revealed by
       abnormally high surrogate recoveries, matrix spike recoveries, or inappropriately high results for
       certain compounds.

    2.  Verify that the CRQLs have been adjusted to reflect all sample dilutions, concentrations, splits,
       clean-up activities, and dry weight factors that are not accounted for by the method.

E.  Action

    1.  Quantitation limits affected by large, off-scale peaks should be qualified as unusable (R).  If the
       interference is on-scale, the reviewer can provide an approximated quantitation limit (UJ) for each
       affected compound.

    Note: Single-peak pesticide results are checked for rough agreement between  quantitative  results
          obtained by the two GC columns. The potential for co-elution should be considered and the
          reviewer should use professional judgement to decide whether a much larger  concentration
          obtained on one column versus the other indicates the presence of an interfering compound.
          If an interfering compound is indicated, professional judgement must be used to determine how
          best to report, and if necessary, qualify die data.  Contractually the lower of the two values
          is reported.

   2.  If there  are  any discrepancies found, the  laboratory may be  contacted  by  the designated
       representative to obtain additional information that could resolve any differences. If a discrepancy
       remains unresolved, the reviewer must decide which value  is the best value. Under these
                                             105

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                                                                             Rtgion HI Modification*

Compound Quantitation and Reported CRQLS                                           PEST
       circumstances, die reviewer may determine if qualification of the data is warranted. A description
       of the reasons for data qualification and the qualification that is applied to the data should be
       documented in the data review narrative.

   3.   If the calculated concentrations of detected  compounds do not agree ±25% on both columns,
       qualify the reported value "J", estimated.
                                            106

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                                                                                Region HI Modification!

                                                                                           PEST
                                    XII.  Overall Assessment
A. Review Items:  Entire data package, data review results, and (if available) Quality Assurance Project
    Plan (QAPjP), and Sampling and Analysis Plan (SAP).

B. Objective

    The overall assessment of a data package is a brief narrative in which the data reviewer expresses
    concerns and comments on the quality and, if possible, the useability of the data.

C. Criteria

    Assess die overall quality of the data.

    Review all available materials to assess the overall quality of the data, keeping in mind the additive
    nature of analytical problems

D. Evaluation

    1.  Evaluate any technical problems which have not been previously addressed.

    2.  Review all  available materials to assess the overall quality of the data, keeping in mind the
       additive nature of analytical problems.

    3.  If appropriate information is available, the reviewer may assess the useability of the data to assist
       the data user in avoiding inappropriate use  of the data.  Review all  available information,
       including the QAPjP (specifically the Data Quality Objectives), SAP, and  communication with
       data user that concerns the intended use and desired quality of the data.

E.  Action

    1.  Use professional judgement to determine  if there is any  need to qualify data  which were not
       qualified based on the QC criteria previously discussed.

    2.  Write a brief narrative to give the user an  indication of the analytical limitations of the data.  If
       sufficient information on the intended  use and required quality of the data are available, the
       reviewer should include his/her assessment of the useability of the data within the given context.
       Reference the Region HI Data Validation Reports Requirements, found in Appendix B.
                                              107

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               APPENDIX A
CONTRACTUAL REQUIREMENTS AND EQUATIONS

MULTI-MEDIA, MULTI-CONCENTRATION - MM/MC
                (OLM01.0)

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                                                                      Region HI Modifications

                                                                          APPENDIX A

                       MULTI-MEDIA, MULTI-CONCENTRATION
  CONTRACTUAL REQUIREMENTS AM) EQUATIONS FOR VOLATILE DATA REVIEW
n. GC/MS Instrument Performance Check

Use equation n.l to verify that the laboratory has not made errors in the calculation of the percent
relative abundance.
            % tetative Abundance =                x m%
                                  abundance of Y

For example, the percent relative abundance of m/z 96 (X) relative to m/z 95 (Y) is calculated as follows:

                                          «*"•**» °/ ^ %
                                          abundance of mjz 95
                    % Jfetofre Abundance - «*"•**» °/ ^ % * 100%
III.  Initial Calibration

Data|^jejy_C.riterji; All volatile target compounds and system monitoring compounds must nave a
Relative Response Factor (RRF) of greater than or equal to 0.05 and a percent relative standard deviation
(%RSD) of less man or equal to 30%.

Contractual Criteria:  The maximum %RSD for volatile compounds is 20.5% and the minimum RRF
criteria vary as specified  in Table A.I (The volatile compounds listed separately in Table 2 on page 13
are not contractually required to meet a maximum %RSD but do nave to meet a contractual minimum
RRF of 0.010).  The contractual criteria for an acceptable initial calibration specifies mat up to any 2
volatile target compounds may fail  to meet minimum RRF or maximum %RSD as long as they have
RRFs that are greater than or equal  to 0.010, and %RSD of less than or equal to 40.0%.

             Table A-l Minimum RRF Criteria for Volatile Target Compounds

                    Volatile                                 Minimum
                    Compound                               RRP

                    Broroomethane                           0.100
                    Vinyl chloride                            0.100
                    1,1-Dichloroethene                        0.100
                    1,1-Dichloroethane                        0.200
                    Chloroform                               0.200

                    1,2-Dichloroethane                        0.100
                    1,1,1-TnchJoroethane                      0.100
                    Carbon tetracMoride                       0.100
                    Bromodichloromethane                     0.200
                    cis-t,3-Dichloropropene                    0.200
                                          A-l

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                                                                         Region in Modification*

 MM/MC                                                                    APPENDIX A


         Table A.I Minimum RRF Criteria for Volatile Target Compounds (continued)

                     Volatile                                   Minimum
                     Compound                                EKE

                     Trichloroethene                            0.300
                     Dibromochloromethane                      0.100
                     1,1,2-Trichloroethane                       0.100
                     Benzene                                  0.500

                     trans-1,2-Dichloropropene                   0.100
                     Bromofonn                                0.100
                     Tetrachloroethene                          0.200
                     1,1,2,2-Tetrachloroethane                   0.500
                     Toluene                                   0.400

                     Chlorobenzene                             0.500
                     Ethylbenzene                              0.100
                     Styrene                                   0.300
                     Xylenes (total)                             0.300
                     Bromofluorobenzene                        0.200
Initial calibration RRFs and RRF are calculated using equations ELI and ffl.2
                                      c*
                     where:
                            IMF,   =  "i'th Relative Response Factor
                            A      a:  Area of the characteristic ion (EICP) measured
                            C      =  Concentration
                            is      -  Internal standard
                            x      =  Analyte of interest
The %RSD is calculated using equations EQ.3 and QI.4.
                        a  *
                             N
                                            A-2

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                                                                         Region ffl Modificationi

MM/MC                                                                    APPENDIX A
                         %RSD - ^ Jt 100                  (777.4)
                                  x

       where:
              a =   Standard deviation of 5 relative response factors

              I =   Mean of 5 relative response factors


IV.  Continuing Calibration

Data Review Criteria:  All compounds must be considered for qualification when the %D exceeds the
± 25% criterion.
Contractual Criteria: The percent difference (%D) between the initial calibration RRF and the continuing
calibration RRF is ±  25%  for all compounds listed in Table A.l,  The contractual criteria for an
acceptable continuing calibration specified that up to aqyJE volatile target compounds may fail to meet
minimum RRF or maximum  %D as long as they have RRFs that are greater than or equal to 0.010, and
%D of less than or equal to 40.0%.

Check the continuing calibration RRF calculations for volatile target compounds using equation HL1.
The %D between  initial calibration RRF and continuing calibration RRF  is calculated using equation
IV. 1.


                             RRK-KRF
                     % D -     '      * x 100%                 (IK1)
                                RRF
       where:	
              RRF,  =  average relative response factor from initial calibration
              RRFC  =  relative response factor from continuing calibration standard

VI. System Monitoring Compounds

The Volatile system monitoring compounds (surrogates) and their contractual recovery limits are listed
in Table A.2,

             Table  A.2.  System Monitoring Compound Contractual Requirements

              System Monitoring Compound               % Recovery Limits
                                                Water Samples        Soil Samples

              SMC1 Toluene-d,                    88-110             84 -138
              SMC2 Bromofiuorobenzene            86 -115             59-113
              SMC3 l,2-Dichloroethane-d4           76-114             70 -121
                                           A-3

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                                                                      Region m ModificatioW

MM/MC                                                                  APPENDIX A


Use equation VI.l to check that the system monitoring compound recoveries were calculated correctly:


               % Recovery .
                            Concentrationjamoura spiked


VH. Matrix Spikes/Matrix Spike Duplicates

Hie matrix spike/matrix spike duplicate contractual requirements are listed in Table A.3.

                      Table A3 MS/MSD Contractual Requirements

       Compound           %R - Water   %R - Soil     RPD - Water  RPD - Soil

       U-DicMoroethene    61 -145       59-172         £ 14         £22
       Trichloroetliene       71 -120       62 -137         £ 14         £24
       Benzene             76-127       66-142         £11         £21
       Toluene             76-125       59-139         £13         £21
       CMorobenzene        75 -130       60 -  133         £ 13         £21

Verity that the matrix spike recoveries and RPD were calculated correctly using equations VH.1 and
VTL2.

                 % Recovery - SSR " SR x 100%                  (WO)
                                 ura

       where:
             SSR = Spiked sample result
             SR -  Sample result
             SA =  Spike added
      where:
             RPD =  Relative percent difference
             MSR =  Matrix spike recovery
             MSDR= Matrix spike duplicate recovery
                                         A-4

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                                                                          Region ED Modification*

 MM/MC                                                                     APPENDIX A


 IX. Internal Standards

 Table A.4 contains the volatile internal standards and their corresponding target compounds.  These
 criteria nave been established for packed columns only. Specific criteria for capillary columns have not
 been included in the SOW at this time.

           Table A.4 Internal Standards and Their Corresponding Target Compounds

 Bromochloromethane                 1 ,4-Difluorobenzene                Chlorobenzene-d.

 Chloromethane                      1,1,1-Trichloroethane               2-Hexanone
 Bromomethane                      Carbon tetrachloride                4-Methyl-2-pentanone
 Vinyl chloride                       Bromodichloromethane              Tetrachloroethene
 Chloroethane                        Bromoform                         1,1^^-Tetrachloroethaoe
 Methylene chloride                   1,2-DichJoropropane                Toluene
 Acetone                             trans-l,3-Dichloropropene            Chlorobenzene
 Carbon disulfide                     Trichloroethene                     Ethylbenzene
 1,1-Dichloroethene                   Dibromochloromethane              Styrene
 1,1-Dichloroethane                   1,1,2-Trichloroethane               Total Xylenes
 1,2-Dichloroethene (total)             Benzene                            BromofluorDbenzEne{SMQ
 Chloroform                         cis-l,3-Dichloropropene              Toluene-d, (SMC)
 1,2-Dichloroethane                   Bromoform
 2-Butanone
 l,2-DichJoroethane-d4 (SMC)

 SMC - System Monitoring Compound


XI.  Compound Quantltatlon and Reported Contract Required Quantitatlon Limits (CRQLs)

Check  die reported positive sample  results and quantitation limits with die  quantitation lists and
chromatograms  using  equations XI. 1, XI .2, or X1.3.   Characteristic bus for the volatile target
compounds are contained in Table A.5.  Characteristic ions for System Monitoring Compounds and
Internal Standards are contained in Table A .6.
       Concentration for waters*
                                  A, x L x Df
       Concentration for low level soils:
       (Dry weight basis)
                         ^ " A^xRKFx WtxD                 *
                                            A-5

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                                                                          Region HI Modifications

 MM/MC                                                                     APPENDIX A
        Concentration for medium level soils:
        (Dry weight basis)

                              A, x I, x Vt x 1000 x Df
       where:
               A. =  area of characteristic loo (EICP) for compound being measured
               Aj, =  area of characteristic ion (EICP) for the internal standard
               I, =   amount of internal standard added (ng)
               RRF = daily response factor for compound being measured
               V, =  volume of water purged (ml)
               W. =  weight of sample (g)
               D  =  (100 - % moisture)/100%
               V, =   volume of memanol (ml)*
               V, =   volume of extract added (ul) for purging
               Dr =   dilution factor**
               V, =   volume of the aliquot of the methanol extract (uL) added to reagent water for
                     purging

   *   This volume is typically  10,0 ml, even though only 1.0 ml is transferred to the vial. See the
       SOW for more details.
  **   The dilution factor for analysts of soil/sediment samples for volatiles by the medium level method
       is defined as the ratio of the number of microliters (ul) of memanol added to the reagent water
       for purging (VJ to the number of mictoliters of the metnanol extract of the sample contained in
       volume V.. If no dilution is performed, then the dilution factor equals 1.0.

