United Stales         Office of
           Environmental Protection     Solid Waste and
           Agency            Emergency Response
           ^ *              » / r
                                           ., .
                                      December 1994
           Superfund
SEPA     LABORATORY DATA VALIDATION
            FUNCTIONAL GUIDELINES FOR
            EVALUATING ORGANICS
            ANALYSES
                  REPRODUCED BY
                  U.S. DEPARTMENT OF COMMERCE
                     NATIONAL TECHNICAL
                     INFORMATION SERVICE
                     SPRINGFIELD, VA 22161

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                                                                          9240.1-27
                                                                          PB95-963526
                                                                          EPA540/R-94/082
                                 LABORATORY DATA VALIDATION

                 FUNCTIONAL GUIDELINES FOR EVALUATING ORGANICS ANALYSES


                                           Prepared for the

                              HAZARDOUS SITE EVALUATION DIVISION
                            U.S. ENVIRONMENTAL PROTECTION AGENCY
                                            Compiled by

                                            Ruth Bleyler
                                      Sample Management Office
                                          Viar & Company
                                            Prepared by

                                 The USEPA Data Review Work Group
                                Scott Siders - EPA HQ - Co-Chairperson
                           Jeanne Hankins -  EPA Region III - Co-Chairperson
                                    Deborah Szaro - EPA Region I
                                    Leon Lazarus - EPA Region II
                                    Charles  Sands - EPA Region HI
                                   Charles Hooper - EPA Region IV
                                   Patrick Churilla - EPA Region V
                                    Debra Morey - EPA Region VII
                                   Raleigh Farlow - EPA Region X
A
                                          February 1, 1988

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                                TABLE OF CONTENTS
                                                                                 Page
 INTRODUCTION	1
 PRELIMINARY REVIEW	3

 VOLATILES AND SEMIVOLATILES PROCEDURE	4
 I.     Holding Times	5
 II.     GC/MS Tuning	6
 III.    Calibration	9
 IV.    Blanks	12
 V.     Surrogate Recovery	14
 VI.    Matrix Spike/Matrix Spike Duplicate	16
 VII.   Field Duplicates	17
 VIII.  Internal Standards Performance	18
 IX.    TCL Compound Identification	19
 X.     Compound Quantitation and Reported  Detection Limits	20
 XI.    Tentatively Identified Compounds	21
 XII.   System Performance	23
 XIII.  Overall Assessment of Data for a Case	24
 PESTICIDES PROCEDURE	25
 I.      Holding Times	26
 II.     Pesticides Instrument Performance	26
 III.     Calibration	30
 IV.     Blanks	33
 V.     Surrogate Recovery	34
 VI.     Matrix Spike/Matrix Spike Duplicate	35
 VII.    Field Duplicates	36
 VIII.   Compound Identification	37
 IX.     Compound Quantitation and Reported Detection Limits	38
X.     Overall Assessment of Data for a Case	39

GLOSSARY A:  Data Qualifier Definitions	40

GLOSSARY B:  Other Terms	41
                                                                                  2/8S

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                           LABORATORY DATA VALIDATION

         FUNCTIONAL GUIDELINES FOR EVALUATING ORGANICS ANALYSES


                                     INTRODUCTION
      This  document  is  designed  to offer  guidance in  laboratory  data evaluation and
 validation.   In  some aspects, it  is equivalent  to 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.  These Guidelines have been  updated  to
 include all  requirements in the 10/86  Statement of Work (SOW)  for Organics and  10/86 SOW
 for Volatiles.

      Those areas  where specific SOPs are  possible  are  primarily areas in which definitive
 performance  requirements  are   established.    These  areas  also  correspond  to specific
 requirements in Agency contracts.  These requirements are concerned with specifications that
 are not sample  dependent; they specify performance requirements on matters that should  be
 fully under a laboratory's  control.  These specific areas include  blanks,  calibration standards,
 performance evaluation standard materials, and tuning.   In  particular,  mistakes such  as
 calculation and transcription errors must be rectified by resubmission of  corrected data  sheets.

      This  document  is intended  for technical review.   Some areas  of overlap between
 technical  review   and  Contract  Compliance  Screening (CCS)  exist;    however, contract
 compliance  is not  intended to be a goal of these guidelines.  It is assumed that  the CCS is
 available and can be utilized to assist in the data review procedure.

      Some  requirements are not  identical for every Case or  batch of samples.  Requirements
 for frequency  of Quality  Control (QC) actions  are  dependent  on the  number  of samples,
 sample  preparation technique, time of analysis, etc.  Specific Case requirements and the
 impact of nonconformance must be addressed on a  case by case basis; no specific guidance is
 provided. For example, there is  a contract requirement that a blank analysis be performed a
 minimum of once  every twelve hours of  analysis time. This requirement must be translated
 into the number of blanks required for a specific set  of samples; the data reviewer may have
 to consider  the impact on data quality for a sample analyzed thirteen hours after, a blank,  in
 terms of the acceptability of  that  particular sample.

      At times,  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 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.

      All  data  reviews  must   have,  as  a  cover  sheet,  the Organic  Regional   Data
Assessment (ORDA) form.   If mandatory  actions are  required, they should be  specifically
noted on this form.  In addition, this form is to be  used to summarize overall deficiencies
requiring attention, as well as general laboratory performance and any  discernible trends  in


                                               1                                      2/88

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the quality of the data.  (This form  is not a replacement for  the data review.)   Sufficient
supplementary documentation  must accompany  the  form  to clearly  identify the problems
associated with a Case.   The form and any attachments must be submitted to the Contract
Laboratory Program Quality Assurance Officer  (CLP  QAO), the Regional Deputy Project
Officer (DPO),  and  the  Environmental  Monitoring   Systems  Laboratory  in  Las  Vegas
(EMSL/LV).

      It is  the responsibility of the data  reviewer to  notify the Regional DPO concerning
problems and shortcomings  with regard to  laboratory data.  If there is an urgent requirement,
the DPO may be contacted by telephone  to expedite corrective action.  It is recommended
that all items for DPO action  be presented at one time.  In any case,  the Organic  Regional
Data Assessment form must be completed and submitted.
                                                                                   2/88

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                                PRELIMINARY REVIEW
        In  order to  use  this  document effectively,  the  reviewer  should  have a  general
overview of the 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 is very difficult to
locate.  The site project officer is the best source for answers or further direction.

        CCS  is a source  of a  large quantity of summarized information.   It can be  used to
alert the reviewer of problems in the Case or what may be sample-specific  problems.  This
information may be utilized in data validation.  If CCS is unavailable, those criteria affecting
data validity must be addressed by the data reviewer.

        Cases routinely have unique samples which require  special attention by the reviewer.
Field blanks, field duplicates, and performance audit samples need  to  be identified.   The
sampling records should provide:

              1.  Project  Officer for site

              2.  Complete list of samples with notations on

                  a)  sample matrix
                  b)  blanks*
                  c)  field duplicates*
                  d)  field spikes*
                  e)  QC audit  sample*
                  f)  shipping dates
                  g)  labs involved

                  * If applicable

       The  chain-of-custody  record  includes  sample descriptions  and  date of sampling.
Although  sampling  date  is not addressed by  contract requirements,  the  reviewer must take
into account lag times between sampling and shipping while assessing sample holding times.

       The Case Narrative is another source of general information.   Notable problems with
matrices, insufficient sample volume for analysis or reanalysis, and unusual events should be
found in the  Narrative.
                                                                                     2/88

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                         VOLATILES AND SEMIVOLATILES
                                    PROCEDURE
       The requirements to be checked in validation are  listed below:  ("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.)

