United States        Office of
         Environmental Protection     Solid Waste and
         Agency          Emergency Response
                        7  ^
                                 u « ,
                               December 1994
         Superiund
xvEPA    USEPA CONTRACT
         LABORATORY PROGRAM

         DRAFT STATEMENT OF WORK
         FOR QUICK TURNAROUND
         ANALYSIS

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                                  9240.1-19
                                  PB95-963523
                                  EPA540/R-94/086
                                                  DRAFT
USEPA CONTR&CT IABORAltH|r, PROGRAM


     DRAFT STATEMENT  OF WORK


               FOR ;


          TURNAROUND  ANALYSIS
           -

          -" ,   8/94    ' :
                   U.S. Environmental Protection Agency
                   Region 5, Library (PL-12J)
                   77 West  Jackson Boulevard,  12th Floor
                   Chicago,  IL  60604-3590

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0
                                                                                       DRAFT

                                             STATEMENT OF WORK


                                             TABLE  OF CONTENTS        :


                    EXHIBIT A:   SUMMARY OF REQUIREMENTS

                    EXHIBIT B:   REPORTING AND DELIVERABLES REQUIREMENTS    "   ••  ..

                    EXHIBIT C:   QTM TARGET COMPOUND LIST (QfCL) AND CONTRACT REQUIEM)
                                QUANTITATION LIMITS (CRQL)

                    EXHIBIT D:   ANALYTICAL METHODS       :           :

                    EXHIBIT E:   QUALITY ASSURANCE/QUALITY CONTROL? tEQUIREMENTS

                    EXHIBIT F:   CHAIN -OF -CUSTODY,  DOCUMENT CONTROL; AND STANDARD OPERATING
                                PROCEDURES
                    EXHIBIT G:   GLOSSARY OF TEfQ-ASffii ,MJRONXM LIST

                    EXHIBIT H:   DATA DICTIONARY AUD FORMAT FOR DATA DELIVERABLES IN
                                COMPUTER -READABLE FORMAT

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                                                                         DRAFT

                              TABLE OF  CONTENTS
SECTION I:     Overview	?....:,,;	, A-3

SECTION II:    General Requirements	:,'$&-7

SECTION III:   Specific Requirements	>,»	  A- 9

SECTION IV:    Detailed Technical and Management Requirements	A-19
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                                                                          DRAFT

                                   SECTION I

                                    OVERVIEW

The purpose of this Quick Turnaround Statement of Worfc (SOW) is to provide
analytical methods and associated quality control (QO) procedures and criteria
that will result  in the rapid analysis of hazardous .waste samples and the
generation of data of  known and documented quality for use by-'tfee United
States Environmental Protection Agency (EPA).  EPA will use tHes&vdata to
answer questions  and make decisions  relating to the characterization and
clean-up of sites contaminated with chemicals "that pose significant rissfes to
public health and the  environment.   The analytical method turnaround times are
designed to meet  client needs when activities on site afce awaiting a quick
answer.  Under this contract,  laboratories: :are requireiflf-to analyze and report
data from a maximum of 30 fractional sample,'-analyses f>er day for a maximum of
three different fractions (e.g.,  phenols, volaitilesj and pesticides), and
report the electronic  summary data within 48 hours -after Validated Time of
Sample Receipt (VTSR)  and hardcopy data within seven -'days after VTSR.  If
analyses for more than three fractions are requested f ok ;a-.given Batch of
samples at the time of sample scheduling, the Contractor laboratory shall
report the electronic  summary data t'           'S

•     Electronic  data    - -    witinixi 48 hours after VTSR if three or fewer
                  j             fractional, analyses are performed for a given
                         ..„; , within 72  hours after VTSR if more than three
                              •ipeaetional analyses are performed for a given
              •':„ ,-: ,   •-        Batch sof samples.
              ';   r' •-• ^ -  ' r*          *'•* *•"-;
      Hacdcepy data    " •**;,.,..  within seven days  after VTSR if three or fewer
       •';1,                  :r fractional analyses are performed for a given
      a; •"                    pfiatch of samples.
     «::,                     s«
     '" -ys'\.              --  .-/fejwithin eight days  after VTSR if more than three
         •"*-;„;: ,              -J';'fractional analyses are performed for a given
            -M   f,,.,          1  ;" Batch of samples.
              ; ;,

      Preliminary Fonp >I?:resuits via telefacsimile (fax) or telephone (if
      requested during"ittie scheduling and sample receipt process) --
      preliminary Form I analytical results for  1-10 fractional sample

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                                                                          DRAFT

      analyses within 24 hours  after VTSR.  These  are  limited to a maximum of
      five  (5) requests per seven calendar days.

•     Preliminary raw data results  if requested before receipt of hardcopy
      data  -- within four hours after request.

Analytical  data generated under this SOW will be used  to  answer questions and
make decisions during all phases of the Superfund  site inspection, site
characterization, and remediation process.  This SOW can  be  useU4;< therefore,
for site inspections, site characterizations, jttseatability studies^  i
engineering designs, remedial actions, time-critical removal assessments and
removals, and non-time-critical removal assessments  and removals.

During the  site inspection phase, a site is assessed Co> 'determine if it should
be placed on the National Priorities List fc" -•' ^S' .
                                 "i|v      ' ":*'-:!'>;••>'  -/•   -
Each phase, including emergency removal activities,T'requires rapid turnaround
of certain  analytical data for  the  Siiperfund ipcogram to operate most
effectively.  Since it usually  takes ffiaisy saaftles  to characterize the extent
of contamination, determine the cleanup*tee!mology,  determine when the site
has been cleaned to acceptable  contaminatttjfjlevels, and perform monitoring
analyses, it is anticipated -tfattt ,this SOW will be  used frequently for these
activities, as well as'for identifying critical samples for  confirmatory
analysis.            ,, '?'"
It should be note^^feowever,  tha^ajtsi^s.^QW...!^  not a substitute for the Multi-
Media, Multi-Concerttca^ion Sta®ia8SSKli,i6«idt (SOW)  for Organics Analysis,
which requires different -analytical  methods, QC,  documentation, and data
turnaround time.  The  analy$9*^l methods  and their associated QC requirements
as outlined in this  SOW have^ijjfeSiBssespecially designed for rapid turnaround of
analytical data, ^aistfare not to b^|JB^d in place of the analytical methods
outlined in^:fcfce:MuTt^4ti^tlia,  Multi"-SiWeentration SOW for Organics Analysis.
         •&'            'vA.
This SOW1. ws designed to ge^^ate analytical  data for monitoring the presence
of frefrtehtly occurring organic compounds, to  aid in assessing the extent of
contaailjtation, and to  monitw||iicleanup  technologies for effectiveness.  It is
also d^l^Pied to generate  bo^t qualitative and quantitative analytical data.
As a result:/: sthe analytical ,'^ethods  and the  QC requirements have been designed
to minimize ISjHsteactor timefJInd effort per sample while still providing data
users with analytical  datspiof known  quality.
                   "''''• li~tti-~
Because these analytical.! methods do  not involve the qualitative confirmation
of the presence of target  compounds, the  compound class (e.g., polynuclear

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                                                                           DRAFT

 aromatic hydrocarbons) or compound(s) of interest (e.g., benzopyrene)  for a
 site  should already be known from previous assessments.  General  instances for
 which this  SOW may be appropriate include, but are not limited, to  the
 following activities.

 •      Directing sampling efforts.

 •      Screening sites for organic contaminants (presence/absence).
                                                                -   ';
 •      Provision of target compound-specific analyses (identification and
       quantitation).                                                    ;

 •      Identifying the most appropriate or critical samples for confirmatory
       analysis.                            r

 •      Monitoring presence of target compounds'. ;s  •  ,'

 •      Optimizing analysis conditions (e.g., dilutions^ extract clean-up)  for
       confirmatory analysis.                           :
                                  , ™ -
 •      Whenever activities on-sitej;r«gpi3?e §a,;quick answer.

 •      Whenever on-site feedback is required.   ,!'        ,

 •      Interim  decisions regarding site^ontamlnation and cleanup.

 Specific instances for which this SOW may t»e  appropriate include but are  not
 limited to  the following aet&vlties.       " ';
                                 I*'
 Screening activities..'-           ">~,

 •      Identification^of contamin&iied, and, potentially uncontaminated locations.

 •      Preliminary quanititati.on of pollutants  or target compounds.

 •      Selection  of sampling
•     Optinfealtrloh of ,a-sampling grid/
          * j r *             >*. *
Monitori&k"activities     '•?;'•<
                            \^ %
             and safety of affected residents.
                             Zf
                             4;
                   well placwient.
           vj -? •-,            ; s,
             «';;>.         ^;:
      Selection'
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                                                                          DRAFT

•     Monitoring  the horizontal and vertical contamination plume during an
      extent of contamination study.

•     Monitoring  or testing the effectiveness of a treatability study or
      engineering design prior to confirmatory analysis.

•     Interim actions  (e.g.,  removal,  containment),

•     Monitoring  a cleanup  operation prior to confirmatory analysis.

•     Potential Responsible Party (PRP)  oversight.

Other Activities

•     Preliminary data for  public relations,,-f,       ••

•     Detection of potential sources  of  contaminati*j»n and exposure pathways.

•     Preliminary or interim evaluation  of remedial alternatives or removal
      technologies.               :  ,   ,
                                    "" :  ^;   -v
•     Dictation of disposal requirements of'%as^e -g«Hfrated on-site.
                                               ",3*'   ^ ,  -
•     Waste compatibility.             „       ?;
                                       I'!     .  K
•     Identification of clean-up technologies.

•     Supplemental data collection (for  addressing data gaps).
                        '"- " "'""^ilr          ' :*'
Analytical data generated using l|tuLs  SOW and "ttsed without confirmatory data
may be inappropriatsrflfor certainl^inal decisions,  such as determining National
Priorities Listings ,-CNPL) of sit364iU,o4entif,ipation °^ remedial alternatives,
final risk assessment*,; and cl eaz«lp I action slimits.  Analytical data generated
using this SOW may, howe^WfeT,  be used to  assist in making these decisions if
more quantitative, confirniktSssy analytical data are also provided.
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                                                                          DRAFT

                                   SECTION II

                              GENERAL REQUIREMENTS

Under  this  SOW,  Contractor Laboratories (hereafter called Contractor or
Laboratory)  shall  analyze water,  soil/solid (e.g., sediment and sludge),
oil/oily  (e.g.,  drum waste and oily mixtures), and wipe samples for volatiles,
pesticides,  polychlorinated biphenyls (PCBs) as Aroclors, polynuclear aromatic
hydrocarbons (PAHs),  and phenolic compounds.  Volatiles shall beuasialyzed by a
heated headspace sampler followed by gas chroraatographic (GC) analysis using
photo-ionization (PID)  and electrolytic conductivity (ELCD) detectors fti
series.   Pesticides,  Aroclors,  PAHs,  and phenols shall be analyzed by solid
phase  or  solvent extraction followed by GG>; analysis.  Pesticides and Aroclors
shall  be  detected  by electron capture (BCD).  PAHs shall be detected by flame
ionization  (FID),  and phenols shall be detected, by P£& "or FID.  Exhibit D of
this SOW  specifies the  protocols  for each method.   ';

The Contractor shall transfer a summary of the analytical and QC data to the
appropriate  EPA  official or Region and to the CLP Analytical Services Support
(CLASS) contractor via  the specified electronic data transfer and data
evaluation  system  within 48 hours?l|-bx 72 hoars, if more than three fractions
are analyzed) after  VTSR.   Seven  Says after ''V'ESS. -(«%ght-days after VTSR if
more than three  fractions are analyzed), the Coiitractdx stiall send the
Complete  Batch File  to  the appropriate, Region-lSCC and the complete data
package to  the CLASS contractor and to-'the Region-Client.  Exhibit B specifies
the deliverables and turnaround times re^uifeed by this SOW.  In addition, if
requested during the sample scheduling anclg;receipt process, the Laboratory
shall  report preliminary -1?pie$ji>Ij;vsample res-alts for 1-10 fractional analyses
via fax or  telephone to,;,the reqwe^stor within ,24 hours after VTSR (limited to a
maximum of  five  requests per severikcalendar days).  If requested before
receipt of hardcopy.jiiata,  the ComJicactor shall «end by fax copies of
preliminary  raw  da£a;:results wit^3pt,,four,vhours of the request (see Exhibit B
for additional detail's)«       l,s:fc"'r  ,{.', „•',.

The Quality  Assurance (QA) - program for this  SOW consists of QC samples, sample
preparation  QC procedures,  ins^aru^aent QC procedures as defined in the
analytical methcals .{P&kibit D) • a|jd-external procedures specified in Exhibit
E.  The QA. ^pe%ram'; %!*$«&includes' 
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                                                                          DRAFT

analyzed.  An instrument blank  and PVS  shall be  performed at the end of each
24-hour analytical sequence.  The specific  procedures to be followed are
outlined in Exhibit D of this SOW.

Sample analysis data, sample documentation, and  other;;deliverables shall be
reported as specified in Exhibit B.  Exhibit C of tills ,S®W specifies the
target compounds and their contract required quantisation limits (CRQL).
Exhibits E and F outline the chain-of-custody  and document eo«fcEol procedures
which shall be followed with each Batch of  samples.   Exhibit G, itfe^ glossary
of terms and acronym list, is provided  to ensure a proper under stawlis^; of
language utilized in this SOW.  When a  term IS' used  in the SOW without ••••
explanation, the glossary definition shallJ&erapplicable.  Specifications for
reporting data in computer-readable form appear  in Exhli&t H.  Prior to
accepting any samples from the  Agency,  ttee,Contractor'isfaall have in-house, the
appropriate standards for all target compcnassds, listedlin Exhibit C.
                                              ,\ .'"!> '£*
                                              '"•  3*
The samples to be analyzed by the Laboratory are'-from known or suspected
hazardous waste sites and may contain hazardous  organic^and/or inorganic
materials which could present a significant risk to  human;health and a hazard
to Laboratory instrumentation/equipment.  The  Contractor sh»tild be aware of
the potential hazards associated|w|a4^|i^;is^3i41ing and analyses of these
samples.  It is the Contractor's^^ponslftflSCtlr*fb -'take all necessary measures
to ensure the health and safety of%l±s  employeJ&S;, aiicMfeQlmaintain its
analytical instruments in good  workiiag, condition.
                                     v';     ,:>/;. '•
In addition, the Contractor must be awax^-qfe the importance of maintaining the
integrity of the data generated under thilsj'fcontract,  as the data may be used
to make important decisi«ns;;£«sgarding pub lip, -health  and environmental welfare.
Data generated under tills contuse may  also'$*« used  in litigation against
potential responsibly,parties  (P&S) in the eiteorcement of Superfund
legislation.  Consespbently, the ^itractor  shall take appropriate steps to
ensure the integriSf-; of all datall^ne.^atejd^under this contract.
                    "            ''          '"
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                                                                          DRAFT

                                   SECTION  III

                             SPECIFIC REQUIREMENTS

       Good Laboratory Practices and Contractor Tasks
      During the  length of this contract,  the Contractor -sSfeaJU- adhere tq good
      laboratory  practices and good automated laboratory practices.
      Requirements  for maintaining good laboratory practices and; good
      automated laboratory practices are provided in Exhibit E of this SOW.

      For each sample ,  the Contractor shall perform certain tasks .  These
      tasks are:  (1) receive  and prepare eBSrironmental .samples; (2) analyze
      samples for organic  compounds; (3) qualitatively 'identify the presence
      of organic  compounds in the samples ;  1(4) quantitatively identify the
      concentrations of organic compounds  in tfae samples; (5) adhere to QC
      procedures  outlined  in  this SOW;  and (6) prepare, report, and deliver
      the data.   These tasks  are specifically outlined as follows.

1.1   Task 1 - Receive and prepare environmental samples. •;

      1.1.1 The Contractor shall r&eeive and-lliaadle: ^samples  under the
            chain- of -custody  procedures described in Ixblbits E and F.

      1.1.2 The Contractor shall prepare samples as described in Exhibit D .

1 . 2   Task 2 - Analyze  samples  for organic .compounds .

      1.2.1 Extracts and aliquoiss prepared  £h ;Task 1 shall be analyzed by the
            GC techniques  described in  the  methodologies given in Exhibit D
            for the,rtiarget compoutiils listed in Exhibit C.
      1.2.2 Automatecomputer ^IC^psps, iaa^r; Jb'e  used to facilitate the
            qualitative "identification  and  quantitation of sample results.

1.3   Task 3 - Qualitative identification of  the  organic compounds identified
      in Task -2=.;  ";  : ;          *•-.- ;/
            ;1 , ' -* '  ' " *  *-~;~* ' ;' •         ^  *
      1.3r,l ;the compounds5 .analyzed by GC techniques and initially identified
        J', r in Task 2 shally^e verified by  an analyst competent in the
       ; ;1   interpretation o|;;*GC chromatograms  by comparison of initial
     ;;;:,'     calibration relative or absolute  retention time to the relative or
            absolute retenti&ik time of  the  suspected compound in the sample as
              ecified in Exhibit D.
      1.3.2 If'k~"C8fflpoundf,ai*alyzed by GC techniques  and initially identified
            in Tas"fe2",fsaitoot be verified by the  criteria described above,  but
            in the technical judgment of the GC  interpretation specialist  the
            identification is correct, then the  Contractor  shall  report  that

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                                                                          DRAFT

            identification, comment accordingly  in  the  Batch Narrative,  and
            proceed with quantitation  in Task 4.

1.4   Task 4 - Quantitation of organic compounds verified in Task 3.

      1.4.1 The Contractor shall quantitate  compounds attalyzed by GC
            techniques and identified  and  qualified in  tasks 2 and 3  by the
            external standard method as described in Exhibit* D,,  Quantitation
            shall be performed using calibration factors  determined. during the
            initial calibration.              ,,                    ">'•
                                              ;,                     '"   "''
      1.4.2 The Contractor shall perform a daily one-point calibration check,
            verify its linearity by comparison to the jaajtial calibration, and
            perform a PVS analysis as  outlined in Exhibit D to ensure that
            instrument stability and sensitifety were kaintained during sample
            analysis.                        "  *,;   ('• -
                                                 s *   ' ',
1.5   Task 5 - Adherence to quality control  and  quality .assurance procedures.

      1.5.1 The Contractor shall .adhere to all specific QC procedures
            described in Exhibits ID *«nd£f(^.j|>pB|cedures described in Exhibit E.
            Records documenting tfoe -.use 'orv<€M'$sj*e«i'£i
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                                                                          DRAFT

      1.5.6 Additional QC shall be conducted in the form of the analysis of
            Performance Evaluation (PE) check samples submitted to the
            Laboratory by the  Agency.   The results of all such control or PE
            check  samples may  be used as grounds for termination of contracts
            of non-compliant Contractors.   " Compliant iferformance" is defined
            as that which yields correct compound identification and
            concentration values as determined by ^t&e Ageijcy:, as well as
            meeting the contract requirements for analysis OE^tibit D) , QA/QC
            (Exhibit  E) ,  data  reporting and other deliverables :<,EjJ6hibits B and
            H) , and sample custody, sample documentation, and standard
            operating procedure (SOP)  documentation (Exhibits E and F}>

1.6   Task 6  - Prepare, report,  and deliver' the data,  {"

      Samples shall be analyzed and the data-iseportedvto EPA within the
      specified turnaround times following VTS$U:; - ,Th'e? Contractor shall prepare
      electronic and  hardcopy  data according to irhe procedures outlined in
      Exhibit B.   The Contractor shall report electronic, hardcopy, and
      preliminary  data according to the formats, order ;* assJ , turnaround times
      required by  this contract. ,-,Ihe Contractor shall deliver to EPA all
      summary data, raw data,  QC,;^!6a,!:attd;'chai.n-of -custody information
      generated from  the tasks described ahoveiN  :  •••,;,

2     Data Format                    <   ,

      The Contractor  shall use EPA-provided formats for reporting the data
      generated from  the tasks described abpve.

2.1   The Contractor  shall be  responsible for ^completing and delivering sample
      and QC data  suigBary electronically in tt*e format specified in this SOW
      and within thefetime specifics in the Contract Performance/Delivery
      Schedule.  The ;::f ormats for fefee ..anaJLytical data are contained in Exhibits
      B and H.     " ' ;'; ,»,      .\.:&. t\ ..... 'i "c

2.2   EPA will consider fomafcs, other than those designated by EPA to be
      non- compliant and will'cipnst.itute unacceptable data.  Resubmission in
      the speoisEifed;?f5Qxmat at  no ;^ddi.tional cost to the Government shall be
              '  '   '              '
2.3   Com|mter- generated fclcJBs  may be submitted in the hardcopy data
              s) provided thai;  the forms are in exact EPA format, as specified
         Exhibit B.   Exact EBjji  format means that the order and reporting of
              the same  as onlpach EPA- required form, including form numbers
      and "sfcit&es , page  numbeHfes,  and header information.
             * -'^«*           ,':i-'
2.4   The hardcopgf%4ata submitted to the Region shall contain all information
      reported on fhfe :«l«e"ltronic data transfer (EOT) .   The Contractor shall
      ensure that the -"ilaSormation contained in the electronic data summary is
      consistent with the information contained in the hardcopy data.  If

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                                                                          DRAFT

      after EPA inspection  discrepancies  are found,  the Contractor shall be
      required to re submit  either  or both sets of data at no additional cost
      to the Government.

3     Analytical Equipment

      The Contractor shall  provide analytical equipment and. technical
      expertise for this contract.

3.1   All equipment and instrumentation specified in this SOW are~T»gjjiired and
      shall be in the possession of the Contractor and in good operatiijig
      condition at all times during the length of this contract.  The
      Contractor shall ensure  that in  the jewnt of instrument or equipment
      failure, backup instrumentation  or  ^liipment in sgeod operating condition
      are available to perform sample  preparation and Analysis.  It is
      recommended that the  Contractor  install "<;$essge%a:otectors and have a
      temporary backup power supply source  in order f-to protect analytical
      instruments and equipment in the event of a temporary electrical
      disruption or power surge.                       ;  \,
3.2   The Contractor shall have «t&s^wgjfiC capability to meet all the terms
      and conditions of the contrfttst:.   Iri^t^ffleasi; aSftpiirements are defined in
      I FB' Attachment C, Bidder Responsibility. f jftie  Contractor shall have, at
      a minimum, all analytical equipment  required for this contract and which
      are stated in this contract  at ^&e timerof  contract award.
3.3   The Contractor shall have five dedicated GC  instrument systems. Each
      system shall have .the '-following, as Ascribed in Exhibit D:
                        ~ -    ' vi x / N ~           • /,
                      -; -        -\SL<"           -, :~
      m     The GC fqpE^volatile saaalysis shall -be  equipped with a heated
            automateli*headspace simpler , capillary column,  and an ELCD and PID
            detectpfe-gin series; ^vV,,., ,„„„. ,
                    ^ 3£  ;        •'' "&^£" ^ '?;" - '-1 1"  ; , < ^f
      •     The GCs for pesticide and  Aroclor  analyses shall be equipped with
            a capillary column  and an  ECD;
            Tb.fi! .'jSC^'for :,-PAH analyslf.;;sshall be  equipped with a capillary column
            The GC for phei^JIs analysis shall  be  equipped with a capillary
            column and an FlSu-or PID.
                             , ,
              Functional RegtcLrements
      The miB^BBpa functiona^V±equirements necessary to meet the terms and
      conditionS?X3^:-this jepiitract are listed below and described in IFB
      Atachment C."J3Tj^-..Cji*trtractor shall  designate  and utilize key personnel
      to perform theseiyjutictions.  EPA reserves  the right to review personnel
      qualifications and experience, and  take  contract action as appropriate.

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                                                                     DRAFT

 The minimal  functional requirements are listed below and described in
 detail later in this  Exhibit:

 •     GC Laboratory Supervisor;

 •     Sample Preparation Laboratory Supervisor;-

 •     Quality Assurance Officer;

 •     Systems Manager;                                       !

 •     GC Operators;

 •     Extraction/Concentration  Experts;

 •     Programmer Analyst;  and

 •     Technical Staff Back-up.

 Response to  Requests       *>

 After the Region's  receipt *<$£ »the  hardcopty da*:a,,  the Contractor shall
 respond within  two  days or wiiltin  specified  times -fo requests from data
 recipients for additional  information ox ^explanations that result from
 the Government's inspection and reviewfl   If  before  the hardcopy data are
 due, additional information such as jofev data are  requested,  the
 Laboratory shall deliver the information  via fax  to the requestor within
 four hours of the ,,re$ue$£  (see Exhibit 3  for additional information).
 If requested durijsg the 'stefaeduling and -sample receipt process,  the
 Laboratory shallVdeliver bylgfax or telephone preliminary Form I
 analytical results  for  l-lQ/^ractional sample analyses to the requestor
 within 24 hoars after VTSR4Mmi.tedjto five  requests per seven calendar
                                        '
 Sample Shipment and 'gjbfcacae of Samples and Sample  Extracts
 Sample stejsiBenits, to the Laboratory will be coordinated by  the  CLASS
 contraiejiior acti*ig^|i behalf 'oirjthe EPA Headquarters Administrative
 Project Officer (ABfi)»,  The Contractor shall communicate with  designated
 CMSS contractor personnel or EPA Regional officials by
 telecommunication as «feoessary throughout the process of sample
ff«heduling, shipment, Sp^lysis, and data reporting, to ensure  that
•"e-s are properly processed.
 The Con^f^por shall jps|e serve all sample extracts after analysis  in
 bottles 6T-iVfcafls witjb Teflon- lined septa, and shall maintain  stored
 extracts at '4*C; %±t2$C') .   The Contractor is required to retain the
 sample extracts "f^r '21 days after hardcopy data submission  and samples
 for 60 days after Tiardcopy data submission.  During that time, the
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                                                                          DRAFT

      Contractor shall submit the extracts as directed within seven days after
      request, as specified in the Contract Performance/Delivery Schedule.

7     Non-Routine Situations

      The Contractor shall handle non-routine situaaeioas  in the  manner stated
      below.

7.1   If there are problems with the samples, sample documentation,  or
      paperwork, the Contractor shall immediately contact the CLASS contractor
      or the appropriate Regional official for resolution.   Examples &£•,-
      problems include mixed media, broken ox''leaking containers,  Quick
      Turnaround Method Traffic Report/Chaitj-of-Custody 
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                                                                           DRAFT

      report  such deviations to the APO so that payment considerations  can be
      taken into  account).

      Reanalysis  and Reextraction of Samples

      Conditions  for re-extraction and reanalysis are specified in Exhibit D
      of  this  SOW.   All other re-extractions and/or' reanalyzes of samples can
      only be  authorized by the CLASS contractor acting on "b^fe^-lf of  the
      Regional TPO or Headquarters APO.  Such reanalyses must be.Jformally
      scheduled after the data for the original, ^analysis has been '^ieLlyered.
      In  addition,  the Contractor may not stop;-an analysis once the   <
      preparation,  extraction,  or analysis h»s begun, unless authorized by the
      CLASS contractor acting on behalf of t&e Regional IPO or Headquarters
      APO.                                ,   '         ,, L

      Cases and Batches of  Samples              ' -,   *

      Sample analyses will  be scheduled by groups of" samples, each defined as
      a "Case," and identified by a unique EPA Case and::'Ba,tch number  assigned
      by  the CLASS  contractor.     ><:  >v.
9.1   A Case comprises  a group  of Camples colEUfeefeecL' at one site or
      geographical  area over a  f ini'fce,, time per^eid, 'and «lll include one  or
      more field  samples with associated blanks and LCSs.  A Case of samples
      may be shipped to the  Contractor in a^sijigle shipment or multiple
      shipments over a  period of time,  ctepeiiding on the size of the Case.
                                           .. <•&
9.2   A Case consists of a«e;>ers =more Batch^es) .  A Batch is defined by the
      following,  whichever is most: frequent:  ;,
                     :?'            if
      •     Each  Case of field  samples received, OR
      •     Each  grcusip of  field sJMMqpas,''^NjBL*to 30 fractional analyses) within
            a Case  received, in one day.

9.3   All data for  all samples,, i**, a. Batch are due concurrently to all data
      recipien$is;;ias. -Stipulated itf tke Delivery Schedule in Exhibit B, Section
      I.  H#cd<*opy  d'ata'J'Jpa:  all samplfe  within a Batch shall be submitted in
      one| package in  the'^Ster specified in Exhibit B.  The "Batch No." will
      bejiifidicated  on the  C^6| TR/COC.  If however,  the "Batch No." is not
          cated on  the QTM ili^COC,  the Laboratory shall assign it as the EPA
             number of the fficst sample  received in the Batch.  When several
              are received together in the first Batch shipment, the "Batch
                  be the  lowest sample  number (considering both alpha and
      numeri<*|d£«ignations^ ,-iii the first group of samples received under the
      Batch.  Tffe -"Batch Ni>."  shall be reported on all data reporting forms.

9.4   The Batch receipt ;
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                                                                          DRAFT

9.5   If the Laboratory receives more than  30  fractional sample analyses in a
      given day, then the fractional samples analyses  that exceed the 30
      (e.g., five if 35 fractional sample analyses  were .received) would be
      considered a separate Batch, and the  VTSR would  %fe 8 a.m. the following
      day.

      VTSR for Batch Arrivals on Monday through Thursday  :,•

      If the Batch arrives before 5 p.m. Eastern Standard Time (ESI) ,  the
      electronic sample and QC data for all santples within the Batch are due
      within the specified turnaround time  following VTSR.            ,-
                                            -i
      If a Batch is received after 5 p.m. JEST,  the  VTSB? , shall be at 8 a.m. EST
      the following day, and the electronic sample  and':J3C data for all samples
      within the Batch are due within the specified ..turnaround time following
      VTSR.                                    •>     [•

      VTSR for Batch Arrivals on Friday                 ,,.

      If a Batch is received on a, Friday before 5 p.m. EST; the VTSR shall be
      at 5 p.m. EST Saturday, and< 1:he.||ill%Et;r
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                                                                           DRAFT

       If more than three fractional analyses are requested and performed,  the
       electronic sample and QC data are due 72 hours  after VTSR.   If more than
       three fractional analyses are requested and performed,  the hardcopy data
       is due eight days after VTSR.

 9.6    If the VTSR date is adjusted for samples received'during non-routine
       working hours as described in Exhibit A, Section III/-paragraph 9.5,  the
       Laboratory shall note this in the Batch Narrative(s)  as ;described  in
       Exhibit B,  Section III, paragraph 8.                       /;;

 9.7    The Contractor is responsible for identifying each Batch as  samples  are
       received,  through proper sample documentation as described in  Exhibit B
       and through communication with the CLASS contractor  personnel  or the
       designated Regional official.                   >! ,

 9.8    EPA Case numbers (including Batch numbers), and-UFA sample numbers  shall
       be used by the Contractor in identifying s'ajofples received under this
       contract.   The Contractor shall use these numbexs in reports,  written
       correspondence,  and verbal correspondence.         " ,  -,

 10     Traffic Report/Chain-of-Custody,  f  *   »

       The Contractor shall adhere trojall chain~d£-custody procedures  stated or
       described  in this SOW as indicated below.

 10.1   The Contractor shall adhere to all chain-of-custody procedures  described
       in Exhibits E and F.   Documentation,;,/as described therein, shall be
       required to show that ^ll>-proceduresr'.are being strictly followed.  This
       documentation shall "be reacted as part sof  the Complete Batch  File  (see
       Exhibit B).    ,?„-,        ''=%

 10.2   Each sample received by tha-appn^actxjr shall be labeled with an EPA
       sample  number. ^Iffee QTM TM$jj^$£®ic»£&liat accompany the sample  will bear
       the  EPA sample number and will contain descriptive  information  regarding
       the  sample.   The Contractor shall complete  and sign the QTM TR/COC forms
       on  the  date and  at the"-tfBffie:,,of sample  receipt,  and report the condition
       of  each saajpl* -sand contaihet*  ?,
10.3  The^ClWitractor  shall, .submit  signed copies of the QTM TR/COC forms for
      aliasamples within  a "S%tch to  the  CLASS  contractor within three calendar
      days following  receipt%«f the  Batch.   These forms shall be submitted in
      ilptch sets with a Batct-'"Cover  Sheet containing information regarding the
      "Blffc&h,  The Contractor ;»>«nall prepare a Batch set of QTM TR/COC forms by
      clip$34jg together all  $M TR/COC forms for that Batch.
10 . 4  Samples rotttsj-nely will-- be shipped  to  the  Laboratory through an overnight
      delivery servicses,-,, However, as necessary,  the Laboratory shall be
      responsible for dpcy handling or processing required for the receipt of
      sample shipments, including pick-up of  samples at the nearest servicing

                                                                         08/23/94
                                     A-17

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                                                                          DRAFT

      airport, bus  station,  or  other carrier service within the Laboratory's
      geographical  area.  The Laboratory shall be available to receive sample
      shipments at  any time  the delivery service is operating, including
      Saturdays and Sundays .

10.5  The Contractor shall resolve  all missing or inaccurate information with
      the CLASS contractor or with  the designated Regional official as a
      requirement of this contract.

11    Acceptance of Samples

      The Contractor shall accept all sample's "scheduled by EPA, provided that
      the total number of samples received -,& any calendar month does not
      exceed the monthly limitation state4 3t,n this contract.  Should the
      Contractor elect to accept additional ^samples, s-tfce Contractor shall
      remain bound  by all contract  requirements for&imalysis of those samples
      accepted.                                  ••',  ?

12    Summary of Important Requirements                ,:  ;

      The Laboratory shall adhez» -^ j$33.;-|;zeguirements in this SOW contract and
      in particular to the following.      "-•  1. •• \ , '.  ;

12.1  The Laboratory shall not  deviate;: from tie requirements of this
                                       <     -
12.2  The Laboratory shall follow good laboratory practices and good automated
      laboratory practices.                 '

12.3  Only the Regional.. 13PO  arid Headquaters <&£0 shall have the authority to
      provide instructaons and  c*ar if ications ; tso a Contractor regarding this
      sow.          .;•'            =;•
                                                                      SOW.
12.4  Re-extractiorf-asfd/or  reaa^^:£,o»£ -Dapples ,  not specifically required by
      this SOW, can oriiy&e, authorized by  the CLASS contractor acting on
      behalf of the Regional; JJCfO  or  Headquarters APO.   Such reanalysis must be
      formally scheduled after?i|la.ta  for the original analysis has been
      delivered,.  ' , ';  „         "  ;;-

12.5  The.-J|iifhtractor may\-sas>t stop an analysis once it has accepted samples for
      analysis, unless autffe^&ized by the Headquarters APO or the Regional TPO.
12.6 
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                                                                          DRAFT

                                   SECTION IV

                DETAILED TECHNICAL AND MANAGEMENT REQUIREMENTS

As cited in Section III,  the  Contractor shall have the following technical and
management capabilities  specified below.                ,,

1     TECHNICAL CAPABILITY                        :

1 . 1   Technical Supervisory Personnel          ,                    ;

      1.1.1 GC Laboratory Supervisor

                  1.1.1.1    Responsible , far all technical efforts of the GC
                              laboratory  t&.vieaet  alloterms and conditions of
                              this contract.    ;   ,  *~

                  1.1.1.2    Qualifications:         :

                         1.1.1.2.1  ..Education:

                                  '•  fjMinimum 6£cB8cbeJ(pr^.s  degree in chemistry
                                    •-.or any  scientific/engineering discipline.

                         1.1.1.2.2   Experience:
                                         fcffli: of  three years  of environmental
                                     laboratory  GC  experience,  including at
                                     least  one^ear of supervisory experience.
      1.1.2 Sample Preparation Laboratory  Supervisor
                                              all  technical  efforts of sample
                              preparations to meet all  terms and conditions of
                             -fsthis contract.
                  'l;ll:.;2.2     Qualifications:
                      '•'' - ' ''          ' \tf "
                        l:t-l,;,2.2.1   Education:
                                    Minimum of Bachelor's degree  in chemistry
                                    or any scientific/engineering discipline.
                        1 . 1 ,;2£2 . 2   Experience :
                                    Minimum of three years of environmental
                                    laboratory sample preparation experience,
                                    including at least one year of supervisory
                                    experience.

                                                                         08/23/94
                                     A-19

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                                                                   DRAFT

1.1.3 Quality Assurance Officer

            1.1.3.1     Responsible for overseeing the quality assurance
                        aspects of EPA contract :,  .LI.*.:
                              Minimum of Bachelor's degree with four or
                              more intermediate courses in programming,
                            ,i''^information management, database
                            '"sidmagement systems,  or systems
                              requirements analysis.
                  I.i;.||t2.2   Experience:
                              Minimum of three years experience in data
                              or systems management or programming
                              including one year of experience with
                              software utilized for data management and
                              generation of data deliverables.
                                                                  08/23/94
                               A-20

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                                                                          DRAFT
1.2   Technical Staff

      1.2.1 GC Operators

                  1.2.1.1
Responsible for the analysis of samples in
accordance with QTM SOP methodologies using GC
techniques as required under; this contract.
                  1.2.1.2     Qualifications:

                        1.2.1.2.1   Education^
                                    Minimum lof Bachelor's degree in chemistry
                                    or any, scientific/engineering discipline.
                        1.2.1.2.2   Experience;}
                                    One year of experience in operating and
                                    maintaining a GC and performing
                                   .environmental analysis utilizing GC
                                    $&eitadLqttes,sand interpreting GC data for
                                    volatile^,^E£Hs,v phenols, pesticides, and
                                    Aroclors,  ta& wltti af Bachelor' s degree in
                                    Chemistry !«r a scientific/engineering
                                    discipline, or in lieu of the Bachelor's
                                    degree,*: three years of experience in
                                    operating and maintaining a GC and
                                    performing environmental analysis
                                    utilizing;GC techniques and interpreting
                                    GC data for volatiles, PAHs,  phenols,
                                    pesticides, and Aroclors.
      1.2.2
                  1.2.2.1 ,  ^Responsible for the clean-up and extraction of
                            -;asaBif>les using solid phase extraction technology
                 !;  :,         ahd -Rising conventional sample preparation
                 '' ; '•  •& i    techhologies.

                  1.2.2.2 >',;, Qualifications:
                        1.2.2^2.1
                            1'
      Education:

      Minimum of High  School  diploma and a
      college level course  in general chemistry.
                                    A-21
                                                                        08/23/94

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                                                                     DRAFT
                  1.2.2.2.2    Experience :
                              Minimum of one yeas of experience  in
                              extraction/concentration of samples  for
                              environmental analysis.
1.2.3 Programmer Analyst
            1.2.3.1     Responsible  for the installation, icijseration and
                        maintenance  of software, hardware, and programs
                        generating,  updating and performing quality
                        control  procedures on analytical databases  and
                        automated deliverables to meet all terms  and
                        conditions -&£ this contract .
                                     '•f two years experience in  systems
                 ;-'       ,,,.},    or applications programming including one
               s  ,         "' ;.  year of e^ierience with analytical  data
             ;;             ;"4:  management >«'s of tware .
1.2.4 Back-Up-":Fr0grammer

      Due to the coapiigacity  of the  QTM software and the electronic  data
      transfer system, ^jtfc'.sis highly recommended that a back-up
                 analyst "1»i.  s|jade  available to ensure that all QTM data
               j,.-3:eguirementsS:«aslfspecified in the contract are met.
      Technical Stafff&ack-Up
            The bidder",la^iall  have a minimum of one chemist available  at
            any one ti4»e  as a back-up technical person with the
            following!|<|ealifications,  to ensure continuous operations to
            accompli.stlfthe required work as specified by this  contract.
                                                                    08/23/94
                                A- 22

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                                                                          DRAFT
                  1.2.5.1
                  1.2.5.2
1.3   Facilities
                         Education:

                         Minimum of Bachelor's  degree in chemistry or any
                         scientific/engineering discipline.

                         Experience: Bachelor's -
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                                                                           DRAFT

            hydrocarbon/pesticide/PCB samples, phenol/polycyclic aromatic
            hvdrocarbon/pesticide/PCB standards shall each be stored
            separately.   Samples shall be stored in an atmosphere demonstrated
            to be  free from all potential contaminants.  Volatile samples
            shall  be  stored in a refrigerator used oidy for storage of
            volatile  samples from this contract.  YoLafctle samples for other
            contracts shall be stored in other refrigerators:.,

      1.3.3 Sample Preparation Area

            Adequate,  contamination-free, well-ventilated work space provided
            with:

            •      Benches with chemical resistant tops .and exhaust hoods
                   (Note:  Standards shall b% .prepared sin a glove box or
                   isolated area);            !  "•     ,'

            •      Source  of distilled or demineralia«d ..organic - free water; and

            •      Analytical bala»ce,,(s) located away from dtiaft and rapid
                   change  in tempt^ataqtr*;,'.-;, -,

      1.3".4 Standards              "          ,.''•'.    ;

            The Contractor shall have 'la-hoiase appropriate standards for  all
            .target compounds listed in EsthiMt C,  and System Monitor Compounds
            listed in Exhibit D of the SOW vithin seven day's of contract
            receipt.       -  '-\- ,            •
                        t  -   "" ''•
                               ••',-i            ..?.
1.4   Instrumentation;           f  .           ;
                   ; -' '           , |
      At a minimum, Jthe Contracts&rjLshaJLl,.have  the following instruments
      operative at tfee f£ime  of *t&eiyi®ei8Wd^4 ;Site Evaluation and committed for
      the full durationlol'sJthe contract.

      1.4.1 Primary instrumentijrrequirements for 720 fractional sample
            analysis/month capacity
                                                                         08/23/94
                                     A-24

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                                                                     DRAFT
Fraction
Volatiles
PAHs
Phenols
Pesticides
Aroclors
No. of Instrument(s)
1
1
1 .-;
1 "
i :
Type of
Instrument
iSC/PID/ELCD with
heated headspace
: ' device
GC/FID
GC/FID or GS/PIB
GC/ECD
GC/ECD
1.4.2 Secondary  instrument requirements Ifor 720= fractional  sample
      analysis/month capacity             ::  , ,

      The Contractor shall have the following instruments in place and
      operational at any one time as a back-up system:
                                "fttstaataents/GC  Detectors

                                     GC         ''  ''•
                                     EID
     Quantity        '-'

         1

         1                  '  ;

         1      :  :•<
                 ii,
         i-, :  '     \f:.

      ,;  1            
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                                                                           DRAFT

1.5   Data Management  and Handling

      1.5.1 Computer hardware and software requirements - The Contractor shall
            have all necessary computer equipment and software to meet the
            requirements  of the QTM Data Aquisition ,a*Sd Delivery System.   See
            Exhibit B  - On Line Data Transfer System far --.the specific
            requirements .                            '        : ,

      1.5.2 The Contractor shall also be able to submit reports a$d  data
            packages as specified in Exhibit B;,of this SOW.  To complete this
            task,  the  Contractor shall provide .space ,  tables, a fax 'machine,
            and adequate  copy machines to meet the contract requirements.   The
            Contractor shall also designate personnel tbr'perform tasks
            specified  in  the SOW and to uss> the hardwaa?* and software  listed
            above  in the  performance of sueb'<, tasks .   "Hie laboratory manager
            shall  authorize by signing any data'' tha$£:, lias been manually edited.

2     LABORATORY MANAGEMENT CAPABILITY                , ,
                                                       ;-'; : $,
      The Contractor must have an/organization with well-defined
      responsibilities for each i»«^riySual-",ia the management system  to ensure
      sufficient resources for this;- contract: :'«wJK*o ^maintain a successful
      operation.   To establish thi^-.eapabilitypthe Contractor shall designate
      personnel to carry  out the following responsibilities for this contract.
      Functions include,  but are not limited to,  the following.

2.1   Technical Staff

      Responsible  f or .m£L "' technical efforts ';fpr this contract.  The Contractor
      shall have adecjaaate  numberfiif; technical- personnel to meet the
      requirements ,ipf  this contract.
                   r"             * ' °''
2.2   Project Manager  :r ,      *i ^, U. .;V-i,-'"

      Responsible  for  overall,,aspects of this contract (from sample receipt
      through data deliveryy-ijfjHi-fhall be the primary contact for the  EPA
      Headquay-fcetrs i&$0 and Regioi^tt; -IPO.
2.3   Sanmlte Custodian   ^—u,
        ,-- :f;              s*,:;l-

      l^^ponsible for recei-v^ag,  logging,  handling, and storing EPA samples  as
     J:trfequired by this contraie^t.
     •*<* 'si*                     *•''•*
     •*~\  f,- --, -                   - ';,
       •-Lp'is                  - '-
2.4   Qualtty-^Assurance  Officer
           -^^          ^
      Responsibl* ;ppr overaleeing  the QA aspects of the data and reporting
      directly to itp^^X- |tanagement .
                                                                          08/23/94
                                      A-26

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                                                                         DRAFT

2.5   Document Control Officer

      Responsible for all aspect? of data deliverables:  organizing, packaging,
      copying, and delivering.  Responsible for ensuring that all documents
      generated are placed in the Complete Batch File for inventory and are
      delivered to the designated Regional official or -other designated
      receiver(s).
                                                                        08/23/94
                                    A-27

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                                                       DRAFT
                EXHIBIT B   .,
REPORTING AND DELIVEMBtiES  REQUIREMENTS
                                                    08/23/94

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                                                                         DRAFT
                              TABLE OF CONTENTS
                                                                  Page
SECTION I:    Contract Reports/Deliverables Distribution......	 B-3

SECTION II:   Report Descriptions and Order of: Data	
              Deliverables                  -,
SECTION III:  Forms Instruction Guide.

SECTION IV:   Data Reporting Forms	
SECTION V:    On-Line Data Transfer System	
              and Contractor ADP Requirements
B-30

B-48

B-49
                                     B-2
    08/23/94

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                                                                          DRAFT
                                   SECTION I

                  CONTRACT REPORTS/DELIVERABLES  DISTRIBUTION

The following table reiterates the Contract  reporting,,and deliverables
requirements specified in the Contract Schedule  (Contract -Performance/Delivery
Schedule) and specifies the distribution  that  is required for< each
deliverable.  NOTE:  Specific recipient names  and addresses  are .subject to
change during the term of the contract.   The Administrative  Project Officer
will notify the Contractor in writing of  such  changes when they occur..
           Item
Total No.
 Copies
 Delivery
 Schedule
    Distribution
(1) (2)  (3) (4) (5)
      Standard Operating      3 copies
      Procedures
      Sample QTM Traffic      1 copy
      Report/Chain-of-Custody
      form             .   ;   I'- ,

      Sample and QC ' ssnd^or JEMSL-
        ;    " • . - '^
 LV and -as required
 in Exihibit E.

•'3 €ays after       2
 "VESR* of last
 sample in Batch.**

 48 hours after
 VTSR of last
 sample in Batch.
                                        X
                                  To EPA mainframe
                                  computer
      Sample and QC Hardcopyf  2 copies
      Data Package *****    '-^l ,
        ;41
               Batch File***j;:'l package
      Sample and   i.& , '% ;l«-    1 copy
      QC  data summary'-I1 r
      backup in computer
      readable form
      (diskette)
 7 days after VTSR  X
 of last sample in
 Batch. ****
 Submit to EMSL-LV
 within 7 days after
 receipt of written
 request.

 7 days after VTSR
 of last sample in
 Batch. ****

 Retain for 365 days
 after hardcopy data
 submission; or submit
 within 7 days after
 receipt of written
 request by APO
 and/or EMSL/LV.
                                      As directed
                                     B-3
                                                                      08/23/94

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                                                                           DRAFT
               Item
                       Total No.
                        Copies
               Delivery
               Schedule
                       Distribution
                    (1) (2)  (3)  (4)  (5)
       Contract Compliance
       Screening Hardcopy
       Report
                         3 Copies
H.
Extracts
  Lot
 7 Days after VTSR  X
 of last sample In
 Batch. ****       I-.
 Submit to' EMSL-LV ;
 within 7 days after
 receipt: of written
 request .

 Retain for 21.
 .fiays after hardcopy
 data submiss ion ; or
 withiii; 1... daps
 after receipt of
 written request:
 by APO or the
 contractor.
                                             X
                                                                As  directed
J.
      Unused sample volume
      and used sample
      bottles/containers
Quality Assurance,
Plan
                                                          As directed
K.
             suits for
                 analysis  -
v|-ltcopy
                        1 copyv;
                  raw data  "t'11 copy
                                    least* 140' days,
                                    following submission
                                               tical data.
 Maintain on file       5
 wifljjtn 60 days of
 contact award.
 Submit within 7
, days after receipt
iMtlwritten request
 by APO and/or EMSL-
 LV and as required in
 Exhibit E.

 Within 24 hours after
 VTSR,  of last sample in
 Batch, if requested

 Within 4 hours of
 request.
NOTE:  ALL RfeKIXS ARE TO fiilEPORTED TOTAL AND COMPLETE (including Item  C  and
concurrent delfvegry;;;of I tap! D and E) .   Delivery shall be made such that  all
designated recipients ••sa&eied've items D and E on the same calendar day.
                                      B-4
                                                                 08/23/94

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                                                                          DRAFT

The Contractor must be prepared to receive samples within 30 days of the
contract  award and must be capable of receiving the full monthly contract
requirement within 30 days.   EPA shall determine the start-up schedule.

*     VTSR  (Validated Time of Sample Receipt) is the date and time of sample
      receipt  at the Contractor's facility, as recoxdett on the shipper's
      delivery receipt and QTM Traffic Report/Chain-of-Custody forms.

      The VTSR of samples received during non-routine working hottrs may not
      necessarily correspond to the sample delivery date and time:T :^ee
      Exhibit  A,  Section III,  paragraph 9.5 for the definition of VTSR :of
      samples  received during non-routine working hours.

**    A Batch  is a group of samples withia & Case, received over a period of
      one day  and not exceeding 30 fractional ^analyssss.   Data for all samples
      in  the Batch are due concurrently.       ,    ,  ';

***   Complete Batch File (CBF) shall contain the olrigiiial sample hardcopy
      data package including all original documents described in Exhibit B of
      the SOW  under Complete Batch JFile.
****  if more  than three  fractional^ analyses' .'aire - requested for a Batch of
      samples,  the sample and QC data summary ,by electronic transmission is
      due 72 hours after  VTSR and the -sample hardcopy data package and the CBF
      are due  8 days  after VTSR.      I"    :<

***** Each page of the  hardcopy data package sent to the Region-Client shall
      be labeled "UNVALIDAJB^ COPY" .        =:

NOTE: As specified in the Contract-Schedule OG>6 Government Furnished
      Supplies  and Materials) ,  uttiess otherwise instructed by the CLASS
      contractor,  tibe Contractor'J'sfaall^ dispose of unused sample volume and
      used sample  bottles/contaiijeirs ^uo"=ifear3U.er than sixty (60) days following
      submission of hapdcopy analytical data.
Distribution:                '  '
(1)  Contract ,lssbora,£ory Analytical; Services Support (CLASS) Contractor
(2)  EMSL-L%f '•",- '•* -'• -s- :;;-\v         :; • -
(3)  RegioaxjR-SCC         'I"',,,,
(4)  Regipin'-Client        "^,
(5)  NEl£f                   U
     •«'••' "                     !;=
             Addresses:      ,
           **.  -
           * tft,  * ^
(1)   Contr^e%\;Laboratory Analytical  Services Support (CLASS) Contractor

(2)   USEPA EnviroTimie»fcal Monitoring  Systems Laboratory (EMSL-LV)
      P.O. Box 93478  {;S r
      Las Vegas, NV   89114
      ATTN: Data Audit Staff

                                      B-5                              08/23/94

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                                                                          DRAFT

      For overnight delivery service, use  street  address:
      944 E. Harmon, Executive Center
      Las Vegas, NV  89109
      ATTN: Data Audit Staff

(3)   USEPA REGIONAL SAMPLE CONTROL CENTERS         -   i

      The CLASS contractor, acting on behalf  of the APO, will provide the
      Contractor with the list of addressees  for  the  ten EPA Regional Sample
      Control Centers (RSCC).  The CLASS contractor will provide ifee,,
      Contractor with updated RSCC address/naie lists as necessary tnrbtighout
      the period of the contract.          --:'

(4)   USEPA REGIONAL CLIENT              .:>,
                                          '' f ;
                                          v -•"  *'"      I  ',
      The CLASS contractor, acting on behalf >y     *' '-' *T'* ''-J,  " •'
(5)   USEPA National Enforcement Investigation: Center ::(SEIC)
      Attn: CLP Audit Program       :          -1
      Denver Federal Center Building 53       :
      P.O. Box 25227
      Denver, CO 80225                     ;'
                                      B-6                              08/23/94

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                                                                     DRAFT

                              SECTION II

         REPORT DESCRIPTIONS  AND ORDER OF DATA DELIVERABLES

 General                                         /

 The Contractor laboratory  shall provide reports and ot&er deliverables
 as specified  in the  Contract Schedule (Contract Perforoanee/Delivery
 Schedule) The  required content and form of each deliverabl^I'is described
 in this Exhibit.                         •<                  " "

 All reports and documentation MUST be,:

 •     Legible;                     ,

 •     Clearly  labeled and  completed in accordance  with instructions in
       this Exhibit;                         ;

 •     Arranged in the order  specified in this Section.;  and

 •     Paginated consecutive!^.iji;/aseend-ing order starting from the first
       Batch Narrative.     ';;;;„    "  ''"''''];'  •;

 If submitted documentation does,'not  conform to the above  criteria,  the
 Contractor will be required  to  resubmit;, such documentation with the
 deficiency(ies) corrected, at no additional cost to the Agency.
                       ,              f %f,
 Whenever the Contractor 4Ls.required  to.submit or resubmit data as a
 result of an on-site laboratory evaluation or through  an  APO  action,  the
 data must be clearly markeS'Sas  "ADDITIOU&L DATA" and must be  sent to  all
 three contractual data recipients  (Region-RSCC, the CLASS contractor,
 and Region- .eJJUnt) .   A co^jr .Better.,must  be included  which describes
 what data are feeing deliv«rie!<£ J!t0j-»fef;Ch  EPA Case(s)  the data  pertain,
 and the name of t&e person who  requested the data.
 Sections III and IV of -mlfe. Exhibit contain copies of the  required data
 reporting Bo»s in Agency-«p«eified formats, along with  instructions  to
 assist tiie Contraetipr in accurately providing the Agency with all  the
 required data.   Section V describes the QTM laboratory software  and
 electronic data responsibilities.  The use of the QTM software is  not
 jreguired;  however,  the*laboratory must generate the QTM  forms and
-.transmit the data to thl EPA National Computer Center (NCC)  (the EPA
 mali|tt£ranie computer) in |Jie exact format as is performed  by the QTM
 software.rand as specifMd in Exhibit H.
        ' J; ;          ;-''
 Descriptions >&£ the» xsequirements for each deliverable item cited in the
 Contract Schedule,, ape specified in this Section.  Items  submitted
 concurrently SHAIX; 3BE arranged in the order listed.  Additionally,  the
 components of each item SHALL BE arranged in the order presented in this
 Section when the item is submitted.

                                B-7                               08/23/94

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                                                                           DRAFT

      Examples  of specific data deliverables not included herein may be
      obtained  by submitting a written request to the EPA APO,  stating the
      information requested,  and signed by the Laboratory Manager.

      Updated SOPs                                    '•'.

      As  requested,  the  Contractor shall submit updated copies  of all  required
      Standard  Operating Procedures (SOPs) that were submitted- with the prebid
      Performance Evaluation sample results.  The updated SOPs iasst address
      any and all issues of laboratory performance and operation identified
      through the review of the Performance Evaluation sample data and ihe
      evaluation of  Bidder -Supplied Documentation.  Exhibit E,  Section IV
      specifies the  required SOPs and the SC§* delivery .requirements .

      Sample  and QC  Electronic Data Package"';/

      As  specified in the Contract Schedule, sample:'ajid QC data shall  be
      transmitted via an on-line data transfer and data,-:evaluation system to
      the EPA mainframe  computer within the specified turnaround time.   The
      Sample  and QC  Electronic Daj^i,- Package consists of copies of specified
      items from the Sample and «^i;l^^i^|^ata. Package .  These items are
      listed  below and described teller par^B^s^isspIe, %«up4 QC Hardcopy  Data
      Package.   EPA  has  developed a:;software package :;to Bassist contract
      laboratories in preparing the esquired |iE«rms and in transmitting the
      data to the EPA mainframe computeir,  Tills software will be provided to
      QTM laboratories and must be used.  ,>:jS£ the Laboratory wishes to  develop
      its  own software,  it must be approveit'in advance by the EPA.
                         ' i  ' "\'' \\ •          "..
                         ' ' ' ' '• •' - • ' •''            5
      The  Sample and QC'felectroijjfc Data Packsjge shall be reported as follows
      and sample datattxoras mustljbiej arranged iaa increasing EPA sample  number
      order,  considering both letlt^rs and numbers.  For example, BE400 is a
      lower sample tt&Bnber than Blp.^,,,^is,X,|)ir»ecedes F in the alphabet.
                      ? ' '""'      vl^?,*," "%'j.V ' ?* * $•' * I?X -o-,^*'
      The  Sample and QC'^EJJeetronic Data Package shall contain data for samples
      in  one  Batch of the XJasMt^or each fraction of compounds that are
      analyzed,  as follows:  "'4V' •-';>•
                                '' "  "
              *    i
3.1   By frsS^tion"!t'W)*v:|ilt^H,  PHEN, "P^T,  PCB) and by sample within each
      fraclpion  -  Analysis'«|Ba%ta Sheet with tabulated target compound results,
             Monitor CompouMfc. results ,  and retention time information for
          .d and QC samples  (ff»nn QI  for VGA,  PAH, PEST, and PHEN; Forms QIA
          QIB for PCB) ;      if
      ••   -
3.2   By'fBS^Lpn  (VGA, PAH}'°sfEfIEN,  PEST,  PCB) - Laboratory Control Sample
      Sheet
3.3   By fraction  (IDA, -affl,  PHEN,  PEST,  PCB) - Performance Verification
      Standard Sheet  f^«O* QUI);

3.4   By fraction  (VOA, PAH,  PHEN,  PEST,  PCB) - Initial Calibration Sheet
      (Form QIVA and  QIVB);
                                      B-8                              08/23/94

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                                                                           DRAFT

3.5   By  fraction (VOA,  PAH,  PHEN,  PEST, PCB) - Calibration Check  Sheet (Form
      QV);

3.6   By  fraction (VOA,  PAH,  PHEN,  PEST, PCB) - Analytical Sequence  Summary
      (Form  QVI) ;  and

3.7   By  fraction (VOA,  PAH,  PHEN,  PEST, PCB) - Narrative (Form QVI I) .

3.8   QTM contract compliance screening (CCS) defect report.

4     Preliminary Data Results              ,;

4.1   Preliminary Form I Results           :'

      If  requested at the time of sample scheduling, the Contractor  shall
      provide preliminary Form I analytical fesul£.s;-;ror 1-10 field sample
      fractional  analyses via telefacsimile (fax)  -oz? telephone within 24 hours
      after  VTSR.   Requests for preliminary data results, shall be limited to
      Form I field sample and blank analyte concentratitm and SMC results .
      Requests for preliminary data? results shall  be limite'd "to a maximum of
      five (5) request per seven j(7> *»!LeBJdbsa: -days .
                                 "'• :-     ' '{i '•''' T , '.;
4.2   Preliminary  Raw Data Results '-:          ,<

      If requested, before hardcopy deliver able s are due, the Contractor shall
      provide raw  analysis data (e.g. ,  cnrcmato grams ) within four (4) hours of
      the request  for any sample which  hasibeen  previously reported
      electronically  (satg>l^:,ai^d QC  data sujmmary by  electronic transmission) .
      Preliminary raw data shalitbe limited t:o 3io more than the following: (1)
      standards data,;. (2) associated method blank data;  and (3) sample
      chromatogram
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                                                                          DRAFT

5.1   Quick Turnaround Method Traffic Report/Chain-of-Custody Forms (QTM
      TR/COC)

      A copy of the combined sample QTM TR/COC form mus,t be submitted in Item
      B for all of the samples  in  the Batch.   The QTH TR/COC forms shall be
      arranged in increasing EPA sample number order, considering both letters
      and numbers.  A copy of the  Batch cover sheet (Sectlxm XII,. paragraph
      6.4.3) is to be included  with each copy of the QTM TR/COC,

5.2   Volatiles Data                           :                   ;;

      5.2.1 Batch Narrative (Form  VII-VOA)

            This page shall be  clearly  labeled "VolatjRes Narrative" and shall
            contain documentation  of any quality contxiol, sample, shipment,
            and/or analytical problems  encountered las processing the samples
            reported in the electronic  and hardcofyN&ata package.  At a
            minimum, the laboratory shall identify ia.-ieb,e Batch Narrative all
            samples that were analyzed  in the analytical: sequence,  describe
            the sample matrices, any sample dilutions performed, and any
            difficulties encountsspe*!-ll^ttdtie. -laboratory during sample analyses
            or with meeting method (QC requ:lY«asdat»? ,, The Laboratory shall also
            specify in volatiles Batch  Narrative-the''-'target compounds
            associated with (detected by) eadi:::bf the detectors (PID and
            ELCD) .                    ;:. c    • ,; '

            Whenever data from  sample reaaalyses are submitted, the Contractor
            shall state -in"jaisgrBatch Narrative for each reanalysis whether the
            Contractor/:|CsOTiside'fesmust submit a  cover sheet with the hardcopy
            deliverables tfeafc?^states, verbatim:  "I certify that this data
            package is in compliance with the  terms and conditions of the
                    ,;;-,!> oth technisoiilllly and for completeness,  for other than
                -:c6nMstaU»jas detaileS^aslaibve.   Release of the data contained in
                 data paeksjjge has been authorized by the Laboratory Manager or
            his designee, Ij^mrerified by  the following signature."  This
            statement shall°-$|&. directly followed by signature of the
            Laboratory Manager or his designee with a typed line below it
            containing the s||gner's name  and title, and the date of signature.
                electronical!^ delivered  Narratives shall have, in place of
                               words "Signature Obtained."
      5.2.2 Contract: Compliance Screening Report

      5.2.3 Sample Data
                                      B-10                              08/23/94

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                                                               DRAFT

 Sample Analysis Data  Sheets  shall be  arranged in packets with the
 Volatiles Analysis  Data  Sheet (Form QI-VOA)  followed by the raw
 data for volatile samples.   These sample packets shall then be
 arranged in increasing EPA sample number 0rder,  considering both
 letters and numbers.

 5.2.3.1     TCL results  - Quick Turnaround Analysis  Data Sheet
             (Form QI-VOA).

             The volatile target compounds (Exhibit C)  'shall be
             identified and quantitated.   Relative and absolute
             retention time dataiand the  sample SMC results  shall
             be reported on Form::QI-VOA.   The validation and
             release of the results shall ,be  authorized by a
             specific, signed statement ifi the Batch  Narrative.   In
             the event that the  Laboratory Manager cannot validate
             all data  reported for each sample, the Laboratory
             Manager shall provide a detailed description of the
             problems  associated with  the sample  in the Batch
             Narrative £,, ,

 5.2.3.2     Copies ofllQA chromatograms,

             All chromatograms shall be labeled with  the following
             information:   ,',      -:

             •      EPA sample number;

            ;-.«      Tidltmie or weig&t of sample;

         ,;:    '      Datse and time  (report  in military  convention if
      ,  "          tbie, ,inst,rument,has  this capability)  of analysis;

             *'     GC  column  identification (by stationary phase);

             •     »(?C  instrument  identification;  and

:  •      !  -   '•*,     Identified compounds shall be  labeled with.the
             <\-i   names of compounds,  either  directly  out from  the
               % r> peak, or on a  printout of retention  times  if
                 ff retention times  are printed over the peak.

 5.2.3.3     GC integration report  or data system printout.

<*Si2r!3,,4     Maral&l work sheets  (if any) .
                          B-ll                             08/23/94

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                                                                    DRAFT

5.2.4 Standards Data

      5.2.4.1     Initial Calibration Sheet  (Form QIVA-VOA and QIVB-VOA)
                  - all GC columns , all instruments ,  in chronological
                  order by GC column and instrument.

      5.2.4.2     Calibration Check Sheet  (Form QV-170&;)  -  all  GC
                  columns, all instruments,  in chronological order by GC
                  column and instrument.

                  Calibration check retention time data (Form  QI-^iOA) -
                  all GC columns , all -Instruments , in chronological
                  order by GC column a»d instrument.

      5.2.4.3     Performance Verifi&tjtwn Standard  (PVS)  (Form QIII-
                  VOA) - Tabulated results -MOf'Sisp iked target compounds
                  for the PVS.             '  ]..

                  FVS retention time data  (Form QI-T70A)  -  all  GC
                  columns, all instruments,  in chronological order by GC
                  column
                            •                      , ,
      5.2.4.4     Chromatograms and da ta,/systenr printouts  shall be
                  required for All staradterds .
      5.2.4.5     For all standards chromatograms , Contractors  shall:

                              all chroaatograms with the  "EPA Sample
                              " for standards  (see Forms  Instructions
                        Labesl.all standard peaks for all  individual
                        oiBa^^ji«^-'el.tihjer directly out from  the  peak,  or
                        on the printout of retention times  if retention
                       r> times are printed over the peak;
                       '*.':,-•; -3
                        Listl-.itotal nanograms  (ng) injected  for  each
                     "^"-s: Accompany each chromatogram with  a  printout of
                      v-:s;'xetention times and corresponding peak areas;
                       '
                                 date and time  (report  in military
                      s, ^convention if the instrument has this
                     {j -Y capability) of injection;

                        Provide GC column identification (by stationary
                        phase) ;  and

                        Provide GC instrument identification.

                               B-12                              08/23/94

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                                                                           DRAFT

      5.2.5 Raw QC Data

            5.2.5.1      Blank Data -  both method and instrument blank arranged
                         in chronological order.  NOTE:  This order  is
                         different  from that used for samples.

                         •      Tabulated results (Form Ql-WA),

                         •      Chromatograms and data system printouts for each
                               GC column and instrument used for analysis
                               labeled as in paragraph 5.2.3.2 above .   I

            5.2.5.2      Laboratory Control Sample (LCS^

                               Tabulated results (FoptfQII-VOA) of spiked
                               target  compounds :f or : the LCS.

                               LCS  retention time datai,{lorm QI-VOA) .

                         •      Chixjaatqgrams and data system, printouts for the
                               LCS-l&beleii^as, in paragraph 5.2.3.2 above.
                                   ;    ••  •'•. .• -. •> i '^, ' * ,   *-*  •*•
                                  • ,;;      •»;.,*•}' £  j  . :,
      5.2.6 Analytical  Sequence Summary (Form JPI-VOA)   •
                                      < ':       •>
                                      <>\ '
            In order  of sequence number :or , if more than one instrument is
            used, in  order of instrument IS. '

5.3   Polynuclear Aromatic "fi^teocarbons Data;;
                        / '    " ^ j.           ~
      5.3.1 Batch Narrative (ForM.fi?! I -PAH)
                   - '•>,"':           f|-
                   ; ;-            ;|f'
            This page shall be c%iarXy.,J.aheled "Polynuclear Aromatic
            Hydrocari*eais, Narrat^tfelriae^L^bsflEL contain documentation of any
            quality cohtxoi,, sample,  shipment,  and/or analytical problems
            encountered in processing the samples reported in the data
            package.  At a mintatiffn, the laboratory shall identify in  the  Batch
            Narritfcli^B «11  samplesufeat were analyzed in the analytical
          . ,>s««iuehce •, ififeffoxibe theX!sample matrices, any sample dilutions
        ,  vsf^perf ormed ,  stiQkjiaxy difficulties encountered by the laboratory
       _-, i •  during sample  iaalyses or with meeting method QC requirements.
      f > '                  %,,«
     :_-,-;,',    Whenever  data  frdk sample reanalyses are submitted, the Contractor
     '*'-'>'Ji;  shall state in tie Batch  Narrative  for each reanalysis, whether
        '""• '":  -tfete Contractor csensiders  the reanalysis to be billable, and if so,
            'fe^i:  ;The Contractor shall also include any problems encountered
            (bo'tSi jfeaehniciEL 'and administrative) , the corrective actions taken,
            and
            The Laboratory  shall  submit a cover sheet with the hardcopy
            deliverables that  states,  verbatim: "I certify that this  data

                                      B-13                             08/23/94

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                                                                    DRAFT

      package is in compliance with the  terms and conditions of the
      contract, both technically  and for completeness,  for other than
      the conditions detailed above.   Release of - the data contained in
      this data package has been  authorized by .dfae Laboratory Manager or
      his designee, as verified by the followingjsignature."  This
      statement shall be directly followed by signatxire of the
      Laboratory Manager or his designee with #a typed line below it
      containing the signer's name and title, and the date of signature.
      The electronically delivered Narratives shall have, fax place of
      the signature, the words "Signature -Obtained."

5.3.2 Contract Compliance Screening Report

5.3.3 Sample Data                   \   J          ''{
                                      5^V'.
      Sample Analysis Data Sheets shall  fee;-arranged in packets with the
      Polynuclear Aromatic Hydrocarbons  Analysis Data Sheet (Form QI-
      PAH), followed by the raw data for PAH samples.   These sample
      packets shall then be arranged in  increasing 1PA sample number
      order, considering botfe letters and numbers.
                          ^•r -. 'i4.  ".. ^ ;'   - -•  -
      5.3.3.1     TCL result^ - Quick%fir»ar<«pp(l(,Analysis Data Sheet
                  (Form QI-PAH),,
                                s >
                  The PAH targefci«;ompoands (Exhibit C)  shall be
                  identified and  CpaaBti'tated.  Relative and absolute
                  retention time  data and the sample SMC results shall
                  i»e ^reported on  Fora sfI-PAH.  The validation and
                 ; ;release:f|jf£ the  results, shall be  authorized by a
               f/  specific^vsigned statement in the Batch Narrative.  In
              7   the eventl^iat  the Laboratory Manager cannot validate
            , -•',.   all data|||ip|pxa:t:e,d„£pr  each sample, the Laboratory
              ":/• /feManager^aS^paaanKtSe  a detailed description of the
                 -•pljablems associated with the sample in the Batch
                  Narrative.
                  Copies cr£,fAH. chromatograms.
                 ;»  ,        *''•'* --^
                  A3^t: .chromatograms  shall be labeled with the following
                  iriformation:

                  •    h^EPA sample number;

                  •   ;. -Volume  injected in microliters (^L) ;
                     %, ; '^
                  • ':•„ '••  Date and time  (report in military convention if
                 ;,  ^,    the instrument has this capability) of analysis;

                  •     GC column identification (by stationary phase);


                                B-14                              08/23/94

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                                                                    DRAFT
5.3
               •     GC instrument identification; and

               •     Identified compounds shall be labeled with the
                     names of compounds, either directly out from the
                     peak, or on a printout tH retention times if
                     retention times are printed over the peak.

   5.3.3.3     GC integration report or data system printout.

   5.3.3.4     Manual work sheets (if>\any).

.4 Standards Data                  ;

   5.3.4.1     Initial Calibration!Sheet (Fora QIVA-PAH and QIVB-PAH)
               - all GC columns, :ail instruments, in chronological
               order by GC column ariHliiastirument.
      5.3.4.2
      5.3.4.3
      5.3.4.4
               Calibration Check Sheet (FormUQV-PAH) - all GC
               columns, all instruments, in chronological order by GC
               column and;;,-instrument.
                       . • >^s'.  ; -     ^
               Calibration;, check' retWttion,t;aj»e data (Form QI-PAH) -
               all GC coluHBBS,  all instruments,- in chronological
               order by GC column and instrument.

               Performance Verification Standard  (PVS) (Form QIII-
               PAH) - Tabulated results of spiked target compounds
               for t!b6> FVS.       '  _.

               PVS retention time data (Form QI-PAH) - all GC
               columns,|&tl instruments, in chronological order by GC
               column and.instrument.
            •  - ^ -
                             and data system printouts shall be
                        for all standards.
                  For all st:aaadards  chromatograms  Contractors  shall:
                     Label all chromatograms with the "EPA Sample
                     Number" for standards (see Forms Instructions
                     for details);

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

                     List total nanograms (ng) injected for each
                     standard;
                               B-15
                                                             08/23/94

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                                                                          DRAFT

                         •     Accompany each chroma to gram with a printout of
                              retention times and corresponding peak areas;

                         •     Document  date  and time (report in military
                              convention if  the instrument has this
                              capability)  of injectioh;

                         •     Provide GC column identification,, {by stationary
                              phase) ; and

                         •     Provide GC instrument identification.

      5.3.5 Raw QC Data                    ;>

            5.3.5.1      Blank Data  - both method and Instrument blank arranged
                         in chronological order. /FhNOXS;:   This order is
                         different from  that  used £br .samples .

                              Tabulated results (Form QI-PAH) .
                                         as  '                 '-|,;;
            Batch Narrative ||orm VII-PHE)
                 page shall jtitt clearly labeled  "Phenols  Narrative" and shall
                    documensbition of any quality  control,  sample,  shipment,
                    tnalytieal problems encountered in processing the samples
            reportes jatli.^toe data package.  At a minimum,  the laboratory shall
            identify im:;|t|h;e Batch Narrative all samples  that were analyzed in
            the analytical sequence , describe the sample matrices , any sample
            dilutions performed, and any difficulties encountered by the

                                     B-16                              08/23/9A

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                                                                    DRAFT

      laboratory during sample analyses or with meeting method QC
      requirements.   The Laboratory shall also note in the Batch
      Narrative  the  detector type used.

      Whenever data  from sample reanalyses are submitted, the Contractor
      shall  state in the Batch Narrative for, each reanalysis whether the
      Contractor considers  the reanalysis to-be billable, and if so,
      why.   The  Contractor  shall also include any problems, encountered
      (both  technical and administrative),  the corrective actions taken,
      and resolution.

      The Laboratory shall  submit a cover sheet with the hardcopy
      deliverables that states, verbatim: "I certify that this data
      package is in  compliance with ttie terms and conditions of the
      contract,  both technically and Jbr completeness, for other than
      the conditions detailed above.   Release- of the data contained in
      this data  package has been authorized S»y the Laboratory Manager or
      his designee,  as verified by the following-signature."  This
      statement  shall be directly followed by signature of the
      Laboratory Manager o%M.s designee with a typedVline below it
      containing the signer]|si®ame'.ia»dj title,  and the date of signature.
      The electronically delivered Narratiiv.es«shall have, in place of
      the signature,  the words^-" Signature Obtained.'"

5.4.2 Contract Compliance Screening Report

5.4.3 Sample Data                  ,«;

      Sample Analysis D'ata: Sheets shalllbe arranged in packets with the
      Phenols .Analysis Datasheet (FormfQI-PHE),  followed by the raw
      data for!phenol samp!je|s.  These sample packets shall then be
      arranged;in increasing:EPA, Cample number order, considering both
      letters 'and, numbers,", rii  ', - ;,' . 2
                   \ -
      5.4.3.1      TCI, Results - Quick Turnaround Analysis Data Sheet
                   (Form\j4l---]?HE).

    ,-,;?, •'   y~  :--v,:fhe phenoi"'stadrget compounds (Exhibit C) shall be
   K-  !            "'identified and quantitated.   Relative and absolute
   1               retsejktion time data and sample SMC results shall be
J  . *                repeated  on Form QI-PHE.   The validation and release
"'f.'                 of tile results shall be authorized by a specific,
                   sign
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                                                                     DRAFT

                  All chromatograms shall be labeled with the  following
                  information:

                  •      EPA sample number;      "

                  •      Volume  injected in micr«3.itiers  (/tL);

                  •      Date and time (report in militsary, convention if
                         the instrument has this capability^N>f analysis;

                  •      GC column identification (by stationary gihase);

                  •      GC instrument^ identification; and

                         Identified compounds shall be labeled  with the
                         names of compounids^ either directly out from the
                         peak, or on a printout: of retention times  if
                         retention times are pirSaiteed over the peak.

      5.4.3.3     GC  integration report or data systeot printout.

      5.4.3.4     Manual woxfc.sheets'-fif ^-sky) , :   > ••

5.4.4 Standards Data                    •

      5.4.4.1     Initial Calibration Sheet (Fora QIVA-PHE and QIVB-PHE)
                  - all  GC columns,,,j£Ll instruments, in chronological
                  • oircler:by GC columri;aad instrument.

      5.4.4.2 ,-;• Calibration Check Sheet (Form QV-PHE) - all  GC
             y    columns, lk|l  instruments, in chronological order by GC
             :-     column aj^.ij^t;rume,iit.
             ':   - -'-       ,,'*• i'.&£ ,K-. !-,:!~: ;T
                  ,<5alibration check retention time data (Form  QI-PHE) -
                  al-l ;I*C. .columns,  all instruments, in chronological
                  ordeir'jby £C column and instrument.

              '•''-'  JFexformance"%erif ication Standard (PVS) (Form QIII-
                  *S^B^ - Tabulated results of spiked target compounds
                  fo'irlfche PVS.
                  PVS intention time data (Form QI-PHE)  - all GC
                  columns,  all instruments,  in chronological order  by GC
                  colujiai and instrument.
                     «4>F
                  Chagomatograms and data system printouts shall be
            -'-,,:-,, -.asesquired for all standards.
                " ^ <
      5.4.4.5     For all standards chromatograms Contractors shall:


                                B-18                             08/23/94

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                                                                     DRAFT

                          Label  all chromatograms with the "EPA Sample
                          Number"  for standards (see Forms Instructions
                          for  details) ;

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

                          List total nanograms (ng) injected for -each
                          standard;       -;

                          Accompany each chromatogxain with a printout of
                          retention times and corresponding peak areas;

                          Document date  atid rtinte' '(report in military
                          convention if  the instrument has this
                          capability)  of inj ectloilj!

                          Provide  GC column identification (by stationary
                                » - teaai ~:-
                   •     Provide GC  instrtaasent'lifetltrification.

 5.4.5 Raw QC Data

       5.4.5.1     Blank Data  - both, aoethod and instrument blank arranged
                   in ejhronological  oi;der.   NOTE:   This order is
                  • ,dif feret%. from  that  si^ed for samples .

             ,; J'r   •     TabMated results  (Form QI-PHE) .
                                       and data system printouts for each
                    :     GC column and instrument used for analysis
                       ;  labeled as in paragraph 5.4.3.2 above.

                   Laboratory -Control Sample  (LCS)
       '."          <*..             ^
   :   !           **<^r   Tabulated results (Form QII-PHE) of spiked
  -':•,'                V- -  target compounds  for the LCS.
/ •• '"$•                    '"'•'
f ;                 •   -,'ILCS retention time data (Form QI-PHE).
^  '*^*\
  '- ?• ' ,                  :
    '  ?;:,           •   ;/ Chromatograms and data system printouts for the
       K  ;,  ,         -  -' LCS labeled as  in paragraph 5.4.3.2 above.

5.4.6 Analytical^; Sequence Summary (Form VI-PHE)
                I] ^"~, *

       In order of sequence number or, if  more than one instrument is
       used,  in order of instrument ID.

                                B-19                              08/23/94

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                                                                           DRAFT

5.5   Pesticides Data

      5.5.1 Batch Narrative (Form VII-PEST)

            This page  shall be clearly labeled "Pesticides Narrative" and
            shall contain documentation of any quality-control, sample,
            shipment,  and/or analytical problems encountered ,in processing  the
            samples reported in the data package.  At a mini»um>; the
            laboratory shall identify in the Batch Narrative ali:/samples  that
            were analyzed in the analytical sequence, describe the;,sasple
            matrices,  any sample dilutions performed, and any difficulties
            encountered by the laboratory during sample analyses or with
            meeting method QC requirements;
                                          • ' \' *             -
            Whenever data from sample reana&j^ses are; submitted, the Contractor
            shall state in the Batch Narrative!#<*r each reanalysis whether  the
            Contractor considers the reanalysis ta> &e billable, and if so,
            why.  The  Contractor shall also include?mty problems encountered
            (both technical and administrative), the corrective actions taken,
            and resolution.       ,;,
            The Laboratory  shall  spbmit a coVer- sfeee^t with the hardcopy
            deliverables  that states,*  verbatim;; • **I certify that this data
            package is  in compliance' ;wi,th the >tierms and conditions of the
            contract, both  technically4snd for completeness,  for other than
            the conditions  detailed above. A Helease of the data contained in
            this data package has been authorized by the Laboratory Manager or
            his designee;^; ^.verified  by the following signature."  This
            statement .shMl be i ^ibectly follssred by signature of the
            LaboratoijjbHanager or|*|lis  designee^ith a typed line below it
            containing  the  signerlSps name and title, and the date of signature.
            The electronically dep|£vere.d. Narratives shall have ,  in place of
            the signaSBfize,  the j&l&lisl ^jSk-^^Saire Obtained."

      5.5.2 Contract Compliaafee Sreening Report
                              "* o  '''•f
      5.5.3 Saatpli; IBata.        '^--.
           ,**r •*•  '' '" ' •> «• '•'•        "•';*., f
          ;  ^          "'""- l',;\ .         "-" ~
         ,!•>; Sample Analys^|tJ)ata  Sheets shall be arranged in packets with the
        j|Ji : Pesticides  Ana^l^.s Data Sheet (Form QI-PEST), followed by the raw
      ,, f   data for pesticiffjfe samples.  These sample packets shall then be
     ;' ,  '   arranged in incr^sing EPA sample number order, considering both
     "•=: %f, letters and numbers .
        •\i-i~ :^-v              •:*>
                        TCLrJ^pesults -  Quick Turnaround Analysis Data Sheet
                        (F«|tin QI-PEST).
                             pesticide target compounds (Exhibit C) shall be
                         identified and quantitated.   Relative and absolute
                         retention time data and the  sample SMC results shall

                                      B-20                             08/23/94

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                                                                     DRAFT

                   be reported on Form QI-PEST.  The validation and
                   release of the results shall be authorized by a
                   specific, signed statement in the Batch Narrative.   In
                   the event that the Laboratory Manager  cannot validate
                   all data reported for each safiaple,  the Laboratory
                   Manager shall provide a detailed description of the
                   problems associated with the sample in the Batch
                   Narrative.
                                                           ; ,

       5.5.3.2     Copies of Pesticides dfciromatograms.

                   All chromatograms shall be labeled  with the following
                   information:       ,           ;  <

                   •     EPA sample number;

                   •     Volume injected in mieroliters (/iL);

                   •     Date and time (report in military convention if
                         the instrument has this capability)  of analysis;

                   •     GC column identification (by  stationary phase);

                   •     GC instrument islentification;  and

                   •     Identified compounds shall be labeled with the
                         names of cosajfbunds, either directly  out from the
                       f  f>eak, or on a printout of retention  times if
                         ceteention times are printed over the peak.

       5.5.3.3,,;   GC integration report or data system printout.

       5.5.3.4:;:- - ,~H Manual ,-fciigfcJanets ~|if any) .

 5.5.4 Standards Data  ;;;;
                       'a  I „,
       5,.5:,4.1  ,  Initial Calibration Sheet (Form QIVA-PEST  and QIVB-
      ;;! ' -'    *  "^. -"BEST)  - all* ©C columns, all instruments, in
   *;:/'            e3|ponological order by GC column and instrument.

 ,.:!!:   5.5.4.2     Calibration Check Sheet (Form QV-PEST)  - all GC
:*;'f                 colutes, all instruments, in chronological order by GC
 A'; ^               coluori, and instrument.
   ..''..              ",'•''.
        -, {-•• ,       CalS&ration check retention time data  (Form QI-PEST) -
           • i,  ,.-,    aJJ.:GC columns, all instruments, in chronological
              -, ,.\. ,^rder by GC column and instrument.
                                B-21                              08/23/94

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                                                             DRAFT

5.5.4.3     Performance Verification Standard (PVS) (Form QIII-
            PEST) - Tabulated results of spiked target compounds
            for the PVS.

            PVS retention time data (Form QI-PEST) - all GC
            columns,  all instruments, ill ^chronological order by GC
            column and instrument.

5.5.4.4     Chromatograms and data system printouts shall be
            required for all standards.               :   :

5.5.4.5     For all standards chromatograms Contractors shall:

            •      Label all pJhromatograms.,; with the "EPA Sample
                  Number" for -standards  ,^see Forms Instructions
                  for details);   (

            •      Label all standard peaks for all individual
                  compounds either directlyjoui: from the peak or
                  on £lie printout of retention' -times if retention
                  times'* --aspe tjnriat^d over the peak;
                  List total picograta (pg> injected for each
                  standard;      %•'
                         ''• ,    ' *
                  Accompany ?eaelp chromatogram with a printout of
                  retention feiaes and corresponding peak areas;

                  Dcwpument datelind time (report in military
                  convention if the instrument has this
                  cajiibility) of injection;
                                    identification (by stationary
                  phase) ;  and

                  Provide GC instrument identification.
5.5.5.1     Bllpk Data - both method and instrument blank arranged
            in Ihfonological order.  NOTE:  This order is
                 kent from that used for samples.

                  Tabulated results (Form QI-PEST).

                  Chromatograms and data system printouts for each
                  GC column and instrument used for analysis
                  labeled as in paragraph 5.5.3.2 above .
                         B-22                             08/23/94

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                                                                           DRAFT

            5.5.5.2      Laboratory Control Sample (LCS)

                         •      Tabulated results (Form QJI-PEST) of spiked
                               target compounds for the'LCS.

                         •      LCS  retention time datal;(Form Ql-PEST) .

                         •      Chromatograins and data system'printouts for the
                               LCS  labeled as in paragraph 5.5.3",=2 above.

      5.5.6 Analytical  Sequence  Summary (Form VT-PEST)

            In order of sequence number or, ;if more thgcn one instrument is
            used, in order  of instrument H>«           ::

5.6   Aroclors Data

      5.6.1 Batch Narrative (Form  VII-PCB)

            This page shall be clearly labeled "Aroclors Hatrative"  and shall
            contain documentatiof^oft/^Gfp?'jjuali£y control, sample, shipment,
            and/or analytical problems encotmt^qra?(3:s|to.^|>rpcessing the samples
            reported in the data paasfeage.   At 4>iiinlTmini,' the laboratory shall
            identify in the Batch  NaZiative a£i. samples that were analyzed in
            the analytical  sequence,  dfescribfe''the sample matrices, any sample
            dilutions performed, and any (-difficulties encountered by the
            laboratory  during sample analyses or with meeting method QC
            requirements.-  -j •}             vj-

            Whenever-'idata from sample reanalyzes are submitted, the  Contractor
            shall sJsaite  in  the Bitjs:fi Narrative for each reanalysis whether the
            Contractor  considerate., rean,alysis to be billable, and  if so,
            why.  The;-:Contract»iH'^te3&Mi^finclude any problems encountered
            (both technicalsand  administrative), the corrective actions taken,
            and resolution.   .

            The .pabwratory  shall ..siibniit a cover sheet with the hardcopy
           ..^deiivera-b'les'irthat state^s;^verbatim: "I certify that this data
            package is  iti-^empliance with the terms and conditions of the
       ,,    contract, bothia%chnically and for completeness, for other than
      ,,v"   the conditions  totalled above.   Release of the data contained in
     i:^    this data packagefihas  been authorized by the Laboratory Manager or
     -a3---,  his designee, as-Aerified by the following signature."  This
        "' -,;!,c^|atement shall-lfe directly followed by signature of the
           l&sfonsatory Man,gt^r or  his designee with a typed line below it
            containing  thej^signer's name and title,  and the date of signature.
            The ele^«3Con4dially delivered Narratives shall have, in place  of
            the signature,  the words  "Signature Obtained."

      5.6.2 Contract Compliance  Sreening Report

                                      B-23                              08/23/94

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                                                                    DRAFT

5.6.3 Sample Data

      Sample Analysis Data Sheets  shall  be arranged in packets with  the
      Aroclors Analysis Data  Sheets (Form QIA-PCB and QIB-PCB), followed
      by the raw data for Aroclor  samples.  Theise sample packets shall
      then be arranged in increasing EPA sample tsaaber order,
      considering both letters  and numbers.-        ?   .

      5.6.3.1     TCL results -  Quick Turnaround AnalysisIBaita Sheets
                  (Form QIA-PCB and QIB-PCB).                -°, ;  .
                                       >''•.'                       ''
                  The Aroclor target compounds (Exhibit C) shall be
                  identified  and quaatltated.   The mean sample
                  concentration result (the average concentration of the
                  individual  peak  coiiceatrations) shall be reported  on
                  QIA-PCB.  Relative and-.absolute retention time data
                  and the sample SMC results sikall be reported on Form
                  QIB-PCB.  The validation and:release of the results
                  shall be authorized by a specific;-, .signed statement in
                  the Batch^Narrative.   In the event that the Laboratory
                  Manager eipJBOlfisvalMajt^, all data reported for each
                  sample, tft&'s!-abora;tory4iCa8ager,j shall provide a
                  detailed description oft'-the -prafeieins associated with
                  the sample  injthe Bateti Narrative.