The CRQL for a diluted sample should be calculated as follows:

         Ad/ustedCRQL -  Non-adjustedCRQL x Sample Dilution Factor         (X1.4)

       For example, the adjusted CRQL for a water sample with a 10U non-diluted CRQL and a 1 to
       100 dilution (100.0 dilution factor) would be 1000U, according to the following calculation:

                                    1000C/ « IOC? x
The CRQL adjustment for dry weight for a soil sample should be calculated as follows:

                 Dry Weight CSQL
                                           -          .
                                             100

       For example, .the dry weight CRQL for a soil sample with a 10U non-adjusted CRQL and a 10%
       moisture would be 11U, according to the following calculation:

                                               1QU
                                                100
                                            A-6

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MM/MC
Region ID Modiftcotioni




    APPENDIX A
                Table A.5 Characteristic Ions for Volatile Target Compounds
Analyte
CnJoromethane
Bromomethane
Vinyl chloride
Chloroethane
Methylene chloride
Acetone
Carbon disulfide
1 , 1 -Dichloroethene
1 , 1 -D ichloroethane
1,2-Diehloroetfaene
Chloroform
1 ,2-Dichloroethane
2-Butaoone
1,1, 1-Tr ichloroethane
Carbon tetrachloride
BromodichJoroemethane
1 , 1 ,2 ,2-TetrachJoroethane
1 .2-Dichloropropane
trans- 1,3-Dichloropropene
Trichloroethene
Dibromochloromethane
1 , 1 ,2-Trichloroethane
Benzene-
els- 1 ,3-Dichloropropene
Bromofonn
2-Hexanone
4-Methyl-2-pentanone
Primary Ion*
50
94
62
64
84
43
76
96
63
96
83
62
43**
i 97
117
83
83
63
75
130
129
97
78
75
173
43
43
Secondary Ion(s)
52
%
64
66
49, 51, 86
58
78
61,98
65, 83, 85, 98, 100
61,98
85
64, 100, 98
57
99, 117, 119
119, 121
85
85, 131. 133, 166
65, 114
77
95, 97, 132
208,206
83, 85, 99, 132, 134
—
77
171, 175, 250, 252, 254, 256
58, 57, 100
58,100
                                          A-7

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MM/MC
Region ID Modification*

    APPENDIX A
          Table A.5  Characteristic Ions for Volatile Target Compounds (Continued)
Analyte
Tetrachloroethene
Toluene
Chlorobenzene
Ethyl benzene
Styrene
Total Xylenes
Primary Ion* II Secondary Ion(s)
164
91
112
106
104
106
129, 131, 166
92
114
91
78, 103
91
**     While m/z 43 is used for quantitation of 2-Butanone, m/z 72  must be present for positive
       identification.
 *     The primary ion should be used unless interferences are present, in which case, a secondary ion
       may be used.
   Table A.6  Characteristic Ions for System Monitoring Compounds and Internal Standards
                             for Volatile Organic Compounds
Compound || Primary Ion | Secondary Ion(s)
SYSTEM MONITORING COMPOUNDS
4-Bromofluorobenzene
1 ,2-Dichloroethane-d4
Toluene-d,

Bromochloromethane
1 ,4-Difluorobenzene
Chlorobenzene-dj
95
65
98
INTERNAL STANDARDS
128
114
117
174, 176
102
70, 100

49, 130, 51
63,88
82,119
                                           A-8

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                                                                        Region HI Modifications

                                                                            APPENDIX A

                       MULTI-MEDIA, MULTI-CONCENTRATION
CONTRACTUAL REQUIREMENTS AND EQUATIONS FOR SEMIVOLATILE DATA REVIEW


n. GC/MS Instrument Performance Check

Use equation II. I  to verify that the laboratory has not made errors in the calculation of the percent
relative abundance.

For example, the percent relative abundance of m/z 443 (X) relative to m/z  442 (Y) is calculated as
follows:

                   or D i ^   JL  j       abundance of mlz 443   tnna
                   % Relative Abundance ~ - l — — - x 100%
                                          abundance of mlz 442
III.  Initial Calibration

Data Review Criteria: All semivolatile target compounds and surrogates must have a Relative Response
Factor (RRF) of greater than or equal to 0.05 and a percent relative standard deviation (%RSD) of less
than or equal to 30%.

Contractual Criteria:  The maximum %RSD tor most semivolatile compounds is 20.5% and the minimum
RRF criteria vary as specified in Table A. 7 (The semivolatile compounds listed separately in Table 4 on
page 52 are not contractually required to meet a maximum %RSD but do have to meet a contractual
minimum RRF of 0.010). The contractual criteria for an acceptable initial calibration specifies that up
to any 4 semivolatile target compounds may fail to meet minimum RRF or maximum  %RSD as long as
they have RRFs that are greater than or equal to 0.010, and %RSD of less than or equal to 40,0%.

            Table A.7 Minimum RRF Criteria for Semivolatile Target Compounds

                           Semivolatile                Minimum
                           Compounds                 RRF

                           Phenol                      0.800
                           bis{-2-Chloroethyl)ether        0.700
                           2-Chlorophenol               0.800
                           1 .3-Dichlorobenzene           0.600
                           1 .4-Dichlorobenzene           0.500

                           I.2-Dichlorobenzene           0.400
                           2-Methylphenol               0.700
                           4-Methylphenol               0.600
                           N-Nitroso-di-n-propyiamine    0.500
                           Hexachloroethane             0.300

                           Nitrobenzene                 0.200
                           Isophorone                  0.400
                           2-Nitrophenol                0.100
                           2, 4-Dimethy (phenol           0.200
                           bis(-2-Chloroethoxy)methane   0.300

                                          A-9

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                                                                          Region HI Modifications

MM/MC                                                                      APPENDIX A
      Table A.7 Minimum RRF Criteria for Semivolalile Target Compounds (Continued)

                            Semi volatile                  Minimum
                            Compounds                   RRF

                            2,4-Dichlorophenol             0.200
                            1,2,4-Trichlorobenzene         0.200
                            Naphthalene                   0.700
                            4-Chloro-3-methylphenoi        0.200
                            2-MethylnaphthaJene           0.400

                            2,4,6-Trichlorophenol          0.200
                            2,4,5-Trichlorophenol          0.200
                            2-ChIoronaphthalene           0.800
                            Acenaphthylene                1.300
                            2,6-Dinitrotoluene              0.200

                            Acenaphthylene                0.800
                            Dibenzoftiran                  0.800
                            2,4-Dinitrotoluene              0.200
                            4-ChorophenyI-phenyIether      0.400
                            Fluorene                      0.900

                            4-Bromophenyl-phenylether     0.100
                            Hexachlorobenzene             0.100
                            Pentachlorophenol              0.050
                            Phenanthrene                  0.700
                            Anthracene                    0.700

                            Fluoranthene                   0.600
                            Pyrene                        0.600
                            Benzo(a)anthracene             0.800
                            Chrysene                      0.700
                            Benzo(b)fluoranthene           0.700

                            Benzo(k)fluoranthene           0.700
                            Benzo(a)pyrene                0.700
                            lndeno(l,2,3-cd)pyrene         0.500
                            Dibenz(a,h)anthracene          0.400
                            Benzo(g,h,i)perylene           0.500

                            Nitrobenzene-d,                0.200
                            2-FluorobiphenyI               0.700
                            Terpheny!-dw                  0.500
                            Phenol-d,                      0.800
                            2-FluorophenoJ                 0.600
                            2-Chlorophenol-d4              0.800
                            1,2-Dichiorobenzene-d4         0.400

      Initial  calibration RRF and RRF are calculated using equations  III. 1  and III.2;  %RSD is
      calculated using equations III.3 (pg.A-2,  Appendix A) and  III.4 (pg.A-3, Appendix A).

                                            A-10

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                                                                           Region 10 Modifications

 MM/MC                                                                      APPENDIX A


 IV. Continuing Calibration

 Data Review Criteria:  All semivolatile target compounds should meet a %D criterion of ±25%.
 Contractual Criteria: The percent difference (%D) between the initial calibration RRF and the continuing
 calibration RRF is  ±25.0% for the compounds listed in Table A.4.  The contractual criteria for an
 acceptable continuing calibration specifies that up to any_4jemivolatile target compounds may fail to meet
 minimum RRF or maximum %D as long as they have RRFs that are greater than or equal to 0.010, and
 %D of less than or equal to 40.0%.

 Check the continuing calibration RRF calculations for semivolatile target compounds using equation ID. 1
 (reference p.A-2), and evaluate the %D between initial calibration RRF and continuing calibration RRF
 using equation IV.I (reference p.A-3).

 VI.  Surrogate Spikes

 The semivolatile surrogate compounds  and their contractual recovery limits are listed in Table A.8.


                        Table A.8 Semivolatile Surrogate Requirements

               Surrogate                           %Recovery Limits
                                            Water Samples       Soil Samples

               SI Nitrobenzene-d,              35 - 144            23 - 120
               S2 2-Fluorobiphenyl              43 - 116            30 - 115
               S3 Terphenyl-d14                33 - 141            18 - 137
               S4Phenol-d<                    10-110            24-113
               S5 2-Fluoprophenol              21-110            25 - 121
               S6 2.4.6-Tribromophenol         10 - 123            19 - 122
               S7 2-Chlorophenol-d4             33 - 110*           20 - 130*
               s8 U-Dichlorobenzene-d,        16-110*           20-130*

               * Advisory limits

Use equation VI. I to verify that the surrogate recoveries were calculated correctly.

VII. Matrix Spikes/Matrix Spike Duplicates

The matrix spike/matrix spike duplicate contractual requirements are listed in Table A.9.

Verify  that the  matrix spike recoveries and RPD  were calculated correctly using equations  VII. 1 and
VU.2.  (Reference p.A-4)

DC.  Internal Standards

Table A. 10 contains the semivolatile internal standards and their corresponding target compounds.
                                            A-ll

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                                                                Region IQ Modifications

MM/MC                                                             APPENDIX A


               Table A.9 Semivolatile MS/MSD Contractual Requirements

      Compound                 %R - Water   %R - Soil     RPD - Water  RPD - Soil
                                                                             'k
      Phenol                    12-110     26-90        £42         £35
      2-CUorophenol             27 - 123     25 - 102       £40         £50
      1,4-DicMorobenzene         36-97      28-104       £28         £27

      N-Nitroso-di-n-proplyamine   41-116     41-126       £38         £38
      1,2,4-TriehJorobenzene       39 - 98      38 - 107       £28         £23
      4-Chloro-3-methylphenoI      23 - 97      26-103       £42         £33
      Acenaphthene              46-118     31-137       £31         £19
      4-Nitrophenol              10-80      1! - 114       £50         £50
      2,4-DJnitrotoIuene           24-96      28-89        £38         £47
      Pentachlorophenol           9 -  103      17 - 109       £50         £47
      Pyrene                    26 - 127     35-142       £31         £36
                                     A-12

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 MM/MC
                                         Region III Modifications

                                             APPENDIX A
    Table A.10 Semivolatile Internal Standards and Their Corresponding Target Compounds
 1,4-Dichlorobenzene-d4
 Naphthalene-dg
Acenaphthene-d
                                                                                 10
 Phenol
 bis(2-Chloroethyl)ether
 2-ChJorophenol
 1,3-Dichlorobenzene
 1,4-Dichlorobenzene
 1,2-Dichlorobenzene
 2-Methylphenol
 2,2*-oxybis-( 1 -Chlorapropane)
 4-Methylphenol
 N-Nitroso-Di-n-propylamine
 Hexachloroethane
 2-FIurorophenol (SUIT)
 PhenoWj (surr)
 2-Chloroben2ene-d4 (surr)
 1,2-Dichlorobenzene-d4 (surr)
Nitrobenzene
Isophorone
2-Nitrophenol
2,4-DimethyIphenol
bis(2-Chioroethoxy)methane
2,4-DiehlorophenoI
1,2,4-Triehlorobenzene
Napththalene
4-ChIoroaniline
Hexachlorohutadiene
4-Chloro-3-methylphenol
2-Methy I naphthalene
2-Nitrobenzene-d, (SUIT)
Hexachlorocyclopentadiene
2,4,6-Trichlorophenol
2,4,5-Trichlorophenol
2-Chloronaphthalene
2-NitroIaniline
Dimethyl phthalate
Acenaphthylene
3-Nitroaniline
Acenaphthene
2,4-Dinitrophenol
4-Nitrophenol
Dibenzofuran
2,4-Dinitroto!uene
2,6-Dinitrotoluene
Diethyl phthalate
4-Chlorophenyl-phenyl ether
Fluorene
4-Nitroaniline
2-FluorobiphenyI (SUIT)
2,4,6-TribromophenoI (surr)
Phenanthrene-d
              10
Chrysene-d12
Perylene-d,2
4,6-Dinitro-2-methylphenoI
N-Nitrosodiphenylamine
4-Bromophenyl pheoyl ether
H exachlorobenzene
Pentachlorophenol
Phenanthrene
Carbazole
Anthracene
Di-n-butyl phthalate
Fluoranthene
Pyrene
Butylbenzyl phthalate
3-3*-Dichlorobenzidine
Benzo(a)anthracene
bis(2-Ethylhexyl)phthalate
Chrysene
Terphenyl-d,4 (surr)
Di-n-octyl phthalate
Benzo(b)fluoranthene
Benzo(k)fluoranthene
Benzo(a)pyrene
lndeno(l ,2,3-«l)
Dibenz(a,h)anthracene
Benzo(g,h ,i)perylene
surr = surrogate compound
                                             A-13

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                                                                            Region III Modifications

MM/MC                                                                       APPENDIX A


XI.  Compound Quantitation and Reported Contract Required Quantitation Limits (CRQLs)

Check the reported  positive sample  results  and quantitation  limits with the quantitation lists  and
chromatograms using equations XI.6, XI.7, or XI,8 below. Equation X1.4 (reference p.A-6) should be
used to adjust the CRQL for a diluted sample, and equation XI.S should be used to adjust the CRQL for
a soil sample.  Characteristic ions  for semi volatile target compounds are contained  in Table  A. 11.
Characteristic  ions for semivolatile surrogates and  internal standards are contained  in Table  A. 12.
Characteristic ions for pesticides and Arolclors are contained in Table A. 13.