       I.     Holding Times (CCS - Lab holding times only)

       II.    GC/MS Tuning

       III.    Calibration

             o   Initial (CCS)

             o   Continuing (CCS)

       IV.    Blanks (CCS)

       V.    Surrogate Recovery (CCS)

       VI.    Matrix Spike/Matrix Spike Duplicate (CCS)

    -  VII.   Field Duplicates

       VIII.  Internal Standards Performance (CCS)

       IX.    TCL Compound Identification

       X.    Compound Quantitation and Reported Detection Limits

       XI.    Tentatively Identified Compounds

       XII.   System Performance (CCS)

       XIII.  Overall Assessment of Data for a Case
                                                                                 2/88

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                                 L  HOLDING TIMES
A.     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  or  sample  preparation,  as
       appropriate.

B.     Criteria

       Technical requirements for sample holding times have only been established for water
       matrices.  The holding times for soils are currently under investigation.   When  the
       results are available they  will be incorporated into the data evaluation  process.   On
       October 26, 1984 in Volume 49, Number 209 of the Federal Register, page 43260, the
       following holding time requirements were established under 40 CFR 136  (Clean Water
       Act):

              Purgeables:  If unpreserved, aromatic volatiles must be analyzed within 7 days
              and non-aromatic volatiles must be analyzed within 14 days.  If preserved with
              hydrochloric acid  and stored at 4°C, then  both  aromatic  and  non-aromatic
              volatiles must be analyzed within 14 days.

              Extractables (Includes Base/Neutrals and  Acids):   Both samples  and extracts
              must be preserved at  4°C.  Samples must be extracted within 7 days and  the
              extract must be analyzed  within 40 days.

C.     Evaluation Procedure

       Actual holding times are established by comparing sampling date on the  EPA Sample
       Traffic  Report with dates of analysis  and/or extraction  on Form I.  Examine  the
       sample records to determine if  samples  were properly  preserved.   (If there is no
       indication of preservation, it must be assumed that the samples are unpreserved.)

D.     Action

       If 40 CFR 136 holding times are exceeded, flag all positive results as estimated (J)
       and  sample  quantitation  limits as estimated (UJ) and document that holding times
       were exceeded.

       The following  table illustrates when the qualifiers are to be used for volatiles:

              Matrix	Preserved     > 7 Davs	> 14 Davs

              Water        No           All aromatics  All compounds
                           Yes           None         All compounds

       1.      If holding times are grossly exceeded, either on the first analysis or upon  re-
              analysis,  the reviewer  must  use  professional judgment to determine   the
              reliability  of the  data and  the effects of  additional storage on the sample
              results. The reviewer  may determine that non-detect data are unusable (R).
                                                                                     2/88

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       2.     Due to limited information concerning holding  times for soil samples, it is left
              to the discretion of the data reviewer to apply water holding time criteria  to
              soil samples.
                                  II.   GC/MS TUNING


A.     Objective

       Tuning  and  performance  criteria  are  established  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.

B.     Criteria

       1.     Decafluorotriphenylphosphine (DFTPP)

              m/z        ION ABUNDANCE CRITERIA

                51        30.0 - 60.0 % of m/z 198
                68        less than 2.0% of m/z 69
                70        less than 2.0 % of m/z 69
               127        40.0 - 60.0% 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 than 1.00% of m/z 198
               441        present, but less than m/z 443
               442        greater than 40.0% of m/z 198
               443        17.0 - 23.0% of m/z 442
       2.     Bromofluorobenzene (BFB)

              m/z        ION ABUNDANCE CRITERIA

                50        15.0 - 40.0% of the base peak
                75        30.0 - 60.0% of the base peak
                95        base peak,  100% relative abundance
                96        5.0 - 9.0% of the base peak
               173        less than 2.0% of m/z 174
               174        greater than 50.0% of the base peak
               175        5.0 - 9.0% of m/z 174
               176        greater than 95.0%, but less than  101.0% of m/z 174
               177        5.0 - 9.0% of m/z 176

       Note:  As contracts are modified, new criteria would then apply.

C.     Evaluation  Procedure

       1.     Verify from the raw data that the mass calibration is correct.
                                                                                    2/88

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       2.     Compare the data presented on  each GC/MS Tuning and Mass Calibration
              (Form V) with each mass listing submitted.

       3.     Ensure the following:

              a.      Verify  that Form V is  present  for  each  12-hour period samples are
                      analyzed.

              b.      The laboratory has not made any transcription errors.

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

              d.      The laboratory has not made any calculation errors. For example, the %
                      mass of m/z 443 relative to the mass  of m/z 442 is calculated using the
                      following equation:

                      % abundance    =    relative abundance of m/z 443      x m
                                          relative abundance of m/z 442

       4.     If possible, verify  that spectra were generated using appropriate background
              subtraction techniques.  Since the DFTPP and BFB spectra are obtained from
              chromatographic  peaks   that  should  be  free  from  coelution  problems,
              background subtraction   should  be  straightforward  and  designed only  to
              eliminate   column  bleed  or  instrument  background  ions.     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.

D.     Action

       1.     If mass calibration is in error, classify all associated  data as unusable (R).

       2.     If ion abundance criteria are not met and the data in question are needed on a
              priority basis, professional judgment may be applied to  determine to what
              extent  the data may be  utilized.   Guidelines to  aid  in  the  application  of
              professional judgment to  this topic are discussed as follows:

              a.      DFTPP  — 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 198/199 and  442/443 ratios are critical.  These ratios are based  on
                     the natural abundances of Carbon  12 and Carbon  13 and should always
                     be met.  Similarly, the m/z 68, 70, 197, and  441 relative abundances
                     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.  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-  10-30%)  and other
                     criteria are  met, the deficiency is  minor.  The  relative  abundance  of
                                                                                     2/88

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              m/z 365 is an indicator of suitable instrument zero adjustment. If m/z
              365 relative abundance is  zero,  minimum  detection limits  may be
              affected.  On the other hand, if m/z 365 is  present,  but less  than the
              1% minimum abundance criteria, the deficiency is not as serious.

       b.      BFB — As with DFTPP, the most important factors to consider are the
              empirical results  that  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 ratio, the
              174/175 ratio, the 176/177 ratio, and the 174/176 ratio.  The relative
              abundances of m/z 50 and 75 are of lower importance.

3.      In line  with the above discussion, an expansion of minus 25% of the low limit
       and plus  25%  of the  high limit  for  selected  ions may be  appropriate.   For
       example,  in  DFTPP the m/z 51  ion abundance criteria  might be expanded
       from 30-60% of m/z 198 to 22-75% of m/z 198.

       a.      The complete expanded criteria for DFTPP and BFB are  as follows:

              1)     Decafluorotriphenylphosphine (DFTPP) (Expanded Criteria)*

                    m/z    ION ABUNDANCE CRITERIA

                      51   22.0 - 75.0% of m/z 198
                      68   less than 2.0% of m/z 69
                      70   less than 2.0% of m/z 69
                     127   30.0 - 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   7.0 - 37.0% of m/z 198
                     365   greater than 0.75% of m/z 198
                     441    present, but less than m/z 443
                     442   greater than 30.0% of m/z 198
                     443   17.0 - 23.0% of m/z 442

             2)     Bromofluorobenzene (BFB) (Expanded Criteria)*
                    m/z    ION ABUNDANCE CRITERIA

                      50   11.0 - 50.0% of the base peak
                      75   22.0 - 75.0% of the base peak
                      95   base peak, 100% relative abundance
                      96   5.0 - 9.0% of the base peak
                     173   less than 2% of the base peak
                     174   greater than 50% of the base peak
                     175    5.0 - 9.0% of m/z 174
                     176   greater than 95%, but less than 101% of m/z 174
                     177    5.0 - 9.0% of m/z 176

      *Note:  Does NOT change contract requirements.

      b.     If  results fall within these  expanded criteria, data may be acceptable.

      c.     If  results fall outside these expanded criteria, all data are unusable (R).
                                      8                                     2/88

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               d.      These criteria do NOT establish new contract requirements.  Contract
                      laboratories  meeting   expanded  criteria  but  not  meeting  contract
                      requirements are NOT in compliance.