      5.6.3.2     Copies of PCS chroaatograms.

                  All ebroinatograms shall be labeled with the following
                     ormatfion:         ; ,_

                        EPA:-'Sample number;

                                         in microliters

                      };iDate  and time (report in military convention if
                            instrument has this capability) of analysis;
     :|-v'-!'' ''"** :'.f,*'~    GC  c&laj^Bn identification (by stationary phase);

                   •  \^f-; GC  instrument identification; and

                   •    (f Identified Aroclor quantitation peaks shall be
                       vjjlabeled with the names of compounds, either
     [;;.,,              j--'^directly out from the peak, or on a printout of
      ~i:"--"i" =          -fi>- retention times if retention times are printed
        "*'^' i,,.      •/•? over  the peak.
             •£''?'•• -/| -''
      5.6.3.3  ""- "3&J integration report or data system printout.

      5.6.3.4     Manual work sheets (if any).

                                B-24                             08/23/94

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                                                                    DRAFT

5.6.4 Standards Data

      5.6.4.1     Initial Calibration Sheet (Form QIVA-PCB and QIVB-PCB)
                  - all GC columns,  all instruments,  in chronological
                  order by GC  column and instrument.

      5.6.4.2     Calibration  Check  Sheet (Form QV-PCB) - all GC
                  columns, all instruments,  in chronological order by GC
                  column and instrument.

                  Calibration  check  retention time data (Form QIB-1PCB) -
                  all GC columns,  all -instruments, in chronological
                  order by GC  column,and instrument.

      5.6.4.3     Performance  Verification Staadard (PVS) (Form QIII-
                  PCB) - Tabulated results  of spiked target compounds
                  for the PVS.

                  PVS retention time data (Form {JsIS-jPCB) - all GC
                  columns, .-ailX instruments,  in chronological order by GC
                  column and instrument.

      5.6.4.4     Chromatograis and  data'system-printouts shall be
                  required for all standards.

      5.6.4.5     For all standards  e&romatograms Contractors shall:

                  -»   '-; Label  all  chrotaatograms with  the "EPA Sample
                        Niaasber"  for  stfaaadards  (see Forms Instructions
              '-,'.!'        fok/details);   \

           ...  ,    •     La$*£|., aj.,1  standard Aroclor quantitation peaks
             '•';? ,       eiltihlit: $&£«$£;%• out  from the  peak or on the
                        printout of  retention  times if retention times
                      ';  «are printed  over  the peak;
                        ;/ ,
       .;••. :;!"  ,;,  -,, •     List,<*otal picograms (pg)  injected for each
          "'"  '   -v?  -%    staridspia;

                  • ;v-  Accompany  each  chromatogram with a printout of
                      - ..retention  times and  corresponding peak areas;

                  •   ^Document date and time (report in military
                      '^convention if the instrument  has this
                    ,;   capability)  of  injection;
         ""  '•:
            '; '•'.$'•    Provide  GC column identification (by stationary
                 j i     phase);  and

                        Provide  GC instrument  identification.

                               B-25                              08/23/94

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                                                                          DRAFT

      5.6.5 Raw QC Data

            5.6.5.1     Blank Data  - both method and  instrument blank arranged
                        in  chronological order.   NOTE:  .This  order is
                        different from  that used for  samples.

                        •     Tabulated results  (Form QIA-BCB and QIB-PCB).

                        •     Chroma to grams and  data  system printouts for each
                              GC column and instrument  used for analysis
                              labeled as in paragraph 5.6.3.2  above.   ,;

            5.6.5.2     Laboratory  Control/Sample (LCS)

                              Tabulated results  (Fora;iQII-PCB)  of spiked
                              target compounds, for tile  LCS.

                        •     LCS retention time data (Form QIB-PCB).

                        •     Chromatpgrams and  data  system -printouts for the
                              LC$ iNftfefeiaehi aas- in  paragraph  5.6.3.2 above.

      5.6.6 Analytical Sequence Summary (Form .VI-PCB)

            In order of sequence number or, .if more than one  instrument is
            used, in order  by instrument IB.-:

      Complete Batch File; -   •-,.-

      As specified in tfoe DelivelQr  Schedule, tme, Complete  Batch File  (CBF)
      including the^riglnal  SamppLe and QC Hardcopy Data Package shall be
      delivered to 'She. Region-RSJp? .concurrently  with  delivery  of the  Sample
      and QC Data PacJeage to  th^|&i%<|»atfeifeSnt and the  CLASS contractor.   The
      contents of the raBp xill be numbered according  to the specifications
      described in Sections JII and IV  of Exhibit B.  The  Document Inventory
      Sheet (Form QDC-2) is c«a£ained in Section IV.  The  CBF will contain all
      original'-
-------
                                                                           DRAFT

      6.3.1 QTM TR/COC forms.  For each Batch, the  Contractor shall sign and
            submit the original sample QTM TR/COC page marked "Lab Copy for
            Return to the CLASS contractor" with laboratory receipt
            information.   QTM TR/COC forms shall be submitted in Batch sets
            (i.e.,  QTM TR/COCs for all samples in a -Batch  shall be clipped
            together) ,  with a Batch Cover Sheet attached.

      6.3.2 Airbills.                                         , j

      6.3.3 Sample Tags (if present) sealed inelastic bags.        >:
                                             ,;T :
6.4   All original receiving documents, inclikfling,  but not limited to, the
      following documents:                              ;

      6.4.1 Form QDC-1.                   :          ;  '

      6.4.2 Other receiving forms or copies of receiving logbooks.

      6.4.3 Batch Cover Sheet.                         r

            The Batch Cover Sheet shallL^cttttain the following items:
                                   ,"      ~"  *i: -' t.1 '  -' ; ' ':..'•„
                   Lab name ;          .          ' ,       •  ,

            •      Contract  number;    -',

            •      Sample  analysis price - '£ull sample analysis price from
                   contract::;  ^  ,.,

            •      Dace and  time ©£, sample recei.pt;
                    ?&            • •••
                   Case number; a»d  ,,.  „  ,   „
                    'i ~<       ff'.  f" •''-' -'r  -I- ';,?-'
            •      List t>3E,IEPA sample numbers of all samples  in the Batch,
                   i dent ifyi»|p the first and last samples received.
                               rT'
6.5   All ori^gJaSSl'f laboratory recaaJds (not already  submitted in the Sample and
      QC HatsUJiJpy "Data^Wtekage) of"«*BBple transfer,  preparation and analysis,
                  but  not*13iaiited to,  the following  documents.
      ""
         . 1 Original  preparation and analysis forms or copies of preparation
       ;;    and analysis  logbook pages.
      .-; ]|'^r                   1

      6.5*.l;;-si|tt:ernal  sample -and sample extract transfer chain- of -custody
           Nr/Sf* ^5;  _          ^  ,                                           J
                            '•
      6.5.3 All  inSttra»e|p:i output.

6.6   All other  original  Batch- specific documents in the possession of the
      Laboratory,  including,  but not limited to, the following documents.

                                      B-27                              08/23/94

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                                                                    DEAF!

6.6.1 Telephone contact logs.

6.6.2 Copies of personal logbook pages.

6.6.3 All handwritten Case-specific notes.

6.6.4 Any other Case-specific documents  not  covered by the above.

NOTE: All Case-related documentation may be  used  or admitted as evidence
      in subsequent legal proceedings,   -fazy  other Case-speclf-Cc
      documents generated after the CBF !-is sent to EPA,  as well :as
      copies that are altered in any fashion,  are also deliverables to
      EPA.  (Original to the Region-RSCC and a cof*y to the CLASS
      contractor.)

      If the Laboratory submits Batch -specific /-documents to EPA after
      submission of the CBF, the documents shall  be numbered as an
      addendum to the CBF and a revised  QDC-2  fojCm shall be submitted,
      or the documents shall be numbered as  a  new GBF and a. new QDC-2
      form shall be submitted,, to the Region-RSCC  orilyv

Data in Computer-Readable Folia    '"; '"•'"•< -.     •

The Sample and QC Electronic DsEta Package shall be reported via a
telecommunications network to a central 'mainframe computer located in
Research Triangle Park, NC.  Addit&oaai  information about the QTM data
transfer system can be found in SeetiUm  V, On-Line Data Transfer System.

If the Contractor *$Lsnes -l|$jg->use an electronic  data reporting format
other than the.*0»e specifl^U equivalency must be demonstrated and
approved by tfase^APO prior t&ihe award off the  contract.
In the event odr/aata transf^hs^treai-failure,  the  Contractor shall send
a hardcopy of the^sample and QC data summary (Form QI  -  QVII) to the
Region-RSCC and to thgy'Eifgion-client by overnight  delivery.   The
Contractor shall also's^i-^a diskette of the sample and QC summary data,
in EPA-a$ppettM4 iormat, 'to»,|t%.CLASS contractor by overnight delivery.
The Cj>tol^et6r~.*3|&13. immediat5ea|f contact the CLASS contractor and the
Regjbifi-client or R^ton-RSCC if the  data transfer  system or the data
fQJBtjsatting and forms'^gnerating software fails.

   xacts               !'•'
The-'ikmtractor shall pjigserve sample  extracts  at 4°C (± 2°C) in
bottlex^psls with TejEl»n-lined septa.   Extract  bottles/vials shall be
labeled wiMi ,35FA sample number, Case  number, and Batch number.  A
logbook of sta^sssd,,extracts that lists EPA sample numbers and associated
Case and Batch numbers shall be maintained.
                               B-28                              08/23/94

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                                                                   DRAFT

The Contractor is required to retain extracts for 21 days following
hardcopy data submission.  During that time, the Contractor shall submit
extracts and associated logbook pages within seven days of receiving a
written request from the APO or the CLASS contractor.
                               B-29                             08/23/94

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                                                                           DRAFT

                                  SECTION III

                            FORMS INSTRUCTION GUIDE

This section includes  specific instructions for the cojnpletion of  all  required
Quick Turnaround Method Data Reporting Forms.  Each of , the forms is  specific
to a given  fraction (i.e.,  volatiles, polynuclear aromatic hydrocarbons,
phenols, pesticides, and Aroclors) .   The Contractor shall submit only  those
forms pertaining to the fractions analyzed for a given sample or ''samples .   For
instance, if a  sample  is scheduled for volatile analysis only, provider only
volatile data reporting forms (i.e., Forms QI^TTOA - QVII-VOA).  These";
instructions are arranged in the following order:

      1      General Information and Header .Information;
      2     Quick Turnaround Method Analysis &g£» .Sheets  (Form QI,  QIA,  and
            QIB)

      3     Laboratory Control Sample (LCS) Data Sheet  (form QII)
                                  ' >?;; •- .
      4     Performance Verificata^a',^aiKlax4;,.(PVS) Data  Sheet (Form QIII)
                                  ^V;>^         * ;;• ; ;
      5     Initial  Calibration She&t (Form QIV& and>;QI\&)
                                     ''          •" *

      6     Calibration Check Sheet (Fejcm QV3 ,';

      7     Analytical Sequence Summary (Form QVI)

      8     Narrative  jEform Qfll^           -  :
                     f 'i:         if?.            ;•-,
      9     Sample I^g-In Sheet (jform QDC-1)
                   •0            ^ff,:,s--
      10    Documentwlmrentory , SJ$ISti; r-$jj033&. C^SC - 2 )

      General  Information 'and .-Header Information
                             -' " _ 5,* J;-.
      Values sbaj«l fee  reported OTa;|%e forms according to  the individual  form
                  ;''s".::     Section'. ?v ' !
         .. •• -                -!  -.--
1.1   AjyTijcharacters which lJ'gjpp&aT on the data reporting forms presented in the
      Statement  of Work (S0^«.,( Exhibit B, Section IV) shall be  reproduced by
          Contractor when sutasiLtting data, and the format of the  forms
                 shall  be idetteJLcal to that shown in this SOW.   No information
                   , deleted^?s»r moved from its specified position without
      prior teitefcen approva$,.sbf the EPA APO.  The names of the  various  fields
      and compotasifi ,^e.g.,: *JLab Code", "Benzene") shall appear  as they  do on
      the forms  i
                                      B-30
                                                                        08/23/94

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                                                                          DRAFT

1.2   Alphabetical entries made  on  the  forms by the Contractor shall be in ALL
      UPPERCASE letters.  If an  entry does not  fill the entire blank space
      provided on the form, null characters shall  be used to  remove the
      remaining underscores that comprise the blank litie.   (See Exhibit H for
      more detailed instructions.)  However, do not tealove the underscores or
      vertical bar characters  that  delineate "boxes" ion ;the forms.

1 . 3   Six pieces of information  are common to the  "header sections  of each data
      reporting form.  They are:  Lab Name, Contract,  Lab Code , ;C«tse No.,
      Batch No., and Special Analytical  Service (SAS)  No.  (if applicable).
      This information shall be  entered  on evsry form and must be  the- same on
      every form.

      1.3.1 The "Lab Name" shall be the  name chosen by, the Contractor to
            identify the Laboratory.  It msy'jjpt excseS 25 characters.
                                            '• '•/    j, -
      1.3.2 The "Contract" is  the number of the EP& .contract  under which the
            analyses were performed.  In no case shall. multiple laboratories
            operate under a corporate -wide contract.    ;  , ,
      1.3.3 The "Lab Code" is an /alffea&etiieal abbreviation of up  to  six
            letters, assigned by 'gjA. to Tdeatify' t&a Laboratory  and aid in
            data processing.  This %ode shall ,Jsfe'! ass&gnfed by EPA  at  the time a
            contract is awarded, and shall not be modified by the Contractor,
            except at the direction of ::EPA. ;, If a change  of name  or  ownership
            occurs at the Laboratory, the ,3Jafc code  shall  remain the  same until
            the Contractor is directed by :18?A to use another lab  code assigned
            by the EPA. ,  "• '/             '\  „

      1.3.4 The "Case? So." is thejEPA- assigned "Case number (up to five
            characters) associated with the  sample, and reported  on  the QTM
            TR/COC form.        '^

      1.3.5 The "Batch^So,", will be indicated on the QTM  TR/COC.   If however,
            the "Batch No.*?, Us not indicated on the QTM TR/COC, the  laboratory
            shall assign it as ,t%e EPA sample number of the first sample
            received, in the Batdtu :,"JJhen several samples  are received together
          , ii« 4&e*%i*kt;::Satch shipiaeat, the Batch  number shall be the lowest
         ,,,s; sample number ;|consider ing both numbers and letters)  in  the first
       if--'  group of sampiifesSrireceived under  that Batch.

            The "SAS No."  is'-f&ie EPA assigned number for  analyses performed
            under Special  Anplgrtical Services.  If  the samples are to be
           aaaalyzed under Sa&S only and reported on these forms,  then enter
                    number _in both the "SAS No." and "Case  No." fields.   If
                      e analyzed according to the "Routine  Analytical
            Services* j(Mf)  IFB and have additional "SAS"  requirements,  then
            list both "$&S  No.  and Case No. on the forms.   If the  analyses have
                                     B-31
                                                                      08/23/94

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                                                                    DRAFT
      no SAS requirements, leave "SAS No." blank.   NOTE:
      in a Batch may have a SAS No. while others do not.
                                                                 Some samples
1.4
1.5
The "Sequence No." is also common to most of  the,/forms.   The Sequence
No. is a laboratory-assigned number (up  to  two characters)  that is used
to group sample data with their associated  QC":a3aba -within a fraction.
This number is used by the QTM software  in  generating -the Analytical
Sequence Summary (Form VI).  The software sorts  the  dafca «sing the Case,
Batch, and Sequence number.  If two instruments  are  used '^ analyze a
fraction for a Batch of samples, two different sequence  numbers A( e. g. ,
"01" and "02") should be assigned.  Secftience  numbers among the different
fractions can be the same (e.g., a Se§«ence number of "01"  for both
volatiles and PAH) .  (See the QTM Software  Users Guide for more
details . )                           * 'v
The other information common to most of- 43sje J&wans  is  the  "EPA Sample
No."   This number appears in the upper rig&t-laand corner of Forms QI,
QIA, and QIB (NOTE: Forms QIA and QIB are for kroelors  analysis only).

All samples, LCSs, PVSs, method blanks , instrument blanks,  and standards
shall be identified with asfp^Stl.g^pi^^iiijmber.  For field samples, the
EPA sample number is the unique ideh^i^iiaa^^WBtber given  in the QTM
TR/COC form that accompanied '-,^be sample. -: ?'

1.5.1 For samples, the following jtdenEif,ication scheme  shall be used as
      the "EPA Sample No.":          , ^
      QXXXXX
      QXXXXXRE
      QXXXXXDL,'
      QXXXXX-Yi

      where: ' •£
                           original sample ;;',,
                           reaife£|jjj£zed sample'^.
                           sampleSittialyzed at i-a .secondary  dilution
                           subsample number for multi-phase  samples
>.;.XXXXX U
                                             five character  sample  number
         >.2 For blanks and
         -$-;  shall be used asi*he
                  Y "is£a, suffix number  1,2,3,...  etc.  to differentiate
                  betwteeScWiilti-phase samples  (e.g., QXXXXX- 1 is the
                                   for  the  first  phase unit) .   If
                                         s are  required for a sample
                         the suffix RE  and/or  DL  shall follow the phase
                         number (e.g.,  QXXXXX - IRE ).
                             es, the  following  identification scheme
                            'EPA Sample No."
               methodpLanks shall be  identified  as  QVOBLK##.
               instalment blanks shall be  identified as QVOIBLK##-
                          Control Samples  shall be  identified as
      QVOLCS##.
                               B-32
                                                                 08/23/94

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                                                              DRAFT

Volatile  Performance Verification Standards shall be identified as
QVOPVS##.

PAH method blanks shall be identified as Q?ABLK##.
PAH instrument blanks shall be identified; as QPAIBLK##.
PAH Laboratory Control Samples shall be iideatified as QPALCS##.
PAH Performance Verification Standards shall b6 identified as
QPAPVS##.

Phenol method blanks shall be ident&fied as QPHBLK##. |?
Phenol instrument blanks shall be identified as QPHIBLK$$«
Phenol Laboratory Control Samples shall be identified as QPHLCS##.
Phenol Performance Verification 'Standards shall be identified as
QPHPVS##.

Pesticide  method blanks shall be identified as QPEBLK##.
Pesticide  instrument blanks shall be identified as QPEIBLK##.
Pesticide  Laboratory Control Samples shalj:,be identified as
QPELCS##.                                  ! ;    .
Pesticide  Performance Verification Standards  shall be identified
as QPEPVS##.         ;:   dr ;,' ,; • , .,
                       • ;*     ' *; f'' "-'/
Aroclor method blanks slhall be identified as,QARBLK##.
Aroclor instrument blanks shall bfe .identified as QARIBLK##.
Aroclor Laboratory Control',-Samples shall be identified as
QARLCS##.
Aroclor Performance Verificatioiti Standards shall be identified as
QARPVS##.   ,-  ;  : '             ,: .
            '  '     ','  ;-
NOTE:  "#|1,is  a contactor-defined identification number.
        ''            Is- •  •
      the  "EPA SampIjfrjfo,''  shall be  unique for each QC  sample and
      bLa»kj-,within ja.^^ficiij-- lif «ore than one sequence  is run
      withim/a batch,  the sample number assigned by the Laboratory
      must be'-'ttnl^fue for the  batch,  i.e.,  a blank in sequence one
      must not hssreithe sane  EPA Sample No. as any in sequence
            Within atjEiraction,  a laboratory may achieve this
                 by replacing the  two-character ny^#"  suffix of the
                 with one or  two characters or numbers,  or a
      combination  of both.

      For example,;: given a  batch with two  sequences and two method
      blanks wit&in each sequence, the blanks  may be  identified as
      follows:  ,'.< i
               .'•>•'
    ,v; Sequencp; i: QVOBLK01  and QVOBLK02
               ''2: QVOBLK03  and QVOBLK04
                         B-33
                                                          08/23/94

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                                                                          DRAFT

                  If an instrument blank  is  used in place of a method blank
                  (see method blank "Frequency"  section in Exhibit D) the
                  Laboratory shall use the character "Z" for the first "#" in
                  the EPA Sample No.  (e.g.,  QVOBLKZ1, ,^VOBLKZ2,  etc.).

                  If an LCS extract solution is  usest la :^Lace of the original
                  LCS solution  (see LCS "Frequency^ section1 -,in Exhibit D)  the
                  Laboratory shall use the character "Z" for, £be first "#" in
                  the EPA Sample No.  (e.g.,  QVOLCSZ1,  QVOLCSZ2,  etc.).

      1.5.3 For initial calibration and calibration check standards the
            following identification  scheme  shall be used as the "EPA Sample
            No.":                         /:  T          f,

            QFSTD####                     *;: ,r ,        r

            where:                               ; - '

            F =   fraction (VO  for volatiles, PA for pbljFnuelear aromatic
                  hydrocarbons, PH for phenols,  and PE for pesticides).
                                •>'<•• ^ '^f.^',   >; „
            STD = indicates a standard '"'" -  --,,;-,, ,

            #### =  the concentratioii^JLn  /ig/I*gSor volatile standards or the
                    amount injected ithtag foSsphenol and polynuclear aromatic
                    hydrocarbon and amotint^injected in pg for pesticide (for
                    multi-concentration stiaaaidards use  the lowest
                  - concentration).

            For Arocl^l initial Ssod calibration  .check standards, the following
            identification scheme shall be used  for the "EPA Sample No."
            Name     ;-,;. ,-,,       -;»,= "Zi '^\f'i' 5          EPA Sample No.
            Aroclor 1221  1 ;< .                         QAR1221####
            Aroclor 1232    k;jr,                       QAR1232####
                    .1242       "" ;<"-                    QAR1242####
                    ;12^B -        '-' -S                 QAR1248####
                    12540!;..,         "                 QAR1254####
            Aroclor 1016/l^S mixture                  QAR1660####
            Toxaphene       y..;                         QTOXAP####
                             -
            #### "  tne amouaafe  injected  in pg (e.g.,  if 20 pg is injected for
                    1232,  th^fcproper convention would be QAR12320020) .
1.6         Most: pieces of:*sLhformation  are  common to many of the Data
            ReportM^g So-rais.  These  include:   Matrix,  Sample weight or volume,
            Lab Sample dEB,: and  Instrument ID.


                                     B-34
                                                                       08/23/94

-------
                                                                           DRAFT

       1.6.1  For  "Matrix," enter "SOIL/SOLID" for soil/solid  samples,  "WATER"
             for  water samples, or enter (up to 10 characters)  other types of
             matrices (e.g.,  oil,  wipes, etc.).  The matrix must be  spelled
             out.   Abbreviations such as "S,""W," or "0* shall  not be used.
             Note:  For volatile oil samples enter "OIl,-HNM" for methanol non-
             miscible samples,  "OIL-MMAM" for methamol discible/aqueous
             miscible samples,  and "OIL-MMANM" forrfflethanol aiscible/aqueous
             non-miscible samples.                            ; ,

       1.6.2  For  "Sample wt./volume/other," enter the number  of graias »r
             milliliters of sample used or otteer amounts (e.g., area for"wipe
             samples).                       ,  •

       1.6.3  "Lab  Sample ID"  is an optional; 'laboratorygjgenerated internal
             identifier.  Up  to 12 alphanumeric, characters may  be  reported
             here.   If the contractor does not" hive "asi-ab Sample ID,  this field
             may be left blank.

       1.6.4  "Instrument ID"  is a  unique laboratory-assigned  10 character
             alphanumeric code  to 4$entify a particular instrument.   The
             identifier used  by tfaei|€^w>i5at:o3gr,jnust include some indication of
             the manufacturer and/fe^ ..model ~tfcfidlae%$of• the,.,instrument,  and
             contain additional characters that' Differentiate between all
             instruments of the same tgrpe in tfie Laboratory.

1.7    For rounding off numbers, observe' therxfollowing common rules.   If the
       number following those to be retained!'is less than five, drop it (round
       down).  If  the nunstear\f4vfgreater thaa'-Jfive,  drop it and  increase the
       last number  to be :.retaiiiea|by one (rotEft<3 up).  If the number  following
       the last digit !"to be retainifecl equals five, round up if the  number to  be
       retained is  ocld,  and round jefcawn if that number is even.

1.8    All times shall "be report^sdt'Sl^ijtgjj^sel-Biilitary convention (e.g.,  11PM is
       2300).             ! j

2      Quick  Turnaround Meth6aftiaa.lysis Data Sheets (Form 01 for PAH.  VOA.
       PHEN.  and 'JEST;-and Forms ^llL^amd QIB for PCB)

       Theses' 'forms  are use,<|<;for tabulating and reporting sample, method blank,
       a^ ,instrument blank^^alysis results and retention time information  for
       target compounds.   Thefse forms are also used to report all  retention
     ;<4t!fine data for the LCS,yl?VS,  and calibration check standards.   If not  all
                are requested for  analysis,  only the pages specifically
               shall be submitted.   For example, if only volatiles  analysis is
       requests^submit onjgi.:Form  QI-VOA;   if the  PCB analysis is the only
       analysis'iseqit^sted, ipiily Form QIA-PCB and QIB-PCB shall be  submitted  for
       that sampled  „; ;  ,/'  •
                                      B-35
                                                                       08/23/94

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                                                                           DRAFT

2.1   The Laboratory shall  enter on Form QI the mean RRT and RT values  from
      the initial calibration for each field sample and QC sample.  For
      Aroclors analysis,  two  Form QIs  must be completed:  Form QIA  (analyte
      concentration and SMC results) and Form QIB (RRTiand RT identification
      windows).  If RRT's are used for identification .-purposes, enter both  the
      RRT and RT for positive compound results.  If iSffys axe used for
      identification purposes enter only the RT values. :13lt-,and.RT values  for
      positive compound results  that are outside the identification windows
      calculated from the initial calibration shall be flagged With an
      asterisk "*" (see Exhibit  D) .            ('•'-•                  "  ;
                                             ! - *?
2.2   Complete the header information  on each page of Form QI that is
      required, according to  the instructional in Section" III, paragraph 1.
                                         ,1' - ',     -    •>'':•
2.3   "Date Received" is  the  date of sample ir-eaeipt ,a^ the Laboratory,  as
      recorded on the QTM TR/COC form.   It should b& centered in MM/DD/YY
      format .                                     • -  -

2.4   "Time Received" is  the  time of sample receipt reported in military
      convention (e.g., noon  is  IgsQfiL.and 11PM is 2300).
                                           ^
2.5   "Date Analyzed" is the  date TjpSE  sampli-'afl&ljrsis^  it should be entered  in
      MM/DD/YY format.              :,;         ;",«
                                     ' '        '''•.
2.6   "Time Analyzed" is the  time  of  sample ,&tlalysis reported in military
      convention (e.g., noon  is  1200  and IIJBH is 2300).

2.7   Enter Yes for "Additional .Cleanup" if sulfur cleanup is performed  (for
      PEST and PCB onlyp    "M4          •?- ,
                    ,$ii  '         '£ ,           " '''.-,.
2.8   If a sample hasrbeen dilutefli.|for  analysis1, enter the "Dilution Factor"
      as a single .sgfaole number, ^^Bfb. ;fs. , "JLQ0", for a 1 to 100 dilution of the
      sample.  If a' -staple was ^iStillk^^^nter "1".

      Note: The calculated cjiijtution factor shall consider all factors which
      affect the sample CRQL. dS|fb  5 alphanumeric characters) other concentration
                    >g/m2".)fgf
2.10  For the PMt^ilBHE, PIS3P,  and PCB forms,  enter in the "Extraction Type"
      field "SPE" ^rls^ika phase extracted samples and "SOLVENT" for solvent
      extracted samples,:':


                                      B-36
                                                                       08/23/9A

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                                                                          DRAFT

2.11  Enter in the  "Quantitation Type" field 1, 2, or 3 depending on the
      method of quantitation used.   If mean calibration factors from the
      initial calibration were used for quantitation, enter "1".  If mid-point
      calibration factors from the  initial calibratioa; were used for
      quantitation,  enter "2".   If  K-curve calibraticto' from the initial
      calibration were  used for quantitation,  enter *S?."\ Enter "2" as the
      quantitation  type for all Aroclors analyses,

2.12  For positively identified target compounds,  the Contractor shall report
      the concentrations detected as uncorrected for blank contaminants.

      NOTE: Calculations based on dry weights may occasionally be requested.
      If a request  is made for dry  weight !
-------
                                                                    DRAFT

The 13 EPA-defined  qualifiers to be used are as follows:

U -   Indicates compound was analyzed for but not detected.  The  sample
      quantitation  limit must be corrected for dilution.  For example,
      SOU for phenol  in water is used if the sample final volume  is the
      protocol-specified final volume.   If a -1 -'to; W dilution of  extract
      is necessary, the reported limit is 5QQU.

J -   Indicates an  estimated value.  This flag is used whe&ttiie
      chromatography  indicates the presence of a compound th)at>isafl:ix- 1« .igfpf^nded to ' tt& -UFA sample number on Form QI  for  the
   „' -, Sailuted  samplsv^and all concentration values reported on Form QI
  Ji;/ are flagged  witf^ythe "D" flag.
    '                  *'
       This  flag identiies all field sample and blank data  (detects  and
       non-detects)  in «8fieh the SMC recovery is outside  the advisory
                range cf^J|50-150 percent.
        «'xj  v         -;-
P  -    ThiWofiag idep^^ies all field sample data  in which  the  QC
       criteria: "f«r-^(3ie PVS were not satisfied.  Flag the outlier
       compound(sj ?F" in all associated  field samples.  Laboratories
       shall  only flag those compounds which exceeded the primary

                                B-38
                                                                  08/23/94

-------OCR error (C:\Conversion\JobRoot\$NEPIS SEND\0000039K\tiff\2000AAPO.tif): Unspecified error

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                                                                          DRAFT

      See Exhibit D for more detailed  instructions  concerning the use of these
      data qualifiers.

2.17  SMC results shall be summarized  at  the bottom of Form QI.   "AMOUNT" is
      the calculated amount of  the  SMC in ng injected->(pg for pesticides and
      Aroclors) or total ng for VOAs.   "%REC"  is  the .percent recovery of the
      SMC (Note: enter 999 if recovery is greater than 998% or if peak
      interferences are present).   "SMC area"  is  the area of;tbe SMC from the
      GC data system output report.  "RT" is the  retention time;:«of the SMC in
      this analysis.  "1C RT" is  the mean retention time of the SMC -calculated
      from the initial calibration  analyses.(:! f,S.T %D" is the percent
      difference between the retention time /«£ the  SMC in this analytical run
      compared to the mean RT of  the SMC  calculated frqia the initial
      calibration standards.  RTX D results that  are outside QC limits shall
      be flagged with an asterisk "*"  (see-Inhibit  D|K"!:
                                               ':     !•
2.18  Enter only the retention  time data  (RRT  and Bl$ and the appropriate
      header information on Form  QI for the PVS,  LCS; and calibration check
      standards.  Leave all other fields  (e.g., "Analybfe XJoncentration", "Q",
      and SMC data) blank.        ;.
                                < <•"' ->V
2.19  When entering retention time|3data'ori^oiai.,4i:,fctX".the LCS,  PVS, and
      calibration check standards,  report both*tihe 'RRT a»d RT data on Form QI
      for all fractions except  Arocloars where:«fche RRT and RT data are reported
      on Form QIB-PCB.  Enter only  the-approfirlate  header information as
      described below.                     f

      2.19.1      For the• BJSJ-ienter the EPA Sample  No., Lab Name, Contract,
                  Lab:€dSie, slsJSb. (if applicable), Case No., Batch No.,
                  Se,,;Lab  Sampie4l3J* -»;(if used),  Date Analyzed, Time Analyzed,
           ,r-  •-:"-••'s!and-i;Quantitationv:'*            *<:,"'
2.20  RRILind  RT values thifc aare  outside the identification windows calculated
         in. the initial calibration shall be flagged with an asterisk  "*"  (see
         libit  D).            if
                                      B-40
                                                                        08/23/94

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                                                                           DRAFT

3     Laboratory Control Sample (LCS) Data Sheet (Form QII)

      This form is used to report the results of LCS analyses.   (NOTE:   All
      LCS  retention time data are reported on Form QI» .see Section  III,
      paragraph 2 . )                                   :

3.1   Complete the header information as instructed; in Section  III, paragraph
      1 , including the EPA sample number for the LGS .

3.2   For  the PAH, PHE, PEST, and PCB forms, enter in the "Extractiajai,T;ype"
      field "SPE" for solid phase extracted samples and "SOLVENT" for solvent
      extracted samples.

3.3   Enter the "Amount Added" in terms of :;total ng on -.column.   Enter the
      "Amount Observed" in terms of total tig '^recovered.

3.4   The  Laboratory shall determine the percent ixeeovery for each
      spiked analyte.   LCS percent recovery results "'stfcjat are outside QC
      limits shall be flagged with an asterisk "*" (see":Ixfeibit D) .
                                                            C ti'
3.5   SMC  results shall be summarized at the bottom of Form QII.
      "AMOUNT" is the calculated amount of'*t~h~e -\iSfC ^.B^ng injected (pg
      for  pesticides and Aroclors) or total ngtfor 7OAs;i  "%REC" is the
      percent recovery of the SMC  (Sf&ee: enter 999 if recovery is
      greater than 998% or if peak interferences are present) .   "SMC
      area" is the area of the SMC from thj3,£C system output report.
      "RT" is the retention time of the SJj&i,  "1C RT" is the mean
      retention time of --thfe {§1$3 calculatedljf com the initial calibration
      standards.   "RT,%B*"is tnejfjercent difference between the
      retention time/ifff* the SMC i» the LCS compared to the mean
      retention time^i *IC RT" calculated from the initial calibration.
      RT%  D results.; ithat are outside^QC, , limits shall be flagged with an
      asterisk "*'
      Performance Verification Standard CPVS) Data Sheet (Form QIII)
      This  fozm .i&;:ttse4 _ to report itlpe results of PVS analyses.   (NOTE:  All
      PVS rotwafetibn -bim.data are reported on Form QI, see Section III,
      paxagiraph  2.)       ?y,;;
        js I-.'' s '               " 3':
4.1   ,Ccippplete the  header iriformation as instructed in Section III, paragraph
     ,fll4!' including  the EPA salable number for the PVS.

4.2   Enter' :ehe  "Amount Addedf in terms of total ng on column.  Enter  the
      "AmountsaSimerved" init^rms of total ng recovered.
4.3   The PVS  is  two.fSUn^Si (2x)  the concentration of the low level
      initial  calibratil^il standard (see Exhibit D) .   The Laboratory
      shall determine  the percent recovery for each compound.  PVS

                                      B-41
                                                                        08/23/94

-------
                                                                           DRAFT

      percent recovery results  that are outside QC limits shall be
      flagged with  an asterisk  "*".

4.4   "Resol. % Valley"  is  the  GC resolution between tdae peaks specified  in
      Exhibit D.  "Resol. % Valley"  results that are outside QC limits  shall
      be flagged with an asterisk  "*".   For the Arocilcnes analysis, the
      Laboratory will report  only the highest percent valley result.

4.5   SMC results shall  be  summarized at the bottom of Form QITI,;'
      "AMOUNT" is the calculated amount of the>SMC in ng injected (pg,?,
      for pesticides  and Aroclors)  or total ng-for VOAs.  "%REC" is tfee
      percent recovery of the SMC   (Note:  easier 999 if recovery is
      greater than  998%  or  if peak  interfer^ices are present).  "SMC
      area" is the  area  of  the  SMC  from tt»6TGC system/output report.
      "RT" is the retention time of the SMCi'V^JC El"? is the mean
      retention time  of  the SMC calculated f roisi tfee: initial calibration
      standards.  "RT %D" is  the percent difference %etween the
      retention time  of  the SMC in  the  PVS compared *e» jthe mean SMC
      retention time  "1C RT"  calculated from the initial!^calibration. .
      RT% D results that are  outSjide QC limits shall be flagged with an
      asterisk "*"  (see  Exhibit $& ^  •;~
      Initial Calibration Sheet  (Fora QIVA and^IVBT ~<> ,

      After a GC system has undergone tbe i$L1:ial calibration at the specific
      concentration levels described in !$!xhlf>it D,  and after all initial
      calibration technical acceptance criteria have been met, the Laboratory
      shall complete andts«6mf*  Forms QIVA 'Jsad QIVB for all initial
      calibrations that ,apply to-i|»he samples|3alanks,  LCSs, and PVSs in the
      Batch, regardless of when  ~t|»e initial calibrations were performed.
                   •f'" " '           *-
5.1   Complete all/|*eader  inf orm^^Lpn ,,o.n both forms as described in Section
      III, paragrapii, „!,.;,, Enter ^^feMc^e-'IfeiS* and "Batch No." for the current
      data package, regardless  of  the original Case for which the initial
      calibration was perrojgwssd .   Enter  "Instrument ID", the date and time of
      the calibration analysesjfand the  standard concentrations.

5.2   Enter«;if^BCi1Bfati!©3cis,,.^actor  data'iiaar  each of the calibration points on Form
      QiyA^i' Enter undef^^e column labeled "CF", the mean of the calibration
      fa&gbrs for each anai^s|e.  The Laboratory shall report the %RSD for all
      CsSopounds and the SMC;,t|6For  the Aroclors analysis, calculate and report
      'ly %RSD values for tip.  1016/1260 standards and the SMC.  All %RSD
             outside the QC ilimits must  be flagged with an asterisk "*" .
           ' < X  ~ -            4*:' '
5.3   "ResoI:'-.^;Walley" is,,lite GC  resolution between the peaks specified in
      Exhibit D?;^;*Kjesol.,,-l^alley"  results that are outside QC limits shall
      be flagged witk\an-
-------
                                                                           DRAFT

5.4   Enter  relative  and absolute retention time data on Form QIVB.   Enter
      relative  and absolute  retention time data for each calibration standard
      and enter the "Mean RRT"  and "Mean RT" values under the appropriate
      columns.   Note:  For Aroclors,  report RRT/RT froa the low concentration
      standard.

6     Calibration Check Sheet (Form QV)             ••

      After  a GC system has  undergone the calibration check at*ti* specified
      concentration level (mid  level initial calibration standard). Described
      in Exhibit D, and after all calibration"fcheck technical acceptance
      criteria  have been met, the Laboratorys;shall complete and submit all
      Form QV for all  calibration checks that apply to.Jthe field and QC
      samples in the Batch.   (NOTE:   All (jsarlibration cibeck retention time data
      are reported on  Form QI,  see Sectionollpl, para|3:aph 2.)

6.1   Complete  all header information as in Section III, paragraph 1.  Enter
      the "Case No." and "Batch No." for the currentj&afea package, regardless
      of the original  Case for  which the calibration chfeclc?;was performed.
      Enter  "Instrument ID",  the -date and time of the calibration, and the
                                 **£"• ^ ' •
      standard  concentration.   EAefe'jtijje ^pa^ilwcation factor data for the
      calibration check.   The Lafegatory 'sha|[i|^p,«Kt:r«the %D for all compounds
      and the SMC.  For the  AroclorJrj^analysis^calcttlisteMnd report  only  the
      %D values  for the 1016/1260 standards asl the SMC.  All ZD values
      outside the QC limits  shall be EtaggediMth an asterisk "*".

6.2   Enter under the  column labeled "Initial CF",  the mean calibration factor
      calculated from  tb^itsfjEilal calibration for each compound.  Calculate
      the percent difference 'fXIJ)^between the ^calibration factors.
                     i**           t &, ,           J1"
6.3   SMC results shiU'l be summat3||ed at the bottom of Form QV.  "SMC
      area" is the-a£ea of the S|feJ;£rpm, ,£hft GC system output report.
      "RT" is the relation tinil^Mi^MC  "1C RT" is the mean
      retention time of •*£§£& SMC calculated from the initial calibration
      standards.  "RT %D" ~i&l:fche percent difference between the
      retention time of the SI|Csi|n  the calibration check compared to the
      mean retenfciffa 'time "1C R"P?i/*£alculated from the initial
                          .results tffciaa: are outside QC limits shall be
              with an asterisk  "*"  (see  Exhibit D).
                          ""^S--,
6.4   TJSisol. % Valley" is tife GC resolution between the peaks specified in
              D.  "Resol. X W^Lley"  results that are outside QC limits shall
                 with an asterisk "*".   For the Aroclors analysis,  the
                 will repor$*itjnly the highest percent valley result (see PCB
                              '
                                     B-43
                                                                       08/23/94

-------
                                                                          DRAFT

7     Analytical Sequence Summary  (Form QVI)

      This form is required for  each analytical sequence for each GC system
      and for each GC column used  to analyze  samples.  3Form QVI summarizes the
      date and time of analysis  of field and  QC samples  and standards specific
      to a particular Batch and  associated with each initial calibration or
      valid calibration check.                      ,         ,

7.1   Complete the header information on each Form QVI required-.according to
      the instructions in Section  III,  paragraph 1.
7.2   "Analytical Sequence Start Date"  and fs&aalytical Sequence Start Time" is
      the date and time that the current analytical sequence was started.  The
      initial calibration analytical  sequ^siee begins with the injection time
      of the first initial calibration  stattSlalfcd and ,£fee daily calibration
      analytical sequence begins with the infection if time of the first
      instrument blank.                          !

7.3   "Analytical Sequence Stop Date" and "Analytical Sequence Stop Time" is
      the date and time that the analytical sequence ends ^ritSi a final PVS .
      The final PVS standard in -fi^?,a|j4t^l,^c.aliibration analytical sequence
      must be analyzed within 24 tlfurs  af ter' wibfe i&J«c,tion time of the first
      initial calibration standard -aisd  the final FVS sfcasflard in the daily
      calibration analytical sequence «ust beW«nalyzed within 24 hours after
      the injection time of the first lisstrumetit blank.  If the first PVS does
      not meet all QC criteria, a second ,"SVS,{ analysis may be performed within
      26 hours after the start of the current analytical sequence.
7.4   List all field a&SsQC  saddles  and standards for a specific Batch
      analyzed under, yjiat  initiaTa|ealibration^«3: valid calibration check in
      chronological .r&rder, by  tin^/of analysis -< in military time).  Enter "EPA
      Sample No.," ^liab Sample I|||*_"_Daj;e ^Analyzed, "  and "Time Analyzed" for
      all analyses li&fced  on Fo^sll
-------
                                                                          DRAFT

8.2   The  Laboratory shall specify in the volatiles Batch Narrative the target
      compounds associated with (detected by) each of the detectors (PID and
      ELCD)  and in the phenols Batch Narrative the detector type used (PID or
      FID).

8.3   If dry weight calculations are requested, the-pexe£nt moisture values
      for  all relevant samples shall be documented in the-Batch Narrative.
      The  Laboratory shall also state in the Batch Narrative ;i» bold print,
      verbatim:  "Sample concentrations for this Batch are based on dry weight
      calculations".                           ,                      ;

8.4   Whenever data from sample reanalyses are submitted, the Contractor shall
      state  in the Batch Narrative for each preanalysis .^whether the contractor
      considers the reanalysis to be billable, and if.so, why.  The Contractor
      shall  also include any problems encountered (both technical and
      administrative),  the corrective actions taken, •; and resolution.

8.5   If the VTSR date is adjusted for samples received during non-routine
      working hours as described in Exhibit A, Section'SEIl,.paragraph 9.5, the
      Laboratory shall note this $gx ,£he Batch Narrative(s).;

      If sample extractions and/6'tf«analyse':s" *8»re -s&freed. .after the receipt
      date and before the VTSR as dsfined in Exfaibii-A'i flection III,  paragraph
      9.5, the Laboratory shall state,.in the Jisttch Narrative,  verbatim:  "The
      extraction and/or analyses of the following samples received during non-
      routine working hours were started.'after the sample receipt date/time
      and before the  VTSR as defined in Exhibit A, Section III."  A listing of
      all associated  EPA sample numbers shall follow this statement.
8.6   The Laboratory.j&liall  submiTpa cover sheet with the hardcopy deliverables
      that states, ygfbatim:  "I  certify that this data package is in
      compliance witfc  the terms .^EJj^cpnditions of the contract,  both
      technically and?£or compl|eBe^|s;f=;|fo|r?-other than the conditions detailed
      above.  Release  of the  data contained in this data package has been
      authorized by the Laboratory Manager or his designee,  as verified by the
      following signature."  S^i35,s,statement shall be directly followed by
      signatvure^of..^^ Laborat6r3r||4agiager or his designee with a typed line
      beloW|;i1tiWoritkiia^k% the  signers name and title,  and the date of
      sigpaiture.  The  eii^aponically delivered Batch Narrative shall have,  in
      pljapa of the signatutsfe^  the words "Signature Obtained."
      
-------
                                                                          DRAFT

      the deliverables for  the  other Batch(es).   The  copies should be
      identified as  "copy(ies),"  and the  location of  the original should be
      noted on the copies.                             " •

9.2   Sign and date  the airbill (if present).   Examine  the shipping container
      and record the presence/absence  of  custody seali astnd their condition
      (e.g., intact, broken)  in item 1 on Form  QDG-1.   Record the custody seal
      numbers in item 2.                                       ;':
                                                               * ^ * • ;-
9.3   Open the container, remove  the enclosed ^sample  documentation ^ sarad record
      the presence/absence  of the combined QIM  TR/COC form(s),  the  CLASS
      contractor forms (e.g., packing  list),,,iand airbills  or airbill stickers
      in items 3-5 on Form  QDC-1.  Specify.f'if there is .an airbill present or
      an airbill sticker  in item  5 on  Fona-ljDC-1.  Record the airbill or
      sticker number in item  6.            ™1  ''      if
                                              *.,  '* *    - <
9.4   Remove the samples  from the shipping container^) ,  examine the samples
      and the sample tags (if present), and  record the  Condition of the sample
      bottles (e.g., intact,  broken, leaking) and presence,sor absence of
      sample tags in items  7  and  ^-OsCuJ'orm QDC-1.          : '
9.5   Review the sample shipping doeuments"'atKi-lcos^Kketes the header information
      described in Section  III, paragraph  1.  .fttanpare the information recorded
      on all the documents  and samples;and matt;-the  appropriate answer in item
      9 on Form QDC-1.

9.6   If there are no problems observed  during  receipt,  sign and date (include
      time) Form QDC-1, ,t?fae 'GgRji. ,£R./COC fona^iiand write  the sample numbers on
      Form QDC-1.  Record the appropriate  sample tags and assigned laboratory
      numbers, if applicable.  Trae log-in  dateT$hould be recorded at the top
      of Form QDC-1 -fS&d the date ^apd time  of  cooler  receipt at the Laboratory
      should be receded in iten^pj|Q.,aiid- ,11,,,,,, Cross  out unused columns and
      spaces.      " ,-,-/-        ^SH^i, -' 5.; •- •

9.7   If there are problems ssefeserved during receipt  or  if an answer is marked
      with an asterisk (e.g. ,' ^yfcsent*"),  contact  the CLASS contractor and
      document-ta&ftfSeoatact  as well^ias resolution of  the problem in a CLP
      Commutfissation 1^1. ^Following^t^solution,  sign and date the forms as
      specified in the preceding paragraph and  note, where appropriate, the
      resolution of the
9.8  ,,Jfe^cord the fraction designation  (if  appropriate)  and the specific area
      'declination (e.g., refiiigerator  number)  in the  Sample Transfer block
      lockt«|t'4n the bottom ;le£t  corner  of Form QDC-1.   Sign and date the
      Sample i
                         ,
10    Document Inveiibo^/Sfteet  (Form QDC-2)

      This sheet is used to  record  the  inventory of the hardcopy deliverables .

                                     B-46
                                                                       08/24/94

-------
                                                                         DRAFT

10.1  Assemble the documents in the order specified on Form QDC-2 and in
      Section II of Exhibit B,  and stamp each page with a consecutive number.
      (Do not number the QDC-2 form).  Inventory the CBF by reviewing the
      document numbers and recording page number ranged in the columns
      provided.  If there are no documents for a specific document type, enter
      "NA" in the empty space.                            :

10.2  Certain laboratory specific documents related to the CB3? ;may not fit
      into a clearly defined category.   The Laboratory should review Form QDC-
      2 and determine the most appropriate place to insert documents.
                                     B-47
                                                                      08/24/94

-------
     SECTION IV  Yr'-
DATA REPOKTHJG f^RMS
                                            DRAFT
        B-48
                                         08/23/94

-------
SAMPLE LOG-IN SHEET
Lab Name: Pa8e of
Received RV (Print Namel: Log-in Date:
Received By (Signature):
Case Number:
Ratch:
SAS Number:

REMARKS:
1. Custody Seal(s) Present/Absent*
Intact/Broken
2 Custodv Seal Nos.:


3. QT Traffic Report/Chain- Present/Absent*
of-Custody Forms
4 Packing List Present/Absent*
;, ••"'.
< -•;, ',/'-.
sample tags ag«»f Yes/No* ;;' -
«%. ; •*? *~
10. Date Recefeetftat Lab:
-, - J '''4 - ' ' 1
11. Time Receivd&F*:;: >- ' ''•';'
•-/!- .::•
Sample Transfer / -
Fraction: ' $ - •
Area*: *''• 2
By:
On:

EPA
SAMPLE
#




':= •



V >\ ' VS' 7 }

; ,'•
,:v-'



M, ' I 'd


'%








CORRESPONDING
SAMPLE
TAG
* :

,'






,...*
.- ', . • ^
', •'•''•;

















ASSIGNED
LAB
#
,'



























REMARKS:
CONDITION OF
SAMPLE SHIPMENT,
ETC.



























* Contact the CLASS contractor and attach record of resolution
Reviewed By:	
Date:	
Logbook No.:	
Logbook Page No:
                                                   FORMQDC-1

-------
                   ORGANICS COMPLETE BATCH FILE (CBF) INVENTORY SHEET
  LABORATORY NAME	  CITY/STATE
  CASE NO.	 BATCH NO.	 BATCH NOS. TO FOLLOW	^_ 	 SASNO..
  CONTRACT NO.	 SOW NO.	~	
       All documents delivered in tbe complete Batch file must be original documents where possible. (REFERENCE
       EXHIBIT B, SECTION H AND SECTION m.)                                 «
                                                           PAGENOs      CHECK
                                                   r:      FROM ;tp    LAB   EPA
1.  Inventory Sheet (Form QDC-2) (Do not number)
2.  Batch Narratives (Form QVH)
3.  TrafBc Report
4.  Volatiles Data
   a. QCData                            J "
      Lab Control Sample (Form QH-VOA)    \.;
      Method Blank Summary (Form QI-VOA)
      Performance Verification Standard (Form
      Analytical Sequence Summary (Form QVI-VOA)
   b. Sample Data
      TCL Results - (Form QI-VQj&)    *uJ1,
      Chromatograms for each *Sip8ple         :::f
                         s ''••'             "
   c. Standards Data (AH Instraments)         d
      Initial Calibration
      Chromatograms and IntegratioilJReports for all Standards
      Calibration Check (Form QV-VOA}-''i, ,
5.  PAH Data      „  ,:-; v ,-  ,         '"" $-$- ^
   a. QCData ,',?JS   =--*-   ., ^,., ._         v--^,
      Lab Cootrtil Sample (Form
          A '••&
      Metioa Blank Summary (Form
      E^Hismance Verification Standard (Rsm QIH-PAH)
      Analyieli^equence Summary (FornfagVI-PAH)
   b. Sample DataV-i;,;.,„           /?"--'"
      TCL Results - (Fcirla SS^PAH)^?!
      Chromatograms for eacH «
                                        FORM QDC-2-1

-------
                   ORGANICS COMPLETE BATCH FILE (CBF) INVENTORY SHEET
  CASE NO.	 BATCH NO.	 BATCH NOS. TO FOLLOW	 SAS NO.
                                                             PAGENOs      CHECK
                                                            FROM   TO    LAB   EPA
   c. Standards Data (All Instruments)
      Initial Calibration Data (Form QIVA and QIVB-PAH)
      Chromatograms and Integration Reports for all Standards
      Calibration Check (Form QV-PAH)
6.  Phenols Data
   a. QCData
      Lab Control Sample (Form QU-PHE)
      Method Blank Summary (Form QI-PHE)
      Performance Verification Standard (Form QEH-PHE)
      Analytical Sequence Summary (Form QVI-PHE)
   b. Sample Data                          v
      TCL Results - (Form QI-PHE)
      Cbromatograms for each sample
   c. Standards Data (All Instruments)
      Initial Calibration Data (Form QIVA and QIVB-PHE)
      Chromatograms and Integration Reports for all Standards
                             - -  '    ' °   ,i ^
      Calibration Check (FormXplAPHE)     r?
7.  Pesticides Data          , :
   a. QC Data            j                •      ;    ,
      Lab Control Sample (Fora* pJ&REST)   	
      Method Blank Summary (Form Q1-BEST)
      Performance Verification Standard (Form
      Analytical Se^oseab StoaBI(fjr 

-------
                   ORGANICS COMPLETE BATCH FILE (CBF) INVENTORY SHEET
  CASE NO.	 BATCH NO.	 BATCH NOS. TO FOLLOW	  SAS NO..
                                                               PAGBWOs      CHECK
                                                              FROM   TO    LAB   EPA
8.  Aroclors Data
   a. QCData                                                                      '
      Lab Control Sample (Form QH-PCB)
      Method Blank Summary (Form QI-PCB)
      Performance Verification Standard (Form QIH-PCB)
      Analytical Sequence Summary (Form QVI-PCB)
   b. Sample Data
      TCL Results - (Form QI-PCB)
      Chromatograms for each sample
   c. Standards Data (All Instruments)
      Initial  Calibration Data (Form QIVA and QEVBTOB)  ; {  ,
      Chromatograms and Integration Reports for at! S&andards
      Calibration Check (Form QV-PCB)
9.  Miscellaneous Data
   Original preparation and analysis forms or copies of preparation
   and analysis logbook pages          , ;,                   ,?,
                                    ' !* •-!,',  ?;
   Internal sample and sample extract transfer chais*of-custody forms
10. EPA Shipping/Receiving Daccfeaents         «0
   Airbills (No. of shipments j)             ;JLS'~- .-'   ,;-  ...
   QT Traffic Report/Chain-ofiC«stcJ%.Forms'' '" "'"*     ''"''"'  "'
   Sample Tags                    •,,;;•
   Sample Log-In Sheet (Lab & QDC-1)    '
   Batch Cover SAedi-s ••'''•-'•;,.;;.,;,_:          ~^,  v
   Miscellaneous: Shipping/Receiving Recrards
            *"''                      "
11. Internal Lab Sample Transfer Records and Tracking Sheets
                 '•-<4- vr           -'• -~s
   (describe or list)  ^f;,]  .„       ?;'< '
                                           FORM QDC-2-3

-------
                ORGANICS COMPLETE BATCH FILE (CBF) INVENTORY SHEET
  CASE NO.
BATCH NO.
BATCH NOS. TO FOLLOW
                                                                  SASNO.
12. Other Records (describe or list)
                                                    PAGE NOs     CHECK
                                                  FROM   TO    LAB   EPA
Telephone Communication Log
,, -
13. Comments:


, \
Completed by:
(CLP Lab) (Signature)
Audited bv:
(EPA) (Signature)
' £' - •' •' ;
^ = (PrtotedJflaine/IWe) (Date)
; _ •;
^dated Name/Title) (Date)
                                   FORM QDC-2-4

-------
                                                              EPA SAMPLE NO.
                        VOLATILES ANALYSIS DATA SHEET
Lab Name:
Lab Code:           Case No.
SAS No.:
Instrument ID:
Matrix:
Sample wt./volume/other:
Dilution Factor:
Units:       Wet-Weight
Quantitation Type:
       Contract:
Batch No.:
Sequence No.
       Lab Sample ID:
       Date Received:   /  /
       Time Received:   :
       Date ISnalfzed:   /  /
       Time Analyzed:   :
COMPOUND
vinyl chloride
1 , 1- dichloroethene
trans-1, 2 -dichloroethene
ANALYTE
CONCENTRATION



1 , 1 - di chl oroe thane |
cis- 1 , 2 -dichloroethene
chloroform
1,1,1- trichloroe thane
carbon tetrachloride
benzene
1,2- dichloroe thane
t r ichloroethene
bromodichloromethane
toluene
t e t rachl or oe thene
chl orobenzene
1,1,2,2- tetrachloroethan-
ethylbenzene r
bromoform ,v:
m,p-xylene :: :
o-xylene

,:£;!
> ;•',
• s- «•
?'



i

.- ' ^ t -.
, "••'•£

«,




- ' : 3- * * " :^. --.
; - '* * '

'-, *
'. . .. r.if,<~:-i
.":.,
* 5 '~ --

- ,">• . -
•*'-';':^.;.
/, ;
\

-/



^ <


I' ; ^- -~


RRT s

•t.





* "
~ '-.












1C RRT





















RT


1C RT


I




































                             SYSTEKIMQNITOR COMPOUND
System Monitcec^Compound !;
(QC Limits)
'; "^'
4 - bromof lu^bbenzene
^~f ^^
"^ "W?*"^ -^,
^ '
1^-fv
Af«3UNT
;^
i- f -'
%REC | SMC
(50-150) | AREA
I
RT

_
1C RT

RT %D
(+/- 1%)

  * Value outs^^-,-|)f QC limitsf!
  U Compound anal^^d, f or but fiot  detected.  Value  represents the Contract
    Required Quantifeadfc&pn LifFftl: (CRQL)  for the specified analyte.
    (Note: CRQLs must'lie'jcpojftcscted for dilutions.)
                                 FORM QI  -  VGA
                              12/92

-------
                 VOLATILES LABORATORY CONTROL  SAMPLE DATA SHEET
Lab Name:
Lab Code:
SAS No.:
EPA Sample No.:
Lab Sample ID:
Matrix:
Case No.:
       Contract:
Batch No.:
Sequence No.
                          Instrument ID:
                          Date Analyzed:   /   /
                          Time Analyzed:   :
1
COMPOUND
vinyl chloride
l, 1- dichloroethene
trans -1,2- dichloroethene
1,1- dichloroethane
cis - 1 , 2 - dichloroethene
chloroform
1,1,1- trichloroe thane
carbon tetrachloride
benzene
1,2- dichloroethane ,,
trichloroethene
bromodichloromethane
toluene
tetrachloroe thene
chlorobenzene
1,1,2,2- tetrachloroe thane
ethylbenzene
bromof orm /
m,p-xylene •• '" |;|,
o-xylene :1 • *\;
'-
AMOUNT
ADDED
(ng)



s •;






"' "

.. S;







5
; AMOUFT
OBSERVED
(ng) " -„:. .
<<








"" -












%REC
i- :,,




















System Monitor Compound
(QC Limits)
4 -bromof luorobeazene' • v;s
! ,^
AMOlife ,
:i..
%REC
(50-150)
':f
SMC
AREA

RT

1C RT

RT %D
(+/- 1%)

  * Value outiBlfctle of QC limits
                                 FORM QII - VOA
                                                  12/92

-------
             VOLATILES PERFORMANCE VERIFICATION STANDARD DATA SHEET
Lab Name:
Lab Code:
SAS No.:
EPA Sample No.:
Lab Sample ID:
Case No.:
       Contract:
Batch No.:
Sequence No.
                          Instrument ID:
                          Date Analyzed:
                          Time Analyzed:
COMPOUND
vinyl chloride
1 , 1-dichloroethene
trans -1,2- dichloroethene
1 , 1-dichloroe thane
cis - 1 , 2 -dichloroethene
chloroform
1,1,1- trichloroe thane
carbon tetrachloride
benzene
1,2- dichloroe thane
trichloroe thene
bromodichloromethane
toluene
tetrachloroe thene
chlorobenzene
1,1,2,2- t etrachloroethane
ethylbenzene
bromoform
m,p-xylene
o-xylene ;
AMOUNT
ADDED
(ng)

;
" , 1""' '
*
AMOUNT;
OBSERVED
tag)
!. ., .,.
. ' -,
' ,
f
;%REC
- ;•


RESOL.
IrVALLEY
i
i

                            SYSTEMfiaiONITOR COMPOUND
System Monitor Compound -;
(QC Limits)
4-bromofluorobenzene ;.- ,.
,:'fs;H -^:,S;;V:
AMOUNT
"' ; s''
%REC
(50-150)
;--?h.
SMC
AREA

RT

1C RT

RT %D
(+/- 1%)

  * Value outside of QC
                               FORM QIII - VGA
                                                 12/92

-------
VOLATILES INITIAL CALIBRATION SHEET
Lab Name: Contract:
Lab Code: Case No.: Batch No.: Sequence No.:
Instrument ID :
SAS I


Jo. :

CAL #1
CAL #2
CAL #3
EPA
SAMPLE NO.



LAB
SAMPLE ID



'-
DATE =, ,



TIME


j
STANDARD
CONG
i


COMPOUND
vinyl chloride
1,1- dichloroethene
trans -1,2- dichloroethene
1,1- dichl or oe thane
cis - 1 , 2 -dichloroethene
1,1,1- trichloroethane
carbon tetrachloride
benzene
1,2- dichloroe thane
trichloroethene
bromodichloromethane
toluene
tetrachloroethene
chlorobenzene J:'
1,1,2,2- tetrachloroethase*
ethylbenzene ;;
bromoform •'" -j>
m,p-xylene
o-xylene
4 -bromofluorobenzene
-•:'" V ••
* value outs ids ::>q8:lO.C "l-ima
CF
LOW





' •••••,






• s/ ">: ;i-l:'
'K',l '•

r\ "'.
,:i'-V


'" , '- :
'•*
.ts
CF
MID',, '





;„ '" '•,"

J






\
l~ : ,
|;J>-; ,-' ,',. 1\-





CF 3
HIGH ;



"

' - .'; '







; •• '








;-
CF






















%RSD






















RESOL. j
%VALLEY






















         FORM QIVA -  VOA
7/92

-------
                     VOLATILES INITIAL CALIBRATION SHEET
Lab Name:
Lab Code:

Instrument ID:
Case No.:
       Contract:
Batch No.:

       SAS No.:
Sequence No.
COMPOUND
vinyl chloride
1 , 1 - di chloroe thene
trans -1,2- dichloroe thene
1 , l- dichloroe thane
cis -1,2- dlchloroethene
chloroform
1,1,1- trichloroethane
carbon tetrachloride
benzene
1,2- dichloroe thane
trichloroethene
bromodichlorome thane
toluene
t e t rachl oroe thene
chlorobenzene
1,1,2,2- tetrachloroethane >>
ethylbenzene
bromoform
m,p-xylene
o-xylene
4 -bromof luorobenzene
	
L















i'X^K i
,.j *,;•• , J


':.'•• '

_v;
RETENTIOl
M






,:r
,

r „ >


'<



;> - • ?
•,i \\ ;., _ ;
;; '.,' ' ' '"'




T TIME (B.1
H
-,





















[•)
MEAN




'
:, -
















COMPOUND *~
vinyl chloride I -.
1, l-dichloroetlxeos,,;, ,;,;
trans -1,2- dichlorc4thene
1,1 -dichloroe thane '-,?•-,
cis - 1 , 2 - dichloroethene ": ^ "'
chloroform.^' f,-,f ,
1,1,1- tr jkJlil-cdroe'tilSHje
carbon ,"fc^tracnlori3e^' ..,
i , 2 -dichloroethane * ^
tri^feoroethene V/
broBk^lchloromethane /;•
toluenm-> v >^~
tetrachlori^hene _ /,!"
chlorobenzenk :, , /;:;,
1,1,2,2- tetrachiCKCQe^hane
ethylbenzene ""•- '•<•'.
bromoform
m,p-xylene
o-xylene
4 -bromof luorobenzene
i
RELAT
L
-.$,.- "': ' -•• :.* ,
,;&">, Q ' • ~~]-' -I



i&
• !'-'











^Bffi RETEt
i;;::: M


















i
ITION TIME
H



















: (RRT)
MEAN





































i
ill!
FORM QIVB - VGA 5/92

-------
                       VOLATILES CALIBRATION CHECK SHEET
Lab Name:
Lab Code:           Case No.
SAS No.:
Instrument ID:
EPA Sample No.:
Lab Sample ID:
Standard Concentration:
              Contract:
       Batch No.:
           Sequence No.
              Date Analyzed:   /  /
              Time Analyzed:   :
            COMPOUND
INITIAL CF
MID.
 RESOL.
%VALLEY
    vinyl chloride
    1,1-dichloroethene
    trans-1,2-dichloroethene
    1,1-dichloroethane
    cis-1,2-dichloroethene
    chloroform
    1,1,1-trichloroethane
    carbon tetrachloride
    benzene
    1,2-dichloroethane
    trichloroethene
    bromodi chloromethane
    toluene
    tetrachloroethene
    chlorobenzene
    1,1,2,2-tetrachloroethane
    ethylbenzene
    bromoform
    m,p-xylene
    o-xylene              ,
    4-bromofluorobenzenq  ,
                           SYSTEM MONITOR COMPOUND
System Monitor CompoundT; -
(QC-l^araifes),
, ?. "v~- '* - - :\ :
4 - brom0f Suorobenzenej > > -.
.;£• ' ""5:
SMC
^ >,AREA

RT

1C RT

RT %D
(+/- 1%)

               .e outside of QQJlimits
                                FORM QV - VOA
                                     12/92

-------
                     VOLATILES ANALYTICAL SEQUENCE SUMMARY
Lab Name:
Lab Code:           Case No.:
SAS No. :
Instrument ID:
Initial  Calibration Date:   /  /
Contract i
  Batch No.:
Sequence No.:
Analytical Sequence Start Date:   /  /
Analytical Sequence Start Time:   :
Analytical Sequence Stop Date:   /  /
Analytical Sequebce Stop Time:   :
1

01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
.16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
3 If,
33t-
336
34
35
36
37
38
39
40
EPA
SAMPLE NO.


















,' !
! ;


• -,- r
'"


,-r - ',• - r •
,f r \- ' y
-\:.i'
: ''. ,;- -'


• f 9 '•-
-I K'. ,,
*' '•- M/,. ,
""' • ;;: A ,
1 •• ";
-I":


LAB
SAMPLE ID.









• •<;'.

•::>. ,^ , , _






'" I
4*L,
"- :
,;;1;, '.
i :>~ '-, }-. :1


?< ',
*£~, ; ..'„
"~ •
'••. :''•
\'v~,i
,,|i
•^?^

- kr
••*





DATE
ANALYZED
1 i
II
'• 1 1
II
= : / / :
/ /
/ /
If
1 1
1 1
/ 1
~~ ' '-'/ ' '/'' •"
'/"• / ''
/ /
7 /
" ' / /
II
1 1
' ~, / 1
t /
f i
1 i
X / /
/ /
/ /
/ /
/ /
/ /
/ /
/ /
/ /
/ /
/ /
/ /
/ /
/ /
/ /
/ /
/ /
/ /
TIME-
ANALYZED,
,

^
j.




































                                FORM QVI  - VOA
                                5/92

-------
                          VOLATILES NARRATIVE
Lab Name:                              Contract:
Lab Code:           Case No.:          Batch No.
SAS No.:
                           FORM QVII - VOA                        5/92

-------
                                                             EPA SAMPLE NO.
                           PAH ANALYSIS DATA SHEET
Lab Name:
Lab Code:
SAS No.:
Instrument ID:
Matrix:
Sample wt./volume/other:
Dilution Factor:
Units:       Wet-Weight
Quantitation Type:
Extraction Type:
Case No.:
       Contract:
Batch No.:
Sequence No.
                          Lab Sample ID:
                          Date Received:   /  /
                          Time Received:   :
                          Date/Analyzed:   /  /
                          Time ^'Analyzed:   :
COMPOUND
naphthalene
acenaphthyl ene
acenaphthene
fluorene
phenanthrene
anthracene
f luoranthene
pyrene
benz [a] anthracene
chrysene
benzo [b] / [k] f luoranthene
benzo [a] pyrene
indeno [1,2,3- cd] pyrene
dibenz [a, h] anthracene
benzo [g, h, i] perylene
ANALYTE
CONCENTRATION






,'t , ,^ ^

'•',

•'/\


' t* ,
"1'i'1- -
4-'
;" . ' V.





; ,r
•v" /*s^;






n -
i 	
RRT









1C RRT








'•" •;„ * i
'











RT















1
1C RT















                            SYSTEM;JANITOR .COMPOUND
System Monitor Compound-' ,
! (QC Limits)

,--'.-' , «/ •- ,;;,- .; -s
i ..~:\~ • —;.s
* Value outside of QC lints
AMOUNT

"=;
t^B.
%REC
(50-150)

*-.-'•:

SMC
AREA



RT



1C RT



RT %D
(+/- 1%)



  U Compound spalyzed for buf^tpt detected.  Value represents the Contract
    Required:i^iantitation Limi^(CRQL)  for the specified analyte.
    (Note: 4PQLS must be correcifed for dilutions.)
                                FORM QI - PAH
                                                 12/92

-------
                    PAH LABORATORY CONTROL SAMPLE DATA SHEET
Lab Name:
Lab Code:
SAS No.:
EPA Sample No.:
Lab Sample ID:
Matrix:
Extraction Type:
Case No.
       Contract:
Batch No.:
Sequence No.
                          Instrument ID:
                          Date Analyzed:   /
                          Time Analyzed:   :
1
COMPOUND
naphthalene
acenaphthyl ene
acenaphthene
f luorene
phenanthrene
anthracene
f luoranthene
pyrene
benz [a] anthracene
chrysene =
benzo [b] / [k] f luoranthene :
benzo [a] pyrene I
indeno [ 1 , 2 , 3 - cd] pyrene
dibenz [a, h] anthracene
benzo [g,h, i]perylene
AMOUNT
ADDED
(ng)
$ I ;?• -
h "-•.*>,
AMQUST
OBSER'SED
(ng) -* ,


%REC


                                   MONITOR COMPOUND
System Monitor Compound ;
(QC Limits) J|
2-bromonaphthalene " x4- ,.
•'•
•|>>,,
AMOUNT^
I'-ij
V |2* ^
%REC
i50-150)
i--
'Sl-JK; u!i y:
: SMC
AREA

RT

1C RT

RT %D
(+/- 1%)

  * Value outside of QC limits;
                                 FORM QII - PAH
                                                  12/92

-------
                PAH PERFORMANCE VERIFICATION STANDARD DATA SHEET
Lab Name:
Lab Code:
SAS No.:
EPA Sample No.:
Lab Sample ID:
Case No.:
       Contract:
Batch No.:
Sequence No.:
                          Instrument ID:
                          Date Analyzed:
                          Time Analyzed:
COMPOUND
naphthalene
acenaphthylene
acenaphthene
fluorene
phenanthrene
anthracene
f luoranthene
pyrene
benz [a] anthracene
chrysene
benzo [b] / [k] f luoranthene
benzo [a] pyrene
indeno [ 1 , 2 , 3 - cd] pyrene
dibenz [a, h] anthracene
benzo [g/ h, i] perylene
AMOUNT
ADDED
(ng)





AMOUNT;;,
OBSERVED
(rig)
;,' ,
*


'"'"'"'. 1' ':-, •:. :-,
'
%REC
- ;•"'




RESOL.
%VALLEY





                            SYSTEM MONITOR COMPOUND
System Monitor Compound y ;
(QC Limits) ,-.-'•
2 - br omonaphthal ene
•
* Value outside of QC 1'ind
AMOUNTfi
'&i
, : ll
obs.
%REC
:(50-150)
--
' '?.<' .' :" -.

I'- SMC
~; -: AREA



RT



1C RT



RT %D
(+/- 1%)



                               FORM QIII - PAH
                                                 12/92

-------
                        PAH INITIAL CALIBRATION SHEET
Lab Name: Contract:
Lab Code: Case No.: Batch No.: Sequence No.:
Insti
SAS I
rument ID:
lo. :

CAL #1
CAL #2
CAL #3
EPA
SAMPLE NO.

LAB
SAMPLE ID

DATE
:
TIME
-;-_
5><
STANDARD
CONG
- '•'•'-

COMPOUND

naphthalene
acenaphthy 1 ene
acenaphthene
fluorene
phenanthrene
anthracene
f luoranthene
pyrene
benz [a] anthracene
chrysene
benzo [b] / [k] f luoranthene
benzo [a] pyrene
indeno [ 1 , 2 , 3 - cd] pyrene
dibenz [a,h] anthracene
benzo [g, h, i] perylene /- '-:
2 - bromonaphthalene \
CF
LOW





j
'•i.
>





, t
: " '*"- M
i>i
.•!.;•
CF -ri
MID. ;
'J.




vf ~ -' •
!K< •: : • ,' ,"< ,
N *•'-., >.,.<

:1 ,



• ~il •


f

CF ,
HIGH I


1
•' i



1 -- : : .
?" ; • "'_.
'-,'








CF


















%RSD

















RESOL.
%VALLEY

















* Value outside of QC -limits
                              FORM QIVA - PAH
7/92

-------
                         PAH INITIAL CALIBRATION SHEET
Lab Name:
Lab Code:

Instrument ID:
Case No.
       Contract:
Batch No.:

       SAS No.:
Sequence No.
COMPOUND
naphthalene
acenaphthy 1 ene
acenaphthene
fluorene
phenanthrene
anthracene
f luoranthene
pyrene
benz [a] anthracene
chrysene
benzo [b] / [k] f luoranthene
benzo [a] pyrene
indenb [1,2,3- cd] pyrene
dibenz [a,h] anthracene
benzo [g, h, i] perylene
2 - br omonaphthal ene

L














•i*
.t;">-' j;:, |v.;%
oY- 's-
RETENTIO1
M






-,

's
'^: ^
f' ' •'.'

'';


^ , ,
~ "' • ...• , i
I "TIME (R'
H

















D
MEAN




;-•" :-:












! COMPOUND
\
naphthalene
acenaphthylene '- \
acenaphthene '-• ^
fluorene ,; •-•:•• *
phenanthrene s ,
anthracene ;;;" ~
f luoranthene "Z- ,,- &
pyrene ,: ,,
benz [a] anthracene •-, I
chrysene • , ,f .
lr"?n^o [t>] / [kj'fcli^or'Snt'hpn^ •'
benzo [alj^'jsene" ~ '% 3r.!/ ;,,
indenql:^^ , 3 - cd] pyrene
diben^5KL, h] anthracene^,'*
ben^^g , h, i] perylene |' ~~:
2 -bs^honaphthalene »l
-EELA1]
f
;-_

'I5B RETE1
- •; M

TTION TIM!
H

3 (RRT)
MEAN

                               FORM QIVB - PAH
                                                 5/92

-------
                          PAH CALIBRATION CHECK SHEET
Lab Name:
Lab Code:           Case No.:
SAS No.:
Instrument ID:
EPA Sample No.:
Lab Sample ID:
Standard Concentration:
       Contract:
Batch No.:          Sequence No.
       Date Analyzed:   /  /
       Time Analyzed:   :
COMPOUND
naphthalene
acenaphthylene
acenaphthene
fluorene
phenanthrene
anthracene
f luoranthene
pyrene
benz [a] anthracene
chrysene
benzo tb] / [k] f luoranthene
benzo [a] pyrene
indeno [1,2,3- cd] pyrene
dibenz [a , h] anthracene
benzo [g,h, i] perylene
2 -bromonaphthalene
INITIAL CF










V .. ; •.

,»^j - «-, ;
-. ,, _


MID






is


' j:


r~ ' -^ '..,'
;-'.;•" -' j-;
:\

* *B>.
















RESOL.
%VALLEY
















System Monitor Compound :
(QC Limits} |f
"'^'..r. :-fc
2 -bromonaphthalene ? ,
"' 4- y
i' SMC
'i.«w- ,
-,',l-: -Si ,";-;-

RT

1C RT

RT %D
(+/- 1%)

         * Value outside of QC
                                FORM QV - PAH
                              12/92

-------
                        PAH ANALYTICAL SEQUENCE SUMMARY
Lab Name:
Lab Code:           Case No.:
SAS No.:
Instrument ID:
Initial Calibration Date:   /  /
Contract:
  Batch No.:
Sequence No.
Analytical Sequence Start Date:   /  /
Analytical Sequence Start Time:   :
Analytical Sequence Stop Date:   /  /
Analytical Sequence Stop Time:   :


01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
o o
28
29
30
31jS
34
33i
34
35
36
37
38
39
40

EPA
SAMPLE NO.


!














,;
;••
^ ? ,



~f.


/' '• *, <

,,;, ,;H"*~ *" ' *\ ,
C'l' ' '"
;;!?"
•; :


' ftf'i »-.,-,
' '*''"•%-*,
"* :^-
'•*?'-' ; - <
"•;•, u-



LAB
SAMPLE ID.



•n





..,-:
\ ' T- ;|J> -;;;:-
!' „ ' :
"

^ i


,'';-.,
: ^''^G-
*;'•„"!

r ";
-§£''':LJiJ",!'"^'
:":
'' 1 I -

v?;, ,;.
\ ; ' ^

~|^
"'^1.
'' ','
V"':-
;, > ^
';'• l'
•• J-'';i
,- V -'
iil
t



DATE
ANALYZED
""J^"""
/ /
9'/ /
:' / / ^
5 / / -
' / j •
/ /
/ / !
/ / :
/ /
Ml i

*"K /'••*
/ i
•-, f i
':• 1 1
1 /
i, / /
> -M 1
V /
/ /
/ /
r / /
*" / /
/ /
/ /
/ /
//
/
/ /
/ /
/ /
/ /
/ /
/ /
/ /
/ /
/ /
/ /
/ /
/ /

TH8S
ANALYZED












.;,


























i
|
i
                                FORM QVI - PAH
                                5/92

-------
                             PAH NARRATIVE
Lab Name:                              Contract:
Lab Code:           Case No.:          Batch No.
SAS No.:
                           FORM QVTI - PAH                       5/92

-------
                                                              EPA SAMPLE NO.
                          PHENOLS  ANALYSIS DATA SHEET
Lab Name:
Lab Code:
SAS No.:
Instrument ID:
Matrix:
Sample wt./volume/other:
Dilution Factor:
Units:       Wet -Weight
Quantitation Type:
Extraction Type:
Case No.
       Contract:
Batch No.:
Sequence No.
                          Lab Sample ID:
                          Date  Received:    /  /
                          Time  Received:    :
                          Date,  SShalyzed:    /  /
                          Time  Analyzed:    :

COMPOUND
phenol
2 - chlorophenol
o-cresol
m/p-cresol
2 - nitrophenol
2,4- dimethylphenol
2,4- di chlorophenol
4- chloro- 3 -methylphenol
2,4, 5/6 - trichlorophenol
2,4- dini trophenol
4 - nitrophenol
2,3,4,6- tetrachloropheno
4,6- dinitro - 2 -methylphen
pentachlorophenol

ANALYTE
CONCENTRATION






• ' >s ~,
'''• ' :
i <




j.
,,' '"**

,3 '

•




li ' *
i^ ",:' '_ -



'- NS
/'

\

RET
: •
-
,
/I",


' '••', •











1C RRT
-















RT
















1C RT















                            SYSTEM IH0NITOR COMPOUND
System Monitor Compound ,;
(QC Limits)
o - bromophenol
™Wf
"' - ',-'*••«
Tsb-iso)'
..
SMC
AREA

RT

1C RT

RT %D
(+/- 1%)

  * Value outsidi|'«Jfi">QC*!:l|itii^s.
  U Compound analyzed for Ifrdb^ot  detected.   Value represents the Contract
    Required ®uantitation Lintffe (CRQL)  for the specified analyte.
    (Note: G8$JLs must be corre'elled for dilutions.)
                                  FORM QI -  PHE
                                                   12/92

-------
                  PHENOLS LABORATORY CONTROL SAMPLE DATA SHEET
Lab Name:
Lab Code:
SAS No.:
EPA Sample No.:
Lab Sample ID:
Matrix:
Extraction Type:
Case No.
       Contract:
Batch No.:
Sequence No.
                          Instrument ID:
                          Date Analyzed:
                          Time Analyzed:
COMPOUND
phenol
2 - chlorophenol
o-cresol
m/p-cresol
AMOUNT
ADDED
(ng)



,
2-nitrophenol j <
2,4- dimethylphenol
2,4- di chlorophenol
4 - chloro - 3 -me thylphenol
2,4, 5/6 - trichlorophenol
2,4- dini t rophenol -&
4-nitrophenol ,|
2,3,4,6- tetrachlorophenol "\
4,6- dini t ro - 2 - methy Iphenol
pent achl or ophenol

- '




'*?,,' ;
'. ™ * '"•'• ~
' 5
*'; •-. ;
- ,,• '\s
•» -
AMOUNT
OBSERVED
(ng) ',«












='


%REC
•: •,.


I











                            SYSTEM MONITOR COMPOUND
System Monitor Compound ;
(QC Limits) ,;!
'•:
o-bromophenol ,
AMOUNT.*J
•4
f$
%REC '
(50-150)
>3':i? ^:"
i SMC
'• AREA
:-
RT

1C RT

RT %D
(+/- 1%)

  * Value outside of QC limits
                                 FORM QII  -  PHE
                                                 12/92

-------
             PHENOLS PERFORMANCE VERIFICATION STANDARD DATA SHEET
Lab Name:
Lab Code:
SAS No.:
EPA Sample No.:
Lab Sample ID:
Case No.
       Contract:
Batch No.:
Sequence No.
                          Instrument ID:
                          Date Analyzed:
                          Time Analyzed:
                        /  /
COMPOUND
phenol
2 - chlorophenol
o-cresol
m/p-cresol
2 -nitrophenol
2,4- dimethylphenol
2 , 4 -di chlorophenol
4 - chloro- 3 -methylphenol
2,4,5/6- trichlorophenol
2 , 4 -dinitrophenol
4 -nitrophenol
2^ 4. fi- t"e»1"T"Splil rrtTJTih^noT

4,6- dinitro - 2 -methylphenol
pentachl or ophenol
AMOUNT
ADDED
(ng)
-; ,
H:' *' """ '
K
AMOOJIT, „
OBSERVED
(ng)
^". 1
%' \"i , :"
' •&-', ..„ ,,
" j." •• •-" ':<:
^a,TjT?^i
; tk^rCciL



RESOL.
%VALLEY
' 3'


                            SYSTEM MONITOR .
System Monitor Compound
(QC Limits) s . :;
o-bromophenol :; '
"^ -.>
^j

(50-150) =
:r
SMC
s AREA

RT

1C RT

RT %D
(+/- 1%)

* Value outside of QCJaaaits. ,;,^:s\3ib JSL ^ ,-1:
                               FORM QIII - PHE
                                                 12/92

-------
Lab Name:
Lab Code:

Instrument ID:
SAS No.:
                       PHENOLS INITIAL CALIBRATION SHEET
Case No.
       Contract:
Batch No.:          Sequence No.:

CAL #1
CAL #2
EPA
SAMPLE NO.

CAL #3 |
!
LAB
SAMPLE ID

DATE :-

i
TIME

STANDARD
CONC

•t

COMPOUND
phenol
2 - chlorophenol
o-cresol
m/p-cresol
2 -nitrophenol
2,4- dimethylphenol
2,4- di chlorophenol
4 - chloro- 3 -methylphenol
2,4,5/6- trichlorophenol
2 , 4-dinitrophenol
4 - nitrophenol
2,3,4,6- tetrachlorophenol
4,6- dini t ro - 2 -methylphenol
pentachlorophenol •
o-bromophenol , ::
CF
LOW





.3 ,
Y<"





-*
e .
-
CF ; •
MID :





.,' "';_• •
" ''" " <; "
'••' ,

,/
' '




CF ,
HIGH ;

' i , '
• ""/



' •• '* •- ; ' ^ •>
( '- • .'

-



- xi


j CF



--












%RSD















RESOL. |
%VALLEY

•













 * Value outside of QC limits
                               FORM QIVA - PHE
                                                 7/92

-------
                      PHENOLS INITIAL CALIBRATION SHEET
Lab Name:
Lab Code:

Instrument ID:
Case No.:
       Contract:
Batch No.:

       SAS No.:
Sequence No.
COMPOUND
phenol
2 - chlorophenol
o-cresol
m/p-cresol
2-nitrophenol
2,4- dimethylpnenol
2 , 4 -di chlorophenol
4 - chloro- 3 -methylphenol
2,4,5/6- trichlorophenol
2 , 4 -dinitrophenol
4 - nit rophenol
2,3,4,6- tetrachlorophenol
4 , 6 -dinitro- 2 -methylphenol
pentachl or ophenol
o-bromophenol
L







\
'- :<
1




?^'k! ....
RETENTION
M





jV ;
v" Y


: 1;,
"A " •" ' X




I !TIME (R1]
H
ij












• ; ; ,

[•)
MEAN




..__"•










i
COMPOUND
phenol
2 - chlorophenol
o- cresol ; ' >
m/p-cresol -i- /"" *""( I
2-nitrophenol -"?•: 1
2,4- dime thy Ipheiiai
2,4- dichloropti^ol |
4 - chloro- 3 -meti|gyptoenol , j
2,4,5/6- trichloropliel^ol
2, 4 -dinitrophenol >,v -v-
4 -nit rophenol rr -
2,3,4,6- teferacMficrophenoi- ;
pentactijlorophenol '^T?,|,
.'* . RELA1]
-I,
^ •&. {':'**
.'IVK-.WflHa
,;l-(' M

ITXON TIME
H

: (RRT)
MEAN

                               FORM QIVB - PHE
                                                 5/92

-------
                        PHENOLS CALIBRATION CHECK SHEET
Lab Name:
Lab Code:           Case No.:
SAS .No.:
Instrument ID:
EPA Sample No.:
Lab Sample ID:
Standard Concentration:
       Contract:
Batch No.:
Sequence No.
       Date Analyzed:   /
       Time Analyzed:   :
COMPOUND
phenol
2 - chlorophenol
o-cresol
m/p-cresol
2 -nitrophenol
2,4- dimethylphenol
2 , 4 -di chlorophenol
4 - chloro- 3 -methylphenol
2,4,5/6- tri chlorophenol
2,4- dini trophenol
4 - nitrophenol
2,3,4,6- tetrachlorophenol
4 , 6-dinitro-2 -methylphenol
pentachlorophenol
o - bromophenol
INITIAL CF



;






-- •
."• '£.>••',.. "
•%

:; -
i
MID
~



^ ;,


T

" ' i
'


'<' .; .'''„. „.
'I ~~
f
%»'
r






%VALLEY








i
;











"- '• \ \
System Monitor .Csxtpound
(QC Liming)
o- bromophenol '••-, ^- .%£
..-:. -...
•'•,, SMC
,1 AREA
&•'•!£•%•.' !;:
;RT

1C RT

RT IrD j
(+/- 1%) \

         * Value outside of QC"limits.
                                FORM QV - PHE
                              12/92

-------
                      PHENOLS ANALYTICAL SEQUENCE SUMMARY
Lab Name:
Lab Code:           Case No.
SAS No.:
Instrument ID:
Initial Calibration Date:
         Contract:
           Batch No.:
Sequence No.
         Analytical Sequence Start Date:   /  /
/  /     Analytical Sequence Start Time:   :
         Analytical Sequence Stop Date:   /  /
         Analytical Sequence Stop Time:   :
1
!
I
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31;
^
34
35
36
37
38
39
40

EPA
SAMPLE NO.



















\j

-f:

••* ,^~,



T- ' ",
: : .'if *"• ':'' ,\- '
•'• * * ' *
, *'_;'''" '
Ff ;
•'>'
*"•?:"•'
'V;.-V'
-; '
'"- ; ' ' .-:




LAB
SAMPLE ID.