       Concentration for waters:

                                  A, x L x Vt x Df
       Concentration for soils/sediments:
       (Dry weight basis)
                                          x
       where:
              Ax  =   area of characteristic ion (EICP) for compound being measured
              Aj,  =   area of characteristic ion (EICP) for the internal standard
              I, —    amount of internal standard added (ng)
              RRF =  daily relative response factor for compound being measured
              V0  =   volume of water extracted (MI)
              Vj =    volume of extract injected (Ul)
              V, =    volume of concentrated extract (Ul)
              Df  =   dilution factor*
              D  =   (100 - % moisture)/ 100%
              W.  =   weight of sample (g)

       The dilution factor for analysis of water samples for semivolatiles by the method specified in
       SOW OLM01.0 is calculated using equation XI.S.  If no dilution is performed, then the dilution
       factor equals 1.0.


       nf   uL of the most concentrated extract used * uL of dean solvent        /vro\
       JJT s  - * - _ - — — - - - f - - -        \Al.O)
                        uL of the most concentrated extract used
                                            A-14

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                                                                      Region ID Modification*




MM/MC                                                                  APPENDIX A




             Table A.11 Characteristic Ions for Semivolatile Target Compounds
Analyte | Primary Ion | Secondary Ion(s)
Phenol 94
bis(2-Chloroethyl)ether | 93
2-ChlorophenoI
1 ,3-Dichlorobenzene
1 ,4-Dichlorobenzene
1 ,2-Dichlorobenzene
2-Methylpheaol
2,2'-oxybis(l -Chioropropane)
4-MethylphenoI
N-Nitroso-di-n-propylamine
Hexachloroethane
Nitrobenzene
Isophorone
2-Nitrophenol
2.4-Dimethylphenol
bis(2-Chloroethoxy)methane
2,4-DichlorophenoI
1 ,2 ,4-Trichlorobenzene
Naphthalene
4-Chloroaniliiie
Hexachlorobutadiene
4-Chloro-3-methyIpheQol
2-Methylnaphthalene
Hexachlorocydopentadiene
2,4,6-TrichlorophenoI
2,4,5-Trichlorophenol
2-Chloronaphthalene
2-Nitroaniline .
128
146
146
146
108
45
108
70
117
77
82
139
107
93
162
180
128
127
225
107
142
237
196
1%
162
65
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
128, 127
129
223, 227
144, 142
141
235,272
198, 200
198, 200
164, 127
92,138
                                         A-15

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MM/MC
Regkm HI Modifications




    APPENDIX A
        Table A.11  Characteristic Ions for SemivolatUe Target Compounds (Continued)
Parameter
Dimethyl phthalate
Acenaphthylene
3-Nitroaniline
Acenaphthene
2,4-Dinitrophenol
4-Nitrophenol
Dibenzofuran
2,4-Dinitrotoluene
2,6-Dinitrotoluene
Diethylphthalate
4-ChJorophenyl-phenylether
Fluorene
4-Nitroaniline
4,6-Dinitro-2-methylphenol
N-Nitrosodiphenylamine
4-Bromophenyl-phenylether
Hexachlorobenzene
Pentachlorophenol
Phenanthrene
Anthracene
Carbazole
Di-n-butylphthalate
Fluoranthene
Pyrene
Butylbenzylphthalate
3.3'-DichJorobenzidine
Benz(a)anthracene
bis(2-Ethylhexyl)phthalate
Primary Ion II Secondary Ion(s)
163
152
138
153
1*4
109
168
165
165
149
204
166
138
198
169
248
284-
266
178
178
167
149
202
202
149
252
228
149
194, 164
151, 153
108,92
152, 154
63,154
139,65
139
63,182
89, 121
177, 150
206, 141
165, 167
92, 108
182,77
168, 167
250, 141
142, 249
264,268
179, 176
179, 176
166, 139
150, 104
101, 100
101, 100
91,206
254,126
229, 226
167, 279
                                         A-16

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MM/MC
Region m Modification*




    APPENDIX A
        Table A.11  Characteristic Ions for Semivolatile Target Compounds (Continued)
Analyte
Chrysene
Di-n-Octyl phthalate
Benzo(b)fluoranthene
Benzo(k)fluoranthene
Benzo{a)pyrene
Indeno(l , 2,3-cd)pyrene
Dibenz(a,h)authracene
Benzo(g,h,i)perylene
Primary Ion
228
149
252
252
252
276
278
276
Secondary Ion(s)
226, 229
—
253,125
253, 125
253, 125
138, 227
139, 279
138, 277
                                         A-17

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                                                                       Region ID Modifications




MM/MC                                                                   APPENDIX A




      Table A.12  Characteristic Ions for Semivolatile Surrogates and Internal Standards
Analyte | Primary loo
[ Secondary Ion(s)
SURROGATES
Phenol-d3
2-Fluorophenol
2,4,6-Tribromophenol
Nitrobenzene-d,
2-Fluorobiphenyl
Terphenyl
2-Chlorophenol-d^
1 ,2-Dichlorobenzene-d4

1 .4-DicbJorobenzene-d4
Naphthalene-
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MM/MC
Region ID Modification*




    APPENDIX A
                   Table A.13 Characteristic Ions for Pesticides/Arodors
Analyte
aipha-BHC
beta-BHC
delta-BHC
gamma-BHC (Lindane)
Heptachlor
Aldrin
HeptachJor expoxide
Endosulfan I
Dieldrin
4,4'-DDE
Endrin
Endrin ketone
Endrin aldehyde
Endosulfan n
1,4'-DDD
Endosulfan sulfate
4,4'-DDT
Methoxychlor
Chlordane (alpha and/or gamma)
Toxaphene
Aroclor-1016
Aroclor-1221
Aroclor-1232
Aroclor-1242
Aroclor-1248
Aroclor-1254
Aroclor-1260
Primary Ion
183
181
183
183
100
66
353
195
79
246
263
317
67
337
235
272
235
227
373
159
222
190
190
222
292
292
360
Secondary Ion(s)
181, 109
183, 109
181, 109
181, 109
272, 274
263, 220
355, 351
339, 341
263,279
248, 176
82,81
67, 319
250,345
339, 341
237, 165
387, 422
237,165
228
375, 377
231, 233
260,292
222,260
222, 260
256,292
362,326
362,326
362,394
                                          A-19

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                                                                            Region in Modifications

MM/MC                                                                        APPENDIX A
Calibration standards are prepared at a minimum of five concentration levels (20, 50, 80,  120, and 160
total ng).  Eight compounds listed below require only a four-point initial calibration at 50, 80, 120 and
160 total ng.

         2,4-  Dinitro phenol                          4-  Nitroaniline
       2,3,4 -  Trichlorophenol                         4 -  Nitrophenol
           2 -  Nitroaniline                          4,6 -  Dinitro-2-methylphenol
           3 -  Nitroaniline                                Pentachlorophenol
                                            A-20

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                                                                     Region HI Modifications

                                                                         APPENDIX A
                      MULTI-MEDIA, MULTI-CONCENTRATION
  CONTRACTUAL REQUIREMENTS AND EQUATIONS FOR PESTICIDE DATA REVIEW
Q.  GC/ECD Instrument Perfonnance Check

Check the Perfonnance Evaluation Mixture calculations to ensure correct calculation of DDT and Endrin
breakdown. When using equations 0.2 and 0.3, values for the amount found and the amount injected
should be reported in nanograms (ng). The breakdown of DDT and Endrin in both of the PEM injections
must be less than 20.0 percent, and the combined breakdown of DDT and Endrin must be less than 30.0
percent.
       % Breakdown DDT - *™»»* P™* {DDD+DDE) x 100
                              Amount of DDT injected
    % Breakdown Ewfrin = *""""* •*"""* (J5afriB oldg/^fe * Eadrin ****"**> * 10°    (ff.3)
                                      Amount of Endrin injected
    Combined % Breakdown = % Breakdown DDT + % Breakdown Endrin            (17.4)
All peaks in both injections of the Performance Evaluation Mixture must be 100 percent resolved on bom
columns.  The relative percent difference of the calculated amount and the true amount for each of the
single component pesticides and surrogates in the PEMs must be less man or equal to 25.0 percent using
equation O.5.


                                |C    - C^J
                                        **    x 100
      Where:
                 =  True concentration of each analyte
                 ~  Calculated concentration of each analyte from the analysis of the standard
                                        A-21

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                                                                        Region DB Modification*

                                                                            APPENDIX A
ID.  Initial Calibration

Retention time windows for each analyte and surrogate are calculated using Table A. 14, Windows are
centered around the mean absolute retention time for die analyte established during the initial calibration.
For example, for a given pesticide die mean retention time is first determined from the initial calibration
is found to be 12,69 minutes.   The retention time window for this  pesticide is ± 0.05 minutes.
Therefore, the calculated retention time window would range from 12.64 to 12.74 minutes.
              Table A.14 Retention Time Windows for Pesticide Target Compounds

              Pesticide Compounds           Retention Time Windows in Minutes

                alpha-BBC                                    ±0.05
                beta-BHC                                     ±0.05
                gamma-BBC                                  ±0.05
                delta-BBC                                     ±0.05
                HepatachJor                                   ±0.05

                Aldrin                                        ±0.05
                alpha-Chtordane                               ±0.07
                gamma-Chlordane                              ±0.07
                Heptachlor epoxide                             ±0.07
                Dieldrin                                       ±0.07

                Endrin                                        ±0.07
                Endrin aidehyde                               ±0.07
                Endrin ketone                                 ±0.07
                ODD                                         ±0.07
                DDE                                         ±0.07

                DDT            .                             ±0.07
                Endosulfan I                                  ±0.07
                Endosulfan n                                  ±0.07
                Endosulfan sulfate                              ±0.07
                Methoxychlor                                 ±0.07

                Aroclors                                      ±0.07
                Toxaphene                                    ±0.07
                Tetrachloro-m-xylene                           ±0.05
                Decachlorobiphenyl                             ±0.10
                                          A-22

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                                                                           Region ID Modification*

                                                                               APPENDIX A
 Hie % RSD of the calibration factors for each single component target must be less than or equal to 20.0
 percent.  The % RSD for toe two surrogates must be less than or equal to 30.0 percent. Up to two single
 component target compounds per column may exceed the 20.0 percent limit for  %  RSD, but those
 compounds must nave a % RSD of less man or equal to 30.0 percent. Calibration factors are calculated
 using equations HI. 5 and ffl.6 and the % RSD is calculated using equations in. 3 and DI.4.
                        %KSD .                   x joo                     (Jff.3)
                                       Mean
        where,
                           Standard Deviation - |—	f/2           (flf.4)
       Where:
              5i = each individual value used to calculate the mean
              x = the mean of n values
              n — me total number of values
                                    Area of the Standard
                                          "— - - -
                                     mass injected
                                        n
                                 SF-E  ^
                                       i-I   *

       Where: _
              CF  = Mean calibration factor of a n values
              CF,  = i* calibration factor
              n  = Total number of values
IV.  Continuing Calibration

The retention time (RT) for each target compound and surrogate must be within RT window as calculated
above using the mean absolute RT established during the three-point initial calibration.  The relative
percent difference of the calculated amount and the true amount for each of the compounds in the mid
point concentration of the individual Standard mixtures must be less than or equal to 25.0 percent, using
equation D.S.
                                            A-23

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                                                                          Region ffl Modifications

                                                                              APPENDIX A
VI.  Surrogate Spikes

The advisory limits lor recovery of tetrachloro-m-xylene (TCX) and decachlorobiphenyl (DCB) are 60-
150 percent for both water and soil samples. The surrogate percent recovery is calculated using equation
VI. 1 . The retention time of bom surrogates must be within the calculated retention time windows, i.e.,
TCX must be within  ±0.05 minutes of the mean retention time determined from the initial calibration
and DCB must be within  ±0.10 minutes of the mean retention time  determined from the  initial
calibration.
                                                      J
                        Surrogate Percent Recovery « — - x 100
                                                    v«

       Where:
              Qi = Quantity determined by analysis
              Q, = Quantity added to sample/blank
                                           A-24

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                                                                       Region HI Modifications

                                                                           APPENDIX A
VH. Matrix Spikes/Matrix Spite Duplicate

Tie matrix spike/matrix spike duplicate recovery and RPD requirements are listed in Table A. 15.  The
matrix spike recoveries and RPD are calculated using equations VQ.l and VH.2.
                       Table A. IS MS/MSD Contractual Requirements
Compound
gamma-BHC (Lindane)
Heptachlor
Aldrin
Dieldrin
Endrin
4,4'-DDT
% Recovery
 Water
 56-123
 40-131
 40-120
 52-126
 56-121
 38-127
 RPD
Water
  15
  20
  22
  18
  21
  27
                                % Recovery
                                 Soil
                                 46-127
                                 35-130
                                 34-132
                                 31-134
                                 42-139
                                 23-134
RPD
Soil
 50
 31
 43
 38
 45
 50
                      Spike Recovery
           SSR-SR
               SA
 x 100
       Where:
             SSR - Spike sample result
             SR  = Sample result
             SA  = Spike added
                      RPD
  \MSR - MSDR\
1/2 (MSR + MSDR)
                       100
                         (VU2)
       Where:
             RPD  = Relative percent difference
             MSR  = Matrix spike recovery
             MSDR = Matrix spike duplicate recovery

             The vertical bars in me formula above indicate the absolute value of the
             difference, hence RPD is always expressed as a positive value.
                                          A-25

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                                                                            Region ID Modifications

                                                                                APPENDIX A
IX.  Pesticide Cleanup Check

Every lot number of Florisil cartridges used for sample cleanup must be checked by spiking with 2,4,5-
trichlorophenol and midpoint concentration of Individual Standard Mixture A.  Hie recoveries for all of
die pesticides and surrogates in Individual Standard Mixture A must be within 80 to 120 percent, the
recovery of 2,4,5-trichJorophenol must be less than 5 percent, and no peaks oust interfere with the target
analytes.  Percent recovery is determined using equation DLL
                          Percent Recovery  - — x 100                     (/X.I)
       Where:
               Q4 = Quantity determined by analysis
               Q. — Quantity added to sample/blank

The gel permeation chromatography (GPC) apparatus must be calibrated every 7 days. The calibration
is acceptable if the recovery of each single component analyte is within 80-110 percent and the Aroclor
patterns match patterns previously generated by standards.
X.  Target Compound Identification

Retention times of surrogates, matrix spikes, and reported compounds must fall within the retention time
windows established using the initial three-point calibration.
                                             A-26

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                                                                            Region in Modifications-

                                                                                APPENDIX A
XI.  Compound Quantitation and Reported CRQLs

The concentration of the single component pesticides are calculated using equations XI. 1 and XI.2, as
appropriate. The dilution factor for both soil and water samples is calculated using equation XI.3 and
the adjusted CRQL is calculated using equation XI.4. Equation XI.5 is used to adjust the CRQL for the
sampies's dry weight.  The percent difference (%d) is calculated comparing calculated concentrations for
both columns using equation XI.6.