               e.      Decisions to use analytical data associated  with DFTPP and BFB tunes
                      not  meeting  contract  requirements  should  be  clearly noted on  the
                      Organic Regional Data Assessment Form.

               f.      If the reviewer has reason to believe that tuning criteria were  achieved
                      using   techniques  that  distorted  or  skewed  the  spectra,  full
                      documentation on the  tuning quality  control should be obtained.  If the
                      techniques  employed   are  found  to be  at  variance with  accepted
                      practices, the quality  assurance program of  the laboratory  may  merit
                      evaluation.

               g.      It is up to the reviewer's discretion, based on professional judgment, to
                      flag  data associated with tunes meeting expanded criteria, but not basic
                      criteria.   If only one  element falls  within the  expanded criteria, no
                      qualification may be   needed.   On  the other hand,  if  several  data
                      elements are in the expanded windows, all associated data may  merit an
                      estimated flag (J). Please note that the data reviewer is not required to
                      use expanded criteria.   The reviewer may  still choose to  flag all  data
                      associated with a  tune  not meeting contract criteria as unusable  (R) if
                      it is  deemed appropriate.
                                  III.   CALIBRATION


A.     Objective

       Compliance requirements  for  satisfactory  instrument calibration  are  established to
       ensure  that  the  instrument is capable  of producing  acceptable quantitative  data.
       Initial  calibration  demonstrates  that  the  instrument  is  capable  of  acceptable
       performance  in   the  beginning,  and  continuing  calibration   checks  document
       satisfactory maintenance and adjustment of  the instrument on a day-to-day  basis.

B.     Criteria

       1.     Initial Calibration

              a.      Volatile and Semivolatile Fractions

                     1)      All  average  Relative  Response   Factors   (RRF)  for  TCL
                            compounds must be > 0.05.

                     2)      All Percent  Relative Standard  Deviations  (%RSD)  must  be
                            <30%.
                                                                                      2/88

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       2.      Continuing Calibration

              a.     Volatile and Semivolatile Fractions

                    1)     AH Relative Response Factors (RRF) for TCL compounds must
                           be > 0.05.

                    2)     All Percent Difference (%D) must be < 25%.

C.     Evaluation Procedure

       1.      Initial Calibration

              a.     Evaluate the RRF for all TCL compounds and verify  the following:

                    1)     Check  and recalculate the RRF and RRF   for  one or more
                           volatile and  semivolatile  TCL  compounds;   verify  that  the
                           recalculated   value(s) agrees   with   the   laboratory  reported
                           value(s).

                    2)     Verify that all volatile and semivolatile TCL  compounds have
                           average Relative Response Factors of at least 0.05.

              b.     Evaluate the Percent Relative Standard Deviation  (%RSD) for all TCL
                    compounds and verify the following:
                                               (Xj - X)2

                                                 (n-1)
                                  % RSD = -2— x 100
                                            x

                                  G = Standard deviation of 5 response factors

                                 ~x = Mean of 5 response factors

                    1)     Check  and  recalculate  the  %RSD  for  one or  more  TCL
                           compounds;  verify that the recalculated value agrees  with the
                           laboratory reported value.

                    2)     Verify that all TCL compounds (volatile and semivolatile) have
                           a %RSD of < 30%.
             c.     If errors are detected in the calculations of  either the RRF  or the
                    %RSD, perform a more comprehensive recalculation.
                                             10                                    2/S8

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               Continuing Calibration

               a.     Evaluate the RRF for all TCL compounds:

                     1)     Verify  that all volatile and  semivolatile  TCL compounds  have
                            Relative Response Factors of at least 0.05.

               b.     Evaluate the Percent Difference and verify  the following:

                     1)     Check  calculation   of  %  Difference  (%D)  between  initial
                            calibration average  Relative Response Factors and  continuing
                            calibration  Relative  Response   Factors  for  one   or  more
                            compounds, using the following equation:

                                                                   - RRFC
%D =      	x 100

where,
                                                                 RRFj
                                          RRFj =   average relative response factor from
                                                    initial calibration.

                                          RRp£ =  relative response factor from
                                                    continuing calibration standard.

                     2)     Verify that  the  %D is < 25% for  all volatile and semivolatile
                            TCL compounds.

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

D.     Action

       1.      Initial Calibration

              a.      If any volatile or semivolatile TCL  compound result has  an average
                     Relative Response Factor of less than  0.05:

                     1)     Flag positive results for that compound as estimated (J).

                     2)     Flag non-detects for that compound as unusable (R).

              b.      If any  volatile or semivolatile TCL compound has a % RSD of greater
                     than 30%:

                     1)     Flag positive results for that compound as estimated (J).

                     2)     Non-detects  may be qualified using professional judgment.

       2.      Continuing Calibration

              a.      If any  volatile or semivolatile TCL compound has a Relative Response
                     Factor of less than 0.05:


                                              11                                     2/88

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                      1)     Flag positive results for that compound as estimated (J).

                     2)     Flag non-detects for that compound as unusable (R).

              b.     If any  volatile  or  semivolatile TCL compound  has  a % Difference
                     between Initial and  Continuing Calibration of greater than 25%:

                     1)     Flag all positive results for that compound as estimated (J).

                     2)     Non-detects  may be qualified using professional judgment.



                                     IV.  BLANKS
A.     Objective

       The  assessment of blank analysis results is to determine the existence and  magnitude
       of contamination problems.  The criteria for evaluation of blanks apply to any blank
       associated with the samples.  If problems with any blank exist, all data associated with
       the Case must be carefully evaluated to determine whether or not there is an inherent
       variability in the data for the  Case, or if the problem is an isolated occurrence not
       affecting other data.

B.     Criteria

       No contaminants should be present in the blank(s).

C.     Evaluation Procedure

       1.      Review the  results  of all  associated  blank(s),  Form  I(s)  and  raw  data
              (chromatograms, reconstructed ion chromatograms, quantitation reports or data
              system printouts).

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

D.     Action

       Action in the case of unsuitable blank results depends on the circumstances and origin
       of  the blank.  No positive sample results should be reported unless the concentration
       of  the compound in the sample  exceeds 10 times the amount in  any blank for the
       common contaminants listed below, or 5 times the amount  for other compounds.  In
       instances where more than 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.  The results must not be corrected  by subtracting any
       blank value.  Specific actions are as  follows:
                                              12                                      2/88

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

 2.      Any  compound  (other than  the  five  listed below) detected in the  sample,
        which was also  detected in any associated blank, must  be qualified when the
        sample concentration is less than five times  the  blank concentration.  For the
        following five compounds, the results  are qualified  by elevating the limit of
        detection when  the  sample  concentration  is less  than 10  times  the  blank
        concentration.

        Common lab contaminants:

        a.  Methylene chloride
        b.  Acetone
        c.  Toluene
        d.  2-butanone
        e.  Common phthalate esters

        The reviewer should note  that the blank analyses 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, there 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 water is  one example.
       Although it is not always possible to determine, instances of this  occurring 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 this source  of contamination.
       However, if  the  reviewer determines that the contamination is from a source
       other  than the sample, he/she  should qualify the data.   In this case, the 5x or
        lOx rule does not apply;  the sample value should be reported as a non-detect.

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

       Case 1:     Sample result is greater than the Contract Required Quantitation
                  Limit  (CRQL), but is less than the required amount (5x or lOx)
                  from the blank  result.

                                                               Rule
                                                           lOx     5x
                            Blank Result                       7       7
                            CRQL                             5       5
                            Sample Result                   60     30
                            Qualified Sample Result        60U   30U

                  In the example  for the lOx  rule,  sample  results less than 70 (or 10
                  x 7)  would be qualified as non-detects. In the case of the 5x rule,
                 sample results less than 35 (or 5x7) would  be  qualified as  non-
                 detects.
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              Case 2:     Sample result is less than CRQL, and is also less than the required
                         amount (5x or lOx) from the blank result.