>:
:





- -'' ,;!»- • '?•.
y „ '. ;
'': t
,',,,



:,'" ''VI
' ' *" ' :' i .''
'•*'•?
*'•'*.'
•: -2 '
f- ' **?'" " ',. % ^





. ; ^ >
'lit--
V,
,• '.'•',
v-;i-
4 '•'
-'f! •





DATE
ANALYZED

/ /
7 /
/ /
/ / i
/ 1 :-
• / .'/ :: ," "
/ -/ "'
/ /'•'
/ 1
1 1
5 ,,/ /
'- «;$/ / ;•
/ / ' '';
/ /
,:-/ /
1 1
I 1
-. 1 1
-J 1
-j?. /
/ /
/ /
i^r / /
/ /
/ /
/ /
/ /
/ /
/ /
/ /
/ /
/ /
/ /
/ /
/ /
/ /
/ /
/ /
/ /

TBSE
ANALYZ®}
*









-






























                                FORM QVI - PHE
                                         5/92

-------
                           PHENOLS NARRATIVE
Lab Name:                              Contract:
Lab Code:           Case No.:           Batch No.
SAS No.:
                           FORM QVTI - PHE                       5/92

-------
                                                              EPA SAMPLE NO.
                         PESTICIDES ANALYSIS DATA SHEET
Lab Name:
Lab Code:            Case No.
SAS No.:
Instrument ID:
Matrix:
Sample wt./volume/other:
Dilution Factor:
Units:       Wet-Weight
Quantitation Type:
Extraction Type:
       Contract:
Batch No.:
Sequence No.
       Lab Sample ID:
       Date Received:    /   /
       Time Received:    :
       Date ^Analyzed:    /   /
       Time, Analyzed:    :
       Additional Cleanup  (Y/N)
COMPOUND
alpha -BHC
beta-BHC
gamma -BHC (lindane)
delta-BHC
heptachlor
aldrin
heptachlor epoxide
gamma - chl ordane
endos'ulfan I
alpha - chl ordane
4,4'-DDE/dieldrin
endrin
endosulfan II
4,4'-DDD
endrin aldehyde
endosulfan sulfate ;,
4, 4 '-DDT ,;-V
endrin ketone J
methoxychlor 4;l
ANALYTE
CONCENTRATION


t' ..
"* """ s - ; -. %


;*;
4
' • Vs J>:-' ; '•'
•*'*- -^ L ; , ,'i
&
;'- ;•-
k. ',,',;.


w-:.*;x
;, '
"~ ^
-"?••


KB.T •
: :

' * ':
Y - - -




i

1C RRT


;






RT

1C RT
\
















                                   .MONITOR  COMPOUND
(QC LdjsUs) 's
decachlorobigaienyl
M:
	

(50-150)

SMC
AREA

RT

1C RT

RT %D
(+/- 1%)

  * Value o'Sil|bde of QC limits||\
  U Compound iBa^-zed for but j^fot detected.  Value represents the Contract
    Required QuaiSt^a,j:ion l>±miX*i (CRQL)  for the specified analyte.
    (Note: CRQLs mu&l:fcl« corseted  for  dilutions.)
                                 FORM QI  -  PEST
                              12/92

-------
                PESTICIDES LABORATORY  CONTROL SAMPLE DATA SHEET
Lab Name:
Lab Code:
SAS No.:
EPA Sample No.:
Lab Sample ID:
Matrix:
Extraction Type:
Case No. :
       Contract:
Batch No.:
Sequence No.:
                          Instrument ID:
                          Date Analyzed:
                          Time Analyzed:
COMPOUND
alpha- BHC
beta-BHC
gamma -BHC (lindane)
delta-BHC
heptachlor
aldrin
heptachlor epoxide
gamma- chlordane
endosulfan I
alpha -chlordane f
4,4' -DDE/dieldrin ^
endrin v-
endosulfan II
4, 4' -ODD
endrin aldehyde
endosulfan sulfate
4, 4' -DDT
endrin ketone "- ;
methoxychlor ¥ "- :^,
s "f V'.
AMOUNT
ADDED
(ng)
%, \'

<*


' j



* *-
,*- V ;£ - -
"" **" «-., vi " " S ^- J;

<:




*
jl
s!; .
ANOEMT
OBSERVED ,
(ng) , ;.


















i
%REC


















i
i
                                           COMPOUND
System Monitor Compound 3"
(QC Limits)
decachlorobiphenyl,/ ;- \\ ,,
jC-'sH '= '- -:;; '%('•'•
KJCJQNT
'• y
%REC
(50-150)
' k. ;?
SMC
AREA

RT

1C RT

RT %D
(+/-•!%)

* Value outside of QC limi&s.
                                FORM QII - PEST
                                                  12/92

-------
            PESTICIDES PERFORMANCE VERIFICATION STANDARD DATA SHEET
Lab Name:
Lab Code:
SAS No. :
EPA Sample No.:
Lab Sample ID:
Case No.
       Contract:
Batch No.:
Sequence No.
                          Instrument  ID:
                          Date Analyzed:    /
                          Time Analyzed:
COMPOUND
alpha -BHC
beta-BHC
gamma -BHC (lindane)
delta-BHC
heptachlor
aldrin
heptachlor epoxide
gamma- chlordane
endosulfan I
alpha- chlordane
4,4' -DDE/dieldrin
endrin
endosulfan II
4,4'-DDD
endrin aldehyde
endosulfan sulfate
4, 4' -DDT
endrin ketone
met boxy chl or :
AMOUNT
ADDED
(ng)











. '••-, ,'L; 1
' ;S'
'*' " <




'< * ,.
AMOUNT T
OBSERVED
(ng)


;:
.r ' '

-.- ' -





- -:-,;?•
'-' * ' Jf , i'
* .';-' ,
"'
"



•;%REC
' "'• !


















RESOL.
%VALLEY

j '

















                             SYSTEM I^PNITOR COMPOUND
System Monitor Compoua§ „• ,
(QC Limits) p
decachlorobiphenyl
I 	 ^
.l&BSi
MDUNT
*'~£\ :
(50-150)'
>
SMC
AREA

RT

1C RT

RT %D
(+/- 1%)

  * Value outsiders!*"- QG; -lipji-ts.
                                FORM QIII - PEST
                                                  12/92

-------
Lab Name:
Lab Code:

Instrument ID:
SRS No.:
                      PESTICIDES INITIAL CALIBRATION SHEET
Case No.:
       Contract:
Batch No.:
Sequence No.


CAL #1
CAL #2
CAL #3
EPA | LAB
SAMPLE NO.

SAMPLE ID

!
	
DATE



TIME

<
STANDARD
CONC

:''s
COMPOUND
alpha -BHC
beta -BHC
gamma - BHC ( 1 indane )
delta -BHC
heptachlor
aldrin
heptachlor epoxide
gamma - chl ordane
endosulfan I
alpha - chl ordane
4,4'-DDE/dieldrin
endrin
endosulfan II
4,4'-DDD
endrin aldehyde .f\
endosulfan sulfate /!''
4, 4' -DDT
OT1^T*T n ^** **\ *- f^m f^
ciiuxxn ivcuons
methoxychlor :
decachlorobiphenyl
CF
LOW





1 ' "f
.,.; ^ • * ' ^., ^ •. ..;
=;

V ,--*
!"

' '




! . '«r ' T :: ;



CF
HIGH






; } ^
S '' '.

»











CF





















%RSD





















RESOL.
%VALLEY





















* Value outside qf: ,QC.:limits -,,,..
                              FORM QIVA - PEST
                                                7/92

-------
                       PESTICIDES  INITIAL  CALIBRATION SHEET
Lab Name:
Lab Code:

Instrument ID:
Case No.
       Contract:
Batch No.:

       SAS  No.:
Sequence No.:
COMPOUND
alpha -BHC
beta-BHC
gamma -BHC (lindane)
delta-BHC
heptachlor
aldrin
heptachlor epoxide
gamma - chl ordane
endosulfan I
alpha - chl ordane
4,4' -DDE/dieldrin
endrin
endosulfan II
4,4' -DDD
endrin aldehyde
endosulfan sulfate •
4, 4 '-DDT
endrin ketone
methoxychlor
decachlorobiphenyl
L







',
',,





" ~, •
• *- ; - ^; <
* *> ' - *
* :
;-

RETENTION
M









; s






" '*"t-| -;%, 3
'i *
' ';

I = TIME (R1]
H


_ 5,
'J-,'



:~









i<


D
MEAN



:-1
















,-
COMPOUND ; 'J1' "'"' *=V
alpha -BHC „. •*
beta-BHC I:
gamma -BHC (lindaae), , ;;>
delta-BHC ; :
heptachlor \ ),.
aldrin 'v-;/^
heptachlor^fipep^de '^
gamma - chSolpSane1 ^ ;? .. s
endosuU^n I j, -
alpha^^ilordane """;; ,-
4 , 4 '.-liDE/dieldrin '%
entf%TOlfaT1 TT "' -
endrin al^!s%yde ---f
endosulfan' MlSate I
4, 4 '-DDT '• T ;;,-•, A '•••
endrin ketone
methoxychlor
| decachlorobiphenyl
!
RELA1
L
.;! .,,...,..».
!fc ';:^, .'.-J
-" ; - 4
UVE RtfL'K*
-;=. M

ITION TIME
H

! (RRT)
MEAN

                                 FORM QIVB - PEST
                                                   5/92

-------
                       PESTICIDES CALIBRATION CHECK SHEET
Lab Name:
Lab Code:           Case No.:
SAS No.:
Instrument ID:
EPA Sample No.:
Lab Sample ID:
Standard Concentration:
              Contract:
       Batch No.:
           Sequence No.
              Date Analyzed:   /  /
              Time Analyzed:   :
            COMPOUND
INITIAL CF
MUD
 RESOL.
%VALLEY
    alpha-BHC
    beta-BHC
    gamma-BHC (lindane)
    delta-BHC
    heptachlor
    aldrin
    heptachlor epoxide
    gamma-chlordane
    endosulfan I
    alpha-chlordane
    4,4'-DDE/dieldrin
    endrin
    endosulfan II
    4,4'-DDD
    endrin aldehyde
    endosulfan sulfate
    4,4'-DDT
    endrin ketone
    me thoxychlor
    decachlorobiphenyl
                          , .SYSTEM^
System Monitor Compound
(QC Limits) '• s ,
decachloriibiplies^i " \,
£'.*•' 'V,\.
SMC
AREA

RT

1C RT

RT %D
(+/- 1%)

         * VaJE|ie outside of Q0;;;limits
               '
                                FORM QV - PEST
                                     12/92

-------
                     PESTICIDES ANALYTICAL SEQUENCE SUMMARY
Lab Name:
Lab Code:           Case No.:
SAS No.:
Instrument ID:
Initial Calibration Date:   /   /
Contract:
  Batch No.:
Sequence No.:
Analytical Sequence Start Date:   /  /
Analytical Sequence Start Time:   :
Analytical Sequence Stop Date:   /  /
Analytical Sequence Stop Time:   :
1

01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31S
3HJT
33.;
34
35
36
37
38
39
40
i
EPA
SAMPLE NO.


















.;,-
4 '•'•'
'!'


".;:;; >


rn , Z- "
£•& " v "'^ %
. ;:".i~?
• €' '
'!''
ij
:il ;, .,
'"*.'.,"', ; '.^
*^'*M'r'-"
-- i • . _
i!'-'f ~- 1
r . !•
''


LAB
SAMPLE ID.









*-
-"' ' P ' ' ""'; ' ;
-?|, ~ • -i- -,(
*'~
*



' ": ' ' •',
'"' ''# ,^
"'*; "
V'";
,^E"
^-l^fc^-'i?! ' :?

" .'? : ,;
*""^l->;.
:;-^.;.,;,
'•''\* '•'
• ""'•:,
'^|Sr
';"|,_
• < .. %

•''• ;:
^ fe - "
Jl.
.'•'"'"





DATS
ANALYZED

•"'/ /
•l / /
/ / /
' / / •
' •/- 11 '
/ /:
/ /< ' -,
1 /
1 1
> • / 1
''*%'$'•'
-------
                          PESTICIDES NARRATIVE
Lab Name:                              Contract:
Lab Code:           Case No.:          Batch No.
SAS No.:
                           FORM QVII - PES                        5/92

-------
                                                              EPA SAMPLE NO.
                         AROCLORS ANALYSIS DATA SHEET
Lab Name:
Lab Code:
SAS No.:
Instrument ID:
Matrix:
Sample wt./volume/other:
Dilution Factor:
Units:       Wet-Weight
Quantitation Type:
Extraction Type:
Case No.:
       Contract:
Batch No.:
Sequence No.
       Lab Sample ID:
       Date Received:
       Time Received:
       Date Analyzed:
       Time
       Additional
   up (Y/N):
COMPOUND
toxaphene
Aroclor-1016
Aroclor-1221
Aroclor-1232
Aroclor- 1242
Aroclor-1248 ,
Ar ocl or - 12 5 4 •< '-. -
Aroclor -12 60 !"r;|
ANMjYTE
CONCWTRATION ;
>'• •' ;,'•
'-•'•* V ! ; , -
" ' X » ',, ~ _
-::• ' ;•:<
Q

                            SYSTEM MONEK3R
System Monitor Compound
(QC Limits)
decachlorobiphenyl ~
J-"
AMOC3NT
* "" % ,M
" -A
S* 5
%REC-<;
(50- 150 j

SMC
AREA

RT

1C RT

RT %D
(+/- 1%)

  * Value outside of QCJ21 imits.
  U Compound analyzed f ut not
     fValue represents the Contract
    Required Quantitation Sijpit  (CRQL) for  the  specified analyte.
     (Note: CRQLs must be corJsected for dilutions.)
                                  FORM QIA -  PCB
                                12/92

-------
                                                             EPA SAMPLE NO.
                         AROCLORS ANALYSIS DATA SHEET
Lab Name:
Lab Code:
SAS No.:
Instrument ID:
Matrix:
Quantitation Type:
Case No.
       Contract:
Batch No.:
Sequence No.
                          Lab Sample ID:
                          Date Analyzed:
                          Time Afflklyzed:
                        /  /
COMPOUND
Aroclor-1016



Aroclor-1260




toxaphene


Aroclor-1221


Aroclor-1232 ;

Aroclor- 1242

- ,;3
Aroclor-1248,,. ;
., >" " """ V ,,

f l";" f •
Arocloa|~s1254 \
•';? .£:.
'H,
:V;i'' ,;,
;...L -....,...>.?
PEAK
1
2
3
4
5
1
2
3
4
S, ..
3r -'i
3 •;
4
1
2
3
1
- "a
4-'-
;K,-
' '3'
4
2^'
3
4
5
1
. 2
3
4
5
RRT



!





'&• ' ;•• V ;
'*•
''-
i • v (-
•,'


^
	
* ' • •" '










1C
RRT



.;,-'

;




; ' - - • ;- ~;


















,
"






--_





















1C
RT
"' „ ';




























                                FORM QIB - PCB
                                                 5/92

-------
                 AROCLORS LABORATORY CONTROL SAMPLE DATA SHEET
Lab Name:
Lab Code:
SAS No.:
EPA Sample No.:
Lab Sample ID:
Matrix:
Extraction Type:
Case No.
       Contract:
Batch No.:
Sequence No.
                          Instrument ID:
                          Date Analyzed:   /
                          Time Analyzed:   :

COMPOUND
toxaphene
Aroclor-1016
Aroclor-1221
Aroclor-1232
Aroclor-1242
Aroclor-1248
Aroclor-1254
Aroclor-1260
AMOUNT
ADDED
(ng)






AM00ST
OBSERliiEfi
(ng) ""•: f/-.





•' ,

%REC






System Monitor Compound
(QC Limits)
decachlorobiphenyl
AMOUNT

t-*REC
(§8-150)
' " V*
/ ,SMC ';;- -.
; AREA
-,,-r,-,- -^
'
RT

1C RT

RT %D
(+/- 1%)

  * Value outside of QC
                                 FORM QII  - PCB
                                                  12/92

-------
           AROCLORS PERFORMANCE VERIFICATION STANDARD DATA SHEET
Lab Name: Contract:
Lab Code : Case No . : Batch No . : Sequence No . :
SAS No . :
El
Lc



=A Sample No.: Instrument ID:
»b Sample ID: Date Analyzed: / /
Time Analyzed; :

COMPOUND
Aroclor-1016
Aroclor-1260

AMOUNT
ADDED
(ng)



AMOUNT
OBSERVED
(ng)


i
; j RESOL.
%RSC % VALLEY
i
-,:,,. |

-. i i
                          SYSTEM MONITOR -COMPOUND :
System Monitor Compound
(QC Limits)
decachlorobiphenyl
AMOUNT
1?
%REC
(50-150)
V-:;,
!SPC
AREA

RT

1C RT

RT %D
(+/- 1%)

* Value outside of QC limits
                             FORM QIII - PCB
12/92

-------
                        AROCLORS INITIAL CALIBRATION SHEET
 Lab Name:
 Lab Code:
 SAS No.:
Case No.:
       Contract:
Batch No.:
Instrument ID:
Sequence No.


CAL #1
CAL #2
CAL #3
toxaphene
1221
1232
1242
1248
1254

EPA SAMPLE NO.











LAB SAMPLE ID










-
DATE









';
'
TIME







- '• !">
Vt


STD. CONC.









!>*'

AROCLOR
Aroclor- 1016




Aroclor- 12 60

"


decachlorobiphenyl
toxaphene
?i
Aroclor-1221 •''••


Aroclor-1232

„•: "?l
Aroclor- 1242 £, ••> '"'•* •> .;*•

•? : ;*- ,
Aroclor- I2*jpu- H-
01 ^«"s

'!-s'';5 _.
'•' *j; ,_ x
Aroclor- 1254
...



\ 	 ^ — . 	 __
PEAK
1
2
3
4
5
1
2
3
4
5
1
1
4
1
2
3 -
; 1
3>'-"4
4 t;
1
iK"2
|f
^.-.'
'S.

s'i',,4
i:-r 5
1
2
3
4
5

CF LOW:>




,
•'.' ,; '•',-;••' '-
• ; s, ' -' si
•-

" ,


,-'

,',-- i
~j- ,;
-------
                       AROCLORS INITIAL CALIBRATION SHEET
Lab Name:
Lab Code:
SAS No.:
Case No.:
       Contract:
Batch No.:
Instrument ID:
Sequence No.
COMPOUND
Aroclor- 1016




Aroclor -12 60



toxaphene



Aroclor- 1221

, *• • " '
Aroclor- 1232 ;-
-A

Aroclor- 1242
,;,;-
#s :
Aroclor- 1918
. '-., r 4:' *'-<
'•' ;:
'
Aroclor- 1254 !, >
' -':'< • ! " • " . „
"";- '' !-- ' „• . ; J "'
<"' ' ' * V $
/ "* %-
PEAK
1
2
3
4
5
1
2 •"•;
3
5
1' :
2 :;
3
4
1
2
; -3 f
•'•'1-: "•;"
2 ,,;
4; ~,
f''
'-3 -.
5 '! !«
1
-,.?...
"" 4
5
1
2
3
4
5
RT
LOW








-,-''






















RRT
LOW































                                                M
                                     H
                         MEAN
         Retention Time ,-
                               FORM QTVB - PCS
                                                 5/92

-------
                        AROCLORS CALIBRATION CHECK SHEET
Lab Name:
Lab Code:           Case No.:
SAS No.:
Instrument ID:
EPA Sample No.:
Lab Sample ID:
Standard Concentration:
       Contract:
Batch No.:
Sequence No.
       Date Analyzed:   /  /
       Time Analyzed:   :
COMPOUND
Aroclor-1016



Aroclor-1260




decachlorobiphenyl

PEAK
1
2
3
4
5
1
2
3
4
5
1

INITIAL CF









<- i^..
' ^ '*•• ^ \ ' '• " >
MID



';
\ \



•'"''.


. -%D
'•v; ..










RESOL.
%VALLEY











                           SYSTEM MONltDR COM3&ODND
System Monitor Compound
(QC Limits)
decachlorobiphenyl •• ~' " " <\ „
* Value outside;^of QC limj
SMC r
AREA {'
A
RT
•I;
1C RT

RT %D
(+/- 1%)

t&t.
                                FORM QV - PCB
                               12/92

-------
                      AROCLORS ANALYTICAL SEQUENCE SUMMARY
Lab Name:
Lab Code:           Case No.:
SAS No. :
Instrument ID:
Initial Calibration Date:   /  /
Contract:
  Batch No.:
Sequence No.:
Analytical Sequence Start Date:   /  /
Analytical Sequence Start Time:   :
Analytical Sequence Stop Date:   /  /
Analytical Sequence Stop Time:   :
1
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
|22
|23
24
25
26
27
28
29
30
31:
O SJ J
J34
35
36
37
38
39
40


EPA
SAMPLE NO.
_ _ _



















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                                FORM QVI - PCB
                                5/92

-------
                           AROCLORS NARRATIVE
Lab Name:                               Contract:
Lab Code:           Case No.:           Batch No.
SAS No.:
                             FORM QVII -  PCB                       5/92

-------
                                                  DRAFT
          "SECTION V
  ON-LINE DATA TUSJISpll  SYSTEM
AND CONTRACTOR A0P JffiQUIREMENTS
              B-49
                                               08/23/94

-------
                                                                          DRAFT

         LABORATORY QTM SOFTWARE AND ELECTRONIC DATA RESPONSIBILITIES

1     QTM Process Overview

      QTM involves the delivery of analytical results to the site 48 hours
      after the laboratory receives the samples.   In^coriier to achieve this
      goal, traditional field analysis methods were revised, and linked to
      software products to speed up the analysis,  quality assurance,  data
      transmission, and reporting processes.                     ' •'••  ,
      The laboratory is responsible for assemling  the  data package,
      that the data meets minimum quality assurance standards ,  and delivering
      the data to the EPA mainframe for distribution  to £he designated user
      community.  The laboratory process *i presented as ^a  flow chart in Figure
      1, is described as follows.  The labossMt^ry reports the required
      analytical results into the QTM laboratory, ^software.   After data has
      been loaded into the system, either through .cbftta  entry or importing an
      exhibit H format file, it must be processed thrmigh the Contract
      Compliance Screeening (CCS) software. The  first :p".afefc . of CCS assesses the
      data for structural defects* .These defects must  be corrected before the
      remaining quality assurane!fe^cKe«1feis «fflavp£oceed.   Once the laboratory has
      corrected all the structural -'defects , "•^a^'^t^^i^ xesubmitted through
      CCS again.  Once CCS is completed, the laboratory -ssrill receive a CCS
      defect report.  The laboratory n*ist corfrect all correctable CCS defects
      reported.   The CCS defect identification and  correction process
      continues until no correctable defect /statements  appear.   Once the data
      passes through CCS, the results are submitted to  the mainframe.
                              S5!            ^  •
      QTM data recipients (Regions, EMSL-LV, Headquarters,  and the CLASS
      contractor) will! use a QTM. ijftegional so£%«are  product to receive the
      results and generate report^,  For QTM purposes,  the EPA mainframe is
      analogous ta',a-post off ice j4,:,QJM,us,ers^ will dial  the mainframe and
      download data Ifasikages of,ii&eiibsir/3Siince the  user is dialing the
      mainframe, users'-'Catt retrieve information  from  any  location as long as
      they have access to ^.;^|pne line.  The impact of  this design is that now
      individuals at the site4i£a*i- obtain results within the 48  hour time
      period ,as nestll as the peopl,*! '--at the Regional  offices .  In addition to
      downllfcadfeg^data,,'! £fee QTM RegiQ&al software produces reports .   The
      analysis recipient-lMJl obtain not only the analytical data package, but
      ait£«mated data review-results generated by QTM  CADRE, CCS screening
      results, and other insinuation that may be helpful  to their decision
               Figure 2 summarizes the QTM  electronic data transfer process.
          •• ..
      As"'s&gsa^s the data package arrives on the mainframe,  the CLASS
      contrae^rprocessesrit^e data package through the  CLASS contractor's
      version olE XKS^ and £asapares it to the CCS results  received from  the
      laboratory (Hiiltfi^tiae CLASS contractor CCS version is  the same as the
      laboratory versiiola:):.  If differences are found, the CLASS contractor may
      contact the laboratory to assist in reconciling the information.

                                     E-50
                                                                       08/23/94

-------
                                                           DRAFT
 libontory ttsponsibilitj'
      Regirdinj  the
QTH Electronic Dili /isseibly
    ind Delivery Process
          Figure 1




           B-51
                                                       08/23/94

-------
              QTM  ELECTRONIC  DATA  TRANSFER

 1.  Simple Analys Is
               iiboriiorr A
               GC integrator
                            ciitrtttir-prtfiaig
                            lilirriei
 2. Data Formatting
                          PC
                                          Structural elite):
                                          PC  CCS
 3. Dili Transfer
                                                EPi Ittintuiu
 4.  Regional  Data  Re vie*
    and  VaIidation
                                       Rejlonil
                                   «T« CAD8E Dili
                                                                                    DRAFT
                                                                    QTM Reporting
                                                                       F«rns
                                                                      otmiu
                                                                   (Bictup of EOT
                                                                    Dellreriblec]
                                                                    Nut Ions I GTN  CADRE
EPA tegunil
    PC
•;-fi; iBd Users
                                                  Bejunil
                                                       PC
           Site Miniger
              PC
                                      Figure  2
                                       B-52
                                                                                08/23/94

-------
                                                                          DRAFT

2     General Responsibilities

      The Contractor will  support the QTM Software and, -Electronic Data in the
      following manner:

2 . 1   Personnel

      The Contractor will  provide personnel to support the automated portion
      of the analytical  service  described in this SOW.  Individuals will meet
      the minimum  qualifications described below.

2.2   Computer Hardware  and Software        :

      The Contractor will  provide compute?: Hardware anal software to support
      the automated portion of the analytical service Described in this SOW.
      The computer hardware and  software  will meet: .the minimum requirements
      described below.

2.3   Data Processing

      The Contractor will  provide 'datB^rixsessJ.ng support for the automated
      portion of the analytical  sl&vice deser.i^4 $n this SOW.   The area of
      data processing responsibilities includes, --'but is not limited to:
      hardware, software,  system security,  and#electronic data package
      assembly and delivery.  The data processing responsibilities will meet
      the minimum  requirements described
2.4   Electronic Data  Storage and Retrievals

      The Contractor :"«S.ll provid3b£ifiir»; ^

2.5   Documentation         ,"

      The Contractor -pill produce}"4ocumentation for all standard operating
      procedures' (SOPs.) ^sed in fulfilling  the automated portion of the
      analytical service '^Ses-cribed  in this  SOW.   The documentation
      resSfsonsibilities will&beet  the minimum requirements described below.

     ..-^teaffing and Equipment,;'':
                              ^5
                    are the -ifittiimum functional  requirements.
            •"  •-'';'.           ,!.'*' '
3.1   Personnel"'--  ,       .;'-

      The minimum fundtltmal  requirements necessary to  meet the terms and
      conditions  of this contract are  listed below and  described in IFB

                                     B-53
                                                                       08/23/94

-------
                                                                          DRAFT

      Attachment C.  The Contractor shall designate and utilize key personnel
      to perform these functions.  EPA reserves the right  to  review personnel
      qualifications and experience, and take contract Action as  appropriate.
      The minimal functional requirements are listed below and described in
      detail in Exhibit A:

      3.1.1 Systems Manager;

      3.1.2 Programmer Analyst; and
                                              v'
      3.1.3 Back-Up Programmer Analyst (recommended, see Exhibit  A, Section
            IV,  paragraph 1.2.4).          -,^

3.2   Equipment and Software

      The Contractor shall provide analytical'iaad computer equipment  and
      technical expertise for this contract.    fbe,' software  and  equipment
      necessary to meet the terms and conditions of t&is contract are listed
      below and described in IFB Attachment  C.  The ComtasacJtor shall  designate
      and utilize key personnel to use this  equipment to perform  the  functions
      of this SOW.  The minimal ^qaSarespests ^are listed below and described in
      detail in Exhibit A:       'f -   """•-••"&  .-;;„,|--'->   ^ ,_


      3.2.1 The Contractor shall have ist misiffium the following computer
            equipment hardware configuration^

                  IBM AT/PS2/1$0386-compatible personal computer  (PC);
                             , ;   *^\

                  64@Kmandom Access Memory  C8&&0 J

            •     i!§ .Megabytes od^Medic.^^  free space on  the hard disk;
                   s:- •  >,       ,;f it;^i?\SF;;F
            •     2 Megabytes of expanded memory; and

            •     a 9600 bauH Jtayes compatible modem which is compatible with
             ,„;,»-- :gjbli»-.EPA TelecdB^teaaications Network.
                above specifications are minimum requirements  for operating
            the QTM softwa^;  It is recommended that  the  Contractor use
            higher end equifpent to decrease the QTM software  processing time.
            The anticipated -Ipipact of operating on enhanced configurations is
            described in further detail in paragraph 7 - Optimizing the QTM
      3.2.2 The!ilawtractors,*hall have at minimum  the  following computer
            software', -
                  QTM Laboratory Software, to be provided by EPA;

                                     B-54
                                                                       08/23/94

-------
                                                                           DRAFT

                   Base SAS Software*;

             •      DOS  Version 3.X or 5.X or higher; and
                   Note:  Running the QTM Software under DOS 4.X  is not
                   recommended.

             •      PC Anywhere*.

                   * These software packages are available at lo'cal^retail
                   software outlets .                                "

             Refer  to the QTM Laboratory SofCware Users Manual for more
             specific installation requirements.  The abosre specifications are
             minimum requirements for operating the QXfcE jsof tware .  It  is
             recommended that the Contractor use any additional  software
             products that would assist in the 'fulfiUaient of the terms of this
             contract.   The Contractor may purchase; commercial products,
             develop products in-house or commission a -vendor to develop
             software products to assist in the mission *bj? the contract.

      3.2.3  To receive improved perfairpance af , .the QTM Software, it is
             recommended that the ^sotracto'f paqpcfaase ;4isk caching software.
             The  anticipated impact 0$ operating" on eiihanced configurations is
             described  in further detail in paragraph 7 - Optimizing the QTM
             Software.                  -•'     " '

4     Data Processing                      ; .;

      The Contractor is .^responsible for the fallowing:

4.1   Hardware     v'f'           '. p

      4.1.1  Installi-^g,~?maintaiaai^:i ?iip4attSTiS, operating, and managing the
             computer equipment  and troubleshooting the hardware and software.
      4.1.2 Providing  first 'ligse ,;support for any problems encountered.
                 ,':' "'             wY.
      4. 1.3; liiletitifyiTsg>, -Bracking a^cT^orrecting any problems encountered.   In
         -»>;the  event  o£'-%ti%&a. transfer system failure, the Contractor shall
        ,cy!  send a. hardcopy-;i»f the sample and QC data summary (Form QI  - QVII)
      ..?    to the Region-RS|fC and to the Region- client by overnight delivery.
      ,]•'-'    The  Contractor sfjimil also send a diskette of the sample and QC
     "  :°.*.o  summary data, infSPA- approved format, to the CLASS contractor by
        '!L' ' -ifipernight  deliveiy.   The Contractor shall immediately contact the
            'G3^|S, contracto3r,.?and the Regional client or RSCC if the data
            tratisfer, systg»'';or the data formatting and forms generating
            so f twar« , iiiiis -;
                       :f~
      4.1.4 Ensuring that the hardware systems are configured to be compatible
            with the QTM software  system.
                                      B-55
                                                                        08/23/94

-------
                                                                          DRAFT

      4.1.5  Identifying areas of process or product improvement and providing
             suggestions to EPA.

      4.1.6  Ensuring that the systems are operational,,:at all times.
                                                      I -
4.2   Software

      4.2.1  Installing,  maintaining,  updating, operating, and .managing the
             computer systems .

      4.2.2  Providing first line support for iny problems encountered.1

      4.2.3  Assisting in tracking and correcting any problems encountered
             (refer  to Exhibits A and B foar.ffiore detailed information).
                                              \'      """
      4.2.4  Identifying areas of process or p*roidttct 'improvement and providing
             suggestions to EPA.

      4.2.5  Ensuring that the system software is configured to be compatible
             with  the QTM software system.
                                 ->r, " s- :.-'  '• ~
      4.2.6  Ensuring that the systems are opesa&toaal ,:at; all times.

4.3   System Security                        ;.'

      4.3.1  Ensuring that only authorized personnel have access to systems.

      4.3.2  Initiating ;aad maintaining EPA aainf rame identifications according
             to EPA  Tei^itaimmunicliiions Security Procedures.
                    ,
4.4   Electronic Data Package Assembly and Delivery Process

      4.4.1 Preparfi^?M^ectronj^HJii3fe4«?to8|ge in accordance with
            specif icatieas;, in Exhibit H and B.
            Note:   The QTK Software data entry module can be used but is not
            required         • ,,;•%:,
      4.4.2 JEr©cesslBg)4&«ctronic 'idfeaisa package using the QTM Software.

      4,i|Sy3 Correcting anyelftdentified defects resulting from the QTM Software
      I.,'*'*'   evaluation.     ',§..
      ",'•"•                    ;-,-••
      *ff>$jf£r Providing qualit^f.aassurance/control (QA/QC) measures prior to
         ^ff, "^Submitting the ^ectronic data package through the QTM Software
           '
            4.4.4.1    j$H&& electronic data package must match the hardcopy
                        :'data package.

            4.4.4.2     The electronic data package must meet all requirements
                         specified in the SOW.
                                      B-56
                                                                       08/23/94

-------
                                                                          DRAFT

      4.4.5 Submitting  the QA'd  electronic  data package which has been
            processed through  the QTM  Software to  the  EPA mainframe within the
            required time period (see  Exhibits A & B) .

      4.4.6 Ensuring that the  processes  are operational at all times.

5     Data Storage and  Retrieval                 <• •        : '

      The Contractor is responsible  for  storing backups of all Electronic
      deliverables.  The Contractor  will develop a procedure for t'raeking
      historical information which occurred Coring the  assembly,  processing,
      and transfer procedures  of each  electronic deliverable .  A procedure
      will be developed for archiving, retrieving  and  reproducing each
      deliverable upon  request.  Refer to ^Exhibits B and F for more detailed
      information.                        -  =        ,"  •

5.1   Storing the electronic data package as the ioff tcial back-up and  for
      future reference  and/or  submission, if needed. 1   t,
                                                          '•• •
5.2   Retrieving any previous  electronic data packages  and^sttbmitting  them to
      EPA upon request.          !;  „ ;j;  " ' • ,--

6     Document Standard Operating Procedures
                                             • i
                                             ' *
      The Contractor shall submit updated copies of all required Standard
      Operating Procedures as  described "In jlixliibits E  and F.
                                         • '4
1     Optimizing the QTM
      This section provides suggestions for optimizing the QTM software
      operating environment .  Following these suggestions will help  to
      minimize the-- ,fc4me required; 1por,mdata upload, download, and processing.
7.1   Hardware
        ;-*i
            Using a faster computer processor such as an 80386 or  80486  with  a
                  jspeaad of 25-33"^jSz.. or higher will reduce processing time
                            The folfcoifcing compares the performance of the
                  80386, 'rmal the 80486 processors.
                                     B-57
                                                                      08/23/94

-------
                                                                   DRAFT

     Processor/Clock Speed Benchmarks

     Computer                PC -XT       386SX        486

     Running Time            32 min.     6.5 min.     4  min.
     Bios                    IBM         AWARD  I  -,    AMI
     Processor (Intel)       8088        8G3S6SX  < f   e,0486
     Clock Speed             5.7 Mhz     16 Mhz       3S Mhz
     Math Coprocessor        None        Present      Prese&t
     RAM                     640        : 640          640  '*,'
     Expanded Memory         0       '.=   1316K        3832K   '•
     Monitor                 Mono   ,  .   VGA          VGA
     DOS Version             3.3   ,!     5.0    j!      5.0
     Hard Disk               32 Meg:,     80 Me^g;      106  Meg

     Note:   These benchmarks were obtained, by ^performing  the "submit
     results" option in version 0,14 of the QTM laboratory software.

     Increasing the EXTENDED or EXPANDED RAM memory .will  allow the use
     of disk caching software which reduces the time :it takes to read
     data from the hard di«ftc»7, ;1Me following compares running the QTM
     software with differetifc size
                             .
     Disk Caching Benchmarks  •        :

     Amount of Disk Cached         processing Time

             OK   -, '  T  .           :9:35 min.
            720K       Y:          5:4-5 min.
                         :A        5:00aain.
     Note: .ji^Lese benchmarks .were,, obtained by running the
     Criteri'i^DJMtlier r^s^t^. ^f&ion 0.14 of the  QTM Regional
     software.  -"3!h« computer equipment used was a  386X,  operating at 16
     Mhz, with 102&X -Attended memory.
                the QTM 1'sotrt«are on local hard disk  rather than using a
               ^h^ce the tinise|it: takes to read data,  making substantial
   f; ^difference InlNgfae processing time.
?,'• '                 "" \
'?•    Using high speec|;3Biodems or communications networks with dedicated
;     data lines will Decrease downloading time by  at least 10-15
;,',::; ;  minutes depending :jon the file size, see below.
                              B-58
                                                                08/23/94

-------
                                                                          DRAFT

            Transmission of Speed Benchmarks

            Transmission Speed            Transmission Time

            56 K dedicated line                 2:40 mln.
            2400 Baud                           20:08 Bin.
            1200 Baud                           21:40 min.

            Note:  These benchmarks were obtained by running the Deceive
            option in version 0.14 of the QTM,Regional software.  !t3se  computer
            equipment used was a 386SX, operating at 16 Mhz, with 1024K::
            extended memory.  The size of th£ file used in transmission was
            114802 bytes.                 ,  ^
7.2   Software
            Using DOS version 5.0 or higher, makes use of high memory,  leaving
            more conventional memory for the program.

            Installing a disk caching program to utilize extended or expanded
            memory will reduce the/aaoust: ••«£ ;time the computer spends reading
            data from the hard di'sfc..      v ••''•'  f     •;  _.,

            Performing regular maintenance on-tine hard disk using disk
            optimization utility software to,perform disk compression will
            remove deleted files, rewrite fragmented files, and reorganize
            your disk.  Optimizing your disk will reduce the time it takes  to
            read data from the hard disk.
                        " '    ^  •.; '• •.
                               i?r;
            Setting ug>;-the CONFI^jSYS file for loading DOS in the upper memory
            (DOS version 5.X only)i'-«ill free more space in conventional memory
            for usflby the progrfmfe ^ ...The.^cQnf ig. sys file should contain the
            f ollowing'l line:
                                     B-59
                                                                       08/23/94

-------
                                                         DRAFT
                   s,
                  EMIBIT C
    QTM TARGET COMPOUND LIST (QTCL) AND
CONTRACT REQUIRED QUANTII^iriON LIMITS  (CRQL)
                                                      08/23/94

-------
                                                                    DRAFT
                QTM Target Compound List (QTCL) and
           Contract Required Quantitation Limits  (CRQL)1


1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
21.

Volatiles
Bromofonn
Bromodichlorome thane
Benzene
Carbon Tetrachloride
Chlorobenzene
Chloroform
1 , 1-Dichloroethane
1 , 2 -Dichloroethane
1 , 1 -Dichloroethene
cis-1, 2-Dichloroethene
trans -1,2 -Dichloroethene
Ethylbenzene
1,1,2 , 2-Tetrachloroethane
Te trachloroethene
Toluene
1,1,1 -Trichloroethane
Trichloroethene , :
Vinyl Chloride / :, ;
ortho-Xylene ";
meta-Xylene „ , -
para-Xylene ,;";,'
IllnlSlm 	 	 1 	 -8,

Water
Quantitation
Soil/ Oil3
.Solid2
Limits
Oil4
Oil5
CAS Number H&/L PS/^S MS/kg A'gAg Mg/^
75-25-2
75-27-4
71-43-2
56-23-5
108-90-7
67-66-3
75-34-3
107-06-2
75-35-4
156-59-2
115SB41-4"
7&S4-5
127-18-4
108-88-3
71-55-6
79-01-6
,13-01-4
"lfe-47-6
1IN5-38-3
IBS -42;: 3,
• is k-
20
20
20
: 20
20
20
20
20
20
20
"••' ^v-20
,20
; 20
20
20
20
20
20
40
40
40
40
40
40
40
40
;4Q,
40
40
- 40:,'
40
40
40
40
40
40
40
40
400,
400
400
400
400
400
400
400
400
400
400
400
400
400
400
400
400
400
400
400
400
jvSOO
£;'8QO
sdov
800
800
800
800
800
800
800
800
800
800
800
800
800
800
800
800
800
800
400
400
400
400
400
400
400
400
400
400
400
400
400
400
400
400
400
400
400
400
400
Sppcffic quantitatio%:|p.imits  are  highly matrix dependent.   The
qjsgoititation limits limited herein are provided for guidance and may not
       be achievable, {i';
             limits  listed for  soil/solid are based on wet weight.
     "'••':?,.         4P
Quantitat4oas:i,limitS!=l:|isted are  for methanol non-miscible oil samples and
are based on"Optimaia1 sample size.

Quantitation limits  listed are  for methanol miscible/aqueous non-
miscible oil samples and are based on optimum sample size.

Quantitation limits  listed are  for methanol miscible/aqueous miscible
oil samples.   Based  on optimum  sample size.

                                C-2

-------
                                                                    DRAFT
                QTM Target Compound List (QTCL) and
           Contract Required Quantitation Limits  (CROP1
(Cont'd.
Polynuclear Aromatic CAS Number
)
Quantitation Limits
Water -Soil/Solid2
MS/L , MiAg
Oil3
A*gAg
Hydrocarbons (PAHs)
22.
23.
24.
25.
26.
27.
28.
29.
30.
31.
32.
33.
34.
35.
36.
37.
Acenaphthene
Acenaphthylene
Anthracene
Benz [a] Anthracene
Benzo [a] Pyrene
Benzo [b] Fluoranthene
Benzo [k] Fluoranthene
Benzo [g,h,i] Perylene
Chrysene
Dibenz [a,h] Anthracene
Fluo r anthene
Fluorene
Indeno [1,2,3-cd] Pyrene
Naphthalene
Phenanthrene
Pyrene
83-32-9
208-96-8
120-12-7
56-55-3
50-32-8
205-99-2 :
207-08-9
191-24-2
218-01-9
53-70-3
206-44-0
*B-13M? - :•
l?S-;S9-5 * ' '
91-Z9r3
85-01-8
129-00-0
20
20
20
20
20
'. 20
' '-20
'10:
20 :
20
20
,,50
•"£:» k
20 ;
29
20
330
330 ; r
330
330
330
; 330
3.30
330
330
330
330
330
. , 330
- -; 330
330
330
20,000
20,000
•-10,000
ii>,ooo
20,000
20,000
20,000
20,000
20,000
20,000
20,000
20,000
20,000
20,000
20,000
20,000
Specific 'ip^ia:itation;1dimits are highly matrix dependent.  The
quantitation ilai£^:;listed herein are provided for guidance and may not
always be achievli&lfe.

Quantitation limits listed for soil/solid are based on wet weight.
Quantitation limits listed for soil/solid are based on sample
preparation utilizing solvent extraction (see Exhibit -D Section IV).
Based on optimum sample size.
                                C-3

-------
                                                                    DRAFT
                QTM Target Compound List (QTCL) and
           Contract Required Quantisation Limits (CROP1

38.
39.
40.
41.
42.
43.
44.
45
46.
47.

48.
49.
50.
51.
52.
53. .
Phenols
2 - Chloropheno 1
4 - Chloro - 3 -Methylphenol
2 , 4-Dichlorophenol
2 ,4-Dimethylphenol
4 , 6-Dinitro-2 -Methylphenol
2 , 4-Dinitrophenol
o-Cresol
m-Cresol
p-Cresol
2 -Nitrophenol

4-Nitrophenol T
Pentachlorophenol
Phenol
2,3,4, 6 -Tetrachlorophenol
2,4, 5 -Trichlorophenol
2,4, 6 -Trichlorophenol
(Cont'd.)
Quantitation Limits
Water :, Soil/Solid2 Oil3
CAS Number P&ftj ' • * MgAg fgAg
95-57-8
59-50-7
120-83-2
105-67-9
534-52-1 ,
51-28-5'
95-48-7
108-39-4
106-44-5
88-75-5
f
°10Q-i02-||,>
''-*87-£6-5::-'-'
l£&-95-2
58-90-2
95-85-4 ,
88-Q6T2; ;
50
,. 50
: 50
50
50
,'", 50 IV
-'"'"•', 50'-
'••'-50'
50 :'!r,
50 '"-',

50
" '-• 50' ;
V 50n -.
50
50
50
V«*r,
830 '4 ,
830 ;
830
830
830
830
830
830
, 830
k
830
830
830
830
830
830
830
830
-. 830
830
830
830
830
830
830
830

830
830
830
830
830
830
Specific fi%[«^itati<||t-siimits are highly matrix dependent.  The
quantitation:-i|pi,t£ flisted herein are provided for guidance and may not
always be achievable.

Quantitation limits listed for soil/solid are based on wet weight.
Quantitation limits listed for soil/solid are based on sample
preparation utilizing solvent extraction (see Exhibit D Section IV).
Based on optimum.sample size.
                                C-4

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                                                                    DRAFT
                QTM Target  Compound List  (QTCL)  and
           Contract Required Quantitation Limits CCRQL)1
(Cont'd.)
Quantitation Limits


54.
55.
56.
57.
58.
59.
60.
61.
62.
63.
64.
65.
66.
67.
68.
69.
70.
71.
72.
73.

Pesticides
Aldrin
alpha -BHC
beta-BHC
alpha- Chlordane
gamma- Chlordane
delta-BHC
Dieldrin
4, 4' -ODD
4, 4' -DDE
4, 4 '-DDT
Endosulfan Sulfate
Endosulfan I
Endosulfan II
Endrin
Endrin Ketone
Endrin Aldehyde
gamma -BHC (LindaneJ
Heptachlor
Heptachlor Epoxlde
Methoxychlor '"

CAS Number
309-00-2
319-84-6
319-85-7
5103-71-9
5103-74-2
319-86-8
60-57-1
72-54-8
72-55-9
50-29-3
103li?^ '
959-118-8
33213-65^
72-20-8 -
53494-70-5 :?
7421-93-4
:, ,': 58-89-9
' 7'6'?*44-8
1024^:57-3
72 -i3- 5
Water , -
MgA
0.1
0.1
•fiLl
0.1
: o.i
D»l
Ovl
0.1
0.1
0.1
i; .«.!
'L ^JcSL '• '
OJ1 '•
cfci
y tf: 1
0.1
0.1
- 0^1
^,1
0.1
Soil/Solid2
;#BAg
1.7 ';:
1.7 :
1.7
1.7
1.7
1.7
1.7
1.7
1.7
= 1;7
1.7'
, .1.7
, 1.7
1.7
1.7
1.7
1.7
1.7
1.7
1.7
Oil3
MgAg
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
100
Specific 'q^Kititati«a,limits are highly matrix  dependent.   The
quantitation ^IliBa^ts*8.1sted herein are provided  for guidance and may not
always be achievable.
Quantitation limits listed for soil/solid are based on wet weight.
Quantitation limits listed for soil/solid are based on sample
preparation utilizing solvent extraction (see Exhibit D  Section  IV)
Based on optimum sample size.
                                C-5

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                                                                         DRAFT
                      QTM Target Compound List (QTCL)  and
                 Contract Required Quantitation Limits (CROP1
                                   (Cont'd.)
      PCBs/Aroclors
CAS Number
                                                      Quantitation Limits
                                                           Soil/Solid2   Oil3
74.   Aroclor-1016
75.   Aroclor-1221
76.   Aroclor-1232
77.   Aroclor-1242
78.   Aroclor-1248

79.   Aroclor-1254
80.   Aroclor-1260
81.   Toxaphene
12674-11-2
11104-28-2
11141-16-5
53469-21-9
12672-29-6

11097-69-1
11096-82-5
 8001-35-2
1
2
1
1
1

1
1
'5
XT'.
33
17
17
17

17
17
83
1000
2000
1000
1000
1000

1000
1000
5000
                                   are highly matrix dependent.  The
                                 herein are provided for guidance and may not
      Quantitation limits listed for soil/solid are based on wet weight.
      Quantitation limits listed for soil/solid are based on sample
      preparation utilizing solvent extraction (see Exhibit D Section IV) .
      Based on optimum sample size.
                                      C-6

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                                                                         DRAFT
           General Guidance  for  Calculating  CRQLs  for Other Matrices
      In general, the CRQLs for other matrices for each fraction not specified
in Exhibit B  (e.g. , tissue, wipes,  etc.) may be calculated by multiplying the low
concentration standard concentration by  the  final  extract volume and dividing
this result with  the  amount  of sample extracted or for  wipe samples the area
sampled.
              calibxatj.cn standard (pg/ml) x final simple ext&act volume (ml)
           amount of sample extracted or area or volume sampled i±Et If/kg/area)
                                     C-7

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                                                                          DRAFT
                               TABLE OF CONTENTS
ANALYTICAL METHOD FOR VOLATILES

SECTION I   Introduction                              " •,
SECTION II  Sample Storage and Turnaround Times  and Equipment and Standards
SECTION III Instrument Quality Control  Procedures  and Requirements
SECTION IV  Sample Analysis and Compound Identification and QuatitSitation
SECTION V   Sample Quality Control Procedures jatd  Requirements    -";  •

ANALYTICAL METHOD FOR POLYNUCLEAR AROMATIC HYDROCARBONS (PAHs)
                                            •A
SECTION I   Introduction                 ,            ,,r
SECTION II  Sample/Extract Storage and  Turnaround  Times and Equipment and
            Standards
SECTION III Instrument Quality Control  Procedures-and Requirements
SECTION IV  Sample Analysis and Compound Identificatilon,.and Quantitation
SECTION V   Sample Quality Control Procedures and  Requirements

ANALYTICAL METHOD FOR PHENOLS   ,'-  i  "-;   ;;.
SECTION I   Introduction            ,,           •       :
SECTION II  Sample/Extract Storage  an4-Turnar*°  ~   "'••-,           : ^ ',
ANALYTICAL METHOD FOR
                                       Turnaround Times  and Equipment and
SECTION I   Introduction
SECTION II  Sample/Extassct
            Standards""--  ;
SECTION III Instrument  QuaXfey, Control Procedures  and Requirements
SECTION IV  Sample Analysis and Compound Identification and Quantitation
SECTION V   Saaple;:Qaality Control procedures  and  Requirements

ANALYTICAL:«ETHOD FOR FCBJS US  AROCLORS
        = -•;                ' .( ,,_,
SECTION-!'   Introduction    fy
SECTIofc;!!!  Sample/Extract Storage and Turnaround  Times and Equipment and
     H' ^4   Standards       |/
SECTION TiSCiJiistrument  Qualify Control Procedures  and Requirements
SECTION IV "!'S^i(ip3se Analysis.fi&id Compound Identification and Quantitation
SECTION V   Samples Quality^ Control Procedures  and  Requirements
APPENDICES

Appendix A
Appendix B
Appendix C
            Dry Weight Calculations
            General Guidance  for Unusual  or High Concentration Samples
            Modified Solid  Phase Extraction Procedures  for Pesticides and PCBs

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                                               DRAFT
        EXHIBIT D  :




QUICK TURNAROTH) JETHODS




    METHOD FOR WATILES (VOAs)
       D-1-VOA-Q                           08/23/94

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                                                                           DRAFT

                               TABLE OF CONTENTS
                                   VOIATILES

SECTION                                                                    Page

I     Introduction ....................................... . ................. D-3

II    Sample  Storage  and Turnaround Times                    ; .
      and Equipment and Standards .............................. i „„,.. ....... D-4

      1     Sample Storage  and Turnaround Tii»fes ..................... '. . .u .D-4
      2     Summary of  Method .............. , .« ......................... . . .D-4
      3     Interferences .................. i .......... .:. .................. D-5
      4     Apparatus and Materials ....... » .......... ; ; ................... D- 6
      5     Reagents ....................... ; ,;f ...... _, ..................... D-7
      6     Standards ........................ :,»...,; ..................... D-8

III   Instrument Quality Control Procedures  and Requirements .............. D-12

      7     Instrument  Operating Conditions .............. '.' ... ............. D-12
      8     Calibration of  the G£ jSjr&Ssearr Initial Calibration ............ D-14
      9     Calibration of  the GC Astern - ciil^ration Check .............. D-19
      10    Calibration of  the GC Sy&tem - PVS;; ^ . ; . ; . A .' ................. D-22
      11    System Performance - GC Resolutioati ........................... D-25

IV    Sample  Analysis and Compound  Identification and Quantitation ........ D-28

      12    Summary ____ .,, «^ .V?- 1 ........... * .............................. D'28
      13    Procedure. *£...'. r?.-|U ......... '.*«. ............................ D-28
      14    Instrumental Analysit.;, .......... u ........................... D- 31
      15    Dilutions ........... -v. ....................................... D-33
      16    Identification  of Taj£gifet, Compounds ............................ D-35
      17    Calculatioas, ....... li^V^y* i>~|:. ............................. D-36
      18    Technical fticc«s3»tance Criteria ................................. D-38
      19    Corrective  Acticmi ............................................ D-39
      20    Documentation. . . M» j,» . ........................................ D-40

V     Sanipl«;iquality;>"©^itr>ol  Proce'du^s and Requirements .................. D-41
             '         ' '
            ' Method Blank A^rsis ......................................... D-41
            Instrument Blank|*nalysis ..................................... D-44
            Laboratory Contr%, Samples .................................... D-47
                                   D-2-VOA-Q                           08/23/94

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                                                                    DRAFT
                             SECTION I

                            INTRODUCTION
This Quick Turnaround Method (QTM)  is designed for -use.in determining
the concentration  of various volatile (VOA)  organic coapoiinds in water,
soil/solid, and oil samples.   Exhibit C lists the compounds,that will be
determined by this method  along with the, .Contract Required Qtiantitation
Limits  (CRQLs).  The method yields  identification and quant itatixm of
the analytes listed in  Exhibit C using-a'a" single column, gas
chromatographic/dual detector (photo-iOnization ajiid electrolytic
conductivity) method (GC/PID,  ELCD),,  'Target comjseund concentrations in
samples are reported on an "as-received* basis^'-tk> dry weights are
calculated.  The primary objective  of tMs QTKlis to provide analytical
data in a timely manner for decision-making>«teing site inspections,
remediations, and  emergency removal activities.•& 13ae VOA QTM is to be
used when rapid data turnaround is  required,  when'itlje- data requestor
knows of (or strongly suspect^) .the presence of volatile contamination,
and there is knowledge  regarding potential matrix interferences at the
site.  The QTM is  not equivalent to, "ins»r-*3a-asep'3;ac«Jnent for, the CLP
Organics Multi-Media Multi-CoTjiisentrationiuialy'sisv.t;
                             D-3-VOA-Q                           08/23/94

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                                                                          DRAFT

                                   SECTION II

                      SAMPLE STORAGE AND TURNAROUND TIMES
                                      AND
                            EQUIPMENT AND STANDARDS


1     Sample Storage and Turnaround Times                    ,

1.1   Procedures for Sample Storage           ,                        ;

      Samples shall be protected from light,,,and refrigerated at 4°C (±  2°C)
      from the time of receipt until 60  days  after  delivery of a complete data
      package to the Agency.                           . ;

      Samples and standards must be stored separately.

1.2   Contract Required Sample Turnaround Times

      Samples shall be analyzed and.a summary of the  analytical and QC  data
      shall be reported to the ajipjro^cla^'EEA  Region via  telecommunications
      network within 48 hours (orlj£2 hdurk'-ft^Boj^  than three fractions are
      analyzed) of Validated Time  o£^Sample Re6eipt:fV3SR).   See Exhibits A
      and B for specific instructions',. concerning sample turnaround time and
      data reporting requirements.    ,      :

2     Summary of Method

2.1   This analytical method'"isy-A  heated headspace  method  for the analysis of
      volatile organises in water'^-'soil/solid,'-said oil samples.   All samples
      shall be analyzed utilizing-pt heated headspace  apparatus and gas
      chromatography ,(GC) with dniPL.. detectors.   All analyses shall be
      performed witfhfnsa contra4fe^P^^fiedAnalytical sequence that shall not
      exceed 24 hours.    ;,
2.2   Target compounds are i&epfeified and quantitated on the  basis  of
      retenticaivtioe ^windows arid ,ii€Libration factors  established during
      initi^lCjaallTsfaCioaav  During^t&Etial calibration,  a mean relative
      reteitWon time (RRlK|'|v.a mean retention time  (RT),  and an identification
             (± 0.005 RRT iteit of the mean RRT  or  ± 1.0  percent of  the mean
          are established fopt^-each compound.  Mean calibration factors are
        so established duringjtinitial calibration  and the percent relative
            rd deviation (%R^() of the calibration factors  for each target
               and the SysteaifMonitor Compound  (SMC)  must be  less than or
      equal H3of525.0 percenjCfli Sample compound concentrations  are calculated
      from the^Saaifcial caliltration using  the average  of  the three calibration
      factors, usit^!:*^e;fliitd point calibration  factor (if it  is within ± 10
      percent of the jcsreirsge of the high  and low calibration  factors) ,  or
      using line segments (K Curve).


                                   D-4-VOA-Q                           08/23/94

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                                                                          DRAFT

2.3   A check  of  the  initial  calibration shall be performed no less than every
      24 hours by the analysis of the mid point standard.  All calibration
      factors  calculated from this calibration check standard must be within
      ± 35.0 percent  of the mean calibration factor calculated from the
      initial  calibration for each target compound ari>»rill be a "go/no-go analysis".
      That is, if the LCS meets performance'criteria as_j stated in paragraph
      23, sample  analyses may proceed.   l£,,-; however,  f&e LCS does not meet
      acceptance  criteria, corrective actien,i»ist be;ftkken before sample
      analyses are performed.   The PVS is tw6'"-t^sies :iptie concentration of the
      low calibration standard and shall be analyzed, at least once during each
      analytical  sequence to  verify instrument perf &XHaijce.   All samples shall
      be bracketed by valid PVS analyses or a valid initial calibration or a
      valid calibration check standard and a valid PVS.     S

2.5   A System Monitor Compound ($$|0 shall%e';|k4 a retention time marker to
      calculate RRTs  for the  identification of ^target compounds and to assess
      the effectiveness of the heated ^ieadspace sampler.  When the recovery of
      the SMC  in  a field sample is less :t&ain;10 percent, greater than 200
      percent, or peak interferences are'fizssent,  absolute retention times are
      used for target conipoandJidentificatioB,.   The SMC recovery criterion of
      50-150 percent  is~advisd*y-i^nly.   Rean4tysis of samples are not
      performed if tbjefilSMC recov^y is  outside ifehe advisory recovery limits.

3     Interferences'              ,:V
         """ "      	"             "\A "	
3.1   The analytical sysjfcem must be  demonstrated to be free from contamination
      under conditions of th»analysis by analyzing method blanks.   The use of
      non-Teflon plastic tubliig^iion-Teflon thread sealants,  or flow
      controllers =l»xtihi rubber ccmrpaiients  should be avoided.
            .-r '-'' '-'-H.  L't          -HP
3.2   Samples can be cohTjAinated by diffusion of volatile organics through
      theysS'epturn seal duringh-shipment and storage.  A field blank prepared by
            samplers from reagent water and carried through the sampling and
               protocol as billnds or labeled as blanks can serve as a check on
          -.contamination.   ~ -j •
3.3   GC intferleE-ences by s^p>le carryover may be minimized by using
      disposable^giassware;.ffturing sample preparation and employing the maximum
      possible rinse sCyc3Je:!for the automatic  injection system.
                                   D-5-VOA-Q                           08/23/94

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                                                                          DRAFT

3.4   Cross -contamination problems  are minimized by analyzing instrument
      blanks after samples with high  levels  of target compounds or other
      interferents (see paragraph 22) .

3.5   Dehydrochlorination of Tetrachloroethene to Triehloroethene may occur
      because of contamination or active  sites in the feeadspace sample flow
      lines.  If the Laboratory suspects  this is oecuring.,,! it shall be noted
      in the Batch Narrative .                                ,,

4     Apparatus and Materials                  ,                    7"

      Brand names, suppliers, and part numbeirs are for illustrative purposes
      only.  No endorsement is implied.   Eqativalent performance may be
      achieved using apparatus and materials other thai£ "those specified here;
      however, demonstration of equivalent i$>«rforaane«:Tneeting the
      requirements of this SOW is the responsibility la^ ali :^ePessary accessories and detector
      systems designed or modifie^ijKo acceptta^pitlary. analytical columns.
      The GC system shall be capabM of temperJitaure programming and flow
      control that is stable throughout an analytical sequence.   All GC
      carrier gas lines shall be constsbocted^itom stainless steel or copper
      tubing.  Non-polytetrafluoroethyleae fPTFE)  thread sealants, or flow
      controllers with rubber components  shall not be used.
                           ' <*•*»             ;'-

      4.1.1 Gas Chromat^graphf-^lumn - 30 aba: 0.53 mm ID bonded phase
            silicone§&&ated fuse%iailica  capillary column (J&W DB-624,  or
            equivalent).  A filmjtitickness of 3.0 jim is recommended.
                  ; > "           A ,: '
            NOTE:  The xise of a^gttkfdrcol^an^ is recommended.
      4.1.2 Chromatography^Bet^ectors  - The GC  shall  be  equipped with a
            photoionization "Sefasetor  (PID) and an electrolytic conductivity
            detector -,-?(ELCD ) in
                  4.1.2!-^,-  Detector 1  -  PID with 10.2  ev lamp.
                          "f-^i.
                  4.1.2.2   -^"Detector 2  -  ELCD.
                            ?'',&.
                  4.1.2.3    JfThe two detectors operated  in series may be
                            ,|; rinterfaced  by a short length of uncoated fused
                          ,Jf silica capillary column.
                  5  .      ,":i':
                  j ^,^-    •"• *>"
                       ff^ ','   Gas Supply  -  The carrier  gas must be ultrapure
                       *S v    helium.
                                   D-6-VOA-Q                           08/23/94

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                                                                           DRAFT

4.2    Automated Headspace Sampler  - Hewlett-Packard Model 19395A,  or
       equivalent .

4.3    Vials for Headspace Sampler  - Headspace vials,  5/yaL,  with Teflon-faced
       septa,  (or equivalent 5-mL vials).  Note:  Larger sheadspace vials may be
       used if equivalence in terms of meeting the  CSSJLik'equirements can be
       demonstrated.

4.4    Data System - The GC shall be linked  to a  data system capable of
       integrating peak areas for any compound detected at or above ,wne-half
       the  CRQL,  providing retention time labeling,  and relative retention time
       comparison.   It is required  that the  lialjoratory be equipped with a PC-
       or microcomputer-based GC data collection  and reduction system for this
       purpose.   The Laboratory shall possess, this  equipment to provide the
       quick turnaround of electronic data.  ;lfee  Laboratory shall also be
       equipped with a microcomputer and contfacS-ispeJesified hardware and
       software  to  electronically transfer the QTM;dsta to the Regions.

4.5    Glassware -   Sufficient glassware to  meet  contract: requirements shall be
       reserved for exclusive use in^support of this contract,
      4.5.1  Disposable Pipets -

      4.5.2  Autosampler Vials - appropriate fVnp the GC  system.
                                        -„     ,\-;.
      4.5.3  Volumetric Pipets/Repipets '- jD.-Sr-', 1.0-,  5.0-,  10-,  and 25-mL.

      4.5.4  Volumetric Flasks- '- ,10-, 25-, 50^, and 100-mL.

      4.5.5  Teflon-lineH screw c'ag amber bottles.
                     •-'             A             -
                                  v:.-
4.6   Laboratory Hi
      *' * •*                     ^-'-.
     ' -4j|6 f5..  Vortex  Mixer.   ^{
        "'**','*.'?'"*                  ,**r
          ''- ' J •              Ys
5     Reagerit^f>., .         f; I',
                 *' ,  ,       i]
5.1   Reagent wate^-.-Reajgient water is defined as water in which target
      compounds  or  potentially interfering compounds  do not produce  a  signal
      greater than  one half the the response in the corresponding RRT  window


                                   D-7-VOA-Q                            08/23/94

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                                                                          DRAFT

      of the initial calibration  low concentration standard.  Reagent water
      shall be generated by one of  the  following methods.

      5.1.1 Reagent water may be  generated by passing ;!tap water through a.
            carbon filter bed containing approximately. 500 g of activated
            carbon (Calgon Corp., Filtrasorb-300, or ^e^urwalent).

      5.1.2 Reagent water may be  generated using a water purification system
            (Millipore-0-Plus with  Organex Q cartridges, or eqtil*KaJL«nt).

      5.1.3 Reagent water may be  further prepared by boiling for 15 min&tes,
            then bubbling contaminant-free iaett gas through the water for one
            hour while maintaining  the  watear"temperature>a.t 90°C.  While still
            hot, transfer the degassed  water to a narr&v mouth screw-cap
            bottle, seal with a Teflon-lirieiS-i^eptum a^S cap.

5.2   Solvents - Purge and trap grade methanol, 03^equivalent.

5.3   Corn oil.                                         "

6     Standards                  ',  •«;§?, -\,  :-- ,,,

6.1   Stock Standard Solutions      I,          ,       •

      Stock solutions may be prepared fprom ptir-e standard materials as
      described below or purchased  as ctertiftSSed solutions (also see Exhibit E,
      Section V for preparing and verifyingv:the integrity of the stock
      standard solutions.),^  ;'*>•,,.            •<'"

      6.1.1 Place about 9.8 mL ofcaethanol in-* 10-mL tared ground-glass-
            stoppere,volum^^ith  methanol.  Immediately restopper the flask.
            When cbBg«>TBi^4;|purity  is assayed to be 96 percent or greater, the
            weight may'lj^e-'xised without  correction to calculate the
            concentration of the  stock  standard.
                                   D-8-VOA-Q                           08/23/94

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                                                                           DRAFT

      6.1.5 Mix  the  standard by inverting the flask three  times .

      6.1.6 Commercially prepared stock standards may be used  at  the
            concentration certified by the manufacturer or by  an  independent
            source.   The Laboratory shall maintain certificates of  analyses
            with its case files.                      .  •-. >

      6.1.7 Transfer the stock standard solution into a Tefloifc-sealed screw-
            cap  bottle.   Store,  with minimal headspace, in freezer -and protect
            from light.                                                 :,

      6.1.8 Prepare  or acquire fresh standards no less than every six months.
            The  Laboratory shall replace at^adards whenever comparison with
            check standards indicate a problem.

6.2   Secondary  Dilution Standards           * ,

      6.2.1 Using stock standard solutions,  prepare secondary  dilution
            standards in methanol, containing the compot»Kls of interest.
      6.2.2 Secondary dilution s^f«4a.il^ isfesll ,be stored in a freezer  (-10°C
            to  -2OC)  with  minimal Iheadspace'-^asid etefcked frequently for  signs
            of  degradation  or  evaporation.   These protsfetlares are especially
            important just  prior to  jrioej>aring<%jalibration standards.   Each of
            the secondary dilution stawilards" sliall not be used any longer than
            one week  after  vial is opened, --/'Unused vials of the secondary
            standard  solutions may be  storiid in the freezer for up to  six
            months from ,ffe<& ,£|MB the origit%l stock standard solutions were
            prepared.^; \- "    ~"J-']-          ','•
                                 X --•
            NOTE:  ^Standards  shcmfcS not be stored in volumetric flasks,
            especially when theyfsajfe,, .pxejpared with solvents with low boiling
              „    ™   '         '}'•. i "•£•'*' 'j*# *-• & "f.~ "{''?' '^ ••{
            poxnts. -   , -.,      , £i;^,-;-;  J&il  A
                         tf
6.3   Calibration Standards;'; .,,,

      6.3.1 CaHfarateion standardsj'fimtial  and check) must be prepared on the
           - ^tay-'thkt*tsh?y ,are  us edTTsyCssp iking an appropriate amount of
         -.'••  secondary  dilii^ion standard into a 5-mL headspace vial containing
        ,,.;' 2 mL of reagen€f%ater.   The lower concentration standard shall be
            at the CRQL as  listed  in Exhibit C.   The high concentration  level
            shall be near the|
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                                                                           DRAFT

      6.3.2 VOA  calibration standard concentrations.
                   Calibration Ranges
                   Compound _ Low      Mid     Hieh
Benzene
Bromodichlorome thane
Bromoform
Carbon tetrachloride
Chloroform
Chlorobenzene
1 , 1 -Dichloroethane
1 , 2 -Dichloroethane .;
1 , 1 - Dichlor oethene
cis-l,2-Dichloroethene -'• '••
trans - 1 , 2 -Dichloroethene
Ethylbenzene
1,1,2,2- Tetr achloroe thane
Tetrachloroethene
Toluene
ortho-Xylene •;>- -;' ,;j
para-Xylene* '-'.- ~ ' '^V
1,1,1 -Trichloroef2wae
Trichloroethene > ;
Vinyl chloride t-
4-Bromofluorobenzene (SM£)
20
20
20
20
,20
20
20
20
20 ,
20 .<
J2Q ?-
20
20 .
20
20
, 20
& .-20 ,- -
",20 :- •'
'•' 20
20
20
100
ISO
100
100
100
100
100
100
100
100
100
100
, 100
ISO
100
100
„ 100
: 100
100
100
100
500
500
,500
500
500
500
500
500
500
500
500
500
500
500
500
500
500
500
500
500
500
                  Meta- ,-aft«i ftafa-xylene eoelttte in the GC system.
                  Cons«jpetitlyV':<;*Jhese compounds are quantitated on the basis
                         para-xyleae  calibration factor.
6.4   Calibration Sfe&ck Standard-f,.,
                                , ';'%'." IV t  "" '  •"*"
      The calibration check, is  a daily one-point check on the initial
      calibration.  The califesation check standard shall be prepared by adding
      an appropriate amount oC/Sjecondary dilution standard into a 5-mL
      headspace .-J^Sal ,xontaining"'%-liii»  of  reagent water.  The concentration  of
      the ci^Jjlfe^StloTtjjdbtodc standarH^s  the same as the mid level standard
      use4pn the initia^isgilibration'.

6.5   SJfcsfcem Monitor CompounH „

            stem Monitor Compsaind (SMC),  is 4-Bromofluorobenzene (BFB). A
                     in metljiSiiQl shall be prepared as described in paragraph
      6.1, an%'^0i SMC spiki^ solution at a concentration of 50 ptg/mL in
      methanol l^ill De pf^ared from the stock.  Each sample shall be spiked
      with the SMtf^oiiatlisai before analysis.   The SMC is used to monitor the
                     j. t t >•'<*,              J
      headspace sampled «aad GC  system, and to  provide a retention time marker
      on which to base relative retention time calculations.
                                   D-10-VOA-Q                          08/23/94

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                                                                         DRAFT

6.6   Performance Verification Standard

      The Performance Verification Standard  (PVS) shall "be analyzed at least
      once during each analytical sequence to assess system stability.  The
      PVS is two times the concentration of  the low, level calibration standard
      used in the initial calibration as specified In -paragraph 6.3.2.

6.7   Laboratory Control Sample                              ^ ,- ,s

      Laboratory Control Samples (LCS) containing known amounts of :!cmiget
      compounds traceable to primary standardisjwill initially be supplied by
      the Agency.  Following these initial supplies, however, the Laboratory
      shall prepare its own LCS standards ((paragraph 23 specifies the LCS
      compounds and concentrations).  The 1£S shall be spiked into a clean
      matrix and prepared using all steps bflthis protocol.  An appropriate
      amount of the LCS shall be added to reagete mter and analyzed with each
      Batch of water samples.  An appropriate amount of the LCS shall be added
      to clean quartz sand and analyzed with each Batcli -of soil/solid samples .
      An appropriate amount of the LCS shall be added txi'i clean corn oil and
      analyzed with each Batch of 4 oil samples.  If a Batch contains water,
      soil/solid, and oil samples^ an ijCSJ^hall be prepared and analyzed for
      each matrix.  All LCS compot»»is must'liavi, recoveries between 30 percent
      and 110 percent before sample :«nalys is may/begrri (see paragraph 23).

      NOTE:  The Laboratory is expecteft to maintain control charts of the
      recoveries of at least three (3) representative LCS compounds as an
      internal QC procedure .              :

6.8   Storage of Standard Solutions          -,:, ,
                      $<*          "£             "I
      6.8.1 Stock a^td 'secondary standard solutions shall be stored at -10°C to
            -20°C £n"'Teflon-line^;ScrewF-cap, amber bottles.

      6.8.2 Initial calibration standard solutions shall be stored at 4°C
            (± 2°C) in Tefloii!" sealed headspace vials until use.
      6.8.3 All^fawaacds shall' -"be protected from light.

      6 . &J^.: 'Samples and standards shall be stored separately.
                                  D-11-VOA-Q                          08/23/94

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                                                                          DRAFT
                                  SECTION III

            INSTRUMENT QUALITY CONTROL PROCEDURES AND REQUIREMENTS
7.2
      Instrument Operating Conditions

      The following are the suggested gas chromatographic  analytical
      conditions.
                                              & '.
      Column:     J&W DB-624  (or equivalent) ,:S30 m x 0.53  mm  ID,  3.0 pat "film
                  thickness fused silica capillary column  (FSCC).
      Carrier Gas:
      Flow Rate:
      Initial Column Temperature:
      Initial Column Holding Time:
      Ramp Rate:
      Final Temperature:
      Final Hold Time:            ./
      Approximate GC Cool Down
                                              Helium  j
                                           ""'ill-13 ati/min
                                              W»
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                                                                          DRAFT

      7.3.1 Temperature Settings

            Sampler bath temperature:            60°C

            Valve loop temperature:              100°G >

      7.3.2 Gas pressure and settings  (for Hewlett Packard Model 19395A)

                  Gas Mode          Type  Gas           Gauge  Preiastare (Barr)

                  Carrier            Helium    :'              0.7      " •

                  Auxiliary          Helium,.            -     1.1

                  Servo Air          Air                     3.1

      7.3.3 Programming timing for valve  operation:events
            Set Points
            Displays (time
            reading in sec.)
Key,.Jfco Press
Func t i on/Ac t ivi ty
            "01"


            "03"


            "13"     •'


            "14"

            "25"

           ^;*m*'''!: -~~~ jJ

       X"'" "227"

      j^l.    «228"
      ," ;  ?
         ;'*., -

7.4   Detector ;:Qi>eration
   PROBEv



   PRESSURE

  i "'
   3RRESSURE

    < '^^ **-A - "    s '
  ••• - w#..-, -A ,., -- S<,'  /,-.
   VENT/FILL  LOOP

   :VENT/FILL  LOOP

   IHJ1GT

   INJECT

   PROBE
Probe enters vial


Starts
pressurization

Stops
pressurization

Starts venting

Stops venting

Starts injection

Stops injection

Raises probe from
vial
      The ELCD and S1*IO!-retire more  care  and attention than most other GC
      detectors.  The "'Billowing guidance  in the  operation of these detectors
      is provided to laboratories using this method.   Laboratories that follow
      this guidance should have less downtime and fewer unpaid sample reruns.
                                  D-13-VOA-Q
                                         08/23/94

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                                                                          DRAFT

      Note: The Laboratory shall specify  in  the Batch Narrative  the target
      compounds associated with (detected by) each  of the  detectors.

      7.4.1 The ELCD nickel reaction tube should be replaced once a month as
            they may develop hot spots and burn pinhol-ies which affect detector
            response and background noise level.      ,;

      7. A. 2 The Teflon transfer line of the  ELCD should be replaced if peak
            tailing is observed.
                                              -*•                        '<
      7.4.3 An instrument log should be maintained  which includes response
            data.  If the response obtained ,Jtri an initial  calibration changes
            more than 20 percent from historical values,? the ELCD should be
            checked for leaks before sampJbss are analyzed.

      7.4.4 The PID area response should  be  moril to re>fi using toluene and
            ethylbenzene .  If the response ratio changes by more than 20
            percent, or if either area response decreases  more than 20
            percent, the detector window  should be  cleaaeti or the PID lamp
            bulb replaced         ,, ,
                                ; .'  '; ;,'*„   >  ,!;,•?,,
      7.4.5 Control charts should .'Site maihtaiSwik^pM: bsonoform and chloroform
            response on the ELCD.  'ffee ratio h&feween title, ,:bromo form and
            chloroform responses is an indication of reactor tube condition.
      7.4.6 Use of control charts for tbe m&t  level  calibration responses of
            broraof orm and chloroform on tljaf ELCD  and  for  toluene and
            ethylbenzene am l&e.jPID should3*e updated daily.   It is  generally
            not necessaaTf to mosi&or more thito,  these  four compounds  in control
            charts.  * '"'         "', •'           -"i.

8     Calibration *>'£ the GC Svst&ir...... Initial Calibration
                   ':  .. -. ,       JliL'fe C/ ;/
8 . 1   Summary         :  ;
      8.1.1 Prior to the anagrapts^of samples  and required blanks,  each GC
                   *os.t be initl«p^^-. calibrated to  ensure that the instrument
                              perfbl&feice requirements  of the method.   The
          ^'initial calibiation is accomplished by  analyzing three standards;
          ;" the low level , *&&£. level, and high level mixtures as specified in
            paragraph 6.3.2.Yf-The technical acceptance  criteria for the
            initial calibrator! are given in  paragraph  8.5.   The initial
          -, calibration shaljpybe used to establish  the  calibration factors
                 for compound 'kjuantitation, to define the retention time
                    for compound identification,  and to determine the  mean SMC
                      time^jfbr evaluating SMC shift during analyses.   Detector
            response Jmusf.t-sbe linear for all target  compounds .  All samples
            shall be aiisfeiyzed during the contract specified 24-hour analytical
            sequence .
                                  D-14-VOA-Q                          08/23/94

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                                                                          DRAFT

      8.1.2 Sample quantitation shall be based on the mean compound
            calibration  factor,  line segments ("K" curve), or the mid level
            calibration  factor  from the initial calibration.  (The use of the
            line segment or  "K"  curve is suggested.)  &11 field and QC samples
            and standards within a Batch and all fieM and QC samples and
            standards analyzed  in the same analytical' sequence shall be
            quantitated  using the same quantitation1 method,-  :

      8.1.3 Compound identification shall be based on RRT windows sifcstablished
            during initial calibration in all -field samples where ^jie SMC
            recovery is  greater  than or equal; *o 10 percent and less than or
            equal to 200 percent.
                                             .          _s •
      8.1.4 Compound identification shall 3*e based onsi|ibsolute retention time
            windows established during inrttiatl calibration in all field
            samples where the SMC recovery is'l«ss _ titan 10 percent, greater
            than 200 percent, or peak interferences axe present.

      8.1.5 Shifts in the chromatographic peaks shall be: evaluated by
            comparing the RT of  the;?SMC in all analyses with *he mean RT of
            the SMC calculated  fifOBNtfeie; l&ttf&al.calibration.  The retention
            time shift is referred|j?o as feTS^srIS? XH>;|<,see paragraph 17.4.1).
            The SMC RT for field arM §C sample^asalyses'lewist be within ±1.0
            percent of the mean RT caloulated,tiErom the initial calibration.
8.2   Frequency
      8.2.1 An initial three-jp&int calibration shall be performed to determine
            the linearity  of resfSWase of allHttarget compounds and the SMC.  A
            new initial calibration is required whenever calibration check
            standard^ »r PVSs  cara^ut satisfy QC criteria.   A new initial
            calibration shall  al^o-^e, performed whenever major instrument
            maintenance -has beeJir^l£8b^&~ 'Ss&ch as column or detector
            replacement ,?' :jto initial calibration must be performed for each GC
            and for each cteaaatographic column which are used to perform
            these analysis.  X;'; -
      8 .2.2 .^'•^aly^esfclysequence 'I-JSJ-"a contractually- defined sequence of GC
          , :', ^analyses whicfctc;eonsists  of an initial three-point calibration or a
        '-f. ' valid calibratiSbii^ check,  field samples,  LCSs, method and
        •':"'    instrument blanks*! PVS,  and other QC samples run within a 24-hour
      I,  f    period  (see paragaph 14 for the required sequence of samples).
                     of the , Initial  calibration shall begin with the injection
                   high lev*pl' standard followed by the mid level and low level
            standards     f :

      8.2.4 The analytaSjjal sequence  concludes with an acceptable analysis of
            an instrument  blank  and  a PVS (see paragraph 10) .
                                   D-15-VOA-Q                          08/23/94

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                                                                          DRAFT

      8.2.5 Samples shall be  analyzed  only  after meeting the technical
            acceptance criteria for  the  initial calibration.

8.3   Procedure

      8.3.1 The GC system shall be set up per  the  requirements of paragraph 7.

      8.3.2 Prepare calibration standard solutions containingifche SMC and all
            target compounds  using the procedure listed in paragraph 6.3.

      8.3.3 The initial calibration  solution .'.shall be  analyzed at the same
            temperature as  the  samples.      i

      8.3.4 Analyze each calibration standard  by using-^the same headspace
            sampler, headspace  vial  size, and  GC conditions to be used for the
            samples and blanks.              V:    V

8.4   Calculations                                    :;

      8.4.1 Calculate the calibratjUm .factor (ratio of the -total peak area or
            height to the mass  ai|a3^ii&;|%!^a,l) for each target compound and
            the SMC in the  three initial cali&ation standard analyses using
            equation D.I (EQ. D.I).  ifNote:  Calculate '-the SMC calibration
            factor by using the response froa^the  PID  detector.


                                  Total AX6S- of Peak 01 Peak Height
                                  	     - <.	=	:	. . ,—;	f	 -on  n  -i
                                     Mass of Ana2yte in  Vial (ng)    «-Q- O.I
                                 &'
      8.4.2 Calculate! >rthe mean  c^fcibration  factor  for  each  target compound and
            the
                                .           ,,
      8.4.3 Calculate tfee,s3SR.SD  of  the calibration factors  of the low level ,
            mid level, aridAlIgh level standards  for  the  initial calibration
            using the following' ,<%quation.
           /  '         "' 4- s    *RSD = -IP x 100                   EQ. D.2
                           '* ^           X


            where SD =  Stands^. Deviation.

          --lilStandard Deviatii&a is  calculated using the  following equation:
                                        -
                                   D-16-VOA-Q                          08/23/94

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                                                                           DRAFT

            where:       x^ =  individual calibration  factor (per compound).

                         x  =  mean of three initial calibration factors (per
                               compound).               ;

                         N  -=  number of calibration standards.

            Equation D.4 is the general formula for the mean .of a set of
            values:                                              • t '
\* xi---  '•
ft *-•>•
                                                                      EQ. D.4
            where:       X  -  Mean of values,  •;

                         Xt -  Value.

                         N  =  Number of values.
      8.4.4 Calculate the RRT f or ^ch taVg^ici^K>u»6l-*jsing  the following
            equation:               *'; •          "•'

                                          »
                                                                  EQ . D . 5
            Note: The  LaboHrdtascfy may select? the SMC retention time used with
            above equation" froiBjillte PID or E^3) chromatogram.   The Laboratory
            shall consistently usse&:either the'"^lC RT from  the PID or ELCD
                     ;$  .''       J    * ..            ~ ••••
            chromatogram (i.e., otipe the detector is selected to  derive the
            SMC RT ;
-------
                                                                          DRAFT

      8.5.3 The peak resolution between  cis-l,2-dichloroethene and chloroform
            shall be evaluated in  the  low level initial calibration standard
            before proceeding with sample analyses (see paragraph 11).

      8.5.4 The chromatographic peak response for all :target compounds in the
            low concentration standard must be greaterrittean 10 percent of
            full-scale deflection.

8.6   Corrective Action                                         \s

      8.6.1 If the %RSD for more than  two compounds in the initial calibration
            is greater than 25.0 percent or ii any compound exceeds 40.0
            percent RSD, the instrument  has.siot demonstrated adequate
            linearity to be used for this^asethod.   Connective action shall be
            taken and documented.          ;-'- i,,,      •'

      8.6.2 If the peak resolution criterion is not met, the Laboratory shall
            perform corrective action  and demonstrate adequate resolution
            before samples can be  analyzed.            'i

      8.6.3 If the SMC RT is not I^tfai4;j|£-%0,,percent of the mean SMC RT
            calculated from the tffjfee  initial^calibration standards, the
            Laboratory shall perf ormNcorrective^actritm libich may include a new
            initial calibration.   DO'UOT proofed with sample analysis until
            the retention time shift £lp!S)  is «i thin ±1.0 percent.
      8.6.4 If the peak response  for any target compound in the low
            concentratical istsp&ard is not gjreater than 10 percent of full-
            scale deflection," i%||iLaboratory3^tiall perform corrective action
            and make |a^propriate'%ipE4justments 1*efore sample analyses are
            started,, %o ensure  tK^t all  target compound peak responses in the
            low concentration st^&iard.rare greater than 10 percent of full-
            scale def||est:tion.  ^Lit I ^'V rj: ,,l)'<

      8.6.5 Corrective action, may include optimizing ELCD detector linearity
            by adjusting gas;'C|!>vs, replacing the ELCD nickel catalyst, by
            cleasing-detector optics* or by replacing the bulb.  Action may
           -,^lSo "fhcfeide'^replacing^-t^e pre-column, removing 0.5 - 1 m of the
         -; -^analytical coltram,  or replacing the standards.
        : •-"•                "" ••'?;
      .;.'..''.'  Note: major cori^tive actions (e.g., column, detector
     *-; .     replacement, etc|J)  will require a new initial calibration.
     V' -. -'•'..,.                  'r-
      v'.'-,!t.                 &•
      8.6"l6,-;|kll initial calibration technical acceptance criteria shall be met
           ^b^BSS-e any samples  or required blanks are analyzed.  Any samples
            or ?4Efeijpdjred bj^flcs  analyzed  when the initial calibration criteria
            have ribfc
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                                                                           DRAFT

8 . 7   Documentation

      Initial  calibration results are reported on Forms QIVA-VOA, QIVB-VOA,
      and QVI-VOA.   Reporting requirements are listed In Exhibit B.

9     Calibration of the GC System - Calibration Chfecfe.-.

9 . 1   Summary                                                 :>   =

      A check  of the calibration curve shall be/performed at the beginning of
      every  24-hour analytical sequence that jfiacludes field sample analyses.
      This check of the  calibration shall be i*erformed using the mid level
      standard and shall contain all targe tj;! compounds aod the SMC.  The
      percent  difference (%D)  between the 'Calibration, fiactor in the
      calibration check  standard and the a^ejsage calibration factor from  the
      initial  calibration is calculated for e-acl*, target compound and the  SKC,
      and must meet the  technical acceptance critserisa given in paragraph  9.5.
      The SMC  RTS and column resolution must also meet: Technical acceptance
      criteria as stated in paragraph 9.5 and paragraph 11; r, respectively.
      Only after all these criteria, are met can sample analysis begin.
                                  V • ^ If' '-y, "  V, -
      NOTE:  Compound identification and '" quassfctibation ..shall be performed  based
      on calibration factors and compound RRT ,3Bj2 KT wiJHfiws established
      during the initial calibration;;,,.
                                       " ,•      '':
9.2   Frequency                            ,

      9.2.1  Each GC used:!f^i3malysis shall be checked to verify the initial
             calibration  ior eacfc:<^4-hour perj|s«J of operation.  This procedure
             is  to ensure? that  the'Jbnstrument eotitinues to meet the instrument
             sensitivity  and linearity requirements of this method.
                   .               ^ "
      9.2.2  An analytical seque,lK|sx|;S\^::4oi*xactually-defined sequence of GC
             analyses whSelv -consists of an initial three-point calibration or a
             valid calibration scheck standard, field samples,  LCS, method  and
             instrument blanks^: 'IESS ,  and other QC samples run within a 24 -hour
             period ^»ee  paragraph
             ,          .
      9.2»,| 3he analyticaSf^equence shall be concluded with an acceptable
        ,";'• analysis of an^'ijffcstrument blank and a PVS (see paragraph 10) .
        : -^                  .'.I.
       r,v)                  ;fc ,
      y  '                    W'
      -S,;2.4 Samples shall be^tnalyzed only after meeting the technical
      ='s -,,\i  acceptance criteria for a valid calibration check standard.
        *3;. 'V'                ;, i
          " ~ „, ,.              .'.- !
9 . 3   Procedto^ > ,         /„:

      9.3.1 The GC ^fs-temf -iliall be  set up per the requirements of paragraph 7 .
                                   D-19-VOA-Q                          08/23/94

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                                                                          DRAFT

      9.3.2 Prepare calibration check standard solutions containing the SMC
            and all target  compounds  using the procedures listed in paragraphs
            6.3 and 6.4.

      9.3.3 Analyze the calibration check standard by r*|»ach target compound and
            the SMC in the  calibration check standardiaaix using the following
            equation.  Note: Calculate the SMC calibratHoxlrfactor by using the
            response from the  PID 4e,tector.
             Calibration Factor =       ***** °f ft*8*'"**-**** Height
                                      Mass Analyze in Vial  (ng)     EQ- D-b
      9.4.2 Calculate the~%lt\between the calibration factors from the
            calibration :check  standard and the .average calibration factors
            from the oSijitial calibration using ^;he following equation.
                                       _   __                    EQ. D.7
                         •* ,           x
                         '- < '•
                  where,      "'-flt  ,„

                              of three!;initial calibration factors (per
                         caliteation factor from current calibration check
                             V* t"
                         standard (per compound).
9.5   Teda'
            ieal Acceptance  Cg^teria
             ' »! ':X ':         ,' ''~"~
      9.5.1 The* *|>-Ijetween; tiie  calibration factors for each target compound
            and the:>!SMS|-.,J%-.the  calibration check standard and the mean
            calibratioiC factor  for that compound in the initial calibration
            must  be within ±  35.0 percent.  Up to two target compounds may
            exceed ±  35.0  %D; however,  all compounds must be within ± 45.0 %D.

                                   D-20-VOA-Q                          08/23/94

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                                                                          DRAFT

      9.5.2 All target compound absolute and relative retention times must be
            within the windows  established during the initial calibration.
            Report calibration  check RT and RRT data on Form QI-VOA  (see
            Exhibit B) .                                '1

      9.5.3 The retention  time  of the SMC in the calprtsation check standard
            must be within ±  1.0 percent of the meaji SMC retention time
            calculated from the three initial calibration standards.

      9.5.4 The peak resolution between cis-l,2-
-------
                                                                          DRAFT

9.7   Documentation

      Calibration check  standard results  are  reported on Forms QI-VOA, QV-VOA,
      and QVI-VOA.  Reporting requirements  are  listed.In Exhibit B.