Concentration for water samples:


                           Concentration  uglL =    ^  ^  '               (JO.l)
       Where:
              A, =  Area of the peak for the compound to be measured.
              CF =  Calibration factor for the mid point concentration external standard (area per ng).
              V0 =  Volume of water extracted in milliliters (mL).
              V; =  Volume of extract injected in micro!iters (uL).  (If a single injection is made on
                     to two columns, use one half the volume  in the syringe as the volume injected
                     on to each column.)
              Vt =  Volume of the concentrated extract in microliters (uL) (this volume must be
                     10000 uL, see Section E, 7.2.3).
              Df =  Dilution Factor. The dilution factor for analysis of water samples by this method
                     is defined as follows:


                 uL most cone, extract used for dilution +  uL clean solvent           ty. ^
                          uL most cone, extract used for dilution
              If no dilution is performed, Df = 1.0

              If GPC is performed on a water sample extract, V, becomes 5000 uL, and a factor of 2
              must be added to the numerator, as described below for soil/sediment samples.
                                            A-27

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                                                                            Region M Modifications

                                                                                APPENDIX A

 Concentration for soil samples (Dry weight basis)


                        Concentration  ug/Kg  *	               (XI.2)
        Where:
               A, and CF are as given for water, above,
               Vt =<   Volume of the concentrated extract in microliters (uL) (this volume must be 5000
                      uL, see Section n, 7.2.3)
               V; =   Volume of extract injected in microliters (uL)  (If a single injection is made on
                      to two columns, use one half the volume in the syringe as the volume injected
                      on to each column.)
               D  =   100 - %  moisture
                          100
               W. =   Weight of sample extracted in grams (g).
               Df =   Dilution Factor.  The dilution factor for analysis of soil samples by this method
                      is defined as follows:
Dilution factor (Dr):
                 n -  «£ most cone, extract used for dilution + uL clean sovcnt        .„. „.
                   f             uL meat cone, extract used for dilution
               If no dilution is performed, Df = 1.0.

               The factor of 2.0 in the numerator is used to account for the amount of extract that is not
               recovered from the mandatory use of GPC cleanup. Concentrating the extract collected
               after GPC to 5.0 mL rather man 10.0 mL-for water samples not subjected to GPC (see
               Section n. 7.2.3 in the  CLP SOW  OLM01.0 or subsequent revision),  maintains the
               sens|tiyi|y of die soil method comparable to that of the water method, but correction of
               the numerical result  is  still required.
Dilution factor (Df):
                  n  - "*• "»*** conc- extract used for dilution + uL clean solvent
                   f            uL most conc. extract used for dilution
CRQL  (Adjusted for dilution)

                             (CRQL) (D) = Adjusted CRQL                     (XI. 4)
       Where:
              CRQL =  contract required quantitation limit
              Df     =   Dilution factor

                                             A-28

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                                                                          Region ID Modificalkmi

                                                                              APPENDIX A
CRQL  (Adjusted for samples dry weight)
       Where:
              D     =      100 - % moisture
                                  100
              CRQL =      contract required quantitation limit
              D,     =      dilution factor

       If no dilution is performed, D, =  1.0

If a sample extract cannot be concentrated to the protocol-specified volume, this fact must be accounted
for in reporting the sample quantitation limit. (SOW:  Exhibit C)
Percent difference:
                                      ConcL

       Where:
              COUCH = The higher of the two concentrations for the target compound in question
                    = The lower of the two concentrations for the target compound in question
                                           A-29

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              APPENDIX B




REGION III STANDARD OPERATING PROCEDURE




      FOR DATA VALIDATION REPORTS

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                                                                    Appendix Bp
                                                                   Page 1 of 6


                  ORGANIC DATA VALIDATION REPORT PREPARATION

1.0    Purpose

       The purpose of this procedure is to establish a report format for organic
       data review  report  writing  according  to EPA Region III protocol and is
       based on and applies to organic data review level M3 only.

2.0    Discussion

       After completion of data  review,  the  data reviewer will be responsible
       for  compiling  review notes  and  writing a  report.   The  outline below
       describes  the  steps  to follow  in preparing  the  organic data  review
       report.

3.0    Procedure

       3.1    Organic Data Validation Narrative

              The validation narrative is for the data user.  Because the data
              user may not be familiar with EPA abbreviations, it is necessary
              to write out commonly used  acronyms such as RAS, DAS, etc..

              3.1.1    The first  page  of the report  should be printed  on
                       letterhead.   The address of the report should include the
                       following  information  and be  in the  established format
                       for Region III,  as:


                      Date:      Month DO, YEAR  (Date report is  sent to EPA)

                      Subject:    Organic Data Validation for Case {case #)
                                 Site  (write site name)

                      From:      Reviewer Name        Oversight Reviewer Name
                                 Reviewer Title       Reviewer Title

                      To:         Remedial Project Manager
                                 EPA Region III
              3.1.2    Overview

                       The first section of the report is the overview, and is
                       presented in paragraph form after the title "OVERVIEW".
                       Information in this paragraph should include:
                           Case or DAS  (Delivered  Analytical  Services)  Number
                           Analytes
                           Number of samples
                           Matrix (or matrices and number of  samples  of each
                           matrix)
                           Number of QC samples (field and/or equipment blanks,
                           trip blanks,  field  duplicates,  etc.)
                       -    The  SOW under  which  the laboratory  performed  the
                           analyses
                           Laboratory name and its CLP  Code

                       A  statement should  also be  made that the samples were
                       analyzed  through  the Contract Laboratory Program (CLP),

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                                                      Appendix B
                                                     Page 2 of 6

         and whether they were performed as a Routine Analytical
         Services (RAS) or Delivered Analytical  Services (DAS).
         If results  exceeded  the levels identified  in the EPA
         10-day Chemical Health A'dvisory Levels  (Attachment A),
         such  exceedances   are*  mentioned   in   the   overview
         paragraph(s).
3.1.3    ««•»» »-y
         The summary section,  written below the title "SUMMARY",
         is  a general statement noting whether  the  samples were
         successfully analyzed  or  if  there  were  any  analyses
         determined   unsuccessful   (e.g.,   data  were  qualified
         unusable}.
3.1.4   Maior Problems
        After  the section  title,  "MAJOR PROBLEMS",  any problems
        identified during  the validation that  seriously  affect
        data usability and any data that are qualified unusable,
        "R",   is   noted  in   this  portion   of   the  narrative.
        Identification of  the support documentation included in
        the appendices  of  the report  (see  Section  3.1.8)  which
        identifies each  problem  is  referenced.   Each identified
        problem is reported  in a  separate paragraph.

        NOTE: Paragraphs in the major  and minor problems sections
        and  the  "Notes" section  are  presented in  "bulleted"
        format.
3.1.5   Minor Problems
        The  section title,  "MINOR PROBLEMS"  is  followed by  a
        series   of   bulleted  paragraphs   describing   biases
        identified during the data review which may qualify data
        as  "J",  "UJ",  "K",  "L",  or  "UL".    Examples of  these
        problems  are  discussed  thoroughly  in  the  Functional
        Guidelines  for Organic Data  Validation as Modified  by
        Region  III.    As in  the  reporting  of major  problems,
        support  documentation  is referenced  for each  problem
        described.

        Problems  listed in  this  section of  the narrative  are
        listed   according   to  the  hierarchy  of  qualifiers,
        beginning with the  most serious ("J", "UJ")  first.   If
        problems  are   identified  in   more   than  one  organic
        fraction, each fraction is identified.

        Notes

        This section  follows the minor problems  section  and  is
        used to  Identify issues  and  information which may  be
        beneficial to the data user,  and includes a paragraph
        describing any blank contamination found and its possible
        effects on sample results.  Maximum  levels  of the blank
        contaminants  are listed   in  tabular  form.  Common  lab
        contaminants are identified with an asterisk (*)•  Other
        Information  which  shall  be   included  in  the  "Notes"
        section  includes, but is not limited to:   variances  in
        methodology which did not  affect samples, dilutions used,
        non-spiked   MS/MSD   comparisons,   a  field   duplicate

-------
                                                             Appendix B
                                                            Page 3 of 5

                comparison summary (In tabular form with relative percent
                differences [RPDe]), and a  general statement regarding
                actions taken during the review of tentatively identified
                compounds  (TlCe) .    As  in  the problems  descriptions,
                reference is made  to support  documentation included in
                the appendices of the report.

        3.1.7    Report Content Statement

                A  short paragraph,  not  bulleted,  follows  the  notes
                section stating that the data were reviewed  in accordance
                with the Functional  Guidelines for  Evaluating Organic
                Analyses, as modified for use in Region III, and that the
                text of the report only addresses  those  problems which
                affect data usability.

        3.1.8
                Under  the  sectio'n  title  "ATTACHMENTS" .   a  list  of
                appendices  and  their  contents  is   included.     The
                appendices normally listed and their order  are:

                     Appendix A - Glossary of  Data Qualifiers
                     Appendix B- - Data Summary Forms
                     Appendix C - Laboratory Reported Results
                     Appendix D - Laboratory Reported TICs
                     Appendix E - Support  Documentation
3.2    Appendices
       Appendices are separated from the main body of the report by title
       pages  containing,  centered on the  page,  the appendix name  and
       title.

       3.2.1    Appendix A - glossary  of  Data  Qualifier Codas

                A listing of all organic  data  qualifiers  used  in Region
                III  and  their definitions is included  in  Attachment  D.

       3.2.2    Appendix B ~ Data S"twarv Forms

                3.2.2.1  The full title of this appendix is
                        "Data Summary.  These Include:
                        (a)    All positive results  for target compounds
                               with qualifier codes where applicable.
                        (b)    All unusable detection limits (qualified
                               "R")."

                3.2.2.2  Included  are  Data   Summary  Forms  for   all
                        fractions   analyzed,    sequentially  numbered
                        beginning with the volatile organic  fraction,
                        for all  samples  analyzed.   Information  on  the
                        Data Summary  Forms includes:  organic fraction
                        identified, sample matrix,  concentration units,
                        site, case number, SDG number  if  multiple SDGs
                        are reported,  sampling date(s),  sample numbers,
                        dilution factors used (if none,  identified as
                        1.0), sample locations,  sample  Identifications
                        (e.g.,  trip blank,  field duplicate), contract
                        required quantitation  limit for  each analyte,
                        all target  analytes,  all positive  results  and

-------
                                                      Appendix B
                                                     Page 4 of 5

                 quantitatton limits with  qualifier codas where
                 applicable, and  all unusable  detection limits
                 qualified "R".

              NOTE: Standard generation of the Data Summary Forms
              can be  done on a spreadsheet program.   Blank Data
              Summary Forms for both aqueous and  solid samples are
              included in Attachment E.

3.2.3    Appendix C	- Results as Reported bv  toe Laboratory for
         all Target Compounds

         After the  title page, Appendix C contains photocopies of
         all of the Form Is.  The Form Zs for all samples for the
         volatile organica  fraction are included first, followed
         by Form  Is  for all  samples  for  semivolatile  organic
         compounds  and pesticides/PCBs.   The  sample order of the
         Form Zs should  match the sample order  as  listed on the
         Data Summary Forms.

3.2.4    Appendix  P  ~   Reviewed   and  Accepted   ICorrectedI
         Tentatively  Identified Compounds

         Appendix  D  contains  photocopies  of  the  Tentatively
         Identified Compounds forms (Form I VOA  - TIC and Form I
         SV - TIC) for each  sample,  with all volatile organics
         forms preceding ail  semivolatiie  organics  forms.   If
         corrections  to the TIC forms are made during validation,
         use the word "corrected* in the appendix title.  All TIC
         forms are included even if no TICs were identified by the
         laboratory.

3.2.5    Appendix F — Support Documentation

         Appendix. F for  the organic data review report includes
         all support documentation needed to substantiate  the
         findings described in the narrative.   In addition  to
         copies  of   specific  supporting  forms  from  the  data
         package, the appendix will includes

         3.2.5.1 Table   I,    "Calibration    Outliers",   is   a
                 compilation  of   all   Response   Factors  (RFs),
                 percent Relative  Standard Deviations  (%RSDs),
                 and percent Differences  (%Ds) which were outside
                 of  the  control  limits  for  both volatile  and
                 semivolatile organic  compounds.   Examples  of
                 Table I are included in Attachment F.   Table I
                 also includes  the  qualifiers  applied  during
                 validation to compound results  because of these
                 outliers,  and the definitions  of  the qualifier
                 codes used.

         3.2.5.2 Initial and  continuing calibration  data  are
                 included  for  all volatile and  semivolatile
                 compounds  (Forms VI VGA, VII VOA,  VI  SV-1 and -
                 2, and VII SV-1 and -2), with a  reviewer-written
                 list of samples  affected by  each calibration.

         3.2.5.3 Copies  of  the  laboratory case narrative, sample
                 traffic report/chain of custody  (TR/COC),  and
                 EPA  Shipping Log.

-------
                                                                    Appendix B
                                                                   Page 5 of 5
          *itiftHliiici tiic Report
       The organic report shall be assembled in the order presented in Sections
       3.1  and  3.2  of  this  document.    The  narrative  is  followed  by the
       Appendices as described.

5.0    Review and Distribution

       After  the report  is completed  and assembled,  it  should be reviewed
       internally by optional peer review(s), oversight chemist review(s), and
       team manager review.

       5.1    The report should be submitted to a senior oversight chemist for
              its first  internal  review.   The internal review may be assigned
              to another validator or be performed by the oversight chemist.

              5.-1.1    The reviewer will review the document.  Any deficiencies,
                       inconsistencies,  or  other comments should be returned to
                       the validator.

              5.1.2    The reviewer will return the review to the validator, who
                       will make the required corrections.

              5.1.3    The process will  continue (Steps 5.1 - 5.1.2)  until the
                       document requires no further revision.

              5.1.4    The  validator  will  initial  the  first  page  of  the
                       narrative next  to his/her name.

              5.1.5    The final review is performed by the  team manager, who
                       will read  and  review the document.   If the  report is
                       acceptable to  the  team  manager,  he  will initial the
                       narrative next  to his name.