                                                                      Rule
                                                                  JOx     5x

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

                         Note that data are not reported as 4U, as this would be reported as
                         a detection limit below the CRQL.

              Case 3:     Sample result is greater than the required amount (5x or lOx) from
                         the blank result.

                                                                      Rule
                                                                  10x     5x

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

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

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

       5.      If inordinate amounts  of other TCL compounds are found at low levels in  the
              blank(s), it may be  indicative of a problem at the laboratory  and should be
              noted in the data review comments which are forwarded to the DPO..

       6.      Similar consideration should  be given to TIC compounds which are found in
              both the sample and associated blank(s).  (See Section XI for TIC guidance.)
                            V.   SURROGATE RECOVERY
A.     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  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 review and validation of data  based on specific sample results is
                                             14                                     2/88

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        frequently subjective and  demands analytical experience and  professional judgment.
        Accordingly, this section consists primarily of guidelines,  in some cases with several
        optional approaches suggested.

 B.     Criteria

        Sample and  blank surrogate recoveries for  volatiles and  semivolatiles must be within
        limits as per applicable SOW (Form II).

 C.     Evaluation Procedure

        1.      Check raw data (i.e.,  chromatograms,  quant list,  etc.) to verify the recoveries
               on the Surrogate Recovery (Form II).

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

               a.     If  any two  surrogates within a base/neutral or acid  fraction (or one
                     surrogate for the VOA fraction) are out of specification, or if any one
                     base/neutral, acid or VOA surrogate has a recovery of less than 10%,
                     then there should be a reanalysis with surrogate  results still outside the
                     criteria,   (Note:   When  there  are unacceptable  surrogate  recoveries
                     followed by  successful re-analyses, the labs are required to report only
                     the successful run.)

               b.     The lab has  failed to perform  satisfactorily  if surrogate recoveries are
                     out of specification with no evidence  of repurging, reinjection, or re-
                     extraction.

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

        3.      Any time there are  two or more analyses for a particular fraction the reviewer
               must determine which are the best data to report.

               Considerations should include:

     -   "       a.     Surrogate recovery (marginal vs. gross deviation).

               b.     Holding times.

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

D.     Action

       For  surrogate spike  recoveries  out of  specification,  the  following approaches are
       suggested based on a review  of all data  from  the  case,  especially considering the
       apparent complexity of the  sample matrix:

        1.      If at least  two surrogates in a base/neutral or  acid fraction or  one surrogate in
              the volatile fraction are out of specification,  but  have recoveries  greater than
               10%:

              a.     Positive results for that fraction are flagged as estimated (J).
                                               15                                      2/88

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              b.     Negative  results  for  that  fraction  are  flagged  with  the  sample
                     quantitation limit as estimated (UJ).

       2.     If any surrogate in a fraction shows !ess than  10% recovery:

              a.     Positive results for that fraction are flagged as estimated (J).

              b.     Negative results for that fraction are flagged as unusable (R).

       3.     No qualification with respect to surrogate recovery is placed on data unless at
              least  two surrogates are out  of  specification  in the  base/neutral  or acid
              fraction, or one in the volatile fraction, or unless any surrogate has a less than
              10% recovery.

       4.     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 there  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  judgment  allows
              some  use of the  affected  data,  analytical  problems  remain  that  must  be
              corrected by the laboratory.
                   VI.  MATRIX SPIKE/MATRIX SPIKE DUPLICATE
A.     Objective
       These  data  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.

B.     Criteria

       1.      Spike  recoveries  must  be  within  the  advisory  limits  established  in the
              appropriate IFB and  on  Form III.

       2.      Relative Percent  Differences (RPD) between matrix spike and matrix spike
              duplicate recoveries must be  within the advisory  limits  established  in the
              appropriate IFB and  on  Form III.

C.     Evaluation Procedure

       1.      Inspect results for the  Matrix  Spike/Matrix Spike Duplicate Recovery (Form
              III).

       2.      Verify transcriptions from raw  data and verify calculations.
                                              16                                      2/88

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 D.   Action
      No action  is taken on  Matrix Spike/Matrix Spike Duplicate (MS/MSD) data alone to
      qualify an  entire Case.   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.

      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.

      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 the  MS/MSD results that a lab is having  a
      systematic problem in the analysis of one or more analytes, which affects  all associated
      samples.

      Note:  If a field blank was used for the MS/MSD, the information must be included on
      the ORDA form.

                               VII.  FIELD DUPLICATES
A.    Objective

      Field duplicate samples may be taken and analyzed as an indication of overall precision.
      These analyses measure both  field and  lab precision; therefore, the  results  may have
      more variability than lab duplicates  which measure only lab  performance.  It  is also
      expected that soil duplicate results will have a greater variance than water matrices due
      to difficulties associated with collecting identical field samples.

B.    Criteria

      There are no specific review criteria for field duplicate analyses comparability.

C.    Evaluation Procedures

      Samples which are field  duplicates  should be identified using EPA Sample Traffic
      Reports or sample field sheets.  The reviewer  should compare the results reported for
      each sample  and calculate  the Relative Percent Difference (RPD).

D.    Action

       Any evaluation  of  the  field  duplicates  should be  provided  with  the  reviewer's
       comments.
                                              17                                     2/88

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                    VIII.  INTERNAL STANDARDS PERFORMANCE
 A.    Objective
      Internal Standards (IS) performance criteria ensure that GC/MS sensitivity and response
      is stable during every run.

B.    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 associated calibration standard.

C.    Evaluation Procedure

      1.    Check raw  data (i.e.,  chromatograms,  quantitation  lists,  etc.) to  verify  the
           recoveries reported on the Internal Standard Area Summary (Form VIIIA, VIIIB).

      2.    Verify that  all retention times and IS areas are acceptable.

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

           a.    Magnitude of the shift.

           b.    Holding times.

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

D.    Action

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

           a.    Positive results  for  compounds  quantitated using  that IS  are  flagged as
                 estimated (J) for that sample fraction.

           b.    Non-detects for compounds quantitated  using that  IS are flagged  with the
                 sample  quantitation limit  classified  as  estimated (UJ)  for  that sample
                 fraction.

              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-detects should  then be flagged as unusable (R).
       2.      If an  IS  retention time varies by  more than 30  seconds, the chromatographic
              profile for that 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 for that sample fraction.
                                              18                                     2/88

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                        IX.  TCL COMPOUND IDENTIFICATION
 A.   Objective
      The objective of the 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 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.

B.    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  ions specified above  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 greater than  10%  in  the sample  spectrum but not present  in  the
                 standard spectrum must be considered  and accounted for.

C.    Evaluation Procedure

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

      2.    Check the laboratory standard spectra vs. the sample compound spectra.

      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 judgment to determine  if instrument cross-contamination has affected
           any positive compound identification.
                                             19                                     2/88

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 D.     Action
        1.     The application of qualitative criteria for GC/MS analysis  of TCL compounds
              requires   professional  judgment.     If  it   is  determined   that   incorrect
              identifications were made, all such data should be flagged  as not detected (U)
              or unusable (R).

       2.     Professional judgment must be used to qualify the data if it is determined that
              cross-contamination has occurred.
        X.  COMPOUND OUANTITATION AND REPORTED DETECTION LIMITS
A.     Objective
       The  objective  is to ensure that the reported  quantitation  results and  CRQLs are
       accurate.

B.     Criteria

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

       2.      Compound RRF must be calculated based on the IS specified in the  SOW for
              that compound.   Quantitation must  be  based  on the quantitation ion  (m/z)
              specified in the SOW.  The compound quantitation must be  based on  the  RRF
              from the appropriate daily standard.

C.     Evaluation Procedure

       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.

       2.      Verify that the correct internal standard, quantitation ion, and RRF were used
              to quantitate the compound.

       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.