10     Calibration of the GC System  -  Performance Verification Standard (PVS)

10.1  Summary                                                ,

      A PVS shall be analyzed at the  end  of every  24-hour analytical .sequence.
      The analysis of the PVS shall be  started  within 24 hours after °tfe
      injection of the first initial  calibration standard or the instrument
      blank analyzed before a valid calibration check standard.   The PVS is
      two times the concentration of  the  lefcr  level statsiard from the initial
      calibration (see paragraph 6.3.2);  therefore,  ttie  PVS shall contain all
      target compounds and the  SMC.             J   ,   ,

10.2  Frequency

      An acceptable PVS  must be analyzed  at the conclusion :af the analytical
      sequence.  The PVS analysis £&&jUC>&e^stasted within 24 hours after the
      injection of the first initial_ calibf £t'is£i -standard or the instrument
      blank analyzed before a valid,sea.libratia&! check «t&ndard.   If a
      successful PVS analysis is not Job.tained -&t the conclusion of the
      analytical sequence, all  samples^|snaly2ed since the last successful PVS,
      initial calibration, or valid calibration check standard shall be
      reanalyzed in a valid analytical  sequence at no additional expense to
      the Agency.  The I^»r4t*0jry is  encouraged to run additional PVS analyses
      during an analytical sequence to  minimize unpaid reanalyses.  If an
      acceptable PVSJLs  analyzed"'Soring an  analytical sequence,  the Laboratory
      may continue feo collect dat&"under  the  current calibration until the
      conclusion o£?t!he  current ^?#h,p,ux,sequence.   If at any time an
      unsuccessful CTS.-analysis^J^E^iaie',,- Jfee  Laboratory  shall stop sample
      analysis and imme:
-------
                                                                           DRAFT

      10.3.3       The recovery of each compound and the  SMC  in the PVS is
                   quantitated using the mean calibration factor,  the mid
                   point,  or by using a K curve established during the initial
                   calibration. (NOTE: Only one method Q£ quantitation shall be
                   used for analyses within a given analytical  sequence and for
                   a given Batch of samples.)       - ;  ";  ••-

10.4  Calculations                                          s '",'•,

      The amount of FVS compounds and the SMC recovered  shall  be  calculated
      using the following equations:         - - :                        *';

                                                2        *''
                              Amoun t absez3»g= --      . \             EQ.  D. 8
      where:       A^    =     area or peak height of '.the PVS  compound or SMC.

                   CFm   -     cal^r,ation factor established  by  one of three
                               tecianisues daring the initial calibration.
                                   Jxj  * "<*&, J !•* •• "_. ?,* - Y^* ^

                   Note:  Calculate t$i&6.SMC amou»i; usin^ tshe response from the
                   PID detector.      '"*'- ,      ,*
                                                    ,      x 100         EQ.  D.9
                                                    (ng)
                      ':,\,"~'       ''* *~"i .
                     , '-!           'frlh            :
10.5  Technical Acce^fcance CriterlSt''
                                 . , •• '^ ''

      10.5.1      ll'-|;;s£SS targe,4",;«|fis>l«i4i;M~fl*st have a calculated recovery of
                  75-1.25K,|3»rcent in order to report data without  flags.
                           ' * tz? -,.
      10.5.2      If recovery, ,^IE-a compound is not within 75-125  percent but
                f- -iSitill  within in-^|)ianded recovery window of  50-150 percent,
             ? >  -- "fee^asisociated saiipd|« analyses results shall be  flagged (see
                               . 6) .
                          "^,^x
                       SMC Te'iJ*yeTy criterion of 50-150 percent is  advisory
                  only.   Rea^ltysis of the PVS is not made if  the  SMC recovery
                  i-s  outside ji|iie advisory recovery limits.  The SMC  recovery
         ' .,  ;li,   in  tne PVapsust,  however,  be greater than or equal to 20
             !i?V«;> percent aaclTless than or equal to 200 percent (see paragraph
              •%HM).  |<"
                    ' "  ',  -f  """'
      10.5.4      All 'target  compound absolute and relative retention times
                  must be within the windows established during the  initial
                                   D-23-VOA-Q                           08/23/94

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                                                                          DRAFT

                  calibration.  Report PVS RT and RRT  data on Form QI-VOA (see
                  Exhibit B).

      10.5.5      The RTS for the SMC in the PVS must %e within ±1.0 percent
                  of the mean SMC RT calculated from the initial calibration.

      10.5.6      The peak resolution between cis-l,2-dicliloToethene and
                  chloroform shall be evaluated in the  PVS before proceeding
                  with sample analyses (see paragraph  11).     " , :':

10.6  Corrective Action

      10.6.1      If recovery of a compound ''"is not within  75-125 percent but
                  still within an expande^d -'window of ,50-150 percent,  flag the
                  outlier compound "P" in alX-associated field sample results
                  generated since the last valid. -EVSv  initial calibration or
                  valid calibration check standard.

      10.6.2      If any PVS compound is outside the expanded range,  another
                  PVS shall be analyzed immediately.   If ,  on reanalysis, any
                  compound is still outside the expanded recovery range, stop
                  sample analyses, perform" Twbasefeisive .action,  run a new
                  initial calibration, and reanalyze all samples run after the
                  last valid PVS, initial calibration,  or  valid calibration
                  check standard before proceeding with sample analyses .

      10 . 6 . 3      If the RT or RRT for any .compound is  not within the RT and
                  RRT windows established during the initial calibration,
                  analyze' ~ another1.- ,PVS.  If upon reanalysis a compound is still
                  outride the wiBsdbws, a new initial calibration must be
                  performed before samples can 'be analyzed.   The instrument
                  ,08*St be recaliifepaluied _as .described in  paragraph 8 and
                  reanalyze alkh^i^i^jaseia.rafter the  last valid PVS, initial
                  caliTbBation, or valid calibration check  standard before
                  proceeditigiiwith sample analyses.

      10.6.4   , ""7ie 'the SMC RT^paSterion is not met  for  a PVS, sample
          ,.: •'•'-'• •"-' analjjstife^. shall be^gtiopped and another PVS shall be
          .;        immediately analyzed.  If the SMC RTS is still outside the
       ,.' ,,--        criterionl'fBpon reanalysis, corrective action shall be
       ;..  *         performed'^yiich may include a new initial calibration.  DO
      .*;j"          NOT contiritfe'; with sample analyses until  the RTS is within ±
      ~i~ -75,,        1.0 percent^  Reanalyze all samples  that were run between
        *,;:&,,,    the noncomjliiant PVS and the last valid  PVS, initial
           "''!,:!","'., calibration, or valid calibration check  standard before
                  gproceediisg with sample analyses.
      10 . 6 . 5      If t%& 3?VS SMC recovery  is  less  than 20  percent or greater
                  than 2t)0 percent, or if  peak  interferences are present, stop
                  sample analyses, perform corrective  action,  and immediately

                                  D-24-VOA-Q                           08/23/94

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                                                                           DRAFT

                   reanalyze another PVS.  If the SMC recovery  is  still out on
                   reanalysis,  perform corrective action and start a new
                   analytical sequence.  All samples analyzed since the last
                   valid PVS, initial calibration, or valid calibration check
                   standard shall be reanalyzed within a valid  analytical
                   sequence .                             - -   ,

      10.6.6       If the peak resolution criterion is not met^ -the Laboratory
                   shall perform corrective action and demonstrate adequate
                   resolution before samples can&be analyzed (see  paragraph
                   11).                       .:,:?'                     '•!•'
                                            ' ,- ''
      10.6.7       If all PVS criteria canno*'>be met after having  taken
                   corrective action, reanalyze the associated  field samples in
                   another valid analytical • sequence . ;'If on reanalyses all QC
                   sample criteria are met and tshe,P¥S criteria still cannot be
                   met,  then submit all sample daira from both sequences.  The
                   Laboratory shall describe in the Batch narrative the
                   problems associated with the PVS and Ttfavr --the field sample
                   matrix may have 
      Results of  PVS  analyses l|te; .reported on Forms QI-VOA, QIII-VOA,  and QVI-
      VOA.  Ref^l$t:ilBg s^equiremehtsiarse listed in Exhibit B.
11    Sysfeeil' Performance ''I^SC Resolution

11.1  Sjottmary               ";'

           ^resolution betwee|i,:.(?is-1,2-dichloroethene and chloroform  shall be
               to  establish ;£bat there is sufficient chromatographic
      resolufcipitifor accuraie- compound identifications and quantitations.
      When minimsm peak resolution cannot be met, identification and
      quantitation is ;a«tefersely affected due to the difficulty in establishing
      the baseline.   !^l :1

11.2  Frequency

                                   D-25-VOA-Q                           08/23/94

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                                                                          DRAFT

      11.2.1      Initial calibration  - The peak resolution between cis-1,2-
                  dichloroethene and chloroform shall be  evaluated in the low
                  initial calibration  standard  before proceeding with sample
                  analyses.

      11.2.2      Calibration check standard  -  The sgpeaki'-Tesolution between
                  cis-l,2-dichloroethene  and  chloroform shall  be evaluated for
                  each calibration check  standard before  proceeding with
                  sample analyses.                               ,;' ,

      11.2.3      Performance verification staaadard  - The peak resolution
                  between cis-l,2-dichloroetibene and chloroform shall be
                  evaluated for each PVS  t&afc is analyzed in a valid
                  analytical sequence.    ;•).-,„        - • '••

11.3  Calculations                              ''<,-,    ,

      Determine resolution by calculating the percent- \ralley between two peaks
      using the following equation (see figure  1) .     • -  V
         Percent Valley =                                           Q
                                  Peak height of smaller
                                   peak beingl&esol'ved
11.4  Technical Acceptance Criteria

      11.4.1      Initial calibration  - The ^percent valley must be less than
                  or|equal to 25'sgercent between cis-l,2-dichloroethene and
                  chiMjroform in t& analysis  of the low  standard of the
                  jlMtial
      11.4.2      Calibration check  standard -  The percent  valley must be less
                  than or "'eg&al to 25 percent between cis-l,2-dichloroethene
                  and chloror^rasi 4.n  the  calibration  check standard.

      11.4,&;'>'' 's"*PeTfrijrmance verification standard  - The percent valley must
         j:J/      be less-itiian or equal  to 35 percent between cis-1,2-
        ,5. "'       dichloro'etfcene and chloroform in the analysis of the PVS.

11.5 tC.o'rrective Action      ;1!

                  If the peakResolution for the two compounds indicated in
                 „paragraphf-Ji.1 exceeds the 25 percent valley criterion in
                      low,4|svel standard analyzed during the initial
                             i, corrective action shall be taken,  and a new
                           calibration shall be  performed and documented before
                  proceeding with sample analyses.


                                  D-26-VOA-Q                          08/23/94

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                                                                          DRAFT

      11.5.2      If the peak resolution for  the  two  compounds indicated in
                  paragraph 11.1 exceeds the  25 percent valley criterion in
                  the mid level calibration check standard,  corrective action
                  shall be performed.  A valid calbration check must be
                  demonstrated or a new  initial calibration shall be performed
                  and documented before  proceeding witti"sample analyses.

      11.5.3      If the percent valley  for the PVS does not >nse£t the
                  technical acceptance criteria indicated in paragraph 11.4,
                  another PVS shall be immediately analyzed.   If a-fter
                  reanalysis the PVS percent^fcsolution is still outsile
                  criterion, corrective  acti«aa shall  be performed and a valid
                  calibration check demonstrated  or new initial calibration
                  performed. Reanalyze all: samples run after the last valid
                  PVS, initial calibration, ,««ra  valid''calibration check
                  standard before proceeding  with sample analyses.

      11.5.4      A high percent valley  could indicate Column  degradation;
                  therefore, column maintenance may be '-treijttired.   Maintenance
                  may include rem^ing 0.5  -  1 m  of the coltsin.   If these
                  measures do not work,  column replacement should be
                  considered.    '"'V.,,       <-"'Z~>. vr *',;•"-  .

11.6  Documentation

    .  Percent resolution results are reported on  Forms QIII-VOA,   QIVA-VOA,
      and QV-VOA.  Reporting requirements"'.,are listed  in Exhibit B.
                                  D-27-VOA-Q                           08/23/94

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                                                                          DRAFT

                                  SECTION  IV

         SAMPLE ANALYSIS AND COMPOUND IDENTIFICATION  AKD QUANTITATION
12

12.1  This method is designed for use in the  rapid analysis olf- water,
      soil/solid, and oil samples for the  target  compounds listed-;in Exhibit
      C.  If upon inspection of a sample the  Contractor suspects tfatt the
      sample is not amenable to this method, ..contact  the Regional TPO aor the
      CLASS contractor for instructions.   F«e Superfund emergency removal
      actions, contact the Regional Technical Project Officer or the
      Headquarters APO for instructions. rXf, for emejpgency response actions,
      the TPO or APO are not available, cbtsfcaet the Rfegional On-Scene
      Coordinator (OSC) for instructions.  The ,£abor«tory must remember that
      it shall follow the requirements  in  this StSJ, Without deviation.

12.2  Before samples or required blanks can be analyzed^ the instrument must
      meet initial calibration or>,calibration check standard and column
      resolution technical acceptameesCEritscscia.   All  samples, required blanks,
      LCS, PVS, and calibration standards'slial| be soialyzed under the same
      instrumental conditions.

12.3  Blank samples such as trip blanks and«field blanks supplied by the
      Region and included with a batch of iiield samples shall be prepared,
      analyzed, and reported as a water S&ssple.   Occasionally, a water QC
      sample (e.g., field -&&&;-*txip blanks) st?ill be included with a batch of
      soil samples.  If 'idle lafeoisatory  is  no%:?certain whether a water sample
      associated with a batch of';j|pil samplesC'is  a QC sample, contact the
      Regional TPO of the CLASS contractor.
                                <. i'
      NOTE: If water -IjAanks pTO&jjgdjggl3j$r "tjjtyei;{'Region such as trip and field
      blanks are included r^ln a batch of  soil  samples,  the laboratory will not
      prepare and analyze *aa~;associated  water method blank or a water LCS.

12.4  If unusual soir;feigh concentration samples are received,  see Exhibit D,
      Appendix'"B"for-rgfeniecal guidance «n screening and sample preparation.
         -f '"'£            !"t ' '.,:
         -, ,.$>•             v . ^


13.1 ..-ifese Separation      ^
                   samples sljiall be phase-separated into their individual
      phases J'J-ppixe phase separation techniques employed will vary according to
      the types%if, samplef -;£>eceived.   Since  it is impossible to know the
      number and tyg%$-«o|;'Chases that  will be present in a sample, the choice
      of phase separatsjjem/techniques is  left to the discretion of the analyst.
      Various techniques can be employed to  separate the phases.   These
      include pipetting off  liquid phases  (decanting should not be done),

                                   D-28-VOA-Q                          08/23/94

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                                                                           DRAFT

      centrifuging to remove suspended solids, and use of spatulas  to  remove
      solids  (wooden tongue depressors work well) .  Whenever possible, phase
      separation operations should be done with disposable glassware.  The
      phases  should be separated into glass containers; ^ri.th teflon- lined  screw
      caps.   This allows for storage and handling of tjie waste in a safe
      manner .                                          '   :.           .

      13.1.1       Samples received containing multiple phases soph  as  water,
                   oil,  and soil/solid in the same sample jar sh&ll! ,be  "phase
                   separated" into individual pjhases.

      13.1.2       Each individual phase is tafeen through the procedure as a
                   subsample.  Report analytical results; if. or each sample phase.
                   Note:  Each multi-phase saiiple shall fibe identified using the
                   EPA sample number convention for mij&ti -phase samples as
                   specified in Exhibit B.         . ,  -I:-'

      13.1.3       Do not analyze any phase that represents less than 10
                   percent of the total sample volume .  •" - , .
                                  /^  ,;•
      13.1.4       In the followiag|«f8&c[fed^£ea&, /where applicable, references to
                   "samples" explicitly mean-'!*"*i33gle;:|phase units."
                                     ' {
13.2  Sample  Preparation - Water Samples      ;'

      13.2.1       Transfer 2 mL of sample to -;a 5-mL headspace vial,  using a
                   gas tight syringe.    '-  -f
                         W   I *'*••• ~r.,         ' i   -
      13.2.2       Spike  She samf|f&, with 4 pi 
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                                                                    DRAFT

does not increase dramatically.  If the volume of methanol  increases
dramatically, this is an indication of a complex mixed phase,  treat the
sample as methanol non-miscible and note in  the narrative.   If it is
hard to determine if the sample separates, then more methanol  should be
added.  If the sample is miscible with methanol (no visible separation),
then it should be tested for water miscibilityi  '

13.4.1      Oil sample  - Methanol Non- Miscible

            If the oil  sample is characterized as methanol  extract able
            (not miscible with methanoli), then the following procedure
            shall be used.

            NOTE: For these samples j the soil/solid CRQL  of  all the
            volatile target compounds will be Jascreased  by  a factor of
            10.  The CRQL values on Form ijI-VOA must reflect this
            adjustment.                    •

            13.4.1.1    Weigh 6 g of oil sample inSo a wide-mouth test
                        tube. , (Oily mixtures should first  be  phase-
                        separated peepzding  to the procedures  in
            13.4.1.2    Add 6 mL of methanol  and mix  for  15  seconds
                        us ing a *ssor text liixer .

            13.4.1.3    Centrifuge the test tube containing  the  sample
                   , ,  ;!'|:after extraction for  approximately 5 minutes  at
                 .       *4|P to 200° rPIL   (Increase  centrifugation time
                j        fdi|;,sainples tha^ appear to  contain fine
                        particulates . )
            13*4.1.4    T&ug£*Jjp8^^g;ht  syringe,  transfer  100 /iL of
                  ,;:  ,   methanol layer  to  a  5-mL headspace vial
                    >  .^-.containing  2 mL of reagent  water spiked with 4
                      '"• uLt
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                                                                           DRAFT

                   13.4.2.1    Using a gas tight syringe, transfer  100  /iL of
                               sample to a 5-mL headspace vial containing 2  mL
                               of reagent water spiked with 4 uL of the SMC  (50
                               /ig/mL) .

                   13.4.2.2    Cap the vial immediately.

       13.4.3       Oil sample - Methanol Miscible/Aqueous Non~KLscible

                   If the oil sample is miscible with methanol and  is.jaon-
                   miscible with water, it canf;probably be characterized as  an
                   organic solvent,  and the following procedure shall be used.

                   NOTE:  For these samples tile soil/solid CRQL of all the
                   volatile target compounds iwLLl be increased by a factor of
                   20.  The CRQL values on Form. :QI~V0A- must reflect this
                   adjustment.

                   13.4.3.1    Weigh 6  g of oil sample iatp^a wide -mouth test
                               tube^. ,X,Oily mixtures should first be phase-
                               se|jaTat^d; according to the procedures in
                               paragraph "13*' iif .">;';;, '- •- f  =-,
                                     &.*                  '
                   13.4.3.2    Add 6 mLf metfaanol and mix for 15  seconds
                               using a
                   13.4.3.3     Centrifuge 'tibe test tube containing the sample
                         : , ;  {'-a^ter extraction for approximately 5 minutes at
                       s   "    "^p, to 2000 r$a|.  (Increase centrifugation time
                     <;'        foi|5$3Jiiples that: appear to contain fine
                     4          par^tleulates . )
                   Sjs4.:3.4    Tli&llfaSig^iSght syringe, quickly transfer 100
                              /zL of the methanol diluted sample to a 5-mL
                            ;.-;-headspace vial containing 2 mL of reagent water
                                      with 4 uL of the SMC (50 /ig/mL) .  Cap the
14    Instjgaihental

14.1  S^^up the GC system psfr  the  requirements in paragraph 7.
      •- '\^                     "'*$
                  Allow sample^  to  equilibrate for 30 - 60 minutes at 60°C
               ;   prior to smarting the injection cycle.

             '"% *"**"?!•.        * 'T('~
      14.1.2   ! s ; Samples flattst be analyzed according to the following
                  r^K&ceiients .  An analytical sequence consists of field
                  sample tinalyses and all associated standards, blanks, and QC
                  analyses performed within a 24-hour period on one
                  instrument.  There are two types of analytical sequences: an

                                  D-31-VOA-Q                          08/23/94

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                                                                    DRAFT

            initial calibration analytical sequence and a daily
            calibration check analytical sequence.  All samples  shall be
            analyzed within one of these analytical sequences .

            14.1.2.1    An initial calibration analytical sequence
                        begins with a three -point: calibration, an
                        instrument blank, anXCS, and. a method blank.
                        The initial calibration analytical sequence is
                        as follows:                       ',

                        •     Initial T3toree -point Calibration (analysis
                              of the Jifgh standard followed by the  mid
                              and Iqwjstandards)/,
                                  4% • v            :
                              Instrument; JBlank^

                        •     Laboratory Control Sample (s);

                              Method Blank(s);
                                                ) ; and
                               •--        '•'
                        •     Perifprmarose Verification Standard(s) .

            14.1.2.2    A daily calibration check analytical sequence
                  , '"; t-i&egins with an instrument blank, a valid
                ,  ;      calibration ch^sk standard, a method blank, and
              ,-?/,       an^JS.  The daily calibration analytical
               • :         sequence is as follows :
                                         Blank;

                              Calibration Check Standard;

                             ^Method Blank(s);

                              Laboratory Control Sample(s);

                              Field Sample(s);

                              Instrument Blank(s); and

                              Performance Verification Standard(s).

14.1.3      I^f ,.a^l;«cceptance criteria for these analyses  are met,  then
            the"IssSwsratory may proceed with sample analyses.



                            D-32-VOA-Q                           08/23/94

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                                                                           DRAFT

       14.1.4      All analytical sequences conclude with an acceptable
                  instrument blank and a PVS analysis.  The PVS shall be
                  started within 24 hours after the injection of the first
                  initial calibration standard or the ^first instrument blank
                  in the daily calibration sequence,

                  NOTE:  If a PVS reanalysis is required because of a non-
                  compliant initial PVS analysis, the PVS reaaaalysis must be
                  started within 26 hours after the start of the;current
                  analytical sequence.       ,;

       14.1.5      For a  matrix group of samples that are analyzed in an
                  analytical sequence, the dissociated method blank and LCS
                  shall  be analyzed in this ^ame analytical sequence.

14.2   Computer reproductions of chromatograms that /are attenuated to ensure
       that all peaks are on scale over a 100-fold grange are acceptable.
       However, post  analysis attenuation shall be no.igrjeater than a 100-fold
       range.  This is to reduce the potential for RTSs '=«£, compounds due to
       column overload and to ensupe >that the detector is operating within the
       calibration range.   If any sample compounds exceed the calibration
       range, the sample  shall be 'Itiuted a'ct&«ftiB$ *txj ^paragraph 15.
                                               4 •'    -.>'*,'
14.3   If any saturated non-target comp&und chssematographic peaks are evident
       or if any chromatographic peaks B^rerl^ laore than one RRT and/or RT
       target compound windows,  the LaboratO.lJJ' shall  use the "E,N" flags on
       Form QI-VOA to indicate this situation.

       14.3.1      If sftt^ated"*^omatographis^peaks outside target compound
                  RRIctmd/or RT ^tandows are evident, flag the nearest target
                            "E,N" ifjj, Form QI-VOA.
      14.3.2      If-'--*^.pmatogE^^«-%e^!8S:,.-#isrerlapping more than one target
                  compboilt;£RT and/or RT windows are evident,  flag the
                  correspotwtiaasg  target compounds "E,N" on Form QI-VOA.
                              "*«••."'  ' *
14.4  ChromatQgra^Kfc ,|?eak respotisge-aaiust be greater than 10 percent and
      less J&ah I'O^p^co^at of full^ifkale deflection to ensure that
      indfe^dual compounds:will  be visible during data review.

15    Piltttions            'f-;:

15.1  l^i^ples with compoundsifxceeding the calibration range of the GC must be
               with the "E" JUjita flag as described in Exhibit B.   Upon
                  the Region, jiaay require that the samples be diluted and
                      valiAsanalytical sequence  as additional paid samples.
      Reextraction -and^oijiireanalysis  of samples  can only be authorized by the
      CLASS contractor-aleting on behalf of the Regional TPO or Headquarters
      APO.  The Laboratory shall perform the dilution analysis as specified
      below in paragraphs  15.2.2 and  15.2.3.

                                  D-33-VOA-Q                          08/23/94

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                                                                          DRAFT

15.2  The Laboratory may dilute samples  prior to initiating sample analysis.
      The resulting analysis  of those samples must produce chromatograms with
      at least one target compound present at a concentration greater than
      that found in the mid point calibration mixturej- If no compound is
      identified in the diluted sample at a concentration that exceeds the mid
      level standard, then the undiluted sample shall be reanalyzed at no
      additional cost to the  Agency.              ,

      15.2.1      At the request of the  Region, sample dilution p^y be
                  required prior to the  initial&analysis.  If no target
                  compounds are detected in tfee diluted samples at the aid
                  point concentration or greater,  then the undiluted sample
                  shall be reanalyzed as an. additional paid sample.

      15 . 2 . 2      Dilutions of water samples lor methanol miscible/aqueous
                  miscible oil samples (see paragraph 13.4) shall be made by
                  using an appropriate aliquot of ssaple diluted with reagent
                  water .                           '' >' ~ ,-

                  NOTE:  Dilute samples  prior to the addition of the SMC.
      15.2.3      Soil/solid  samples  requirii^HiSfci-on. _, shall be prepared by
                  adding a  smaller !i sample aliquot to 2 il of reagent water.
                  The minimum amount?iof soil/s&lid sample that can be used is
                  100 mg.   If dilutions gremay be necessary to sonicate and/or centrifuge some
                  types of>jSQ|Lids in  order to disperse and fractionate these
                  matrices  fot£',iB«»re effective extractions.
                               "*'   *
                 -      .           -,  ^
      15. 2.^; VI-'  '" "Di;l*^|S>f^is  of the"%«iaianol non-miscible oil (see paragraph
          ';','      13 .4.1^|ifcad methanol  miscible/aqueous non-miscible oil  (see
        -!,\         paragrapSfl*3.4.3)  shall be made by adding smaller amounts of
      ,,-;f :         the  sample, ffextract to 2 mL of the reagent water spiked with
      *;? ;          4 /tL of  SMC.'fcLn a  5-mL headspace vial.  For large  dilutions,
      "V'v;        the  extract^, may  be serially diluted in water and a portion
         \ "%| ,.    may  be ad^d to 2 mL  of the reagent water spiked with 4 jiL
            "b^t':-, of SMC i»,|a 5-mL  headspace vial.  If methanol extraction or
               ""- - s.:14ilutio*;lts performed, the Laboratory shall also prepare a
                  method:iblank spiked with the same amount of methanol (see
                  paragraph  21) .
                                   D-34-VOA-Q                          08/23/94

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                                                                          DRAFT

      15.2.5      Sample dilutions  shall be  analyzed in a valid analytical
                  sequence which  includes  the associated method blank and LCS.

      15.2.6      If sample reextractions  and reanalys«s are required, the
                  Laboratory  shall  also reextract and reanalyze an associated
                  method blank and  LCS.

16    Identification of Target Compounds

16.1  Retention Time Standard - The SMC shall.be used as the RT masker for
      compound identification.  The SMC shall ialso be used to monitor -heated
      headspace sampler efficiency.
                                           ,  * *           ^
      In each analysis, the SMC RT  must be 'Within ± l.!0 percent of the mean RT
      of the SMC established  during the initial  calibration.

16 . 2  Compound identification when  SMC  recovery  is greater than or equal to 10
      percent and less than or equal  to 200  percent.   ,

      16.2.1      target compounds ?shall be  identified on the basis of RRT in
                  all field sampfW'.fior: wfciieh the SMC recovery is greater than
                  or equal to 10  petcent and "lejss , .t&axi. or equal to 200
                  percent.

      16.2.2      Peaks in sample chroKatograffls  shall be identified as target
                  compounds if their  RRT isr within ±  0.005 RRT units of the
                  mean RRT established  during initial calibration.
16.3  Compound identification wh^a SMC  recovery  is  less  than 10 percent,
      greater than 2@$r,percent, oivif peak  interferences are present.

      16.3.1      ikrget compound^ ;:shall -he,,, identified on the basis of
                  absolute RT im^iilci^sM ^samples  for which the SMC recovery
                  is i'ess'Hthan 10 percent,  greater  than  200  percent, or if
                  peak interferences are present.
      16.3.2. " , .' g&ak^ in samplfelychromatograms  shall be  identified as target
          ,   -     compoiinds if their%absolute RT is within ±1.0 percent of
          ;, ',        the meafrilT established during the initial  calibration.
        -•--'" '                 ' « ,
      li$,I3.3      Any compouSI^. identified on the basis  of absolute RT shall be
       :?:,          flagged witii.the qualifier "T" (See Exhibit B) .
      "H'/!.>                  l'^
      16 .3:14 ';>    If the reGiBfwery of  the SMC in  a field sample is less than 10
           1 - -- -             ''£ is
             t, j,  percent, jgf eater than 200 percent, or if peak interferences
               :" ' y'fSXp preheat,  acceptable recovery of the SMC must be obtained
                  In stbe.' Associated method blank and LCS  (see paragraphs 21
                  and 1235 .
                                  D-35-VOA-Q                           08/23/94

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                                                                          DRAFT

16.4  If multiple peaks are within  the  identification windows (target compound
      and SMC), the Laboratory  shall use  professional judgement to properly
      identify the appropriate  peak.  The Laboratory should consider the
      inherent matrix effects of the sample  on peak shifting, masking, and
      overlaps when making identification determinations.   The Laboratory
      should take into consideration the  mean RT  and JKIHfjrom the initial
      calibration, RT and RRT from  the  calibration^seheck standard, and the SMC
      RT from relatively clean  samples  analyzed before and aflfcfej: the sample in
      question as a basis for selecting the  most  appropriate peak.  The
      Laboratory shall describe in  the  Batch Efarrative the rationales ssed for
      choosing a particular peak (e.g., chosei^eak closest to the RT eff the
      peak in calibration check standard)  as piche  target compound or SMC and
      how the field sample matrix may have, ^affected peak' identification.

17    Calculations                         '"!= " i ;     (,f

17.1  Calculate the RRT of a sample component or % Standard using the
      following equation:                           l  ;


                                                                     EQ.  D.ll
      where:                                >' -

      RRT — relative retention  time         :'

      RTcomponent = retention feiae of the  target  compound

      RTSMC = retention time of tie SMC
17.2  Calculate the '-calib.rationC^cs^jrK'iBiif-^" compound by one of three
      techniques using -da".^,. collected during an acceptable initial calibration
      (paragraph 8) .  Only #v&e> ,of the quantitation techniques listed below
      shall be used for quantifcifcing samples within a Batch and analyzed
      within a.~|gi'«feni:analytical"^^|!pence.   The  use of the line segment or "K"
      curve ps' -^suggested;,,         "--^1
                           ,
                  Use the ^f curve  (line  segments)  established during initial
       ~if         calibration^   The  segments  run from the low to the mid point
      : ,f          and from tle^ mid to the  high point calibration mixtures.
     ^•'i'^n       (Note: do not:  extend  line segment  through the origin if the
        'M ""-'-:.-.   concentraticm  is below the  CRQL) .
            \'l- , v,,-,          -U*'
              . '• ' i ,         vr~;
      17.2.2   '•*-* jjset the -calibration factors based  on the mid point of the
                  rcatsLaJtrtfalibration curve.   This option may be used as long
                  as tihie^laiid point values  are within ± 10 percent of the
                  average of  the high and  low point  values.
                                   D-36-VOA-Q                          08/23/94

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                                                                          DRAFT

      17.2.3      Use the mean  calibration factor established during the
                  initial calibration.

      17.2.4      Quantitation  of  compounds is  based on the calibration
                  factors established during the initial calibration.

      17.2.5      All calibration  requirements,  including the initial
                  calibration %RSD and the calibration check.jtD criteria, must
                  be met regardless of the quantitation techniqafeiused.

17.3  Quantitation of Target  Compounds       f"

      Calculate the concentration  in the sample using q-ne of the following
      equations for external  standards.  .tjfce response .-ban be measured by
      automated peak height or  integrated -pe^j .area .measurements.

      17.3.1      Water and Oil (Methanol Miscible/Aqueous Miscible)
                                                        '>*

                        Concentrates tjis/L) =  f         !           E0- D'12
                  where:

                  AX    -      response £or.,«he analyte to be measured.
                                           r
                  CFm   *; ^  :,,calibration feijtor established by one of three
                       .;>  ' '     %ec|»niques dur.|30|g the initial calibration.
                               (NQpS:  Only one" -Method of quantitation may be
                    ,'-          usel^for samples =within a Batch and analyzed
                               wi^faln an analytical sequence).
                   -" ,  ; -        -;M- ^i'Jf-  'T -
                  Vs   'v>*  :,    volume of water analyzed (mL).

                  DF       -  »,sfiil.ation Factor.

      17.3,aJ ?';  ''' SbiO^Sadad  (Wet-wei^it basis) and Oil (Methanol Non-Miscible
          3 ::     and  MetJtSaol Miscible/Aqueous Non-Miscible)
                       Conceation
                           - -,;f
                     .re:   I -
                            =  same  as  given in Equation D.12.

                  Wg        =  weight of sample analyzed (g).

                                  D-37-VOA-Q                          08/23/94

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                                                                          DRAFT
                  DF       =  Dilution Factor.   If methanol extraction was
                              performed,  DF —  mL methanol added to sample
                                                mL methanol extract analyzed
                              If methanol extraction w£s not performed, DF=1.
17.4  Calculate the SMC amount observed and amount ^{NBCceat)  recovered using
      equations as described in paragraph 10.4.   ,~'f

17.5  The RTS shall be monitored using  the SMC  (paragraph 16.lj; 4fhe RTS
      shall be measured for all analyses.     , ''.-.-                  '•'-',!; „,

      17.5.1      Calculate the retention tiste  percent difference (RT %D) of
                  the SMC in the field  and QC samples  or subsequent standards
                  analyzed and the mean SllC;'RT  from  masfe recent initial
                  calibration analyzed  usiiig the  following equation.


                             RttD = RTc~RT" x 100                    EQ-  D-14
                                      RTC

                  where:

                  RT %D -     Retenfi^n time sMft:  : >'  :

                  RTS   =     Retentioa'.ttime-of the  SMC in a  field and QC
                              sample or subsequent standard.

                  RT_   *r ;  '^Eean retenti'db'ttime of the SMC  from the most
                    **    S5 -< - „. / (  ' si,           ";••
                                     initlal«|
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                                                                          DRAFT

18.6  The RTS  for the  SMC RT must be within ±1.0 percent between any sample
      in a Batch and the mean RT of the  SMC analyzed during the initial
      calibration.  The RTS is not evaluated if the SMC ,is not recovered in
      the sample or if peak interferences  are presents

18.7  The advisory recovery limit for  the  SMC is 50-l'50-:ipercent.  Reanalysis
      of field samples are not made if the SMC recovery is outside the
      advisory recovery limits.  Note: The SMC amount recovered, is calculated
      using the response from the PID  detector.                   - .
18.8  The SMC recovery must be greater  than or'. «qual to 10 percent
      than or equal  to 200 percent  in order. ato use RRT for identification
      purposes.  The identification window is  ±  0.005 unit of the mean RRT of
      each target compound from the initi&l ^calibration.   If the recovery of
      the SMC is less than 10 percent,  greater than 200 percent, or is if peak
      interferences  are present (but is adequately .recovered in the method
      blank) , the absolute RT of the compounds shall be used for
      identification purposes .   The identification Window is ± 1.0 percent of
      the mean absolute RT of each  target  compound from tfee initial
      calibration.               -  ;-->
                                f  ' ' - ^ ' • "- ; ^ ,
                                '- '•  ' :'JW1, -',,-•  , ,
19    Corrective Action           ,'"        ;=  :;.  „*,  •; >..,
             '""                      '              ;. ,  ..,  • •• '

19.1  Flag all sample results "S" if the SMC is  outside the advisory recovery
      limits of 50-150 percent.        ;"

19.2  Flag all sample results "T" if the -absolute RTs are used for
      identifications .    ',",;,

19.3  An SMC recovery ~-pf  less than 20 percent , in the method blank or LCS
      associated wilfc :a sample Batseh is an indication that serious problems
      have occurre&r4uring the atyaB^sis , „ .Corrective action shall be performed
      and the unacceptable metbodcllank and/or LCS and all samples associated
      with the unacceptable method blank and/or  LCS  shall be reanalyzed at no
      additional expense  to4he Agency.
19.4  If the R1S' fetiteidon is not?met for  any  field sample,  sample analysis
      shall•f^^topp^ed;;«ajid. the noncoapliant  sample  rerun.   If the RTS
      criterion is still %*it upon reanalysis,  analyze  an instrument blank.  If
      thfSinstrument blank^-SttC shift is outside  the criterion,  perform
      corrective action whici|:3nay include  a  new  initial  calibration.  DO NOT
     ,:«^htinue with sample awi|yses until  the  RTS is within ±1.0 percent.  If
      "t:hai,;i.nstrument blank S|EC? shift meets the criterion,  sample analyses may
      conrli*)j»%  The Laboratpiby shall report both sets of noncompliant sample
      data aftdjiflag the resttlis "M". Note: the RTS  is  not evaluated if the SMC
      is not recovered in.tie sample or if peak  interferences are present.
                  ' ••';' ',  *"
19.5  All target compound concentrations which exceed  the upper limit of the
      initial calibration range will be flagged  "E"  (see Exhibit B).


                                  D-39-VOA-Q                          08/23/94

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                                                                         DRAFT

      NOTE:  Unless otherwise stated in Exhibit D, all sample data from the
      initial analysis shall be reported to the appropriate Region.   Samples
      not meeting any one of the contract technical acceptance criteria and
      not requiring automatic reanalysis shall be flagjged by the Laboratory.
      The Region will evaluate the noncompliant samples and may specify that
      these be reanalyzed as additional paid samples. :?  /,

20    Documentation                                           -  ,

      Sample results shall be reported on Forms QI-VOA and QVI-VOA.   'Reporting
      requirements are listed in Exhibit B.   \'
                                  D-40-VOA-Q                          08/23/94

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                                                                          DRAFT

                                   SECTION V

               SAMPLE QUALITY CONTROL PROCEDURES AND REQUIREMENTS
21    Method Blank Analysis                            .;  r

21.1  Summary  - A method blank for water and methanol miscible/aqueous
      miscible oil samples is  2 mL of  a reagent water spiked witfk the SMC.   A
      method blank for  soil/solid samples is l^g of clean quartz  'saasd^spiked
      with the SMC in 2 mL of  reagent  water. -, '"&. method blank for  metha»01 non-
      miscible and methanol miscible/aqueousjhaon-miscible  oil samples is  6 g
      of clean corn oil prepared  and added ;ts& 2 mL of reagent water  spiked
      with the SMC.  A  method  blank spiked ^writh metharaol and 4 pi. of SMC  shall
      also be  prepared  when soil/solid sampiiss,. from .fSfai Batch are extracted
      with methanol and diluted in reagent water*; jfethod  blanks  shall be
      carried  through the entire  analytical  procedure (paragraphs 13 and  14).

21.2  Frequency                                        :::  ,,

      A method blank analysis  sh^|;^T^V|Pf^f>pi>£d for each  matrix  type (water,
      soil/solid, or oil), with ea|ti set of ss^p|les,, pud, whenever soil/solid
      samples  are extracted with  met&anol and diluted in reagent  water.   A set
      of samples is defined as those %amples :from one Batch  that  are analyzed
      on one instrument during a  24-hoU£, analytical  sequence .

      21.2.1      The method blank and all ^associated samples shall  be
                  analyzed in:>i:he same analytical sequence.   If samples from a
                  batc&vtare ahafjij^aed in moret^j&an one analytical  sequence,  the
                  associated meti$!*l blank mustyalso  be analyzed in the same
                  analytical sequence .

      21.2.2      An >afeceptable;?^|^Q»ti>^^fe; -shall be analyzed before running
                  any saiajjles  within an analytical sequence .
      21.2.3      Criteria f or^an-- acceptable  method blank are  defined  in
                               "
21.3  Pro^e^are for MetHoAaiank Preparation
                  Prepare th:method blanks  at  the frequency  listed  in
                  paragraph
                  Measure oujfeflS mL of reagent water  for each water and
                 , methanol ntiscible/aqueous miscible oil method blank sample
                  :a!4.quot '^m:o a 5-mL headspace vial.  Spike with 4 /tL of  the
                             mL) and immediately  cap.
                      -''
      21.3.3      Soil/solid method blanks are 1  g of clean quartz sand  spiked
                  with 4 fj,L of the SMC  (50 pg/mL) in 2 mL of reagent water in

                                  D-41-VOA-Q                          08/23/94

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                                                                          DRAFT

                  a 5-mL headspace vial and vortexed,  as described in
                  paragraph  13.3.  Proceed with the analysis procedure
                  described  in paragraph 14.

      21.3.4      Methanol non-miscible and methanol wlscible/aqueous non-
                  miscible oil method blanks are 6 ^g. !o£ 'clean corn oil
                  prepared as described in paragraph 13.4, J; Proceed with the
                  analysis procedure  described in paragraph St4, •-,
                                                                •''  '-. n
      21.3.5      Method blanks  spiked  with methanol shall be prepared
                  whenever soil/solid samples are extracted with methanol and
                  diluted into reagent  water.!  Spike the same amount of
                  methanol that  was used fiar soil/solid8- sample dilution into
                  2 mL of reagent water sfi%ed with kf^jL of the SMC (50
                  /ig/mL) .  If more than QTX&. sample iji'-tihe Batch is extracted
                  with methanol, the  amount of %ethai3961 used for the method
                  blank  shall be the  greatest amoumt: .used for soil/solid
                  sample dilution.

21.4  Technical Acceptance Criteria,.

      21.4.1      All method blari3&,^shail!1^?4ftlg6tjaed.tWi,thin an acceptable
                  analytical sequence on a GC sy'stem ffleeting the initial
                  three-point calibration or A'sralid calibration check
                  standard criteria (psragraflis 8 and 9) , and the PVS
                  acceptance criteria (paragraph 10) .
      21.4.2      The R"BS > Joi: ;$h.e SMC  in tfee^ethod blank must be within ± 1.0
                  percejSt "betwesifcthe  blank tjaaxi the mean SMC RT calculated
                  frost- the initial: calibration;'
                     "S;:           .$
      21.4.3      ,,-lhe. SMC recove^^cr.iterion^of 50-150 percent is advisory
                  onljr..™ The SH^JM^Jc^^^i^the method blank must, however,
                  be greater than or equal  to  20 percent and less than or
                  equal to.dlOG^percent.
                            ''  "
      21.4.4   ;,'"?Ibe target cbnrpbtatds  or  potential interferences in the
            '--. '£ "!met:1sM»^ blanks muk€-|feave  a response less than one -half the
                  response 4n the corresponding RRT window of the initial
                  calibraiiipi low concentration standard.
                            J>;%;
                  A method bl|tak may  contain a detectable  but acceptable
                  concentratl||ii of  a  target compound (less than one-half the
                  response ojfllthe initial  calibration low concentration
            ''-'. '<*• •:•,„ „ s tandardVjvif
             sv ift ', ;; ,        '$• / *
                 j : | s -     - "f"
      21.4.6      Ilf'al;4-,1&Siteria are satisfied,  the method blank analysis  is
                  acceptable and samples may be analyzed.   If the method blank
                  is unacceptable,  corrective action shall be taken and an
                                  D-42-VOA-Q                          08/23/94

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                                                                          DRAFT

                  acceptable method blank must  be  analyzed prior to analyzing
                  the associated samples.

21.5  Corrective Action

      21.5.1      If a method blank does not meet  t&e  technical acceptance
                  criteria, the Contractor shall e*msideT cjje. analytical
                  system to be out of control.  It is  the Contractor's
                  responsibility to eliminate method interferences* caused by
                  contaminants in solvents, reagents,  glassware,  and (other
                  sample storage and processing hardware  that lead to discrete
                  artifacts and/or elevatedfjfeaselines  in  gas chromatograms.
                  If contamination is a prol&em, the source of the
                  contamination shall be investigatedJand appropriate
                  corrective measures shall |>ej  taken «kid  documented before
                  further sample analysis proceeds .4

      21.5.2      If a compound is found in the method blank (less than one-
                  half the response in the corresponding  RRT window of the
                  initial calibration, low concentration stataiard) and  is also
                  detected in an>paf&0pn reanalys&s the  method  blank SMC recovery is
                  still •thitsideitfee the recowry limits,  the method blank and
                  all..associated'ifi3mples shall  i»e  reanalyzed at no additional
                  c***t to the Ageia|y.
                  , ~ -           ^,1 j; , ,,  ,,,,.,	
      21.5.4      Flag, all methoi"i3.ai0]5Jirfe.s|its "S"  if the SMC does not meet
                  the aeivJbsory recovery criterion  of 50-150 percent.

      21.5.5      If the RTS'-cutlerion is not met  for  a method blank,  sample
                                   ^stopped and another method blank shall be
                             If the-*pJS criterion  is still out on reanalysis,
                  perfof&ijporrective action which  may  include a new initial
                  calibrati<£|u  DO NOT continue with sample analyses until the
                  RTS is witpta ±1.0 percent.
       •1»|>*6      Any samplei!processed with a method blank that is out of
         :;   ,     control (iisB. ,  does not meet any of the  technical acceptance
           '"'"';   ;:  criteria)ishall be reextracted and/or reanalyzed at no
                ;  additionai expense to the Agency.
                                  D-43-VOA-Q                           08/23/94

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                                                                          DRAFT

21.6  Documentation

      Method blank results  are  reported on Forms QI-VOA -and QVI-VOA.
      Reporting requirements  are  listed in Exhibit B.

22    Instrument Blank Analysis                    -

22.1  Summary

      An instrument blank is  2  mL of  reagent water spiked with 4 /iL,t*£,SMC
      stock solution  (50 pg/mL).   At  least twflfpC^) acceptable instrument
      blanks shall be analyzed  within an analytical sequence --one before
      sample analyses and one following sample analyses.
                                            >',,          j:C  -
22.2  Frequency                              ;f -,

      An instrument blank shall be analyzed at least twice during the
      analytical sequence to  ensure that the instrument,-is free from potential
      contaminants.  The first  instrument blank analysisV&hall be performed
      after the initial three-pointsjcalibration in the initial calibration
      analytical sequence or  as fJae^<3fJtjE^fe,;8n8p.yjsis in a daily calibration
      check analytical sequence.  "^Ijjbe second^l&B$!Miafen£ blank analysis shall
      be performed immediately  befofce the PVS ajaSlys'rs;  ilfhe Laboratory is
      encouraged to run additional inj$tgrument^~tp.anks during the analytical
      sequence, especially  when highly ^contaminated or complex samples are
      analyzed.  Instrument blanks must be analyzed after analysis of samples
      with high levels of target  compounds [or interferents (see paragraph
      22.5.6).          ,; :-; ,;f-  ,          " \:
22.3  Procedure for Instrument  BBsrak preparation

      A instrument^&iiank  is  2 nil^l^sa&e.nt: ..water spiked with 4 /xL of SMC
      stock                       '       ''
22.4  Calculations         <>-\:y

                        the  SMC "s«»is -.-arty target compounds in the instrument
                          ;, accordirijg S) the procedures described in paragraph
      17. allote: The targ^Hsscompound concentrations (detected concentrations
               values) in ra^- instrument blank shall be reported in the
            jriate concentratrijiia  units (e.g., report in >ig/L if the associated
         jles are water and  iti pg/Kg if the associated samples are soil) .
22.5  Techt^al Acceptance
            xi' ;*-> -
             ''*\< :  ,         .
      22.5.1     ,gji,:|RiiiimuW'-of two instrument blanks shall be analyzed during
                   3tk'«$^lj$ical sequence on a GC system meeting the initial
                   three*rf»oant calibration or valid calibration check standard
                   criteria  (paragraphs 8 and 9) ,  and the PVS acceptance
                   criteria  (paragraph 10) .

                                   D-44-VOA-Q                          08/23/94

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                                                                          DRAFT

      22.5.2      The RTS  for the SMC  in the  instrument blank must be within ±
                  1.0 percent of the mean SMC RT  calculated from the initial
                  calibration.

      22.5.3      The SMC  recovery criterion  of 50-150 percent is advisory
                  only.  The SMC recovery in  the  instrument blank must,
                  however, be greater  than or equal; to 20 percent or less than
                  or /equal to 200 percent.

      22. 5. 4      The target compounds or potential interferences' ia the first
                  instrument blank (analyzed  immediately after the initial
                  calibration or before a valid calibration check) must have a
                  response less than one -half the respoa&e in the
                  corresponding RRT windows of the initial calibration low
                  level standard.

      22.5.5      Subsequent instrument blanks are acceptable with low level
                  contamination.  These instrument blanks may contain target
                  compound concentrations up  to twice t1ie-CS.QL (2x CRQL) .

      22.5.6      Following the anal3r$asr|»f-|a -field sample containing high
                  levels of target-compounds -^-;l33t*:e§erents,  an instrument
                  blank shall be analyzed and oust meet acceptance criteria
                  before following witifa sample/^analyses .   If an autosampler is
                  utilized then the field saargles run after a high level
                  sample must be carefully evaluated for carryover.   The field
                  sample immediately following the high level sample shall be
                  reanalyzed Ustteng with any^other samples analyzed after the
                  high-level sample which she«is evidence of carryover.
      23.5.7      H$gh level sampjjfs are defined as  being field samples that
                  dsgfctain target|icst8!tppun,ds , at < concentration levels that exceed
                  tfw%«?e,~the hig&M|J&b&^<& > standard concentration and/or
                  interfersents that are detected at  levels greater than the
                  mid level :iaitial calibration standard concentration
                  response of >,%$& .nearest target compound.
22.6  Correefeisre
                            „
          >;.l      All groupjs',#pf samples analyzed shall be bracketed with two
                  acceptableiiinstrument blanks.  If  either  instrument blank is
                  unacceptable, corrective action shall be  taken and all
                  samples notL&racketed by two valid instrument blanks shall
         ".<,„',, ,    be reanalyzed at no additional expense to the Agency.
            ''''"•'/••"            ,|i
      22.6.2    -  !3|£r«any twiget compound in an instrximent blank analyzed after
                  tSte, Initial calibration or before  a valid calibration check
                  stati&aareE is greater than or equal  to one -half the response
                  in the corresponding RRT window of the initial calibration
                  low concentration standard, corrective action shall be

                                  D-45-VOA-Q                           08/23/94

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                                                                     DRAFT

             performed, and the system shall be demonstrated to be clean
             by the analysis of additional instrument blanks until all
             target compounds are within QC limits,,

 22.6.3      If any target compound in an instrument blank analyzed after
             field/QC sample analyses is greater than two  times the CRQL,
             another instrument blank shall bi& analyzed » :  If on
             reanalysis, contamination still exceeds thei .criterion,
             corrective action shall be performed and the
             demonstrated to be clean.  Iben, all associated
             samples analyzed since thejfmst valid instrument blank or
             method blank which containrslthose target compounds  or
             interferents found in the ii-nstrument iilank  at levels greater
             than twice the CRQL shall be rerun. /r

 22.6.4      If an instrument blank (othec thsli : the first  instrument
             blank in the analytical sequence ) ^contains  target  compounds
             or interferents between one -half response and two  times the
             CRQL, all positive results (results g^atser than or equal to
             the CRQL) for those compounds in samples ^analyzed  after the
             last valid inslseliB^Bt^^Lppik^shall be flagged  with  a "B" .
                                  '     '    "
                              _                  _  , ,
 22.6.5       Flag all instrument:, blank revolts "*8* '-/if the  instrument
             blank SMC does not~i®ftet theyJadvisory recovery of  50-150
             percent .            •>-'»   ---'J'

 22.6.6       If the instrument blank tjjSC recovery is less  than 20
             percen^yf;gce^aier than 200 ;j^ercent , or if peak interferences
             are prfesent* is^tple analysis^shall be stopped,  corrective
             action performefii, and another, instrument blank  shall be
             analyzed.  If tijife; SMC is still out on reanalysis,  corrective
             aastdon which m^i'incj^de^a ^^.new initial calibration shall be
             performed.   Al:l:^«S»pleSf;-analyzed since the last valid method
             or instrument blank shall be reanalyzed after a valid
             instrument blank has been demonstrated.
 22.6.7  .- ' "t'3Lf;';the RTS critl^iispn is not met for an instrument blank,
      ;   /•   sampl,e;1analyses shiijl be stopped and another  instrument
     A       blank fiiitaj.l be analyzed.  If the RTS criterion  is still out
  ,j , !        on reana^^is, corrective action which may include  a  new
 '">$'         initial ca^bration shall be performed.  DO NOT continue
-:%          with samplipanalyses until the RTS is within  ±1.0  percent.
 22 i^rfc/^.    Any sampleii?aiot bracketed by valid instument blanks  or a
       '%;  :-, valid ins?dSament blank and a method blank and  shall  be
                        at no additional expense to the Agency.
                             D-46-VOA-Q                           08/23/94

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                                                                          DRAFT

22.7  Documentation

      Instrument blank results  are  reported on Forms QI-VOA and QVI-VOA.
      Reporting requirements  are  listed in Exhibit B.

23    Laboratory Control Samples

23.1  Summary

      The QTM VOA LCS mixture initially will be, .supplied to contractors by the
      Agency.  The LCS mixture  will contain t&fget compounds at several known
      concentrations.  The Laboratory  shall spike  the LCS mixture into a clean
      matrix that is similar  to the samples Ibeing  analyzed.   The spiked matrix
      shall be prepared and analyzed using ithe procedures described for field
      samples.   Analysis of the LCS will assess the .performance of the
      analytical system prior to  analyzing field samples.

23.2  Frequency                                     'I  ,

      An LCS shall be analyzed  once ,per matrix per analytical sequence (24
      hours) per instrument.  Tb»^X£S^-^^ljt,^l3ft,analyzed after the first
      instrument blank in the inft^a.!  caTfbi?iit3^ai: analytical sequence or after
      the method blank in the daily =ealibratio&; analytical sequence.

      An LCS shall be analyzed  with each:   ,-.,"

      •     Set of water field  samples  (LGSJfprepared from reagent water);

      •     Set of soil/Solid BLe^-d samples (ILCS prepared with quartz sand);
            and      ;' '•          "  1;
                    '7
      •     Set of 611y field sastgles,  £LCS, prepared with corn oil) .

23.3  Procedure

      Spike the appropriate matrix  with the LCS standard mixture and prepare
      as follows.:-:'  -=           '" '*  ,,
      23.3,1      Water l^Sfeand Methanol Miscible/Aqueous Miscible  Oil LCS
            23.3.1.1    Allo|ir~;the LCS mixture ampules to  reach room
                        temperature before opening.  The  ampules must not  be
                        openeduntil preparation/analysis  is  to occur.
            ;  ,          ExersbiEse care in breaking the ampules open  to avoid
              "• "         injury.
                • *  * ••       ^
            23.3.1;2..  ],. Spike 2 mL of the clean reagent water matrix with  10
                      f J£L of the LCS standard mixture as  described in the
                        instructions provided with the LCS mixtures.   Use
                        syringes to perform the spiking to ensure accuracy.

                                  D-47-VOA-Q                           08/23/94

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                                                                    DRAFT

                  Prepare  as  described in paragraph 13 . 2 . 2 and proceed
                  with  the analysis as described in paragraph 14.

      23.3.1.3    Nominal  aqueous  LCS target compound concentrations are
                  as  follows:

                  Vinyl chloride            60. pig/L
                  1,1-Dichloroethene      380 jtg/L
                  cis-l,2-Dichloroethene  375 /tg/L         ':•
                  1,1,1-Trichloroethane ; ,500 Mg/L
                  Trichloroethene      ,'    40 ftg/L               '
                  Bromoform           '    500
                  Ethyl benzene        '     60
                  m-Xylene          ,      375
23.3.2      Soil LCS

      23.3.2.1    Allow  the  LCS mixture  ampules "£o reach room
                  temperature before opening.   The; ampules must not be
                  opened until preparation/analysis is- to occur.
                  Exercise4i$a«« ;,|h$ Breaking the ampules open to avoid
                  injury.  "V -       'i: "->" n, :< ••:    ,,.,

      23.3.2.2    Spike  1  g  of tihe clean; -quartz sand matrix with 10 jjL
                  of  the LCS standard (mixture  as described in the
                  instructions provided  with the LCS mixtures.  Use
                  syringes to perfotot the spiking to ensure accuracy.
                             describe*! lin paragraph 13.3.2 - 13.3.3 and
                  ,i^roceeicfeloroethene   750
                \- 1,1,1-Trichloroethane   1000
                  Ifeiphloroethene            80 /igAg
                  Brettoform               1000
                  Eth^tebenzene             120
                  m-Xy|ine                  750
            Oil LCS  (Mlfhanol  Non-Miscible and Methanol Mis cible /Aqueous
           . Non-Mis cibie)
                 sectn.cn has not been finalized.  The LCS composition
            and Concentrations for oils are currently being
            investigated.
                             D-48-VOA-Q                          08/23/94

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                                                                          DRAFT
            23.3.3.1    Allow  the  LCS mixture ampules to reach room
                        temperature  before opening.   The ampules must not be
                        opened until preparation/analysis is to occur.
                        Exercise care in breaking the ;ampules open to avoid
                        injury.                     : '

            23.3.3.2    Spike  6 g  of the clean corn oil matrixmLth  ????600
                        pL???? of  the LCS standard mixture as described  in the
                        instructions provided .with the LCS mixtures;;,  ,;Use
                        syringes to  perform ttie" spiking to ensure accuracy.
                        Prepare as described in paragraph 13.4.1.2 - 13.4.1.5
                        and proceed  with this analysis as (described in
                        paragraph  14.    ;! "

            23 . 3 . 3 . 3    Nominal LCS  target compound-concentrations are as
                        follows:
                        Vinyl  chloride           1200
                        1,1-Dichlagoethene       7600
                        cis-l,2-Iiciil«|rO|ftthene;   7500
                        1,1,1- Tr iSt&proetTi&rfe' *• :JU$©Q;
                        Trichloroetteae       , >:  8GV fig/kg
                        Bromoform   -Jj        ;f  10000 f*gAg
                        Ethyl  benzene : ;,    „:    1200 jtgAg
                        m-Xylene                 7500 jtgAg
23.4  Technical Acceptance
                        , ;     '  ' I ' ;l .          ,
      23.4.1      All>I*CS compouSis must have Recoveries between 30  and 110
                  percent.  Up tc^*wo LCS compounds may, however, exceed the
                        recovery;%Tif,er,ipn of 110 percent.
      23.4.2      All LCS;% target compound absolute and relative retention
                  times must^e within the windows established during  the
                  initial calibration.
      23.4,,3 :='  "'The;-;-iCC;<»,f  the SMC-
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                                                                          DRAFT

                  all associated field and QC  samples  shall be reextracted
                  and/or reanalyzed. If one  or two LCS compounds are outside
                  the recovery criterion, proceed with-'sample analyses, and
                  flag all sample results of those compounds that were out in
                  the LCS with an "L" flag.

      23.5.2      If the recovery of the SMC is  less than 20 percent,  greater
                  than 200 percent, or if peak interferences are present in
                  the LCS, sample analysis shall be stopped and another LCS
                  shall be analyzed.  If the L<*S SMC recovery is st£tl: outside
                  the criterion upon reanalysi-s, corrective action sna.il be
                  performed and the LCS and All  associated samples shall be
                  reextracted and/or reanalyzed.

      23.5.3      If the RT or RRT for any £6S..compound is not within the RT
                  and RRT windows established  discingthe initial calibration,
                  reanalyze another LCS.  If uponjseanalysis a compound is
                  still outside the windows, a new 'in.it:i.al calibration must be
                  performed before samples can be analyzed,.  The instrument
                  must be recalibrated as described in paragraph 8.
                                •tfc"'  f.; -y-f. -. * ",« »
      23.5.4      If the RTS criterion is; Wt?«et<'dSjtr  -fh& LCS,  sample analysis
                  shall'be stopped itttd another/Ishall lie L€S reanalyzed.  If
                  the RTS is still outside th«^criterion upon reanalysis,
                  corrective action which, may'sinclude  a new initial
                  calibration shall be performed.  DO  NOT proceed with sample
                  analyses until the RTS 'is  within ± 1.0 percent.
                          '•  '/
      23.5.5      Any ssmp'les processed withi«n  LCS that is out of control
                  (i^e», does no^jneet any of  the technical acceptance
                  criteria) shallf&fi reextracted and/or reanalyzed at no
                  Additional expepse to the  Agency.
                  ' - ' '"           p;;" 1-i.:"s; ;?;- ,; ^
23.6  Documentation    ; ;  :>-t.

      Laboratory Control Samples results are  reported on Forms QI-VOA,  QII-VOA,
      and QVI-^IA,.; "Reporting re^iaiirements are listed  in Exhibit B
            " * *   '     '            '  '
                                  D-50-VOA-Q                           08/23/94

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                                                                 DRAFT
LO-
            COLUMN RESOLUTION CALCULATION
                                               % Valley-x/y 100
 8:30
                   9*0
  8:50
Time
                                                        1CKOO
                              Figure 1
                             D-51-VOA-Q
                          08/23/94

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                                                                           DRAFT

                                       Table 1.

                         List of Volatile Compounds in Order of Elution*

                               Vinyl chloride
                               1 , 1-Dichloroethene
                               trans-1 , 2-Dichloroetfaene
                               1 , 1-Dichloroethane
                               cis- 1,2 -Dichloroethene            •
                               Chloroform       ;                   ~  ;'
                               1,1,1-Trichlorobthane
                               Carbon tetracKEoxide
                               Benzene     _;'' •"          ,;
                               1 , 2-Dichlor0ethane
                               Bromodichloromethane !'^
                               Toluene            ~ ;
                               Tetrachloroethene
                               Chlorobenzene            •
                               1 , l^>-2 , - Te tr achlor oethane
                               ortho-^flene     :
                               Bromof orm,
                               4-Bromofluoc^be'nzene (SMC)
*     This elution orde|f:is gi-^e4ias general :,guidance and is based on
      suggested  instiaaBental opeic«£ing conditiraas as given  in paragraph 7.
                     • if"            ''"",'"
**    Para-Xylene CoiQ-Utes  with jseiaj^Xy.lene .   The sum of both Xylenes will  be
      measured and'-«ill*be  quanjfcU^f«Si«^a34g the calibration factor of  the
      para isomer.     %;- -4
                                   D-52-VOA-Q                           08/23/94

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                                                                  DRAFT
                           EXHIBIT D   '.;         -




                   QUICK TURNAROUND' METHODS




ANALYTICAL METHOD FOR,: P.OLYNUCLEAR MIOMATIC HYDROCARBONS (PAHs)
                           D-1-PAH-Q                           08/23/94

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                                                                            DRAFT

                                TABLE OF CONTENTS
                       POLYNUCLEAR AROMATIC HYDROCARBONS

SECTION                                                                     Page

I     Introduction	,	D-3

II    Sample/Extract Storage and Turnaround Times
      and Equipment and Standards	s.«i	D-4

      1      Sample/Extract Storage and Turnaround Times	,!i.. .D-4
      2      Summary of Method	, i	D-4
      3      Interferences	,.;	D-5
      4      Apparatus and Materials	, ,.	,;	D-6
      5      Reagents	 .:,,„,,„	*,»	D-8
      6      Standards	'..,..,;	D-8

III   Instrument Quality Control Procedures  and Requirements.	D-12

      7      Instrument Operating .Conditions	' „,;,	D-12
      8      Calibration of the Qfi-.f^RB^tsit^.rli^itial Calibration	D-12
      9      Calibration of the GC-%stem ~'-'!^lLil*rat$»n,Check	D-17
      10     Calibration of the GC System  -  PVS^:-..'. A ...,	D-20
      11     System Performance - GC HesoluticaiT	D-23

IV    Sample Analysis and Compound Identification and Quantitation	D-26

      12     Summary	.,. »V;,^J	-, *	D-26
      13     Procedure,,,; .. '.'.',*:'::,,-,	,s*,,	D-26
      14     Extract Cleanup	,;»	:..,	D-31
      15     Instrumental Analysis,,	D-32
      16     Dilutitm^	^,» . ..,	D-35
      17     Identification of XaSTf^i?Ces^>qap»ds	D-35
      18     Calculations, ^	D-37
      19     Technical Acce|>1a||ttce Criteria	D-39
      20     Corrective Actionv,,,,»	D-40
      21     Dacia»emtsa.tion	.:. »,;.:»	D-41
              ' ,  ^ - ™' •  '* -           " V - .'
V     Samjile equality Contipci^. Procedures and Requirements	D-42

      Jgt''*'   Method Blank An|t|a?sis	D-42
      2§;    Instrument Blankr/i|inalysis	D-45
      :'t4 ?   Laboratory Contr^,' Samples	D-48
                                    D-2-PAH-Q                            08/23/94

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                                                                    DRAFT

                             SECTION I

                            INTRODUCTION
This Quick Turnaround Method (QTM)  is designed £br,«use in determining
the concentration of various polynuclear aromatic hydrocarbon (PAH)
compounds in soil/solid, water,  oil,  and wipe samples^  Exhibit C lists
the compounds that will be  determined by this method along, isith the
Contract Required Quantitation Limits (GIQLs).  The method yields
identification and quantitation of  the ;>aaalytes listed in Exhibit C
using single column gas chromatographyl'iflame ionization detector
(GC/FID).  Target compound  concentrations in samples are reported on an
"as-received" basis; no dry weights.are  calculated.  The primary
objective of this QTM is to provide assalyticaL,-
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                                                                          DRAFT

                                   SECTION II
                  SAMPLE/EXTRACT STORAGE AND TURNAROUND tIMES
                                      AND
                            EQUIPMENT AND STANDARDS
1     Sample/Extract Storage and Turnaround Times

1.1   Procedures for Sample Storage          ,,                     V

      Samples shall be protected from light-vaaad refrigerated at 4«C (± 2°C)
      from the time of receipt until  60  day£ after delivery of a complete data
      package to the Agency .             ;   ~,          ~ '•

1.2   Procedure for Sample Extract Storage    >  , .

      Sample extracts shall be protected from  light #tt4 stored at 4«C (± 2°C)
      for 21 days after delivery of a complete data paclcage to the Agency.
                                  ';';-.,
      Samples, sample extracts,  ;and ^standards  must be stored separately.

1 . 3   Contract Required Sample Turnaround Timeg        ;
      Samples shall be extracted,  analyzed,, ss& a summary of the analytical
      and QC data shall be reported to -the;;iappropriate EPA Region via
      telecommunications network within  48;;tiours (or 72 hours if more than
      three fractions are, aqaalipzed)  of Validated Time of Sample Receipt
      (VTSR) .  See Exba.lbl'ts A'^af^B for  specific instructions  concerning
      sample turnaround time andiijLata reporting requirements.
                     * '           -X-
                   ,  '            -'/•''•
2     Summary of Met&od          ,',„; Si  ,.,  , ,. ,,

2.1   This analytical meiEh,©d is  a  GC/FID method for the analysis of
      polynuclear aromatic (li^rocarbons  (PAHs)  in water,  soil/solid, oil, and
      wipe samples .  All targ^tSeompounds and the System Monitor Compound
      (SMC) shall- ifce -^solvent extisaotsed from field and QC samples followed by
                 c'oltHHB selean-up.  ''^ ,/
2.2   Sa^^le analyses shaft^je  performed using gas chromato graphic techniques
          dn a contract specified analytical sequence that shall not exceed 24
              Target compounlts,  are identified and quantitated on the basis of
              n time windowsj.,;«hd calibration factors established during
      ini*6iiai, -calibration.  JBaring initial calibration,  a mean relative
      reten-B-iJ^^^me (RRT) f'M mean retention time (RT) ,  and an identification
      window (i '&U$&8 RRT,;iaait  of the mean RRT or ± 1.0  percent of the mean
      RT) are establi^ae«l;fbr each compound.   Mean calibration factors are
      also established-sparing the initial calibration and the percent relative
      standard deviation  (%RSD)  of the calibration factors for each target
      compound and  the SMC must be less than or equal to 25.0 percent.  Sample

                                   D-4-PAH-Q                           08/23/94

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                                                                          DRAFT

      compound concentrations  are  calculated from the initial calibration
      using the average  of the three  calibration factors,  using the mid point
      calibration  factor (if it is within ± 10 percent of  the average of the
      high and low calibration factors) ,  or using line segments (K Curve).

2.3   A check of the  initial calibration shall be perifoiated no less than every
      24 hours by  the analysis of  the mid point standard,  ij&ll calibration
      factors calculated from  the  calibration check standard must be within
      ± 35.0 percent  of  the mean calibration factor calculated "£re '-a^iyaed ,_.»£,,,least once during each
      analytical sequence to verify instrument if»fcrf6riBaa.
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                                                                          DRAFT

      after samples with high levels  of  target  compounds or other interferents
      (see paragraph 23) .

4     Apparatus and Materials

      Brand names, suppliers, and part numbers  are  £or, illustrative purposes
      only.  No endorsement is implied.   Equivalent performance may be
      achieved using apparatus and materials  other  than thbsfe, specified here;
      however, demonstration of equivalent performance meeting tfee
      requirements of this SOW is the responsibility of the Contractor .

4.1   Gas Chromatograph - The gas chromatograjihy (GC)  system shall be capable
      of temperature programming and  flow control that ifCs stable throughout an
      analytical sequence.  The system shall  be suitable for splitless or on-
      column injection and have all required  accessories, including syringes,
      analytical columns, and gases.  All GC  carries: sgas lines shall be
      constructed from stainless steel or copper I3ti!ba,ng.  Non-
      polytetrafluoroethylene (PTFE)  thread sealants ,!«*«• flow controllers with
      rubber components shall not be used.               ;;
      4.1.1 Gas Chromatography Gs&SBapt: ;« -'Tjj5>> &ux, 9 -53  mm ID bonded phase
            silicone- coated fused '•sfcilica 'caflllU^y acolumn (Supelco SPB-5, J&W
            DB-5, Restek, or equivil«nt) .  A filffli tnl^kaess of 0.25 to 1.0 ^m
            is recommended.           .         I-

            NOTE:  The use of a guard coluaa' is recommended.

      4.1.2 Chromatography Befcector  - The ^ shall be equipped with an FID.
                       -:   '    '* . -«-;          vj
4.2   Data System - Jlhe GC shall ,l>e  linked to /a data system capable of
      integrating p^aik areas for:|my compound detected at or above one -half
      the CRQL, prowi-ding retentifepn.,,t,ime labeling, and relative retention time
      comparison.  :%£^;fcs  requi®e.Mi$at:S^e.Jliaboratory be equipped with a PC-
      or microcomputei>l»a$ed GC data collection and  reduction system for this
      purpose.  The Laboritfe^y, shall possess this equipment to provide the
      quick turnaround of el^etgronic data.   The Laboratory shall also be
      equipped-Ktifih-y^-microcomptrter ,and contract  specified hardware and
      software' -'to^ electronically tr«assfer  the QTM data to the Regions.
         /;" -,"            v'"l>
4.3   G^s^sware - Sufficiei^^lassware to  meet contract requirements shall be
               for exclusive^gise in  support  of this  contract.
                            '
       ,-^,1       ErlenmeyerJiFlasks  -  125 mL.
        ^1 .'.-.              /I
      4.3.2' \ r  Beaker  - /£&Q mL .

      4.3.3       feoi3een££4tor tubes  -  10 mL.
                     'v:'^v
      4.3.4       Kimax concentrator  tube  (graduated)  - 25 mL.
                                   D-6-PAH-Q                           08/23/94

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                                                                           DRAFT

      4.3.5        Graduated test tubes  - graduated from 1 to 10 mL.

      4.3.6        Autosampler vials - appropriate  for t"he GC system.

      4.3.7        Centrifuge tubes - 40 mL.

      4.3.8        Powder funnel - 6 cm  (60°).

      4.3.9        Chromatography column w/teflon stopcocks - 10ba|B,i.d. X 20
                   cm.                          ••                    *l' '. -
                                               ;                         \' -
      4.3.10       Pasteur pipets.

      4.3.11       Side-arm flask - 500 mL.';           .;

      4.3.12       Buchner funnel.            ''•*-..''

4.4   Laboratory Hardware - The following equipment' is required for sample
      preparation.                                      - •"• ,

      4.4.1        Ultrasonic Cel^;|j^Jrtjigtie9:>;,JHeat  Systems Ultrasonics, Inc.
                   Model  W-385 Soriieator''(&$'.fet-wifchpulsing capability, No.
                   200  1/2" tapped disrupter horti plttls So; 419 1/8" standard
                   tapered microtip pttfbe), or<*:equivalent device with a minimum
                   of 375 watt output capability.  The 1/8" microtip shall be
                   used for extraction of.all"soil/solid  samples.   (NOTE:   In
                   order  to ensure that sttffstcient energy is transferred to the
                   sample -during ,the extraction, the microtip probe must be
                   replaced if tfce,s;tip begins; to erode.   Erosion of the  tip is
                   evidenced by a'risough surface.)

      4.4.2       Balance - Calibrated and accurate to 0.1 g.
                   •<; .,..|         v:f !-'V'ii''".?;'!,!^5'
      4.4.3        Baiafnee r Calibrated and accurate to 0.1 mg.

      4.4.4        Centrifuge:- ,'

      4.4.5;,-:.  '?   Hiemsjrringe - i&r^fL,  50-^L, and 100-|iL.

      4.||^6        Spatula '^'Stainless steel.
      . .If              "     "':-^
     -4;lP4.7       Hot  plate sjtirrer.
     •:V--:C..                  J'
      4.4il^   ,    Teflon cospfed magnets.

      4.4.9    " 'ri'.feLass  wpoi.
                   -r i~. ,£::
      4.4.10      Whatswaci-#42  filter paper.

      4.4.11      Whatman vacuum holder.

                                   D-7-PAH-Q                           08/23/94

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                                                                          DRAFT

      4.4.12      Nitrogen blowdown apparatus.

      4.4.13      Water bath.

5     Reagents

5.1   Reagent water - Reagent water is  defined  as water  in which target
      compounds or potentially  interfering compounds  do  not produce a signal
      greater than one-half  the response  in the corresponding RKf ^window of
      the initial calibration low  concentration standard.  Reagent  water shall
      be generated by one of the following methods.                      ;

      5.1.1 Reagent water may be generated "by passing tap  water through a
            carbon filter bed containing  approximately ;SOO g  of activated
            carbon (Calgon Corp.,  Filtrasorb-300, or  equivalent).

      5.1.2 Reagent water may be generated using a water purification system
            (Millipore-0-Plus with Organex Q cartridges, or equivalent).

      5.1.3 Reagent water may be prepared by boiling  for 15 minutes then
            bubbling contaminant-:!?see jiwsrt =gas through  the water for one hour
            while maintaining the'"v-s*ater tenrplkcittars at 90°C.  While still hot,
            transfer the degassed  water to a n«trow~i»oiul2i  screw-cap bottle,
            seal with a Teflon-lined septum,  and cap.

5.2   Solvents -  Acetonitrile, hexane  (BV gfcade), methanol,  methylene
                  chloride,  acetone (CAP -K3G grade), and  isoctane.

5.3   Sodium hydroxide solutioTt,r|0.5 N).

5.4   Sulfuric acid &iolution(0.5 |Sf} .

5.5   90:10 Methylene'«hloride/a4et3^n»  solution.

5.6   Silica Gel 100-200 mesa grade 923.

5.7   Sodium Ssdfarte,,           •=:,'-.
            *3 '*, " '     *   --" .         " "-;
5.8   Soditar Chloride.

5.9   Qtti oil.               ---:
6.1   Stock'-Sirdard

      Stock soluti:o^s:,ma,vt1>e prepared from pure  standard materials or
      purchased as certified solutions.   Standard  solutions  shall be prepared
      by dissolving pure" standards  in a  suitable solvent in  volumetric flasks.
      The addition of Toluene may be necessary to  dissolve some  of the target

                                   D-8-PAH-Q                           08/23/94

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                                                                          DRAFT

      compounds in highly concentrated stock standards.  When  compound purity
      is assayed to be 96 percent or greater, the weight may be used without
      correction to calculate the concentration of the stock standard.
      Exhibit E, Section V provides further directions for preparing and
      verifying the integrity of stock standard solutions.

6.2   Secondary Dilution Standards                 .'      , .*

      6.2.1 Using stock standard solutions, prepare secondary  idiitation
            standards in methylene chloride.  .,  -,-

      6.2.2 Secondary dilution standards shall be stored at 4°C (±  2°C) with
            minimal headspace and checked frequently for-,signs of degradation
            or evaporation.  These procedures are important, especially just
            prior to preparing calibrationmtandardsffirom the  dilution
            standards.                         ?  ,/••-;'

            NOTE: Standards shall not be stored in volmetric  flasks,
            especially when they are prepared with solvents with low boiling
            points.
                                      i
                                i  .•"' • •>,!  •••'  -,- - „„
6.3   Calibration Standards        r         r ,<_ , ,   ,

      6.3.1 Calibration standard mix'fcmres shall, he prepared at three
            concentration levels in volumetric flasks and diluted to final
            volume with hexane.  The low /concentration standard as  specified
            in paragraph 6.3.2, achieves'tfee sample extract compound
            concentrations equivalent to the-sample compound CRQLs  as  listed
            in Exhibit *8 -(see -paisagraph 14.9Ji  The high concentration level
            shall bej%mar the up^r end of the,.linear range.   The compounds
            and concsmtrations uSfftd for these calibration mixtures  are
            presented in paragra^fi,6.3V2. .JJOTE:  The high level standard
            concentrations are tiie:miniffixait required under this method.  The
            Laboratorjr%sy-,s;prepare standards at higher concentration levels as
            long as the %KSB^criteria are met.
                                   D-9-PAH-Q                          08/23/94

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                                                                           DRAFT
      6.3.2 PAH  calibration standard mix concentrations.
Calibration Ranges

Compound
                                              Low
:Hid
High
Naphthalene
Acenaphthylene
Acenaphthene
Fluorene
Phenanthrene
Anthracene
Fluoranthene
Pyrene , ;
Benz (a) anthracene
Chrysene
Benzo(b)fluoranthene *
Benz o ( a ) pyr ene
Indeno (1,2,3- cd) pyrene
Dibenz ( a , h) anthracene
Benzo ( g , h , i ) pe^3Je^f *
2 -Bromonaph thalei?fi (SMC) s
2.0
2.0
2.0
2vQ
£.0
2-0
: 2.0
2.0
:2,0
2*0:
2.0;
2.0
2.0
2.0
,2-0
'J2.JO -
,. 20 r
20
20
20
20
20
20
120
;120
• 20
20
20
2®
20
20
20
100
: 100
' IDS'- >
100 \
100
100
100
100
100
100
100
100
100
100
100
100
                  *      Coelutes wit&rbenzo(k)Jrluoranthene,  quantitate the
                         total in terms of tbfe-'-b isomer.

       6.3.3      All  standards shall be'-.stored at 4«C  (±  2°C)  in Teflon-
                  sealed jglass bottles .   Calibration solutions  shall be
                           'aiftrekjjB months, oarssooner, if comparison with check
                             indicates a problem.

6.4   CalibrationJ&eck Standard,^'; ,  ,„,„,.  „
                  * -  -e<\ , ,         ,-if 'if- " ij""-r'' -'•  r'j~
      The calibration  clbefelk, is a daily one-point check  on  the initial
      calibration.   The cajilsxation check standard shall be  prepared in a
      volumetric flask and dliJ^ifced to final volume with hexane.   The
      concentisati-brnjiof, the calibration check standard is the same as the mid
      level-'isdaridara:'ttietl, in the iiiitial calibration.
6.5   Syssjsem Monitor
                            -
          System Monitor  Con^kond (SMC), 2-Bromonaphthalene,  shall  be employed
     'v%od|j|etect shifts  in re|SBntion time of eluting compounds.   Additionally,
      the'-lis^JBe. compound shalp-:be used to monitor the extraction efficiency.
      The Lai^iolcjstory  shall^apepare a solution in methanol  containing 2-
      Bromonaplil^lbene  atjiisi-'concentration of 2 mg/mL.  The Laboratory shall
      add 10 /tL of Mt^s /standard to a 100-mL water sample,  or 10 pL to 6 g of
      soil/solid sample,;"For oil analysis, prepare 2-Bromonaphthalene at a
      concentration of  200 /tg/mL and add 1 mL of this solution to 1 g of oil
      sample.
                                   D-10-PAH-Q
                                                     08/23/94

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                                                                           DRAFT

 6.6   Performance Verification Standard

      The  Performance Verification Standard (PVS) shall.be analyzed at least
      once during each analytical sequence to assess system stability.  The
      PVS  is  two times the concentration of the IpwJLiflrel calibration
      standard.                                     -; \-  ...

 6.7   Laboratory Control Sample                             ,:i  .

      Laboratory Control Samples (LCS) contaioisg known amounts oS'ifairget
      compounds  traceable to primary standards fwill initially be supplied by
      the  Agency.  Following receipt of thes«'initial supplies, however, the
      Laboratory shall prepare its own LCSjiitandards. ^The LCS shall be spiked
      into a  clean matrix and prepared usiijg all steps|iof this protocol.  An
      appropriate  amount of the LCS shall -feec'^added tao jreagent water and
      analyzed with  each Batch of water samplteSi, ,Aa-^appropriate amount of the
      LCS  shall  be added to clean quartz sand ami; analyzed with each Batch of
      soil/solid samples.   An appropriate amount of-t^ LCS shall be added to
      clean corn oil  and analyzed with each Batch of oil ismmples,   If a Batch
      contains water,  soil/solid, -and oil samples,  an LCS :-«shall be prepared
      and  analyzed for each matrix;",  •$&$&}; •-.fb* Agency will provide the
      laboratory with further ins"'6l*ctioris'"'&wi;-fihei»'yj^paxation and analysis  of
      LCSs  for wipe samples.)  All^iGS compo\xa&&must?i*i*re recoveries between
      30 and  130 percent before sample .-.analysis may begin (see paragraph 24).

      NOTE:   The Laboratory is expected -to"asaintain control charts of the
      recoveries of at least three repres^ative LCS compounds as an internal
      QC procedure.      ( -•:••", ;-,           ': '•;:
                       •'"' ;        ' ^
6.8   Storage of StaiSiitrd  Soluti

      f O          "'''            **"•
      6.8.1 Stock, secondary stasjfard,,,solutions,  and working standard
            solutions .afeall be i^-M'Sst-ii^P' (±  2«C)  in Teflon-lined screw-cap
            amber bottl-asi 
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                                                                          DRAFT

                                  SECTION III

            INSTRUMENT  QUALITY CONTROL PROCEDURES AND REQUIREMENTS


7     Instrument Operating Conditions

      The following  are the suggested gas  chromatographic analytical
      conditions .                                                '  -

      Column:     J&W DB-5 (or equivalent),  15fm x 0.53 mm ID, 0.25 to 1.0 /m
                  film  thickness  fused siliea capillary columns (FSCC) .

      Carrier Gas:                        •',    Helium :;,
      Flow Rate:                           ;    ,;5-7 mL/jSln
      Injector Temperature:                    ':2$Q°C:
      Detector Temperature (FID) :              3D&<>C
      Initial Temperature:                     75°C   ,   -,
      Initial Hold Time:                       3 min     ;-
      Ramp Rate:                   ,.           12°C/min
      Final Temperature:        .' :' ,4.  , ;  : >  280° C
      Final Hold Time:            ' :        • "•'•'& min ' ,  -
                                   *,            ,           f

      The FID requires  hydrogen and air supplied to the detector according to
      manufacturer's specifications.    >

      NOTE: The typical run time  under these conditions is 25 minutes.  It may
      be necessary to adJxast-SC^ conditions ;on individual instruments to
      optimize compound aseparat&fti-   It may<->be necessary to adjust detector
      conditions to  :0p>i:imize instrument sensitivity.

8     Calibration jaifcthe GC Svstaegi.-  Initial Calibration
                   . , ^^           ^ ^ts ,-  ^  <~ v - ''--s
8.1   Summary           ' ;::  ,,
      8.1.1 Prior to  the  analsjs^i^ ,of samples and required blanks, each GC
            system ipust be  initially calibrated to ensure that the instrument
          „' "HB&ets " tlbie'J^^simum perf&nBince requirements of the method.  The
         f.^.1 "initial calilsic^ion is  accomplished by analyzing three standards ;
       ,, K-  the low level, 'aKt-d level,  and high level mixtures as specified in
      ,; .':": ':•   paragraph 6.3.2;|,J,The technical acceptance criteria for the
      f',,   initial calibration are given in paragraph 8.5.  The initial
      •!  \ti , , calibration shal^Gbe used to establish the calibration factors
         "-  3sps,ed for  compouaii;;quantitation, to define the retention time
           'Wife&aws for compound identification, and to determine the mean SMC
            reteastiipn timc^for evaluating SMC RT shifts during analyses.
            Detector, JiJeg^Onse must  be linear for all target compounds .  All
            samples shall be analyzed during the contract specified 24-hour
            analytical sequence .
                                   D-12-PAH-Q                          08/23/94

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                                                                           DRAFT

      8.1.2  Sample  quantitation shall be based on the mean compound
             calibration factor, line segments ("K" curve),  or  the mid level
             calibration factor from the initial calibration (The use of the
             line  segment or "K" curve is suggested).  &11  field and QC samples
             and standards within a Batch and all field and QC  samples and
             standards  analyzed in the same analytical .s"tiie -,SK.C
             recovery is greater than or equalitb 10 percent  and less than or
             equal to 200 percent.           'i,''.
                                           - ' S* *'
      8.1.4  Compound identification shalltfee based on-absolute retention time
             windows  established during initt^, calibration in  all field
             samples  where the SMC recovery isljtss-s .tfggan 10 percent,  greater
             than  200 percent,  or if peak interference are  present.

      8.1.5  Shifts  in  the chromatographic peaks shall *§e-~$valuated by
             comparing  the RT of the.;,.SMC in all analyses wlt% the mean RT of
             the SMC  calculated £ae^->£|^iijai.|jjaj. calibration.' The retention
             time  shift is referreijlftp as"f'T£T^»1:-^i-': 5v ,        -i;---«:'
      8.Z^2:An analyticall|is«quence is a contractually defined sequence of GC
        ;?;:  analyses which'lisensists of an initial three-point calibration or a
      ,, ftf   valid calibratio^check,  field samples,  LCS, method and instrument
     |<- :    blanks, PVS, and|^,ther QC samples run within a 24-hour period (see
     ' ^ *f*^~paragraph 15 for^phe required sequence of samples).

      8.2.3v«akly,sis of the.jisiitial calibration shall begin with the  injection
            of ifeellxigh Iflffel  standard followed by the mid level and  low level
            standstills, ,,'W,
                      ;
      8.2.4 The analytical sequence concludes  with an acceptable analysis  of
            an instrument blank and a PVS  (see paragraph 10).

                                  D-13-PAH-Q                          08/23/94

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                                                                          DRAFT

      8.2.5 Samples shall be  analyzed  only after meeting the technical
            acceptance criteria for  the  initial calibration or a valid
            calibration check standard.

8.3   Procedure

      8.3.1 The GC system shall be set up per the requirements of paragraph 7.

      8.3.2 Prepare calibration standard solutions containing the SMC and all
            target compounds  using the procedure listed in paragraph 6.. 3.

      8.3.3 The calibration solutions  shall:-i>e equilibrated to ambient
            temperature before injection (approximately:;! hour).

      8.3.4 Inject between 1  and 5 /*L  of ea'calibration standard.  The same
            injection volume  shall be  used fox a'llrleaiibrations and field/QC
            sample analyses.

8.4   Calculations                                      :';

      8.4.1 Calculate the calibrat&«lj4^&fc8^,ifeatio of the total peak area or
            height to the mass injected) '"for^eaeih iitiargst; .compound and SMC in
            the three initial calibration staiaiard "'analyses using equation.D.I
            (EQ. D.I).              :
             Calibration factor =  Total Area^f Peak ox Peak Height        EQ. D .
                            ;, :,          Mass .injected (ng)
                                              "
      8.4.2 Calculate the mean oa^|p3Xatio,n .factor for each target compound and
            the                              '
      8.4.3 Calculate the HEgSB of the  calibration factors of the low level,
            mid level, and h'frgh: -level  standards  for the initial calibration
                      following «ijsaation .


                                                               EQ. D.2
          ,%
        '!•;• '''ii»feere SD - standard deviation.
           '^- - J 'A.           .. ~: •*
            Stalaiiard devist^ion is calculated using the following equation:
                                  D-14-PAH-Q                          08/23/94

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                                                                            DRAFT
            where:   x^ = individual calibration factor (per compound).

                     x  = mean of three  initial calibration factors Xper
                          compound).

                     N  = number of calibration standards.