       5.2    The completed report is submitted .to the EPA oversight chemist for
              review.

              5.2.1    All  internal review  checklists are removed, and the rest
                       of  the document is" copied for  the validator files.  The
                       internal review checklists and  document copy  are then
                       placed in a filing area.

              5.2.2    The   original, document  is  placed  in  an  inter-office
                       envelope addressed to the EPA  RPM.

       5.3    Upon completion  of  review  by  the  EPA  oversight  chemist,  the
              document will either be approved  as submitted  or revisions will
              be required.

              5.3.1    If revisions  are  required by the EPA oversight chemist,
                       the  validator must complete those revisions and submit
                       the   document  for internal review  as  outlined  above
                       beginning in  section 5.1.

                       5.3.1.1  All resubmissions are  labelled as revision  1 (or
                               subsequent).

-------

-------
                             ATTACHMENT A
     Qraanics
     Water  ftta/Ll
Chemical Tan Dav Health Advisory List

                     Metals
                     Water fticr/Ll

                     Arsenic
                     Cadmium
                     Chromium
                     Lead
                     Nickel

                     Soil fppml

                     Lead


                     Inorganics

                     Nitrate



                     Nitrite



                     Cyanide
     Acrylamide                 300
     Alachior                 15000
     Aldicarb                    12
     Benzene                    233
     Carbofuran,                 50
     Carbon Tetrachloride       160
     Chlordane                   63
     Chlorobenzene             1800
     2,4-D                      300
     DBCP                        50
     1,3-diclilorobenzene       8930
     1,4-dichlorobenzene      10700
     1,2-dichloroethane         740
     1,1-dichloroethylene      1000
     cis-1,2-dichloroethylene  1000
     trans-i,2-dichloroethylene2720
     D i chloromethane           1500
     1,2-dichloropropane         9 0
     p-Dioxane                  568
     Dioxin                 1 x 10**
     EDB                          8
     Endrin                       5
     Epichlorohydrin            140
     Ethylbenzene              2100
     Ethylene glycol           5500
     Heptacblor                  10
     Hexachlorobenzene           50
     n-Hexane                  4000
     Lindane                   1200
     Methoxychlor              2000
     Methyl ethyl ketone
         (2-butanone)          7500
     Oxamyl                     350
     Pentachlorophenol          300
     Styrene                  200OO
     Tetrachloroethylene      34000
     Toluene                   6000
     Toxaphene                   80
     2,4,5-TP (Silvex)          200
     1,1,1-trichloroethane    35000
     Vinyl chloride            2600
     Xylenes                   7800
     PCB                   hundreds
              50
               8
            1400
              20
            1000
             500
 10 mg/L - 4 kg
111 mg/L - other
  1 mg/L - 1 kg
 11 mg/L - other
        220
RD0073A23.LIS

-------

-------
                           ATTACHMENT B
            GLOSSARY OF DATA QUALIFIER CODES  (ORGANIC)


CODES  KBtfATED TO IDENTIFICATION
      (confidence concerning presence  or absence of compounds)

          U =  Not  detected.    The  associated  number  indicates
                approximate sample concentration necessary to be
                detected.

          HO CODE - Confirmed identification.

          B «  Not detected substantially above the level reported
                in laboratory or field blanks.

          R -  Unusable result.  Analyte may or may not be  present
                in the sample.
                                        t
          N B  Tentative   identification.     Consider  present.
                Special methods  may  be  needed  to  conform  its
                presence or absence in  future sampling  efforts.


CODES  RELATED TO OUANTITATION
     (can be used for both positive results and sample quantitation
limits):

          3 =  Analyte present.    Reported  value  may  not  be
                accurate or precise.

          K =  Analyte present.   Reported value may be  biased
                high.   Actual  value is  expected to be lower.

          L «  Analyte present.  Reported value may be  biased low.
                Actual value is expected to be higher.

          UJ = Not detected.  Quantitation limit may be inaccurate
                or imprecise.

          UL = Not detected.    Quantitation  limit  is  probably
                higher.
OTHER CODES
          NJ • Qualitative identification questionable due to poor
               resolution.   Presumptively present at approximate
               quantity.

          Q -  No analytical result.

-------

-------
   Attachment C



Data Summary Forms

-------

-------
                                                                    DATA SUMMARY FORM:    VOLATILES   1
                                                                                                                             Page
of
Site Na

Case i:
                                                              HATER  SAMPLES
                                                                 Cug/L)
Sampling  Oate(s):
                                                                                                                                        To calculate sample quant)tat Ion UralIB:
                                                                                                                                                       (CROL * Dilution Factor)



CRQL
to_
10
19
10
10
10
10
10
10
10
!0_
1
-------

-------
                                                                   DATA SUMMARY FORK;   VOLATILES   2
                                                                                                                                                 Page
                                                                                                                                            of
Site Na

Cut f:
                                                              WATER  SAMPLES
                                                                 (ug/0
Sampling  Date(s):
                                                                                                                                      To calculate aanple quant Station Knits:
                                                                                                                                                      (CRDL * Dilution Factor)



OWL
10
10
10
10
10
10
10
10
10.
10
10
10
10
10
10
10
10







Sanple No.
Dilution Factor
Location
COMPOUND
•1 ,2-Dichlorowooar*
CU-1 .3-Dlchloroprooene
Trlchloroethene
Dlbromochloroawthana
1 .1 .2-Tridiloroctharw
*B«nzerM
Trana-1 .3-01 dildropropana
Brooofom
4-Rathvl -2-Dantanoiw
2-Mcxanofw
*Tetrachloroethene
1.1.2.2-Tatrachloro*than«
*Toluene
*Chlorobenzene
•Ethvlbanzana
•Stvrene
•Total XvlenM
,
.

























































































































































































































































































_






















































































































.












































































































CROL • Contract Required Quantitatloti Halt
                                                    •Action Level Exlata
                                                                                                                        SEE NARRATIVE FOR CODE DEFINITIONS
                                                                                                                                            revised 07/90

-------

-------
                                                                   DATA SUMMARY  FORM:   VOLATILES   1
                                                                                                                                                Page
                                                                                                                                           of
Sit* Ha

Cat* f:
                                                              SOIL SAMPLES
                                                                (ug/Kg)
SanpUng  Date(»):
                                                                                                                                     To calculate swiple quantitatIon Units:
                                                                                                                             (CRQL  * Dilution factor / ((100 • X*o«Bture)/100)




CRQL
W_
18
10
to
10
10
16
10
10
10
10
18
10
M-
10
10








Sanple »0.
Dilution Factor
X Moisture
Location
COMPOUND
Chlorenethane
Brojwmethan*
Vlnvl Chloride
Chloroethane
ttethvlana Chloride
Acetone;
Carbon Oitutf Ida
1.1-Dichtoro*thane
1.1-Dlchtoroethane
Total 1.2-Dichloro«thene
Chloroforv
1.2-Oidiloroethen*
2-ftutenone
1.1.1-THdilarMthane
Carbon Tetrachloride
Bronodlchloromethane









































.




























mmmmmmmmmmm
.-••••••••I























.














































































































































. .


























































































































mmmmmmmmmmn
•........-•






















































































.___
"•"
































,


















I





























 CRQL  •  Contract Required Ouantitation Linit
                                                                                                                       SEE NARRATIVE FOR CODE DEFINITIONS
                                                                                                                                           revised 07/90

-------

-------
                                                                    DATA SUMMARY  FORM:   VOLATILES    2
                                                                                                                                                  Pag*
                                                                                                                                   of
Site Da

Case f:
                                                     SOIL SAMPLES
                                                       (ug/Kg)
Date(s):
                                                                                                                                       To calculate sanple quantltatlon limits:
                                                                                                                               (CROL * Dilution factor / ((100 - XMolsture)/100)




CRQL
to
10
10
10
10
10
10
10
10
10
_ WL
w_
10_
10_
10_
10_
10







Sanple No.
Dilution Factor
% Moisture
Location
COMPOUND
1.2-Dichloroorooene
Cfa-LS-Dlcfiloropfopene
Trtehloroetltem
Dfbrooochlon*«thar»«
I.I.Z-THchlerocthaiM
ianzerw
Trana- 1 , 3-DlcMoropropene
Broaofona
4-Mathvl -Z-oentanoiM
2-N«xanon«
Tetrachloroethane
1 f 1.Zf 2-T«trachloro«th«n»
Toluene
Chlorobenzene
Ethvlbanz«ne
Stvr«M
Total Xvlanea
B

























































































.






































'•














-













1-







































































































































































































































































L


































































.







































CROL • Contract Required Quantltatien Llalt
                                                                                                               SEE NARRATIVE FOR CODE DEFINITIONS
                                                                                                                                   revised 07/90

-------

-------
                                                                        DATA SUMARV FORM:   B N A
                                                                                                                                                 Page
                                                                                                                                            of
Sit* Ha

Cam f:
                                                            WATER  SAMPLES
                                                                (ug/L)
Sampling  Date(s):
                                                                                                                                       To calculate sample quantitation limits:
                                                                                                                                                      (CRDL * Dilution Factor)



CRQL
10
10_
16
10_
10
10
10
10
10
10
10
10
10
10
10
«L
10
10
10
10




Saapl* No.
Dilution Factor
Location
COMPOUND
Phenol
bl •(2-Ch I oroethvl lather
• 2-Chloroohenol
•1.3-Dicnlorabenzene
•1,4-Dichloroberuene
1.2-Diehlorobenzene
2-Hethvluhenol
2.2'-oxvblt<1-ehloropropene)
4-Hethvlrtienol
N-Nltrmo-dl -n-woovlamine
Hexactiloroathana
Nitrobenzene
Ivochororw
2-HttroDhenol
2,*-D««ethvloher»l
biB(2-Chtoroethoxv)«ethar»
2.4-Dlchlorochenol
1.2.4-Trichlorobenzene
HeDhthalene
4-ChloroaniUne


























































































































I-

































































































































































































































































































































































































CRQL • Contract Required Aiantltatlon Limit
                                                    •Action Level ExUt«
                                                                                                                        SEE NARRATIVE FOR CODE DEFINITIONS
                                                                                                                                            revised 07/90

-------

-------
                                                                        DATA SUMMARY FORM:   I N A
Sit* Name:

Case *:
                                                            MATER  SAMPLES
                                                                (Ufl/L)
Sanpllna  Date(s):
                                                                                                                                       To calculate taspte quant I tat ion Units:
                                                                                                                                                      (CRDL * DIHjtton Factor)



CRQL
10
10
10
10
10
25
11« No.
OJlutJon Factor
Location
COMPOUND
Hwtaditorobutadtan*
4-Chloro-3-«Bthvloh«nol
2-NcthvtnaehthalWMi
Hax*chlorocyclop«ntadf«nt
2.4.6-Trlchloroch«nol
2.4.5-Tr«chlorooh«nol
2-CtiloronaDthatene
2-NitroanUfrw
DlMthyletttlulate
Acenaehthvltn«
2.6-Dlnltrotoluam
S-Nitrewi(ltrw
Acmwiithcne
2.4-Dtnitroohcnol
*-Nltroohenol
Otbeniofuran
2.4-Olnltrotolueoe
Diathvlphthalata
4-Chloroc*«nyl-i*enYl«th«r
Fluorww
4-N1trotnlllm
4.6-01nltro-2-nethylp»i«K)t


























































































































































































































































































































































































































































































































(SOL • Contract Required Quantltatlon
                                                    •Action l*v*l Ixltta
                                                                                                                         SEE NARRATIVE FOR CODE DEFINITIONS
                                                                                                                                            revised 07/90

-------

-------
                                                                        DATA SUMMARY FORM:   SNA
                                                                                                                                                  Page
                                                                                                                                            of
Site Name:

Case f:
                                                            WATER  SAMPLES
                                                                (ug/L)
Sampling  Date(t):
                                                                                                                                       To calculate sanple quantltatlon  limits:
                                                                                                                                                       (CRDL * Option  Factor)



CftQL
10
10
10
25.
1
-------

-------
                                                                         DATA SUWARV  FORM:    IMA
                                                                                                                                                    Pag*
                                                                                                                                                                     of
Sit* Mane:

Case «:
                                                                                   SOIL    SAMPLES
                                                                                       (ug/Kg>
                     Sampling  Dat«(s):
                                                                                                                                         To calculate tangle quantltatlon Units:
                                                                                                                                (CRQL * Dilution factor / ((100 - Xn»lsture)/100)
 CRQL

 .330.
 530.
 330_
 330.
 330_
 .330.
 .330.
 .330.
 330.
 .330.
 330.
 .330.
 .330.
 .338.
 .330.
 .330.
 .330.
 .330.
 .330.
  330
Sanpla No.
Dilution Factor
X Moisture
Location
COMPOUND
Phanot
blt(2-Ch loroathvl )»th«r
2-Chloroeh*nol
1 .3-Dlchlorobenz«n*
1 ,4-0 Idilorobenzarw
! .2-0 Ichlorobanzane
2-Methylrfwnol
2r2'-oxvbli(1-chloropropan«)
4-H«thvloh«x>l
N-i 1 trosa-df -n-0ropy la»l na
Ncxachloroetharw
nitrobenzene
IcoDhoron*
2-Mltroohenol
2.4-0 iMttwlehanol
bla(2-ailefoathoxy)Mthana
2.4-Dlchloroohenol
t .2.4-Tr Ichlorobanzena
Nachthalene
4-Chloroanlllne
















































































































'











___________
...........
































































































































































































































































































'















































































































CRQL • Contract Required Quant I tatIon Limit
                                                                                                                                                 SEE NARRATIVE FOR CODE DEFINITIONS
                                                                                                                                                                     revised 07/90

-------

-------
                                                                        DATA SUMMARY  FORM:   SNA
                                                                                                                                                  Pas*
                                                                                                                                            of
Site Name:

Case •:
                                                             SOIL   SAMPLES
                                                                Cug/Kg)
Sampling  Date(«):
                                                                                                                                       To calculate sample quantI tatIon limits:
                                                                                                                              (CRQL * Dilution factor / ((100 - X«»l8ture>/100)