D.     Action

       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 circumstances, the reviewer may determine
       qualification of data is warranted.
                                             20                                     2/88

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                     XL  TENTATIVELY IDENTIFIED COMPOUNDS
 A.     Objective
        Chromatographic  peaks in volatile and  semivolatile  fraction analyses that are not
        target compound  list (TCL) analytes, surrogates, or internal standards are potential
        tentatively  identified compounds (TIC).   TICs  must  be qualitatively  identified  by
        (GC/MS) library search and the identifications assessed  by the data reviewer.

 B.     Criteria

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

               Note:  SOW revision October 1986 does not allow the laboratory to report as
               tentatively identified compounds (TICs) any TCL compound which is properly
               reported  in  another  fraction.    (For example,  late  eluting   volatile  TCL
              compounds must not be reported as BNA TICs.)

       2.     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 TCL compounds.

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

              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".

C.     Evaluation Procedure

       1.      Check the raw data to verify that the laboratory has generated a library search
              for all required peaks in the chromatograms (samples and blanks).
                                              21                                     2/88

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       2.     Blank chromatograms should be examined to verify that 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 than  10 percent  of the  internal standard height, but present  in the
              blank chromatogram at similar relative retention time.

       3.     All mass spectra in every sample and blank must be examined.

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

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

              Examples:

              a.     Common lab contaminants:  CC^ (m/e 44), siloxanes (m/e 73), diethyl
                     ether,  hexane, certain freons (l,l,2-trichloro-l,2,2-trifluoroethane or
                     fluoro-trichloromethane),  phthalates at  levels  less than  100  ug/1 or
                     4000 ug/kg.

              b.     Solvent preservatives:   cyclohexene is   a  methylene chloride preser-
                     vative.   Related  by-products include  cyclohexanone,  cyclohexenone,
                     cyclohexanol, cyclohexenol, chlorocyclohexene, chlorocyclohexanol.

              c.     Aldol reaction products of acetone include:  4-hydroxy-4-methyl-2-
                     pentanone, 4-methyl-2-penten-2-one, 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 data from the entire Case may be affected.

       7.     TCL compounds  may be  identified  in  more than one fraction.   Verify  that
              quantitation is made  from the proper fraction.
D.     Action
       1.      All  TIC results should be  flagged as tentatively identified  with estimated
              concentrations (JN).

       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-TCL
                     compound  is  not  acceptable,  the  tentative  identification should  be
                     changed to  "unknown" or an appropriate identification.
                                              22                                     2/88

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               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 net
               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 of
               common laboratory contaminant, the result may be flagged as unusable (R).

        5.      In  deciding  whether a  library  search  result  for a TIC represents a  realistic
               identification, professional judgment must be exercised.  If there is more than
               one reasonable 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 (1,3,5-trimethyl benzene  to trimethyl
               benzene isomer)  or to  a compound  class  (2-methyl, 3-ethyl  benzene  to
               substituted aromatic compound).

        6.      The reviewer may elect to report all similar  isomers as  a total.   (All alkanes
               may be summarized and reported as total hydrocarbons.)

        7.      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.

        8.      Physical constants, such  as boiling point, may  be factored  into  professional
              judgment of TIC results.
                               XII.   SYSTEM PERFORMANCE


       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.

       Some examples of instrument performance  indicators  for various  factors are as
follows:

       1.  Abrupt,  discrete  shifts in reconstructed  ion chromatogram (RIC)  baseline  may
           indicate gain or threshold changes.

       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.



                                              23                                     2/88

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            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 may result in inaccurate quantitation.

       Continued analytical activity with degraded  performance suggests lack of attention or
professional experience.  Based on the instrument performance indicators, the data reviewer
must decide if the system has degraded to the point of affecting data quality or validity.  If
data quality may have  been affected,  data should be  qualified  using the reviewer's best
professional judgment.
                XIII.  OVERALL ASSESSMENT OF DATA FOR A CASE
       It  is appropriate for the data reviewer to make professional judgments and express
concerns and  comments on  the validity of the  overall data package  for a Case.   This is
particularly appropriate for Cases in  which there are several QC criteria out of specification.
The additive nature of QC factors out of specification is difficult to  assess in  an objective
manner, but  the reviewer has a responsibility to inform users concerning  data quality and
data limitations  in order to assist that user in avoiding inappropriate use of the data,  while
not precluding any  consideration of the data at all.   The data  reviewer would  be greatly
assisted in this endeavor if the data quality objectives were provided.
                                              24                                      2/88

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                              PESTICIDES PROCEDURE


       The requirements to be checked in validation are listed below.  ("CCS" indicates that
the contract requirements for these items will also be checked by CCS;  CCS requirements are
not always the same as the data review criteria.)

       I.     Holding Times (CCS - Lab holding times only)

       II.     Pesticides Instrument Performance (CCS)

       III.    Calibration

             o   Initial (CCS)

             o   Analytical Sequence (CCS)

             o   Continuing (CCS)

       IV.    Blanks (CCS)

       V.     Surrogate Recovery

       VI.    Matrix Spike/Matrix Spike Duplicate (CCS)

       VII.   Field Duplicates

       VIII.   Compound Identification

       IX.    Compound Quantitation and Reported Detection Limits

       X.     Overall Assessment of Data for a Case
                                            25                                    2/88

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                                  I.  HOLDING TIMES
 A.    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  or  sample  preparation,  as
       appropriate.

B.     Criteria

       Technical requirements for sample holding times have only been established for water
       matrices.   The holding times for soils  are  currently under  investigation.  When the
       results are available they will be incorporated into  the data evaluation process. On
       October 26, 1984 in Volume 49, Number 209 of the Federal  Register,  page 43260, the
       holding time requirements for pesticides  were established under 40 CFR 136 (Clean
       Water  Act).   Samples  must be  extracted  within 7  days and the extract must  be
       analyzed within 40 days. Both samples and extracts must be  stored at 4° C.

C.     Evaluation Procedure

       Actual holding times are established by comparing sampling  date on the EPA Sample
       Traffic Report with dates of analysis and extraction on Form I.  Examine the sample
       records to determine if samples were properly preserved. (If there is no indication of
       preservation, it must be assumed that the samples are  unpreserved.)

D.     Action

       If 40 CFR  136 holding times are exceeded, flag all  positive results as estimated (J)
       and  sample quantitation limits as estimated (UJ) and document to  the  effect that
       holding times were exceeded.

       1.     If holding times are grossly exceeded, either on the first analysis or upon re-
              analysis,  the reviewer must use  professional  judgment  to  determine  the
              reliability  of the data  and  the effect of additional storage  on the . sample
              results.  The reviewer may determine non-detect data  are unusable (R).

       2.     Due to limited information concerning holding times  for soil samples, it is left
              to the discretion of the data reviewer to apply water holding  time  criteria to
              soil samples.
                    II.  PESTICIDES INSTRUMENT PERFORMANCE
A.     Objective
       These criteria are established to ensure  that adequate chromatographic resolution and
       instrument sensitivity are achieved by the chromatographic system. These criteria are
       not sample specific; conformance is determined using standard materials.  Therefore,
       these criteria should be met in all circumstances.
                                             26                                     2/88

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B.     Criteria

       1.     DDT Retention Time

             DDT must have retention time on packed columns (except OV-1 and OV-101)
             greater than or equal to 12 minutes.

       2.     Retention Time Windows

             The laboratory must report retention time window data on the Pesticide/PCB
             Standards Summary (Form IX) for each GC column used to analyze samples.