            Equation D.4 is the general f^mula for tbie mean of  a set  of
            values.                         -'- .:"; -,-     <• .
                                       v xi          ,:          EQ. D.4
            where:   X  •= mean of vsatfues.  "'"'-'L-       , ,

                     X^ = value.     •','       -"•>'

                     N  = number of values, '  '

      8.4.4 Calculate the: IBEf^por each  targel:  compound using the  following
            equation: „- --;    '  •> j,'-          « -
                     ^**"'          '^;"           '':'  -:
                                                                  EQ. D.5
      8.4.5 Calculate the'a^a^ RRT and RT  for each target compound by using
            equation D.4.    '-/'*".',•-
8 .5   Techjjiigia.5' licceiptsfBpjoe,, Criterifc..-;
      SjSlil The  %RSD of thfeSpalibration  factor for each target compound and
      ,  ;'   the  SMC in the ijittial calibration must be less than or  equal  to
      •^.4    25.0 percent.   Up^sto two target compounds may exceed 25.0 percent
      ':-,i|! ->, RSD, however,  all compounds  must be less than or equal to 40.0
                     RSD.    ,?M
      8.5.2 The^ir^fceaation.'l^me of the  SMC  in each standard must be within ±
            1.0 perferist-.^ffthe mean retention time calculated from the  three
            initial calibration standards.
                                   D-15-PAH-Q                           08/23/94

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                                                                          DRAFT

      8.5.3 The peak resolution between phenanthrene  and anthracene,  and
            between indeno(l,2,3-cd)pyrene and dibenz(a,h)anthracene  shall be
            evaluated in the low level initial calibration standard before
            proceeding with sample analyses  (see paragraph 11 System
            Performance - GC Resolution).

      8.5.4 The chromatographic peak response for all target compounds in the
            low concentration standard must be greater than <1Q -percent of
            full-scale deflection.                                ;,

8.6   Corrective Action                      ;                            '

      8.6.1 If the %RSD for more than two compounds in,$r$ceed with sample analysis until
            the RTS is within ±1.0 perceat.

      8.6.4 If the peal: respori&ejfor any tarjgset compound in the low
            concentration standai&d\ is not greater than 10 percent of  full-
            scale deflection, thccfikaboratory shall perform corrective action
            and make appropriate Adjustments _ before sample  analyses are
            started*, /to ensure ?'£&^*^Xk $gbirget compound peak responses in the
            low concehtarjaifcipn standard are greater than 10  percent of full-
            scale deflection; ,;.
      8.6.5 C^rr^clSlve,,action may! include optimizing  FID detector linearity by
          ,,
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                                                                          DRAFT

8 . 7   Documentation

      Initial calibration results are reported on Forms QIVA-PAH, QIVB-PAH,
      and QVI-PAH.  Reporting requirements are listed in Exhibit B.

9     Calibration of  the  GC System -  Calibration Cheek

9.1   Summary

      A check of  the  calibration curve shall toe -performed at the beginning of
      every 24 -hour analytical sequence that ,jpcludes field sample analyses.
      This check  of the calibration shall be ^performed 'using the mid level
      standard  and  shall  contain all  target ^compounds and the SMC.  The
      percent difference  (%D)  between thejSscalibration,|£actor in the
      calibration check standard and  the average calibration factor from the
      initial calibration is calculated for esri&^tatget compound and the SMC,
      and must  meet the technical acceptance crita33;I,a,,given in paragraph 9.5.
      The SMC retention time shift (RTS) and column resolution must also meet
      technical acceptance criteria as stated in paragraph ;-9 . 5 and paragraph
      11, respectively.   Only after^-all these criteria are?fflet can sample
      analysis  begin.            -   <'l  ,£•  ,%

      NOTE:  Compound identification  and quantisation -snail be performed based
      on calibration  factors and compound RT =sad RRT windows established
      during the  initial  calibration.  -:       :

9.2   Frequency                          '  ;

      9.2.1 Each  GC used  for analysis  shall be. checked to verify the initial
            calibrat^efe for each ~'2fc- hour period -,-of operation.   This procedure
            is  to eosiire  that the Instrument continues to meet the instrument
            sensitaivijty and linea^ijtjy,, requirements of this method.
                     •t<* :."       *-' ,.Jfe^B\  -X '{'"
      9.2.2 An  analytical Sequence  is  a contractually -defined sequence of GC
            analyses which'Wc&nsists of an initial three -point calibration or a
            valid calibration check standard,  field samples, LCS , method and
                       blanks,  ?¥§£,,. .and other QC samples run within a 24-hour
                        tpar agraph
         .,.,..                 .,
      9. ,213 The analytical 'Sequence  shall be concluded with an acceptable
       ,„"--   analysis of an  instrument  blank and a PVS (see paragraph 10).
      '£' \.                    :'-~l:
            Samples shall be :ajialyzed  only after meeting the technical
          ,'-  cceptance crite£f&  for  the  initial calibration or a valid
                        cheese standard.
9.3   Procedure    ^ ,'.$..£ ''
                     "'Si!-",'5

      9.3.1 The GC system shall be  set  up  per the requirements of paragraph 7.



                                  D-17-PAH-Q                          08/23/94

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                                                                          DRAFT

      9.3.2 Prepare calibration check standard solutions containing the SMC
            and all target compounds  using the procedures listed in paragraphs
            6.3 and 6.4.

      9.3.3 The calibration solutions shall be equiliMrated to ambient
            temperature before  injection (approximately labour).

      9.3.4 Inject between 1 and 5  (iL of the mid level calibration standard.
            The same injection  volume shall be used for all calibrations and
            field/QC sample analyses.          .                   '

9.4   Calculations                          ,;
                                            's
      9.4.1 Calculate the  calibration facicji: (ratio ojf-'ihe total peak area or
            height to the  mass  injected)  fesr-«ach taa^get compound and the SMC
            in the calibration  check  standard'-aEx using the following
            equation.
             Calibration Factor = •*P**j&M of. *?** ° fea* S&i9ht        EQ.  D.6
                                                      (ng)
      9,4,2 Calculate the  %D between the ".calibration factors from the
            calibration check  standard  and-the average calibration factors
            from the irubfci&l; tiali.br ati on usii^g the following equation.
                                                                  EQ. D.7
                  where,  "  -  -

                 •jjfc- ««.  mean  of ;€^ree  initial  calibration factors (per
                    -  -^ caompound) ."•;•'

                            L&ration  factor  from current calibration check
                        stanssird  (per  compound).

9.5  ^ejltoaical Acceptance  Criteria
      9.5.1 TQa^JiH) between >t$fi  calibration  factors for each target compound
            and fee:;iSMC rrtitrhe  calibration  check standard and the mean
            calibraitl.0i*;>i|£ctor  for  that compound in the initial calibration
            must be wit^dBa ±  35.0 percent.   Up to two  target compounds may
            exceed ± 35.0 %D, however, all  compounds must be within ± 45.0 %D.
                                   D-18-PAH-Q                          08/23/94

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                                                                          DRAFT

      9.5.2 All target  compound absolute and relative retention times must be
            within  the  windows  established during the initial calibration.
            Report  calibration  check RT and RRT data on Form QI-PAH (see
            Exhibit B) .

      9.5.3 The retention  time  of the SMC in the calibration check standard
            must be within ±1.0 percent of the mean SMC 'retention time
            calculated  from the three initial calibration s6ariptords .
                                                                 "i
      9.5.4 The peak resolution between phenanthrene and anthracene:;,', and
            between indeno(l,2,3-cd)pyrene anj
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                                                                          DRAFT

9.7   Documentation

      Calibration check standard results are reported  O«L Forms QI-PAH, QV-PAH,
      and QVI-PAH.  Reporting requirements are  listed  lii Exhibit B.

10    Calibration of the GC System  - Performance Verification Standard (PVS)
                                                            Ks;
10.1  Summary                                                :

      A PVS shall be analyzed at the end of every  24-hour analytical sequence.
      The analysis of the PVS shall be started *within  24 hours after "the
      injection of the first initial calibration standard or the instrument
      blank analyzed before a valid calibration check  standard.  The PVS is
      two times the concentration of the low level standard from the initial
      calibration (see paragraph 6.3.2).   '•    ,,

10.2  Frequency

      An acceptable PVS must be analyzed at the conclusion ;;«f the analytical
      sequence.  The PVS analysis^shall be started within 24 iiours after the
      injection of the first ini^ial-.l'esiiaJkKa.tion standard or the instrument
      blank analyzed before a val'S^L ;caiibra^i«ollect data under the current
      calibration until the conclusion of the current  24-hour sequence.  If at
      any time an unsuccessful PS^SJ^ana^s^s^is  made, the Laboratory shall stop
      sample analysis.and immedS^^I^^CH^pp^ze the PVS.   If on reanalysis the
      PVS is still outside *QC criteria, the Laboratory shall take corrective
      action and recalibratelithe GC (run a new  initial calibration) prior to
      reinitiating sample analyses,.  Recalibration will  begin a new analytical
      sequencer ,;  ly   _         --.-.' '«.

10.3  Procedure         • = *' v
        Xv              '!;?L
                           '••'A~ ',
      £0.3.1      The GC comitions shall be the same  as those used for
     .••''';          analyzing staples.
     '•^--Vr                 ;,;'
      10 .'3^!2 [,*    The PVS ij£:1t3wo times the concentration of the low level
            : ^i ii  standard,i£xx>m the initial calibration  (see paragraph 6.3.2).
               W <;          ,:- '

      10.3.3      The"P-VS 'solution  shall be equilibrated to ambient
                  temperature prior to injection (approximately 1 hour).


                                  D-20-PAH-Q                           08/23/94

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                                                                          DRAFT

      10.3.4      The same injection volume  shall  be used for all field and QC
                  samples and standards  including  the PVS.

      10.3.5      The recovery of each compound and the SMC in the PVS is
                  quantitated using the  mean calibration factor,  the mid
                  point, or by using a K curve  established, during the initial
                  calibration. (NOTE:  Only  one method of'fquantitation shall
                  be used for analyses within a given analytic.*! sequence and
                  for a given Batch of samples.)                "<,.=;

10.4  Calculations                            ^
                                           t',/--
      The amount of PVS compounds and the SHC recovered'sshall be calculated
      using the following equations:     -V.;;             ~:

                            Amount Observed  = '—-"  "\            EQ- D-8
      where:      A,,    =     are*.%ox peak height  of the PVS compound or SMC.
                   A             ^ ' - ; .. jfa j-       '-'
                                ct,:;f' -&\$: •'<&'*.
                  CFm   -     calibration "'faetfesie-sfcablished by one of three
                              techr&fues during tSie imtiial calibration.
                                    ,
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                                                                          DRAFT

      10.5.5      The RTS for  the SMC  in  the  PVS  must be within ±1.0 percent
                  of the mean  SMC RT calculated from the initial calibration.

      10 . 5 . 6      The peak resolution  between phenanthrene and anthracene ,  and
                  between indeno(l,2,3-cd)pyrene  and dibenz(a,h)anthracene
                  shall be evaluated in the PVS before -piroceeding with sample
                  analyses (System Performance  -  GC 'Resolution,  paragraph 11).

10 . 6  Corrective Action

      10.6.1      If recovery  of a PVS compound is not within 75-125 'percent
                  but still within an  expanded  recovery window of 50-150
                  percent, flag the outlier; compound "F" ;in all associated
                  field sample results generated  since:xthe last valid PVS,
                  initial calibration, or v«3,3-'d cali&sation check standard.

      10.6.2      If any PVS compound  is  outside  the expanded range,  the PVS
                  shall be reanalyzed  immediately.  Ijf, on reanalysis,  any
                  compound is  still outside the expanded ^recovery range, stop
                  sample analyses^.-jjerform corrective action,  run a new
                  initial calibi
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                                                                          DRAFT

                  a new analytical sequence.   All samples analyzed since the
                  last  valid PVS,  initial calibration or a valid calibration
                  check standard shall be reanalyzed witMn a valid analytical
                  sequence.

      10.6.6      If  the peak resolution criteria are ««t-:met, the Laboratory
                  shall perform corrective action and demonstrate adequate
                  resolution before samples can be 'analyzed (.see. System
                  Performance -  GC Resolution,  paragraph 11).   ;   k-
                                              * <
      10.6.7      If  all PVS criteria cannot be met  after having taken:;
                  corrective action,  reanalyze (do not re-extract) the
                  associated field samples in another valid analytical
                  sequence.   If on reanalyses all QC sample criteria are met
                  and the PVS criteria stiMisannot  Jtee>rmet, then submit all
                  sample data from both sequences^ , -J02ie Laboratory shall
                  describe in the  Batch narratives-tile .problems associated with
                  the PVS and how the field sample matrix may have affected
                  the PVS analyses.   If the Laboratory "can .demonstrate that
                  the problems are ,due to matrix effects, then both sequences
                  are billable.
      10.6.8      If a  PVS  reanalysls .is required be
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                                                                          DRAFT

11.2  Frequency

      11.2.1      Initial calibration  - The peak  resolution for phenanthrene
                  and anthracene, and between  indeno (.1*2,3-cd)pyrene and
                  dibenz(a,h) anthracene indicated in paragraph 11.4 shall be
                  evaluated in the  low initial calibration,standard before
                  proceeding with sample analyses,
                                                               -4

      11.2.2      Calibration check standard - The peak resolution for
                  phenanthrene and  anthracene^,. and between indeno (L,2.r 3-
                  cd)pyrene and dibenz (a,h) anthracene  indicated in paragraph
                  11.4 shall be evaluated £02?; each valid calibration check
                  standard before proceedia^-with sample ^analyses.

      11.2.3      Performance verification-*«Sa»idard^f  The peak resolution for
                  phenanthrene and  anthracene-'-jiml;iafetween indeno(1,2,3-
                  cd)pyrene and dibenz(a,h)anthracene  indicated in paragraph
                  11.4 shall be evaluated for  each WS'stiiat is analyzed in a
                  valid analytical  sequence.            ''" '•',
                                 <-£?5>,,' * ,
11.3  Calculations              ;
                                  j ' ',            V  $ '   • -.-.  \
      Determine resolution by  calcutating  the ^arcent' valley between two peaks
      using the following equation (see  f igujse'tl) .
                               Height of £b&-valley between
                                        ) an3,
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                                                                          DRAFT

      11.4.3      Performance verification standard - The percent valley must
                  be  less  than or equal to 45 percent between phenanthrene and
                  anthracene  in the analysis of the PVS,.  The percent valley
                  must be  also less than or equal to 45, percent between
                  indeno(l,2,3-cd)pyrene and dibenz(rocee1ling;|^ith?|sample analyses.

      11.5.3      If  the percent val'lfy for thef:PVS does not meet the
                  technical acceptance .criteria indicated in paragraph 11.4,
                  the PVS  shall be immediately reanalyzed.  If after
                  reanalysis  the PVS percent resolution is still outside
                  criterion,  
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13
                                                                          DRAFT

                                   SECTION IV

         SAMPLE ANALYSIS AND COMPOUND IDENTIFICATION AND QUANTITATION
12

12.1  This method  is designed for use in the rapid analysis^of >;water,
      soil/solid,  oil,  and wipe  samples for the target compounds*;fisted in
      Exhibit C.   If upon inspection of a sample the Contractor suspects that
      the sample is not amenable to  this method, contact the Regional IfO or
      the CLASS contractor for instructions£  For Superfund emergency removal
      actions, contact  the Regional  TPO orj-^jbe Headquarters APO for
      instructions.  If,  for emergency response actioxssi the TPO or APO are
      not available, contact the Regional ^iSeene O&Srdinator (OSC) for
      instructions.  The  Laboratory  must remeafeer--ttiSCC it shall follow the
      requirements in this SOW without deviation.;  "H

12.2  Before samples or required blanks can be analyzed, :i:he instrument must
      meet initial calibration orpwj.id calibration check 'Standard and column
      resolution technical acceptarjife^s^yiit^ria.  All sample extracts, required
      blanks, LCS, PVS, and calibration st:a«daMs;:,sital|. be analyzed under the
      same instrumental conditions apd shall be allowed ;to warm to ambient
      temperature  (approximately 1 hour) before preparation/analysis.
                                            * "••
12.3  Blank samples, such as trip blanks .and field blanks, supplied by the
      Region and included with a batch of field samples shall be prepared,
      analyzed, and Tepat£*&.-J$B,,-a. water sample.  Occasionally, a water QC
      sample (e.g. , fisSia. and':tii|p; blanks) «333. be included with a batch of
      soil samples.  '3ijE the labo'^&.ory is not'certain whether a water sample
      associated wit&Ja batch of isoil samples is a QC sample, contact the
      Regional TPQfior the CLASS  4||atrae;|;or! .„ ,„
      NOTE: If water blsa!iss,j>rovided by the Region,  such as trip and field
      blanks, are include'3,;,J|t a batch of soil samples,  the laboratory is not
      required to prepare  an'dMJfa^JLyze an associated water method blank or a
      water
12.4  If aaiasual or high -iamcentration samples are received, see Exhibit D,
      Appendix B for general; guidance  on screening and sample preparation.
        ' '
           _
13.1  Phale;;J^|>aration      $'>

              "• «^ * * '' „        -'^ 'tC1""
      Multi-phas3^ samples'; -&hall  be phase -separated into their individual
      phases.  The^{fca»f; Reparation techniques employed will vary according to
      the types of saafklell received.   Since it is impossible to know the
      number  and types  o'f  phases  that will be present in a sample, the choice
      of phase separation  techniques is left to the discretion of the analyst.

                                   D-26-PAH-Q                          08/23/94

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                                                                           DRAFT

      Various techniques can be employed to separate the phases.  These
      include pipetting off liquid phases (decanting should not be done) ,
      centrifuging  to remove suspended solids,  and use of spatulas to remove
      solids (wooden tongue depressors work well).  Whenever possible, phase
      separation operations should be done with disposable glassware.  The
      phases should be separated into glass containers with teflon- lined  screw
      caps .  This allows for storage and handling of the waste in a safe
      manner.                                                 ,  ;

      13.1.1      Samples received containing Multiple phases suchSias swater ,
                  oil,  and soil/solid in the .jsame sample jar shall be '"fhase
                  separated" into individual-jphases .

      13.1.2      Each individual phase isfrtaken through the procedure as a
                  subsample.  Report analytical ^ result^ for each sample phase.
                  Note:  Each multi-phase samples: .^haJ3.- be identified using the
                  EPA sample number convention f ox anilti -phase samples as
                  specified in Exhibit B.

      13.1.3      Do not analyze amy .phase that represents less than 10
                  percent of the-^teagt'/s^tole volume.
                                  ^     *x' ' '     '   •
      13.1.4      In  the  following fnspcedures , jsjiiere --applicable, references to
                  "samples"  explicitlt^mean "single phase units."

13.2  Sample Preparation  and Extraction - ilfter  Samples

      A 100 mL aqueous  sp|>ie;£s serially extracted using two 10 mL portions
      of methylene chloride"  (MeCS^) .   Extractions are performed in 125 mL
      Erlenmeyer flasjfa^ with a m^ietic stirring bar.  One gram of NaCl is
      added to the a^aeous sample; ,:j minutes after the first methylene chloride
      extracting solvent  is  adde
-------
                                                                           DRAFT

      13.2.6      Add  1 gram of NaCl to  sample during stirring and  stir for an
                  additional 3  minutes .
      13.2.7      Remove  stir bar  and allow aqueous and MeCl2 layers  to
                  separate.

      13.2.8      Transfer the MeCl2 by pasteur pipset to a 25,, mL concentrator
                  tube .                                      ',",..
                                                                '; ,  ,
      13.2.9      Repeat  steps 13.2.4 - 13.2.5£and 13.2.7 - 13.2.8; ."Combine
                  extracts.  Discard extractedsaqueous sample.       "  \
                                            > \
      13.2.10     Prepare a  drying column jb^ plugging ttie. bottom of a  funnel
                  with glass wool  and add^tg. approximately 15 grams of
                  powdered anhydrous sodium jilalf ate . - /ffour extract through
                  funnel  and collect in a 25''"fflL"graiiaated concentrator tube.
                  Rinse the  extract container witSi ^minimal volumes of  MeCl2
                  and pour through the funnel. Rinse sodium sulfate twice  with
                  minimal volumes  of MeCl2.             V ,,-
      13.2.11     Concentrate  ex|pa6t-gt&»ja^pajoximately 0.5 mL using  the
                  nitrogen-blowdowti^procedoEr^^iiilsvaljSO'C,,water bath.  To
                  minimize analyte ^jfeess  due tQivfclati'li:*|f occasionally rinse
                  sides of concentrator  tube fl^th isoctane during  the  blowdown
                  procedure.   Add 5  mL.of isfojgitane to concentrator tube  and
                  mix vigorously.  Reconpeflfeeate to approximately  1  mL.   Do
                  not let the  extract go sdigf during concentration.
      13.2.12     Proceed "to "eaStKact clean-trjrMstep (paragraph 14).
                     .'--- S,        ''-'i.,          %; ,-
                    •*"           V*.-           -•'•
13.3  Sample Preparation and  Extinction -  Soil/Solid Samples
                    . ''            £. ,~>j£:
                  ,, ,;.           ^jj; iv ......... _____
      A 6 g sample Oif -soil  is ml^E-::wi:t:h,::|)|wdered anhydrous sodium  sulfate and
      is serially extfifetfisd, with  a 20 mL and a 10 mL portion of MeCl2/acetone
      (90:10) using an ulta^s^nic  probe.   Extracts are combined,  filtered, and
      dried through powdere«fs«&i^drous  sodium sulfate, and concentrated with
      solvent,s«ssdiaajge,,into isoct^S?; to a  1  mL volume using the nitrogen
                            Non- PAH" ^ttrac tables are removed from  the  extract
             silica-gel e^ljamn clean-up procedure.  Final extract volume is 1
        .3.1      Decant  and-^scard any water layer on a soil/solid sample .
         j         Mix  samples|ffchoroughly,  especially composited  samples.
                  Discard anyjl'foreign objects such as sticks, leaves,  and
                  rocks.   ,:'-''.';1
      13.3.2      '1fe;|^, ^[^froximately six grams of a representative  sample to
                  the:-iiearest 0.1 g into a 150 mL beaker.
                                   D-28-PAH-Q                           08/23/94

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                                                                    DRAFT

13.3.3      To the weighed sample  add a  sufficient amount of powdered
            anhydrous sodium sulfate  to  prepare a free flowing mass upon
            mixing.  Mix well.

13.3.4      Spike the sample with  10  fjL  of  the  SMC (2.0 mg/mL) ,  mix
            further .

13.3.5      Add 20 mL of MeCl2/acetone (90:16).

13.3.6      Sonicate at microtip maximunpfrower ;  cool the sample during
            sonication.  The sonicator most be  set for 50 percent; ?pulse
            action. Sonicate for 3 minutes.   The power output may have
            to be adjusted to ensure Jisfaat the sample extract does not
            splash excessively; any isignif icant , less of sample during
            sonication is not acceptable;'.   Rinse the sonicator tip after
            each sample extraction with *1 ,atL,o%HeCl2/acetone (90:10).
            This rinse liquid shall be combined with the sample extract.

13.3.7      Remove and collect solvent layer  in a '•$§ mL centrifuge tube.
13.3.8      Add 10 mL of Me^&cfetose^SO^O)  and repeat  steps 13.3.6
            and 13. 3. 7.    ^ "" "*' '?•&•'. , i  ......
                              i  ,         r ,      •"*•'.,
13.3.9      Combine extracts and^filter-fey  gravity or vacuum filtration.
            Complete filtration "wjr transferring entire  sample contents
            to funnel and rinse wit&i .sate additional 10 mL MeCl2/acetone
            (90:10).               -••{
                   *-£ " '* " ••'£            " -.'
                        ®caf;,-;gravity filiation,  prepare a.
                        f iteration/ drying ;bed with Whatman #42 filter
                        papfr filled with' : approximately 15 grams of
                        po^jifered ^anhydrous  sodium  sulfate  in a 6 cm
                        p«^fer}:^&ae'>l:s Rinse sodium sulfate and
                        filterpaper with MeCl2/acetone  (90:10) and
                        discard rinsate.  With  the filter  and sodium
                        ^ilfate wetted, decant  combined extracts through
                        the 'Backed funnel and collect in a 40 mL
                        centirSSi^e tube.  Rinse the extract  container
                        with minimal volumes  of MeCl2/acetone (90:10)
                        and pour through the  funnel. Rinse filter/sodium
                         ulfate with 10 mL  of MeC^/acetone  (90:10).

            13.3.9.2   ~;j£or vacuum filtration use  Whatman  #42 filter
                      f,:.f>aper in a Buchner  funnel.   Pre-wet  the paper
                       ;~with MeCl2/acetone  (90:10)  and  discard rinsate.
                        Transfer combined extracts  into funnel,  apply
                        vacuum, and collect filtrate.   Rinse filter with
                        an 10 mL of MeCl2/acetone  (90:10).   Pour
                        filtered extract through a powder  funnel plugged
                        with glass wool and filled with powdered

                            D-29-PAH-Q                           08/23/94

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                                                                           DRAFT

                               anhydrous sodium sulfate and collect  in a 40 mL
                               centrifuge tube.  Rinse the extract container
                               with minimal volumes of HeCl2/acetone (90:10)
                               and pour through the funnel.  Rinse sodium
                               sulfate with an additional 10 mL MeCl2/acetone
                               (90:10).            ..' ;>   .,

      13 . 3 . 10     Concentrate  extract to approximately 25 mL using  the
                  nitrogen-blowdown procedure in a 30°C water "batJi,,   Transfer
                  extract  concentrate to a 25 jffiL concentrator tube'  aaod
                  concentrate  further to approximately 0.5 mL.  Add 5;,aiL of
                  isoctane to  concentrator Cube and mix vigorously.
                  Reconcentrate to approximately 1 mL. .r Bo not allow extract
                  to go dry during concen^i*-^011 •   To.pfnimize analyte loss
                  due  to volatility,  occasiefea|.ly rime sides of centrifuge
                  and  concentrator tubes witnUasocfctaal during the blowdown
                  procedure.                       '•'<-  ,

      13.3.11     Proceed  to extract clean-up step (paragraph 14).
                                   *-
13.4  Sample Preparation and Ex t^»oti.«^:-J .Oil -.Samples
      NOTE: The PAH target  compound -CRQL for ail samples : is 20,000 pgAg (see
            Exhibit C).              : :/       -f
                                      %    -; ; ''
      13.4.1      Add  1.0 g of sample to ,9, 3.0 mL volumetric flask.

                  Note: Qi3.y -matures shoiilti, first be phase -separated
                             tb'^sbe procedures. lin paragraph 13.1.
                                 '  -           - '*
      13.4.2      AM'l.O mL of Slfe (200 ug/mL) to the sample.
                  %'            1 1 .... ,.,-,..,..
      13.4.3      AM:lteCl2/ace;t^:li(^:J:0>afco the volumetric flask until
                  reacfoiiis;f»the 10 mL meniscus mark.
      13.4.4      Cap with st<^gt>er and mix for one minute.

      13.4.-5>Hi"";:  Tip^fc'/exactly l.tKaC out and concentrate extract  to
         4;«      approxlbsjiljfcely 0.5 mL using the nitrogen-blowdown  procedure
        s!,-;^:       in a  30<>%^ater bath.  To minimize analyte loss due  to
      «r         volatility|fepccasionally rinse sides of concentrator tube
                  with  isoctane during the blowdown procedure.  Add 5  mL of
                  isoctane tgjjieoncentrator tube and mix vigorously.
             ,^    Reconcentr^e to approximately 1 mL.  Do not let  the extract
                   go  dry during concentration.
      13.4.6      'ytiatseejSjiiilth clean-up and final concentration as  specified
                   in |*a£agraph 14.
                                   D-30-PAH-Q                           08/23/94

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                                                                           DRAFT

 13.5   Sample Preparation and Extraction - Wipe Samples

       A wipe sample containing PAHs is serially extracted with two  portions of
       methylene chloride (MeC^) using an ultrasonic pjrobe.   Extracts are
       combined, filtered, and dried through powdered anhydrous sodium sulfate.
       Non-PAH extractables are removed from the extract With a silica-gel
       column clean-up procedure.  The cleaned extract is  concentrated to 1 mL
       using the nitrogen blowdown procedure.                 ,   ,

       NOTE:  The target compound CRQLs for wipe-samples will  be specified by
             the Agency.                        •                      ''•''•

       13.5.1      Pour off any free solvent ;from the saasple  jar into a clean
                   Erlenmeyer flask of appropriate size.,

       13.5.2      Spike the sample with 10 uL~«f the;-SMC  (2.0  mg/mL) .

       13.5.3      Add enough clean MeCl2 to the sample jar to  cover the wipe
                   sample .                              •
                   13.5.3.1    If^td^-ste&pe'-'fbf, the sample jar is not amenable
                               to '•sriaicatloiij %fdastita.ti.yely transfer  the
                               sampl& 'to an appr-epfiate 'container .  Rinse the
                               sample ,j,ar withjS-lO mL of hexane and transfer
                               to the ne» sampie container.

      13.5.4       Follow steps 13.3.6 - 130.11.  In step 13.3.9, filter the
                   combined'i-extjracts by gravity filtration.

14    Extract Clean-va>>;         -^           ''  ..

      The extract  .clean- up procesfeepe removes alkane and branched alkane
      interferences l&iom extracJ^||^ili^,laH3alysis by GC/FID.  This procedure
      involves  slurry-i&eking a glass column with silica gel, rinsing the
      column with  solvents,; >«dding the sample extract to the column, eluting
      alkane interferences wi=tfc-^ weak solvent, hexane,  and then eluting PAH
                   ^!aa. stronger "solvent mixture, hexane/MeCl2 .  Final
                   tvesi!^,Ysa3-t exchange , into 1 mL hexane is performed using the
                blowdown
              Effectiveness *ȣ this extract clean-up procedure is dependent on
          completeness  of any-jfpreceding solvent exchange steps.  All extracts
      
-------
                                                                           DRAFT

      closing of the stopcock will aid in following the steps of this
      procedure.)

14.3  Add 1.8 grains of activated silica gel to a 50 mL beaker.  Add 10 mL of
      methylene chloride and mix well to generate a slurry.
14.4  Using a small funnel,  transfer  the silica geiyanethylene chloride  slurry
      to the glass column.   Do not allow the solvent in the .coJUimn to go below
      the silica layer.  Transfer  the residual silica gel slurryaiasing
      methylene chloride rinses.   Excess methyiene chloride in thei'column  is
      removed by flowing through the  column tie waste.  Do not allow soJtvent
      layer to go below the  silica gel.   After silica-gel slurry transfer  is
      completed, add 1-2 centimeters  powde^fefl anhydrous sodium sulfate  to  the
      top of the column.   If needed,  add 433itional Mefel.2 to wet sodium
      sulfate.  Do not allow solvent  layer &o go beloW^ the sodium sulfate.
                                              - '?-' >  % *.'.'
14.5  Bring solvent level  to just  above  the sodium i-gulf ate layer and rinse
      with 10 mL of methylene chloride.   As methylewKfehloride level reaches
      to just above the sodium sulfate layer, add 10 mL -'%*f jhexane .  Bring
      hexane level to top  of sodium sjalfate layer while continuing to pass
      eluate to waste.          ..'['h-> A- "  -  f'.\

14.6  Add sample extract (in isoctajse solvent) v*b siliea ,gel column.  Rinse
      the concentrator tube  with two>4).5 mL petitions of isoctane to complete
      transfer of sample extract.     ••:••     /

14.7  As extract level nears the sodium  sttlfate add 10 mL of hexane.  Bring
      hexane level to topjsJaf .asejdium sulfatei  Discard eluate.
                         "J SJ\  'y  *'•-,.

14.8  Add 10 mL of hexaae/MeC^ '^^D^O)  and collect the first 10 mL of  eluate
      in a 10 mL concentrator
                  .,               ,_„ ..........
14.9  Concentrate exatzpct using:Ml|SSSS8gfti~biowdown procedure in a 30°C water
      bath.  To minimifflelfaOaalyte  loss  due to volatility be sure to rinse  sides
      of concentrator tubejBatth hexane during blowdown procedure.  Final
      extract volume is  1 mL>-4'!1feis  final volume is suitable for extract
      compound«|Coa|Ksentrations  o1fi2£ift jfg/mL to 100 f»g/mL.  This is equivalent
      to sajaipleconipotiiia. concentrations  of 20 to 1000 pg/L for water  samples,
      330^ "tip 16600 jig/k|^l: soil/solid samples, and 20,000 pgAg to  1,000
               the extract  tfr-San  autosampler or other 1-mL vial and analyze
                to paragraph |3.15.
                             %-v
15    Instruii^yisal Analysislfj.

15.1  Set up the GG ';S3$s£ eat -per the requirements in paragraph 7.
      15.1.1       Solvent-flush manual injection or automated sample  injection
                   is recommended  for analysis.

                                   D-32-PAH-Q                           08/23/94

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                                                                    DRAFT

15.1.2      An analytical  sequence consists of field sample analyses and
            all associated standards,  blanks,  and QC analyses analyzed
            within a  24-hour period on one instrument.  There are two
            (2) types of analytical sequences: an initial calibration
            analytical sequence and a daily calibration check analytical
            sequence.   All samples shall be analyzed within one of these
            analytical sequences.

            15.1.2.1     An initial calibration analytical^sequence
                         begins  with a three-point calibrations,'an
                         instrument blank,  an LCS, and a method blank.
                         The initial calibration analytical sequence is
                         as follows:  :

                         •     Initial ;£hree-po4st calibration (analysis
                              of the hi'gtoi stao$ard followed by the mid
                              and  low standards);

                         •     Instrument Blank;   - ;:

                         •  -;.}/t^bratdejcjr Control  Sample(s);

                              JSethod Blarik(s)r- *  V.J

                              Field Sample(s);

                         •     Instrument Blank(s); and
                     *'''-'  *'<  ,           >•
                j,  *      »-,'x";  Performance  Verification Standard(s) .
               '"V          fS,*
            15-1.2.2    A  dally calibration check analytical sequence
                        be^as  with an instrument blank,  a valid
             •  •••;,       cafi^ratljoii:-cTafick  standard,  a method blank,  and
               '   -, ,   an LCS.  The daily calibration analytical
                       „ ^sequence is  as follows:
                       1 %^'
       ,,  •-''-];\"-•<-!,         •'*'-:':'-,;,-Instrument Blank;

                              Calibration  Check Standard;

                              Method Blank(s);

                              Laboratory Control  Sample(s);

                              Field  Sample(s);

                              Instrument Blank(s); and

                              Performance  Verification Standard(s).


                            D-33-PAH-Q                          08/23/94

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                                                                          DRAFT

      15.1.3      If all  acceptance  criteria for these analyses are met, then
                  the Laboratory may proceed with sample analyses.

      15.1.4      All analytical sequences  conclude with an acceptable
                  instrument blank and a PVS analysis ;\  The PVS shall be
                  started within 24  hours after the infection of the first
                  initial calibration  standard or ttee first '.instrument blank
                  in the  daily calibration  sequence.

                  NOTE: If a PVS reanalysis iSjXequired because of ta. non-
                  compliant initial  PVS analy&I-s,  the PVS reanalysis mist be
                  started within 26  hours afSSeT the start of the current
                  analytical sequence .     ,  1?

      15.1.5      The method blank and all  associated samples shall be
                  analyzed in the same analytical sequence.  If samples from a
                  batch are analyzed in more than one analytical sequence, the
                  associated method  blank must also1 be analyzed in the same
                  analytical sequence.   If  a method blaaic, extract is used up
                  because of multiple  analyses,  the Laboratory shall
                  substitute an •mstjrumeirt-sblank in place of a. method blank in
                  all subsequent iktialytlcal- sequences.,  .The Laboratory shall
                  note this in the -llatch Narrative an& Haall use the EPA
                  identification number as  described in Exhibit B for this
                  instrument blank.    '      -:{
                                        ~':'   • >. i
                                            . ,' ' '
      15.1.6      The LCS shall be analyzed"' with all associated samples in the
                  same anal/jrt'ieal sequence.," Jf samples from a batch are
                  analyzed in''mo*«* than one "aeEjalytical sequence, the
                  associated LCS^^jjall be analyzed in the same analytical
                  sie%eence.  If afiiLCS extract 4s used up because of multiple
                  ,SS|ilyses , the |iiboratory  shall dilute the LCS standard
                        .e (the j^g^^t.^t^ipc mix) and use this solution in
                               original LCS sample in all subsequent
                  analytical -sequences (see paragraph 24) .   The Laboratory
                  shall note!*tS^S,in the Batch Narrative and shall use the EPA
                  A^ntification-^tsfcaber as  described in Exhibit B for this LCS
                                  "*'
15.2  Computer reproductioni|iof chromatograms that are attenuated to ensure
           all peaks are on!*|^ale  over  a  100-fold range are acceptable.
              , post analysis «piftenuation  shall be no greater than a 100-fold
              This is to redt^e the potential for RTS of compounds due to
                   ad an(j  tq,%nsure that  the detector is operating within the
      calibra&^a range.   £fj|any sample compounds exceed the calibration
      range,  they shall be-'- diluted according to paragraph 16.
                   ''-'''**  *f :"$
15.3  If any  saturateoV'iiCHH- target  compound chromatographic peaks are evident
      or if any chromatographic peaks overlap more than one RRT and/or RT


                                   D-34-PAH-Q                          08/23/94

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                                                                          DRAFT

      target compound windows,  the  Laboratory shall use the "E,N" flags on
      Form QI-PAH to indicate  this  situation.

      15.3.1      If saturated chromatographic peaks otttside target compound
                  RUT and/or RT windows  are  evident, flag the nearest target
                  compound  "E,N"  on Form QI-PAH.       "

      15.3.2      If chromatographic peaks overlapping more than; one target
                  compound  RRT and/or RT windows  are evident, flagithe
                  corresponding target compounds  "E,N" on Form QI-B&8L
                                              &»:
15.4  Chromatographic peak  response must be ;gceater than 10 percent and
      less than 100 percent of full-scale (Inflection to/ ensure that
      individual compounds  will be  visible-curing data:rfiview.

16    Dilutions                                 ,;  ,   ;

16 . 1  Samples with compounds exceeding the calib ration, 'xange of the GC must be
      reported with the "E" data  flag as described in Exhitidt B.   Upon
      evaluation, the Region may  require that the samples 1b*e diluted,
      reextracted, and/or reanalj&ed •;$&':& 3»lJLd analytical sequence as
      additional paid samples.  Re^trac"tio%''^aai4/&y.; ^analysis of samples can
      only be authorized by the CLASS .contractor  actiiig^xm behalf of the
      Regional TPO or Headquarters  APG.  The li-boratory shall perform the
      dilution analysis as  specified below is paragraph 16.2.
                                       "• ••  }'
16.2  The Laboratory may dilute samples  pxSwe to  initiating sample analysis.
      The resulting analysis jof, ;-those samples must produce chromatograms with
      at least one target compo«tt^i  present a(gm concentration greater than
      that found in t^ife mid pointi,^calibration;Mbcture .  If no compound is
      identified in ,'jme diluted staple at a  concentration that exceeds the mid
      level standard!,, then  the  ui&lllufed sample shall be reanalyzed at no
      additional cbsfe)*®, the                  '
                          --t? •
      16.2.1      At the request of  the Region,  sample dilution may be
                  required prise|r«,^o  the initial  analysis.   If no target
               ;•  coHtpounds are^'Mdi^jftpted  in  the  diluted samples at the mid
            v?i" '^'^TpbSbsfe^Escgacentratie^br  greater,  then the undiluted sample
         .vf-      shall linejaseanalyzed  as  an  additional paid sample.
         v^ ''               *%'< '*~>-
      yGi&.2      Sample dilutions shall  be  made by  using an appropriate
     .:;|;!f;          aliquot of;iSbe extract  diluted in  isoctane.  After making a
      ~'*,'Ti:,      dilution, add sufficient SMC solution to bring up to proper
         ':;H; ':,  ,   concentration (20  pg/mL) .
           "^f,'^,         ,f;
      16.2.3   'M.£J5ap)le (JjptAtions shall  be  analyzed in a valid analytical
                  ''. 'which includes the associated method blank and LCS.
                                  D-35-PAH-Q                           08/23/94

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                                                                           DRAFT

      16.2.4      If sample  reextractions and reanalyses are required,  the
                  Laboratory shall  also reextract and reanalyze an associated
                  method blank and  LCS .

17    Identification of Target Compounds             J

17.1  Retention Time Standard - The SMC shall be used as t&e -E.T marker  for
      compound identification.  The SMC shall alsoi:be used to^iaonitor
      extraction efficiency.                                      -,' -

      17.1.1      The SMC shall be  added to all field and QC samples prior  to
                  extraction.
      17.1.2      In each analysis,  the  SSKS ;RT must ber-awithin + 1.0 percent  of
                  the mean RT of the SMC esij^lJ-shed Jdixring the initial
                  calibration .                 „*

17.2  Compound identification when SMC recovery is greater than or equal  to  10
      percent and less than or equal to  200 percent.  "»•
      17.2.1      Target compoura|s «i«pl.;;3*fc ^identified on the basis of RRT  in
                  all field sampleskfor  wnlt^'.^eiSllG recovery is greater than
                  or equal to  10 pexcent and l«sss" thaW-sor, equal to 200
                  percent.           . ;::       . , •
                                      '?.     Ti'
      17.2.2      Peaks in sample chronafcogasams  shall be identified as target
                  compounds if their RRT %Cfwi thin ± 0.008 RRT units of  the
                  mean RKfHeitfelished durii   initial calibration.
17.3  Compound identification whSwjfcsSMG recovery is less than 10 percent,
      greater than 2P8 percent, ofci.if peak interferences are present.

      17.3.1      Target compouadsSsh2Lll-::i>e:identified on the basis of
                  absoltdtC'sRT in all field samples for which the SMC recovery
                  is less"^8ipl».,10 percent,  greater than 200 percent, or  if
                  peak interr«ESftiaces are  present.

      17.3r2ji , '*  "Te^ks;|5aa sample 'cle^matograms shall be identified as target
                  compounaaKu.f their absolute RT is within ±1.0 percent of
        ') ;"•        the mean1'^! established during the initial calibration.
      ,/if                  «5f';
        '.3.3      Any compouiai identified on the basis of absolute RT shall be
        g;;-._       flagged wii&.j the qualifier "T" (See Exhibit B) .

        .3.4I;;^:,-.,| If the res^ery of the  SMC in a field sample is less than 10
              "^ 4<',-1*^rcent#;>^:eater than 200 percent, or if peak interferences
                  atffer|»-r,e|siBnt, an acceptable recovery of the SMC must be
                  obtained in the associated method blank and LCS (see
                  paragraph 22 and 24).


                                  D-36-PAH-Q                          08/23/94

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                                                                           DRAFT

17.4  If multiple peaks are within the identification windows  (target  compound
      and SMC),  the  Laboratory shall use professional judgement to properly
      identify  the appropriate peak.  The Laboratory should consider the
      inherent  matrix affects of the sample on peak shlsfting, masking,  and
      overlaps  when  making identification determinations.  The Laboratory
      should  take into consideration the mean RT andSKt,£rom the initial
      calibration, RT and RRT from the calibration/check standard, and the SMC
      RT from relatively clean samples analyzed before and aiSter the sample in
      question  as a  basis for selecting the most appropriate peak^  The
      Laboratory shall describe in the Batch Narrative the rationalejiised for
      choosing  a particular peak (e.g., chose j>eak closest to the RT t>f the
      peak in calibration check standard) as~fche target compound or SMC and
      how the field  sample matrix may have Effected peafe identification.

18    Calculations                          <%•••*'
                                                /.
18.1  Calculate  the  RRT of a sample component or •& -standard using the
      following  equation:
                                                                 EQ. D.ll
      where:

      RRT = relative re tenion J:time
                                 , -  -•           ;
      ^component = f^^ntion titae, of the  targeit compound
                    t'-l ''           ii:
      RTSMC = retention time of  jafe^SMC
                   s  •• s         "% 'Jv"11* Xa *• "•* *  r ••
                    1 , < ; *       ••'  ** •" ••  ••' ' J    •.
18.2  Calculate the calUfoation  factor for a  compound by one of three
      techniques using datai^ollected during  an acceptable initial calibration
      (paragraph 8).  The use^frffesthe  line  segment or "K" curve is suggested.
      Only one..o^ 'tfee^guantitati-ctittschniques listed below shall be used for
      quantitsattng 'sai^>3^5 within  a-jifctch  and analyzed within a given
      analytical sequence^ (- ,

      y&yz.l      Use the nB^>;?curve (line  segments)  established during initial
     _JV"          calibratiolt,!   The segments  run from the low to the mid point
     ';« -~,*f        and from the~mid to  the  high point calibration mixtures.
         ' '  j, .,    (Note:  do jjaaet  extend line segment  through the origin if the
            "N|/> -, concentration  is below the  CRQL) .
      18.2.2      tlse 1&«|;: calibration factors based  on  the mid point of the
                  inlcbsaC: -calibration curve.  This option may be  used as long
                  as the mid point values are within ±  10 percent of the
                  average of the high and low point  values.

                                  D-37-PAH-Q                           08/23/94

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                                                                          DRAFT
      18.2.3      Use the mean calibration factor established during the
                  initial calibration.

      18.2.4      Quantitation of compounds is based 
-------
                                                                          DRAFT
                  V
                  W
                               volume of concentrated extract (use 1000 jiL or a
                               factor of this when dilutions are made).

                               weight of sample extracted in g.
                               Note:  for oil samples,,  Divide Wg by 10.  The
                               factor of 10 for the"Ifs,  is ;i»ecessary because
                               only one -tenth of the extract is ^processed and
                               analyzed.
18.4  Calculate the SMC amount  observed and amount (percent) recovered its ing
      equations as described  in paragraph 10,^4.

18.5  Retention time shifts (RTS)  shall be: iaonitored uplng the SMC (paragraph
      17.1).  The RTS shall be  measured for* jgU, analyses.

      18.5.1      Calculate the retention time perc«n$ difference (RT %D)
                  between the RT of the SMC in the 'field- and QC samples or
                  subsequent  standards  analyzed and the mean SMC RT from the
                  most recent initial calibration analyzed ttMng the following
                  equation:      "  ;':  >, , ;:-'; ' •;  . ,
                                                                     . D.14
                  Where :  ,
                  RT -3£D =
                  RT
                              retsieation time  shift.
                                  ' -''

                              recetion .time  o f the  SMC in a field and QC
                                                   standard.
                          s ,,  ' ^mean retention  time  of the SMC from the most
                                      initial  calibration.
                           Criteria'
                e within a »|tch  shall be  analyzed on a GC system meeting the
              calibration orjjisalid calibration check standard technical
       ||:eptance criteria (p^fcagraphs 8  and  9) .
19

19.1



19.2
19.3  Each sample withtfel^ Batch shall be run within a valid initial
      calibration or daily calibration check analytical  sequence that
                  within a B«fe;h shall be  analyzed after an acceptable method
      and iriili$p§nt blank jjparagraphs 22  and  23),  and after an acceptable LCS
                                  D-39-PAH-Q
                                                                       08/23/94

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                                                                          DRAFT

      concludes with an acceptable instrument blank (paragraph 23) and an
      acceptable PVS (paragraph 10) .

19.4  Each sample within a Batch shall be  analyzed and results reported within
      the contract required turnaround times .

19.5  Each sample matrix within a Batch shall have an acceptable method blank
      analyzed during the same analytical  sequence.           ^  .-,

19.6  The RTS for the SMC RT must be within ±Jb0  percent between aiytsample
      in a Batch and the mean RT of the SMC aaialyzed during the initfal,
      calibration.  The RTS is not evaluated ifX  the SMC is not recovered in
      the sample or if peak interferences  j&e present.  ,.„
19.7  The advisory recovery limit for the 'IC :ls  50- ISO percent.  Reanalyses
      of field samples are not made if the  SMCJarecov^ry is outside the
      advisory recovery limits.                   '   ~

19.8  The SMC recovery must be greater Chan or equal tc^'10 percent and less
      than or equal to 200 percent^jln^ order to use  RRT f or -'txlentif ication
      purposes .   The identi£icat£o^M^^iMr^i!^ ± 0 . 008  unit of the mean RRT of
      each target compound from tfeXinitial^-^^C^ratfi-o^j. , If the recovery of
      the SMC is less than 10 perce*^, greaterri&anv'2^.' percent , or if peak
      interferences are present (but\|ls adequately  recovered in the method
      blank) ,  the absolute RT of the ccpapouiiiisr shall be used for
      identification purposes.   The ideatJfpLcation window is ± 1.0 percent of
      the mean absolute RT of each target compound  from the initial
      calibration.           *'*'•
                             ''*; '"f \
                                '^V v           '' '•
20    Corrective Action         \f ,
                   ,;-':~'           i,-k,
20.1  Flag all sample,, results "SJ^i.'f.jthe SMC _is outside the advisory recovery
      limits of 50 -15$ percent ^lil/'fi.Jl, H;?-"
20.2  Flag all sample result-->"T"  if the absolute  RTs are used for
      identifications.       •-!> I-
                              < , ?' .??
20.3  An SMg^asectArery j&T^ess than ^^.jpercent in the method blank or LCS
      associated with a sample Batch is  an  indication that serious problems
      majri^ave occurred during the extraction process.   Corrective action
      shall be performed andl|the unacceptable method blank and/or LCS and all
     #4iniples associated witSbthe unacceptable method blank and/or LCS shall
      %e^eeextracted and reanalyzed at no additional expense to the Agency.
           .
20.4  If the*^K3.;E.TS criter^n  is not met  for any field sample, sample
      analysis shijl^ be stf^jjjped and  the noncompliant sample rerun.  If the RTS
      criterion iss st^xUL/^pt upon reanalysis,  analyze an instrument blank.  If
      the instrument IJI&de SMC  RTS is outside the criterion, perform
      corrective action which may include  a new initial calibration.  DO NOT
      continue with sample analyses  until  the RTS is within ± 1.0 percent.  If

                                  D-40-PAH-Q                          08/23/94

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                                                                         DRAFT

      the instrument blank SMC RTS meets the criterion, sample analysis may
      continue.  The Laboratory shall report both sets of noncompliant sample
      data and flag the results "M".  Note: the RTS is not evaluated if the
      SMC is not recovered in the sample or if peak interferences are present.

20.5  All target compound concentrations which exceed ;tfce upper limit of the
      initial calibration range will be flagged "E". (see Exhibit B).

      NOTE:  Unless otherwise stated in Exhibit D, all sample data from the
      initial analysis shall be reported to the appropriate Region, i-l'Samples
      not meeting any one of the contract tectaiical acceptance criteria- and
      not requiring automatic reextraction as8/or reanalysis shall be flagged
      by the Laboratory.  The Region will ^saluate the jraemcompliant samples
      and may specify that these be reanalyzed as additional paid samples.

21    Documentation                          '  r~  •   : *

      Sample results shall be reported on Forms QI-P&H and QVI-PAH.  Reporting
      requirements are listed in Exhibit B.
                                  D-41-PAH-Q                          08/23/94

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                                                                          DRAFT

                                   SECTION V

              SAMPLE QUALITY CONTROL PROCEDURES AND  REQUIREMENTS


22    Method Blank Analysis

22.1  Summary - A method blank for water samples  is  100  mL ofl-areagent water
      spiked with the SMC and carried through the entire analy"tie&l scheme.  A
      method blank for soil/solid samples is 6*g  of  clean quartz sazicb^piked
      with the SMC and carried through the eatdEre analytical  scheme.   A"Method
      blank for oil samples is 1 g of corn ,oll spiked with the SMC and carried
      through the entire analytical scheme>»Sf Method  blaiifcs shall be carried
      through the entire analytical procedure.        - -•''

      NOTE: The Agency will provide the laboratory with  further instructions
            for the analysis of method blanks for wipe samples.

22.2  Frequency                                        ;i  V
                                 ' •* '                       '
      A method blank analysis shail Jjec;||er*ormed  for each matrix type (water,
      soil/solid, or oil) and wita<«ach se't'-ofe-samples,.,   A set of samples is
      defined as those samples fronr^ene Batch ?;£hat are "extracted and analyzed
      on one instrument during a 24-fetmr analytical  sequence.
                                      ~?      'f-
                                      9    :"' '
      22.2.1      The method blank and all associated samples  shall be
                  analyzed in the same analytical sequence.   If samples from a
                  batch are analyzed in more than one analytical sequence,  the
                  associated meJ^tpd blank mu^fc also  be analyzed in the same
                  analytical sequence.  If a »6thod  blank extract is used up
                  because of multiple analyses, the  Laboratory shall
                  •substitute an i|^5tCTme,nt,b,lank  in  place of  a method blank in
                  all -!^bsequemte1»llyjfcl^i,lsequences.   The Laboratory shall
                  note-'t&is, in the Batch Narrative and shall use the EPA
                  identification number as described in  Exhibit B for this
                  instrument 'I
      22.2.^ ^~---" 'An acceptable mef&pd blank shall be analyzed before running
         •\'
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                                                                          DRAFT

                  extract and clean-up the method blank according to
                  paragraphs 13 and 14.

      22.3.3      Prepare the soil/solid method blank, by weighing
                  approximately 6 g of clean  quartz  sand and adding sufficient
                  amount of powdered anhydrous  sodi«nt spulfate to create a
                  free flowing mass upon mixing.   Sf»ike with J.O /jL of the SMC
                  and extract and clean as described in paragraphs 13 and 14.
      22.3.4      Spike 1.0 g of corn oil with,X-0  mL of SMC (200'pgjtaL) and
                  proceed with the PAH extraction and analysis procedure
                  (paragraphs 13.4.3 - 13.4,55.

      22.3.5      Analyze the method blank extracts.  /;Calculate the results
                  according to paragraph 18,,  ;

22.4  Technical Acceptance Criteria

      22.4.1      All method blanks shall be  analyzed within an acceptable
                  analytical sequence on a GC system meeting the initial
                  three-point callfirsfc'ioii ,c,rij:eria  (paragraph 8) or valid
                  calibration checkistandarfe ^tti^ftrJUt-^paragraph 9), and the
                  •PVS acceptance criteria (paragraph 10)1
                                     "-        -U
      22.4.2      The RTS for the SMC lit the jrfethod blank must be within ±1.0
                  percent between the bliank'lS&C  RT  and the mean SMC RT
                  calculated from the initial calibration.

      22.4.3      The &1C "recovet^ criterion:,^  50-150 percent is advisory
                         The SMC;jj?ecovery in  t|be method blank must,  however,
                      reater than/^r equal to 20 percent and less than or
                  e«3|iial to 200 pe¢..^

      22.4.4      The target compounds or potential interferences in the
                  method blanks must have a response less  than one-half the
                  response in,Site .corresponding  RE.T window of the initial
               ;, :-calibration low concentration  standard.

      22.4,5'      A method-blank may contain  a detectable  but acceptable
                  concentration of a target compound (less than one-half the
      • ';.<\         response a^.sthe initial calibration low  concentration
      Ili!          standard) . V=,
      "• A -'• .                 ''
      22.4i6;;     If all criisearia are satisfied,  the method blank analysis is
            •:     acceptably land samples may  be  analyzed.   If the method blank
                  pis, .unacceptable, corrective action shall be taken and an
                  accief£aijl,e method blank must be analyzed prior to analyzing
                  the'Associated samples.
                                  D-43-PAH-Q                           08/23/94

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                                                                           DRAFT

22.5  Corrective Action

      22.5.1       If  a method blank does not meet the technical  acceptance
                   criteria,  the Contractor shall consider the  analytical
                   system to  be out of control.  It is'the Contractor's
                   responsibility to eliminate methad::tofe&rferences  caused by
                   contaminants in solvents, reagents, cartaslldges, glassware,
                   and other  sample storage and processing hardware  that lead
                   to  discrete artifacts and/or elevated baselines|lin gas
                   chromatograms.   If contamination is a problem, "fcfae" ,„
                   Contractor shall investigate? the source of the     --|-
                   contamination,  and appropriate corrective measures shall be
                   taken  and  documented before further sample analysis
                   proceeds.               }-  ,         '-;:  °
                                          ' ,!\ • Jli ,        *
                                           * • rfj. < ..,
      22.5.2       If  a compound is found in the ssethod blank (less  than one-
                   half the response in the corresponding RRT window of  the
                   initial calibration low concentration standard) and is also
                   detected in an associated field sample sat less than the
                   CRQL,  the  compoiaiwJ, shall be reported as -a nondetect,  i.e.,
                   with a "U" flagj'-';.-•„-;;"-  $*>•>
                                 •*1~    !"-''-H'*7s>/v- ,  ,
      22.5.3       If  the  SMC recovery in the mlHshod'felasfc' is  less than 20
                   percent,  greater tJuro 200 pefscent, or if peak interferences
                   are present,  the method bisaaak shall be  immediately rerun.
                   If  on reanalysis the aetjio-,:::^  iac'alsl>3^5t;ion.  DCMlSifj! continue with sample analyses until the
         ..^V       RTS  fs^slbthin ±1.0 percent.
        ,x '"-               "'HA
        •-.-;'•-                 "y-^
                   Any  samplefc-processed with a method blank that is out of
                   control (ilpS,.,  does not meet any of the technical acceptance
      ; :4|^|';         criteria) ffiall be reextracted and/or reanalyzed at no
         "%dj'~,    additionaljf-sexpense to the Agency.
           '^Ilirj           3$
22.6  Documenta^iipi,,       -""

      Method blank r^siites are reported on Forms QI-PAH and QVI-PAH.
      Reporting  requirements are listed in Exhibit B.


                                   D-44-PAH-Q                           08/23/94

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                                                                           DRAFT

23    Instrument Blank Analysis

23.1  Summary

      An instrument blank is 1 mL of hexane spiked wit& 10 jiL  of  SMC  (2.0
      mg/mL) .   At least two acceptable instrument bianks,:,shall be analyzed
      within an analytical sequence, one before sample analyses and one
      following sample analyses.                              ,'[_•

23.2  Frequency                               !

      An instrument blank shall be analyzed 9£ least twice during the
      analytical sequence to ensure that the instrument -,is free from potential
      contaminants.   The first instrumenjt*J>lank analysis shall be performed
      after  the initial three-point calibrat|;«*» in tise initial calibration
      analytical sequence or as the first analysis ffcti a daily  calibration
      check  analytical sequence.   The second instxtaaent blank  analysis  shall
      be performed immediately before the PVS analysis,;, The Laboratory is
      encouraged to run additional instrument blanks dtaitisg the analytical
      sequence,  especially when highly contaminated or complex samples  are
      analyzed.   Instrument blanksjffiuiSi: be :maalyzed after analysis of samples
      with high levels of target 'e^pouridi: isir'i^ijeetSfereiits (see paragraph
      23.5.6).                     '><;           .?•;••  '---  •',;

23.3  Procedure for Instrument Blank preparation

      An instrument blank is 1 mL of hexaneCspiked with 10 fiL  of  SMC  (2.0
      mg/mL).

23.4  Calculations  ~£<         "',-',,          •>'

      Concentration^ of the SMC .atijj^any^Jtarjjet compounds in the instrument
      blank  are calWiwt.ed accoi^^glStl&feliprocedures described  in paragraph
      18.  Note:  The CkEgpt compound concentrations (detected  concentrations
      and CRQL  values)  in stJie, .instrument blank shall be reported  in the
      appropriate concentration units (e.g.,  report in /ig/L if the associated
      samples ^ns^raEtoar and in 'JtgjSSg if the associated samples are soil).
23.5  Tec^BKial Acceptane^-Xriteria
      Z^i'^.l      A minimum'•#£ two (2)  instrument blanks shall be analyzed
     -,/y:          during  an imalytical  sequence on a GC system meeting the
     '•^|'?V       initial thts^-point calibration criteria (paragraph 8) or
        '^'.Jt'-1. .v,   fc^e valid jfcailibration check standard criteria (paragraph 9),
                  and the Ff5- acceptance criteria (paragraph 10).
      23.5.2      '"Tfce,^XSrdfor the  SMC in the instrument blank must be
                  within a  1.0 percent between the blank SMC RT and the mean
                  SMC RT calculated from the initial calibration.
                                   D-45-PAH-Q                          08/23/94

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                                                                          DRAFT

      23.5.3      The SMC recovery criterion of 50-150 percent is advisory
                  only.  The  SMC recovery  in the instrument blank must,
                  however, be greater  than or equal to ,20 percent and less
                  than or equal to 200 percent.        :.

      23.5.4      The target  compounds or  potential 'interferences in the first
                  instrument  blank (analyzed immediately after the initial
                  calibration or before a  valid calibration cfeeck) must have a
                  response less than one-half the response in the
                  corresponding RRT windows of the initial calibration, low
                  level standard.            „ ''•:                       :,

      23.5.5      Subsequent  instrument bl&iSks are acceptable with low level
                  contamination.  These instrument blanks may contain target
                  compound concentrations '-ajpto twice  ,the CRQL (2x CRQL).

      23.5.6      Following the analysis of a field sample containing high
                  levels of target compounds or inteiSfexents,  an instrument
                  blank shall be analyzed  and must meet acceptance criteria
                  before proceeding, with sample analyses.   If1 an autosampler
                  is utilized, t]3$&5t|$e-:Il$riid,.,,samples  run after a high level
                  sample must be ~&sg*efullySe*li3^|stse&sjEor carryover.  The field
                  sample immediately" jfollowingl'llhe' high, lievel sample shall be
                  reanalyzed, along with any toiler samples analyzed after the
                  high level  sample whiteh  shows evidence of carryover.

      23.5.7      High level  samples are defined as being field samples that
                  contain-taaorgat compounds -at concentration levels that exceed
                  twice* tftie hl'gjs-Calibration Standard  concentration and/or
                  infelSferents tlaat are detected at levels greater than the
                  mill level init$M3, calibration concentration response of the
                          target^Sepppund...
23.6  Corrective Action  ;,  ,

      23.6.1      All groups~xg$ Samples analyzed shall  be bracketed with two
               ,  ;.taeeeptable instalment blanks.   If either instrument blank is
            % r •   unacceptable, correlative  action shall be taken and all
         :-, ,"'      samples ;&ot bracketed by  two valid instrument blanks shall
        ,,-V        be reana%ped at no additional expense to the Agency.

        .6.2      If the resf^ovse of any  target  compound in an instrument
                  blank analyzed after the  initial calibration or before a
                  valid cal$j|32ation check standard is greater than or equal to
              jy  ;., one -half ftps response in  the corresponding RRT window of the
                 ;| Initial -sbklibration low concentration standard, corrective
                  acsi|»3Vj$i»all be performed and  the system shall be
                  demoi*§e£ated to be clean  by the analysis of additional
                  instrument blanks until all target compounds are less than
                  one-half response.

                                  D-46-PAH-Q                          08/23/94

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                                                                           DRAFT

       23.6.3       If any target compound in an instrument blank analy2ed after
                   field/QC sample analyses is greater than  two  times the CRQL
                   another instrument blank shall be analyzed.   If,  on
                   reanalysis, contamination still exceeds the criterion,
                   corrective action shall be performed¥.and  the  system
                   demonstrated to be clean.  Then, ..all ^associated field/QC
                   samples analyzed since the last,valid  instrument blank or
                   method blank which contain those target cooposaads or
                   interferents found in the instrument blank atytesrels greater
                   than twice the CRQL shall beStaerun.             *"'fV

       23.6.4       If an instrument blank (otter than the first  instrument in
                   the analytical sequence ),;i  ''f1': .slg"..,,
       23.6.6       If the ins trumetit:'.blank"1^fC<;^co^stopped and another instrument
                   blank ;lfcall be analyzed.  If the RTS criterion is still out
                   on reanalgrjl&s ,  corrective action which may include  a new
                   initial cal$$|&i&Lon shall be performed.  DO NOT continue
                        sample an^^se.s until the RTS is within ±1.0  percent.
                  Any  samples not bracketed by valid instument blanks or  a
                  valid instalment blank and a method blank and shall be
                  reanalyze<%f|t  no additional expense to the Agency.
23.7  Tkwisaentation
      Instrument-blank  resu&fes  are reported on Forms QI-PAH and QVI-PAH.
      Reporting3-xies<5«iremeKt^  are  listed in Exhibit B.
                                   D-47-PAH-Q                          08/23/94

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                                                                          DRAFT

24    Laboratory Control Samples

24 . 1  Summary

      The QTM PAH LCS mixture initially will be  supplied to contractors by the
      Agency.  The LCS mixture will contain target compounds at several known
      concentrations .   The Laboratory shall spike  the LCS iftixture into a clean
      matrix that is similar to the samples being  analyzed. <3&e .spiked matrix
      shall be prepared and analyzed using  the procedures described for field
      samples.  Analysis of the LCS will assess,', the performance of ;;£ne
      analytical system prior to analyzing  f^elid samples.              "

      NOTE: The Agency will provide the laboratory with further instructions
            for the analysis of LCSs f or .^ipe samples^'?

24 . 2  Frequency                                , "f     :

      An LCS shall be analyzed once per matrix per analytical sequence (24
      hours) per instrument.  The LCS shall be analyzed Maffeer the first
      instrument blank in the initial .calibration  analytical-sequence or after
      the method blank in the da&jr Se^lffiSSfbUna  analytical sequence.

      24.2.1      An LCS shall be analyzed  witiif eachV ""

                  •     Set of water field  saagples (LCS prepared from reagent
                        water) ;            ;': '?
                        Set: |fi: -soil/solid fisld samples (LCS prepared with
                       >:quartz -Isand) ; and    ;-'-'*
                       '          """!' '
                        Set of oiiy  field samples  (LCS  prepared with corn
                        oil).   _.O. „_  „ _
      24.2.2      The l^S ^shall be analyzed with  all  associated samples in the
                  same analytical sequence.   If samples from a batch are
                  analyzed insjaor.the Laboratory shall  use  the original stock mix
        ^'Z*       diluted 3^|ao hexane in place  of the original LCS sample in
      ,j          all subseqlgsnt analytical sequences.  The Laboratory shall
     '-";;,?          prepare thtfe; solution by diluting 100 pL of the LCS standard
      C:* "%~s       mixture into. 5 mL of hexane and concentrating to 1 mL using
         'H"\;,    nitrogen blowdown.  The  Laboratory  shall note this in the
            ^•lv>,:£; Batch Narrative and shall use the EPA identification number
               '---', 'ms,. descrJfcfed in Exhibit  B for this  LCS solution.
                                  D-48-PAH-Q                          08/23/94

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                                                                           DRAFT

24.3  Procedure
      Spike the appropriate matrix with the LCS standard mixture and prepare
      as follows.

      24.3.1      Water LCS                         '       ;•   ,

            24.3.1.1    Allow  the  LCS  mixture ampules to reach rbojm
                        temperature before opeping.  The ampules must not be
                        opened until preparation/analysis is to occur.  ;
                        Exercise care  in breaking the ampules open to avoid
                        injury.             ;:           j  -

            24.3.1.2    Spike  100  mL of reagent water,with 100 /zL of the LCS
                        standard mixture as de&4rib°ed-'in the instructions
                        provided with  the LCS mixtisilr^s.  Use syringes to
                        perform the spiking to ensure ^accuracy.  Add the SMC
                        and mix and carry through the extraction and clean-up
                        process as*described in paragraphs 33 and 14.  Proceed
                        with the ^analysis as  described in paragraph 15.

            24.3.1.3    Nominal aqueous LCS taz^et cbmpoiihd concentrations are
                        as follows:  ':  ,

                        Acenaphthylene    >:            54 /jg/L
                        Anthracene         f'<.;            78 /*g/L
                        JBeazs^lOanthracene5:^,           52 ^g/L
                       iSenzo(TS>a.oranthene -;;          68 /zg/L
                    /  ^Benzo(g,i|i)perylene            36/tg/L
                   „<    Chrysene \y                     43 ng/L
                  f,    Dibenz(a4it|;an^racene          43 /ig/L
                   - •-  !'^Naphthalisispilr^jl:-,'y-^'''          90
                      ; tBbenanthrene                    41

      24.3.2      Soil LCS  ^'  -
             '?' '-; V"~, ' '^.-         '*- ; '~J< '-'
                     sfl.'Ailow the EGSimixture ampules to reach room
                        ^sigierature before opening.   The ampules must not be
                        opeassd until preparation/analysis is to occur.
                        Exercise care  in breaking the ampules open to avoid
              ,3.2.2    Spiki ;« g of quartz sand with 100 /tL of the LCS
             V>C : s,      staMard mixture as described in the instructions
              ""'•iY . v   presided with the LCS mixtures.   Use syringes to
                   :1   .perform the spiking to ensure accuracy.   Add the SMC
                      : Jsbtd mix and carry through the extraction and clean-up
                        process as described in paragraphs 13 and 14.  Proceed
                        with the analysis as described in paragraph 15.

                                  D-49-PAH-Q                           08/23/94

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                                                                           DRAFT
            24 . 3 . 2 . 3     Nominal LCS target compound concentrations are as
                         follows :

                         Acenaphthylene                  900  /tg/Kg
                         Anthracene                    1,300  /ig/Kg
                         Benzo (a) anthracene         ,    !; &67  >ig/Kg
                         Benzo(b)floranthene       /. '  1,133: jig/Kg
                         Benzo (g,h,i)perylene            600  jig/Kg
                         Chrysene                        717  jigMg*
                         Dibenz (a, h) anthracene ,          717  |tg/Kg  v
                         Naphthalene          f*..'       1,500  /ig/Kg   '
                         Phenanthrene                    683  /ig/Kg

      24.3.3      Oil  LCS                  /            ;

                  This section has not been finalized.  The  LCS  composition
                  and  concentrations for oils are: currently  being
                  investigated.                     .
            24.3.3.1    Allow ths |UG5» ^tpLsctiUj* ampules to reach  room
                        temperatuiie, before'^^eJXitlg. ,, -The ampules  must not be
                        opened until'^preparatiefe/analysis  ±s  to occur.
                        Exercise cafe :

            24.3.3.2    Spike 1 g of corn>eil with 1 mL of the  LCS standard
                        JBixtaar* , as describecliin the instructions  provided with
                       ;V-the 'nJSfjgxtures.  Tlsei syringes to perform the spiking
                     j,;p:to ensure? -accuracy .   '•ftod. the SMC and  mix  and carry
                   ,; ": *' through t|be extraction and clean-up process as
                   'k .   describesSr'in paragraphs 13.4.3 to  13.4.5.
                   '*;••»           j ,s j< x:  "*! ••••>{ ^^, --^j^*
                                           '
            24.3.3.3  "" -^BNMBinal LCS target compound concentrations are as
                         follows :
                                                        54,000
                                                        78,OOO^g/Kg
                                                        52,000  |»g/Kg
                         Be^^(b)floranthene            68,000  /tg/Kg
                         Benz||g,h,i)perylene           36,000  /ig/Kg
                               ie                       43,000  /*g/Kg
                                 , h) anthracene          43,000  /ig/Kg
                         Naphlbalene                     90,000  /ig/Kg
                         Phei&ithrene                   41,000  /ig/Kg
                             '
24.4  Technical Ac^ptamce^'Criteria
                                   D-50-PAH-Q                           08/23/94

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                                                                          DRAFT
      24.4.1      All LCS compounds must have  recoveries between 30 and 130
                  percent.  Up to  two LCS  compounds  may, however,  exceed the
                  upper recovery criterion of  130  percent.

      24.4.2      All LCS target compound  absolute and relative retention
                  times must be within the windows established during the
                  initial calibration.             .        :  .

      24.4.3      The RT of the SMC must be within ±1.0 percent •$£ the mean
                  RT of the SMC established during the initial calibration.

      24.4.4      The SMC advisory recovery -criterion is 50-150 percent.  The
                  SMC recovery in  the LCS jsust, however, be  greater than or
                  equal to 20 percent and';J.ess  than  orr- equal to 200 percent.

24.5  Corrective Action                      ''X
      24.5.1
      24.5.2
      24.5.3
 If any LCS compound recovery  is  lesss:than 30  percent or more
 than two LCS compounds exceed 130 percent,  the LCS shall be
 reanalyzed.  If, .upon reanalysis, more 'tbaprt two LCS target
 compounds are «tt£M^\%ttt~ recovery  criterion,  the LCS and
 all associated f|>eld and QC-Jsamples shall be  reextracted and
 reanalyzed.  If 6tie or two LCS cotitpowacis  are  outside the
 recovery criterion, proceed'«ith sample analyses,  and flag
 all sample results of- .compounds  that were out in the LCS
 with an "L" flag.        :,
 If the rsecbviery of the SitC is less  than  20 percent,  greater
 than.'JiO© pertsae^c, or peak "Interferences  are present  in the
 LCS'i ^-sample aritlysis shall ike stopped  and the  LCS
 reanalyzed.  If!;ihe LCS SMC recovery is  still  outside  the
 Criterion upoujxianalysis^  corrective  action shall be
 performed, an&h^BJLCSi{aiKi all associated samples
 reextaaeted and reanalyzed.

 If the RT OCf&KT for any LCS compound  is not within  the RT
         windows-established during  the initial calibration,
           the LC§; 'If upon reanalysis a compound is still
 outsieteigthe windows,  a new initial  calibration must  be
        <•«/.> *,-*
 performeaei*efore samples can be analyzed.  The instrument
 must be rfessalib rated as described in paragraph 8.

 If the RTS;ieriterion is not met for the LCS, sample  analysis
 shall be sffcepped and the noncompliant  LCS reanalyzed.   If
, the RTS i-S,;istill outside the criterion upon reanalysis,
 Corrective action shall be performed,  which may include a
             calibration.   DO NOT proceed with  sample
          until the RTS is within +  1.0 percent.
                                  D-51-PAH-Q
                                                     08/23/94

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                                                                         DRAFT

      24.5.5      All LCS technical acceptance criteria shall be met before
                  any samples or required blanks are analyzed.  Any samples or
                  required blanks analyzed when the LCS criteria have not been
                  met shall require reextraction and/or reanalysis at no
                  additional cost to the Agency.      -,

24.6  Documentation                                         :

      Laboratory Control Sample results are reported on Forms QI-BfLH, QII-PAH,
      and QVI-PAH.  Reporting requirements are Jtisted in Exhibit Bts :
                                  D-52-PAH-Q                          08/23/94

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                                                                    DRAFT
LO-
             COLUMN RESOLUTION CALCULATION
                                                  % Valley — x/y • 10O
  9:3O
                    9.-.4O
  9:5O
Time
                                                            10:00
                                Figure 1
                               D-53-PAH-Q
                           08/23/94

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                                                                           DRAFT

                                    Table 1.

                   List of PAH Compounds in Order of Elution*

                   Compound                Retention Tiae (mlns)

                   Naphthalene                   5.71    -';
                   Acenaphthylene                8.B9
                   2-Bromonaphthalene(SMC)       9.14           '.;  '
                   Acenaphthene                 , 9.26              r ...
                   Fluorene                  ,,=  ,; 10.23                   :
                   Phenanthrene             > -f   11.99
                   Anthracene               j    12.07
                   Fluoranthene           :: ^    14.22  '
                   Pyrene                 '  '.;- „ 14.60  "
                   Benz( a) anthracene             '16 »:5Sl
                   Chrysene                      16.^9
                   Benzo(b)fluoranthene **       18.87
                   Benzo(k)fluoranthene **                   ,
                   Benzo(a)pyrene ,  s,            19.32
                   Indeno(l,2,3-c4^p?eise;;- ,5  , 21.08
                   Dibenz(a,h)antnl2£bene    ''!; ,21.18,  ,
                   Benzo(g,h,i)peryi^ae          -21.52   '
*     This elution order is _given as genetral guidance and is  based on
      suggested  instrumental^^iiierating conditions as given in paragraph 7.

**    Benzo(k)fluoraa£hene coeluta&S with Benzo^b)fluoranthene.   The sum of
      both Benzofluosanthenes willfrbe measured and quantitated using the
      calibration J&fctor of the IsuHsoraer,. .„
                  
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                                                          DRAFT
             / MHIBIT D
             •I ; ' -^~{,'- ''-,'rh ••••:< •

       QUICK Ttl3SIAROUND 'ltetiK>BS- ;   ;


ANALYTICAL METHOB:-?OR PBESKJLS  (PHENs)
               D-1-PHEN-Q                             8/23/94

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                                                                           DRAFT

                                TABLE OF CONTENTS
                                     PHENOLS

SECTION                                                                    Page

I     Introduction	,.'..,,	D-3

II    Sample/Extract Storage and Turnaround Times            '<••  :
      and  Equipment and Standards	'..»-;»	D-4

      1      Sample/Extract Storage and Turnaround  Times	1,. .D-4
      2      Summary of Method	«j,:»	D-4
      3      Interferences	;..	D-5
      4      Apparatus and Materials	 *	D-6
      5      Reagents	-.^	*•„	D-ll
      6      Standards	,«„„,.,.;;	D-12

III   Instrument Quality Control Procedures and Requirements	D-16

      7      Instrument Operating Conditions	D-16
      8      Calibration of the GC5, Sj^ft^B —lamt.ial Calibration	D-17
      9      Calibration of the GCK%stem  -''datotgtatijjn Check	D-21
      10     Calibration of the GC Sgptem  - PVS,!r£ ! .. v..»	D-24
      11     System Performance - GC 'Resolutioa.1,	D-28
                                       *v ;\    ' ,
IV    Sample Analysis and Compound Identrifjabation  and  Quantitation	D-30
      12    Summary.....,,«.,,,.««	D-30
      13    Phase  Separation!!.. ^>	v*,	D-31
      14    Solvent ^Kt;raction and;,Cleanup. .. r,_»	D-31
      15    Solid  PKs^e Extracticto^and Cleanup	D-35
      16    Sample,;RCieparation a^iigE^str,act,ion  - Oil  Samples	D-38
      17    Sample' P«^^aration ^^i^tt^ate^ion  - Wipe Samples	D-39
      18    Instrumental Dialysis	D-41
      19    Dilutions	,\.J. .*	D-43
      20    Identification of !f|iKget Compounds	D-45
      21    CaJbctjOka«i»ns	."; v.:j;U	D-46
      22   ^'^iSitffitrif'j^c^ptance Criteria	D-48
      23 ; ;'i Corrective Acsf^Lon	D-49
      2V;;'! Documentation. .'-;|w	D-50
       •iff                  1r
V     s^fimple Quality Control;[procedures and Requirements	D-51
     ^'                        * '
      25    ,l^£hod Blank Anal^is	D-51
      26    'lijssbzaiment Blanfe;l^nalysis	D-54
      27    Laboxafeary Coutarol Samples	D-57
                                   D-2-PHEN-Q                            8/23/94

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                                                                     DRAFT

                             SECTION  I

                            INTRODUCTION
This Quick Turnaround Method (QTM) is designed fb^.-use in determining
the concentration  of  various phenolic compounds inHwater, soil/solid,
oil, and wipe samples.   Exhibit C lists the eompounds^iHiait will  be
determined by this method along with the Contract Requireld %iantitation
Limits  (CRQLs).  The  method yields identification and quantiSsafclon of
the analytes listed in Exhibit C using.sfingle column gas
chromatography/flame  ionization detector (GC/FID) or gas
chromatography/photoionization detector (GC/PID) «,•?•' Target compound
concentrations in  samples are reported on an "asf-ireceived" basis;  no dry
weights are calculated.   The primary•sohjsectivertiif this QTM is  to provide
analytical data in a  timely manner for -3ecti.sj.oii*making during  site
inspections, remediations,  and emergency removal activities.   The  phenol
QTM is to be used  when rapid data turnaround iS,,,$Bquired, when the data
requestor knows of (or strongly suspects)  the preseikse of phenol
contamination, and there  is,|knpwledge regarding potential matrix
interferences at the  site.  :jf?h%-fQ|M^s*:npt equivalent to, nor  a
replacement for, the  CLP  OrganJ.cs' Muliri^fet^'lMulti,-Concentration
Analysis.                     ;          •:••  '  "" - :: f!
                            D-3-PHEN-Q                            8/23/94

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                                                                          DRAFT

                                   SECTION II
                  SAMPLE/EXTRACT STORAGE AND TURNAROUND TIMES
                                      AND
                            EQUIPMENT AND STANDARDS  ,
1     Sample/Extract Storage and Turnaround Times              : ,

1 . 1   Procedures for Sample Storage            ,                    t ,-'

      Samples shall be protected from  light; srnd refrigerated at 4°C (± 2°C)
      from the time of receipt until 60  days? after delivery of a complete data
      package to the Agency .              ~            v *

1 . 2   Procedure for Sample Extract Storage     ;„

      Sample extracts shall be protected from light aad, stored at 4°C (± 2°C)
      for 21 days after delivery of a  complete data paiclcage to the Agency.
      Samples, sample extracts, /and-^ standards  shall be stored separately.
                                 '"' ,    ""'"<';', *--,;-;s£'"4' ,
1 . 3   Contract Required Sample Turnaround Times ;,  :

      Samples shall be extracted, analyzed, .-land a  summary of the analytical
      and QC data shall be reported to the appropriate EPA Region via
      telecommunications network within 48 hours  (or 72 hours if more than
      three fractions are analyzed) of Validated Time of Sample Receipt
      (VTSR) .  See Exhibit's A and B for speotlfiLc instructions  concerning
      sample turnarovind time and; data  reporting requirements .

2     Summary of Me€faod          Y-.
                   ^•^       A! SifrX:^ J=
2.1   This analytical method is  a GC/FID  or GC/PID method for the analysis of
      phenols in water, stSSJfCsolid, oil,  and wipe  samples.   All target
      compounds and the SystewfKonitor Compound (SMC) shall be extracted from
      field and ;@C',-samples utilfizJLjig. either solvent or solid phase extraction
      (SPE>j|: |lf':'~sblv^|t,,-«xtraction!'i^S utilized, field and QC samples are
      serjyilly extracted >js|sing two 10  mL  portions  of methylene chloride
      (M^eGi^) under basic %|id acidic conditions.   If SPE is utilized, field
      and QC samples are pa|sed  through a disk containing a solid matrix
        . g. , silica) coated ^Ifth a chemically  bonded styrene di vinyl benzene
            organic phase (03: ^equivalent) .  The target compounds and SMC are
                  from the ^traction  disk with methylene chloride.
           "•>,,*"'" '* x ,            «-,
            ''Xi'^S.         "'' "5"
2.2   Sample arimysses shaj.l"ibe performed  using gas chromatographic techniques
      within a confeCa^-fT^spiiecified analytical sequence that shall not exceed 24
      hours.  Target cscnapbunds are identified  and  quantitated on the basis of
      retention time windows and calibration factors established during
      initial calibration.  During initial calibration, a mean relative

                                  D-4-PHEN-Q                            8/23/94

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                                                                           DRAFT

       retention time (RRT),  a mean retention time  (RT),  and an identification
       window (± 0.008 RRT unit of the mean RRT or  ±  1.0  percent of the mean
       RT)  is established for each compound.  Mean  calibration factors are also
       established during the initial calibration and sine percent relative
       standard deviation (%RSD) of the calibration factors  for each target
       compound and the SMC must be less than or equal-'-.to 25.0 percent.   Sample
       compound concentrations are calculated from tile initial calibration
       using the average of the three calibration factors, u^iEgs-the mid point
       calibration factor (if it is within ± 10 percent of the a^eifeage of the
       high and low calibration factors), or usiijg  line segments (K C«Eve).
                                              '•», •                       -''I-  ,
2.3    A  check of the initial calibration shall be performed no less than every
       24 hours by the analysis of the mid point standard.   All calibration
       factors calculated from the calibration check  sjaaSdard must be within
       ±35.0 percent of the  mean calibratitJ^SSactor  Calculated from the
       initial calibration for each target compound .and the  SMC.

2.4    An analytical sequence also includes method blanks and instrument  blanks
       in which no compound can be observed at signals greater than one-half
       the  response in the corresponding RRT window of the 'initial calibration
       low  concentration standard,^: lfe,||^3.jt^cal sequence  shall  also include
       the  analysis of Laboratory Tfeatrol' Samplfe^: i^ySS) -and  Performance
       Verification Standards (PVS) Hf|The LCS wiiS. !T>e"-Ha;*go/no-go" analysis.
       That is,  if the LCS meets perfiiEfflance qjjiteria as  stated in paragraph
       27,  sample analysis may proceed/ Iilf, ?-$i0wever, the LCS  does not meet
       acceptance criteria, corrective action Imust be taken  before sample
       analyses are performed.   The PVS is tp^o times the  concentration of the
       low  calibration sta^wisjt^iand shall be analyzed at  least once during each
       analytical sequela*1'to vesrj|;y instrume^g performance.   All  samples shall
       be bracketed by;;;wilid  PVS ja|jfilyses or a:l%alid initial calibration  or  a
       valid calibration check staplard and a valid PVS.

2.5    A  System Moni-feB>r^eompound;ilii®!;iMl^||'sSe added to all field and QC
       samples  and stariistSa,  The SMC is used as a retention  time marker to
       calculate RRTs  for'tfwf identification of target compounds and to assess
       extraction efficiency,  sllfaen the recovery of the SMC  in a field sample
       is less; ,,-?ifc|a$]M> percent, 'glsfelfteex than 200 percent,  or if peak
                      -®fc>|^r;esent,  absolute retention times are  used for target
                identificfetpjen.   The  SMC recovery criterion  of  50-150  percent
       is^&visory only.   Relci*alysis  of samples are not performed  if the  SMC
       r$c&very in the samplers outside the advisory limits.
      •5 '*                    M %*
     •-• '«•                     *r'
3    " -I&iasacferences          it'
3.1   Polynuttlseai:,,aromatic^bjprocarbons may be present with phenols in some
      samples, "^t^ntionRiffles  for  target PAHs are given in Table 2 using the
      GC conditiorisl:Js^cf||ied  in Section III.
3.2   A number of method* interferences  may affect quantitative determination
      of phenolic compounds using  this  method.   The FID detector is relatively

                                   D-5-PHEN-Q                           8/23/94

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                                                                           DRAFT

      nonspecific;  it will respond to all molecules containing  carbon-
      hydrogen bonds including phthalate esters and PAHs.  It is  incumbent on
      the  data requestor to establish that phenols on the Target  Compound List
      (TCL)  are the primary extractable contaminants at a site  before using
      this method to establish their concentration.  ;

3.3   Degradation of phenols will occur if the GC,i»jecti0a.,port  becomes
      contaminated with nonvolatile residues.  Low'recoveries &f,  the  LCS and
      PVS  compounds may indicate injection port contamination. tJssalysts must
      clean  or replace injection ports if this-contamination occurs,;;,;, Analysis
      of colored extracts or samples from contaminated sites may  require more
      frequent GC maintenance.              f:V

5.4   The  analytical system must be demonstrated to b^tfree from  contamination
      under  conditions of the analysis by Taaiiiyzing sfcgfhod blanks.  Cross-
      contamination problems can be minimized l»y analyzing instrument blanks
      after  samples with high levels of target compounds or other interferents
      (see paragraph 26).                           '-,'-•
                                                       '  *• I
4     Apparatus and Materials    -,,-„ ,                      • ^
                                  :[,,';.  j>;;!-.,,„
                                 % 5.S;*  * { '^~\~- '' *'' " ^ '/'
      Brand  names,  suppliers, and%art nuilb^l^^jeJ&«;,:,illustrative purposes
      only.  No endorsement is  implied.   Equiv^,lent;*pei£ormance may be
      achieved using apparatus  and materials .ai&her than those specified here;
      however,  demonstration of equivalent p&Bformance meeting  the
      requirements  of this SOW is the resfyosslbility of the Contractor.

4.1   Gas  Chromatograph,-j."fijse'Has chromatdgasaphy (GC) system shall be capable
      of temperature p#p|^ammli|g,*53nd flow coapstirol that is stable  throughout an
      analytical seqaeilce.   The Ts^tem shall  %e. suitable for splitless  or on-
      column injection and have aM.  required accessories,  including syringes,
      analytical colaamns,  and gasejs,. ^All GC  carrier gas lines  shall  be
      constructed fi«a,gstainles4:i^^&7li3:iiiicPpper tubing.  Non-
      polytetrafluoroe-l^iene (PTFE) thread sealants, or flow controllers with
      rubber components s"hall snot be used.
      4.1.1 Ga^s-^to^aatography IG&^BBQ - 15 m x 0.53 mm ID bonded phase
            :|siff-iconi-.<4^Cfd fused silica capillary column (Supelco SPB-5,  J&W
         -  jlt>B-5, Restedv|j•• ;^__	           Si**'.
      4.1.3 Gas chrJiaiiaispgfcaphy injector - A deactivated injector specifically
            designed fijritse with 0.53 mm ID columns shall be used for
            collecting data with this method.  The Laboratory shall establish
            which of the various injector liner design provides optimum

                                   D-6-PHEN-Q                           8/23/94

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                                                                           DRAFT

             performance with their specific GC hardware.  Laboratories that
             have  difficulty using this method shall investigate the use of
             injector liners with shapes or dimensions optimized to reduce
             injection flashback and analyte pyrolysis, .