OWL
330
.330
330
330
330
800
330
800
330
330
JS30
MO
330
800
800
330
330
330
330
330
BOO
800


Sarnpla Ho.
Dilution Factor
% Mofaturt
Location
COMPOUND
Haxachlorofautadlana
*-Chloro-3-nethytDhtnol
2-H«thylnaohthalene
Haxachlorocvclooentadltna
2.4.4-Trlchlorochenol
2.*.5-Trlchloroohenol
2-Chtoronanthalen*
2-Nltremlllm
DlwathvlDhthalata
Acanachthvlene
2.6-BlnltratoluaM
3-Kltroantltne
|' Aetntohthmt
| 2>-D1n1tr«*anol
i-Nltroohenol
Olbamofuran
2,4»DlnttrototiMrw
Dlathylphthalat*
4-ChlorophenYl-ph*ftylathar
Fluorana
4-MltroaflUlM
4.6-D1n1tro-2-«athylphanol






























































































































.





























































































































































































-

































-













































































































































































 CROl  • Contract Raqulred Quantltatlon Llilt
                                                                                                                         SEE NARRATIVE FOR CODE DEFINITIONS
                                                                                                                                             revUed 07/90

-------

-------
                                                                        DATA SUMMARY FORM:   B N A
                                                                                                                                                 Page
                                                                                                                                            of
Sit* Dane:

CM* f;
                                                             SOIL   SAMPLES
                                                                (ug/Kg)
Sampling  Date(s):
                                                                                                                                      To calculate senple quantitation Halts:
                                                                                                                              (CRttL • Dilution factor / ((100 - Xmolature)/100)




CROL
330
330
330
800
330
330
330
330
.330
330
330
330
330
330
330
330
330
330
330
330
330
330


Staple lo.
Dilution Factor
X Motatura
Location
COMPOUND
N-Nitroaodfeh*nylanfne
4-Brofflcehenyl-phenylether
Hexachloroberuene
Pentachloroohenol
Phenenthrene
Anttiracana
Carfaezole
Dl -n-butvichtlialat*
FlueranthwM
Pvrafw
ButvlbenzvlDhthalat*
3.3'-i>fchlorobenzidinc
Benzo(a)anthracena
Chrvsane
bf t(Z-Ethvlhexvl )phthalat*
Dl-n-octvluhthalate
Bamofblf luorantKena
Benzo( k) f luoranthana
Benzo(a)Bvr«n«
Indeno(1.2.3-cd)Dvrefw
Dfb«nz(a.h)anthracene
Beftto(g.h.l)D*rvl«n«







































































































































































































•






































mmmmmmmmmmm
mmmmmmmmmmm




































































-



































































































1









































































































1










 CROL » Contract Required Quantttatlon Limit
                                                                                                                        SEE NARRATIVE FOR COD! DEFINITIONS
                                                                                                                                            revised 07/90

-------

-------
                                                         DATA SUMMARY FORM:   PESTICIDES    AND    P C • S
                                                                                                                                              Pag*
                                                                                                                                         of
Sit* Nam:

     f:
                                                             HATER  SAMPLES
                                                                (ug/U
Sampling  Date(s):
To calculate sample quant I tat ion Units;
               (CftDl * Dilution Factor)
Sanpla Ho,
Dilution Factor
Location
CRQL COMPOUND
0.05| elcht-BHC
0.05 ( bita-BHC
0.05 | etelta-iKC
0.05) *oanwa-IKC (lindana)
0.05) " *Naetachlor
0.05 | Aldrln
0.05 1 Hwtachlor EooKida
0.05) Endoauifan I
0.10) Dtaldrln
0.10) 4.4'-DDi
0.10| *Endrin
0.10) Endoauifan 11
0.10) 4,4'-DDO
0.10J Endoauifan Sulfata
0.10| *.4'-DOT
0.50 | *N*thQXvehlor
0.10| Endrin Ketooe
0.10| Endrin Aldehyde
0.05) *aloha-Chlord«ne
0.05 1 *gaBwa-Chlortten*
5.0 *Toxaphan*
1.0 *Aroclor-1016
2.0 *Aroclor-1221
.0 *Aroelor-lS2
.0 *Aroclor-1Z42
.0 *Aroeler-tZ48
.0 *Aroelor-1S4
.0 *Aroclor-1260
CROL * Contract l*quir*d Quantitatton Lli
































•it




































•••••••••_•
mmmmmmmmmm,




















V





.

























...









































•Action I








^























lava






























'

I Exiata






































































































































































































































SEE
































NARRATIVE
































FOR (
*t































3»E DEFIKll
































nous
                                                                                                                                                              revised 07/90

-------

-------
                                                          DATA SUWARY  FORK:   PESTICIDES    AND    P C i S
                                                                                                                                                Page
                                                                                                                                          of
Sit* NBIWJ

CMC f:
                                                             SOIL  SAMPLES
                                                               (ug/Kg)
Sanpling  Date(s):
         To calculate sanple quant i tat I on Units:
(CRQL * Dilution factor / ((100 - Xmoistup*)/100)




CRQL
1.7
1.7
1.7
1.7
J-7_
1.7
J«7_
1.7
3.3
3.3
3.3
.3.3.
_3.3.
3.3
_3'3L
17
3.3
3.3
1.7
1.7
170
33
67
33
33
33
33
33
CSQL •
Sample No.
Dilution Factor
X MoUtura
Location
COHPOUNO
aloha-BHC
b«ta-BHC
delta-BHC
ganna-BHC (Llndant)
Heotachlor
Aldrln
Heotachlor Eooxlde
EndoMjlfan I
Dleldrin
4.*'-DOE
Endrin
EndOMJlfan II
4.4' -DOB
Endoaulfan Sulfate
4.4' -DOT
Nethoxvchler
Endrfn Katone
Endrln Aldehyde
alpha-Chlordane
ganiM- Ch I ordana
Toxachen*
Aroclor-1016
Aroeler-1H1
Aroclor-1232
Aroclor-1242
Aroclor-1248
Aroclor-1254
Aroclor-1260
Contract Raquirad Quant Itatl on Lit

































•It






































mmmmmmmmmmm



































































mm*mmmmmmmt



































































.

















,

















































_-_„,_--„.. 	






































































































































































































SEE

































NARRATIVE 1

































r« 1
^













•


















DODE DEFINI1

































news
                                                                                                                                                                revised 07/90

-------

-------
Attachment D



  Table  I

-------

-------
                                      TABLE I
                                                Page	of
 .CASE/SAS No..
 ENVIRONMENTAL PROTECTION AGENCY REGION III
            CALIBRATION OUTLIERS
           VOLATILE HSL COMPOimDS
	CONTRACTOR 	
| Instrument* Unit. Cal. Cont. Cal.
! DATE /TIME: I
1 SRF %RSD * RF !%D *
! Chlorome thane ! '
f Bromomethane ! !
Vinvl Chloride ! !
Chloroethane ! i
Methvlene Chloride i
Acetone !
Carbon Dieulfide 1 ! ! !
1,1-Dichloroethene ! ! ! !
1,1-Dichloroethane ! ! If ! !
Total-1.2-Dichloroethene ! ! ! ! ! !
Chloroform \ ! ! ! !
1,2-Dichloroethane I : ! ! !
2-Butanone ! ! \ [ ! !
1.1.1-Trichloroethane !!!!!!
Carbon Tetrachloride i ! !
Bromodichlororaethane ! ! ! ! ! !
1,2-DichlorooroDane ! ! ! ! !
cis-1, 3-DichloroDrooene ! ! 1
Trichloroethene ! !
Dibromochloromethane t !
1. 1,2-Trichloroethane ! !
Benzene ! 1 i
trana-1 . 3-DichloroDrooene !!;!!!
Bromoform ! ! ! !
4-Methvl-2-Pentanone ! ! ! ! !
2-Hexanone ! ! ! ! !
Tetrachloroethene ! ! ! ! !
I 1,1.2.2-Tetrachloroethane ! ! ! !
! Toluene ! ! !
Chlorobenzene f ! ! ! !
Ethvlbenzene ! !
Stvrene ! j
Total Xvlenes 1 ! f ! !
i i
•
AFFECTED j
SAMPLES: ! !
! Cont .
!
!RF
!
i
|
J
[


i
i

!





















1
i



Cal. !
{
%D f * !
i i
J j
j j
i ^
i i
i i
i i
i i
i t i

I 1 1
I j j
j J
i i
j j
j [
j j
i i
i i
j j
t i
j !
• j
!
1
I
! i
i i
i i
i i

i i
t i
1 1
|
1 !
j
i
i
Reviewer
Initials/Date:.
* See last pace of this table for DEFINITION OF CODES.

-------

-------
  CASE/SAS No..
                TABLE I

 ENVIRONMENTAL PROTECTION AGENCY REGION III
            CALIBRATION OUTLIERS
 SEMIVOLATILE  HSL COMPOUND 'Part 1  of  2}
	CONTRACTOR 	
                                                                      Page	of
Instrument/
DATE /TIMEs

Phenol
bis r 2-Chloroethvl lether
2-Chloroohenol
1 , 3-Dichlorobenzene
1 . 4-Dichlorobenzene
1 , 2-Dichloroben rene
2-MethYlpherjol
bie(2-ChloroiBODroDvl 1 ether
4-Methvluhenol
N-Nitroso-di-n-DroDvlamine
Hexachloroethane
Nitrobenzene
Isoohorone
2-NitroDhenol
2 . 4— Dimethvlohenol
! bis f2-Chloroethoxv> methane
1 2 .4-Dichloroohenol
1. 2 . 4-Trichlorobenzene
Naohthalene
4-Chloroan i 1 ine
Hexach lorobut ad iene
4-Ch loro-3-Met hv iDheno 1
! 2-Methvlnachthalene
Hexachlorocvclooentadiene
2.4. 6-Trichloroohenol
2,4. 5-TrichloroDhenol
2-Chl oronaoht ha Iene
! 2-Nitroaniline
DimethvlDhthalate
! Acenachthvlene
I 2 . 6-Dinitrotoluene
1 3-NitroanM.ine
Acenaohthene
2 . 4-DinitrophenoJ.
4-Nitrot>henol

AFFECTED
SAMPLES:

le viewer j
nitiala/Date:




llnit
j
!RF
i
J
!
I
i
i
i
*
j
i


•
|
j
!
i
i



}
!
!


t
t







\










. Cal.

!%RSD
I
J
!
i
t
!
•
j
i
I
\



i
i
i
i



























ICont. Cal. ICont. Cal. 'Cont. Cal.
[ ! j
! * ! RF %D ! * ! RF ! %D ! * ! RF ! %D *
it iii iii
! ! ! ! ! ! !
ii iii ii
I ! ! ! ! ! i J
ii iii iii
iii iii iii
iii iji iii
iii iii iii
• ' t 1 ' ' i . t i
1 j 1 1 1 1 1 1 1
II 1 'II 1 II 1
III III III
II III III
! ! ! ! ! ! ! ! ! - |
i i i i i i i i
i iii iii
! 5 ! ! ! J
. ! ! ! ! ! ! i
it i i i i
j i ii iii
(ill ! !

! ! i ! i !. ! i
i iii iii i
• j i j j !S 1 J
ij j j i ! ! ! ! !
ii i j i | i j
i i i i i
1 ' i ! !
it ii
I !
1 ! ! !
i ii i i
i iii iii i
! ! ! ! ! ! !
! } ! i ! ! !
! ! ! ! III!
J >
i i i
! !
i i
i ! i

i

i
	 - - "

* See last page of this tablefor DEFINITION OF CODES.

-------

-------
                                      TABLE I
Page   of
                       ENVIRONMENTAL PROTECTION AGENCY REGION III
                                  CALIBRATION OUTLIERS
                       SEHIVOLATILE HSL COMPOUNDS (Part 2 Of 2)
j Instrument/ flnit. Cal.
1 DATE/TIMEt
i
t
Cont
« Cal. Icont. Cal*
1
|RF SiRSD !* RF
_i_ Dibenzofuran !
2,4-Dtnitrotoluen0 !
Diethylphthalate !
4-Chloronhenvl-ofienvlether !
Fluorene !
4-Nitroaniline !
4 , 6-Dinitra-2-methvlohenol !
N-Nitroaodiphenvlamine !
4-BromoBhenvl-ohenvlefcher 1
Hexachlorobenzene !
Pentachlorophenol !
Phenanthrene !
Anthracene

Carbazole
Oi— n-butvlohthalate !
Fluoranthene !
Pvrene

Butvlbenzylphthalate !
3 , 3 ' -Dichlorobenzidine !
Benzof a) anthracene !
Chrvaene

bis ( 2-ethvlhexvl 1 phtha late


L Di-n-octvlchthalate 1
Beqzo ( b \ f luorant hene
Benzo ( k ) f luorant hene


Benzo f a 1 uvrene !
Indeno (1.2,
Dibenzfa.h]
Benzofa.h, :


, 3-cdlovrene j
anthracene !
. loervlene




f%0 » RF !%D
i
! !
! !
|


























t
!
j
|
!
i






t
j
i
J
i

I
I \

!
! !






i
4 j
1
[
J
!
i
i i
j
!
J

S
AFFECTED

















t
i
!
s
{
t
i
i
!
i
i
i
i
<
t
j
i
' j


»
i
i i
*




















i i i
L i

! 1 !
i < i

I i
i i i
| ' !
j


j
i



iii i
1
i
i
SAMPLES! ! !
Reviewer
[nitiala/Datc


** -- _,,„,

j
j

j


i i







\
Cont. Cal.

RF S%D * i
i
j
j
j
j
{
\
j
!
i
i
j
! _j
i
p

s
i
i
i
i
i
i
!
j
j
1
j
i
f



J

t
i
i i
J 1
I ! !
1 11






] [
i i
J
!
j j
i j
! t

1
i
j
i
i
i
i


* See last pace ofthis table for DEFINITION OF CODES.