       3.     DDT/Endrin Degradation Check

             The total percent  breakdown for neither DDT nor endrin may exceed 20%.
             The percent breakdown is the amount of decomposition that endrin and 4,4'-
             DDT undergo when analyzed by the chromatographic system.

             a.     For endrin, the percent  breakdown is  determined  by the presence of
                   endrin aldehyde and/or endrin ketone in the GC chromatogram.

             b.     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.

             c.     A combined percent breakdown must be calculated  if there is evidence
                   of a peak at the retention time  of endrin  aldehyde/4,4'-DDD, which
                   co-elute on the OV-1 packed column (or an equivalent column).

             d.     Percent breakdown is calculated using the following equations:

             % Breakdown      Total DDT degradation peak area (DDE + DDD)
             for 4,4'-DDT      Total DDT peak area  (DDT + DDE + DDD)


      n, _   , .       Degradation Peak Areas (endrin  aldehvde + endrin ketone)
      % Breakdown _	'_	  x 100
      for endrin      Peak Area (endrin + endrin aldehyde + endrin ketone)


                    Note 1:      Peak area of endrin aldehyde must be measured during
                                the degradation check  to verify  system performance.
                                Endrin aldehyde is not reported on Form 1 because  it is
                                removed by alumina cleanup.

                    Note 2:      The term "peak height"  may be substituted for the term
                                "peak area".

                                        Total degradation peak areas
      Combined    =            (DDE + DDD + endrin aldehyde + endrin ketone)
      % Breakdown
                                     Total DDT and endrin peak areas
                      (DDT + DDE -f DDD + endrin + endrin aldehyde + endrin ketone)
                                          27                                    2/88

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       4.     DEC Retention Time Check

              The retention time of DBC in each analysis must be compared to the retention
              time of DBC in Evaluation  Standard Mix  A.  The  Percent  Difference  (%D)
              must not exceed  2.0% for packed  columns,  0.3% for  narrow-bore capillary
              columns, and 1.5% if wide-bore capillary columns are used.

                                                          - RTS
                                            %D    =  	     x 100
                                                         RT,
              where,
              RTj    = Absolute retention time of dibutylchlorendate in the initial standard
                       (Evaluation Standard Mix A).

              RTS    = Absolute  retention time of dibutylchlorendate in  the subsequent
                       analyses.

C.     Evaluation Procedure

       1.      Check raw data to verify that DDT retention time is greater than 12 minutes
              on the  standard chromatogram and that there is adequate resolution between
              peaks.

       2.      Check raw data to verify that retention time windows  are reported on Form
              IX, and that all  pesticide standards are within the established retention time
              windows.

       3.      Check  raw  data  to verify  that the  percent  breakdown for  endrin and  4,4'
              -DDT,  or the combined percent  breakdown,  does  not exceed 20%  in  all
              Evaluation Standard Mix B analyses on Form VIII D.

       4.      Check  raw  data  to verify that the percent difference  in retention time for
              dibutylchlorendate  in all standards and samples is  < 2.0% for packed column
              analysis, <  0.3% for capillary column  analysis, and < 1.5%  for  wide-bore
              capillary column analysis on Form VIII E.

D.     Action

       1.      DDT Retention Time

              If the retention time of DDT is less than 12 minutes  (except on  OV-1  and
              OV-101), a close examination of the chromatography is necessary to ensure
              that adequate separation of  individual components is achieved.  If adequate
              separation is not achieved, flag all affected compound data as unusable (R).

       2.      Retention Time Windows

              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.
                                             28                                     2/88

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       a.    For the affected samples, check to see if chromatograms contain  any peaks
            within  an  expanded  window surrounding  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, there is usually no effect on the data.  (Non-detected values can
            be considered  valid.)

       b.    If the affected sample  chromatograms  contain peaks  which may be  of
            concern (i.e., above the CRQL and either close to  or within  the expected
            retention time  window of the pesticide  of interest), then  two options are
            available to the reviewer to determine the extent of the effect on the data.

            1)    If no additional effort is warranted by the reviewer, flag all positive
                  results and quantitation limits as unusable (R).  The  narrative should
                  emphasize the possibility of either false negatives or false positives, as
                  appropriate.

            2)    In some  cases, additional effort is warranted by the reviewer (e.g., if
                  the data  are needed on a  priority basis  and if the peak(s) present
                  might represent a level  of concern  for that particular pesticide).  In
                  these situations, the reviewer may undertake the following additional
                 efforts to determine  a  usable  retention  time window  for affected
                 samples:

                 (a)  The reviewer should 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.

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

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

                 (d)   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.

3.     DDT/Endrin Degradation Check

      a.    If DDT  breakdown  is greater than  20%,  beginning  with  the samples
           following the last in-control standard:

           1)    Flag all  quantitative results  for DDT as estimated (J).   If DDT was
                 not detected,  but  DDD  and  DDE  are  positive,  then  flag  the
                 quantitation limit for DDT as unusable (R).

           2)    Flag results  for  DDD and/or  DDE as presumptively present at an
                 estimated quantity (NJ).
                                        29                                      2/88

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            b.    If endrin breakdown is greater than 20%:

                 1)    Flag  all quantitative results for endrin as estimated (J).  If endrin was
                       not  detected,  but  endrin  aldehyde and endrin  ketone  are  positive,
                       then  flag the quantitation limit for endrin as unusable (R).

                 2)    Flag  results  for  endrin  ketone  as   presumptively present  at  an
                       estimated quantity  (NJ).

      4.     Retention Time Check

            a.    If the retention time shift for dibutylchlorendate (DEC) is greater than  2.0%
                 for packed column, greater than 0.3% for narrow-bore capillary column, or
                 greater  than  1.5% for wide-bore capillary  column,  the  analysis  may  be
                 flagged  unusable for that sample(s) (R), but qualification of the data is left
                 up to the professional judgment of the reviewer.

              b.     The retention time shift cannot be evaluated in the absence of DEC.
                                  III.  CALIBRATION
A.    Objective

      Compliance  requirements for  satisfactory  instrument calibration  are  established  to
      ensure that the instrument is capable of producing acceptable quantitative data.  Initial
      calibration demonstrates that the instrument  is capable  of acceptable performance in the
      beginning, and  continuing  calibration checks document satisfactory maintenance and
      adjustment of the instrument over specific time periods.

B.    Criteria

      1.    Initial Calibration Linearity Check

              The Percent  Relative  Standard  Deviation (%RSD)  of calibration factors  for
              aldrin,  endrin,  DDT,  and dibutylchlorendate must  not exceed  10%.    If
              toxaphene is  identified and quantified,  a three-point  calibration is required.
              If  the  calibration factor for DDT  or  toxaphene  is  outside  the  10% RSD
              window,  calibration curves must  be used for quantitation of  DDT, DDE,
              DDD, or toxaphene.

                    Calibration Factor -  Total Area of Peak
                                          Mass Injected (ng)
                                              30                                     2/88

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                                   cr
                     %RSD =    	 x  100
                                  CF

                 where,

                     6   = Standard Deviation

                     CF = Mean Calibration Factor
             Note:   The  10% RSD linearity check is required only for columns which are
                     used  for quantitative  determinations.   Quantitation of  the surrogate
                     requires the use of a column shown to meet the 10% linearity criterion.
                     Columns used only to provide qualitative confirmation are not required
                     to meet this criterion.

      2.    Analytical Sequence

           a.    Primary Analysis

                     At  the beginning  of each 72-hour period  all  standards must  be
                     analyzed.

           b.    Confirmation Analysis

                 1)    Evaluation Standard Mix A, B, and C are required for the curve.

                 2)    Only the standards containing  the  compound(s)  to be confirmed are
                      required.  These standards  must be repeated after every five samples.

                 3)    Evaluation Mix B is required after every ten samples.

      3.    Continuing Calibration

           The calibration  factor  for each standard must  be within 15% of  the standard at
           the beginning  of the analytical sequence on  quantitation columns   (20%  on
           confirmation columns).