4.2   Data  System -  The GC  shall be linked to a data '^system. capable of
      integrating peak areas for any compound detected at or above one -half
      the CRQL, providing retention time labeling, -and relative retention time
      comparison.  It is required that the Laboratory be equipped-fwith a  PC-
      or microcomputer-based GC data collection and reduction systWlfor  this
      purpose.  The  Laboratory shall possess ,,t^ls equipment to provide ;
      quick turnaround of electronic data. .pChe Laboratory shall also be
      equipped with  a microcomputer and cordtact- specified hardware and
      software to electronically transfer 'vt&e QTM datapfco the Regions.
4.3   Solid Phase Extraction Disk Processing 'St^ciotf:- As SPE is a developing
      area in environmental chemistry,  EPA expects £hat advances will occur
      within the lifetime of the  QTM contracts.   Therefore,  the brand names
      listed below are  included for  illustration purposes .only.  Any
      comparable equipment is  acceptable,  regardless of bramd.
      4.3.1 Extraction disks  - Di'sllss  shall^b^-ktaitle Joi-Ieflon and include at
            least 500 mg of styrene ,i$ivinyl benfienes ^SHl) bonded silica
            (Varian/3M Empore",  or equivalent)'.:  Disks shall be 47 mm in
            diameter.  (Note: an alternative, :f*hase may be used if this phase
            can be demonstrated  to meet ;tfee 'QA/QC requirements of this
            method.)                       ;

      4.3.2 Vacuum holder'- Tne|j;9$acuum holde$jplll be glass and comprised of
            five (5) ,»||arts: the  x^teuum head, iSje  sample reservoir, a metal
            clip tojhftld the  resei^pir to  the head,  a large volume receiver
            (greater, "than 200 mL> ^r^^e^sample  after elution,  and a small
            volume receiver (10-|2fl|pL|'!^jio'ir$he  solvent after extraction.  The
            vacuum holbeic-^except for the  solvent receiver)  is sold as a HPLC
            solvent f iltracl*^ device (Gelman 4012,  or equivalent).   The
            solvent receiver §€s|»imply a tube with a ground glass fitting that
                '     s=the vacuum

      4.3-«>;3:1::Vacuum manifblS.; - A 4- to 6-port vacuum manifold may be used to
       ,l '>? facilitate simti3jt|eneous disk extractions.

     ,4f3.4 Use of depth filter (Whatman Multigrade GMF  150,  or equivalent) or
      '--S;',!,:-,, inert materials sScch as Celite 545  (diatomaceous' earth,  Baker #,
         ! :K;»*]C; equivalent) &%& encouraged when  samples contain particulates.
           "1B|sa$pth filtecsjare utilized, each lot shall be  tested for
            contamination .jjclor to use with this method.  The depth filters
            may be '^e^ke^'-iin conjunction with  the SPE disks  (depth filters
            are placeStiiaU-top of the SPE disks) by following  the procedure
            outlined in paragraph 4.3.5.
                                  D-7-PHEN-Q                            8/23/94

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                                                                    DRAFT

4.3.5 Solid Phase Extraction (SPE) Recovery Check

      4.3.5.1     Summary

                  Before field or QC samples ar>e; extracted using the SPE
                  disks, their efficiency shall" lie, verified.   An
                  extraction recovery and cotttamiriatifaia check shall be
                  performed in order to evaluate the i*ecoyery of
                  compounds on the disk, and to check  for contamination.

      4.3.5.2     Frequency            ;                           :"

                  A check shall be performed on each individual lot of
                  disks , and for ev«ry 300 units^f a  particular lot .

      4.3.5.3     Procedure             '•',<  .  %•
                                              ' ';
                  4.3.5.3.1   Before samples aite extracted using a lot
                              of SPE disks, the Lairipi3?atory shall perform
                           ,;> -a, recovery check of  thafe'lot.   Two (2)
                           :>, 
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                                                                DRAPT

                          analyzed according to the procedures in
                          Section IV.

             4.3.5.3.3    The SPE recovery check standard  solutions
                          shall be analyzedlin a valid  initial
                          calibration or jClaily^calibration
                          analytical sequence (see paragraph 18.1).
                          Note:  if the SPE recovery lisbeck  standards
                          are the only samples analyzed'- in the
                          analytical,:;«equence , the method <%lank
                          shall be ^replaced with an instrument blank
                          and the £U5S shall be prepared by diluting
                          100 jiL-^f LCS stock^BELxture into 5 mL of
                          hexanfc.-aind concenfcicating to ImL  using
                          nitrogennMowdowEu '•;  The EPA identification
                          numbers fox Staadards as described in
                          Exhibit E sh'all;3>e used for the  low and
                          high SPE recovery *£&eck standard solutions
                          (i.e.,  QPHSTD####, ^ere #### is the
                      • , s^amount injected).  The 'IFA identification
                     -t;- "
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                                                                          DRAFT

                         Laboratory during the term of the contract and shall
                         be available to the Agency during on- site laboratory
                         evaluations or if requested by the TPO or APO.

4.4   Glassware  - Sufficient glassware to meet contract requirements shall be
      reserved for  exclusive use in support of this.eoataBact.

      4.4.1       Erlenmeyer Flasks - 50 and 125 mL.           v

      4.4.2       Beaker - 150 mL.             •<                    ,

      4.4.3       Concentrator tubes - 10 mL,

      4.4.4       Kimax concentrator tube (graduated) ^f ,25 mL.

      4.4.5       Graduated test tubes - graduated .from 1 to 10 mL.

      4.4.6       Autosampler vials - appropriate far,! tie GC system.

      4.4.7       Wide-mouth centrifuge tubes (optional).
                                 ^j,f  ^r,,
      4.4.8       Powder funnel -'c
      4.4.9       Centrifuge tubes - 40 mL.
                                      vr •
      4.4.10      Pasteur Pipets.           ,'

      4.4.11
4.5   Laboratory HardWpre -  The fallowing equipment is required for sample
      preparation: .; -:            :5,-,
                  ;p; v            !%,,»
      4.5.1       tttlpcasonic Ceil'^^fe^aglec:- Heat Systems Ultrasonics, Inc.
                  Mo dell ^-,35 5 Sonicator (475  watt with pulsing capability, No.
                  200  1/2"jfaagped disrupter horn plus No. 419 1/8" standard
                  tapered mieitojt^p probe) ,  or equivalent device with a minimum
                  ?o£.3-75  watt oiufcgpt,,,capability.  The 1/8" microtip shall be
            :;:,;;  -tisecL-,£«r.  extractl«^,',bf all  soil samples.  (NOTE: In order to
          */,  :     ensure!'lj|bat sufficient energy is transferred to the sample
        Ai /       during  t:liei<*xtraction,  the  microtip probe must be replaced
                  if the  tipffcegins to erode.  Erosion of the tip is evidenced
                  by a rough|-£urface.)

                  Balance - jd&librated and accurate to 0.1 g.
             ' \              v1'
      4.5.3    "v :, Balance^-'Calibrated and accurate to 0.1 mg.

      4.5.4       CenfcillLdiige.
      4.5.5       Microsyringe -  10-fiL,  50-^L, and 100-^L.

                                  D-10-PHEN-Q                           8/23/94

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                                                                           DRAFT

       4.5.6       Spatula - Stainless steel.

       4.5.7       Hot plate stirrer.

       4.5.8       Teflon coated magnets.             . ,

       4.5.9       Glass wool.                               .

       4.5.10      Whatman #42 filter paper.                     •- \

       4.5.11      Whatman vacuum holder.     ,,"'"                         ;

       4.5.12      Nitrogen blowdown apparatodub.

       4.5.13      Water bath.                ?  „     .- '

       4.5.14      pH paper or meter.                ;

5      Reagents                                         • I"

5.1    Reagent water - Reagent wa*as@r-iii;S£i|(SefiBed.,>as water in which target
       compounds or potentially interfering cdDipomds do not produce a signal
       greater than one-half the response in  the corresponding RRT window of
       the  initial calibration low coiicsntratiotl standard.   Reagent water shall
       be generated by one of the following methods.
                                             '•,!
       5.1.1 Reagent water may be generated iry passing tap water through a
             carbon filter bed Containing approximately  500 g  of activated
             carbon (Catgon Corp,^|,,Filtrasorb;f3pO, or equivalent).
                     •  !          'I • .
       5.1.2 Reagent;«mter may be ^generated using a water purification system
             (Millippre-0-Plus wiffclQrganex _CJ cartridges,  or equivalent).
                    !  '.<•'-,      . ^)iv*4k! "'"9,2" '«; j-
       5.1.3 Reagent waiakr,aa-ay prepared by boiling for 15 minutes  then bubbling
             contaminant-free; Inert gas through the water for  one  hour while
             maintaining the watbe*; temperature at 90°C.   While still hot,
             transrfeir  the degasseSr^ter to a narrow-mouth screw-cap bottle,
            .^al'^wlth^ feflon-line% septum, and cap.

5.2    SoJtvsfents -  Acetonitr5&|.,  acetone,  methylene chloride, and methanol
        ^sticide  quality,  or;liquivalent).
5.3  'iS^iJ|Mm hydroxide solution (0.5 N).
        "^'i'J^-              4:
5.4   Hydrocfn||«r^.c acid so^cfi^Lon (0.5 N).

5.5   5:100 methandl/^srater,,Solution.

5.6   50:50 methylene  chloride/acetone solution.
                                  D-11-PHEN-Q                            8/23/94

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                                                                          DRAFT

5.7   Powdered Anhydrous Sodium sulfate.

5.8   Sodium chloride.

5.9   9:1 acetonitrile/acetone solution.              ^

5.10  Corn oil.                                     ;

6     Standards                                                   •

6.1   Stock Standard Solutions                :

      Stock solutions may be prepared from pure  standard materials  or
      purchased as certified solutions .  Standard  solutions  shall be  prepared
      by dissolving pure standards in a suitable solvsent in  volumetric flasks.
      The addition of toluene may be necessary ta»  dissolve some  of  the target
      compounds in highly concentrated stock  standards.  When compound purity
      is assayed to be 96 percent or greater, the  weight may be  used  without
      correction to calculate the concentration  of the irtoeJs standard.
      Exhibit E, Section V provides. .further directions for^preparing  and
      verifying the integrity of --stock; jsfeai^dard  solutions .

6.2   Secondary Dilution Standards '\ ,_        ,'•    '~   ,.','

      6.2.1 Using stock standard solutions, -prepare secondary dilution
            standards in acetonitrile i£ 'SIfEMs  used  for sample  preparation or
            methylene chloride if solvent Extraction  is  used for sample
            preparation. :  •>;' . * c , ,         " ;

      6.2.2 Secondary,4ftilution s^idards shaft. :i>e  stored at  4°C  (±  2«C) with
            minimaLstofeadspace and; Checked  frequently  for signs of degradation
            or evaporation.   These <;prEp,cedures are  especially important just
            prior to preparing ::oa'libiriafeion;.:;:S:tandards  from them.
            NOTE: Standards, shall not be stored  in volumetric flasks,
            especially wKei ~t%ey are prepared with solvents  with low  boiling
            points.          --;'  .;

6.3                               '
            Calibration st'asSard mixtures  shall be prepared at three
            concentration lefells in volumetric flasks  and diluted to  final
            volume with methjjftene chloride if SPE is used for sample
            preparation or hexane if solvent  extraction is used for sample
            ^reparation.  Th*,5low concentration standard as specified in
            $83Sagraph 6 . 3 . 2Y^chieves the sample extract compound
            coneeaitxations Equivalent to the  sample compound CRQLs as listed
            in Exhib;itjC f^see paragraphs 14.1.17, 14.2.22,  and 15.5.8).   The
            high conceiifcaSartion level shall be near the upper end of the  linear
            range.  The compounds and concentrations used for these
            calibration mixtures are presented in paragraph 6.3.2. NOTE:  The

                                  D-12-PHEN-Q                          8/23/94

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                                                                           DRAFT

            high  level standard concentrations are  the minimum required under
            this  method.  The Laboratory may prepare  standards at higher
            concentration levels as long as the %RSD  criteria are met.

      6.3.2 Phenols calibration standard mix concentrations.
                                                        i-
                   Calibration Ranges  (/jg/mL)
                                                              "*,"
                   Compound	Low	Mid     'High
Phenol
2 - Chlorophenol
o-Cresol ; ,
m-Cresol*
2 -Nitrophenol
2 ,4-Dimethylphenol
2 ,4-Dichlorophenol
4-Chloro-3-Methyl Phenol
2,4, 6 -Tr ichlorophenol**
2 ,4-Dinitrophenol
4 -Nitrophenol , " ;1 " ',^-' •" f • •>
2,3,4, 6 -TetrachlS»ropheh61;>'
•4 , 6-Dinitro-2-metb$lphenol
Pentachlorophenol !t , ,
o-Bromophenol (SMC) ?
s § .0
,5.0
5.0
5.0
< 5.0
5-J&.
s.e, ,
5.0
5.0
5.0
,:5.0
';'!S»:SO.; ,
y$ ' '
-,Trichlorophenol.  Quantitation will be
                        .based o^|ii|t;!--iesBliijral;ion factor of 2,4,6-
                        • Ihcichlorophenol .
       6.3.3      All standards* £daall be stored at 4<>C  (± 2<>C)  in Teflon-
                  sealed amber gla^s bottles .  Calibration solutions  shall be
                            after 6Niaoi*ths, or sooner if comparison with check
                            ^indicates a problem.  CAUTION: Phenols are
        ,t ' :       particulssrly susceptible to photode gradation.
       $:*'                 "^-
6.4  .^libration Check Standard
      1'.. ^S' /                   \~- i
       ''• "'••.. -                   j' ;"
      The«.«cMi.bration check ,fi a daily one -point check on the initial
      calibratjfes^.  The calibration check standard shall be prepared  in a
      volume tr£ci::Jlau?k and. fluted to final volume with acetonitrile  if SPE is
      used for samp'Sft1 preparation or hexane if solvent extraction is  used  for
      sample preparatitjlt.,^ The concentration of the calibration check standard
      is the same as  the -mid  level standard used in the initial calibration.
                                  D-13-PHEN-Q                            8/23/94

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                                                                          DRAFT

6.5   System Monitor Compound

      The System Monitor Compound  (SMC),  o-Bromophenolj, shall be employed to
      detect retention time shifts  (RTS)  of eluting compounds.  Additionally,
      the same compound shall be used to  monitor the sexstraction efficiency.
      The Laboratory shall prepare  a solution in methaoiol containing
      o-Bromophenol at a concentration of 2 mg/mL. ; The Laboratory shall add
      25 jiL of this standard to a  100-mL  water sample,  or 25 fSk to 6 grams of
      soil.  For oil analysis, prepare o-Bromophenol at a concentration of 50
      fj.g/mL and add 1 mL of this solution to 1 *g of oil sample (see section
      IV.)                                    ;""                     ""•-  ::

6.6   Performance Verification Standard

      The Performance Verification  Standard CPV.S) shall be analyzed at least
      once during each analytical  sequence to *s&?essrsystem stability.   The
      PVS is two times the concentration  of the  'low -level calibration
      standard.

6.7   Laboratory Control Sample  .x                         ;
                                ,. •-,  ^  '% ^ '  *" f~.
      Laboratory Control Samples 'tl|?S) corita^iii^, loaoi^-amounts of target
      compounds traceable to primar%-<^standards,|*jf.il IfilttaLally be supplied by
      the Agency.  Following receipt ;»f these-initial supplies, however, the
      Laboratory shall prepare its  own^^LCS sitandards.   The LCS shall be spiked
      into a clean matrix and prepared using).all steps  of this protocol.  An
      appropriate amount of the LCS shall', T»e added to reagent water and
      analyzed with each BattaiM'of water samples.  An appropriate amount of the
      LCS shall be added'to clea%-quartz  sanllfand analyzed with each Batch of
      soil/solid samples.  An appropriate amo:tet of the LCS shall be added to
      clean corn oil-,and analyzedijrith each Batch of oil samples.  If a Batch
      contains wat«r,r soil/soli<^:j|5Jn,dro,il,,samples,  an LCS shall be prepared
      and analyzed for- ;ieach natar&&',,t>i8<>.t^«-|J3E wipe sample analyses are
      performed, the Agieac^r will provide  the Laboratory with further
      instructions for the%«£eparation and analysis of LCSs for wipe samples.
      All LCS compounds must'^^e; .recoveries between 30 and 130 percent before
      sample analysis may begin (spse, paragraph 27).

      NOTE,?,  The Laborata^ ..is expected to maintain control charts of the
      recoveries of at leas^jthree  representative LCS compounds as an internal
      QCh-p'rocedure.         *$"

6.8   'Storage of Standard Solutions

      6.8.1 :$iffcfb&,,. secondarjjfc-istandard solutions, and working standard
            solcttioas shaMfbe stored at  4°C (±  2°C) in Teflon-lined screw-cap
            amber bettlles^also see paragraph 6.3.3).
      6.8.2 All  standards  shall be protected from light.  CAUTION: Phenols are
            particularly susceptible  to photodegradation.

                                  D-14-PHEN-Q                           8/23/94

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                                                                   DRAFT
6.8.3 Samples,  sample extracts,  and standards shall be stored
      separately.
                           D-15-PHEN-Q                          8/23/94

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                                                                     DRAFT

                             SECTION III

       INSTRUMENT QUALITY CONTROL PROCEDURES AND REQUIREMENTS


 Instrument Operating Conditions              „  -  =

 The following are the suggested gas chromatographic analytical
 conditions.

 Column:      DB-5 (J&W Scientific), or  equivalent,  15-m x 0.53-naa ID,
             0.25 to 1.0 fw film thickaeiss

 Carrier Gas:                       j     Helium  >.
 Flow Rate:                             ;: ,5  - 7  aL/min
 Injector Temperature:                    &00»C  j*
 Detector Temperature (FID):              3000C
 Detector Temperature (PID):              300°C  **
 Initial Temperature:                     65°C     >:
 Initial Hold Time:           -:,           3  min
 Initial Ramp Rate:         \  £  ;    ~>    10°C /min
 Intermediate Temperature:  '  ;:      ': ''-',!|85*C;.'
 Intermediate Hold Time:       =          ,1  min
 Ramp Rate 2:                     ,        30°C/min
 Final Temperature:               :         275"C
 Final Hold Time:                     .    5  min

 * Cold on-column injectors that allow;injection directly into 0.53 mm ID
 columns may be used for t&iis method as 'jfeong as the column resolution
 criteria in paragraph 11 aiie:met.       ' ~
               A
 ** Or as specified by the aianufacturer., The detector temperature shall
 be sufficient!^1 ;Mgher tbao!'ll:S|.7f&jalj; column temperature to prevent
 phenols from condensing on the detector.

 FID requires hydrogen anil; air supplies  to  the  detector according to
                specifications, ,
 The;,;fl'l5 requires a':l^«2-ev bulb.
   •>: •'                *'"'- '''%
   "K •'-                 ')-,*
     Laboratory shall »N&e in the Batch  Narrative the detector type used.
:"H01|E; The typical run time under these  conditions is 25 minutes.  It may
 be"''n«c^|sary to adjustffSSC conditions  on individual instruments to
 optimisil^PniP011110^ separation.  It may be necessary to adjust detector
 conditions; tOt^optimi^se' instrument sensitivity.
                             D-16-PHEN-Q                           8/23/94

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                                                                           DRAFT

8      Calibration of the GC System - Initial Calibration

8.1    Summary

       8.1.1  Prior to the analysis of samples and required blanks,  each GC
             system must be initially calibrated to ,««ST£fee that the instrument
             meets the minimum performance requirements  of tjhe method.   The
             initial calibration is accomplished by analyzing'fjbree standards;
             the  low level, mid level, and high level mixtures asxispecified in
             paragraph 6.3.2.   The technical aceejjtance  criteria fbr'ithe
             initial calibration are given in paragraph  8.5.   The initial
             calibration shall be used to esjfcaSlish the  calibration factors
             used for compound quantitation^lfco define tifee retention time
             windows for compound identification, and tovldetermine  the  mean SMC
             retention time for evaluating SlK3j*,shift <&klng analyses.   Detector
             response must be linear for all target coinpounds.   All samples
             shall be analyzed during the contract specified 24-hour analytical
             sequence.

       8.1.2  Sample quantitation shall, be based on the mean compound
             calibration factor, liB6^»)^ie«teSj,.^"K" curve),  or the  mid  level
             calibration factor from the iii£:elal.'-gCa,I£bza.tion.   (The use of the
             line segment or "K" curve^is suggested.')  'All field and QC samples
             and  standards within a Batch and ^11 field  and QC samples  and
             standards analyzed in the same analytical sequence shall be
             quantitated using the same qiaaafcitation method.

       8.1.3  Compound identification shall be based on RRT windows  established
             during inttat«l' cal"S%|ation in alltpield samples  where  the  SMC
             recovery yifcs greater "f;bsn or equalise* 10 percent and less than or
             equal tp,t«00 percent s"*«

       8.1.4  Compound-,4deritifica4Sliit'^s8a^U;-:Jfe^'*"based on absolute retention time
             windows estrsiiliished during initial calibration in all  field
             samples where •'SagrajSMC recovery is  less than 10 percent,  greater
             than 200 percent7-4% if peak interferences  are present.

       8.1.5  ^£T"ty""infi<>t^';chromatogr'i|^hic peaks shall be evaluated by
          ,.v;r comparing tn'te^HT- of the SMC in all analyses  with the mean  RT of
        /";;"->'  the  SMC calculai&sd from the initial calibration.   The  retention
       .j|j, :   time shift is referred to as RTS or RT ZD (see paragraph 21.4.1).
      %°-JC    The  RT of the SM<3|f?or field and QC sample analyses must be within
       ^•4^ .± 1-0 percent of^fcjie mean RT calculated from the  initial
         '%!, Calibration.    ('-'•'

8.2   Frequency7  :-Xj;_:.    ; ;!

       8.2.1  An initial ,:^j*ee-point calibration shall be  performed  to determine
             the  linearity of  response of all target compounds  and  the  SMC.   A
             new  initial calibration is required whenever calibration check

                                  D-17-PHEN-Q                            8/23/94

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                                                                           DRAFT

            standards  or  PVSs cannot satisfy QC criteria.  A new initial
            calibration is  required whenever major instrument maintenance has
            been performed  such as column or detector replacement.  An  initial
            calibration must be performed for each GQ-«nd for each
            chromatographic column which are used to>.,;i»erform these analyses.

      8.2.2 An analytical sequence is a contractually-defiled sequence  of GC
            analyses which  consists of an initial three-point:''Calibration or a
            valid calibration check,  field samples, LCS,  method atvd instrument
            blanks, PVS,  and other QC samples^tom within a 24-hour period (see
            paragraph  18  for the required segitence of samples).

      8.2.3 Analysis of the initial calibration shall begin with the injection
            of the high level standard fallowed by the-'oid level and low  level
            standards.                     '•»£„. = v      /;, "
      8.2.4 The analytical  sequence concludes wit&jan acceptable analysis  of
            an instrument blank and a PVS  (see paragraph 10).

      8.2.5 Samples shall be  analysed only after meeting tfee technical
            acceptance criteria <^£Ht^e.^m^|,al calibration or a valid
            calibration check stats|ard.   ~s~&-"-'-»^i jfs "~}., - ,t
                                               4 '•"*    '   ?J
8.3   Procedure                               /•

      8.3.1 The GC system shall be set tip .pea: the requirements of paragraph  7.

      8.3.2 Prepare califeegxtlian. standard s&ku^tions containing the SMC and  all
            target compounds  using the procedure listed in paragraph 6.3.

      8.3.3 The calibration solutions shall be -equilibrated to ambient
            temperature before iftjfec^ion,(^approximately 1 hour).

      8.3.4 Inject between,!  and 5 pL of each calibration standard.  The same
            injection voltase}vshall be used for all calibrations and field/QC
            sample analyses.''   ;. ,

8.4   Calcuiatltfhs"  *,';„,,- _        '"'~\"

            Calculate the *M|a.bration factor (ratio of the total peak area or
            height to the m^i's injected) for each target compound and SMC  in
            the three initiat-cealibration  standard analyses using equation D.I
            (EQ. D.I).      r


                         r^2*.n,. - Total Area of Peak or Peak Height       EC*-  D-1
                        XvCtCT&C/Z ~ ' -• —I '—— •- _. _i— . ,f« -.§ .. ,-» ——- — — ...-,-, «_v^_ ...
                        ^                Mass injected (ng)
                                  D-18-PHEN-Q                            8/23/94

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                                                                    DRAFT

8.4.2 Calculate  the  mean calibration factor for each target compound and
      the  SMC.

8.A.3 Calculate  the  %RSD of the calibration factors of the low level,
      mid  level,  and high level standards for the initial calibration
      using  the  following equation.           ',    "
      where SD -  standard deviation.               ,»•

      Standard deviation is  calculatedaising the following equation.
                           _  If
                             Nft
   w  ,_.  _^2                          EQ.  D.3
   —«^  » i  "/
   ^   AT — 1            *
   :1   •"  J-
      where:  x^ = individual, calibration •£-actor {.per compound).

              x  - mean of three  initial calibration factors (per
                   compound).         /

              N  = iiHBsliij^of  calibration standards.
      Equation JBji'4 is the  general  formula for the mean of a set of
      values. ' -'

           ': "X; j|<«-«ean of valaies.
              X.:
               J-
              N  = numteeir of values.
8.$ :& Ipalculate the
           Ion:
each target compound using  the  following
                            D-19-PHEN-Q                           8/23/94

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                                                                           DRAFT

      8.4.5 Calculate  the mean RRT and RT for each target compound by using
            equation D . 4 .

8.5   Technical Acceptance Criteria                   ",.

      8.5.1 The %RSD of the calibration factor for -,  i-        '".:
                                            ': ' '\       < <
      8.5.3 The peak resolution between o-cresol anclpi-cresol shall be
            evaluated  in the low level initial cal-ilMEation standard before
            proceeding with sample analyses (see paragraph 11 - System
            Performance) .                                 ;
      8.5.4 The chromatographic ffealt, izjespo&se. -f or all target compounds  in the
            low concentration stan&ard must W^greftt^ea; l< -than 10 percent  of
            full-scale  deflection.  °f ,         ,  >
                                               3-

8 . 6   Corrective Action                 -    ,!

      8.6.1 If the %RSD for more than  twa compounds in the initial calibration
            is greater  t&aa 'Sl5,i!0 percent or; if any compound exceeds 40.0
            percent RSB>j,:the itistaaoment has njfSt demonstrated adequate
            linear ityabo be used'"^>r this method.  Corrective action shall be
            taken anE 'documented.: | ,
      8.6.2 If the pe^Kxesolutioil:«ritl6M«»t is not met, the Laboratory shall
            perform corr*6t4ve action and demonstrate adequate resolution
            before samples icaai.be analyzed.

      8.6.3 If -sSfhe s^HG> _RT is  not'JM,tJxin ± 1.0 percent of the mean SMC RT
            !l|4l-!culatefcfeEi«m the thrfeftrjinitial calibration standards, the
         ,f s .^Laboratory sii«|l  perform corrective action which may include a new
        -•-IT  initial calibration.   Do not proceed with sample analysis until
      ,.'•%   the RTS is withi^'i 1.0 percent.
      '•},                     I"'
     "*8'^tt4 If the peak resp
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                                                                          DRAFT

      8.6.5 Corrective  action may include optimizing detector linearity by
            adjusting gas flows  (FID), cleaning detector optics (FID), or
            replacing the bulb (FID) .   Actions also may: include replacing the
            GC  injector liner, column, or the pre-colxam, removing 0.5 - 1m
            of  the  analytical column,  or replacement -efT the standards.

      8.6.6 All initial calibration technical acceptance criteria shall be met
            before  any  samples or required blanks are analyzed. -
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                                                                          DRAFT

      9.2.3 The analytical  sequence  shall be concluded with an acceptable
            analysis of an  instrument  blank and a PVS (see paragraph 10).

      9.2.4 Samples shall be  analyzed  only after meetiag the technical
            acceptance criteria  for  the  initial calibration or a valid
            calibration check standard.
                                                    !!
9.3   Procedure                                              :~, • ?

      9.3.1 The GC system shall  be set up per^ihe requirements of '^paragraph 7.

      9.3.2 Prepare calibration  check  standard solutions containing the  SMC
            and all target  compounds using ',fctie procedures listed in paragraph
            6.3 and 6.4.                  \'{

      9.3.3 The calibration solutions  shall be%feju^LU3>rated to ambient
            temperature before injection (approximately 1 hour).

      9.3.4 Inject between  1  and 5 (iL  of the mid level Standard.  The same
            injection volume  shall-vbe  used for all calibrations and field/QC
            sample analyses.     ; ''«-,  K,   : ,-s t/,. ^
                                 ** «  ""   * K* ':$•''? <*'^
9.4   Calculations                '  -j          :        ,  ,/

      9.4.1 Calculate the calibration :<£ac tori (ratio of the total peak area or
            height to the mass injected) foir?each target compound and the SMC
            in the calibration check standard mixture using the following
            equation.     §  -   >•


                        Factoz = ^tal ^ea of JfeaJc or PeaJ: Height        EQ- D-6
                                 l;       Mass injected (ng)
      9.4.2 Calculate the^lDF-jketween  the  calibration factors from the
            calibration check ,,sEtandard  and the  average calibration factors
            fros*-t&e initial calibration  using  the  following equation.

         -   '-'           • , '('-
        .','-"               5':.-:.       x -  x                                 EQ-  D-
        *r                  -'H-  %D =   _ c x 100
        " "                  =J,         x
                  where,    I? ;
                            ,in-
                  >i;>>. =  me^b of  three  initial  calibration factors (per
                  xc =  calibration factor  from current calibration check
                        standard  (per  compound).

                                  D-22-PHEN-Q                           8/23/94

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                                                                          DRAFT

9 . 5   Technical Acceptance  Criteria

      9.5.1 The %D between  the  calibration factors for -each target compound
            and SMC in  the  calibration check standard -and the mean calibration
            factor for  that compound in the initial calibration must be within
            ± 35.0 percent.  Up to  two target compoaads^iaay exceed ± 35.0 %D,
            however, all  compounds  must be within ±/&5.0 ,SKD_«

      9.5.2 All target  compound absolute and relative retention ytlaes must be
            within the  windows  established during the initial calffeation.
            Report calibration  check RT and B&T data on Form QI-PHEN '•(&&&
            Exhibit B).                     s , ;

      9.5.3 The retention time  of the SMC "3a the calibration check standard
            must be within  ±1.0 percent af *be mean=.$MC retention time
            calculated  from the three initial ' ':i|«Brcent.         -,;V-
              '
      9.6.4 If Tfee.i^eak re^saalution criterion is not met,  the Laboratory shall
            perform 4i*opgre«tive action and demonstrate  adequate  resolution
            before samples can be analyzed.
                                  D-23-PHEN-Q                           8/23/94

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                                                                           DRAFT

      9.6.5 All calibration check technical acceptance criteria  shall  be  met
            before  any samples  or required blanks are analyzed.  Any samples
            or required blanks  analyzed when the calibration check criteria
            have not been met shall require reanalysis at no additional cost
            to the  Agency.

9.7   Documentation

      Calibration check results are reported on Forms QI-PHEN, 
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                                                                          DRAFT

      10.3.2      The  PVS  is two times the concentration of the low level
                  standard from the initial calibration (see paragraph 6.3.2).
      10.3.3      The  PVS  solution shall be equilibrated to ambient
                  temperature prior to injection ( approximately 1 hour).

      10.3.4      The  same injection volume shall be used for, ail field and QC
                  samples  and standards including the FVS .       -  \,

      10.3.5      The  recovery of each compouiiS and the SMC in the PVS;:;is
                  quantitated using the mean =ealibration factor, the mid
                  point, or by using a K curve established during the initial
                  calibration.  NOTE: Only otxe method of- quant i tat ion shall be
                  used for analyses within-^a igiyen analytical sequence and for
                  a given  Batch of samples.  :- •'•:•;- •••  f •

10.4  Calculations                                    <;

      The amount of PVS compounds ^and, the SMC recovered shall be calculated
      using the following
                                     :=',%        '&**'    '  "'                  EQ.  D.8
                             Amount Observed*, «*=-
      Where:      A^    «O ;oax-ea or peak li^ght of the PVS compound or SMC.

                  CFi6; ' =      calibration fac'teai established by one of three
                      '•         tedbaaiques during the initial calibration (see
                                         ,211,  .
                                         ••"-..   JiS'  -
                                                         X 100         EQ .  D . 9
                                                   t
                                      Amount Added (ng)
10.5  TeclipScal Acceptancs4\iiriteria
                           '
                  All PVS taa^et  compounds must have a calculated recovery of
                  75-125 per<|iat  in order to report data without flags.
                             IP-"
                  If recover^-ibf  a  PVS  compound is  not within 75-125 percent
                  .but stillsiirthin  an expanded recovery window of 50-150
                  percent Jgtaie associated sample analyses results shall  be
                           5see paragraph 10.6).
      10.5.3      The SM& recovery  criterion of 50-150 percent is  advisory
                  only.  Reanalysis of  the PVS  is  not performed if the SMC

                                  D-25-PHEN-Q                •           8/23/94

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                                                                          DRAFT

                  recovery  is  outside  the advisory recovery limits.  The SMC
                  recovery  in  the  PVS  must,  however,  be greater than or equal
                  to 20 percent and less  than or equal'to 200 percent  (see
                  paragraph 10.6).

      10.5.4      All  target compound  retention and re-lsati-ve retention times
                  must be within the windows established during the initial
                  calibration.   Report PVS RT and KRT data on l*orm QI-PHEN
                  (see Exhibit B).                                ;

      10.5.5      The  RTS for  the  SMC  in  the iFKS must be ± 1.0 percent "between
                  the  PVS SMC  RT and the  SMJp^ean RT calculated from the
                  initial calibration.     '">           -S'

      10.5.6      The  peak  resolution  betweeuf»Q-creso;l. 'and m-cresol shall be
                  evaluated in the PVS before p3roc.eeiding with sample analyses
                  (see paragraph 11 -  System Performance).

10.6  Corrective Action                                 :

      10.6.1      If recovery  o&^3PBSl'.£aM|H>wii4 i-s not within 75-125 percent
                  but  still withiifean  exp'anQe&asecovery, window of 50-150
                  percent,  flag the outlier  compound "P* in all associated
                  field sample resulfcsygeneratdsd since the last valid  PVS,
                  initial calibration,T^X valid calibration check standard.
      10.6.2      If any PVS  compound is  ooptside the expanded range, the PVS
                  shall,,%etl5|aaalyzed immediately.   If,  on reanalysis, any
                  compotfed is gt^L  outside ttie expanded recovery range, stop
                  saoigie analyse'44%perform corrective action, run a new
                  initial calibration,  and reanalyze all samples run after  the
                  la&t valid  PVSJJIJa^jtyLal-jsalibration,  or valid calibration
                  cheek  standarailJJiifoxe;: proceeding with sample analyses.

      10.6.3      If the KI i-^JRRT for any compound is not within the RT and
                  RRT windows*^?»t|!blished during the initial calibration,
                 "• '.reanalyze the'"lip*''! _ If  upon reanalysis a compound is still
            ;t-.\;  " butsii^e, Jthe windotS%J a  new  initial calibration must be
          , ; f      perform|iif.before samples can be analyzed.  The instrument
        -;/!. c       must be fi^alibrated as described in paragraph 8.  Reanalyze
      $ff:!        all samplelrirun after the last valid PVS, initial
      1:f;          calibratioi|V or valid calibration check standard before
      "''%?!„       proceedings;*|ith sample  analyses.
          "' -" o-' Vi,             &• f
      10.6.4^'*'}j.,- If the SMSpilTS  criterion is not met for a PVS, sample
                 V apalyses/iJhall  be  stopped and the noncompliant PVS
                  iaaae
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10.7
                                                                           DRAFT

                   1.0  percent.  Reanalyze all samples that were run between
                   the  noncompliant PVS and the last valid PVS, initial
                   calibration, or valid calibration check standard  before
                   proceeding with sample analyses.

      10.6.5       If the PVS SMC recovery is less thani&D -percent,  greater
                   than 200 percent,  or if peak interferences Are present,
                   sample analyses shall be stopped, corrective-laction shall be
                   performed, and the noncompliant PVS immediately' "      ..'~*
      10.6.6       If the peak resolution criterion, is*not met, the  Laboratory
                   shall perform corrective action .and demonstrate adequate
                   resolution before  samples can be ankl^ed (see paragraph
                   11).                                '  '<•"(:••

      10.6.7       If all PVS cri^£ria-fs'aias0£.«»be met after having taken
                   corrective actia&i^, reaha^ly&BfeiJfjIo ftfft^re.-extract)  the
                   associated field samples in another valid analytical
                   sequence.   If on reasalyses Mil QC sample criteria  are  met
                   and  the PVS criteria;istillsicannot be met, then submit all
                   sample data from both se4juences.  The Laboratory  shall
                   describe in the Batch narrative the problems associated with
                   the  PVS ••«w$i!itow the field-Cample matrix may have  affected
                   the ,.F?S analy&es.   If the IJaboratory can demonstrate that
                   the%f»roblems ar^ij-due to matrix effects, then both sequences
      10.6.8       If -tLPyS  reanii^&sliM|-jr4ifnired because of a non- compliant
                   initial -'-BVS  analysis,  the PVS reanalysis must be started
                   within 2€?'rl»seurs  after  the start of the current analytical
                   sequence,  v , •
                  •Beea«s«f:reanalysis>j at no additional cost to the Agency, is
                  requireiS.^f PVS  technical acceptance criteria are not met,
                  more freqjpwit analysis of the PVS is recommended, especially
                  when highiysicontaminated or complex samples are analyzed.
      Results fltefPVS analys^- are  reported on Forms QI-PHEN, QIII-PHEN, and
      QVI-PHEN. "Reporting ?3feequirements  are listed in Exhibit B.
                                  D-27-PHEN-Q                           8/23/94

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                                                                          DRAFT

11    System Performance  - GC Resolution

11 . 1  Summary

      Peak resolution between o-cresol and m-cresol sliall be measured to
      establish that there is sufficient chromatogEaplilce .resolution for
      accurate compound identifications and  quantisations.- JJhen minimum peak
      resolution cannot be met, identification and quant itaticm is  adversely
      affected due to the difficulty in establishing the baseline,,

11.2  Frequency                               ''"'<

      11.2.1 '     Initial calibration - Thetpeak resolution between o-cresol
                  and m-cresol shall be evaluated in tbe low initial
                  calibration standard before ::,proceediiag with  sample analyses.

      11.2.2      Calibration check standard - The ;$>eak resolution  between
                  o-cresol and m-cresol shall be evaluated  for each
                  calibration check standard before proceeding with sample
                  analyses.
                                ' !. ''  ' ' ' *' 4',  <,>  ;* *'
      11.2.3      Performance verification -staadaecd -,Ihe peak resolution
                  between -o-cresol "sad m-cresol Jshall"%es;.evaluated  for each
                  PVS that is analyzecUin a  valid analytical sequence .
                                      , J      '-.••>
11.3  Calculations                           r

      Determine resolutjsftti^fcy, Calculating tto* percent valley between o-cresol
      and m-cresol using-the fbllljewing equation (see figure 1).
                      *           '"
                                      of the valley between             „_  n , n
                                                                            '
                       ,   -         peafc being resolved
11.4  Technical,-jAciteptance Criteria
                  Initial*::«^libration' - The percent valley must be less than
                  or equal -|pQ, 25 percent between  o-cresol  and m-cresol in the
                  analysis the low standard of the  initial calibration.
                            -
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                                                                           DRAFT

11.5  Corrective Action

      11.5.1       If the peak resolution for the  two  compounds indicated in
                   paragraph 11.1 exceeds the 25 percent:: valley criterion in
                   the low level standard analyzed during  the initial
                   calibration, corrective action  shall be>taken,  and a new
                   initial calibration shall be performed  and ^documented before
                   proceeding with sample analyses.           ;
      11.5.2       If the peak resolution for tihe two compounds indibi.1ted in
                   paragraph 11.1 exceeds the,J|5 percent valley criterion in
                   the calibration check sta|tSird, corrective  action shall be
                   performed.   A valid calibration check' must  be demonstrated
                   or a new initial calibration shall big;, performed and
                                          '•• * 5- •."• !: "•
                   documented before proceexSftsg ,,with .sample  analyses.
                                              ••" , , - ';cKr-s-j^w Initial calibration
                   performed.  Reanalyze all sampies run after  the last valid
                   PVS,  initial calibration, oac^alid calibration check
                   standard before proceeding:: with sample analyses.
      11.5.4      A high percent valley dCBpLd indicate  injector contamination
                  or colijaa4;pjfc|pcadation; tl^efore, injection port and/or
                  colulnNmaintj&Ma&ce may be «^§uired.   Maintenance may include
                  replacement of|lbe injectof^TiLner and/or removing 0.5 - 1m
                  ofxfihe column. |s;IKf these measures do  not work,  column
                  l^jilacement sh|^;4 ,J^e_ ccsns idered .
                  N'!"^4-       ^l^i^ll^^-ljf"'
11.6  Documentation   '*• •', ';-,-,-
                          •- ;.;«-_».,
      Percent resolution resu!Ke»;*a,re reported on Forms  QIII-PHEN,  QIVA-PHEN,
      and QV-P,IiM;:=-:,il^)orting reXjUxgements are listed in Exhibit B.
             '* '•*'•>'• -"**  -"'          '"-''  '
                                  D-29-PHEN-Q                           8/23/94

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                                                                          DRAFT
                                  SECTION IV

         SAMPLE ANALYSIS AND COMPOUND IDENTIFICATION ASD QUANTITATION
12    Summary

12.1  This method is designed for use in the rapid  analysis  of «ater,
      soil/solid, oil, and wipe samples for the target  compounds  listed in
      Exhibit C.  If upon inspection of a sample the  Contractor suspeclts that
      the sample is not amenable to this method, contact  the Regional TPO or
      the CLASS contractor for instructions..  For Superfund  emergency removal
      actions, contact the Regional TPO orifche Headquarters  APO for
      instructions.  If, for emergency response actions',  the TPO  or APO are
      not available, contact the Regional Oh-$i?ene  Coordinator (OSC) for
      instructions.  The Laboratory must remember that  it shall follow the
      requirements in this SOW without deviation. "  '

12.2  Before samples or required blanks can be analyzed, "'the instrument must
      meet initial calibration or^vialt4 ^calibration check standard and column
      resolution technical accep'tfiace' ''•cr£^B^4f! -sAll  sample  extracts,  required
      blanks, LCS ,  PVS, and calibration standa^M .sb^l^e analyzed under the
      same instrumental conditions and shall be allowed 'to warm to ambient
      temperature (approximately 1 hotlr) before preparation/analysis.

12.3  The laboratory shall perform sample extraction  and  cleanup  of water
      samples utilizing either,,,. solvent (paragraph 14) or  solid phase
      (paragraph 15) ex*£3acti©ij,:.fnd cleanup'*}, -.The laboratory must meet all
      QA/QC requiremeatfcs as statist under this -.contract  using either of these
      extraction/cle&up techniqi|5s .   The solvent extraction procedures are
      recommended for' the cleanup, and extraction of all samples;  however, the
      phenols SPE *pr«e used  if equivalency to the
      solvent extracticai •procedures'" call "'°oe : %emonstrated by the Laboratory.
      Solvent extraction «a&d -cleanup procedures shall be  used for all non-
      aqueous samples .      [  <-'
12.4  Blank ^anp-les'; sfeoh as trip!%Laanks and field blanks,  supplied by the
      Regisejdt'-and incluBelelMWith a batch of field samples  shall be prepared,
      anajfzed, and reports^!., as water samples.  Occasionally,  a water QC
           e (e.g., field atgU trip blanks) will be included with a batch of
           samples.  If the laboratory is not certain whether a water sample
                 with a batcfivof soil samples is a QC sample,  contact the
               TPO or the CLASS contractor.
      NOTE: IJ^WHBter blanks! (provided by the Region,  such as  trip and field
      blanks are iaacCfcude^in a batch of soil samples,  the laboratory is not
      required to prepJaaSe and analyze an associated  water method blank or a
      water LCS.         "
                                  D-30-PHEN-Q                           8/23/94

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                                                                           DRAFT

 12.5   If unusual or high concentration samples are received,  see  Exhibit D,
       Appendix B for general guidance on screening and sample preparation.

 13     Phase  Separation

       Multi-phase samples shall be phase -separated -mtrt*' tiheir individual
       phases.   The phase separation techniques employed will Trary according  to
       the types of samples received.  Since it is impossible aCftfknow  the
       number and types of phases that will be present in a sample!^ the  choice
       of phase separation techniques is left t« ithe professional  jtMgement of
       the analyst.   Various techniques can be employed to separate the.j,|*hases.
       These  include pipetting off liquid phases (decanting should not be
       done), centrifuging to remove suspended solids, and use of  spatulas to
       remove solids (wooden tongue depres&e>£s work wellj .  Whenever possible,
       phase  separation operations should bef dene with} disposable  glassware.
       The phases should be separated into gla^s^contspltiers with teflon- lined
       screw  caps.   This allows for storage and hamdling of the waste  in a safe
       manner.                                         • -,;
                                                       !«*  vs*

       13.1  Samples received containing multiple phases such as water,  oil,
             and soil/solid in the!-Psaaey«4a^l«;^ar shall be phase  separated
             into individual phases'.';.    '"' ;'*- i-"/
       13 . 2  Each individual phase is -taken though the procedure  as a
             subsample.   Report analytical  results for each sample phase.
             Note:  Each multi -phase samplfe shall be identified using the  EPA
             sample  number convention for mttiti -phase samples as specified in
             Exhibit B.     ' '". -E- ,
                      ,:        ' "X^i          '"•"•-,
       13.3   Do  not  analyze any pnfise that  represents less than 10 percent of
             the  total "sample volume.
                                  '
                                      ,
      13.4  In the 'fc&lowing prdfeiire»;vl»i^re applicable, references to
            "samples" esBpliibcitly mean "single phase units."

14    Solvent Extraction and ?t31jfeaaup
              „, •;,:• \;- ,         " --' ,y;
14.1  SampLe'sfreparalf-itm and Extraction -  Water Samples
           '~'             '
      A ISO" mL aqueous sampfej-,is  serially extracted using two 10 mL portions
      p&iaethylene chloride IjpSJeC^)  under basic and acidic conditions.
      JSltractions are perfon|iia in 125 mL Erlenmeyer flasks with a magnetic
      Staffing bar.  Initial jp£traction  of the water sample is performed with
      MeCT^ .^t^high pH to rejlbye  non-phenolic compounds.   Methylene chloride
      from tBe||tmtial extractions is discarded.   Sodium chloride is then
      added to tlk Water ftffegple and is extracted with two portions of MeCl2 at
      low pH to rem@s$et=thfe ttarget phenolic compounds.   Extracts are combined,
      filtered, and drletj through powdered anhydrous sodium sulfate, solvent
      switched to hexane, and concentrated to a 1 mL volume using the nitrogen
      blowdown procedure.

                                  D-31-PHEN-Q                           8/23/94

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                                                                    DRAFT

14.1.1      Measure 100 mL of sample  into a 125  mL Erlenmeyer flask.

14.1.2      Spike the sample with  25  uL of the SMC (2.0 mg/mL) .

14.1.3      Adjust the pH of the sample to greater than pH 11 using 0.5
            N Sodium hydroxide solution.

14.1.4      Add teflon stirring bar.
                                                        -?
14.1.5      Add 10 mL of MeCl2.         ,                     V ,:.;

14.1.6      Place the sample on a  magnfeiic stirring plate and stir for
            three minutes.  The stirring rate shosuid be sufficient to
            mix the MeCl2 throughoutT:the sample,,.,,!
                                      < ^ -       .1
14 . 1 . 7      Remove the stir bar and allow? , tihe ,%queous and MeCl£ layers
            to separate.

14.1.8      Remove the MeCl2 layer with a Pasteurr:pipet and discard the
            solvent.        ;• , ,
14.1.9      Repeat steps 1413,,;4  - "1

14.1.10     Cool the sample  to;4*C  in atfdce  bath.   Carefully adjust the
            pH of the sample to ^R ,2.Qi-i^ 3.0  using 0.5 N hydrochloric
            acid solution.   Be suT«,»tf|« sample does not heat up during
            this acidification.      *

14.1.11     Add teuton "storing  bar.   ,;:/
               ,*" ,          *S f ' f           ""*
14.1.12     Gainfully add 25"^g of NaCl to the sample and stir for 3
            minutes.      <*--! ..... ,„ ,.
14.1.13     Repeal: f,fceps  14.1.5  -  14.1.7.

14.1.14     Remove the IS^Slj with  a Pasteur pipet and transfer to a 25
14.J,:t|5     Repeat ^astfps  14.1.5  -  14.1.7 and 14.1.14 ,  combining the
  £ ?'•       MeClo la^ip^.   Discard extracted aqueous sample.
 ^ ^ *:*                   >: .
                        „
            Prepare  a  ^ying column by plugging the bottom of a funnel
            with glass Jwool  and adding approximately 15 grams of
            powdered sifaydrous  sodium sulfate.   Pour extract through
          % ,., funnel an*|lbcollect  in a 25 mL graduated concentrator tube .
           >>;IUynse t^ie Extract container with minimal volumes of MeCl2
            anil j^gi^hthrough the funnel. Rinse  sodium sulfate twice with
                   l volumes  of
                            D-32-PHEN-Q                           8/23/94

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                                                                          DRAFT

      14.1.17      Concentrate  the  extract to approximately 0.5 mL using the
                   nitrogen blowdown procedure in a. 30°C water bath (to
                   minimize analyte loss due to volatility, occasionally rinse
                   sides  of concentrator tube with MeClJ2 during the blowdown
                   procedure) .  Add 5 ml of hexane to concentrator tube and mix
                   vigorously.  Reconcentrate to 1 mC.j: Ito not let extract go
                   dry during concentration.   This fjitial vo^ame is suitable for
                   extract  compound concentrations af 5.0 ^g/mL: to 250 jjg/mL.
                   This is  equivalent to sample compound concentrations of 50
                   to  2500  /jg/L for water samples.                  •,
                                              }'- '
      14.1.18      Transfer the extract to an sautosampler or other 1-mL vial
                   and analyze  the  extract according to .paragraph 18 .

14.2  Sample Preparation and Extraction - Soii/(So lid Samples

      A 6 gram sample of soil/solid is mixed with powdered anhydrous sodium
      sulfate and  is  serially  extracted with two portions of methylene
      chloride (MeC^) using an ultrasonic probe.  The ife£tract layers are
      collected and the  phenolic compounds are back -extracted into clean
      reagent water at high pH. < f&mpfiejjai&ic e,xtractables in the MeCl2 are
      discarded.   Sodium chloride  is then addect to the aqueous phase and is
      extracted with  two portions  o1?:MeCl2 at JjJow pH'~to xemove the phenolic
      compounds.   Extracts  are combined,  filtered,  and dried through powdered
      anhydrous sodium sulfate, and comsentirafeed to a  1 mL volume using the
      nitrogen blowdown  procedure.

      14.2.1       Mix samples ^thoroughly,  especially composited samples.
                   Discard  any 'resign ob j ects^ such as sticks, leaves, and
                   rodlcs.'        "".. '           :l "

      14.2.2       feigh  approxima^fe^Jj, .grams, of a representative sample to
                   the; ^nearest  O^L^-!i;fit;p4A5§"50 mL beaker.
      14.2.3      To the Weighed sample, add a  sufficient amount of powdered
                  anhydrous sojiitOB. sulfate to prepare  a free flowing mass upon
                           Mix 'wets.,-
                                    ' J
      14.2^      Spike ''tlf^.sample with 25 uL of  the  SMC  (2.0 mg/mL) .

      14>?2.5      Add 10 mL !s& MeCl2/acetone (50:50).

                  Sonicate atfifpaicrotip maximum power;  cool  the sample  during
                  sonication;.?!! The sonicator must be  set  for 50 percent pulse
                 ,,action.  jSbkiicate for 3 minutes.  The power output may have
                  ifeo.be adjusted to ensure that the sample  extract does not
                                      any significant loss  of sample during
                             is not acceptable.   Rinse the  sonicator tip after
                  each sample extraction with 1 mL of MeCl2/acetone (50:50).


                                  D-33-PHEN-Q                           8/23/94

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                                                                    DRAFT

14 . 2 . 7      Remove and collect the MeCl2/acetone  layer in a 50 mL
            Erlenmeyer flask.

14.2.8      Repeat steps 14.2.5  - 14.2.7.

14.2.9      Add 10 mL of reagent water  at  pH greater , than 11 to the
            sample extract.

14.2.10     Add teflon stirring bar.

14 . 2 . 11     Place the sample on a magnetic stirring plate and stilr for
            three minutes.  The stirrjiig rate  should be sufficient to
            mix the solvent layer and &!he  reagent ;JWater .

14.2.12     Remove the stir bar and ''allow  aqueete and  solvent layers to
            separate.                    ,-<,  , , •'•=• '
14.2.13     Remove the aqueous layer by  Pasteur ip4Pet and transfer to a
            50 mL Erlenmeyer flask.               •   ,;
14.2.14     Repeat steps 14jp£f;-s''J^,SLJL3,  combining  the aqueous layers.
            Discard the extracted sdlvfeafc Jtayier.;. .,
                             '«          ,£
14.2.15     Cool the aqueous phase to 4<*S in an  ice bath.   Carefully
            adjust the pH of theC&l^ to  pH 2.0  - 3.0 using 0.5 N
            hydrochloric acid solution;-  Be sure the  sample does not
            heat up or splash during :fshis acidification.

14.2.16     Carefully aad-.il, 4g of NaCl *o:the sample and stir for 3
            mintifees.      °T-
14. 2 . 17     &4d 10 mL of M

14 . 2 . 18     Repeal s*eps 14 . 2 10 - 14. 2.12.
                   '"•^->: ,
14.2.19     Remove the '^tClg by Pasteur pipet  and  transfer to a 25 mL
            Repeat stpps 14.2.17 - 14.2.19,  combining the MeCl2 layers.
            Discard tatie aqueous phase.
                      ;K;.
            Filter the Combined extracts by  gravity  or vacuum
            filtrationl;.;'.*- Complete filtration by  transferring entire
            sample con:%eaits to funnel and  rinse  with an additional 10 mL
                        For gravity filtration, prepare  a
                        filtration/drying bed with Whatman #42 filter
                        paper filled with approximately  15 grams of
                        powdered anhydrous  sodium sulfate in a 6 cm

                            D-34-PHEN-Q                           8/23/94

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                                                                           DRAFT

                               powder funnel.  Rinse the sodium sulfate and
                               filter paper with MeCl2 and discard rinsate.
                               With the filter and sodium sulfate wetted,
                               decant combined extracts -trhrough the packed
                               funnel and collect in al> 50 mL centrifuge tube.
                               Rinse the extract container- with minimal volumes
                               of MeCl2 and pour through "the- funnel.  Rinse
                               filter/sodium sulfate with 10 "oL^of MeCl2.
                                                               ••*  ' tt-.
                   14.2.21.2   For vacuum filtration use Whatman
                               paper in a Bucbaier funnel.  Pre-wet the paper
                               with MeCl2 and'discard rinsate.  Transfer
                               combined extracts into funnel, apply vacuum, and
                               collect fittakte.  Rinse Jrilter with 10 mL of
                               MeCl2 .   Pour '£||t«red Detract through a powder
                               funnel  plugged wit:b :,gijss wool and filled with
                               anhydrous sodium sulfatee and collect in a 60 mL
                               centrifuge tube.   Rinseytfee extract container
                               with minimal volumes  of MeCl^ and pour through
                               the funnel.   Rinse sodium sulfate with an
                                                sMeC!2 .
      14.2.22     Concentrate extract to approximately -25 mL using the
                  nitrogen blowdown procedure;jarn a 30°C water bath.  Transfer
                  extract concentrate Itfp a 2S;tmL concentrator tube and
                  concentrate further to approximately 0.5 mL (to minimize
                  analyte loss due  to volatility,  occasionally rinse sides of
                  centrlf^gejf^d concentrator,, tubes with MeCl2 during the
                  blowSawn prboejfeire ) .  Add 'tS-apL of hexane to the concentrator
                  tubtfeand mix vigorously.  Re4»ncentrate to 1 mL.  Do not
                  alidw extract HS,rgo dry during concentration.   This final
                  volume is suita^fee^f^c^ extract compound concentrations of
                             to J^;^^l8iii.>;, fliis  is equivalent to sample
                           sconcentrations of  830 to 41 , 000 /tg/kg for
                  soil/soli$:;»amples .

      14.2.23  ,/'  ;jta%sfer the extract to an  autosampler or other 1-mL vial
            ^^-i-  and^amajLyze the exja^act according to paragraph 18.
         "H •"• '             '-ie|j phase can be deatonstrated to  meet the QA/QC requirements of this
                 n addition^:' filter disk  is required when water samples
      contain paj&l^ulatesiy'Upon opening  a package  of  disks,  they shall be
      used immediately |^,r «»tored in a desiccator  (over  Drierite,  or
      equivalent).  F&fgseproducible extraction efficiencies ,  all directions
      given below shall be followed as closely as possible.  NOTE:  The
      Laboratory shall not use SPE for non-aqueous samples.

                                  D-35-PHEN-Q                           8/23/94

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                                                                          DRAFT

      Because many disk extraction vacuum hardware  components are available
      commercially, the Laboratory should follow  the  manufacturers directions
      for the proper use of these devices.  The Laboratory should also refer
      to the extraction disk package  inserts for  additional details on the
      proper use of the disks and disk vacuum apparatus.

15.1  Sample Filtration

      All water samples extracted using SPE disks shall be filtered.  The
      filtration step may be combined with the Extraction by placing '*. filter
      disk designed to fit inside the neck ojJHIhe sample  reservoir and'-'
      proceeding with the water sample cleanup and  extraction as specified in
      paragraphs 15.2-15.5.

15.2  Disk Extraction Set-up and Condi tionlngl  y     •,  :

      15.2.1      Place a 47 mm Styrene Divinyl Benzene  (SDB) Empore™ disk
                  onto the base unit  of a glass filtration assembly (without
                  the reservoir and clamp).   Use of  a Btanifold for
                  extractions is acceptable .
                  NOTE:  When performing fhe -i-pfce'-uaSh,, .wash,  and conditioning
                  steps as described "below, ther Laboratory may want to
                  consider collecting solvent- (Pastes  separately from the
                  sample wastes in order to aainimize  the creation of large
                  volumes of hazardous wastes mixed with water samples .

      15.2.2      NOTE: 4Siea ^safe-cleaned SBB^disks  are used,  the following
                  pre-«ssK profeed&re is not accessary.   Pre- swelling with
                  acetdke, howevebc, will prevebt. cosmetic "wrinkling" of the
                  disk which willhaot affect performance.
                  . L^.            0 4 ..  ^ ,   ~ , „
                  Tor swell the ^!e«ijfc';apiia.-j^35eiwash the SDB disk,  pipette 2-4 mL
                  of acetone onto the disk surface.   Allow to soak for
                  approximately 3 minutes .  Draw the  acetone through and allow
                  the disk to-iidry^  Repeat using 2-4  mL  of isopropyl alcohol.
      15.2,3°;.";  '  'Tlaee '£&e glass reservoir on  the  base  unit and clamp in
         .&        place. -IsjiSently pinch the clamp  to assure even pressure
        -, -T'       around tS^Mdisk.

      dt3!- 2.4      Wash the e|s.^caction apparatus and disk by adding 5 mL of
      '•"jy:|        methylene ^lloride to the reservoir, rinsing down the sides
         :':«" ;.,3:l=    of tne resli'voir in the process.   Draw a small amount
            !s~r;:?  through |hS disk with a vacuum; turn off the vacuum and
                     Low tbe«aisk to soak for approximately 1 minute.  Draw the
                       Lnjipf solvent through the disk and allow the disk to
                  dry';\i' I'r
                                  D-36-PHEN-Q                           8/23/94

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                                                                          DRAFT

      15.2.5      Condition  the  disk by adding approximately 5 mL of methanol
                  to  the  reservoir,  drawing a small amount through the disk
                  then letting it soak for approximately 1 minute.  Draw most
                  of  the  remaining methanol through tbJe disk, leaving 3-5 mm
                  of  the  methanol on the surface of the disk.

                  NOTE: THE  DISK SHOULD NOT BE ALLfHID T&£0.sDRY FROM THIS
                  POINT UNTIL THE END OF SAMPLE EXTRACTION': gKES-IDUAL VACUUM
                  IN  THE  EXTRACTION  DEVICE MUST BE VENTED TO PRSOTCT THE DISK
                  FROM DRYING OUT.    MOST VAGUER MANIFOLD DEVICES  > ' ,  ,
                  AUTOMATICALLY  VENT WHEN THEMACUUM IS TURNED OFF. "life
                  VACUUM  LINE MAY NEED TO BE-DISCONNECTED IN ORDER TO VENT THE
                  RESIDUAL VACUUM IF SUCTIQff TLASKS ARBjtKED.
                                                      J' '"
      15.2.6      Add 10  mL  of reagent water *p the eHLsk.  Using the vacuum,
                  pull most  of the water throti^g^ again leaving 3-5 mm of
                  water on the surface of the disk..:-
                  NOTE:  AS DESCRIBED IN THE  PREVIOUS 'SfiF^, RESIDUAL VACUUM IN
                  THE EXTRACTION  JBEVICE MUST  BE  VENTED TO SMBVENT THE DISK
                  FROM DRYING          "
15.3  Compound Extraction and Elutioa- Using
                                     • : -       •'.<'•
      NOTE: The phenols water CRQLs  ar-e^the |$aiae  as the solvent extracted
            sample CRQLs as stated in  Exhibit:  C.

      15.3.1      Pour 1P0, iffilf ,*ȣ water sample  into a clean Erlenmeyer flask,
                  Fleafeearvbeake^4';,?separatory!j&jnnel, or any other suitable
                         chamber^'  :
      15.3.2      Adjust the pH ^t;he., water  sample to f 2 using 0.5 N
                  Hyctaochloric .&Sli»? ^$08. 8J.5 mL of methanol and 5 g NaCl to
                  100 WL?
-------
                                                                          DRAFT

                  the disk with a disposable  pipette,  rinsing sides of the
                  filtration reservoir in the process.

      15.3.8      Draw half of the solvent through the*disk then release the
                  vacuum.  Allow the remaining methylese chloride to soak the
                  disk for approximately  1 minute tfcen; 4saw remainder through
                  under vacuum.                    •      '

      15.3.9      Repeat the solvent rinse of the sample bottle-saasijig 5 mL of
                  methylene chloride and  transfer to the apparatus^ Rinsing
                  down the sides of the reser^eir.   Add  5  mL of methylene
                  chloride directly on the disk and draw through under vacuum.

      15.3.10     Add 8 g of anhydrous sog&un sulfate^o dry the eluate.
                  Pipet the eluate into a b&iieentratea: tube.  Rinse the
                  collection tube and sodium  salfate^with  two 5 mL portions of
                  methylene chloride and  combine the rinsates with the sample
                  eluate in the concentrator  tube.   *PX£E:  If large clumps
                  form on addition of the sodium sulfai§evep the sample eluate,
                  break up the clumps before  adding the  rinses.
      15.3.11     Concentrate extract to 1:«m!'^5tfex"jge^tl,e stream of nitrogen
                  (may be warmed gemfc^y -  appr-efematel^ -?Q degrees C.)  To
                  minimize analyte lotos due  t*M volatility, occasionally rinse
                  sides of centrifuge' said,  cdfceentrator tubes with methylene
                  chloride during the blo«4o»n procedure .   This final volume
                  is suitable for extract  compound concentrations of 5 . 0
                  to 250 |ig/mL.  This is equivalent to sample compound
                  conc«atra'tibns: |of 50 to  25^ /jg/L for water samples.
                     /.Vv         ?%!            «' ,
                     -. ~ :,*          .z ;            '<>
                     >,;--:-          \A,            • .
      15.3.12     T,taasfer the esfcract to  an autosampler or other 1-mL vial
                      analyze thfeSextract  ^according to section 18.
                                 f"^*'"'  ' - *"  *  f>**~*°
                     ,..
16    Sample Preparation ated Extraction  -  Oil Samples

      NOTE: The phenols targe*;jkai>mpound  CRQL for oil samples is 830 jig/kg (see
            ExMfcliSt- 'f hexane and shake vigorously.
               •'•  N-    -*"
16.4  Transfer mixtaare' oatfp a 125 mL separatory  funnel.
                     '\^-- r
16.5  Add 10 mL of reagent water at pH greater than 11 to  the sample extract.
      Shake 3 minutes .

                                  D-38-PHEN-Q                           8/23/94

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                                                                          DRAFT

16.6  Allow aqueous and solvent  layers to separate and discard solvent
      (hexane) layer.

16.7  Add 10 mL of hexane. Shake 3  minutes and discard the hexane layer.

16.8  Cool the aqueous phase to  4«C in an ice bath. '^Carefully adjust the pH
      of the sample to pH 2.0  -  3.0 using 0.5 N hydrochloric acid solution.
      Be sure the sample does  not heat up or splash during this -acidification.

16.9  Carefully add 5 g of NaCl  to  the sample .-and shake until dissfclwd.

16.10 Add 10 mL of MeCl2 and shake  for 3 miraadtes.

16.11 Allow layers to separate and  collect the solvents layer in a 25 mL
      concentrator tube.                              ">

16.12 Repeat steps 16.10 - 16.11, combining the M&C1.2 .layers.  Discard the
      aqueous phase.                                    ~-

16.13 Concentrate extract to approximately 0.5 mL using the nitrogen blowdown
      procedure in a 30°C water  l>atfe^X^i'|stl*imize analyte loss due to
      volatility, occasionally rinsjp* side's"vdr" l^e,, concentrator tube with MeCl2
      during the blowdown procedure!.   Add 5 mL'oif hexane to the concentrator
      tube and mix vigorously.   Reconcetitrate to 1 mL.   Do not allow extract
      to go dry during concentration.  ;<,This, final volume is suitable for
      extract compound concentrations  of 5.0 /ig/mL to 250 ^tg/mL.  This is
      equivalent to sample compound concentrations of 830 to 41,000 jig/kg for
      oil samples.        .',,-..           •
16.14 Transfer the extract to an%attosampler or other 1-mL vial and analyze
      the extract according to paragraph 18.
17    Sample Preparation. and Extmfctkofe- - Ifj-pe Samples

      A wipe sample containing phenols is serially extracted with two portions
      of methylene chloride ^MeGlg)  using an ultrasonic probe.   The extract
      layers sax collected and the-pbenolic compounds are "back- extracted"
      into ,c|tea.Ti' reage»t:j:aBater at liEgh pH.   Non-phenolic extractables in the
      MeClg-jare discarded>xv>.Sodiuni chloride is then added to the aqueous phase
      an4:|J.s extracted witnfefcwo portions  of MeCl2 at low pH to  remove the
      phenolic compounds.  E^Jracts  are combined,  filtered,  and dried through
               anhydrous sodiiHSi sulfate,  and concentrated to a  1 mL volume
            the nitrogen blowdown procedure.
         ' '** ?,                 .'•**•
      NOTE: Ttte'i^arget compjoalid CRQLs for wipe samples will be  specified by
                           '
17.1  Pour off any free ''solvent from the sample jar into a clean Erlenmeyer
      flask of appropriate size .


                                  D-39-PHEN-Q                           8/23/94

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                                                                          DRAFT

17.2  Spike the sample with 25 uL of the SMC (2.0 mg/mL) .

17.3  Add enough clean MeCl2 to the sample jar to just cover the wipe sample.

      17.3.1       If  the  shape of the sample jar is aert amenable to
                   sonication,  quantitatively transfer-1 "tshe^s ample to an
                   appropriate  container.  Rinse the sample ! jar with 5-10 mL of
                   hexane  and transfer to the new sample container.

17.4  Sonicate at  microtip  maximum power;  cool the sample during sonication.
      The sonicator must  be set for 50 per cent .pulse action.  Sonicate -for  3
      minutes.  The power output may have to'.>&e adjusted to ensure that the
      sample extract  does not  splash excesslhFely; any significant loss of
      sample during sonication is not acceptable.  Rinse the sonicator tip
      after each sample extraction with 1 MLJof MeCljf,

17.5  Remove the MeCl2 layer from the sonication and.,combine it with the
      solvent in the  Erlenmeyer flask.             :

17.6  Repeat steps 17.3 - 17.5.   j,

17.7  Add teflon stirring bar  to Hxe Erlerime'^eZ'i.flasfc.  ,
                                               5<    's* '•'  K,
17.8  Add 10 mL of reagent  water at pHfigreater -fithan 11 to the sample extract.

17 . 9  Place the sample on a magnetic stlrxifcg plate and stir for three
      minutes.  The stirring rate should t»e>*sufficient to mix the organic
      solvent and  the
17.10 Allow aqueous sffld ' organic Sc&vent layeffif to separate.
17.11 Remove the aeneous  layer bvjpasteur pipet and transfer to a clean  50 mL
      Erlenmeyer                 '*"'*"    '•'  *  '"
17.12 Repeat steps  17.8  -'-1|I7,-.lJ.,  combining the aqueous layers.  Discard  the
      extracted organic  solvetttliayer.

17.13 Cool 4$j$J&fa&cni&fjibase for 5'^aiibtes in an ice bath.  Carefully adjust
      the|j*II'of the samplej:to pH 2.0 -  3.0 using 0.5 N hydrochloric acid
      solution.  Be sure t1«ej»sample does not heat up or splash during this
      acidification.        "|x.
17.l4-AM;;TEeflon  stirring
        '"'';;§,;; ._               -,
17.15 CarefullNrAadd  5  g of JfetiCl to the aqueous phase and stir for 3 minutes.
               • l~>. -,,,,>
                "V  -: ,       ~* *
17.16 Add 10  mL of'ifej&l^t,*';;;
                     ^ '', ^^
17.17 Repeat  steps 17.9'- 17.10.



                                   D-40-PHEN-Q                       •    8/23/94

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                                                                           DRAFT

17.18 Remove  the MeCl2 by Pasteur pipet and transfer to a clean  25  mL
      concentrator tube .

17 . 19 Add  5 mL MeCl2 to the aqueous sample .   Repeat steps 17 . 17  - 17.18,
      combining  the MeCl2 layers in the 25 mL concentrator tube.  Discard the
      aqueous phase.

17.20 Filter  the combined extracts by gravity filtration.    ;.

      17.20.1     Prepare a filtration/drying^bed with Whatman #42:<,iilter
                   paper filled with approximately 15 grams of powdered
                   anhydrous sodium sulfate iii/a 6 cm powder funnel.   Rinse the
                   sodium sulfate and f ilterjlpaper with ,-MeCl2 and discard
                   rinsate.   With the filter, and sodiuat sulfate wetted,  decant
                   combined extracts througli thte packed funnel and collect in a
                   clean 25 mL concentrator tube'.-  RJase the concentrator  tube
                   with an additional 5 mL MeCl2 ,  anS transfer the rinse
                   solvent to powder funnel.   Rinse powder funnel with 10  mL
                   MeCl2.                                : j  .
17.21 Concentrate  the extract to ;4w*^siatato&|y:, ,0 . 5 mL using the nitrogen
      blowdown procedure in a 300 system per  tb«i;regui,re.ments in paragraph 7.

                                       '
                                   -
      18.1.1      Solveit»'flush manual injection or automated sample injection
                  is  recommended  for analysis.
      18.1.2  ,;.=.;*;3Ba^analytical''sesjjftence consists of field sample analyses and
            ,>VfV  a'Hi-iissociated  stlaiards,  blanks,  and QC analyses performed
         f i- •      within:"«a;:,24-hour  period on one instrument.   There are two
        fe"-:       (2)  typesll^f analytical sequences: an initial calibration
                  analytical||$             f*:
             ,(•;„;, 18.1.2.1/  fAn  initial calibration analytical sequence
                ~<'f> '>'_••••,,     ,r '  begins with a  three-point calibration, an
                  "' ,  <-,.;!   instrument blank,  an LCS,  and a method blank.
                       i'A-     The initial calibration analytical sequence is
                              as  follows:
                                  D-41-PHEN-Q                           8/23/94

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                                                                    DRAFT
18.1.3
                •      Initial three-point Calibration (analysis
                      of the high standard proceeded by the mid
                      and low standards) ;

                •      Instrument Blank;  :*

                •      Laboratory Control Sample (s) ;

                      Method Blank(s) ;            :

                      Field Samj3;Le(s);
                             •\s  '
                •      Instrvaseiit Blank(s>; sand

                •      Performance Verification Standard(s) .

   18.1.2.2     A  daily calibration check analytical sequence
                begins with an instrument blank, a valid
                calibration check standatid^-a method blank, and
                an LGS.   The daily calibration 'analytical
                          » «is JE ollows :
                         -   i '- ,'  f v •

                    '! Instrument ffBlarik*   '/;

                      Calibration Check Standard;

                      Method,Slank(s);

                      Laboratory .Control Sample(s);
                              *  \?
                      Field Sample (s) ;

                    j^InstaeuwBnt Blank(s) ; and

           ",;,-,.•      Performance Verification Standard(s) .
                •* '  ( '
r y:lfxall  acceptatiiee^criteria for these analyses are met, then
1 ' -""The«:JSfb^atory may -proceed with sample analyses .
            All analytical sequences conclude with an acceptable
            instrument|;|^lank and a PVS analysis.   The PVS shall be
            started wi'tS^n 24 hours after the injection of the first
            initial calibration standard or  the  first instrument blank
            in the daijfy5 calibration sequence.
           :«JKQTE: Ifitf PVS reanalysis is required because of a non-
            :e<&Bpiia^ri: initial PVS analysis,  the  PVS  reanalysis must be
            s target ?wi thin 26 hours after  the  start  of the current
            analytical sequence.
                            D-42-PHEN-Q
                                                          8/23/94

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                                                                          DRAFT

      18.1.5      The method blank and all associated samples shall be
                  analyzed in  the same analytical sequence.  If samples  from a
                  batch are analyzed in more than one analytical sequence,  the
                  associated method blank must also be;analyzed in the same
                  analytical sequence.  If a method blank extract is used up
                  because  of multiple analyses,  the*Laboratory shall
                  substitute an instrument blank iiyplace--,o£ «a method blank in
                  all subsequent analytical sequences.  The''laboratory shall
                  note  this in the Batch Narrative and shall use ;jtshe EPA
                  identification number as described in Exhibit B ^fpr^this
                  instrument blank.

      18.1.6      The LCS  shall be analyzed<*rith all associated samples  in  the
                  same  analytical sequence';* •  If samplers.5from a batch are
                  analyzed in  more than one ^balytical;,-sequence, the
                  associated LCS shall be analysed -it*."the same analytical
                  sequence.  If an LCS extract is'-^tti&d up because of multiple
                  analyses,  the Laboratory shall di^&beq the LCS standard
                  mixture  (the original stock mix) and 'itse',this solution in
                  place of the original LCS sample in all"' subsequent
                  analytical seqiiepbesf j|sjee .paragraph 27).  The Laboratory
                  shall note this'u^t the''Ba^^^Siaxa1:we and shall use the  EPA
                  identification number as desetribed in Inhibit B for this  LCS
                  Solution.          ' ?       /"'
                                            ; -
18.2  Computer reproductions of chromatograms that axe attenuated to ensure
      that all peaks are on scale over a lOQ-fold range are acceptable.
      However, post analysis'jiie&enuation slfiill be no greater than a 100-fold
      range.  This is t& reduce^ttjte potential^for RTS of compounds due to
      column overload'sssid  to enstiee that the detector is operating within the
      calibration raipge.   If any sample compounds exceed the calibration
      range, they fliill be dilutes?according to paragraph 19.
                  -' !-               '      ' '   "'"
18.3  If any saturated^-'isom-.farget compound chromatographic peaks are evident
      or if any chromatographic  peaks overlap more than one RRT and/or RT
      target compound windows^-^ffete Laboratory shall use the "E,N" flags on
      Form QlrEHE tio'-indicate  tfii$5|situation.
                  If  satu^||ted chromatographic peaks outside target compound
                  RRT and/oT',§lT windows are evident, flag the nearest target
                  compound ^fjN" on Form QI-PHE.
                  If chromatfgjfaphic peaks overlapping more than one target
         <:>; ;,     compound RlgE5 and/or RT windows are evident, flag the
            4: ;>,;'  corresponding target compounds "E,N" on Form QI-PHE
                 '•'•''''\~     f,-~'
18.4  Chromatographllc fteaHc^Tesponse  must be greater than 10 percent and
      less than 100 peirc«st of full-scale deflection to ensure that
      individual compounds will be visible during data review.


                                  D-43-PHEN-Q                           8/23/94

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                                                                          DRAFT

19    Dilutions

19.1  Samples with compounds exceeding  the  calibration range of the GC must be
      reported with the "E" data  flag as  described infJ&hibit B.  Upon
      evaluation, the Region may  require  that the samples be diluted,
      reextracted, and/or reanalyzed in a valid analyti«&3l sequence as
      additional paid samples.  Reextraction and/or rearialysis of samples can
      only be authorized by the CLASS contractor acting on "be&alf of the
      Regional TPO or Headquarters APO.   The Laboratory shall perform the
      dilution analysis as specified below  in.paragraph 19.2.     ,,'

19.2  The Laboratory may dilute samples prioac to initiating sample
      extraction/analysis.  The resulting^sniilysis of tpbtose samples must
      produce chromatograms with  at least|one target compound present at a
      concentration greater than  or equal ^to.fthe mid»''f>6int calibration
      mixture.  If no compound is identified las! fiheilSiluted sample at a
      concentration that exceeds  the mid  level standard,  then the undiluted
      sample shall be reextracted and/or  reanalyzed at ^ao additional cost to
      the Agency.                                      ''*<  "•'
      19.2.1      At the requesfe^if'CNtTpt^ttxn,.sample dilution may be
                  required prior ~%*,s>the  irif€im,|'iKKSferf*Jt3Lon and analysis.  If
                  no target compounds  are  detected in -the diluted sample at a
                  concentration that^exceeds (jghe mid level standard, then the
                  undiluted sample shal!! be, r^extracted and/or reanalyzed as
                  an additional paid sample.

      19.2.2      Dilutions-j»>,^01vent  extracted,  oil,  and wipe samples

                  1942J2.1    Dilutions  of sotront extracted,  oil, and wipe
                   ;~r         saagjkes  shall be'=made by using an appropriate
                  ,,-  ,,         al^ppts.Qf-^fhLe extract diluted in hexane.
                   '  :  -•-,      Ali^r-ititaklj^,^ dilution, add sufficient SMC
                      •?-; J.,  solution to  bring up to proper concentration (50
      19.2.3  -~,.. 'idUUktions - SPE-ypxtracted samples
           -  -'-'" -  =':.{'.         ^;;y>
                            .-  Dilutions of water samples shall be made by
                            |l using  an appropriate aliquot of sample diluted
                            •f-'to  100 mL with methanol/water (0.5:100) at a pH
                            i;5of  £ 2 with 5  g of Nad (see paragraph 15.3.2).
                            |-,Xontinue with  sample extraction and cleanup as
                            xfvtiescribed in paragraph 15.
                            • P'
                            :<'<'
                            '" NOTE:  Dilute  samples prior to the addition of
                              the SMC.
      19.2.4      Sample dilutions  shall be analyzed in a valid analytical
                  sequence which  includes  the associated method blank and LCS.

                                  D-44-PHEN-Q                           8/23/94

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                                                                           DRAFT

       19.2.5       If sample reextractions and  reanalyses are required, the
                   Laboratory shall also reextract  and reanalyze an associated
                   method blank and LCS.

20     Identification of Target Compounds               :
                                                     "*'  &
20.1   Retention Time Standard - The SMC shall  be us^d as -t:l*fe,£T marker for
       compound identification.  The SMC shall  also be used to imonitor
       extraction efficiency.                                    !, *',''(,:

       20.1.1       The SMC shall be added to alt field and QC samples pi|ior to
                   extraction.                
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                                                                          DRAFT

20.4  If multiple peaks  are within the identification windows (target compound
      and SMC), the Laboratory  shall use professional judgement to properly
      identify the appropriate  peak.  The Laboratory should consider the
      inherent matrix  effects of  the sample on peak shifting, masking, and
      overlaps when making identification determinations.  The Laboratory
      should take into consideration the mean RT and f> <£rom the initial
      calibration, RT  and RRT from the calibration^eheck'sesBxdard, and the SMC
      RT from relatively clean  samples analyzed before and attest the sample in
      question as a basis for selecting the most appropriate peafe;;'. The
      Laboratory shall describe in the Batch Narrative the rationaleJased for
      choosing a particular peak  (e.g.,  chose|Ipeak closest to the RT 'of^.the
      peak in calibration check standard) as'Mthe target compound or SMC and
      how the field sample matrix may havej.-.affected peak' identification.

21    Calculations
                                             ' '5 ^''V
21.1  Calculate the RRT  of a sample component or a^sfeandard using the
      following equation:                            'if  -

                                   •-.-...   grcoqpnn«nt                   EQ. D. 11
      Where:                         ','         ',

      RRT - relative retention  time     'f   /

      RTcomponent = reteati»» Siae of the  target compound
                                •^            ri
      RTSMC = retent jj&ti time  of 'tisfe  SMC      ^;
                    ;V£            I' - '             *'
21.2  Calculate thei-sealibration jias^jf.pr, „£o^ a  compound by one of three
      techniques using sdata coLle^edNdualfcnig1 an acceptable initial calibration
      (paragraph 8).  di&J|r5yone  of the quantitation techniques listed below
      shall be used for qfraaafiiitating samples  within a Batch and analyzed
      within a given analyticatLiiSjeguence.   The  use of the line segment or "K"
      curve if —~	'—'          ''''
                      ^'•T j,         '"'-?•'
                  Use thfe'l'JK;11  curve  (line segments) established during initial
                  calibration.  The  segments run from the low to the mid point
                  and from  tile, mid to the high point calibration mixtures.
                  Many data systems  calculate "K" curves automatically.
                  (Note: do &$t extend line segment through the origin if the
                  concentradtiih is below the CRQL).
      21.2.2   "^:^f^  thess«iibration factors based on the mid point of the
                  i«S|t%ai|;6alibration curve.   This option may be used as long
                  as tife;pid point  values are within ± 10 percent of the
                  average of the high and low point values.
                                  D-46-PHEN-Q                           8/23/94

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                                                                          DRAFT
      21 . 2 . 3      Use the mean  calibration factor established during the
                  initial calibration.

      21.2.4      Quantitation  of compounds is based oa the calibration
                  factors established during initial calibration.
      21.2.5      All calibration requirements,  including t&e initial
                  calibration %RSD and  the  calibration check ZJ> criteria, must
                  be met regardless of  the  quantitation technique used.

21.3  Quantitation of Target Compounds       ,;';

      Calculate the concentration in the saasple  using one of the following
      equations for external standards.  Ifee response scan be measured by
      automated peak height or  integrated peak area Jtt&asurements.

      21.3.1      Water

                                               (A ) (VO  I              EQ. D.12
                     Concentiation (]ig/L) =      x


                  where:         "'<•*      ""'•"'",&•;. .  ^

                  AX    -     response  for  thei.analyte to be measured.

                  CFm   -     calibration ,fk<6tor established by one of three
                              techniques <^aring  the initial calibration.
                            v .(ilOTE: Only oae, method of quantitation may be
                              tised for  samples within a Batch and analyzed
                    ,*|        wil&Ln a  given !!inalytical sequence).
                              vol^qne ,of r concentrated extract (use 1000 ^L or a
                                            s! when dilutions are made).
                  V^    = >  /!volume of extract  injected

                  '%    =     volsipe of water  extracted (mL).
                   '•  H-' -••         *s:<' ^

                  Soll/Soi^t^.(Wet-weight basis)  and Oil

                                               UJ  (ve)                 EQ.  D.13
                     Conception
                         f' V^ — same as given in Equation D.12

                  Vt    =     volume of concentrated extract (use 1000 jiL or a
                              factor of this  when dilutions are made).

                                  D-A7-PHEN-Q                           8/23/94

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                                                                          DRAFT

                  Ws    =      weight of sample extracted in g.

21.4  Calculate the SMC amount observed and amount (percent) recovered using
      equations as described in paragraph 10.4.

21.5  RTS shall be monitored using  the SMC (paragraph 20»1) .  The RTS shall be
      measured for all analyses .                    ;        :

      21.5.1      Calculate  the retention time percent difference,; {RT %D)
                  between  the RT  of the SMC in;*he field and QC samples or
                  subsequent standards analyzjed and the mean SMC RT fr«a most
                  recent initial  calibration ;ianalyzed using using the
                  following  equation.      :- •          ,;'

                                                                     EQ-D-14
                  where :

                  RT %D =      retention time  percent difference.
                  RTS   •=      retiajij^ion tite-'^ £%eiSHC.,in a field and QC
                               sample  or subsequent  standard.

                  RTC   =      mean retention 6ime of the SMC from the most
                               recent  irii£ia|t calibration.
22    Technical Acceptance	
                        •  '     •-'•*•          '•'
22.1  Each sample witfein a Batch':-Jhall  be  analyzed on a GC system meeting the
      initial calibration or valill,~calibration «heck standard technical
      acceptance criteria  (parag£$td|&. 8 .and, 9) .
22.2  Each sample within A Batch  shall  be  analyzed after an acceptable method
      and instrument blariMjjJpacagraphs  25  and 26),  and after an acceptable LCS
      (paragraph 27) are
22.3  Each ,Sf«i&e Vitlijfc&j » Batch  sfft£KL"be run within a valid initial
      calibration or daiij^siealibration check analytical sequence that
      concludes with an ao&tfjJQj^able  instrument blank (paragraph 26) and an
      acceptable PVS (paragr|fh 10).
     : ,;|U                    l!:
22.4  ISttdfelHiSample within a B^fech  shall be analyzed and results reported within
      the''*!e|pp6ract required .Jptkrnaround times.
              ' ?' \           ~
22.5  Each sample matrix wjt^nin a Batch shall have an acceptable method blank
      analyzed duriigg 1^tie,|same analytical sequence.

22.6  The RTS for the SMC must be within ± 1.0 percent between any sample in a
      Batch and the mean RT of the  SMCs analyzed during the initial

                                  D-48-PHEN-Q                           8/23/94

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                                                                          DRAFT

      calibration.   The  RTS  is not evaluated if the SMC is not recovered or  if
      peak interferences are present.

22.7  The advisory  recovery  limit for  the SMC is 50-150 percent.  Reanalyses
      of field samples are not made if the SMC recovery is outside the
      advisory recovery  limits.                         :••

22.8  The SMC recovery must  be greater than or equal to 10 percent and less
      than or equal to 200 percent in  order to use RRT for identification
      purposes.  The identification window is ^0.008 unit of the messa RRT of
      each target compound from the initial dss&Ibration.  If the recovery of
      the SMC is less than 10 percent,  greater than 200 percent, or if peak
      interferences are  present (but is adequately recovered in the method
      blank), the absolute RT of the compounds shall b%:tised for
      identification purposes.    The identification window is ± 1.0 percent of
      the mean absolute  RT of each target compbojad sfrom the initial
      calibration.                                  :> ,

23    Corrective Action

23.1  Flag all sample results "S?;1aiL;$fie"SE|3,,;is.outside the advisory recovery
      limits of 50-150 percent.   -'K     '  "-«h;,- ::,   :  ;,

23.2  Flag all sample results "T" if' *"he absolute RTs are used for
      identifications.                  ,      ;

23.3  An SMC recovery of less than 20  percent in the method blank or LCS
      associated with a, saopl^J&atch. is an iattdication that serious problems
      may have occurred:during!?ilcl% extractioi&iirocess.   Corrective action
      shall be perforated and the Niiiacceptable >:method blank and/or LCS and all
      samples associ«teed with thei;«macceptable method blank and/or LCS shall
      be reextractid and reanalyzpai^a-t,no.,. Additional expense to the Agency.
                     •^•', f         , i-  •• "< '<  ,~  5 ,  ',' ^ '
                     ,f   „,      * * ,< * ' * ^.K; - * ,' "",, ;., „£ (
23.4  If the SMC retention .time  shift  (RTS) criterion is not met for any field
      sample, sample analysis; shall be stopped and the noncompliant sample
      rerun.  If the RTS critissjclfaa is  still out upon reanalysis analyze an
      instrument:ItaSUoak,^  If  the  S^Cpiment blank SMC RTS is outside the
      criteci|on;;' 'peffVs4ii;:corrective --afction, which may include a new initial
            ation.   DO NOT^sontinue with sample analyses until the RTS is
               1.0  percent;»i|j4f the instrument blank SMC RTS meets the
                 sample  analyses  may continue.   The Laboratory shall report
           sets of  noncomplisiit  sample data and flag the results "M".  Note:
            S is not evaluated,if the  SMC is  not recovered or if peak
      intteatfjerijences are  pres

23.5  All targetiiiboig)ound;ib
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                                                                         DRAFT

      not meeting any one of the contract technical acceptance criteria and
      not requiring automatic reextraction and/or reanalysis shall be flagged
      by the Laboratory.   The Region will evaluate the noncompliant samples
      and may specify that these be reanalyzed as additional paid samples.

24    Documentation                                   i;  -

      Sample results shall be reported on Forms QI-PHEN and
      Reporting requirements are listed in Exhibit B.
                                 D-50-PHEN-Q                           8/23/94

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                                                                          DRAFT

                                   SECTION V

              SAMPLE QUALITY CONTROL PROCEDURES AND REQUIREMENTS


25    Method Blank Analysis

25.1  Summary - A method blank  for water  samples  is 100 mL oifi tr««gent water
      spiked with the  SMC  and carried through the entire analytical scheme.  A
      method blank for soil/solid samples is  6,g  of clean quartz s§na& spiked
      with the SMC and carried  through the entire analytical scheme.  A.Sinethod
      blank for oil samples  is  6 g of clean «orn  oil spiked with the SMC and
      carried through  the  entire analytical jscheme.   Method blanks shall be
      carried through  the  entire analytical- procedure,;,
                                           '"'"*>         '*
      NOTE: The Agency will  provide  the Laboratory With further instructions
            for the analysis of method blanks for wipe samples.