-------

-------
                                             Page 	  of
          DEFINITION OF CODES USED IN TABLE I
%RSD exceeded 30% in the initial calibration, positive
results are qualified "J".  When the %RSD exceeded 50%,
quantitation limits are qualified "UJ",

%D exceeded 25% .in the continuing calibration, positive
results are qualified "J".  When the %D exceeded 50%,
quantitation limits are qualified "UJ",

RF less than 0.05 in the calibration.  All quantitation
limits are qualified "R" and positive results are qualified
ML".

The "B" qualifier, denoting blank contamination, supersedes
the qualifier issued in this table.

The "R" qualifier, denoting unusable results, supersedes the
qualifier issued in this table.

-------

-------
                                                  Region 01 Modifications
                 APPENDIX C




CONTRACTUAL REQUIREMENT COMPARISON TABLES

-------

-------
                                                      Region m Modifications

                                                          APPENDIX C
Table C.I.  Comparison of Requirements for
           Volatile Data Review
REQUIREMENT
Target Compound List
Data Turnaround r
Technical Holding Time
Initial Calibration
Continuing Calibration
Blanks
SMC/Surrogates
MS/MSD
LCS
Regional QA/QC
Internal Standards
CRQL
ncs
MULTI-MEDIA
MULTI-CONCENTRATION
33 Target Compounds
35 days
7 days if not preserved
14 days if preserved
5 levels: 10 -200 ug/L
mid-level: SO ug/L
Method Blanks
Instrument Blanks
SMC:
1 ,2-Dichloroethane-
-------
                                                     Region ID Modification*

                                                          APPENDIX C
Table C.2.  Comparison of Requirements for
         SemivolatHe Data Review
REQUIREMENT
Target Compound List
Data Turnaround
Technical Holding Time
Initial Calibration
Continuing Calibration
Blanks
Surrogates
MS/MSD
LCS
Regional QA/QC
Internal Standards
CRQLs
TICs
MULTI-MEDIA,
MULTI-CONCENTRATION
64 Target Compounds
35 days
Extraction - 5 days
Analysis - 40 days after
extraction
5 levels: 20 - 160 ug/L
mid-level: SO ug/L
Method Blanks
Instrument Blanks
8 compounds
Frequency: 1 per 20 samples,
per matrix
N/A
PEs - variable
IS Area: -50% to + 100% 	
IS RT Shift: ±30 sec.
10 - 50 ppb (water)
330- 1700 ppb (low soU)
10,000 - 50,000 (med soil)
largest 20 2 10% of nearest IS
LOW CONCENTRATION
WATERS
60 Target Compounds
14 days '
Extraction - 5 days
Analysis - 40 days after
extraction
5 levels: varies
mid-level: varies
Method Blanks
Instrument Blanks
Storage Blanks
6 compounds
N/A
1 perSDG
PEs - 1 per SDG
- IS Area: - 50% to 100%
IS RT Shift: ±20 sec.
5 - 20 ug/L
largest 20 2 50% of nearest IS
                  C-2

-------
           APPENDIX D

      PROPOSED GUIDANCE TOR
TENTATIVELY IDENTIFIED COMPOUNDS
          (VOA AND SV)

-------

-------
                                                                               in Modific«tk>m

                                                                              APPENDIX D
     PROPOSED GUIDANCE TOR TENTATIVELY IDENTIFIED COMPOUNDS  (VGA)
A.    Review Items:   Form IVOA-TIC, chromatograms, library search printout and spectra for three
                       TIC candidates, and GC retention time data.

B.    Objective

       Chromatographic peaks in volatile analyses mat are not TCL compounds, system monitoring
       compounds, or internal standards are potential tentatively identified compounds (TICs) or library
       search compounds  (LCSs).  TICs  must be qualitatively identified by a library search of the
       National Institute  of Standards  and Technology  (MIST) mass spectral  library, and  the
       identifications assessed by the data  reviewer.

C.    Criteria

       For each sample, the laboratory must conduct a library search of the NIST mass spectral library
       and report the possible identity for the 10 largest volatile fraction peaks which are not surrogates,
       internal standards, or TCL compounds, but which have a peak  area greater man 40 percent of
       the peak area of the nearest internal standard.  TIC results are reported for each sample on the
       Organic Analysis Data Sheet (Form I VOA-TIC).

       Note:  Since the SOW revision of October 1986, the CLP does not allow the laboratory to report
              as tentatively identified  compounds any TCL compound which is properly reported in
              another  fraction.  (For example, late eluting volatile  TCL  compounds  must  not  be
              reported as  semivolatile TICs.)

D.    Evaluation

       1.   Guidelines for Tentative Identification are as follows:

            The interpretation of library search compounds (LSCs) is one of the aspects of data review
            which calls for the fullest exercise of professional judgement.  The reviewer must  be
            thoroughly familiar with the principles and practice of mass spectral interpretation and of
            gas chromatography.  Because the interpretation process is labor-intensive, it is important
            to document the process involved hi arriving at a tentative  identification.

            Worksheets for "Tentative Identification of Library Search Compounds" are provided in
            Appendix B for the volatile GC/MS fractions to assist in generating the information needed
            to make  a reasonable tentative identification of the LSCs.

            The process involved in  tentatively  identifying a library search compound may  be
            summarized as follows:

            a.   Identify all samples in the related group (Case, SAS or SDG) in which  the unknown
                compound occurs. Calculation of relative retention times (KIT) and comparison of
                RRT and mass spectral data across samples Is extremely helpful in identifying
                                           D-l

-------
                                                                           Region III Modification*

VGA                                                                          APPENDIX D
                unknowns that occur repeatedly in related samples.  Use one worksheet per unknown
                for all samples in which it OCCURS.

            b.   Inspect the library search spectrum retrieved for each unknown, to determine if detailed
                mass spectral interpretation is necessary. Often "A is obvious mat the correct match is
                among the spectra retrieved for the unknown from the several samples in which it is
                found. It may only be necessary to check the unknown's RRT versus a reference list
                of VOA  (generated under similar conditions and after  accounting for bias in the
                sample) to arrive at a satisfactory  tentative identification.   Some references are
                provided. If a reference RRT is  not available, men a comparison of the unknown's
                RRT or boiling point to the RRT  or boiling point of a closely related compound may
                also provide a .satisfactory tentative identification. Within a compound class, retention
                time increases with increasing boiling point.

            c.   In the event that serious ambiguity still exists after examining the library spectra and
                RRT data, a Ml mass spectral interpretation can narrow down the possibilities. While
                a full  discussion of manual  mass  spectral interpretation is beyond the scope of mis
                document, several key points may be mentioned as important objects:

                o    Determine a likely molecular weight (MW).   Depending on the unknown, the
                     MW may or may not be apparent due to the extent of fragmentation. The MW
                     of the retrieved library spectra, interpreted in light of The RRT, may be helpful
                     if the molecular ion  is not present

                o    Determine the isotope ratios (M+i)/M,  (M+2)/M, (M+4)/M, etc. (where M
                     is the molecular ion) and determine a short list of possible molecular formulas.
                    Isotope ratios will also reveal the presence of S, Cl, and Br.

                o    Calculate the total  number of rings-plus-double-bonds in the unknown by
                     applying the following equation to the likely molecular formulas, to determine
                    the degree of unsaturation.

                             Number of rings-plus-double bonds (r+db):

                            (r+db)  -c--    +     + l
                             where:       C = no. of carbons
                                          H — no. of hydrogens
                                          X = no. of halogens
                                          N = no. of nitrogen

                             Note:    oxygen and sulfur do not need to be accounted for.   An
                                     aromatic ring counts as four rings and double bonds.

                     Calculate the mass losses represented by major peaks in the unknown spectrum,
                     and relate these to the fragmentation of neutral moieties from the molecular ion
                     or otter daughter ions.
                                            D-2

-------
                                                                           Region III Modifkabom

VGA                                                                          APPENDIX D
                o    Using the information gathered on molecular weight, molecular formula, degree
                     of unsaturation, and mass losses  in the unknown spectrum, combined whh the
                     RRT data, give as precise a description of the unknown as possible, including an
                     exact identification if it is justified.

            d.   In the event mat the unknown spectrum is not that of a pure compound, mass spectral
                interpretation may not be possible.  However, in some instances, a mixed spectrum
                may be recognized as two compounds having very similar relative retention times.
                Target compounds, surrogates and internal standards may also be responsible for extra
                ions in an unknown spectrum.

       2,   Check the raw data to verify that th& laboratory has generated a library search spectrum for
            all required peaks  in the chromatograms for samples and blanks.

       3.   Blank chromatograms should be examined to verify that the TIC peaks present in samples
            are not found in blanks. When a low-level non-TCL compound that is a common artifact
            or laboratory contaminant is detected in a sample, a thorough check of blank chromatograms
            may require looking for peaks which are less man 40 percent of the internal standard peak
            area or height,  but present in the blank chromatogram at similar relative mention time.

       4.   All mass spectra for every sample and blank must be examined.

       5.   The reviewer  should be aware of common laboratory artifacts/contaminants and their
            sources (e.g., aldol condensation products, solvent preservatives, and reagent contaminants).
            These may be present in blanks and not reported as sample TICs.

            Examples:

            a.   Common laboratory contaminants:  CO^m/z 44), siloxanes (m/z 73), diethyl ether,
                hexane,   certain   freons   (l,l,2-trichloro-l,2,2-trifluoroethane   or   fluoro-
                trichloromenthane), and phthatates at levels less man 100 ug/L or 4000 ug/Kg.

            b.   Solvent preservatives such as cyclohexene which is a methylene chloride preservative.
                Related   by-products   include   cydohexanone,  cyclohexenone,   cyclohexanol,
                cyclohexenol, chlorocyclohexene, and chlorocyclohexanol.

            c.   Aldol condensation reaction  products  of acetone  include:  4-hydroxy-4-metbyI-2-
                pentatone,  4-methyl-2-penten-2-one, and 5,5-dimethyl-2(5H)-furanone.

       6.    Occasionally, a TCL compound may be identified in the proper analytical fraction by non-
           target library search procedures, even though it was not found on the quantitation list. If
           the total area quantitation method was used, the reviewer should request that the laboratory
           recalculate the result using the proper quantitation ion.  In addition, the reviewer should
           evaluate  other  sample  chromatograms and  check library reference retention times  on
           quantitation lists to determine whether the false negative result is an isolated occurrence or
           whether additional  data may be affected.
                                            D-3

-------
                                                                          Region ID Modifications

VGA                                                                         APPENDIX D
       7.   TCL compounds may be identified in more than one fraction.  Verify that quantitation is
            made from the proper fraction.

       8.   Library searches should not be performed on internal standards or surrogates.

       9,   TIC concentration should be estimated assuming a RRF of 1.0.

E.     Action

       1.   All TIC results should be qualified as tentatively identified (N) with estimated concentrations
            g)or(NJ).

       2.   General actions related to the review of TIC results are as follows:

            a.   A non-TCL compound is not considered to be "tentatively identified" until the mass
                spectrum and retention time  data have been reviewed according to the evaluation
                guidelines in XD.D. The review should be documented on the Tentative Identification
                of Library Search Compound worksheet.  The worksheet will be useful if a better
                library match for the unknown is retrieved hi another Case, SAS, or SDG. It may also
                be used in  writing a Special Analytical Service Statement of Work to identify the
                unknown, or if the sample is sent to an EPA research laboratory LSC identification by
                multiple spectral techniques.

            b.   If all contractually required peaks  were  not  library  searched,  the  designated
                representative could request these data from the laboratory.

       3.    TIC results which are not sufficiently above the level in the blank should not be reported.
            (Dilutions and sample size must be taken into account when comparing the amounts present
            in blanks and samples.)

       4.    When a compound is not found in any blanks,  but is a suspected artifact or common
            laboratory contaminant, the result may be qualified as unusable (R).

       5.    The reviewer may elect to report all similar  isomers as a total.  (All alkanes may be
            summarized  and  reported as total hydrocarbons.)

       6.    The data reviewer should state the degree of confidence (high, medium, low) in the tentative
            identification after completing the review process.

       7.    The complete "Tentative Identification of Library Search Compound" worksheet should be
            attached to the final data review report
                                           D-4

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 VGA
                                                 R«gk>n in Modifmtkxu

                                                     APPENDIX D
                                        APPENDIX
Equation 1:
                                      RTunk - RTz
                                              - RTz
                                1002
                     where:  RTunk is the retention time of the unknown
                             RTz Is the retention time of the preceding retention index standards
                             RTz+1 is the retention time of the following retention index standard
                             Z = number of rings in the retention index standard
                             RI = Lee Retention Index
                            Retention Index Standards
                            naphthalene
                            pbenanthrene
                            chrysene
                            Benzo(g,h,i)
                             perylene
                        z-2
                        z-S
R]=200.00
RI=300.00
RI=400.00
RI-500.00
                        when these compounds are not found in the sample of interest, RT data for
                        die deuterated internal standards or most recent calibration may be used.
                        Retention time shifts and bias must be accounted for.
Equation 2:
                        Number of rings-plus-double-bonds (r+db):

                            (r+db)  - C - — -£ + ^*i
                                            222
                Note:
where:   C = no. of carbons
         H - no. of hydrogens
         X — no. of halogens
         N = no. of nitrogens

oxygen and sulfur do not need to be accounted for.  An aromatic ring counts
as four rings and double bonds.
                                           D-5

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                                                                        Region ffl Modifications

VGA                                                                       APPENDIX D


                                      REFERENCES

1.     Lee, MX. Vassilaros,  D.L.,  White.   C.mM., and Novotny,  M., "Retention Indices  for
       Programmed-Temperature Capillary-Column  Gas Chromatography  of Polycyclic Aromatic
       Hydorcarbons", Analytical Qieipistry. V.51, no. 6» 1919, pp. 768-T73.

2.     Rostad,  C.E.,  and Pereira,  W.E., "Kovats and Lee Retention  Indices  Determined  by Gas
       Chromatography/Mass Spectrometry for Organic Compounds of Environmental Interest*
       J, High Resolution Chrom. and Chromf Commun... vol.9,1986, pp. 328-334.

3.     Silverstein, R.M., Bassier, G.C., and Morrill, T.C.  Spectrometric Identification of Organic
       Compounds 4tn ed.. Wilev. New York,  1981.