C.    Evaluation Procedure

      1.    Initial Calibration

           a.     Inspect the Pesticide Evaluation Standards Summary (Form VIII)  and verify
                 agreement  with  the  raw  GC   data  (chromatograms  and  data  system
                 printouts).

           b.    Check the raw data and recalculate some of  the calibration  factors and the
                percent   relative  standard  deviations   (%RSD)  for  aldrin,  endrin,
                4,4'-DDT, and dibutylchlorendate at the three calibration concentrations.
                                              31                                      2/88

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               c.      Verify that  the  %RSD for  the calibration  factor  of each specific
                      pesticide is less than or equal to 10% for each 72-hour period.

               d.      If  errors  are detected,  more  comprehensive  recalculation  should  be
                      performed.

               e.      If  toxaphene or the  DDT series  was identified and quantitated,  verify
                      that a three-point calibration was established.

       2.      Verify that all standards were analyzed in the 72-hour sequence.

       3.      Continuing Calibration

               a.      Review the  pesticide sample data to verify whether  the  standard was
                      used as a quantitation standard or as a confirmation standard.

               b.      For the quantitation standards,  check the raw data to verify the percent
                      difference (%D),  using the following formula,  for approximately  ten
                      percent of the reported values by recalculation.
                                                                    x,00
                      where,
                      Rj = Calibration Factor from first analysis
                      R2 = Calibration Factor from subsequent analysis

D.     Action

       I.      Initial Calibration

              If criteria for linearity are not met, flag all associated  quantitative results as
              estimated (J).

       2.      Analytical Sequence

              If the proper standards have not been analyzed, data may be  affected.  The
              data reviewer must use professional  judgment to determine  severity  of the
              effect and qualify the data accordingly.

       3.      Continuing Calibration

              a.      If the %D between  calibration factors is  greater  than  15%  for the
                     compound(s) being quantitated (20% for compounds being confirmed),
                     flag all associated positive quantitative results as estimated (J).
                                              32                                       2/88

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                                      IV.   BLANKS
 A.     Objective

       The assessment of blank analysis results is to determine  the existence and magnitude
       of contamination problems.  The criteria for evaluation of blanks apply to any  blank
       associated with the samples.  If problems with any blank exist, all data associated with
       the Case must be carefully evaluated to determine whether or not there is an inherent
       variability  in  the  data for the  Case, or the problem is an isolated occurrence  not
       affecting other data.

B.     Criteria

       No contaminants should be present in the blank(s).

C.     Evaluation  Procedure

       1.      Review the  results  of  all  associated  blank(s),  Form  I(s)  and raw  data
              (chromatograms, quantitation reports or data system printouts).

       2.      Verify that  the method  blank analysis(es)  contains  less than  the Contract
              Required Quantitation Limits  (CRQL) of any Pesticide/PCB  or interfering
              peak.

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

D.     Action

       Action in the case of unsuitable  blank results depends on  the circumstances and  the
       origin  of  the blank.   No positive sample results  should be reported unless  the
       concentration of the compound  in  the  sample exceeds  5  times the amount in  the
       blank.  In  instances  where  more than 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   The  results  must  not  be corrected  by
       subtracting  the blank value.  Specific actions are as follows:

       1.      If a Pesticide/PCB is found  in the blank but  not found in  the sample(s), no
              action is taken.

       2.      Any Pesticide/PCB detected in the sample and also  detected in any associated
              blank, must be qualified when the sample concentration is  less than 5  times
              the blank concentration.

              The  reviewer should note that the blank  analyses 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 criteria,  such that a
              comparison  of the total amount of contamination is actually made.

              Additionally,  there  may  be  instances  where  little  or  no contamination was
              present in the associated  blanks, but qualification of the sample  was deemed
                                              33                                     2/88

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               necessary.  Contamination introduced through dilution  water is one example.
               Although it is not always  possible to determine, instances of this 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 that the contamination is from a source
               other than the sample, he/she should  qualify the data. In this case,  the 5x rule
               does not apply; the sample value should be reported  as a non-detect.

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

               Case 1:       Sample  result is greater than the CRQL, but is less  than the
                            required amount (5x) from the  blank  result.
                                   Blank Result                      1.0
                                   CRQL                             .5
                                   Sample Result                     4.0
                                   Qualified Sample Result            4.0U

                            In this case, sample results  less  than 5.0  (or  5 x  1.0) would  be
                            qualified as non-detects.

              Case 2:        Sample result is greater than the required amount (5x) from the
                            blank result.

                                                                     5x
                                   Blank Result                      1.0
                                   CRQL                             .5
                                   Sample Result                     6.0
                                   Qualified Sample Result            6.0
                             V.  SURROGATE RECOVERY
A.     Objective
       Laboratory performance on  individual samples  is established by  means  of spiking
       activities.    All  samples are  spiked with  a surrogate compound  prior  to sample
       preparation. The evaluation of the results of these surrogate spikes is not  necessarily
       straightforward.   The sample itself may prod.uce 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 review and validation 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.
                                              34                                     2/88

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 B.     Criteria

        Sample and blank  recoveries  of dibutylchlorendate must be  within limits as per
        applicable SOW (Form II).

 C.     Evaluation Procedure

        1.      Check raw data  (i.e., chromatograms, quant list, etc.)  to verify the recoveries
               on the Surrogate Recovery (Form II).

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

 D.     Action

        If pesticide  surrogate  recoveries are outside of  advisory windows,  the following
        guidance is suggested:

        1.      If low recoveries are obtained, flag associated positive  results and quantitation
               limits as estimated (J).

        2.      If high  recoveries  are  obtained, professional  judgment should  be  used to
               determine  appropriate  action.   A high  bias  may  be  due  to co-eluting
               interferences.

        3.      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, flag all negative results as unusable  (R).
                   VL  MATRIX SPIKE/MATRIX SPIKE DUPLICATE
A.     Objective
       These  data 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.
B.     Criteria
       I.      Advisory  limits are established for  spike  recovery limits  in the appropriate
              SOW and on Form III.

       2.      Advisory limits are established for relative percent difference between matrix
              spike  and matrix spike  duplicate recoveries in the appropriate SOW and  on
              Form  III.
                                               35                                     2/88

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 C.     Evaluation Procedure

       1.      Inspect results for the  Matrix Spike/Matrix Spike Duplicate Recovery (Form
               III).

       2.      Verify transcriptions from raw data and verify calculations.

 D.     Action

       No action  is taken on Matrix Spike/Matrix Spike Duplicate (MS/MSD) data alone to
       qualify an entire Case.   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.

       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.

       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 the  MS/MSD results that  a lab is having a
       systematic  problem in the analysis  of one or more  analytes, which  affects all
       associated samples.
                               VII.  FIELD DUPLICATES


A.     Objective

       Field  duplicate  samples may  be taken  and  analyzed  as an  indication  of overall
       precision.  These analyses measure both field and lab precision; therefore, the results
       may have more  variability than lab  duplicates which measure only lab performance.
       It is also expected that soil duplicate results will have a greater variance than water
       matrices due to difficulties associated with collecting identical field samples.

B.     Criteria

       There are no specific review criteria  for field duplicate analyses comparability.

C.     Evaluation  Procedures

       Samples which are field duplicates  should  be identified  using  EPA  Sample Traffic
       Reports or  sample field sheets. The  reviewer should compare the results reported  for
       each sample and calculate the Relative Percent Difference (RPD).

D.     Action

       Any evaluation  of  the field  duplicates should be  provided  with  the  reviewer's
       comments.
                                              36                                     2/88

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                          VHI.  COMPOUND IDENTIFICATION
 A.    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).

B.     Criteria

       1.     Retention times  of reported  compounds must fall  within  the calculated
              retention time windows for the two chromatographic columns.

       2.     GC/MS confirmation is required if the concentration of a compound exceeds
              10 ng/uL in the final sample extract.

C.     Evaluation Procedure

       1.     Review Form I,  the associated  raw data (chromatograms and data  system
              printouts) and the Pesticide/PCB Identification  Summary (Form X).  Confirm
              reported  positive  detects, using  appropriate retention times and retention  time
              windows, and verify  that the compounds listed as "not detected" are correct.