25.2  Frequency

      A method blank analysis sh«tii>'3a£ ffetfponed  for each matrix type (water,
      soil/solid, or oil)  and witii-f&ach set «Ev samples,..  A set of samples is
      defined as those samples  from  one Batch .that are extracted and analyzed
      on one instrument during  a 24-"hour  analytical sequence.

      25.2.1      The  method blank and all 'associated samples shall be
                  analyzed in the same analytical sequence.   If samples from a
                  batch-are  analyzed in more'-than one analytical sequence, the
                  associated method  blank must:, also be analyzed in the same
                  analytical seqciesnce.  If a  method blank extract is used up
                  because  of mult8.f»le analyses, the Laboratory shall
                  sobstitute an ^m.txument, blank  in place of a method blank in
                  all  -s^sequei^,    '"~AriA'a4f[*i»table methsiS blank shall  be analyzed before running
          •_,;;/     any  samples within an  analytical  sequence.

          .3      When analysing highly  contaminated samples  using SPE disks
                  on more  thap one manifold,  the  Laboratory should analyze one
          :        method blaxjp per extraction manifold.   If an unacceptable
          I' ; •],,    method blank is analyzed and  the  contamination can be
             fj ;->  isolated &* a particular manifold,  only samples extracted on
                       mantfold will have  to be reextracted.   If an
                               method blank is  analyzed,  and  only one method
                  blanki'is used, all samples from all manifolds shall be
                  reextracted.
                                  D-51-PHEN-Q                           8/23/94

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                                                                          DRAFT

      25.2.4      If all field samples  in a  Batch are filtered, the associated
                  method blank shall also be filtered.   If only a partial set
                  of samples in a Batch are  filtered,  then a separate method
                  blank shall be run through the filter,  extracted, and
                  analyzed.

      25.2.5      Criteria for an acceptable methoS blank is,, defined in
                  paragraph 25.4.                                «

25.3  Procedure for Method Blank Preparation „   ;                  *? :>••
      25.3.1      Prepare the method blanks *#£ the  frequency listed in
                  paragraph 25.2.         j '}?

      25.3.2      Measure out 100 mL of  reagent waterftfor each water method
                  blank sample aliquot.      '•    ;;

      25.3.3      Soil/solid method blanks are 6 g  of-clean quartz sand.

      25.3.4      Prepare water awi,soil/solid method blanks as described in
                  paragraph 14 orl 15 dreading on whether solvent or solid
                  phase extractions, |ls utiif^&$l,;'«>; ;„-  „=
                                   '* '' f         •'! 7       "- ,
      25.3.5      Oil method blanks ax$,  6 g  o£jcorn oil spiked with 1 mL of
                  the SMC (50 jig/mL) aa£&. extracted  with hexane.  Follow the
                  sample preparation arid-^tiraction procedures as described in
                  paragraph 16.          ''&•'

      25.3.6      Analyae the nts^iod blank e^^racts.   Calculate the results
                  accoj&ing to pl^agraph 21. ''^,,

25.4  Technical Acceptance Criteria,, ,,
                   ' !'   .         =!X^V?x-" ,-,
      25.4.1      All me€bpd blanks shall be  analyzed within an acceptable
                  analytic«4^equence  on a  GC system meeting the initial
                  three-pointH:jea^fibration criteria (paragraph 8) or valid
                ,: :«salibration cbejpfestandard  criteria (paragraph 9), and the
                     : jȣ<3jeptance  cftLfigisria  (paragraph 10) .
                  The RTS IttE the  SMC  in the method blank must be within ±1.0
                  percent beli^en  the  blank SMC RT and the mean SMC RT
                  calculatedlpjrom  the  initial calibration.
                             ~>M:
                             , i~f
                  The SMC recovery criterion of 50-150 percent is advisory
                |\, only.  Th^lSMC recovery in the method blank must, however,
               8:l••"$$..greater ''than  or equal to 20 percent and less than or
                  &&BJL ,t|5»€200 percent.

      25.4.4      The target compounds or potential interferences in the
                  method blanks must have a response less than one-half the

                                  D-52-PHEN-Q                           8/23/94

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                                                                          DRAFT

                  response in the  corresponding RRT window of the initial
                  calibration low  concentration standard.

      25.4.5      A method blank may  contain a detectable but acceptable
                  concentration of a  target compound (less than one-half the
                  response of the  initial  calibration low :concentration
                  standard).                        -       - ;

      25.4.6      If all criteria  are  satisfied,  the method blaiik analysis is
                  acceptable and samples may be analyzed.  If the wetfeod blank
                  is unacceptable, corrective, action shall be taken anadtan
                  acceptable method blank  music be analyzed prior to analyzing
                  the associated samples.   ;?

25.5  Corrective Action                     ft      j
                                                    •',!•
      25.5.1      If a method blank does not  meet £h$ technical acceptance
                  criteria, the Contractor shall consider the analytical
                  system to be out of  control.   It is tbeflContractor's
                  responsibility fcs,-eliminate method interferences caused by
                  contaminants ir»:*so.lv^nt:s:!I' ^reagents,  disks,  glassware,  and
                  other sample storage  and' •p'iofCessing hardware that lead to
                  discrete artifacts;iand/or elevated baselines in gas
                  chromatograms.   If ^contamination is a problem, the
                  Contractor shall invelstigftile' the source of the
                  contamination, and appropriate corrective measures shall be
                  taken and documented before further sample  analysis
                  proceeds, ;;<;'? ?:.
                      -., I  '  "• r|, ,\          ',»,-.„
      25.5.2      If ,ife|;compound S^'found in the^method blank (less than one-
                       the response in the corresponding RRT  window of the
                          calibr^^on,, lo,wrst  to the Agency.
        •'Y i; -;', _              {-,:,!
      25.5.4;-^V;;b .Flag all j^ithod  blank results "S" if the SMC does not meet
               ""'Mdte advisory recovery criterion of 50-150 percent.

      25.5.5      If tTiedRTS criterion  is  not met for a method blank,  sample
                  analyses shall be stopped and the noncompliant blank rerun.
                  If the RTS criterion  is  still out on reanalysis,  corrective

                                 D-53-PHEN-Q                           8/23/94

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                                                                          DRAFT

                  action  shall be performed, which may include a new initial
                  calibration.  DO NOT continue with sample analyses until  the
                  RTS is  within ± 1.0 percent.

      25.5.6      Any samples processed with a methodIblank that is out of
                  control (i.e.,  does not meet any ,of" "t&e technical acceptance
                  criteria)  shall be reextracted and/or reanalyzed at no
                  additional expense to the Agency.

25.6  Documentation

      Method blank results are reported on Fcspms QI-PHEN and QVI-PHEN.
      Reporting requirements are listed in:;t&hibit B. ,(

26    Instrument Blank Analysis             =' ,,      .'••

26.1  Summary

      An instrument blank is 1 mL of methylene chlorideXJtf .-samples are
      extacted utilizing  SPE or 1 mL p,f hexane for solvent Extracted, oil,  and
      wipe samples.  Instrument b||s«^ sake-^^ked with 25 pi of SMC (2.0
      mg/mL).   At least two  accep"tslal»;j.e instS*te»»t,;l>l«siks shall be analyzed
      within an analytical sequence ^?one befor«fsample ^analyses and one
      following sample analyses.     \  ,      ,,| '•

26.2  Frequency                           ,   '

      An instrument blank-jslmll:,be analyzed->at least twice during the
      analytical sequeabe' 'to ettettte that theiJtustrument is free from potential
      contaminants.  ;1Cbe  first instrument blank analysis shall be performed
      after the initial three-poiigt calibration in the initial calibration
      analytical sequence or as dp ,fi?Lrst.,,analysis in a daily calibration
      check analytic^ ^quence^4'fi^e*?:»ecao|t|S-instrument blank analysis shall
      be performed immediately before the PVS analysis.  The Laboratory is
      encouraged to run addit&Qnal instrument blanks during the analytical
      sequence, especially wh«»,,%ighly contaminated or complex samples are
      analyzed^-- ..Jl&SfCrument  blanfckjsaust be analyzed after analysis of samples
      with Jtei^n" levels*itkf ^target compcmnds or interferents (see paragraph
      26.5^6).          ''"'•
26.3  l^pcedure for InstrumeaBO:; Blank preparation
     M-.                     ^
      5At» ;-^astrument blank is.,|i'-mL of methylene chloride if samples are
      ext'ase&agrd;, utilizing  SPEn^r 1 mL of hexane for solvent extracted, oil,  and
      wipe slN»ij3l>fes.   Instrusasit blanks are spiked with 25 /jL of SMC  (2.0
      mg/mL).  :-'4,  , ,     4-S
                                  D-54-PHEN-Q                           8/23/94

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                                                                           DRAFT

26.4  Calculations

      Concentrations  of the SMC and any target compounds in the instrument
      blank are calculated according to the procedures described  in paragraph
      21.  Note: The  target compound concentrations ,(Detected concentrations
      and CRQL values)  in the instrument blank shall be deported  in the
      appropriate concentration units (e.g., reportp-in ftgX!L':Af t'ie associated
      samples are water and in ^g/Kg if the associated samples jare soil).

26.5  Technical Acceptance Criteria            i                   '"v:

      26.5.1      A minimum of two (2) instrument blanks shall be analyzed
                  during an analytical seq&ieiice on a GC! system meeting the
                  initial three-point calI3^c,ation criteria (paragraph 8)  or
                  the valid calibration chefefc standard criteria (paragraph 11),
                  and the PVS acceptance criteria, (paragraph 12).

      26.5.2      The RT for the SMC in the instrumetit blank must be within ±
                  1.0 percent between the blank and the:uttean SMC RT calculated
                  from  the initiaj,-, calibration.            :
                                 ;>J -"VJ| "*>„* !;;-,;• ,,
      26.5.3      The SMC recover^ 'criter'ioTi"Kdfe;§p-il50 .percent is advisory
                  only.   The SMC ret^Iuvery in t|tevinstr^aient blank must,
                  however,  be greater-jttian or/iqual to 20 percent and less
                  than  or equal to 200|j>erce3it.

      26.5.4      The target compounds or;jw»t:ential interferences in the  first
                  instrument blank (analyzed; immediately after the initial
                  calibltt&rtion 6%~iaefore a va^JM calibration check) must have  a
                  resjj^snse less iSan one-half tfabe response in the
                  corresponding K^T windows of "':the initial calibration low
                  y-iUs^el standard^-!': ._,

      26.5.5      Subsequent instrument blanks are acceptable with low level
                  contamina&Son.   These instrument blanks may contain target
                  compound cbiijS^titrations up to twice the CRQL (2x CRQL) .
      26.5.,6;> "i~-  ''Tolipi^ig  the anM^is of a field sample containing high
         .,:. ••<'      levels;"^|?target compounds or interf erents , an instrument
        ,4'J        blank sna|3t: ^e analyzed and must meet acceptance criteria
      ,:;:'Z'        before preceding with sample analyses.  If an autosampler
                  is utilize^|:. then the field samples run after a high level
                  sample musCfbe carefully evaluated for carryover.  The field
                  sample immfiiilately following the high level sample shall be
                  reanalyzes!;,! along with any other samples analyzed after the
                       ley^t sample which shows evidence of carryover.
                           '
      26.5.7      High'Stevel  samples are defined as being field samples that
                  contain target  compounds at concentration levels that exceed
                  twice the high  calibration standard concentration and/or

                                  D-55-PHEN-Q                           8/23/94

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                                                                          DRAFT

                  interferents  that are  detected at levels greater than the
                  mid level  initial calibration concentration response of the
                  nearest target compound.

26.6  Corrective Action

      26.6.1      All groups of samples  analyzed snail be bracketed with •two
                  acceptable instrument  blanks.   If either instrument blank is
                  unacceptable, corrective  action shall be taken ^nd all
                  samples not bracketed  by  twotwalid instrument blaaaScis shall
                  be reanalyzed at no additional expense to the Agency, •

      26.6.2      If the response of any target compound in an instrument
                  blank analyzed after tlss  initial caU3*ration or before a
                  valid calibration check siasjdard is^-greater than or equal to
                  one-half the  response  in  thfe•/asorxes.ponding RRT window of the
                  initial calibration low concenti>a"tion standard, corrective
                  action shall  be performed and the S|RSf;em shall be
                  demonstrated  to be clean  by  the analysis--of additional
                  instrument blanks until all  target compounds are less than
                  one-half respooseevi , j'"- --, ,.,
                                 '•*$$?    "•«>"= '"* '"I",'' £ '
                                  t       ""'"' ;*,'  '  ?,•<.::
      26.6.3      If any target compound in anSfastronietit:'blank analyzed after
                  field/QC sample analyses  is ifreater than two times the CRQL,
                  another instrument blJank  sball be analyzed.  If, on
                  reanalysis, contamination li-till exceeds criterion,
                  corrective action shall'-T^ie performed and the system
                  demonstxa*«4fiito be clean1. /'Then,  all associated field/QC
                  samples"5'anaijrz^ since the(3Jast valid instrument blank or
                  met^ifca blank  wfipeh contain "ifctoose target compounds or
                  ilBserferents  fcfRld in  the instrument blank at levels greater
                       twice thejjpEQL^shall be rerun.
      26.6.4      If an:instrument blank  (other  than the first instrument
                  blank iti'it&e,,analytical  sequence)  contains target compounds
                  or interfering .between  one-half response and two times the
                      », all posit:i.4e,>results (results greater than or equal to
                            for thoS^Ncompounds  in samples analyzed after the
                  last Va^&L instrument blank  shall  be flagged with a "B".

         ,86.5      Flag all ^^itrument blank results  "S" if the instrument
                  blank SMC IIInot within  50-150 percent.

                  If the insjfcCument blank  SMC  recovery is less than 20
                  .percent, ,^§reater than 200 percent, or if peak interferences
                  ,-tee presiest, sample analyses shall be stopped; corrective
                  ac%Ifjn.<£»ierformed, and another  instrument blank shall be
                  analf3&6aa.  If the SMC is still out upon reanalysis,
                  corrective action which  may  include a new initial
                  calibration shall be performed.  All samples analyzed since

                                  D-56-PHEN-Q                           8/23/94

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                                                                           DRAFT

                  the  last  valid method or instrument blank  shall be
                  reanalyzed after a valid instrument blank  has been obtained.

      26.6.7      If the  RTS criterion is not met for: an instrument blank,
                  sample  analyses shall be stopped and another instrument
                  blank shall be analyzed.  If the,;BfS^criterion is still out
                  on reanalysis, corrective actio&.which aay include a new
                  initial calibration shall be performed.  DO SQT continue
                  with sample analyses until the RTS is  within ^ U;0 percent.

      26.6.8      Any  samples not bracketed byfvalid instument blanks pr a
                  valid instrument blank and a method blank  and shall be
                  reanalyzed at no additional expense ta» the Agency.
                                          > ,'         - -fi
26.7  Documentation                        ' _ '• ,.     -t -
                                               t[ :  '3
      Instrument blank results are reported on Forafe QI-PHEN and QVI-PHEN.
      Reporting requirements are listed in Exhibit IB,.,

27    Laboratory Control  Samples ;  >.,.,,
                                 V*>:;. *•> "-,g .-  .
27.1  Summary                     "'\-.       "'~"°- T, >; •   - j,,,
                                    ~          •'  '-  •t./iZ:
      The QTM Phenol LCS  mixture initially will be supplied  to contractors by
      the Agency.  The LCS  mixture will ;coneain target compounds at several
      known concentrations.   The Laboratoryfihall spike  the  LCS mixture into a
      clean matrix that is  similar to the ^samples being  analyzed.   The spiked
      matrix shall be  p;resyar«
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                                                                          DRAFT

                  •     Set of  oily  field samples (LCS prepared with corn
                        oil).

      27.2.2      The LCS shall be analyzed with all associated samples in the
                  same analytical sequence.   If samples, from a batch are
                  analyzed in more than  one analytical ils«quence,  the
                  associated LCS shall be analyzed in the same analytical
                  sequence.  If an LCS extract is used up because of multiple
                  analyses, the Laboratory shall use the original|;Stock mix
                  diluted into  hexane in placejof the original LCSf> sattple in
                  all subsequent analytical sjesjpuences.   The Laboratory ;:^hall
                  prepare this  solution  by sffituting 100 ftL of the LCS standard
                  mixture into  5 mL  of hexane and concentrating to 1 mL using
                  nitrogen blowdown.  The ^laboratory sUtall note this in the
                  Batch Narrative and shall: use the EPA identification number
                  as described  in Exhibit B facHihisM.CS solution.
27.3  Procedure
      Spike the appropriate matrix. >,with  the  LCS  standard mixture and prepare
      as follows.               • •;_ ^ ,;',,[•"' *\ -,,

      27.3.1      Water LCS        ' \          J;

            27.3.1.1    Allow the LCS is|LxturS; ^ampules  to reach room
                        temperature be for* ?O|Jening .  The ampules must not be
                        opened until preparation/ analysis is to occur.
                              se care in breaking the  ampules open to avoid
                                   ,
            27.3.1.2 •   Spike  100 pL of  reagent water with 100 pL of the LCS
                   ;, .   standardtireb|,ture. as  described in the instructions
                   •- :- -,,provide4.?^^i *£j&& |S*S mixtures.   Use syringes to
                        ,;;P«rform  the spiking  to ensure accuracy.  Add the SMC
                        an4 ;aix  and carry through the extraction and clean-up
                        process las described in paragraph 14 or 15, depending
             ,.,;„::;; ,,;    on whethe^isolvent or solid phase extraction is
             p* "' ""•''•*•• -V, ^utilized.  4fe«(ceed with the analysis as described in
                       '            18.'
                                  D-58-PHEN-Q                           8/23/94

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                                                                     DRAFT

       27.3.1.3    Nominal aqueous LCS target  compound concentrations are
                   as follows:

                   Phenol                         2000  /jg/L
                   o-Cresol                     . •  160  jtg/L
                   p-Cresol                     >  l£00  jtg/L
                   2-Nitrophenol             , ;•    360
                   2,4-Dimethylphenol             1800
                   2,4,6-Trichlorophenol           100
                   4-Nitrophenol          -        2100  pg/L      ;-
                   4,6-Dinitro-2-methyl#itenol      300  /tg/L
                   Pentachlorophenol              1800  /tg/L

 27.3.2      Soil LCS                           ,
                                       . '        ;
       27.3.2.1    Allow the LCS mixture -^ssjsul&s  to  reach room
                   temperature before opening,/ The  ampules  must not be
                   opened until preparation/analysis is  to occur.
                   Exercise care in breaking the  ampules open to avoid
                   injury.
       27.3.2.2    Spike 6 gietf quarte'saM --witfe ,100  pL of  the LCS
                   standard mixture as described  in "the instructions
                   provided with,: the LCS|mixtures.  Use syringes to
                   perform the spUgLng-'-tfO ensure  accuracy.   Add the SMC
                   and mix and carry through the  extraction and clean-up
                   process as described in paragraph  14.  Proceed with
                   the analysis as described in paragraph 18 .
       27.3.2.3.; V Nominal T%}S target coiapound concentrations  are as
                   follows: : f
                 ^-.Phenol -^!.?->#-. j'. = !          33,333
                   o-Cresol                       2,700
                                                 27,000 jjgAg
                                                  6,000
        -;   '     .  2,4-Dimetliylphenol            29,000
    ,?>1 »"•'•""'  -; ;;2,,4,6-Tricfilidtophenol           1700 ^gAg
   ,':'J:'           "4-lp.trophenol                 35,000
  ",;?'"              4,%«^initro-2-methylphenol      5000
  " •''''               Pentiehlorophenol             30,000

"2?-,||.3       Oil LCS   '=:':,

This section has not lieen finalized.  The LCS composition and
concentrations for oils are currently being investigated.
             ' ''*\\~\fi '~
      27.3.3.1  - J.;mllow the LCS mixture ampules to reach room
                   temperature before opening.  The ampules must not be
                   opened until preparation/analysis is to occur.

                            D-59-PHEN-Q                            8/23/94

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                                                                          DRAFT

                        Exercise care in breaking the  ampules open to avoid
                        injury.

            27.3.3.2    Spike 1 g of corn oil with 1 mL of the LCS standard
                        mixture as described in the instructions provided with
                        the LCS mixtures.  Use  syringes tic perform the spiking
                        to ensure accuracy.  Mix and carry through the
                        extraction and cleanup  process adding;"1.0 mL of SMC
                        (50 jig/mL) and further  prepare as  descriiea in
                        paragraphs 16.3-16.14.                   -   ,

            27.3.3.3    Nominal LCS target compound concentrations are as
                        follows:             ,"           ,

                        Phenol                         33,000 /igAg
                        o-Cresol               '.  ,;      2,700 jigAg
                        m-Cresol                  =     27,000 figAg
                        2-Nitrophenol                   6,000 /tgAg
                        2,4-Dimethylphenol             29;»i$QO
                        2,4,6 -Tripfa^Lorophenol            17GO'
                                                       35,000
                                                         5000
                        Pentachloro^benol      ,;:      30,1000 jtgAg
                                      ';. s      '  f
27.4  Technical Acceptance Criteria    ,=     .,-,

      27.4.1      All LCS compounds, must;<"feave  recoveries  between 30 and 130
                  percent,. •; I^?*o, two LCS oonjpounds may, however, exceed the
                  upper irecover^ajcriterion of' 130 percent.
                     !'-•'',         '*','"•            ,
      27.4.2      A11;,LCS target Compound absolute and relative retention
                  times must be jfitihin, the windows established during the
                  inifcial
      27.4.3      The RT of-'tshe SMC must be  within ±1.0 percent of the mean
                  RT of the ^HCl ^established  during the initial calibration.
      27.4.4,i'-: ' "Tne-«iSMC .advisory ~*Y*|iovery criterion is 50-150 percent.  The
         ,,:; "      SMC recovery  in the LCS  must,  however, be greater than or
         '~f       equal tol^p percent and  less than or equal to 200 percent.
        ;                    ; !'
      •3* *•                     ^
27.5 ,-^rrective Action      Y,
     ''^V;-:>                  i :
      27.^3; ;:,   If any LCSr|cbmpound recovery is less than 30 percent or more
            " ?»  :  ..than two JJsS  compounds exceed 130 percent, the LCS shall be
                '' '..y^nalyzerf.   If,  upon reanalysis, more than two LCS target
                  %ra^euji^  are outside the recovery criterion, the LCS and
                  allSaissociated field  and QC samples shall be reextracted and
                  reanalyzed. If one or two LCS compounds are outside the
                  recovery criterion, proceed with sample analyses, and flag

                                  D-60-PHEN-Q                           8/23/94

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                                                                          DRAFT

                  all  sample  results of compounds that were out in the LCS
                  with an  "L"  flag.

      27.5.2      If the SMC  recovery is less than 20 percent, greater than
                  200  percent,  or if peak interference^ are present in the
                  LCS,  sample  analyses shall be stopped and the LCS
                  reanalyzed.   If the LCS SMC recovery is still outside the
                  criterion,  corrective action shall be performed, and the LCS
                  and  all  associated samples shall be reextracted, and
                  reanalyzed.                   ;;

      27.5.3      If the RT or RRT for any W$ compound is not within the RT
                  and  RRT  windows established during the Initial calibration,
                  reanalyze the LCS.   If tstp^jn reanalysjis a compound is still
                  outside  the  windows,  a new initial calibration must be
                  performed before samples can be analyzed.  The instrument
                  must be  recalibrated as described''in paragraph 8.
                                                    , • r
      27.5.4      If the RTS criterion is not met for tfae ,LCS, sample analysis
                  shall be stopped and the noncompliant LCS /reanalyzed.  If
                  the  RTS  is stilptfsastJJ^I^-f'/^l^,criterion upon reanalysis,
                  corrective actioblNwhich" may 8,ije,fe>dei a.jiew initial
                  calibration  shall i^e performed-  'BO NQfT proceed with sample
                  analyses until the'<13S is within ± 1.0 percent.
                                       ' s
      27.5.5      All  LCS  acceptance  cfitboria shall be met before any samples
                  or required  blanks  are'analyzed.   Any samples or required
                  blanks sa3Bal|^zed when the i£S have not been met shall require
                  reext*»
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                                                                     DRAFT
             COLUMN RESOLUTION CALCULATION
l-O-j
L0-
                                                  % Valley-x/y 100
  B-.3O
  0:50
Time
                                                            fffcOO
                                Figure 1
                               D-62-PHEN-Q
                             8/23/94

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                                                         DRAFT
                   Table 1.
List of Phenol Compounds in Order of EJution*
        Compound

        Phenol
        2 -Chlorophenol
        o-Cresol
        m-Cresol**           v
        p-Cresol**
        2-Nitrophenol      :
        2,4-Dimethylphenol ;
        2,4-Dichlorophenol '  -
        4-Chloro-3-Methylphen61>
        2,4,6-Trichlorophenol***
        2,4,5-Trichlorophenol***
        2,4-Dinitrophenol
        4-Nitrophenol.
        2,3,4,6 -
        4,6-
        Pentachloroifihenol
                                     Retention Time (mins)

                                          2.88
                                          2.919  :
                                          4.36  ---
                                          4.77
                                          5.69
                                          6.05
                                          6.28
                                          8.22
                                          9.01
                                          9.07
                                         10.94
                                         11.35
                                         11.48
                                         12.20
                                         13.69
        This  elution dr4er jsj-given as general guidance and is
        based on suggestsed.Instrumental operating conditions
        as  given in paragraph 7.

       "Compoundstcoelute,  report the total in terms of total
       :Cresol.  ' Qaantitation'siwill be based on the calibration
        factor of,;ji-Cresol.
**
  *** i; ,,
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                                                       DRAFT
                 Table 2.
List of PAH Compounds in Order of Elation
            Compound

            Naphthalene
            Acenaphthylene
            Ac enaphthene
            Fluorene
            Phenanthrene     >
            Anthracene
            Fluoranthene
            Pyrene     ,-'  -'
            Benz(a)anthracene
            Chrysene       ~ • ./•*
            Benzo(b)fluoranthen^ *
            Benzo(k)fluoranthene *
            Benzo(a)pyrene
            Indejjo (1,2,3-cd)pyrene
            D
Retention Time (mins)

      3.95
      7,21
      7.58 -
      8.53  ! ,
      10.22
      10.31
 :     12.37
      12.73
      14.97
      15.04
      16.86

 ' :"  ,17.28 '
      18.92
      19.02
      19.24
           Compounds  coelsit-e.
               D-64-PHEN-Q
                 8/23/94

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                                                              DRAFT
               QUICK TUREiROUND MEEBODS




ANALYTICAL METHOD FOR ORGAN0eHLOR|»E PESTICIDES (PESTs)
                       D-1-PEST-Q                          08/23/94

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                                                                           DRAFT

                               TABLE OF CONTENTS
                                   PESTICIDES

SECTION                                                                    Page

I     Introduction	,	D-3

II    Sample/Extract Storage and Turnaround Times              :,
      and Equipment and Standards	£„	D-4

      1      Sample/Extract Storage and Turnaround Times	,',;. .D-4
      2      Summary of Method	,,';;	D-4
      3      Interferences	ȣ'	, I	D- 6
      4      Apparatus and Materials	,	',.	D- 6
      5      Reagents	t,. *	i	D-12
      6      Standards	 ,	. /:	D-13

III   Instrument Quality Control Procedures and Requirements	D-17

      7      Instrument Operating Conditions	»'	D-17
      8      Calibration of the GC_^Hp8,;y% Imtial Calibration	D-17
      9      Calibration of the GC' Astern *-4Oali|>ratiO>n Check	D-22
      10     Calibration of- the GC Sf&tem - FVS/1 ,*........,;	D-25
      11     System Performance - GC Resolution.	D-29
                                       &
IV    Sample Analysis and Compound Identification and Quantitation	D-31

      12     Summary... . ,i,^ ;,. .-*;...,	,	D-31
      13     Phase  Separation.!. „;»],	,;lv	D-31
      14     Solvent Extraction atp Cleanup. ....,,	D-32
      15     Solid  Phase Extractioltt;>and Cleanup	D-37
      16     Sample /Preparation a^idL Extraction  - Oil  Samples	D-41
      17     Sample 'Preparation ,^fc|g*t^c1cioti  - Wipe Samples	D-41
      18     Instrumental-Analysis	D-42
      19     Dilutions	-.'; ,i,,	D-45
      20     Identification ofslTsiSget Compounds	D-46
      21     Calculations	••.,„>„	D-47
      22   „  -f«cshnical.^e^ptance Crl'fceria	D-50
      23  ;?  Corrective Ac^Blfn	D-50
      24;;-;; ^Documentation. Ji-^,	D-51
       . wi-'                    ••"' £'
V    ,,:|ifiaHple Quality Control Procedures and Requirements	D-52
      25 *>!;^ethod Blank Ana|.^is	D-52
      26    "ij^tfeiment Blan&:-^nalysis	D-55
      27    Lab'oieat^rj ConS^ol Samples	D-58
                                   D-2-PEST-Q                           08/23/94

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                                                                    DRAFT

                             SECTION I

                           INTRODUCTION
This Quick Turnaround Method  (QTM) is designed for iuse  in  determining
the concentration of various  organochlorine pesticides  in  water,
soil/solid, oil, and wipe samples.  Exhibit 0  lists  the>compounds  that
will be determined by this method along with the  Contract  Squired
Quantitation Limits (CRQLs).  The method .yields identification: jand
quantitation of the analytes  listed in J&Siibit C  using  single  column gas
chromatography/electron capture detector  (GC/ECD).   Target compound
concentrations in samples are reported" on an "as^received" basis;  no dry
weights are calculated.  The primary;§»bjective of this  QTM is  to provide
analytical data in a timely manner f»r, -s&ecisios-making  during  site
inspections, remediations, and emergency''       v\ *~;            ;
                            D-3-PEST-Q                           08/23/94

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                                                                          DRAFT

                                  SECTION II
                  SAMPLE/EXTRACT STORAGE AND TURNAROUND TIMES
                                      AND
                            EQUIPMENT AND STANDARDS   ,  ,
1     Sample/Extract Storase and Turnaround Times

1.1   Procedures for Sample Storage           , ',t                   'I  ,

      Samples shall be protected from light sand refrigerated  at 4°C (±  2°C)
      from the time of receipt •until 60 daysjlafter delivery of a  complete data
      package to the Agency.              \- '\           •-,,
                                            ~e         <
                                           * •" V V      '-I**
1.2   Procedure for Sample Extract Storage    " ; ,:,  ;»

      Sample extracts shall be protected from light'and stored at 4°C (± 2°C)
      for 21 days after delivery of a complete data paclfcage to the Agency.
      Samples, sample extracts, and %tajjftards:  sshall be stored  separately.

1.3   Contract Required Sample Turnaround Times' "  '   '-'

      Samples shall be extracted, analysed, <&(!&  a. summary  of the analytical
      and QC. data shall be reported to tWe ^appropriate EPA Region via
      telecommunications network within 4S,^ours (or 72 hours  if more  than
      three fractions ar
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                                                                          DRAFT

      initial calibration,  a mean relative retention time (RRT), a mean
      retention time  (RT),  and an identification window (± 0.005 RRT unit of
      the mean RRT  or ±  1.0 percent of the mean RT) are established for each
      compound.  Mean calibration factors are also established during initial
      calibration and the  percent relative standard deviation (%RSD) of the
      calibration factors  for each target compound *&& Jthe SMC must be less
      than or equal to 25.0 percent for all compounds except: JDDT,
      methoxychlor, and  endrin which must be less than or eqml to 30.0
      percent for a valid  initial calibration.   Sample compound .concentrations
      are calculated  from  the initial calibration using the average'.'ttjE the
      three calibration  factors,  line segmentiy(K Curve), or the mid ptamt:
      calibration as  long  as it is within ±..3.0 percent of the theoretical mid
      point calculated using all  three calibration points.
2.3   A check of the  initial calibration sftaSJlube performed no less than every
      24 hours, using the  mid point calibration^ sspliflfeion.  All calibration
      factors calculated from the calibration check;-aiust be within ± 35.0
      percent of the  mean  values  established during !\|aitial calibration for
      all target compounds and the SMC except DDT,  endrini, ^and methoxychlor
      which must be within ± 40.O^percent.   Identification.i8j!!iidows must also
      be confirmed during  the calib3dation:^5;heck.

2.4   An analytical sequence also isfcludes  method blanks and instrument blanks
      in which no compound can have a -response tgreater than one-half the
      response in the corresponding RKEtwindo*? of the initial calibration low
      concentration standard.   The analyfxe&J sequence shall also include the
      analysis of Laboratory Control Samples (LCS)  and Performance
      Verification Standawdbsfe^PVS).   The Les shall be bracketed  by valid PVS analyses or a
      valid initial calibratio^jipr valid calibration check and a valid PVS
      analysis^ -^- s  - v        '*''';^",,
2.5   A SjfSISem Monitor ost^tund  (SMC)  shall be added to all field and QC
      sasjj&es and standards^ The  SMC  is  used as a. retention time marker to
      csaii|eulate RRTs for th^ldentification of target compounds and to assess
         raction efficiencyJlfHhen the recovery of the SMC in a field sample
              than 10 percent^-greater than 200 percent, or if peak
                    are preset, absolute retention times are used for target
      compott j|)dentificat^^at   The SMC recovery criterion of 50-150 percent
      is advisd^!:o^ly.  Reteialyses of samples are not performed if the SMC
      recovery is oidtsidei''Sh6 advisory recovery limits.
                                  D-5-PEST-Q                          08/23/94

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                                                                          DRAFT

3     Interferences

3.1   Phthalate  esters  are common interferents encountered in pesticide
      analyses.   Interferences  may be minimized by the oise of pesticide grade
      or ultrapure reagents,  thorough cleanup of glassware,  and avoidance of
      plastic materials in laboratory operations.  "."'  /

3.2   A variety  of coextracted  materials including polychloriuated biphenyls
      (PCBs), nontarget pesticides,  and chlorinated diphenyl egte*s,may result
      in interfering chromatographic peaks and Elevated baselines ^m-'^&G/ECD
      analyses.                               '!

3.3   The analytical system must be demonstessted to be .free  from contamination
      under conditions  of the analysis by analyzing method blanks.  Cross-
      contamination  problems  can be minimiz«&t,iby analysing instrument blanks
      after samples  with high levels of targe%?p*V ;'-.'V
4     Apparatus  and  Materials      ~s.;<         .,;'-    '•''• ;

      Brand names, suppliers, and part*tombe«s'"-: are for illustrative purposes
      only.  No  endorsement is  implied.  .Bcpaivalent performance may be
      achieved using apparatus  and materials other than those specified here;
      however, demonstrates ?iil^«equivalent performance meeting the
      requirements of ,ttils ' SC^'lijejthe responsibility of the  Contractor.
4.1   Gas Chromatogrijpli  -  The  gasijehromatography (GC) system shall be capable
      of temperature }programming.|||fld, .fjpw ^control that is stable throughout an
      analytical  seqafeaee.   The,J^^^^»^^tpl>e suitable for splitless or on-
      column injection"onp,!have  all required accessories, including syringes,
      analytical  columns, 'apKlU-gases.  All GC carrier gas lines shall be
      constructed from stainle^'jsteel  or copper tubing.  Non-
      polytetrethylene  (P13F|I}.; thread sealants, or flow controllers with
                               not    *
            Gas Chromatogrlglijr Column -  15 m x 0.53 mm ID DB-5 megabore bonded
            phase silicone-cs^pted fused  silica capillary column (J&W DB-5, or
            equivalent).   (T^; use of a  guard column is also recommended.)
                               '
      4. lf£ ;ibromatography Defector -  The GC shall be be equipped with an
            %l«ii|trpn  captuz£sMetector  (ECD).
               *"'>>•- ' "•••        ,. V
      4.1.3 Gas  cht*ma3&gpjxphy injector - A  deactivated injector specifically
            designed  rt^ditse with 0.53 mm ID columns shall be used for
            collecting data with this  method.   The Laboratory shall establish
            which of  the various injector liner design provides optimum

                                   D-6-PEST-Q                          08/23/94

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                                                                          DRAFT

            performance  with its  specific GC hardware.   Laboratories that have
            difficulty using this method shall investigate the use of injector
            liners with  shapes  or dimensions optimized to reduce injection
            flashback and analyte pyrolysis.   Cold (anibient)  on-column
            injectors that allow  injection directly into 0.53 mm ID column may
            be used  for  this method  as  long as peaks Jare gaussian, retention
            times are stable, and calibration criteria
4.2   Data System  - The GC  shall be  linked  to  a  data system capable of
      integrating  peak areas  for any compound ,4«stected at or above r lone-half
      the CRQL.  It is required that the  Laboratory  be equipped with a ,'FC - or
      microcomputer-based GC  data collection ||*arts: the vss^uum head, the sample reservoir,  a  metal
            clip tf'f&pld the resjWfpp^r.to, the head, a large  volume  receiver
            (gr eater: '^ban 200 m^-^^i^^Bple after elution,  and a small
            volume rece'$wse^ (10-20 mL) for the solvent after extraction.   The
            vacuum holder 5%^fee(pt for the solvent receiver)  is  sold as  a HPLC
            solvent filtraticfeijeyice (Gelman 4012, or equivalent).   The
                      ;eiver is «|ip»ly a tube with a ground  glass fitting that
                                  '
            Vacuum manifol^|f» a 4- to 6-port vacuum manifold may be used  to
            facilitate simultaneous disk extractions.
            Vse of depth filler (Whatman Multigrade GHF 150, or equivalent)  or
            iJiert materials |Xch as Celite 545 (diatomaceous earth, Baker #,
           "o-^v^uivalent) ,«^e encouraged when samples contain particulates.
            If se|«ih,,filtejrs-'are utilized, each lot shall be tested for
            contami«s&ip;R.|prior to use with this method.  The depth filters
            may be che<^te in conjunction with the SPE disks (depth filters
            are placed oh top of the SPE disks) by following the procedure
            outlined in paragraph 4.3.5.

                                  D-7-PEST-Q                    .      08/23/94

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                                                                     DRAFT

4.3.5 Solid Phase Extraction (SPE)  Recovery Check

      4.3.5.1     Summary

                  Before field or QC samples are extracted using the SPE
                  disks, their efficiency shall:fee verified.   An
                  extraction recovery and contamination check shall be
                  performed in order to evaluate the"recovery of
                  compounds on the  disk and to check for contamination.

      4.3.5.2     Frequency            ;'H                      '""''

                  A  check  shall be  performed on each individual  lot of
                  disks, and for  eveicy 300 units sof a particular lot.
                                     -  f:       t  :
      4.3.5.3     Procedure           "' -i'' r   :?

                  4.3.5.3.1   Before samples are;iextracted using a lot
                               of  SPE disks, the Isalioratory shall perform
                            -,.„ A recovery check of that;41ot.   Two (2)
                           ,  -si;<^ec|^ solutions shall be'prepared.   The
                            ":;• ,firs't""l^::S&p;JiB£,^iof!S: jreagent water spiked
                             ""••KSLth  1 ml &£'* the -l&w., initial calibration
                               sjtandard ,0so demonstrate lack of
                               contamination), and the second  is  100 mL
                               of  rieagjeat water spiked with 1  mL  of the
                               high  initial calibration standard  (to
                   <   ; ,,      demonstrate adequate SPE capacity).
                         ';  :•-,           tb
               '1 I'4.3.5.3.1*-   The low aad high SPE recovery check
              %             :'f  standard solutions used to evaluate SPE
              ;:            .,;;,• .disks .are prepared by diluting  the
            '-•>'-,•,<,         :^rv]aca^g|^si,::stock calibration solution in
                 :   ,,,         methanol.  The low and high SPE recovery
                     r=; ,       standard concentrations are equivalent to
                        ;h s;v   the low and high calibration standard mix
           ;-  >r ..        ' .;;  '^concentrations respectively.  Laboratories
      ,-;,;,    "-!:  .4 •;.,           -'sjiall prepare the SPE recovery  check
   ,;,              "   •'..,         standards in methanol and add 1 mL of each
  ,;,, -i                 <:'--:A       calibration solution to 100 mL  of  reagent
^•'                   7!       water.  If the Laboratory experiences
                       ig       solubility problems in preparing the SPE
                       ^•-      recovery check standard solution,  the
                       IS-       Laboratory shall prepare the SPE recovery
         ;-;          ;' j£       check standards in methanol, add 1 mL of
          -, 1  ,,    ^  i        each  calibration solution to 4  mL
            "-X -J-,... ';|f.          methanol, and add the resulting solution
               ''••[: ;•'"          to  100 mL of reagent water.  The recovery
                               check samples shall be prepared and
                             D-8-PEST-Q                           08/23/94

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                                                               DRAFT

                         analyzed according  to  the procedures in
                         Section IV.

             4.3.5.3.3   The SEE recovery  check standard solutions
                         shall be analyzed: i*1 a valid initial
                         calibration or ^1%, Calibration
                         analytical sequence (see  paragraph 18 . 1) .
                         Note: if the SFE  recovery ,%eheck standards
                         are the only samples analyze!) in the
                         analytical sequence , the  method 4>!Lank
                         shall be .Replaced with an instrument blank
                         and the -3LCS shall be prepared by diluting
                         100 jiL-of LCS stock -mixture  into 5 mL of
                         hexane and concentrating  to  ImL using
                         nitroge^|'b,lowdowi3.i;.  The EPA  identification
                         numbers f or ^standards  as  described in
                         Exhibit B shall -t»e  used for  the low and
                         high SPE recovery check standard solutions
                         (i.e., QPESTD####, arfiere  #### is  the
                      :   amount injected).   The IPA identification
                     ,i;  jdsBpSser^. =a^ described in Exhibit B shall be
                     *''•  -used fitSr $S$& 4i$s,trument  blank and LCS.
4.3.5.4      Technical Aceeftance <3iflteria
                                .! •* • "
             The recovery of ' tne'^iheck compounds spiked at the
             upper limit of tlie,;falibration range must demonstrate
             reoofsreirjr of 30-110 percent to establish  that the SPE
           ,  media iiabfethe capacity,, to retain compounds at the
         l"   upper en^qof the cal illation range (i.e., no
       j"y   breakthrough of target compounds is occurring).  The
      ,; "\     recovery^pc^eck at the low concentration  level shall be
      ''":.:,,/,,, evaluate^ ;^(| i^aifeStscate that the system performs at
          " ;l«w levels and does not introduce method
             intfead&erences .   If any compound recovery is less than
             30  peng&O£ or is  greater than 110 percent, then that
  ;,-:, ^   j    lot of "diiifcS, shall not be used.

 .''.3.5.5     tk«3cective Action
                '
            If  t^|  disks do not exhibit acceptable recovery of any
            spike|l  compound at the low or high concentration
            levels,,  the entire lot shall not be used to extract
            samp^ss,  since the system cannot be demonstrated to be
            functioning at those levels.
                '"'
4.3.5.6 ',
            All data  and related documentation for the SPE
            recovery  check analysis shall be maintained by the

                       D-9-PEST-Q                          08/23/94

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                                                                      DRAFT

                   Laboratory during the term of the contract and shall
                   be available  to the Agency during on-site laboratory
                   evaluations or if requested by the TPO or APO.

 4.3.6 Extract Cleanup  Cartridges - Florisil,  0»',5 g solid phase glass
       extraction cartridges  with stainless steel.or Teflon frits (Varian
       Florisil PR, or  equivalent).  Bake the;::jglass florisil cartridges
       at 140°C overnight  to  activate (do not exceed 150*C),

       4.3.6.1     Florisil Cartridge Performance Check       ?. ,

                   Each lot of Florisil-cartridges must be tested by the
                   following  procedures-tbefore it >|i,s used for sample
                   clean-up.   Mix O.S.fflL of 2,4,5*at:richlorophenol
                   solution (0.1 ^g/mLVitif,hexaneO • and 0.5 mL of the  mid
                   point calibration mixtai^e (taetal volume 1 mL) .  Place
                   the  mixture onto the top ~k>f §a prewashed Florisil
                   cartridge,  and elute it witti'9\;,so'iutici*|'f5hall be an$p|fzed in a valid initial
                s< '-;' calibratlferaa or daily Calibration analytical sequence
               f°   (see paraigriaph. 18.1).   liote: if the florisil cartridge
               : :   performaj^l; .qhecjjc ..standard is the only sample analyzed
                •   in the 4aiJa%rt^eai:,Sequence,  the method blank shall be
                 : replaced with an instrument blank and the LCS shall be
                   prepared by diluting 100 pL of LCS stock mixture  into
                   5 mL"-tJ^.,3be.xane and concentrating to ImL using nitrogen
        , ;••,,  ,  -  blowdowit-Jcl'^ite EPA identification numbers for
      .:>">,'     "" :v  ,s|;andards  as|%escribed in Exhibit B shall be used for
     ;  "            &&%?J-ow an^- high SPE recovery check standard solutions
   i\:'~             (i-^Vs,  QPESTDy/###,  where #### is the amount injected).
 „  iv-               Thelllk identification numbers as described in Exhibit
;/;'^                B shiiBL be used for this instrument blank and LCS.

                   Documentation

                   Al|tf.*lata and  related documentation for the florisil
                  , recovery check analysis shall be maintained by the
                 • wl^boratory during the term of the contract and shall
                   be available  to the Agency during on-site laboratory
                   evaluations or if requested by the TPO or APO.

                             D-10-PEST-Q                          08/23/94

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                                                                          DRAFT

4.4   Glassware  - Sufficient glassware to meet contract requirements shall be
      reserved for exclusive use in support of this contract.

      4.4.1       Erlenmeyer Flasks - 50 and 125 mL.

      4.4.2       Beaker  -  150 mL.

      4.4.3       Concentrator tubes - 10 mL.                 :

      4.4.4       Kimax concentrator tube (graduated) - 25 mL.    * '•
                                             " V' ,'                       -  ,
      4.4.5       Graduated test tubes - graduated from 1 to 10 mL,
                                            \            ''
      4.4.6       Autosampler vials - appropriate for the GC system.
                                            % •        '/'
      4.4.7       Centrifuge tubes  - 40 mL.    -    >;'-

      4.4.8       Powder  funnel  - 6 cm (60°).

      4.4.9       Pasteur Pipets.                            •'•'
                                  ••'<  I '' ' -.-'  •/....
      4.4.10      Side-arm  flask •?  50(f mL/'- ;;: ^  ;, .
                                     \-r           >    •-;••;
      4.4.11      Wide-mouth centrifuge tubes-^bptional).

      4.4.12      Buchner funnel.

4.5   Laboratory Hardware: --^Ehe  .following equipment is required for sample
      preparation.    r       '
      4.5.1       Ultrasonic  Celljillisrupter -  Heat Systems Ultrasonics,  Inc.
                  Model W-385 Soi)S$ator (475 watt with pulsing capability, No.
                  200&-/2" tapp^|J|is^^^fer;:;Sorn plus No.  419 1/8" standard
                  tape*«t;aaicrotip  probe),  or  equivalent device with a minimum
                  of 375 wat-|&:output capability.  The 1/8" microtip shall be
                  used for exlfc±afetion of all soil/solid samples.  (NOTE:  In
             „ - ;'  toxder to ensuislr'^at sufficient energy is transferred to the
               v' ^as^ie'jduring  the%«£traction,  the microtip probe must be
                  replac^lif the tip begins to erode.  Erosion of the tip is
                  evidence'Jl|3|iy a rough surface.)

     ^;/5.2       Balance - Calibrated and accurate to 0.1 g.
     '^-4,-                 .-:v
      4.>;;3 U     Balance - JiElalibrated and accurate to 0.1 mg.

      4.5.4    ''•  3 O|ntrifjige-.
                   -•':'- '   ^ "
      4.5.5       Vo rt&x -Mixer.

      4.5.6       Microsyringe - 10-^L,  50-^L,  and 100-^L.

                                  D-11-PEST-Q                          08/23/94

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                                                                           DRAFT

      4.5.7        Spatula -  Stainless steel.

      4.5.8        Hot  plate  stirrer.

      4.5.9        Teflon coated magnets.

      4.5.10       Glass  wool.

      4.5.11       Whatman #42  filter paper.                       -;

      4.5.12       Whatman vacuum holder.                                ',""

      4.5.13       Nitrogen blowdown apparatus.

      4.5.14       Required equipment for extract cleanup cartridges.

      4.5.15       Water  bath.                     \  '.

      4.5.16       pH paper or  meter.                    -;;

5     Reagents                   ,4,  '•',:',],•., _'" t .f

5.1   Reagent water -  Reagent  water fts defined-}*s wafeer-/jln which target
      compounds or potentially interfering confounds do not produce a signal
      greater than one-half  the response,, in /life corresponding RRT window of
      the initial  calibration  low concentration standards.  Reagent water
      shall be generated by  one of the following methods.
                          :;' ?*•*"&• $_.,          '"'•••
      5.1.1 Reagent wataer'Tnay""b^;generated b|f gassing tap water through  a
            carbon fi'Mer bed  coBflsBiining approximately 500 g  of activated
            carbon  .(Saigon Corp. JWiltrasorb- 3060, or equivalent).

                  ,' ••! ,           ~;l,|. '-!••»-_.,>»!»- •-,.,„  «
      5.1.2 Reagent water may be:8;gefltfirat;ed.:::asing a water purification system
            (Millipore'«©;p:£iLus with Organex Q cartridges , or equivalent) .
                         "   "
      5.1.3 Reagent water majrs,^e, prepared by boiling for 15 minutes  then
            bubbling ,cpntaminant%£pee inert gas through the water for one hour
            •Aiie "-liaiajfcfctaiing the'wate^r temperature at 90«C.   While  still hot,
         ,£  transfer  the-^Sje^assed water to a narrow-mouth screw- cap  bottle,
         " l\- seal with a  Te'fl©n-lined septum, and cap.
       v. : :'?                  \s^
5.2  
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                                                                          DRAFT

5.6   5:100 methanol/water  solution (methanol in water v/v) .

5.7   90:10 hexane/acetone  solution (90 percent hexane;;in acetone v/v).

5.8   50:50 hexane/acetone  solution (50 percent hexane in acetone v/v).

5 . 9   Powdered Anhydrous  Sodium sulf ate .

5.10  Corn oil.                                               '  , :,

6     Standards                                                         !:;

6.1   Stock Standard Solutions
      Stock solutions may be prepared frowflBtire  standard materials or
      purchased as certified solutions .   Standard .so-Sutions  shall be prepared
      by dissolving pure standards  in a  suitable solvent in  volumetric flasks.
      The addition of toluene may be  necessary to distsolye some of the target
      compounds in highly concentrated stock  standards i ;';>s-l3hen compound purity
      is assayed to be 96 percenter  greater,  the weight majr "be used without
      correction to calculate the ^tts^teratipn  of  the stock standard.
      Exhibit E, Section V provides ,furth'er-^ir^Jfei             :
                      •  * '    ''M 'i,            '"',.
      6.2.2 Secondar^s&Ilution standards  shal't" Ibe stored at  4«C (± 2°C) with
            minimaibtteadspace and Checked frequently for signs of degradation
            or evaporation.  This is = especially  important just prior to
            preparing eal ibrat ion ;Staadards:" :f rom them .
            NOTE: Standards iShould not be stored in volumetric  flasks,
            especially when fhey ..are prepared with solvents with low boiling
                                '  '
                      ,  .
6.3   Calibration Standariis

      6l3.1 Calibration stafjftard mixtures shall be prepared at  three
     |r -/    concentration le^CLs in volumetric flasks and diluted to final
     1
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                                                                    DRAFT

6.3.2 During the initial calibration, each single  component pesticide
      must be analyzed at three different concentrations in order to
      establish calibration factors for each compotmd and to demonstrate
      detector linearity.

6.3.3 The calibration standard mixture solutions must be prepared in
      either hexane or isooctane at the concentratrixras listed below.
      The mid point concentration for all target compotip&s must be at
      least five times the low point concentration for each -isarget
      compound and the SMC.  The high concentration standard iSsust be at
      least 25 times the low point concentration for each target ; ?,
      compound and the SMC.  The high point concentration defines the
      upper end of the concentration j-xsnge for whifeh the calibration is
      valid.  It is suggested that ^concentration- 100 times the CRQL be
      used as a high point calibrati^oi fpxovidedj trhat the concentration
      is within the linear range of the -sletsectoa: .

6.3.4 Low concentration standard mixtures for single component
      pesticides                                 -'
                                      ; point
                           ::, Y  CoricewtfritjUm
            Compound         : ••       (ng/mI0    '  '-' •
            alpha- BHC                 10 ,,0
            beta-BHC                  10J9
            gamma -BHC  (Lindane)    ,   1.4.0
            delta-BHC                 10.0
            Heptachlor;  -             10,0
            Aldrii*, '"     ',, :           iCjO
            Heptaehlor epoxltde        10:©;
            gaama - Chlor dane^           10.0'
                       I  ,'fl'{;>r ..... _ ,„ 10.0
                                    '-M. 0
                                      io.o
            Endrin  •>:'.-:               10.0
            Endosulf an "II ;            10.0
                                      10.0
                   -aldehyde  • -t ;      10.0
            Endosul^a sulfate        10.0
            p,p'-DDT^:L              10.0
            Endrin ket:*^             10.0
            Methoxychldi;             10.0
            DecachloroKIfhenyl  (SMC)  10.0
                      t% \
                      '' g -'
                coelut^s with dieldrin.  The sum of both compounds will
               measuiet!  and will be  quantitated using the calibration
                      DDE.
 6.3.5      All standards shall be stored  at 4«C  (± 2«C)  in Teflon-
            sealed glass bottles .  Calibration solutions  shall be

                            D-14-PEST-Q                          08/23/94

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                                                                           DRAFT

                   replaced after 6 months, or sooner,  if comparison with check
                   standards indicate a problem.

6.4   Calibration Check Standards                     .:

      The calibration check is a daily one-point chedc^of the initial
      calibration.   The calibration check standard .shall%e'rprepared in a
      volumetric  flask and diluted to final volume with  hexanei;or isooctane.
      The concentration of the calibration check standard is  thess-ame as the
      mid level standard used in the initial calibration.         "'

6.5   System Monitor Compound

      The System  Monitor Compound (SMC) ts4^e.cachloro'bt|lhenyl.   A stock
      solution in acetone shall be prepared*a^,.described in paragraph 6.1,  and
      a SMC spiking solution at a concentration of S'gQ /jg/mL  in  acetone shall
      be prepared from the stock.   Each sample shall-lbe  spiked with  the SMC
      before analysis.   The Laboratory shall add 10 "'/tL'Mȣ this standard to  a
      100 mL water sample, or 10 ^L to 6 g of soil/solia,-^ ;Eor oil analysis,
      prepare decachlorobiphenyl 4t.--a, concentration of 0.5 $g/mL and add 1.0
      mL of this  solution to 1 g-gficii^fs^>.3ie:;s(see Section IV.)  The SMC will
      be employed to detect shifts in retent'ltait giste qtf fluting  target
      compounds.  Additionally, the 'SfclC shall h£-srseSl4t»Atonitor  the  extraction
      efficiency.                     ;'        •
                                      * ~ *    ~'J "'
      Note: Reagent grade acetone shall ;be tised to prepare the SMC stock and
      working solutions.   The Laboratory'sKall ensure that the acetone used to
      prepare the SMC stock aitd .working solutions is free  of  any
      contamination.    ;'::r     ' l,,l'-
                     i           ^ ; ,             '•'
6.6   Performance Verification Standard

      The Performance |?fe|:ificat^orf;;Sta»Eiiia,Bd^(PVS) shall be analyzed  at least
      once during each^'fealLytical sequence to assess system stability.   The
      PVS is two  times  (2x} =fee concentration of the low  level calibration
      standard.               - ,  • <

6.7   Laboratsory  'Cb'htrDol  Sample    -"^j-!,
        ,- •'•• -/'*             x>x'-."ii'i
      La&jratory  Control  Sa«|ies  (LCS)  containing known amounts  of target
         pounds traceable tor^farimary standards  will initially be  supplied by
          Agency.   Following |tseceipt of these initial supplies, however,  the
           itory  shall prepare; its  own  LCS standards.  The LCS shall be spiked
      in€bl||»lean  matrix aiajUprepared  using all steps of  this protocol.  An
      appropr-liifce,ramount  of'^faie  LCS shall  be added to reagent water  and
      analyzed'wiJi&^each  Bafsch of water samples.   An appropriate  amount of  the
      LCS shall be i^B^U^> clean quartz sand and analyzed with  each Batch  of
      soil/solid  sampMisi"' An appropriate  amount of the LCS shall be added  to
      clean corn  oil  and  analyzed with  each Batch of oil samples.  If a Batch
      contains water, soil/solid, and oil  samples,  an LCS  shall be prepared

                                  D-15-PEST-Q                           08/23/94

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                                                                         DRAFT

      and analyzed for each matrix.  Note: If wipe sample analyses are
      performed, the Agency will provide the Laboratory with further
      instructions for the preparation and analysis of LCSs for wipe samples.
      All LCS compounds must have recoveries between 30 and 130 percent before
      sample analysis may begin (see paragraph 27).

      NOTE:  The Laboratory is expected to maintain- control charts of the
      recoveries of at least three representative LCS compounds as an internal
      QC procedure.

6.8   Florisil Cartridge Check Standard       ;,                         :

      The Florisil cartridge check standard'-is 2,4,5 - triehlorophenol.  A stock
      solution of this should be prepared Jtn a volumet£l.c flask and diluted to
      volume with hexane to obtain a 0.1 pgfaiL concentration.

6.9   Storage of Standard Solutions               :

      6.9.1 Stock, secondary standard solutions and worTcfisg standard solutions
            shall be stored at 4°:S,,:.|fet«ji!0C) in Teflon-lined screw-cap amber
            bottles (also see
      6.9.2 All standards shall be fratected fafoiB light.

      6.9.3 Samples, sample extracts, and standards shall be stored
            separately.                 „   v.f
                                  D-16-PEST-Q                         08/23/94

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                                                                           DRAFT
                                   SECTION III

             INSTRUMENT QUALITY CONTROL PROCEDURES AND REQUIREMENTS
      Instrument Operating Conditions             , -

      The following are the suggested gas chromatographic analytical
      conditions.                                                 ?.

      Column:      DB-5 (or equivalent), 15 m,*r0.53 mm ID megabore capillary
                   column.
      Carrier  Gas:
      Flow Rate:
      Injector Temperature:
      Detector Temperature:
      Makeup Gas:
      Makeup Flow:
      Initial  Temperature:
      Initial  Hold  Time:
      Ramp Rate:
      Final Temperature:
      Final Hold Time:
                                         Helium
                                         ;5.5
                                         •ISO -f2©0*
                                         30CHC  ,
                                         P-5
                                         60 mL/min
                                         150«C
                                       • ,,0.5 min
                                        JfT5«C
                                        *•& min
      * Cold  (ambient)  on-column injectors, irfeat allow injection directly  into
      0.53 mm ID column may be used for this method as long as peaks are
      gaussian, retention Jtfisies-are stable;; and calibration criteria are  met.

      NOTE: The typical run time'-lkinder these conditions is 20 minutes.  It may
      be necessary  cb ^adjust GC csoaditions on individual instruments to
      optimize compe&nd separati^^ _ It ,may also be necessary to adjust
      detector condltieais to opllig^^itaiita^asient sensitivity.
8     Calibration of the  6CiL-.lystem -  Initial Calibration
                             '4

8.1   Summary &•>''•<•• • -         " ' ''-- •
              ''     "              '
    ;
8 . Lat
                          ,            .
            ifrior to the'^^|^,lysis  of samples and required blanks, each GC
            system must be^ltiiitially calibrated to ensure that the instrument
            meets the minimu|»9|)erformance requirements of the method.  The
            initial calibratil^i is accomplished by analyzing three standards :
            the low level, mj|| level, and high level mixtures as specified in
                      6. 3. 4 c;1 -'The  technical acceptance criteria for the
                    calibration are given in paragraph 8.5.   The initial
                        shjkli  be used to establish the calibration factors
            used f6i£:cDi|pDfind  quantitation,  to define the retention time
            windows fc«j|asompound identification,  and to determine the mean SMC
            retention time for evaluating SMC retention time shift (RTS)
            during analyses.   Detector  response must be linear for all target
                                  D-17-PEST-Q
                                                                 08/23/94

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                                                                          DRAFT

            compounds.  All samples shall be analyzed during  the  contract
            specified 24-hour analytical sequence.

      8.1.2 Sample quantitation shall be based on the mean  compound
            calibration factor, line segments ("K" curve),  or the mid level
            calibration factor from the initial calibration.   (The use of the
            line segment or "K" curve is suggested);.  All field and QC samples
            and standards within the same Batch and all  field .and QC samples
            and standards analyzed during the same analytical segitence shall
            be quantitated using the same method of quantitation."''
                                             V;                         .*-
      8.1.3 Compound identification shall be Abased on RRT windows established
            during initial calibration in all field samples where the SMC
            recovery is greater than or ecpial to 10 pe%eent and less than or
            equal to 200 percent.           :<=',         ;
                                               • ' '• :
      8.1.4 Compound identification shall be based on absolute  retention time
            windows established during initial calibration  in all field
            samples where the SMC recovery is less than?10,-percent,  greater
            than 200 percent, or if^peak interferences are  f«?esent.
      8.1.5 Shifts in the chromatogj^aphic" pBakSisShall be  evaluated by
            comparing the retentioriflbime (RT) jap•th'e%MC  in all  analyses with
            the mean RT of the SMC calculated? ,2£rom the  initial calibration.
            The retention time shift ig'Vrefetdied to as  RTS  or RT %D (see
            paragraph 21.4.1).  The RT of J$&e= SMC for field and  QC sample
            analyses must be within ± 1.0 Jpfercent of the  mean RT calculated
            from the initial sso&libration.  :  ,
8.2   Frequency
      8.2.1 An initial three -poiiSg 'calibration shall be performed to determine
            the linearJlsy of re«p^is4ldli?iW.V-'target compounds  and the SMC.  A
            new initial'";balibration is required whenever  a  calibration check
            standard or P7Sy|saqnot satisfy QC criteria.   A  new initial
            calibration is als3|ation muitMb performed for each  GC  and for each
         „ • -'^hromatographdisjiscolumn which are used to perform these analyses.
           '               ^ ''
         i2 An analytical salience is a contractually-defined sequence of GC
     i?-<*    analyses which cejijlsists of an initial three -point calibration or
     ;^ ~^K • /valid calibratiottitsheck, field samples, LCS, method and instrument
         ^ «|; iK|anks ,  PVS, and|lpther QC samples run within a 24-hour period (see
            piassagraph 18 forjShe required sequence of  samples).
              ' "^ ^-     v"
      8.2.3 Analysis |^»^lfe|t  initial calibration shall  begin with the injection
            of the high iWel standard followed by the mid level and low level
            standards .
                                  D-18-PEST-Q                          08/23/94

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                                                                          DRAFT

      8.2.4 The analytical  sequence shall be concluded with an acceptable
            analysis of  an  instrument blank and a PVS standard (see paragraph
            10).

      8.2.5 Samples shall be analyzed only after meeting the technical
            acceptance criteria  for the  initial calibration or calibration
            check standard.

8.3   Procedure

      8.3.1 The GC system shall  be  set up per"'tfhe requirements of paragraph 7.

      8.3.2 Prepare calibration  standard solutions containing the SMC and all
            target compounds using  the procedure listed in paragraph 6.3.

      8.3.3 The calibration solutions shall bes^fui^brated to ambient
            temperature  before injection (approximately one hour).

      8.3.4 Inject between  1 and 5  pL of each calibration standard.   The same
            injection volume shall be used for all calibrations and field/QC
            sample analyses.     j,  '• v, \" = ;::'-;,:-,,

8.4   Calculations                   ! ,           :

      8.4.1 Calculate the calibration ^factor* (ratio of the total peak area or
            height to the mass injected>;,;for; each target compound and the SMC
            in the initial  calibration standard analyses using equation D.I
            (EQ. D.I).   . "'•::.-. .          .-;=
                        Factoi               f Peak °* Peak
                                  '
                                              .
                                             injected (ng)
      8.4.2 Ca|j*5t^ats&--the mean 'calpfaration  factor  for  each  target compound and
               *         '          '"
      8 .^ji;3 Calculate the UliSD of the calibration factors  of  the  low level,
       •;:fj    mid level, and fiSjgh level standards  for  the  initial calibration
     pr:,,:    using the following equation.


              '-<••'^~          ::l:  %RSD = -IP x 100                 EQ.  D.2
              --.. ,„,,         ^ ,,, •          x
            where SD = standard deviation.
                                  D-19-PEST-Q                          08/23/94

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                                                                           DRAFT

            Standard deviation is calculated using the following equation:
                                                                   " D'3
            where:  x^ =  individual calibration factor (per compound).

                    x  =  mean of three initial^calibration factors (peri;
                          compound) .          ,";

                    N  -  number of  calibration standards.

            Equation D.4  is  the general formula; jBorttfce mean of a set of
            values.                               "   :
                                                                  -  D-4
            where:  X  = mean of values,

                    X^ = value.

                    N  = «nifflfoer of values.

      8. A. 4 Calculate||it:he RRT for'ieach target"';compound using the following
            equation!?:
                                                                 EQ.  D.5
      8.4.5 Caleulgite  the mean RET and RT for each target compound by using
8.5   Te4Wical Acceptance ij|S.teria
        :;5.1 The ZRSD of  the  calibration factor for each target compound and
        4|:;, the SMC in the ijilkial calibration must be less than or equal  to
         ^-,i|^5<,0 percent, ex&ejpt for DDT,  endrin,  and methoxychlor which must
                   s than ortleiqual to 30.0 percent.
      8.5.2 The re6eM:ioa!^time of the SMC in the standards must be within ±
            1.0 perceiftt 
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                                                                           DRAFT

      8.5.3 The  peak resolution between endosulfan I and  a-chlorodane shall be
            evaluated in the low level initial calibration standard before
            proceeding with sample analyses (see paragraph 11).

      8.5.4 Endrin/DDT breakdown.  There is no specific calculation for endrin
            or DDT breakdown required for this method '.Breakdown will occur
            as the injector becomes contaminated; in such & -case, the percent
            recovery will change in the PVS standard when they -are  analyzed.
                                                                 - cv;  •
      8.5.5 The  chromatographic peak response,-for all target composoHis(in the
            low  concentration standard must be greater than 10  percen!f::ef
            full-scale  deflection.           ;
                                            '*t
8.6   Corrective Action                 , j; ,
                                         '••-•''•         sl.

      8.6.1 If the %RSD for any compound in trie Jsoitaial calibration is greater
            than 25.0 percent,  except for DDT, etidrln,,  and methoxychlor which
            may  be up to 30.0 percent,  the instrument? has not demonstrated
            adequate linearity to be used for this methbcL ;  Corrective action
            shall be taken and documented..
                                 >f ;2i» -i'  ?i., - ,,
                                 •£>•" - •.••   ' * L. ' ^  S  ' •. ~\ * •:-.
      8.6.2 If the peak resolutiottj«|pritertbti'>safe,i^ofe'-i^t,,, the Laboratory shall
            perform corrective action, and demqnstrat* «flfequate  resolution
            before samples can be analyzed.   :v

      8.6.3 If the SMC  RT is  not within .£ 1*0 percent of the mean SMC
            retention time calculated freaClthe three initial calibration
            standards,  the: Laboratory shalt-perform corrective  action  which
                          •>••' •• •>?:••;  ,     •*     < < >* •
            may  include^ new^iaxftial calibration.   DO NOT proceed with sample
            analysis^iimtil the  KtS;  is within % 1.0 percent.
                   •:, V
      8.6.4 If thes!,f«ak responsenjlor any.,..target  compound in the low
            concentmt&wn stani^i|;j4S;i^i3$,.*g;'?eater tnan 1° percent of full-
            scale deflection,  the Laboratory  shall perform corrective  action
            and make apprcifirlsate adjustments before sample analyses are
            started, to  ensufee ;tifaat  all  target compound peak responses in the
            low jcaoacfwatration stipiard are greater than 10 percent of  full-
                '                  "''  "
            Corrective ac€ig|pt may  include  optimizing detector linearity by
        v   cleaning the ECE|Metector using high temperature (350«C) overnight
        •    or by hydrogen fibciw for  two hours  to reduce breakdown.  Actions
        |f ^ also may includeifjfeplacing the GC  injector liner, column, or the
           |pi;e-column, rem^tng 0.5 - 1 m of  the analytical column, or
             " "facing the siphdards.
      8.6.6 All initial.j^l'ibration technical  acceptance criteria shall be met
            before anyiaf^nples or required blanks  are analyzed.   Any samples
            or required blanks analyzed when the initial calibration criteria
                                  D-21-PEST-Q                          08/23/94

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                                                                          DRAFT

            have not been met shall require reanalysis  at no additional cost
            to the Agency.

8.7   Documentation

      Initial calibration results are reported on  Eexoas -IpVA-PEST,  QIVB-PEST,
      and QV1-PEST.  Reporting requirements are  listed  in Esdiibit B.

9     Calibration of the GC System - Calibration Check

9.1   Summary                                -i/.                       ;  ,,

      A check of the initial calibration crtrve shall be performed at the
      beginning of every 24-hour analytical:;,sequence tt&pt includes field
      sample analyses.  This check of the iatitial  calibration shall be
      performed using the mid level standard sa^t".ash-all  contain all target
      compounds and the SMC.  The percent difference (%D) between the
      calibration factor in the calibration check  standard and the average
      calibration factor from the initial calibration istfcalculated for each
      target compound and the SMC; and must meet the technical acceptance
      criteria given in paragrapW^JS^|f.';^lsfe,rS|lC,,R.TS and column resolution must
      also meet technical acceptance criterife3;^s;»::sCated::in paragraph 9.5 and
      paragraph 11, respectively.  %ily after £JJL  tnese Criteria are met can
      sample analysis begin.         •;       >•*':/
                                            ,' f
      NOTE:   Compound identification and:; xjU^Bfcitation shall be performed based
      on calibration factors and compound S3? and RRT windows established
      during the initial calilt£ation.     ^ ;
                     .!>'  '   ' '^4\.-         %:
9.2   Frequency      ;;,;'.;         * •%          *:&
                                 '••f>
      9.2.1 Each G
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                                                                          DRAFT

9.3   Procedure

      9.3.1 The  GC  system shall be set up per the requirements of paragraph 7.
                                                       \
      9.3.2 Prepare the calibration check standard solution containing the SMC
            and  all target compounds using the procedure disced in paragraph
            6.4.                                   ..     " ,' r;!

      9.3.3 The  calibration check standard solution shall be eqiitldLbrated to
            ambient temperature before injection (approximately om;!h«xur).

      9.3.4 Inject  between 1 and 5 fiL of the Aid level calibration standard.
            The  same injection volume shall?be used for,,all calibrations and
            field/QC sample analyses.     - }          . 'r
                                             $ *       •< •,
9.4   Calculations                            "  ,     e.

      9.4.1 Calculate the calibration factor (ratio «f,the total peak area or
            peak height to the mass injected) for each'ta^get compound and the
            SMC  in  the calibratioi^j.check standard mixture %sing the following
            equation.           ¥-;fl>| - ¥ ,.'«•/ ^ „
             Calibration Factor =  Total,Area ol&eak or Peak Height        EQ.  D.6
                                             , injected (ng)
      9.4.2 Calculate ,t4»B  %D~»e|fc»een the calibration factors from the
            calibratjfibn checks  anxi the  mean calibration factors from the
            initial,*ffiaiibration vising the following equation.
                                                                 EQ.  D.7
                              >f  three  initial calibration factors (per
                        compound).

                  xc =  calibration factor  from current calibration check (per
9.5   Technical' 4*»ej>tancef
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                                                                          DRAFT

            ± 35.0 percent, except for DDT,  endrin,  and methoxychlor which
            must be within ±40.0 percent.

      9.5.2 All target compound absolute  and relative detention times must be
            within the windows established  during thel-initial calibration.
            Report calibration check RT and RRT data -aeBuForm QI-PEST (see
            Exhibit B).                                    :
      9.5.3 The retention time of the  SMC  in the calibration cheefes must be
            within ±1.0 percent of the mean SBC retention time caibeaLated
            from the initial calibration sta^t^ards  (mean RT of all the'/iinitial
            calibration standards).         >-V
                                          /•^"         .:•-
      9.5.4 The peak resolution between e»Sbsulfan  I aa*d a-chlordane shall be
            evaluated before proceeding wlt&S&le analyses (see paragraph
            11).                             "' !/. :  '•;

      9.5.5 Endrin/DDT breakdown.  There is no specific .calculation for endrin
            or DDT breakdown required  for  this method.™1 tfee.akdown will occur
            as the injector becomes contaminated; in such a case, the
            calibration factor p^cc^s*:JSff«,i:fi.nce will exceed the limits for a
            valid calibration che'fck,   "--=,<;.-•--;-,

9 . 6   Corrective Action
                                     ' . i      - A*
                                      * +*,•.*:     ^ S
      9.6.1 If the %D for any target c.vts$*xfe& or the SMC is not within ±35.0
            percent, except for DDT, endrifil and methoxychlor which must be
            within ± 40.0 ,|>ere«nt, reanalyze the calibration check.  If upon
            reanalysisv,*ay comp^sad is still ;,4utside the criterion, a new
            initial calibration sisal 1  be performed  before samples can be
            analyzed. ; The instrument  must be recalibrated as described in
                      8.        . -.•• ~™,-.
                       .        ,           ,
      9.6.2 If the RT W>lB£T for any compound is not within the RT and RRT
            windows established during the  initial calibration, reanalyze the
            calibration checfcjgifeandard.   If upon reanalysis a compound is
                          the witoidbsr,,, a new initial calibration must be
                             sampie^gban be analyzed.   The instrument must be
           .,recalibrated
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                                                                           DRAFT

      9.6.4  If the  peak resolution criterion is not met, the Laboratory  shall
             perform corrective action and demonstrate adequate resolution
             before  samples can be analyzed.

      9.6.5  All calibration check technical acceptance criteria shall be  met
             before  any samples or required blanks are analyzed.  Any samples
             or required blanks analyzed when the calibration .check criteria
             have not been met shall require reanalysis at no additional cost
             to the  Agency.                                       -.

9.7   Documentation                         -,'*'

      Calibration check results are reported on Forms QI-.PEST, QV-PEST, and
      QVI-PEST.  Reporting requirements axe, listed in>Ixhibit B.

10    Calibration of the GC System - Performance•Verification Standard (PVS)

10.1  Summary                                        J  :

      A performance verification standard shall be analyzed at the end of
      every  24-hour analytical s«gEee^ct^ ,:P&e,.analysis of the PVS mixture
      shall be  started within 24 't&eurs "af€&i?3tlte. ta^Jpction of the first
      initial  calibration standard 4ar the instrument bC-siak analyzed before a
      valid  calibration check.   The "F¥S is twso^jtimes the concentration of the
      low level  standard from the initial calibration (see paragraph 6.3.4).

10.2  Frequency                             ;'

      An acceptable PVS ;amist be>i|salyzed at: £be conclusion of the analytical
      sequence.  Thejpys mixture'fsfhall be stained within 24 hours after the
      injection  of  ]&&k first initMl calibration standard or the instrument
      blank analyzed .before a vail&i ..calibration check.   If a successful PVS
      analysis  is nd^^tained^fl^^^^B^as'ion of the analytical sequence,
      all samples analyze*!.since the last successful PVS,  initial calibration,
      or valid calibration^Sflieck shall be reinjected and reanalyzed in a valid
      analytical sequence at*^;= additional expense to the Agency.   The
      Laboratory,-J^i-encouraged "t^Jicsn, additional PVS analyses during an
      analytical"se%reaK!*p-,to minimi^:^unpaid reanalyses.   If acceptable PVSs
      are >asaalyzed  durirtg|;a» analytical sequence,  the Laboratory may continue
      to,-9ibllect data  undet||tlie current calibration until the conclusion of
      tie current 24-hour science.   If at any  time an unsuccessful PVS
     j$e&alysis is made,  the ^&>oratory shall  stop  sample analysis and
     '•iilpfcdiately reanalyze .iffee PVS.   Up to two injections of the PVS mixture
      maySS>e|3ised to satisfyfjche criteria.   If  on  reanalysis the PVS is still
      outsioieV^C ;criteria,,;tlMJ  Laboratory shall take corrective action and
      recalibrate! jllChe  GC |eun a new initial calibration)  prior to reinitiating
      sample analyst^ ^ J&efcalibration will begin a new analytical sequence.
                                  D-25-PEST-Q                          08/23/94

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                                                                          DRAFT

10.3  Procedure

      10.3.1      The FVS solution is  two  times the concentration of the low
                  level standard mixture from the initial calibration  (see
                  paragraph 6.3.4).                   \\

      10.3.2      Analyze the PVS  solution by using^the same GC conditions  to
                  be used for the  field and QC samples and blanks .

      10.3.3      The same injection volume shall be used for allfeeld and QC
                  samples and standards including the PVS solution. ""<  '--,,-

      10.3.4      The recovery of  each compound and the SMC in the PVS are
                  quantitated using the mean calibration factor, the mid
                  point, or by using a K carve, established during the  initial
                  calibration. (NOTE:   Only orae aet^iod of quantitation shall
                  be used for analyses within a given analytical sequence and
                  for a given Batch of samples) .

10.4  Calculations
                                  ' '<;•
                                 .''"•" ~*l ""'-1,-;-  ,'
      The amount of PVS compounds^aiad  ttie 'Sli£Cii|e
      where:      A^ ,   =     are%ror peak heiglit of the PVS compound or SMC.

                                          -factor established by one of three
                          ,,j
                              techniques  during the initial calibration.
                        Recover' A°otmt ?f ff1^ (n& X 100         EQ. D. 9
                       t>         ' -,,f  ^Amount Added (ng)
10.5  T^fchnical Acceptance Criteria
                  All PVS target  compounds  must have a calculated recovery  of
                  75-125 peifg^nt  in  order to  report data without flags.
      10.5.2   "=1 -|f recovei^  of  a PVS  compound is not within 75-125 percent
                  b$ttf«;t:jtlfS: within an expanded recovery window of 50-150
                  per&esft, the associated sample analyses results shall be
                  flagged  (see paragraph 10.6).
                                  D-26-PEST-Q                          08/23/94

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                                                                          DRAFT

      10.5.3      The  SMC  recovery criterion of 50-150 percent is advisory
                  only.  Reanalysis of the PVS is not performed if the SMC
                  recovery is  outside the advisory recovery limits.  The SMC
                  recovery in  the PVS mixture must, however, be greater than
                  or equal to  20 percent and less than ,or equal to 200 percent
                  (see paragraph 10.6).            , ::  : --;/
                                                            ~?
      10.5.4      All  target compound absolute and relative -retention times
                  must be  within the windows established during -t%e initial
                  calibration.   Report PVS RT,,aod RRT data on Form $1>EEST
                  (see Exhibit B).

      10.5.5      The  SMC  RT in the PVS mu^tfbe within,j. -1.0 percent of the
                  SMC  mean RT  calculated sirom the initial calibration.
      10.5.6      The peak resolution between .;c|>JXtaminated; in such a
                  case , the percent Srecovery w^3,l exeefed the limits for a
                  valid PVS.        ;   -      - f
                                       'if     . - - • •
10.6  Corrective Action

      10.6.1      If recov-epgf i&f a compound^ is  not within 75-125 percent but
                  stiljt^sflthin -a&expanded rustSpvery window of 50-150 percent,
                  fl
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                                                                    DRAFT

10.6.4      If the SMC RTS criterion is not met for a PVS, sample
            analyses shall be stopped and the PVS immediately
            reanalyzed.  If the RTS  is still outside the criterion upon
            reanalysis, corrective action shall Ibe performed which may
            include a new initial calibration. ,330. NOT continue with
            sample analyses until the RTS is wi€hS.n ± 1.0 percent.
            Reanalyze all samples that were,r*in between, the noncompliant
            PVS and the last valid PVS,  initial calibration, or valid
            calibration check standard before proceeding Vi^b,;,sample
            analyses.                    ;                    :,  .

10.6.5      If a PVS SMC recovery is ^ess than 20 percent, greater than
            200 percent, or if peak  iailerferences :«re present, stop
            sample analyses, perform ^corrective action, and immediately
            reanalyze the PVS.  If tnefSHC is sljill out on reanalysis,
            perform corrective action an&-ls*ar't:': a new analytical
            sequence.  All samples analyzed isince the last valid PVS,
            initial calibration, or  valid calibration check shall be
            reanalyzed within a valid analytical 'sequence.
                            "•• ^ * s" •• -
10.6.6      If the peak re$gEj|iut3ii^ief^t%££on is not met, the Laboratory
            shall perform cdrr«ctive"actJlie met after having taken
            corrective action, rearSEpge (do not re-extract) the
            assoc^ted^ijeld samples :^i, another valid analytical
            sequ«tfee.  IftoQji reanalysesjilall QC sample criteria are met
            ancfefiie PVS criteria still casKJnot be met, then submit all
            saaple data frcm^i>oth sequences.   The Laboratory shall
            ,Js«cribe in th^f|^ajfccb,,,j|!arxa3tive the problems associated with
            the :EVS and b^tiMs-x£^^Ms$ample matrix may have affected
            the P^ISHaaalyses.  If the Laboratory can demonstrate that
                   c,' •-, ;!L ,
            the problbeiis>^re due to  matrix effects, then both sequences
            are billabi'&/, .•••},
            Tf1 a1^S,,reanalysis;jm.s  required because of a non-compliant
                        analysis, the  PVS reanalysis must be started
            within 26ljii|>urs after the  start of the current analytical
            sequence.

            Because reanalysis, at  no  additional cost to the Agency, is
            required ilfe.il'VS technical  acceptance criteria are not met,
           ,,jnore freqii^it analysis  of  the PVS is recommended, especially
            when highly contaminated or complex samples are analyzed.
                            D-28-PEST-Q                          08/23/94

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                                                                          DRAFT
10.7  Documentation
11
      Results of PVS analyses  are reported on Forms QI-fEST, QIII-PEST, and
      QVI-PEST.  Reporting requirements are listed in Isihibit B.

      System Performance  -  GC  Resolution            ,  '.',  •
11.1  Summary
      Peak resolution between endosulfan I and.»-chlordane shall be measured
      to establish that  there is  sufficient dltsbmatographic resolution -for
      accurate compound  identification and gsantitations .   When minimum peak
      resolution cannot  be met, identifica^feSn and quantisation is adversely
      affected due to the difficulty in establishing t:h& baseline.
11.2  Frequency
      11.2.1
      11.2.2
      11 . 2 . 3
                  Initial calibration -  The peak resojsefcion between endosulfan
                  I and a-chlordane  in the low initial calibration standard
                  shall be  evaluated, .before proceeding with sample analyses.
                  Calibration  checi^standarS-^fee^eak resolution between
                  endosulfan I and %Vtehlordane^to the- «a3L'ibration check
                  standard  shall be  esaluated'&efore proceeding with sample
                  analyses.           *>"»•   »-'f"

                  Performance  verifications-standard - The peak resolution
                  between end.bsulf an I  and a-chlordane shall be evaluated for
                  each 1WS  that\||s analyzed iafb a valid analytical sequence .
11.3  Calculations

      Determine
      pairs using the
                                               percent valley between peak
                                equation  (see  figure 1).
             &&&&aal&Vie&iLey
                                    :t of the valley between
                                          I and a-chlordane
                                             of smaller
                                   peak being zesolved
                                                           „ inn
                                                           X 10U
                                                                    - D.10
       •-                      f.
11.4 -IpBchnical Acceptance Cf^teria
      11.4c»:.  '-,    Initial calibration  - The percent  valley must be less than
           •• ''"%'$&* f-f             •£, '              r             ^
            "X; .fi,, or equal .»tt»-" 7 5 percent between endosulfan I and a-chlordane
              " •, fy-f f. '•.     *   f S- ••-.-*-    *
                -" ,i»' the analysis of the low standard of the initial
                  calibration.
                                  D-29-PEST-Q
                                                                       08/23/94

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                                                                           DRAFT

      11.4.2      Calibration check standard - The percent valley must be less
                  than or equal to 75 percent between endosulfan I and a-
                  chlordane in the analysis of the calibration check standard.

      11.4.3      Performance verification standard - Hie percent valley  must
                  be  less than or equal to 75 percent" between endosulfan  I and
                  a-chlordane in the analysis of the PVS. ,

11.5  Corrective Action                                         '•", '•!.

      11.5.1      If  the  peak resolution for dike two compounds indicated;  in
                  paragraph 11.1 exceeds thel!75 percent valley criterion  in
                  the low level standard aiialyzed during-".t:he initial
                  calibration,  corrective Jafetion shallf-'be taken, and a new
                  initial calibration shall- "&e sperf oraed and documented before
                  proceeding with sample analyses. -

      11.5.2      If  the  peak resolution for the two ferappounds indicated  in
                  paragraph 11.1 exceeds the 75 percent"Va%ley criterion  in
                  the calibration/»?efeeck standard, corrective;Jaction shall be
                  performed.   A ^^lill|5a3|bp^|||>ii check must be demonstrated or
                  a new initial ca|^ratiW'';ifea3tt^|beiai>frfJormed and documented
                  before  proceeding fsplth sample ^analyses,, "
                                     *
      11.5.3      If the  percent valle^f or ,;tfee PVS does not meet the
                  technical  acceptance  c^ri-tleria indicated in paragraph 11.4,
                  the PVS shall be immedimtij&ly reanalyzed.  If after
                  reanalysisrAfe-FVS  percenftjresolution is still outside
                  criterion,  cora^sctive acti%npshall be performed and a valid
                  calibration ch&& standard »ia or new initial calibration
                  peSEormed.  Reani^yze  all samples run after the last valid
                  JP?^  initial ceO^&i^ti^^.or: valid calibration check
                  standard befo^eJljr^eeeSi.iig'with sample analyses.
      11.5.4      A high ^er&mt  valley could indicate injector contamination
                  or column de^i^ation;  therefore, injection port and/or
             .   .-"jsbJtwoi mainten^HEK^.^inay be required.  Maintenance may include
           ., ji " '  rep!aeepaent  of  tn^l>$lhj ector liner and/or removing 0.5  - ID
         /4,"     of the'^^Lumn.   If these measures do not work, column
        *$'.}'       replacemele^j should be considered.
        •^s-                  ' .''"''•
      _,-,-„>                    y'-.'-
11 . 6 'ID&eumentation          t-*: ;
      Pefc4^,wCesolution resets  are  reported on Forms QIII-PEST, QIVA-PEST,
      and QV^S^L  Reporti^s requirements are listed in Exhibit B.
                                  D-30-PEST-Q                          08/23/94

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                                                                          DRAFT
                                   SECTION IV

         SAMPLE ANALYSIS AND COMPOUND IDENTIFICATION A8B QUANTITATION
12    Summary

12.1  This method  is  designed for use in the rapid analysis <**£• <
      soil/solid,  oil,  and wipe samples for the target compounds'listed in
      Exhibit C.   If  upon inspection of a sample the Contractor suspects that
      the sample is not amenable to this metjhod, contact the Regional TPO or
      the CLASS contractor for instructions^  For Super&md emergency removal
      actions, contact  the Regional TPO or-j'lne Headquagiters APO for
      instructions.   If,  for emergency resps&se acticras, the TPO or APO are
      not available,  contact the Regional OtiAScifene gfeiordinator (OSC) for
      instructions.   The Laboratory must remembe^'tjjjfct it shall follow the
      requirements in this SOW without deviation.   <;:.._~,

12.2  Before samples  or required blanks can be analyzed, ^tfep^instrument must
      meet initial calibration or^||ja|ppA.tipn check and coliaam resolution
      technical acceptance criter|^J"i:r'Ail;:.^*yfle^^i.tracts, required blanks,
      LCS, PVS, and calibration standards shall«^e:4aaa2?fzed under the same
      instrumental conditions and shall be allowed to warm to ambient
      temperature  (approximately one Ijjpiur) h^diore preparation and analysis.

12.3  The laboratory  shall perform sample-«fetraction and cleanup of water
      samples utilizing eijCh^r solvent (pafcs^graph 14) or solid phase
      (paragraph 15)  extasaefti&si***nd cleanup;/;,The laboratory must meet all
      QA/QC requiremejKBs as statfea under thisi^ontract using either of these
      extraction/cleanup techniques.  The solvent extraction procedures are
      recommended  for' the cleanup 4and extraction of all samples; however,
      pesticides Slgjprocedures SJ^-'^e^s^ll-^Kiy be used if equivalency to the
      solvent extracti^sprocedures !cgifl!"Bi'":
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                                                                          DRAFT
12.5
13
14.
      If unusual or high  concentration samples are received, see Exhibit D,
      Appendix B for general  guidance  on screening and sample preparation.