4.     Vassilaros, D.M., Kong, R.C., Later, D.W. and Lee, MX,, :Linear Retention Index System for
       polyclyclic Aromatic Compounds.   Critical Evaluation and Additional  Indices".   |.  of
       Chromatographv. 252 (1982) pp. 1-20,
                                           D-6

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                                                                          Region in Modi
                                                                              APPENDIXD
      PROPOSED GUIDANCE FOR TENTATIVELY IDENTIFIED COMPOUNDS (SV)
 A.     Review Items:    Form ISV-TIC, chromatograms, library search printout and spectra for three
                         TIC candidates, and GC retention time data.

 B.     Objective

        Chromatographic peaks in semivolatile analyses that are not TCL compounds, surrogates, or
        internal standards  are  potential tentatively  identified compounds (TICs) or  library search
        compounds (LSCs).  TICs must be qualitatively identified by a library search of the National
        Institute of Standards and Technology (NIST) mass spectral  library, and the identifications
        assessed by the data reviewer.

 C.     Criteria

        For each sample, the laboratory must conduct a library search of the NIST mass spectral library
        and report the possible identity for the 20 largest semivolatile fraction  peaks  which are not
        surrogates, internal standards, or TCL compounds, but which have a peak area greater than 50
        percent of the peak area of the nearest  internal standard.  TIC results are reported .for each
        sample on the Organic Analysis Data Sheet (Form 1 SV-TIC).

        Note:    Since the SOW revision of October 1986, the CLP does not allow the laboratory to
                report  as tentatively identified  compounds any TCL compound which is properly
                reported in another fraction. (For example, late eluting volatile TCL compounds must
                not be reported as semivolatile TICs).

D.     Evaluation

        1.   Guidelines for Tentative Identification are as follows:

            The interpretation of library search compounds (LSCs) is one of the aspects of data review
            which calls for the fullest exercise of professional judgement.   The reviewer must be
            thoroughly familiar with the principles and practice of mass spectral interpretation and of
            gas chromatography. Because the interpretation process is labor-intensive, it is important
            to document the process involved in arriving at a tentative identification.

            Worksheets  for "Tentative Identification of Library  Search Compounds* are provided in
            Appendix B for the semivolatile GC/MS fractions to assist in generating the information
            needed to make a reasonable identification of the TICs.

            The process involved  in tentatively identifying a  library search compound may  be
            summarized as follows:

            a)  Identify all samples in the related group (Case,  SAS or SDG) in which the unknown
               compound occurs.  Calculation of retention indices (R) and comparison of RI and mass
               spectra across samples is extremely helpful in identifying unknowns that occur
                                            D-7

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                                                                           Region ID Modificationi

SV                                                                            APPENDED
                repeatedly in related samples.   Use one worksheet per unknown for all samples in
                which it occurs.  Retention indices are calculated according to the following example:
                           RI
                                                  - RTz

                where:   RTunk is the retention time of the unknown
                         RTz is the retention time of the proceeding retention index standard
                         RTz+ 1 is the retention time of the following retention index standard
                         Z = number of rings in the retention index standard
                         RI = Lee Retention Index

                         Retention Index Standards

                         naphthalene        z=2    RI= 200.00
                         phenanthrene      z=3    RI= 300.00
                         chrysene           z»4    RI =400.00
                         Benzo(g,h,i)       z=5    RI=500.00
                         perylene

                Note:    when these compounds are not dound in the sample of interest, RT data for
                         the deuterated  internal standards or most recent calibration may be used.
                         Retention tune shifts and bias must be accounted for.

           b)   Inspect the library search spectrum retrieved for each unknown, to determine if detailed
                mass spectral interpretation is necessary. Often, it is obvious mat the correct match
                is among the spectra retrieved for the unknown from the several samples in which it
                is found. It may only be necessary to check the unknown's RI versus a reference list
                of SV (generated under similar conditions and after accounting for bias in the sample)
                to arrive at a satisfactory tentative identification.  Some references are provided. If a
                reference RI is not available^ then a comparison of the" unknown's RI or boiling point
                to  the RI or boiling point of a  closely related compound  may  also   provide a
                satisfactory tentative identification. Within a compound class, retention time increases
                with increasing boiling point.

           c)   In the event mat serious ambiguity still exists after examining the library spectra and
                RI data, a full mass spectral interpretation can narrow down the possibilities. While
                a Ml discussion of manual mass spectral interpretation is beyond the scope of mis
                document, several key points may be mentioned as important objects:

                o    Determine a likely molecular weight. Depending on the unknown, the MW may
                     or may  not be apparent due to the extent of fragmentation.  The MW of the
                     retrieved library spectra,  interpreted in light of the RI, may be helpful  if the
                     molecular ion is not present.

                o    Determine the isotope ratios  (M+1)/M, (M+2)/M, (M+4)/M, etc.  (where M
                     is the molecular ion) and determine a short list of possible molecular formulas.
                     Isotope ratios will also reveal the presence of S, Cl, and Br.
                                            D-8

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                                                                           Repon IH ModificBtkiai

SV                                                                            APPENDIX D
                      Calcuiate the total number of rings-plus-double-bonds in die unknown by
                      applying the following equation to the likely molecular formulas, to determine
                      the degree of unsaturation.

                      Number of rings-plus-double-bonds (r+db):
                     where:  C = no. of carbons
                             H •= no. of hydrogens
                             X *= no. of halogens
                             N = no. of nitrogens

                     Ifote:   oxygen and sulfur do not need to be accounted for.  An aromatic ring
                             counts as four rings and double bonds.

                o    Calculate the mass losses represented by major peaks in die unknown spectrum,
                     and relate these to the fragmentation of neutral moieties from the molecular ion
                     or other daughter ions.

                o    Using the  information gathered on molecular weight, molecular formula, degree
                     of unsaturation, and mass losses in the unknown spectrum, combined with the RI
                     data, give as precise a description of the unknown as possible, including an exact
                     identification if it is justified.

            (d)  In ffie event that the unknown spectrum is not that of a pure compound, mass spectral
                interpretation may not be possible. However, in some instances, a mixed spectrum
                may be recognized  as two compounds having  very similar  retention  indices (for
                example, ortho-terphenyl, RI=317.43 and nonadecane, RI«=317.10).  This particular
                coelution would result in an unknown spectrum having a polycyclic aromatic pattern
                at m/z 230, the MW of terphenyl, with an hydrocarbon type pattern at m/z 43,57,71,
                etc. Target compounds, surrogates and internal standards may also be responsible for
                extra ions in an unknown spectrum, and may be treated similarly.

       2.    Check the raw data to verify mat the laboratory has generated a library search spectrum for
            all required peaks in die chromatograms for samples and blanks.

       3.    Blank chromatograms should be examined to verify mat TIC peaks present in samples are
            not found in blanks.  When a low-level non-TCL compound that is a common artifact or
            laboratory contaminant is detected in a sample, a thorough check of blank chromatograms
            may require looking for peaks which are less man 10 percent of the internal standard peak
            area or height, but present in the blank chromatogram at similar relative retention time.

       4.    All mass spectra for every sample and blank must be examined.
                                            D-9

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                                                                            Region m Modifications

 VS                                                                            APPENDIX D
        5.    The reviewer should be  aware of common  laboratory artifacts/contaminants  and their
             sources (e.g., aldol condensation products, solvent preservatives, and reagent contaminants).
             These may be present in blanks and not reported as sample TICs.

             Examples:

             a.   Common laboratory contaminants:  CO2 (m/z 44), siloxanes (m/z 73), diethyl ether,
                 hexane,   certain   freons   (l,l,2-trichloro-l,2,2-trifluoroethane   or   fluoro-
                 trichloromethane); and phthalates at levels less man 100 ug/L or 4000 ug/KG.

             b.   Solvent preservatives such as cyclohexene which is a methylene chloride preservative.
                 Related,  byproducts   include   cyclohexanone,   cyclohexenone,   cyclohexanol,
                 cyclohexenol, chlorocyclohexene, and chiorocyclohexanol.

             c.   Aldol condensation reaction products of acetone include:. 4-hydroxy-4-methyl-2-
                 pentatone, 4-methyl-2-penten-2-one, and 5,5-dimethyl-2(5H)-furanone.

        6.    Occasionally, a TCL compound may be identified in the proper analytical fraction by non-
             target library search procedures, even though "A was not found on the quantitation list. If
             the total area quantitation method was used, the reviewer should request mat the laboratory
             recalculate the result using the proper quantitation ion. In addition, the reviewer should
             evaluate  other  sample chromatograms and check  library reference  retention  times on
             quantitation lists to determine whether the false negative result is  an isolated occurrence or
             whether additional data may be affected.

        7.    TCL compounds may be identified in more than one fraction.  Verify that quantitation is
             made from the proper fraction.

        8.    Library searches should not be performed on internal standards or surrogates.

        9.    TIC concentration should be esthflaiedissuming a RRFDfl .0; ~ ~

£.      Action

        1.    Ail TIC results should be qualified as tentatively identified (N) with estimated concentrations
             (J)or(NJ).

        2.   General actions related to the review of TIC results are as follows:

            a.    A non-TCL compound is not considered to be "tentatively identified: until the mass
                 spectrum and  retention time data have been reviewed as per section Xffl D.  The
                 review  should be  documented on the Tentative Identification  of Library  Search
                 Compound worksheet. The worksheet will be useful  if a better library match for the
                 unknown is retrieved  in another Case, SAS, or SDG. It may also be used in writing
                 a Special Analytical Service Statement of Work to identify the unknown, or if the
                 sample  is sent to an EPA  research laboratory for LSC identification by multiple
                 spectral techniques.
                                             D-10

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                                                                            Regkm m Modificationi

VS                                                                             APPENDIX D
            b.  If  all contractually  required  peaks were not  library searched, die  designated
                representative could request these data from the laboratory.

       3.   TIC results which are not sufficiently above the level in die blank should not be reported.
            (Dilutions and sample size must be taken into account when comparing die amounts present
            in blanks and samples.)

       4.   When a compound is not found in any blanks, but is a suspected artifact or common
            laboratory contaminant, die result may be qualified as unusable (R).

       5.   Hie reviewer may elect to report all similar isomers as a total.   (All  alkanes may be
            summarized and reported as total hydrocarbons.)

       6.   Hie data reviewer should state die degree of confidence (high, medium, low) in die tentative
            identification after completing die review process.

       7.   The complete "Tentative Identification of Library Search Compound" worksheet should be
            attached to die final data review report.
                                            D-ll

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    APPENDIX E
GLOSSARY OF TERMS

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                                                                                            APPENDIX E
                                           GLOSSARY OF TEEMS

   APO          Administrative Project Officer
                                             %
   BFB          Bromofluorobenzene - volatile instrument perfonnance check compound

   BNA          Base/Neutral/Acid Compounds - compounds analyzed by semivolatile technique

   Case          A finite, usually predetermined number of samples collected over a given time period for a particular site,
                 A Case consists of one or more Sample Delivery Group(s).
                                                                            i
   CCS          Contract Compliance  Screening - process in which SMO inspects analytical data for  contractual
                 compliance and provides results to the Regions, laboratories and EMSL/LV.

   CF           Calibration Factor

   CRQL        Contract Required Quantitation Limit

   CSF          Complete SDG Ffle

   DFTPP       Decafluorotriphenylphosphine - semivolatile instrument performance check compound

   DPO          Deputy Project Officer

   EICP          Extracted Ion Current Profile

   GC/EC       Gas Chromatograph/Electron capture
                                     t
   GC/MS       Gas Chromatograph/Mass Spectrometer

   GPC          Gel Permeation Chromatography - A sample clean-up technique mat separates compounds by size and
                 molecular weight. Generally used to remove oily materials from sample extracts.

   IS            Internal Standards - Compounds added to every VOA and BNA standard, blank, matrix spike duplicate,
                 and sample extract at a known concentration, prior to instrumental analysis. Internal  standards are used
                 as the basis for quantitation of the target compounds.

   LCS          Laboratory Control Sample
t
   MS/MSD      Matrix Spike/Matrix Spike Duplicate

\  m/z           The ratio of mass (m) to charge (z) of ions measured by GC/MS

   OADS        Organic Analysis Data Sheet (Form I)

   ORDA        Organic Regional Data Assessment - from earlier version of the Functional Guidelines

   NIST          National Institute of Standards and Technology

   PCB          Polychlorinated biphenyl (Aroclor is a trademark)

                                                    E-l

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                                                                                      Region ID Modification*

GLOSSARY                                                                              APPENDIX E


PE           Performance Evaluation Sample

QA           Quality Assurance - Total program for assuring the reliability of data.

QC           Quality Control - Routine application of procedures for controlling die monitoring process.

RIC           Reconstructed Ion Chromatogram

RPD          Relative Percent Difference (between matrix spike and matrix spike duplicate)

RRF          Relative Response Factor

RRF          Average Relative Response Factor

RRT          Relative Retention Time (with relation to internal standard)

RSD          Relative Standard Deviation

RT           Retention Time

SDG          Sample Delivery Group - Defined by one of the following, whichever occurs first:

              *   Case of field samples

              *   Each 20 field samples within a Case

              *   Each 14-day calendar period during which field samples hi a Case are received, beginning with
                  receipt of the first sample in the SDG.  (For VOA contracts, the calendar period is 7-day).

SMC          System Monitoring Compound - formerly surrogates for volatile analysis.

SMO          Sample Management Office

SOP          Standard Operating Procedure

SOW          Statement of Work

SV           Semivolatile analysis - Method based on analysis by GC/MS for BNA organic compounds.

TCL          Target Compound List

TIC           Tentatively  Identified  Compound - A compound tentatively identified from search of the NIST mass
              spectral library that is not on the TCL.

TPO          Technical Project Officer                                                                    :

VOA          Volatile Organic Analysis - Method based on the purge and trap technique for organic compound analysis.

VTSR         Validated Time of Sample Receipt - Time of sample receipt at the laboratory as recorded on the shipper's
              delivery receipt and Sample Traffic Report.

                                                  E-2

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