       2.     Verify that positive identifications have dissimilar column analysis.  (The 3%
              OV-1 column cannot be  used for confirmation if both dieldrin and  DDE are
              identified.)

       3.     For multipeak pesticides (chlordane  and toxaphene) and  PCBs, the  retention
              times  and relative peak  height  ratios  of  major component  peaks should be
              compared against  the appropriate standard  chromatograms.

       4.     Verify  that   GC/MS   confirmation  was   performed   for   pesticides/PCB
              concentrations in the final sample extract which exceeded 10 ng/uL.

D.     Action

       1.     If  the  qualitative criteria  for  two-column confirmation  were not  met, all
              reported  positive  detects should be considered non-detects.   The  reviewer
              should  use professional judgment 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 CRQL can be reported.

              b.      If the  misidentified peak  poses an interference with potential detection
                     of a  target peak, then the reported value should  be considered  and
                     flagged as  the estimated quantitation limit (UJ).

       2.      If  PCBs  or  multipeak  pesticides exhibit  marginal  pattern-matching quality,
              professional judgment should be  used to establish whether the differences are
              attributable   to   environmental   "weathering".      If   the   presence  of  a
                                             37                                     2/88

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              PCB/multipeak pesticide is  strongly suggested, results should be  reported  as
              presumptively present (N).

              If an observed pattern closely matches more than one  Arocior, professional
              judgment should be used to decide whether the neighboring Arocior is a better
              match, or if multiple Aroclors are present.

       3.     If GC/MS confirmation was required but not performed, the reviewer should
              notify the DPO.
        IX.  COMPOUND OUANTITATION AND REPORTED DETECTION LIMITS
A.     Objective
       The  objective  is to ensure  that the reported quantitation  results  and CRQLs are
       accurate.

B.     Criteria

       Compound quantitation, as well as the adjustment of the CRQL,  must be calculated
       according  to the appropriate SOW.

C.     Evaluation Procedure

       1.      Raw data should be examined to verify the correct calculation of  all sample
              results reported by  the laboratory.  Quantitation reports, chromatograms, and
              sample  preparation  log  sheets should  be  compared to the reported positive
              sample results and quantitation limits.

       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.

D.     Action

       Quantitation limits affected by large, off-scale peaks should  be flagged as unusable
       (R).    If  the  interference  is  on-scale,  the reviewer  can  provide  an   estimated
       quantitation limit (UJ) for each affected compound.

       Note:   Simple-peak pesticide results can  be checked for  rough  agreement between
       quantitative  results  obtained on the  two GC columns.   The reviewer should use
       professional judgment 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, the lower of the two values should be reported and
       qualified as presumptively  present at an estimated quantity (NJ).   This necessitates a
       determination  of an  estimated  concentration on the  confirmation  column.    The
       narrative should indicate that the presence of interferences has obscured the attempt
       at a second column confirmation.
                                             38                                     2/88

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                  X.  OVERALL ASSESSMENT OF DATA FOR A CASE
       It is appropriate for the data reviewer to make professional judgments and  express
concerns and  comments on  the validity of the overall data package  for  a Case.   This is
particularly appropriate for Cases in  which there are several  QC criteria out of specification.
The additive nature of QC factors out of specification is  difficult  to assess in an objective
manner,  but the reviewer has a responsibility to  inform users concerning  data quality and
data limitations  in order to assist that user in avoiding inappropriate use of the data, while
not precluding any  consideration of the data at all.   The data reviewer  would  be  greatly
assisted in this endeavor if the data quality objectives were  provided.
                                              39                                     2/88

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                                      GLOSSARY A


                                Data Qualifier Definitions


For  the purposes of  this document the following  code letters and associated definitions are
provided.

       U    -  The  material  was  analyzed  for,  but  was  not  detected.   The  associated
                numerical value is the sample quantitation limit.

       J     -  The associated numerical value is an estimated quantity.

       R    -  The data are  unusable  (compound  may or may not be present).  Resampling
                and reanalysis is necessary for verification.

       N    -  Presumptive evidence of presence of material.

       NJ   -  Presumptive  evidence  of  the  presence  of the  material  at  an  estimated
                quantity.

       UJ   -  The  material was  analyzed  for, but was not  detected.    The  sample
                quantitation limit is an estimated quantity.

The  reviewer may determine that  qualifiers other than those used  in this  document are
necessary to describe or qualify the data.  In these instances, it is  the responsibility of each
Region to thoroughly document/explain the qualifiers used.
                                              40                                      2/88

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                                    GLOSSARY B


                                     Other Terms


 BFB         Bromofluorobenzene — volatile tuning 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).

 CCC         Calibration Check Compound

 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

 DFTPP      Decafluorotriphenylphosphine  — semivolatile tuning compound

 DPO         Deputy Project Officer

 EICP        Extracted Ion Current Profile

 GC/EC      Gas Chromatography/Electron Capture Detector

 GC/MS     Gas Chromatograph/Mass Spectrometer

 GPC         Gel Permeation Chromatography -  A sample clean-up technique that 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.

 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


PCB         Polychlorinated biphenyl
                                            41
2/88

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 PE Sample   Performance Evaluation Sample


 Primary     One of two types of pesticide/PCB analysis by GC/EC techniques, the other
 Analysis     being confirmation analysis.   If the  two analyses are run at separate times, the
             primary analysis is the first analysis  chronologically, and is used to establish the
             tentative identification  of  any pesticides/PCBs detected.  The identification  is
             then confirmed in the confirmation analysis.  If  the two  analyses  are  done
             simultaneously, either may be considered the primary analysis.   Either may be
             used for quantitation  if contract criteria are met.

 QA          Quality  Assurance - Total program for assuring the  reliability of data.

 QC          Quality  Control  -  Routine  application  of procedures  for  controlling  the
             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
             o   Case of field samples
             o   Each 20 field samples within a Case
             o   Each  14-day calendar  period  during  which  field samples in a -Case are
                 received, beginning with receipt of the  first sample in the SDG. (For VOA
                 contracts, the calendar period is 7-day.)

SMO        Sample Management Office

SOP         Standard Operating Procedure

SOW        Statement of Work

SPCC        System Performance Check Compound

SV          Semivolatile analysis - Method based on analysis by GC/MS for  BNA organic
             compounds.

TCL         Target Compound List

TIC          Tentatively Identified Compound  -  A compound not  on the TCL.


                                             42                                     2/88

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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.

cS           Standard Deviation Estimate (of a sample)
                                            43                                     2/88

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                                                                       Region

                       ORGANIC REGIONAL DATA ASSESSMENT
 CASE NO.	  SITE
 LABORATORY	NO. OF SAMPLES/
                                        MATRIX	
 SDG #	  REVIEWER (IF NOT ESD)

 SOW*	  REVIEWER'S NAME	
 DPO: ACTION	FYI 	  COMPLETION DATE
                           DATA ASSESSMENT SUMMARY

                                        VOA     BNA      PEST      OTHER

 1.    HOLDING TIMES                   	  	   	   	

 2.    GC/MS TUNE/INSTR. PERFORM.      	  	   	   	

 3.    CALIBRATIONS                     	  	   	   	

 4.    BLANKS                           	  	   	   	

 5.    SURROGATES                      	  	   	   	

 6.    MATRIX SPIICE/DUP                	  	   	   	

 7.    OTHER QC                         	  	   	   	

 8.    INTERNAL STANDARDS             	  	   	   	

 9.    COMPOUND IDENTIFICATION        	  	   	   	

10.    SYSTEM PERFORMANCE             	  	   	   	

11.    OVERALL ASSESSMENT             	  	   	   	

   O = Data had no problems/or qualified due to minor problems.
   M = Data qualified due to major problems.
   Z = Data unacceptable.
   X = Problems, but do not affect data.
ACTION ITEMS:
AREAS OF CONCERN:
NOTABLE PERFORMANCE:

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