      Phase Separation

      Multi-phase samples shall be  phase-separated &xdbo.' their individual
      phases.  The phase  separation techniques employed will vary according  to
      the types of samples received.   Since it is impossible -tso- know the
      number and types  of phases  that  will be present in a sample j the choice
      of phase separation techniques is left tso'frthe professional JliBiigement of
      the analyst.  Various techniques can bey employed to separate the phases .
      These include pipetting off liquid phasjes (decanting should not be
      done), centrifuging to  remove suspended solids, and use of spatulas to
      remove solids (wooden tongue  depres^ois work well).  Whenever possible,
      phase separation  operations should DB HJJRjie wititi-iSisposable glassware.
      The phases should be separated into glas^j^ontsilners with teflon- lined
      screw caps.  This allows for  storage and handling of the waste in a safe
      manner.                                          "

      13.1  Samples received  contaaaainjg multiple phase such , as water, oil, and
            soil/solid  in the saine;:;iai^]ye:Jar .shall be phase separated into
            .  1 . • 1  1  1         ' "A-i-H    "*".-.. V, 'll&Sf J vV '".'S
            individual  phases.    *«;i       •-'- %•, ,-;,   v  <-.
                                  ~>i*            , i '  '•;   ' '" ,
                                               s *      -
                                    5 ' -1       $ < *
      13 . 2  Each individual phase is taken through the procedure as a
            subsample.  Report analytical results for each sample phase.
            Note: Each  multi-phase  sample sjjall be identified using the EFA
            sample number convention for mtilti -phase samples as specified in
            Exhibit B.   ,;:;; ;:>/;;;,           "%  ,
                        l;/' "" ''V*            -I1
      13.3  Do not analyze any phase that represents less than 10 percent of
            the total : sample
      13.4  In the ""following pcn^M^e^^ie applicable, references to
            "samples"  explicitly mean "single phase units."
      Solvent Extraction and "
            ,-   -.   ,:-  -,.        *
14.1  Sample&-'fx«piar"atrl<|a -j^nd Extrac^sh -  Water Samples
           "•'*            "^ s*-cf'          '*"
                               is  serially extracted using two 10 mL portions
                               are performed in 125 mL Erlenmeyer flasks with  a
                                e gram of NaCl is added to the aqueous sample
                                hexane extracting solvent is added. Extracts
      are'*sc!J(i!>4.ned,  filtered^' and dried through powdered anhydrous sodium
      sulfate'^ '*a»d concentrated to a 1 mL volume using the nitrogen blowdown
      procedure?^ -S
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                                                                           DRAFT

      14.1.2      Spike  the  sample with 10 /iL of the SMC (5.0 ug/mL).

      14.1.3      Add  teflon stirring bar.

      14.1.4      Add  10 mL  of hexane.

      14.1.5      Place  the  sample on magnetic stirring plate and  stir  for
                  three  minutes.   The stirring rate should "be &ufficient to
                  mix  hexane throughout the sample.           * *  h

      14.1.6      Add  1  gram of NaCl to sample' during stirring and stii for an
                  additional 3 minutes.    ••• •'-

      14.1.7      Remove stir bar  and allow aqueous and hexane layers to
                  separate.                          /•  *

      14.1.8      Transfer the hexane layer by pas;£e«r pipet to a  25 mL
                  concentrator tube.                ',  V

      14.1.9      Repeat steps l%jU4, - 14.1.5 and 14.1.7 :- 14.1.8.  Combine
                  extracts.   Discard extracted aqueous sample.

      14.1.10     Prepare a  drying -column by pj.tjgging tie bottom of a funnel
                  with glass wool  and,; adding approximately 15 grams of
                  powdered anhydrous sodium sulfate.  Pour extract through
                  funnel and collect in Sa £5 mL graduated concentrator
                  tube.Rinse the extract container with minimal volumes of
                  hexane'?3ea& jg&ur  through t|be funnel.  Rinse sodium sulfate
                  twice -with minimal volumes Jsf hexane.
                     .%',:         '''4L.           -"•-
      14.1.11     Concentrate extract to approximately 1 mL using  the
                  M*xogen-blowdji^nsp,.rp3Qedure in a 30°C water bath.  To
                  mitSls&ize anal^M'4Io^c'»^lJ:to volatility occasionally  rinse
                  sidesS»f'.concentrator tube with hexane during the blowdown
                  procedure.-i^Do not let extract go dry during concentration.
      14.1.12.,, -q  :'|Efrcw,«ed to exttraeife clean-up step (paragraph 14.3).
          ^yfl  '^^^J:.^^       "•*%•;,
14.2  Sample" Preparatiori-ialid Extraction -  Soil/Solid Samples
        . ' "               *f|i'-;;;
        ?*/','                  v--'t?'
      A1 16 gram sample of soijafeis mixed with powdered anhydrous sodium sulfate
          is serially extracfjiad with a 20  mL and a 10 mL portion of
                     (50:50)<|aising  an ultrasonic probe.   Extracts are
                filtered, a^Sdried through powdered anhydrous sodium sulfate,
      and cd^^aarated witb/'lSolvent exchange into hexane to a 1 mL volume
      using the !%&t;r<>gen b^«»wdown  procedure.   Non-pesticides extractables are
      removed from •'St^igxtXact with  a florisil column clean-up procedure.
      Final extract volSme is 1 mL.
                                  D-33-PEST-Q                          08/23/94

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                                                                      DRAFT

 14.2.1      Decant and  discard any water layer on a soil/solid  sample.
             Mix samples thoroughly,  especially composited samples.
             Discard any foreign objects such as ssticks, leaves, and
             rocks.                                :
                                                 ;
 14.2.2      Weigh approximately 6  grams of a,representative sample  to
             the nearest  0.1  g into a 150 mL;l»eaker,.

 14.2.3      To the weighed sample  add a sufficient amount-'•&£^powdered
             anhydrous sodium  sulfate to prepare a free flowing mass upon
             mixing.  Mix well.         :v'-:
 14.2.4      Spike the sample with 10 ,pL of the SMC-(5.0 ug/mL), mix
             further.                r \,           "i

 14.2.5      Add 20 mL of hexane/acetone'=(Sf ;5f).

 14.2.6      Sonicate at microtip  maximum power? :€^tqr£'f£bat; the sample extract does  not
             splash excessively; any si^giiificant; loss of sample during
             sonication is  notV«cceptables|*;?Rlnse;:ti»£ sonicator tip after
             each sample extraction withjl'--mL of hexane/acetone (50:50).
             This rinse liquid  shall be^i&bmbined with the sample extract.

 14.2.7      Remove and collect solvent layer in a 40 mL centrifuge tube.

 14.2.8      Add ,10 *mL tiex^m/acetone (§0:50) and repeat steps 14.2.6 and
             14.4/7.        V:;:            -.:

 14.2.9      .Geajbine extractsi^and^ filter, by gravity or vacuum filtration.
             Complete filt^tlstt:::,i?y!itriansferring entire sample contents
             to funnel and  rinse with an additional 10 mL hexane/acetone
             (50:50)7-'^   ,
                         'Jv • -,-
        , .;<;  ~-'.%fK&f9.1    Fotrl|g»avity filtration, prepare a
      \'l '•'•'• '-'""*" ••'.,>•:i      filtfs;iip.on/drying bed with  Whatman #42 filter
    ji. • <            '' '• "(, i   paper  filled with approximately 15 grams of
   ,5%,                 '*>\,;,; powdered  anhydrous sodium sulfate in a 6 cm
 ,,';£>'                  -T-f^owder funnel.  Rinse sodium sulfate and
, "j^                    "iftfilterpaper with hexane/acetone (50:50) and
"""• \$fj*                 vt^scar^- rinsate.   With the filter and sodium
     *fes*"              ^-'sulfate wetted,  decant combined extracts through
      "' '\ Wl,-,^          »::i-the packed funnel and collect in a 40 mL
          ''f:~l.-:^     ,  ;  centrifuge tube.   Rinse the extract container
              ' 'Tj S-.^^r.   with minimal volumes of hexane/acetone (50:50)
                 : ,1-;     and pour  through the funnel.  Rinse
                         filter/sodium sulfate with 10 mL of
                         hexane/acetone (50:50).

                             D-34-PEST-Q                          08/23/94

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                                                                           DRAFT

                  14.2.9.2     For vacuum filtration use Whatman #42 filter
                               paper in a Buchner funnel.  Pre-wet the paper
                               with the hexane/acetone (50:50) solvent and
                               discard rinsate.  Transfer combined extracts
                               into funnel,  apply vacsisa, and collect filtrate.
                               Rinse filter with an ;10'siaL>-*>f hexane/acetone
                               (50:50),  Pour filtered extract through a powder
                               funnel plugged with glass wool ^ctd filled with
                               powdered anhydrous sodium sulfate jemd collect in
                               a 40 mL centrifuge tube.  Rinse the'-fcbptxact
                               container with=ili.tiimal volumes of hexane/icetone
                               (50:50) and peur through the funnel. Rinse
                               sodium sulfatfi with an adSitional 10 mL
                               hexane/acetone (50:50). .fj ?
                                            '  *        *'" •
      14.2.10     Concentrate  extract to approaclaaately 25 mL using the
                  nitrogen-blowdown procedure in ^;;30°C water bath.  Transfer
                  extract concentrate to a 25 mL concentrator tube and
                  concentrate  further to approximately^J5-.mL.  Add 5 mL  of
                  hexane to  concentrator tube and mix vigorously.
                  Reconcentrate ^approximately 1 mL.  To minimize analyte
                  loss due to  volatility/ bt&^f&aaBGaM^rinse sides of
                  centrifuge and concentrator ,^>es:"wtt:iisfiexane during the
                  blowdown procedure^: Do not allow extract to go dry during
                  concentration.       ':
      14.2.11     Proceed  to  extract clean-lip step (paragraph 14.3).

14.3  Florisil Cartridj|«:;'Proceltaf«
                     ^
                     !,F>          '-V
      14.3.1      Attach the  Vacl^pLute vacuum manifold to a water aspirator or
                  vacuum pump with  a trap installed between the manifold on
                   •"-.  '    *  *   •? j^ -.>•••. •* • ; -ft •; •• « * "•* ^'« i -. ••
                  £Jaej;*Vacuum  sa^|c^e'Jjl7^|J^pt the vacuum pressure in the
                              between 5 and 10 pounds of vacuum.
      14.3.2      Place one Fl^Eisil  cartridge into the vacuum manifold for
             ... , :  ieactx sample  extract.

      14.3,r*3      Prior ''taijtcleanup  of samples, the cartridge must be washed
        ?  -.' '       with hexb^/acetone (90:10). This is accomplished by placing
      - "•'). '         the cartr^^e  in  the  vacuum manifold pulling a vacuum and
       j^          passing 5 |S*, of the hexane/acetone (90:10) solution through
       «I :|~        the cartridge.  While the cartridges are being washed,
        'H  y,,    adjust thej^iracuum applied to each cartridge so that it is
                  approxims^Ly  equal.   DO NOT ALLOW THE CARTRIDGES TO GO DRY
                             HAVE BEEN  WASHED.
      14.3.4      Af fc^c Ime cartridges  in the manifold are washed the vacuum
                  is released  and a  rack containing labeled 10 mL volumetric
                  flasks is placed inside the manifold.  Care must be taken to

                                  D-35-PEST-Q                          08/23/94

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                                                                           DRAFT

                   ensure  that the solvent guide from each cartridge is placed
                   inside  of the appropriate volumetric flask as  the manifold
                   top  is  replaced and that the sorbent beds do not  go dry
                   after they have been conditioned.  ;

      14.3.5       After the volumetric flasks are in fiX^de, vacuum  to the
                   manifold is restored and extracts from each field and QC
                   sample  solution is transferred to the top iSrit; of the
                   appropriate Florisil cartridge.
                                              /'' '•
      14 . 3 . 6       The  pesticides in the extract concentrates are then fluted
                   through the column with 9 -anti, of hexane/acetone (90:10) and
                   collected into the 10 mLAlumetric flbasks held in the rack
                   inside  of the vacuum maitifold.      ,;, ;
                                            ''* ;   . ,     ' ' *
      14 . 3 . 7       Transfer the eluate in each";-v41umet:ric flask to a clean
                   centrifuge tube or 10 mL vial.   TJ§e two additional 1 mL
                   hexane/acetone (90:10) rinses of t&e flask to  ensure
                   quantitative transfer of the cartridg6.ei.uate .
                                  •K--,
      14.3.8       Reduce  the to t^tlr ^citapsv.^ .-^he  volumetric tube to 1 mL by
                   using either ni^agen blb^lfej£itt-;0x- aa-cro-Snyder column.
                   This final volume l^s suitable%€or extract analyte
                   concentrations of 'W ng/mL -iiso" 1000 ng/mL.  This is
                   equivalent to sample ^eompsisid concentrations of 0 . 1 to 10
                   /ig/L for water samples,, Jl-7" to  167  /igAg for  soil/solid
                   samples ,  and 100 to 10 ,000 |ig/kg for oil samples .
      14.3.9      If cxjsstals'djfjfculfur are ^tedent or the presence  of sulfur
                  is suspected,  ptbceed to paragraph 14.4.  Sample analyses
                  showing  the  presence of sulfur are not acceptable  and must
                  i»!\reanalyzed ,#ilter,,,sulf ur  removal .
                                „ ; S'."-~-Y': >>.«  ' ••-,: "
                    "                        '
      14.3.10     If stlUer  is  not expected to be a problem, transfer the 1.0
                  mL of saa|Jle,to a GC vial and label the vial.  The  extract
                  is ready fo^/SC/ECD analysis; proceed to paragraph  18.
                        the  extr^iCs-i. at 4»C (± 2°C) in the dark until analyses


14.4  Su3J5ar Removal

     •13$.4.1      Bright  (unoxlLdized)  granular copper is used to remove sulfur
     •Vi,A;,|,       contamination.   Add one to three granules of copper to each
         ;-§-^,>,    hexane  extspabt  in a clean vial.  Tighten the top  on the vial
             3> ,,,,_,and shake-JjSbr 30 seconds.  Filter or centrifuge and then
               " "v:-d*cant  tlajfe solution to remove all solid precipitates.   If
                  e«?f»|>ffer:%|?pears  bright, go to paragraph 18.  If copper
                  chan§e«f-'color,  repeat sulfur removal as necessary.
                                  D-36-PEST-Q                           08/23/94

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                                                                           DRAFT

      14.4.2       If  only a partial set of the samples in the Batch require
                   sulfur  cleanup,  an additional reagent blank of hexane spiked
                   with the appropriate amount of the SMC solution  and cleaned
                   with the copper is required.

      14.4.3       Proceed to paragraph 18 for GC/ECD-analysis.

15    Solid Phase  Extraction and Cleanup of Water Samples   '

      Solid Phase  Extraction using nonpolar Cg;(or equivalent)  or  C^g. disks
      may be used  to  extract water samples (an alternative  disk phase-may be
      used if the  new phase can be demonstrafcjsd to meet the QA/QC  requirements
      of this method).  An additional filte£;'!disk is repaired when water
      samples contain particulates.   Upour4f>pening a p&dkage of  disks,  they
      shall be used immediately or stored itk>•&.desiccator (over Drierite,  or
      equivalent).  For reproducible extraction efficiencies, all  directions
      given below  shall be followed as closely as possible.  NOTE:  The
      laboratory shall not use SPE for non-aqueous sauries.

15.1  Sample Filtration          ~
                                 ~~l \  \i J- >'•'• *'
      All water samples extracted%|sing SPB^i^ti^;,?• ~                  4*;
      15 .(2.'«^. ..    Shake  samp3||s vigorously to mix thoroughly.

      15.2.6   ' , .; -Pfpceed ,-^ith sample cleanup and extraction utilizing  SPE
                                  (paragraphs 15.3 - 15.7).
15.3  Disk Set-up and Conditioning


                                  D-37-PEST-Q                           08/23/94

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                                                                          DRAFT

      15.3.1      Place the disk onto  the  frit on the vacuum head, place the
                  reservoir on  top of  the  head and clip together.

      15.3.2      When filtration is required, a filtration disk or 500 mg of
                  Celite will be placed on top of the .extraction disk.
                                                       - , V'S
      15.3.3      Turn vacuum pump on  and  set pump vacuum ',to 10 inches of
                  mercury.  Do  not exceed  the manufacturer's,, recommendation
                  for manifold  vacuum.   Flow rates can be controlled by
                  opening and closing  vacuum massif old valves or pineih clamps .
                                              **?•* -                         *:•
      15.3.4      Wash each disk with  four 5/rJttL aliquots of hexane/acetone
                  (90:10).  SLOWLY open vaeptuin valves tso sallow the
                  hexane/acetone (90:10) to 'pass thro«^i the disk after each
                  wash .                    '<;'> '-' 1.       '• ' *
      15.3.5      Wash each disk with  four 5 mL '^ateigaots of methanol (MeOH) .
                  Let disks drain after  each wash. !H» aso.t allow the disks to
                  drain dry between washes.              ;
      15.3.6      Wash the disks-«ltt», jsjjt£^y«L aliquots of methanol/water
                  (5:100).  Allow^je firsfc-:S':.';y|-pdrtion to wash through;
                  however, do not a^iow the disK'to "fe&ilti dry.  Next wash the
                  last 5 mL portion tfepugh, keteping the disk wet.   Each disk
                  must remain moist until  the entire sample volume is
                  extracted.  DURING  CONDITIONING,  DO NOT ALLOW DISKS TO DRY.
                  THIS STEP IS CRITICAL POR. GOOD RECOVERIES.

15.4  Compound Extraction

      15.4.1      Svirl the samp^e^from paragraph 15.2) for 20 seconds and
                  carefully decaife^the, sample into the sample reservoir.

      15.4.2      Open manifold valves  to  allow samples to pass through the
                  disks at..g|j»|»r.oximately 3-8 mL/min.  The flow rate must not
                  exceed 10 mtj^Blap..   If the flow rate slows because of
             ,, ...  'jiasfciculate buCf|&iu on the disk or filter, increase the
            •-0:''  '•vaetaairii.o maintatstjIS  - 8 mL/min.  flow.

        •J..        NOTE: It'^wst take  at least 10 minutes for the sample to
      ;  ^               pass?;|ivrough  the disk.

                  Rinse the simple container with 5-10 mL of methanol/water
                  (5:100) inf^f" the sample  reservoir to transfer any remaining
      15.4.4      16Sat>£tfe|.entire  sample  volume has passed through the disks
                  (app^oaSanately 15 minutes),  rinse the sample reservoir with
                  an additional 5  - 10 mL methanol/water (5:100) into the
                  disks .

                                  D-38-PEST-Q                         • 08/23/94

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                                                                           DRAFT

      15.4.5      Wash the disks with an additional  5  mL methanol/water
                   (5:100), continue to apply vacuum  until the top of the disk
                  is  dry.   Turn off vacuum.

      15.4.6      Wipe the reservoir dry with clean  iab tissues (Kimwipes, or
                  equivalent) .                          ::;  ;

15.5  Compound Elution using Disks

      15.5.1      Release  the vacuum on each filtration device, disjaose of the
                  aqueous  eluate in the larger %eceiver.   Do not unclit^tshe
                  reservoir from the vacuum, tfee'ad.
                                             I?*           j
      15.5.2      Place a  clean solvent tsee4Iver over, iefbe drip tip of the
                  vacuum head.             -  |-- ,;,
                                               •', , ,,-.  s,_
      15.5.3      Add 5 mL hexane/acetone (9:1) to ;4ach disk.   If additional
                  filtration media was used, allow tberibexane/acetone to stand
                  in  the reservoir for 2 minutes prior' ISO' applying vacuum.
      15.5.4      Turn vacuum p\s^*w^.,j4^tsB5tsjpump pressure to 5 inches of
                  mercury.        '^;      '-•-^:'(j:. -t'  - -   ^

      15.5.5      SLOWLY open the manifold values  to allow hexane/acetone to
                  soak into the sorbent bed..  DO NOT ALLOW THE HEXANE/ACETONE
                  TO  ELUTE  AT THIS TIME.:, £»Sose valves  and allow disks to soak
                  for 2  minutes .            ; ;
      15.5.6      Afterv2'minut&s^; slowly op^at the manifold valves and collect
                  el^srit into thefeeceiver tulfe,   APPLICATION OF EXCESSIVE
                  VACtJOM WILL RESflLT IN ANALYTE LOSS.
      15.5.7      Ad&£a^econd ^IwfeH^^. jiL hexane/acetone  to each disk and
                  elute::fctt^der vacuum until the disk  is  dry.
                          ' - *' \ >
      15.5.8      If a water•'Is^er is evident in the eluate,  remove by the
              ,,.: :,f-addition  of sb^tua^jsulfate as follows:   (Note:  water
            s, F- !!::*Inj^c^ed  into the^^t? may strip the analytical column phase
         /:;.:?'     and mayfEsuse retention time shifts.)
        .ft'-               '""i?
        ',?^ *'                 '',;".;
      .--»?'        15.5.8.1  %f,Add 5 g Na2S04 to the  eluate.
                  15.5.8.2   ,-,, pJecant the eluate and quantitatively recover the
                            j;,t pesticides by adding additional  90:10
                           l?!"" hexane/acetone to the Na2SO^.  Combine this
               ' j.:- '>.,     £.$' hexane/acetone with the  eluate.

      15.5.9      Bring^fcfhe  total volume in the receiver  tube  to 1 mL by
                  concentration.
                                  D-39-PEST-Q                          08/23/94

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                                                                          DRAFT

15.6  Florisil Cartridge Procedure

      15.6.1      Attach the Vac Elute vacuum manifold to a water aspirator or
                  vacuum pump with a  trap  installed  between the manifold on
                  the vacuum source.  Adjust the vacuum pressure in the
                  manifold to between 5 and 10 pounds  'oi "Vacuum.

      15.6.2      Place one Florisil  cartridge into  the vacuum manifold for
                  each sample extract.                           :>  ,

      15.6.3      Prior to cleanup of sample?/ the cartridge must be washed
                  with hexane/acetone (90:10?)'; This is accomplished by
                  placing the cartridge in t-be vacuum  mamifold pulling a
                  vacuum and passing  5 mL;:«d: the hexase/acetone solution
                  through the cartridge.  Mfljie the  cartridges are being
                  washed, adjust the  vacuum applied";ttO each cartridge so that
                  it is approximately equal .   DO HOT ALLOW THE CARTRIDGES TO
                  GO DRY AFTER THEY HAVE BEEN WASHED.

      15.6.4      After the cartridges in  the manifold are" washed the vacuum
                  is released andrsa j:rack ^cstmtaining  labeled 10 mL volumetric
                  flasks is placet 33iside 'oie'totiif^ld..;;. Care must be taken to
                  ensure that the solvent  guid^Sfrom each, cartridge is placed
                  inside of the appropriate volumetric flask as the manifold
                  top is replaced and tiiat tshe sorbent beds do not go dry
                  after they have been conditioned.

      15.6.5      After the volumetric flasks are in place,  vacuum to the
                  manifold is restored and extracts  from each field and QC
                  sample solution .ts  transferrisa to  the top frit of the
                  appropriate Flcaeisil cartridge.

      15 . 6 . 6      The>pesticideai,-: 3H,jtKe -jJMa&sact concentrates are then eluted
                  througn:;-*       hexane/ac^?ne (90:10)  rinses  of  the flask to ensure
       :'  "         quantitative transfer of the cartridge eluate.
      „_»'                      " Jr
      C *                      ' 1
                  Concentrat^jthe solution to a  1.0 mL volume using either
              s    nitrogen b3|aw-down  or micro-Snyder column.   Measure the
              1 1";! -final volume with a syringe or by transferring the extract
               '- • to-.a vol^mietric flask.   This final volume is suitable for
                  extract: jmalyte concentrations of 10 ng/mL to 1000 ng/mL.
                  This '^ ^equivalent  to sample compound concentrations of 0 . 1
                  to 10 /tg/L for water samples .
                                  D-40-PEST-Q                          08/23/94

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                                                                           DRAFT

       15.6.9       If crystals of sulfur are evident or the presence of sulfur
                   is suspected, proceed to paragraph 15.10.  Sample analyses
                   showing the presence of sulfur are not: acceptable and must
                   be reanalyzed after sulfur  removal.  [

       15.6.10      If sulfur is not expected to be a fusoblem,  transfer the 1.0
                   mL of sample to a GC vial and  label the --vial.  The extract
                   is ready for GC/ECD analysis;  proceed to paragraph 18.
                   Store the extracts at 4°C (± 2°C) in the darklia&til analyses
                   are performed.               v                   ;   ,-"   ,
                                               ' •''                        '^
15.7   Sulfur Removal                       ,.-.;
                                           N*           /
       15.7.1       Add one to three granulpMHof bright,, ^anoxidized)  granular
                   copper to each extract saltation inisa clean vial.   Tighten
                   the top on the vial and shakd ^ *-*'^? ; ^-^'' '          '-;,- ';-
      mark. -\'.'~' "  '" ->,;-'-•••;•          '  K-
                         '              '
16.4  Ca&!^with stopper and^«bc for one minute.
        Z-                    "*1
16.5 ,
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                                                                          DRAFT

      NOTE: The target compound CRQLs  for wipe samples will be specified by
            the Agency.

17.1  Pour off any free solvent from the  sample jar into a clean Erlenmeyer
      flask of appropriate size.

17.2  Spike the sample with 10 uL of the  SMC (5.0 ugjfaL).  >

17.3  Add enough clean hexane to the sample jar to cover the wipe'-sample.

      17.3.1      If the shape of the  sampleJ|«r is not amenable to   ',']'
                  sonication, quantitativelyitransfer the sample to an
                  appropriate container.  .jtj&se the samfle jar with 5 -10 mL
                  of hexane and transfer £g? .the new sample container.
                                          "'"^f ;     /••'•
17.4  Sonicate at microtip maximum power;  codlli&e g&aple during sonication.
      The sonicator must be set for 50 percent pTils^^ction.  Sonicate for 3
      minutes.  The power output may have  to be adjust*^, to ensure that the
      sample extract does not splash excessively;  any significant loss of
      sample during sonication is/siot, acceptable.   Rinse t&e sonicator tip
      after each sample extracti^a^bi|K^|rtU^|, hexane.

17.5  Remove the hexane layer from ^be sonicatjsn aiid;«aowbine it with the
      hexane in the Erlenmeyer flask ;>i-r

17.6  Repeat steps 17.3-17.5.         ;w

17.7  Filter the combined<.exjt33aets by  gravity filtration.

      17.7.1      Prepare a filt£^trion/drying%l»ed with Whatman #42 filter
                  paper filled wilSi approximately 15 grams of powdered
                  anhydrous sodiji^|js,uj.fate,JLn a 6 cm powder funnel.  Rinse the
                  sodium sulfate'-s:aiii":ipjier;';:jpaper with hexane and discard
                  rinsat:«,. .With the filter and sodium sulfate wetted, decant
                  combined (extracts through the packed funnel and collect in a
                  clean concen£$|a£;or tube.   Rinse the Erlenmeyer flask with 10
              ,-/, /;aiL'hexane, an%<>4||aa|sfer  rinse solvent to powder funnel.
            ,'J   ;s "Rinss powder funfte^lwith 10 mL hexane.

17.8  Coventrate extract ^Approximately 20 mL using the nitrogen blowdown
      pacacedure in a 30°C wat»r bath.  Transfer extract concentrate to a clean
     ,^,or 30 mL coneentrat&fcf tube, and  rinse concentrator tube (from
     'pai^graph 17.7.1) withj^mL hexane.   Transfer the rinse solvent to the
      25 "6a£|ifi, mL concentraGtsj? tube, and  concentrate further to approximately
      1 mL. ^j^painimize anaS^te loss  due  to volatility, occasionally rinse
      sides of feetitsifuge toill concentrator tubes with hexane during the
      blowdown procelbj&e.. If-'
                     '•--.  ,
17.9  Proceed to extract clean-up steps (paragraph 14.3).


                                  D-42-PEST-Q                          08/23/94

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                                                                          DRAFT

18    Instrumental Analysis

18.1  Set up the GC system per the  requirements  in paragraph 7.

      18.1.1      Solvent-flush manual  injection or automated sample injection
                  is recommended for  analysis.      -  .:

      18.1.2      An analytical sequence  consists of field simple analyses and
                  all associated standards, blanks,  and QC analyses performed
                  within a 24-hour  period on one instrument.   There.laace two
                  (2) types of analytical sentiences:  an initial calibration
                  analytical sequence and a«^aily calibration check analytical
                  sequence.  All samples  s&all be analysed within one of these
                  analytical sequences .   V

                  18.1.2.1    An initial  callfeSati-OBfianalytical sequence
                              begins  with a three»p6i,nt calibration, an
                              instrument  blank,  an liSS^, and a method blank.
                              The initial calibration analytical sequence is
                              as follows :
                                «V   ••'','"'••'•(•
                                C j 5 '  " v"  v "„ /™  ,. * < f , ..<
                              •  M - ,Initial-^d^«erp®iat; calibration (analysis
                                   - !sof  the higii-,^3"tari€as:
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                                                                           DRAFT

                               •      Field Sample(s) ;

                               •      Instrument Blank(s); ,and

                               •      Performance Verification  Standard(s) .

      18.1.3       If all  acceptance criteria for these analyses  are  met,  then
                   the Laboratory may proceed with sample analyses.
                                                                   _,-!
      18.1.4       All analytical sequences conclude with an acceptable
                   instrument blank and  PVS aaeilyses.  The final PVS '-shall be
                   started within 24 hours afijer the injection of the first
                   initial calibration standard or the first instrument blank
                   in the  daily calibration sequence.  ~\-.
                                              ,
                  NOTE:  If a PVS reanalysis Is^retjuixe'd because of  a non-
                  compliant initial PVS analysis',5 the, PVS reanalysis must  be
                  started  within 26 hours after the -slrbcrt of the  current
                  analytical sequence.
      18.1.5      The method blai&iiul^sall associated samples shall be
                  analyzed in thelsame ahaly^lsaij sequence.  If samples  from a
                  batch are analyzed; in more than one analytical  sequence,  the
                  associated method blank must also be analyzed in the same
                  analytical sequence.'!': If a>riaethod blank extract is  used up
                  because  of multiple analyses, the Laboratory shall
                  substitute an instrument: blank in place of a method blank in
                  all subsequent analytical sequences .  The Laboratory shall
                  note;, this in:'tiie Batch Narrative and shall use  the  EPA
                  idelStlficatiorfJtKsiiber as described in Exhibit B for this
                  instrument blaiie/
                    ' ;              • v 8
                                 , 3 • *!>..,._,. ^ >w .
      18.1.6      TbseULGS  shall,.^e'lifti|l^^dltVith all associated samples  in the
                  same analytical sequence.  If samples from a batch  are
                  analyzed ,ffa= more than one analytical sequence,  the
                  associated"ii£S>.>;:shall be analyzed in the same analytical
              ,; , ^sfajuence.   If^arill-fpS extract is used up because of  multiple
            ;•$ '"'' 'analfsfef,,  the LaStifMtory shall dilute the LCS standard
         ,.-£•'•"'     mixtufe||s^i;he  original stock mix) and use this solution in
        i:;:-::;;:'        place of 'Stifle  original LCS sample in all subsequent
       :r""         analytica!j|s«quences (see paragraph 27).  The Laboratory
      ;T ,          shall note^giis in the Batch Narrative and shall use the EPA
                  identification number as described in Exhibit B for this LCS
             -    Solution.   ;~
18.2  Computer f^flssftductio^ of chromatograms that are attenuated to  ensure
      that all peatfcg •..•$&> &OXC scale over a 100-fold range are acceptable.
      However, post anaHjisis attenuation shall be no greater than a 100-fold
      range .  This is  to"' reduce the potential for RTSs of compounds due  to
      column overload  and  to ensure that the detector is operating within the

                                  D-44-PEST-Q                          08/23/94

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                                                                          DRAFT

      calibration  range.   If any sample compounds exceed the calibration
      range, they  shall be diluted according to paragraph 19.

18.3  If any saturated non-target compound chromatograf*hic peaks are evident
      or if any chromatographic peaks overlap more tfaait one RRT and/or RT
      target compound  windows,  the Laboratory shall ;use *&e "E,N" flags on
      Form QI-PEST to  indicate  this situation.           .  ',,

      18.3.1       If saturated  chromatographic peaks outside tairgfet: compound
                   RRT  and/or RT windows are evident, flag the nearest; tar get
                   compound "E,N" on Form QI-PEST.

      18.3.2       If chromatographic peakslisverlapping ,ffiore than one target
                   compound RRT  and/or RT -Windows are |s^ident,  flag the
                   corresponding target conp^iaads "E.jf? on Form QI-PEST.

18.4  Chromatographic  peak response must be greater than 10 percent and
      less than 100 percent of  full-scale deflection'-toCensure that
      individual compounds will be visible during data t^eview.
                                  i- .;":!
19    Dilutions                  >\^ ^%v|-'^. ,

19.1  Samples with compounds exceed^g the calibration ibange of the GC must be
      reported with the "E" data flag?as described in Exhibit B.  Upon
      evaluation,  the  Region may requfife that 'the samples be diluted,
      reextracted, and/or  reanalyzed in -'j|,.trdtid analytical sequence as
      additional paid  samples.   ReextractfJU*n and/or reanalysis of diluted
      samples can  only be  «*j;ta»r4.zed by the "-CLASS contractor acting on behalf
      of the Regional ,:I3?0  or Hea&guarters AK§:,  The Laboratory shall perform
      the dilution ansiiysis as  s'|e]Cdfied beldw-Yln paragraphs 19.2.2 and
      19.2.3.       -  •           f,*;

19.2  The Laboratoryvaaay, dilute^^l^Jwi^c^r to initiating sample
      extraction/analyses*,;; The resulting analysis of those samples must
      produce chromatogramis: -with at least one target compound present at a
      concentration greater "tfsaajtjhat found in the mid point calibration
      mixture,^^,^.UB^>,compound  ls;||dentified in the diluted sample at a
      concesBBefcircfton ;1!^a|:y^xceeds thfejikld level standard,  then the undiluted
      samgiie" shall be  reettagacted and/or reanalyzed at no additional cost to
                            ":>,*

                  At the reqijfest of the Region,  sample dilution may be
                  required pjfcfcbr to the initial  extraction and analysis.   If
                  no target^pnpounds are detected in the diluted sample at
                  the mid  profit concentration or greater,  then the undiluted
                 :sample shall  be reextracted and/or reanalyzed as an
                              paid sample.
                      v  ,

      19.2.2      Dilutions  - Solvent  extracted,  oil,  and wipe samples
                                  D-45-PEST-Q                          08/23/94

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                                                                          DRAFT

                   19.2.2.1    Dilutions of solvent extracted, oil, and wipe
                               samples shall be made by using an appropriate
                               aliquot of the extract diluted in hexane.
                               After making a dilution, add sufficient SMC
                               solution to bring up to. proper concentration (50
                               ng/mL) .                i; -,,

      19.2.3       Dilutions  -  SPE extracted samples          :

                   19.2.3.1    Dilutions of wateis samples shall be Hade by
                               using an appropriate aliquot of sample dilated
                               to 100 ml withjwethanol/water (5:100) (see
                               paragraph 15.-&I.   Continue "with sample
                               extraction U>|pataon.     *^'-^"
         V-/^            '  "f ''
20.2  Compound identificatEpft when SMC recovery is greater than or equal to 10
      percent and  less than |br equal to 200 percent.
      "" '                      ^'\ ^
                   Target  compjjfands shall be identified on the basis of RRT in
                   all field isJsaaples for which the SMC recovery is greater than
                   or equalJsoflO percent and less than or equal to 200
                 ,.flucent.v;,''

      20.2.2       Peafcs-in sample chromatograms shall be identified as target
                   compounds if their RRT is within ± 0.005 RRT units of the


                                   D-46-PEST-Q                          08/23/94

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                                                                           DRAFT

                  mean RRT of the standard established during initial
                  calibration.

20.3  Compound identification when SMC recovery is less than  10  percent,
      greater than  200 percent,  or if peak interferences are  present.
                                                       > • .
      20.3.1      Target compounds shall be identified on-the basis  of
                  absolute RT in all field samples for which.the SMC recovery
                  is  less than 10 percent, greater than 200 pereetlt,  or if
                  peak interferences are present.                 !;''X
                                              ,s
      20.3.2       Peaks  in sample chromatogcams shall be identified as  target
                   compounds if their absoltt|e RT is wit3iin ±  1.0 percent of
                   the mean RT established; rdsnring the ial'tial  calibration.
      20.3.3      Any  compound identified onl^vqee^asiis of absolute  RT shall be
                  flagged with the qualifier "T"" __ *

      20.3.4      If the recovery of the SMC in a field isample  is less than 10
                  percent,  greatest: xthan 200 percent, or if p«ak interferences
                  are  present fay's a34jjjH|^^».iost appropriate peak.  The
      Laboratory shairiUescribe in the Batch Narrative the rationale  used  for
      choosing a particular'• jfeak (e.g., chose peak closest to the RT  of the
      peak in calibration che^fe standard) as the target compound or SMC and
      how the Afield -sample matrSx-jbay have affected peak identification.

21    Calcialations     '  ->i),,,,

21.1  G&ieulate the RRT  of afisample  component or a standard using the
     =1111(11 owing equation:    l-tV

         ~~'ff- >'i '£              i'; "         or
            ^~l  v            j.~'SRT -     KTcoaeonent                  £Q.  D.ll
             "' -'•"'< '          -'*,            RT	
                                  D-47-PEST-Q                          08/23/94

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                                                                          DRAFT

      Where:

      RRT = relative retention  time

      RTcomponent = retention time of  the  target compound

      RTSMC = retention time of the  SMC

21.2  Calculate the calibration factor for a compound by one of /three
      techniques using data collected  during an -acceptable initial 'calibration
      (paragraph 8) .  The use of the line  segaifent or "K" curve is suggested.
      Only one of the quantitation technique^, -listed below shall be used for
      quantitating field and QC samples witM.n  a Batch Of analyzed within a
      given analytical sequence .         :fL "
                                            '
      21.2.1      Use the "K" curve  (line  segtteulcs^^established during initial
                  calibration.  The  segments  ruir-ftr^osi, the low to the mid point
                  and from the mid to  the  high point: jcsalibr at ion mixtures.
                  (Note: do not extend line segment thf%i«3a may be used as long
                  as the mid point vs$?ues  are^idthin ± 10 percent of the
                  average of the high4asd  lcn»|point values.
                                         ^   --{"
      21.2.3      Use the mean calibration if actor established during the
                                               :
      21.2.4      Quaaifitation o'C^eompounds  i^-'ha.sed. on the calibration
                  factors established during initial calibration.
      21.2.5      Ml ealibratioasirelqiiirepents,  including the initial
                  calibration %RSD and  the  calibration check %D criteria, must
                  be met Tfegaiadless of  the  quantitation technique used.

21.3  Quantitatioapf Target CbmpTBUfisls

      Calculate the concentration in the  sample  using one of the following
      ecpMtions for external Standards.   The  response can be measured by
      automated peak height^ integrated peak area measurements.
     /:r'                   '^.
     '•^.-3.1      Water     :,t
                                                                EQ. D.12
                                  D-48-PEST-Q                          08/23/94

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                                                                            DRAFT

                   where :

                   AX    =     response for the analyte to  be measured.

                   CFm   =     calibration factor established by one of three
                               techniques during the, initial  calibration.
                               (NOTE:  Only one methoS of qpaaatitation may be
                               used  for field and QC samples '^Ilsliin a Batch or
                               analyzed within a given analyticMl ^sequence) .
                                                -. I'f                   ' "'"
                   Vt    =     volume  of concentrated extract (^L)  (use £000 /jL
                               or a  factor of^this when dilutions are made).

                   Vi    =     volume  of esttatact injected (/'.     &...,"

                   AJJ,  CFm, V^ = same  as  given in Equation D.12
                   Vfc    —     "«r^tume  of  conegaOtrated extract  (use  1000 jxL or a
                     ,-V         f aifefcor  of  this -1«9ien dilutions are made) .
                                       of .sample extracted in  g.
                   ..,            - -t *<• '••'.'••*,? 1 <"*' ' •-,','•':.  "<*'"
                     < "•  •• •        tfX ' ••  -1 ¥&• £*• ^fsf >l^-f ' vv' $
                     '••.-.         v* **••*' --v *'.£k ; ff ", }&. *.„,,„?, f
                   NOTE:<'f$ia: oil samples, divide Ws by 10.  The  factor of 10
                         fo£ pie Ws is necessary because only one-tenth of the
                         hexattiejjej&tract is processed and analyzed.
21.4  Calcu^aM " t!he''"1JSQftj5^jount obse^fed  and amount (percent) recovered using
      equations as  descrijpfd in paragraph 10.4.

21.5  |8|S shall be  monitore%msing the SMC (paragraph 20.1).  The RTS  shall be
        asured for  all ana
              j, _    Calculate ^e retention time percent difference  (RT %D)
              l'i;.:^,  between g$^t RT of SMC  in the field and QC samples  or
               : - v -sis^ibsequj^tfc" standards analyzed and the mean SMC RT  from the
                               initial calibration analyzed using the following
                                   D-49-PEST-Q                           08/23/94

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                                                                           DRAFT
                                       RTC

                  where :

                  RT %D =     retention time percent difference.

                  RTS   =     retention time of the SMC in a field. and QC
                               sample or subsequent standard.

                  RTC   =     mean retention .time of the SMC from  the most
                               recent initial calibration.

22    Technical Acceptance Criteria       -;  -:,,

22.1  Each  sample within a Batch shall be analyzed =on a GC system  meeting the
      initial  calibration or valid calibration check 'technical acceptance
      criteria (paragraphs 8 and 9).                   i   ,

22.2  Each  sample within a Batch-'J^ta«^s^,-4^w^rzed after an acceptable method
      and instrument blank (paragraphs 25 2&dtJSUJ$^\ .and-, after an acceptable LCS
      (paragraph 27)  are  analyzed.   ,:«v         ,- f      '.•
                                     r,.\       ~  i '
22.3  Each  sample within a Batch shall'xfee rua.i/ithin a valid initial
      calibration or daily calibration eliac|:2analytical sequence that
      concludes with an acceptable instrument; blank (paragraph 26)  and an
      acceptable PVS analysi:s;;(f>aragraph
                             ' ''
                      ,                        .
22.4  Each sample witt»iii a BatclTislhall be anal^aed and results reported within
      the contract required turnalE-exind times .
                                  **!•'•'
                   -  „            V'-5"^, ,-,,«,«-„«.,
22.5  Each sample malbttx, withinjjia's^l^J^fc^i have an acceptable method blank
      analyzed during the ;same analytical sequence .
22.6  The RTS for the SMC RT'^litf^be within ±1.0 percent between any  sample
      in a Batch ",«ad;,tlie  mean RT^j:,-',t;he SMC analyzed during the initial
      calibration.  *fh#jR3:S is not"' eiluated if the SMC is not recovered or if
      peak: '.interferences'
22.7  |fefer advisory recovery ;ifenit for the SMC is 50-150 percent.  Reanalyses
      jof\ field samples  are  n^, made if the SMC recovery is outside the
               recovery limits,!
22.8  The StfC ;,»efcpvery mustsfee greater than or equal to 10 percent and less
      than or eq^Qt -fo 200>3*ercent in order to use RRT for identification
      purposes.  Th«>i^atification window is ± 0.005 unit of the mean RRT of
      each target composted from the initial calibration.  If the recovery of
      the SMC is less  than 10 percent, greater than 200 percent, or  if peak
      interferences are  present (but is adequately recovered in the  method

                                  D-50-PEST-Q                          08/23/94

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                                                                          DRAFT

      blank), the absolute  RT  of the compounds shall be used for
      identification purposes.   The identification window is ± 1.0 percent of
      the mean absolute RT  of  each target compound from the initial
      calibration.

23    Corrective Action                               ', ;

23.1  Flag all sample results  "S"  if the SMC is outside thesatfeisory recovery
      limits of 50-150 percent.                               "'  ,'  •

23.2  Flag all sample results  "T"  if the absdLate RTs are used for  *   '
      identifications.                       \\

23.3  An SMC recovery of less  than 20 perdeat in the method blank or LCS
      associated with a sample Batch is  an indication that serious problems
      may have occurred during the extraction' fiirecessL   Corrective action
      shall be performed and the unacceptable metlhod blank and/or LCS and all
      samples associated with  the  unacceptable method blank and/or LCS shall
      be reextracted and reanalyzed at no additional expense to the Agency.

23.4  If the SMC retention  time  |^fl;^|E1S|  «=j:iterion is  not met for any field
      sample, sample analysis  shall; be stopp&d and the  noncompliant sample
      rerun.  If the RTS criterion'*s, still  out* wpoiv-ireaiiklysis, analyze an
      instrument blank.  If the  instilment blaik SMC RTS  is outside the
      criterion, perform corrective act|Um wM,ch may include a new initial
      calibration.  DO NOT  continue with.i&aaj^le analyses  until the RTS is
      within ±1.0 percent.  If  the instroa^nt blank SMC  RTS meets the
      criterion, sample aaM^sIs, may continjbe:.   The Laboratory shall report
      both sets of nopeonpliarit"Jlsample data '«aad flag the  results "M".   Note:
      The RTS is not jlsraluated ilLlEhe SMC is'Sot; recovered or if peak
      interferences v-aife present. !-i|;
23.5  All target compound concentellations wtiich  exceed the upper limit of the
      initial calibrationgrange will be flagged "E"  (see Exhibit B) .
      NOTE:  Unless otherwise^tasted  in Exhibit  D,  all sample data from the
      initial.^an&l^sis, shall be reported  to  the  appropriate Region.  Samples
      not meriting anyioja$ iOf the confefeact technical acceptance criteria and
      not, acquiring autoiaz^uc reextraction and/or reanalysis shall be flagged
      by4f3te Laboratory.  Use;, Region  will evaluate  the noncompliant samples
      and may specify that t&ese be reanalyzed as additional paid samples.
      Sample'"Te«ttlts shall JM& reported on Forms QI-PEST and QVI-PEST.
      Reporting %fe4uiremeHis are listed  in Exhibit  B.
                  !,',',",    v
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                                                                          DRAFT

                                   SECTION V

              SAMPLE QUALITY CONTROL PROCEDURES  AND REQUIREMENTS
25    Method Blank Analysis                                ,

25.1  Summary - A method blank  for water  samples  is 100 mL of-reagent water
      spiked with the SMC and carried  through the entire analytical .scheme.  A
      method blank for soil/solid samples is  6 g  of clean quartz sand spiked
      with the SMC and carried  through the enffire analytical scheme, '^method
      blank for oil samples  is  1  g of  clean*sorn  oil spiked with the SMC and
      carried through the entire  analytics,!- ischeme.   Met&pd blanks shall be
      carried through the entire  analytical^procedure/ ;

      NOTE: The Agency will  provide  the Labor£tg|ry .iriith further instructions
            for the analysis of method blanks for wipe samples.

25.2  Frequency

      A method blank analysis shJllixbej^ei^omed  for each matrix type (water,
      soil/solid, or oil) and with leach se'te^ofciSmriipILes.,  A set of samples is
      defined as those samples  from^oiae Batch t^psEt""are. Extracted and analyzed
      on one instrument during  a  24-M«ar  analytical sequence.
                                      ' ",>.",  ,'•",%
      25.2.1      The method blank and aptl ^sociated samples  shall be
                  analyzed in the same analfrtical sequence.  If samples from a
                  batch :am  analyzed in more  than one analytical sequence, the
                  associated metliod  blank must: also be analyzed in the same
                  analytical sequence.  If a  method blank extract is used up
                  because of multljjle  analyses, the Laboratory shall
                  -Substitute an ,ia^.t^a(ie^t.f!blank  in place of a method blank in
                  alt s^sequentivssalia-lpitllajalslisequences.  The Laboratory shall
                  note:4lh|{&;3in  the Batch  Narrative and shall use the EPA
                  identiffeatlpii  number as described in Exhibit B for this
                  instrument %|iank.
      25 .2^L ~~v'''" An-"iaGp^^able method blank shall  be analyzed before running
                  any samples within an  analytical  sequence.
                  When analysing highly  contaminated samples using SFE disks
                  on more tha$ one manifold,  the  Laboratory should analyze one
                  method blanJc per extraction manifold.   If an unacceptable
                  method blarik is analyzed and  the contamination can be
                  isolated,Ja»;'a particular manifold,  only samples extracted on
                  -libat maxt|£bld will have  to  be reextracted.  If an
                  unaccepjfcable method blank is  analyzed and only one method
                  blanfef'fi used, all samples  from all manifolds shall be
                  reextracted  at no additional  expense to the Agency.
                                  D-52-PEST-Q                          08/23/94

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                                                                          DRAFT

      25.2.4      Criteria for an acceptable method blank is defined in
                  paragraph 25.4.

      25.2.5      If all field samples  in a Batch  are filtered,  the associated
                  method blank shall also be filtered**  If only a partial set
                  of samples in  a Batch are filtered,'t3ben a separate method
                  blank shall be run through the filter,Extracted, and
                  analyzed.                                  '=   ?,

25.3  Procedure for Method Blank Preparation

      25.3.1      Prepare the method blanks^at  the frequency listed in
                  paragraph 25.2.          :

      25.3.2      Measure out 100 mL of reagent water'•?£or each water method
                  blank sample aliquot.      !-   *    ;i

      25.3.3      Soil/solid method blanks are  6 g ofiselean quartz sand.
                                                         f\.
      25.3.4      Prepare water  and.*soil/solid  method blanks as described in
                  paragraph 14 ar; 15 depending  on  whether solvent or solid
                  phase extractions utilized*,^'  ",-; ,;J-:

      25.3.5      Spike 1.0 g of corn soil witsK  1.0 mL of SMC (0.5 /jg/mL) and
                  proceed with the pestlfcides>';procedure (paragraphs 16.3 -
                  16.5).                :; ...
                                           <\
      25.3.6      Analyze, theypethod blank extracts.   Calculate the results
                  accojr&ilig tcr ;p|ragraph 21. jl
                    , :-|='          ';),,;
25.4  Technical Acceptance Criteria,
      25.4.1      A'ij.;attethod bli&Efl^iS%a3||rlP' analyzed within an acceptable
                  analytical sequence on a  GC system meeting the initial
                  three-pbiiifeucalibration criteria (paragraph 8) or valid
                  calibratioiklsefeeck criteria (paragraph 9),  and the PVS
             ;si, ;  :«cceptance criteria  (paragraph  10).

                  The SMtfciecovery criteria of 50-150 percent is advisory
                  only.  T^ifjsSMC recovery in the  method blank must, however,
                  be greatefcsjshan or equal  to 20  percent and less than or
                  equal to 2W> percent.

                  The RTS fdc%the SMC in the method blank must be within ±1.0
               :l .percent bebween the blank SMC RT and the mean SMC RT
                =!  calculated 'from the initial calibration.
                     "
      25.4.4      The'•sisirget  compounds  or  potential  interferences in the
                  method blanks must have  a response less than one-half the
                                  D-53-PEST-Q                          08/23/94

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                                                                          DRAFT

                  response  in the  corresponding RRT window of the initial
                  calibration low  concentration standards .

      25.4.5      A method  blank may contain a detectable but acceptable
                  concentration of a target compound (less than one -half the
                  response  of the  initial calibration j&tm , concentration
                  standard) .                       ; -    "  ••<

      25.4.6      If all  criteria  are satisfied, the method blank: analysis is
                  acceptable  and samples may be^analyzed.  If the-iae&iod blank
                  is unacceptable,  correctivepasction shall be taken and;, :an
                  acceptable  method blank most be analyzed prior to analyzing
                  the associated samples .  vf           • '  '•

25.5  Corrective Action                   '^V ' .' ,      , •'-'

      25.5.1      If a method blank does not meet the technical acceptance
                  criteria, the Contractor shall consider the analytical
                  system  to be out of control.  It is tile Contractor's
                  responsibility ^?,,eliminate method interferences caused by
                  contaminants ii'jSoJfwfepts, i/^eagents , cartridges, disks,
                  glassware,  and other sample jEtoragevand processing hardware
                  that lead to discrete artifa£$b smM/ot,. elevated baselines in
                  gas chromatograms . | If contamination is a problem, the
                  Contractor  shall investigate* the source of the
                  contamination, and appropriate corrective measures shall be
                  taken and documented before further sample analysis
                  proceed^ i
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                                                                           DRAFT

                   perform corrective action which may include a new  initial
                   calibration.  DO NOT continue with sample analyses until the
                   SMC RTS is within ± 1.0 percent.

       25.5.6      Any samples processed with a method.blank that is  out  of
                   control (i.e., does not meet any >sof K3je, .technical  acceptance
                   criteria)  shall be reextracted and/ or reanalyzed at no
                   additional expense to the Agency.

25.6   Documentation                           i                     >

       Method blank results are reported on Borms QI-PEST and QVI-PEST.
       Reporting requirements are listed in- Ixhibit B.  j

26     Instrument Blank Analysis

26.1   Summary
                                                     ' '^ t
       An instrument blank is 1 mL of hexane spiked with5tO;^tL of SMC  (5.0
       fig/mL) .   At least two  acceptable instrument blanks sfeall be analyzed
       within an analytical sequej^^^fKb^fo^ sample analyses and  one
       following sample analyses.  /]'    "   ''S-?£>;,J   -  ,-,, !;

26.2   Frequency                     -;;       ?,• "-'
                                              s
       An instrument blank shall be analyze4,?at least twice during the
       analytical sequence to ensure that tibe instrument is free from potential
       contaminants.   The ^ates^nstrument &l«nk analysis shall be performed
       after  the initial|l±tree-^int calibratlfsn in the initial calibration
       analytical seq^B^ce or as 'fee first analysis in a daily calibration
       check  analytical sequence; f&be second instrument blank analysis shall be
       performed immediately  befo^w',t|:hewPVS analysis.  The Laboratory  is
       encouraged ta ij»^additigi^-§|ji^p^p^at blanks during the analytical
       sequence,  especraJ3,^,,when highly contaminated  or complex samples are
       analyzed.   Instrumehi;Jbul«anks must be analyzed  after analysis of samples
      with high levels of target: compounds or interferents (see paragraph
       26.5.6),. •£„,••   ..t       ^>;:.
26.3  Procedure for InslTBttisajent  Blank preparation
        •• , <•  .--               •*:*>••!•. ,-.         *   *•
        ;s/ '"
        ^Instrument blank  iV4l mL of hexane spiked with 10 uL of SMC (5.0
     m
      i-; :•£
26.4
      Concentract,iei«5,, of tb^ :=SMC  and any target compounds in the instrument
      blank are cai«pat^4? according to the procedures described in paragraph
      21.  Note: The tsiilget  compound concentrations (detected concentrations
      and CRQL values) in the  instrument blank shall be reported in the
                                  D-55-PEST-Q                          08/23/94

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                                                                           DRAFT

      appropriate concentration units (e.g.,  report in /tg/L if the associated
      samples are water and  in ^g/Kg if the  associated samples are soil).

26.5  Technical Acceptance Criteria

      26.5.1      A minimum  of two  (2)  instrument blariksrshall be analyzed
                  during an  analytical  sequence on &- GC system meeting  the
                  initial three-point calibration criteria (paragraph 8)  or
                  valid calibration  check criteria (paragraph 9)/-'and the PVS
                  acceptance criteria (paragrajiit 10).              ''"-',

      26.5.2      The SMC RT in the  instrument blank must be within ±1.0
                  percent of the mean SMC R1S calculatecMsErom the initial
                  calibration.             : ,           ^

      26.5.3      The SMC recovery criterion 6^y50-3i50 percent is advisory
                  only.  The SMC recovery in the "ttnstxument blank must,
                  however, be greater than or equal'•%<> 2:0, percent and less
                  than or equal to 200  percent.         , ';-
                                  s^ ,
      26.5.4      The target compj£»mits,w 'fjoteqtial interferences in the  first
                  instrument blank (analyzid iameldiately.j after the initial
                  calibration or before a valii-calibration check) must have  a
                  response less than *ase-half, iSae response in the
                  corresponding RRT  windows &£'"the initial calibration  low
                  level standards.        % ""';

      26.5.5      Subseqo^t juxstrument blaafess are acceptable with low  level
                  contamination.fiiThese installment blanks may contain target
                  cong«*und conceiteations up  'tio/rtwice the CRQL (2x CRQL).

      26.5.6      Ifotjiowing  the i&^.ys,ts,,,of,,ra.,field sample containing high
                  i _±-»_ _^  .—j-^.i||3»an the field samples run after a high level
               iA-  •'•:^ssjy\j^ must be'-iftijiiefully evaluated for carryover.  The field
           /H'•'•""' sampiie immediately proceeding the high level sample  shall be
         -:k~;J     reanalyi^ifed, along with any other samples analyzed after the
        #, '5-'        high levelltsample which shows evidence of carryover.

        ,5.7      High level ispunples are defined as being field samples that
        ,'-|k=,       contain  ta^gjet compounds at concentration levels that exceed
         ^'i-ii' ;,   twice the li|gh level initial calibration standard
            ^ ,|  ;,;,, concentratltlm and/or interf erents that are detected  at
                4*l>esyels greater than  the mid level initial calibration
                                response of the nearest target compound.
                                  D-56-PEST-Q                           08/23/94

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                                                                          DRAFT

26.6  Corrective Action

      26.6.1      All groups of samples  analyzed shall.be bracketed with two
                  acceptable instrument  blanks.   If ellfher instrument blank is
                  unacceptable, corrective  action shall be taken and all
                  samples not bracketed  by  two valid 'iastxument blanks shall
                  be reanalyzed at no  additional expense to t£ie Agency. ,

      26.6.2      If the response of any target  compound in an instrument
                  blank analyzed after the  initial calibration or "before a
                  valid calibration check statidard is greater than or^tequal to
                  one-half the response  in  £he corresponding RRT window of the
                  initial calibration  low ,e0ncentratiou!:ist:andard, corrective
                  action shall be performed and  the system shall be
                  demonstrated to be clean  by  'the analysis of additional
                  instrument blanks until all'itsEtget Compounds are within QC
                  limits.                         i\-

      26.6.3      If any target compound in an instrumetifc'lalank analyzed after
                  field/QC sample analyses  is  greater than Cwo times the CRQL,
                  another instrum%nt|bliatac;;shall be analyzed.   If on
                  reanalysis, coniaminationsscili exceeds criterion,
                  corrective action jslhall be psjblEorme&jifed the system
                  demonstrated to be iclean.  then,  all associated field/QC
                  samples analyzed since the: .last valid instrument blank or
                  method blank which contain those target compounds or
                  interferents found in  ttofc instrument blank shall be rerun.

      26.6.4      If an^'Sinstru&sat blank (otSktr  than the first instrument
                  blank in the analytical sequence)  contains target compounds
                  ojr,-"3Lnterferents:%etween one-Half response and two times the
                  CRQL,  all posijfepre results, (results greater than or equal to
                  the CRQL) for-ailifeie scoapotmds  in samples analyzed after the
                  last; ••^lld instrument  blank  shall be flagged with a "B".

      26.6.5      Flag all ii^tanaoent blank results "S"  if the instrument
                        SMC does*»psC£t .meet the  advisory recovery of 50-150
                  If the iiSsf$rument blank SMC recovery  is  less  than 20
                  percent, gif»ater than 200 percent,  or if peak interferences
                  are presen^ sample analyses shall  be stopped,  corrective
                  action performed, and another instrument blank shall be
                  analyzed. ,f!;if the SMC RTS is still  outside  the criterion
                 .upon reaniptysis, corrective action  which may  include a new
                 > -1jaitiaL;!ejalibration shall be performed.   All  samples
                 '&i!a3|rz^9,>J5ince the last valid method  or  instrument blank
                  shall.: 1*1 reanalyzed after a valid instrument  blank has been
                  demonstrated.
                                  D-57-PEST-Q                          08/23/94

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                                                                          DRAFT

      26.6.7      If the SMC RTS criterion is not met  for  an instrument blank,
                  sample analyses shall be stopped and another  instrument
                  blank shall be analyzed.   If the SMC RTS criterion is still
                  out on reanalysis , corrective action -which may  include a new
                  initial calibration shall be perforated.   DO NOT continue
                  with sample analyses until the RTS is *ithin  ±1.0 percent.

      26.6.8      Any samples not bracketed by valid instumeiit ^blanks or a
                  valid instrument blank  and a method  blank shaHqbe
                  reanalyzed at no additional expense  to the Agency,' -r

26 . 7  Documentation                         ,jf

      Instrument blank results are report^ ,pn Forms Qt^PEST and  QVI-PEST.
      Reporting requirements are listed ins!pihibit Ek,

27    Laboratory Control Samples                    > ,

27.1  Summary                                           !.

      The QTM pesticides LCS mix-|iapii;,ite£lt3^|:l.y .will be supplied to contractors
      by the Agency.  The LCS mixtiire wili^I'm^iift^Eget  compounds at several
      known concentrations .  The Laboratory shall spSfce Sthe LCS mixture into a
      clean matrix that is similar toS'fche samples being analyzed.   The spiked
      matrix shall be prepared and analyzed,, -iadsing the  procedures  described for
      field samples .  Analysis of the ICS atll! assess  the  performance of the
      analytical system prior to analyzingJJfield samples.
                          '
                         ,
      NOTE : The Agency 'rtjS.I'i prosrjjpde the  Labd^^tory with  further  instructions
            for the ^a&lysis of t&s for wipe%samples .
27.2  Frequency
      An LCS shall be analyzed once per matrix per analytical  sequence (24
      hours) per instrument;*?* The LCS shall be analyzed after the  first
      instrument blank in infey^l, calibration analytical sequence or after the
      method >l«t^£hi3» -the daily' H^'tifaxation analytical  sequence.
                  '  '
                          _

      27 .2i3i      An LCS-^feill be analyzed with  each:
        ,^= i?
       -. if !
                               water field samples  (LCS  prepared from reagent
                               soil/solid field samples  (LCS  prepared with
                        quaf*pz sand);  and

                        SJBt of oily  field samples  (LCS prepared with corn
                                  D-58-PEST-Q                          08/23/94

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                                                                            DRAFT

      27.2.2       The LCS shall be analyzed with all associated samples  in the
                   same analytical sequence.   If samples from a batch are
                   analyzed in more than one analytical -sequence, the
                   associated LCS shall be analyzed in >the same analytical
                   sequence.  If an LCS extract  is used; up because of multiple
                   analyses, the Laboratory shall use tibe 'original stock mix
                   diluted into hexane in place  of the original LCS sample in
                   all subsequent analytical sequences.   The Laboratory shall
                   prepare this solution by diluting 100 pL of ^dhfetLCS standard
                   mixture into 5 mL of hexane ^asd concentrating to 3. mL using
                   nitrogen blowdown.  The LabCQSatory shall note this ^tiy the
                   Batch Narrative and shall ssltse the EPA identification number
                   as  described in Exhibit B&or this LQS•,solution.
27.3  Procedure
      Spike the appropriate matrix with the LCS  Sljssaiard mixture and prepare
      as follows:

      27.3.1      Water LCS      ,;, , ;
                                 f>,>*:i"A ,3 „..-'( :,::\--~  .
            27.3.1.1     Allow the^S mixti3O-«"Jf^tlfs r to, reach room
                         temperaturfe'Sbefore opening. '''-The!' -ampules must not be
                         opened until;;ipr;eparat:S!i»n/analysis is to occur.
                         Exercise care     perform tfeie spiking to -ensure accuracy.  Add the SMC
                         and mix 4&4. ?ar.|y .T-^1;011^^  t*ie extraction and clean-up
                  "-v  ^^>rocess,Miga^b5l»^t^a.;"in paragraph 14 or 15, depending
                       >-^m- .whether solvent or solid phase extraction is
                         u£i!J£zed.  Proceed with the analysis as described in
                         paragippfo 19 .
                V- '-',% '           *''<-,*.£? f*
               '-' '  "*{~;  '            ' >';^- ^^
            -El?v'3.!l":3  , - ,;'^c«Einal aqu%ot
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                                                                     DRAFT

27.3.2       Soil LCS

      27.3.2.1    Allow the LCS mixture ampules to reach room
                  temperature before opening.  JEhe ampules must not be
                  opened until preparation/analysis is to occur.
                  Exercise  care in breaking the aa|jules open to avoid
                  injury.                     /

      27.3.2.2    Spike 6 g of quartz sand with 100 ^L o£Jt&e LCS
                  standard  mixture as described in the instructions
                  provided  with the LCS 'mixtures .   Use syringes^tro
                  perform the sp iking. -Vbo' ensure accuracy.  Add the  SMC
                  and mix and carry --^fcrough the esttxaction and clean-up
                  process as described in paragraph 14.  Proceed with
                  the analysis as described injparagraph 19 .

      27 . 3 . 2 . 3    Nominal LCS target compound 'concentrations are as
                  follows :                     ;  .

                  alpha - BHC ,,,  ,           41.7 /ig/Kg
                  ganmia-BBgb?i  &, •,-£••-.•„   31.7 fig/Kg
                  Heptachlo%    '" * ' x< 4  ? f .7' j|g/XS
                  gamma -chlor&ane       4 -AO.O '
                  alpha -chlordaiae       ;'   5.0
                  4, 4' -DDE      "     c ;•   5.0 Mg/Kg
                  4,4'-DDD             !    31.7
                  Endrin aldehyde '        30.0
                              sulfate i ,   36.7 fig/Kg
                                        -\   5.0 jig/Kg
              {.,*•'"         "-f           M ,
27.3.3       Oil-'LCS         -4,

This section haspHJt  been};<^B8iib^$«d£^he LCS conposition and
concentrations for oils are currently being investigated.
      27.3.3.1    Allow JtsbfifeLCS mixture ampules to reach room
        _..,;;.  .;-,;  , , temperat^p&siiefore opening.  The ampules must not be
      v- '.,-'•"-- '-":;  4'. ;;i^p,ened unti^preparation/analysis is to occur.
                      Ecise care in breaking the ampules open to avoid
      27.3.3.2     Spilapl g of corn oil with 1 mL of the LCS standard
                           as described in the instructions provided with
                           mixtures.  Use syringes to perform the  spiking
                        sure accuracy.  Mix and carry through the
                       action and cleanup process adding 1.0 mL of SMC
                    |»5 jig/mL) and hexane and further prepare as
                    ascribed in paragraphs 16.3 to 16.5.
                            D-60-PEST-Q                          08/23/94

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                                                                           DRAFT
            27 . 3 . 3 . 3    Nominal LCS target compound concentrations  are as
                         follows :
                         alpha-BHC               2500
                         gamma - BHC               1900 gg/Kg
                         Heptachlor               400 ii&f&g
                         gamma -chlordane         240(0 (Jg/J£g
                         alpha -chlordane          300 /*g/Kg
                         4, 4 '-DDE                 300 fig/Kg
                         4,4' -ODD              .; 1900 MS/Kg
                         Endrin aldehyde     ? =• 1800 jig/Kg
                         Endosulfan sulfate  »-;   2200 jjg/Kg
                         Endrin ketone       >     300
27.4  Technical Acceptance Criteria         ' : ,      ..:•

      27 .U.I      All LCS compounds must have recoveries between  30 and 130
                  percent.  Up to two LCS compounds *Bay;, however,  exceed the
                  upper recovery criterion of 130 percent,,

      27.4.2      All LCS target,%oapou«^,r!abs,o,lute and relative retention
                  times must be v^ithin the Windows s established during  the
                  • initial calibration.        ,  ;;   ' •' '", ;-,

      27.4.3      The RT of the SMC must be, within ±1.0 percent  of the mean
                  RT of the SMC established during the initial calibration.

      27.4.4      The SMC; a<<$vi«Gry recovery criterion is 50-150 percent.   The
                  SKC recovery' ^!£, ;the LCS musst,  however, be greater than or
                  equal to 20 petcent and les£, than or equal to 200 percent.

27.5  Corrective Action
      27.5.1       If anyjIsCS compound recovery is less than 30 percent  or more
                   than twoQlip^ compounds exceed 130 percent, the LCS  shall be
                   reanalyzed?*c If upon reanalysis, more than two LCS  target
              s!  -';•" compounds  are 4rtjifcside the recovery criterion, the LCS and
             ::,..'!•-  alTsMSsSeciated fl^lsi and QC samples shall be reextracted and
         /=>        reanal^alesd.  If one or two LCS compounds are outside the
         •• "-..               f - , ;
       /, i/         recovery'i^fraterion,  proceed with sample analyses, and flag
      ,;?"           all samplelar-esults of compounds that were out in the  LCS
      "£;'           with an "ifrfflag.
     •-IT---V                   ?'-'
      27."Sk'2;r ;     If the SMGfTecovery is less than 20 percent, greater  than
            " :, X,  200 percent,  or if peak interferences are present in  the
                        sample  analyses shall be stopped and the LCS
                          :ed.   If the LCS SMC recovery is still outside the
                   criterion  upon reanalysis, corrective action shall  be
                   performed  and the  LCS and all associated samples shall be
                   reextracted  and reanalyzed.

                                  D-61-PEST-Q                         08/23/94

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                                                                          DRAFT

      27.5.3      If the RT or RRT for any LCS compound is not within the RT
                  and RRT windows established during the initial  calibration,
                  reanalyze the LCS.  If upon reanalysis ,a compound is still
                  outside the windows,  a new initial calibration  must be
                  performed before samples can be analyzed.  The  instrument
                  must be recalibrated as described-Iris paragraph  8.

      27.5.4      If the SMC RTS criterion is not met for tl»| £CS,  sample
                  analyses shall be stopped and the noneompliant  liCS
                  reanalyzed.  If the SMC RTS Jts still outside the^criterion
                  upon reanalysis, correctiveiaction which may include a new
                  initial calibration shall ie performed.  DO NOT proceed with
                  sample analyses until thelSMC RTS is s&rithin ± 1.0 percent.

      27.5.5      Any samples processed withl/an. LCS tfeftt is  out of  control
                  (i.e., does not meet any of^&x&z,tf'sStnical  acceptance
                  criteria) shall be reextracted>an3/or reanalyzed  at no
                  additional expense to the Agency. •• H -

27.6  Documentation
                                 \:'-«.t!-~ '<-}'.... i
      Laboratory Control Sample rlsi^ts" ar^'•feSpoBfced «aa ^"orrns QI-PEST, QII-
      PEST, and QVI-PEST.  Reporting 'requirements are lifted in Exhibit B.
                                  D-62-PEST-Q                          08/23/94

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                                                                    DRAFT
            COLUMN RESOLUTION CALCULATION
.a-
                                                 % Valley-x/y. 100
 8:3O
                   9:40
  B:5O
Time
                                                           tCfcOO
                               Figure 1
                             D-63-PEST-Q
                           08/23/94

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                                                            DRAFT
                     Table 1.

List of Pesticides  Compounds in Order of Elution*
                                      ,
    Compound                 Retention "T?inie (mins)

    alpha-BHC                        6.28
    beta-BHC                         6.98
    gamma-BHC (Lindane)         ,"    7.20
    delta-BHC                  :,;!    7.83
    Heptachlor                X      9.45
    Aldrin                  ,  ,:'     10.53  .
    Heptachlor epoxide              11.93
    gamma-Chlordane           ••••  ,   12.58
    Endosulfan I                 ,   12:97
    alpha-Chlordane                 13..08
    p,p'-DDE/Dieldrin**             13.82
    Endrin                          14.48  :
    Endosulfan II     .,             14.77
    p,p'-DDD      ',-•:. ;-:-,:   j^f ^ ... .  15.18
    Endrin aldehyde".:,      '  y'~' -., ^15.3B8, -
    Endosulfan sulfate          -   16.17  •
    p,p'-DDT                        16.43
    Endrin ketone             :; -    17.58
    Methoxychlor          ,-=  :,<      18.35
    Decachlorobiphenyl (SMC>        23.77
   *  This  elution'^efeder is giveim ,as general guidance and is
   based on suggeslfcefd instrumental operating conditions as
   given in paragraph. ,7.,

   **  DIffi,,aJad dieldrin coelute on  this  column.
           "; ! :f
   Column:   DB^5-,"S6egabore capillary column,  15  m x 0.53 mm I.D.
                    D-64-PEST-Q                          08/23/94

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                                                                    DRAFT
                              s            --  ,-.,
                      QUICK TWAROUND MgtfiOM

ANALYTICAL METHOD FOR POLYCHLORl^TED SIIHENYLS (PCBs)  AS AROCLORS
                             D-1-PCB-Q                           08/23/94

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                                                                          DRAFT

                               TABLE OF CONTENTS
                                PCBs  AS  AROCLORS

SECTION                                                                   Page

I     Introduction	D-3

II    Sample/Extract  Storage  and Turnaround Times
      and Equipment and Standards	:,	D-4

      1     Sample/Extract  Storage and  Turnaround Times	;";,. .D-4
      2     Summary of Method	,i	D-4
      3     Interferences	,,	D- 6
      4     Apparatus and Materials	»-.,[	D- 6
      5     Reagents	,..;	,-.,	D-12
      6     Standards	I.,.,. .v'.'	D-13

III   Instrument Quality Control Procedures  and Requirements	D-16

      7     Instrument Operating Conditions	D-16
      8     Calibration of  the  G^-$fjgg^|08i>T-,-Initial Calibration	D-16
      9     Calibration of  the  GC%£stem':-  GilXbaration Check	D-21
      10    Calibration of  the  GC System  -  PVS^'.V. .		D- 24
      11    System Performance  - GC 'l^solutioal	D-28

IV    Sample Analysis and Compound Identification and Quantitation	D-31

      12    Summary	,;,,,, »\ »	,'.	D-31
      13    Phase  Separation.'! 4<->	^	D-32
      14    Solvent Extraction  a^d*,,Cleanup. . .\,	D-32
      15    Solid  Phase Extractiora^and  Cleanup	D-39
      16    Samplejfreparation  ai|i|?,Extraction - Oil Samples	D-45
      17    Sample Preparation <|o^|||^^s^t:i^m - Wipe Samples	D-46
      18    Instrumental; Analysis	D-47
      19    Dilutions.. ... S.*	D-49
      20    Identification  of SNo^get Compounds	D-50
      21    Ca3asulatrions	 ,iii .»	D- 52
      22    ,|f^micki.Acceptance Cf!|iea:ia	D-55
      23  ; -Corrective Ac^on	D-55
      24<;   Documentation, y^i	D-56
V    JS«mple Quality  ControlflBrocedures  and Requirements	D-57
     n  *&,                    > '

      25"- v'lfe.thod  Blank Analysis	D-57
      26    *l$is*rument Blank^jAnalysis	D-60
      27    LaKoaasfcory Contfeol  Samples	D-63
                                   D-2-PCB-Q                           08/23/94

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                                                                     DRAFT

                              SECTION I

                            INTRODUCTION
 This  Quick Turnaround Method (QTM) is designe4'.':for mse  in determining
 the concentration of polychlorinated biphenyls: (PCBs) as  Aroclors  in
 water,  soil/solid,  oil, and wipe samples.  The method *e$oires  an
 experienced PCB analyst to determine if an Aroclor pattern jksusts,  then
 calculate the PCB concentration on the basis of a specific Atxscjsor.
 Exhibit C lists the Aroclor mixtures tbjtt will be used  as a basis' »f
 quantitation for this method along wit!r:±he Contract Required
 Quantitation Limits (CRQLs).  The method yields iltentification  and
 quantitation of the Aroclors listed '&&. Exhibit CUftsing  single column gas
 chromatography/electron capture deteefcorr,(GC/EJU) '•'.  Aroclor
 concentrations in samples are reported b&«& *2&- received" basis;  no
 dry weights are calculated.  The primary Defective of this QTM  is to
 provide analytical data in a timely manner for decision- making  during
 Site  Inspections,  remediations ,  and emergency reacriwUfc. activities.  The
 PCB QTM is to be used when rapid data turnaround is required, when the
 data  requestor knows of (ol^FtabwS^S^pa^fcts) the presence of  PCB
 contamination, and when there sis knowle18^^r|f^r4ing potential  matrix
 interferences at the site.  TKe QTM is n^fc -equivalent to,  nor a
 replacement for,  the CLP Organtcs Multi^fedia Multi -Concentration
 Analysis.                        '      :i " '•

 The method specifies the use of sulfairic acid and potassium permanganate
 to remove interferences,; hThe rigor otts cleanup significantly improves
 method  performances' for T*SBf. but makes 'like method unsuitable for the
 analysis of orgfbjochlorine pesticides. "fSulfuric acid/permanganate
 causes  significant degradation of heptachlor, heptachlor  epoxide,
 dieldrin,  en&pfai,  endrin ai^et^yde,, endosulfan I, endosulfan II, and
 endosulfan                   ' ~
The method  is  suitable i^for several multicomponent compounds, Aroclors
1016,  1221,  1232,  1242 ;' -.^4^,  1254, and 1260.  These compounds produce a
complex.fpa.f±i^ra of overlap^»^tg ,GC peaks; multicomponent compounds are
quantiatalle'd on ^^Jje: -basis of majfer peaks within these patterns.
Sucgiessful  use of  tlilif; method requires an experienced staff for data
review, because weatfii|fcing or environmental partitioning can alter
jWLJlbicomponent patternsplin samples.  This method can also be used for
ffbe analysis of toxaph(J|e if it  is added to the initial calibration.
lleipaajse of  the difficufjiy in measuring multicomponent pesticides,
tedh&jical chlordane  sh^«ld be analyzed by the QTM pesticide method where
the maj^jr,- , Components , ^ technical chlordane (alpha -chlordane, gamma-
                            are quantitated as separated compounds.
                             D-3-PCB-Q                           08/23/94

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                                                                          DRAFT

                                   SECTION II

                  SAMPLE/EXTRACT STORAGE AND TURNAROUND 2IHES
                                      AND
                            EQUIPMENT AND STANDARDS   ,:


1     Sample/Extract Storage  and Turnaround Times             , ;

1.1   Procedures for Sample Storage           ,  ,

      Samples shall be protected from  lights^d refrigerated at 4°C (+ 2°C)
      from the time of receipt until 60  days  after  delivery of a complete data
      package to the Agency.              ;;.,  :

1.2   Procedure for Sample Extract Storage   v- .;    /,;;

      Sample extracts shall be protected from light ^nd stored at 4°C (± 2°C)
      for 21 days after delivery of a  complete  data package to the Agency.

      Samples, sample extracts, an&.,stariiSard£-. shall he stored separately.

1.3   Contract Required Sample Turnaround Times5     ;
                                       ,
      Samples shall be extracted,  analyzed, «ad a  summary of the analytical
      and QC data shall be  reported to tfee>Aa|»propriate EPA Region via
      telecommunications network within  4#|fiours (or  72 hours if more than
      three fractions are ^analyzed)  of Vali|i3a,ted Time of Sample Receipt
      (VTSR) .  See Exhibits A ''wad^B for  specific instructions  concerning
      sample turnarounds time  and'Siata reportiafp requirements .
                    ':  •'           $**,
      Summary of Method          >i,
2.1   This analytical aetiiod is  a  GC/ECD  method for  the analysis of Aroclors
      and toxaphene in wat«r> ^soil/solid,  oil,  and wipe samples.  All target
      compounds and the  SystestClfQnitor  Compound (SMC)  shall be extracted from
      field and j$G ^samples  utill&lijg,, either solvent  or solid phase extraction
              fiiriiique^>,;':.lf  solvent*^jaraction is utilized,  field and QC
              are seriaIM>sfextracted using two 10 mL portions of hexane (for
                         •'(.y- "•"•? s
            samples) or  hexane/acetone  (for soil samples).   If SPE is
         lized, field and Q<3i|sainples are  eluted through a disk containing a
            matrix (e.g. silfpa) coated with a chemically bonded Cg or C^g
              phase (or  equi^fiilent) .  The target compounds and SMC are then
                  the extrac^on disk with hexane.
           '-•fc -- i
2.2   Sample ani&jrses  shail^fae performed using gas  chromatographic techniques
      and shall be coBducftfeti within a contract-specified analytical sequence
      that shall not''esas^ed 24 hours.   PCBs are identified and quantitated as
      Aroclors on the  basis of retention time windows and calibration factors
      established during initial calibration.  During initial calibration,

                                   D-4-PCB-Q                           08/23/94

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                                                                          DRAFT

      relative  retention times (RRTs),  retention times (RTs), and
      identification windows (± 0.005 RRT unit of the RRT or ± 1.0 percent of
      the RT) are  established for each quantitation peak for each low
      concentration Aroclor standard.

2.3   Initial calibration consists of a single low.level, -.standard analysis of
      target Aroclors and toxaphene except Arocloxss 1016 ~eej&, 1260 which will
      be combined.   A three-point calibration will^be perform4d-..with the
      1016/1260 mixture  to assess instrument linearity.  Mean calibration
      factors and  percent relative standard deviations (%RSD) shall %e t
      calculated for the calibration factors,^ all 1016/1260 quantitsalkon
      peaks.  The  %RSD of the calibration faefcors for each quantitation peak
      and the SMC  must be less than or equal: to 25.0 parc«nt.

2.4   A check of the initial calibration shall be performed no less than every
      24 hours, using the mid level concentratm«n offv&roclor 1016/1260 and
      SMC.  Calibration  factors calculated from each .quantitation peak and the
      SMC from  this  calibration check standard must"4fee'within ±35.0 percent
      of the mean  calibration factors established for each quantitation peak
      during initial calibration.. .^.Identification windows sfiall also be
      confirmed during the calibs»ti.06a\i^teck»:,,.

2.5   An analytical  sequence also includes method blanks and instrument blanks
      in which  no  quantitation peak earn be observed at concentrations greater
      than one-half  the  response in the corresponding RRT window of the
    .  initial calibration low concentration ^standard.  The analytical sequence
      shall also include the analysis of "laboratory Control Samples (LCS) and
      Performance  Verification Standards (ff;SJ .   The LCS will be a "go/no-go"
      analysis.  Thatfis,/ if feheJIL.CS meets performance criteria as stated in
      paragraph 27,  staple analyses, may procee4.   If, however, the LCS does
      not meet  acceptance criteria,, corrective -action must be taken before
      sample analyses, are perforaed,., ,,The ,PVS  is  two times the concentration
      of the low Iev^-4j016/126fl^aagw*5«cfe|,'s and  standarJgS,.   The SMC is used as  a retention time marker to
              :e RRTs  for tBap^identification of quantitation peaks and to
      assess extraction  efficiency.   When the  recovery of the SMC in a field
     IS^mple is less  than 10,>|iercent,  greater  than 200 percent,  or if peak
     '"1irt%xferences  are  present,  absolute retention times are used for
      qua^l^tation peak  ideafpf ication.   The SMC  recovery criterion of 50-150
      perceftfcj||&-!advisory $lil*y.   Reanalyses of samples are not performed if
      the SMC rewe^ry is,<^ttside the advisory recovery limts.
                 ''•!.?•/'-,   • «'
                                   D-5-PCB-Q                           08/23/94

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                                                                          DRAFT
3.1
3.2
3.3
4.1
Interferences

A variety of chemicals  extracted  from environmental and waste samples
will produce ECD response  and thus  complicate the interpretation of
Aroclor patterns.  Chemicals  such as  chlorophenols,  organophosphorus
pesticides, aldrin,  dieldrin,  endosulfan (I aaadTslI-),  and endosulfan
sulfate, which are normal  PCB interferences aaee removed by the sulfuric
acid/permanganate cleanup  in  this method.   Other organoeblorine
pesticides, particularly,  DDT,  ODD, and DDE should be removed by the
Florisil cartridge procedure.   Chlorina£e",

Phthalate esters are common interfexefets encountered in PCB analyses.
Phthalate interferences may be minimtZiep^by ttoe^.iise of pesticide grade
or ultrapure reagents,  thorough cleanup:'geli: ;glaeisware,  and avoidance of
plastics materials in lab  operations.   The Isafeoratory shall use proper
caution to control phthalate  contamination. ''•'-••'
, .demonstrated to be frefei'from contamination
                 method blanks.   Cross-
                           instrument  blanks
                      or other interferents
The analytical system must
under conditions of  the  a:
contamination problems sha
after samples with high
(see paragraph 26).

Apparatus and Materials          ';':  : ^

Brand names, suppliers^;  and part nunfeeips are for illustrative purposes
only.  No endorsement isxljpiied.   Equivalent performance may be
achieved using|a|>paratus al^materials'giiier than those specified here;
however, demonstration of e|^tivalent performance meeting the
requirements/of this SOW i^Mhe^r^sjjqnsibility of the Contractor.
            ^    '           "*'.lgX'<':'>^£'241 '' -"«;>•" '•~'"ify *••* >'
             '•-.!•.,i-       K 4m9.*~^3i^;in:E•
Gas Chromatograp*h; «)>, The gas  chromatography (GC) system shall be
capable of temperatti£eLf«:ogramming  and flow control that is stable
throughout an analyticalJj|s^quence.   The  system shall be suitable for
splitles»s;«f on-,column inj^tion and have all required accessories,
inclutltiig' ifyriBg^s-i,-,analyticSir®olumns,  and gases.   All GC carrier gas
linelsr-Sshall be consifeutcted  from stainless steel or copper tubing.  Non-
pall^tetrafluoroethyifei^  (PTFE) thread sealants, or flow controllers with
rt&ber components shalltinot be used.
            Gas Chromatograp^ Column -   15 m x 0.53 mm ID bonded phase
                    !-coated/|Siised silica capillary column (J&W DB:608, or DB-
                  Restek,  ofeiaequivalent)  is preferred,  but a methyl silicone
                      .g. S^gtelco  SPB-5,  J&W DB-5,  Restec, or equivalent) may
            be substituted.  A film thickness of 0.25 to 1.0 ftm is
            recommeni
                                                                       08/23/94
      NOTE:  The  use  of a guard column is recommended.

                             D-6-PCB-Q

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                                                                           DRAFT

      4.1.2 Chromatography Detector -  The GC shall be equipped with an
            electron capture  detector  (BCD) .

      4.1.3 Gas Chromatography Injector - Cold (ambient) on-column injectors
            that allow  injection directly into 0.53 mm, ID column may be used
            for this method as long as peaks are gauss ian, retention times
            stable, and calibration check criteria 'tare
4.2   Data System  -  The GC  shall  be  linked to a data system capable of
      integrating  peak areas for any  compound detected at or above one-half
      the CRQL.  It is required that  the Laboratory be equipped with a^PC- or
      microcomputer-based GC data  collection and reduction system for this
      purpose.  The Laboratory shall  posses^ this equipment to provide the
      quick turnaround of electronic  data,,, -'The Laboratory shall also be
      equipped with a microcomputer and contract specified hardware and
      software to  electronically transfer the QSIM data to the Regions.

4.3   Solid Phase  Extraction Processing Station - As SEE is a developing area
      in environmental chemistry,  the EPA expects that Advances will occur
      within the lifetime of the QTM  contracts .   Therefore:, ; the brand names
      listed below are included ^cac',s'I^U%|ara;tipn purposes only.  Any
      comparable equipment is acc'eptableY^^arcftess, of. . brand.
                                    t          \>f- \  "•', " ?- ' ';f'

                                      :i       ' '
      4.3.1 Extraction disks -  Disks  sfeall bfc made of Teflon and contain at
            least  500 mg of  C^g bonded silica (Varian/3M Empore", or
            equivalent).  Disks shall be :'47 ;mm in diameter.  (Note: an
            alternative |»basS«B1»ay  be  used if .this phase can be demonstrated to
            meet the QA/QC '"reqmiSsements of tfcds  method.)
      4.3.2 Vacuum feeptder  - The vaeuum holder will be glass and comprised of
            five (3) ,J>arts : the •^seuum head,  the sample reservoir, a metal
            clip to-SlgLd the res§r^rol|r -tsp "*fie head, a large volume receiver
            (greater tfcaa ,2,00 mL) for  the sample after elution, and a small
            volume receives* ;:,,i£its onto ttm^acuum head5.

      4,?:|l'3 Vacuum manifold \sflJA 4-6 port vacuum manifold may be used to
     d;l-;    facilitate simultaneous disk extractions.
                of depth fi^fekr  (Whatman Multigrade  GMF 150,  or equivalent) or
                  materials- -^ach as Celite  545  (diatomaceous  earth,  Baker #,
            or %sqila.valent^Laare encouraged when  samples contain particulates.
            If dep"t&":£i^,fcepfcs are utilized,  each lot  shall be  tested for
            contaminat^lpi /prior to use with this method.   The depth filters
            may be checked in conjunction with  the SPE disks  (depth filters
                                   D-7-PCB-Q                           08/23/94

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                                                                    DRAFT

      are placed on top of the  SPE disks) by  following the procedure
      outlined in paragraph 4.3.5.

4.3.5 Solid Phase Extraction  (SPE) Recovery Cheek

      4.3.5.1     Summary                       "

                  Before field  or QC  samples  are  extracted using the SPE
                  disks, their  efficiency shall be  verifi«S., f An
                  extraction  recovery anfl contamination checld shall be
                  performed in  order  to Devaluate  the  recovery df
                  compounds on  the disk,; and  to check for contamination.
                                      ;;•••          -;
      4.3.5.2     Frequency        :              !
                                   ''-  -C        '
                  A check shall be perfolbaed •&& each  individual lot of
                  disks, and  for every 300 tm|ts  of a particular lot.

      4.3.5.3     Procedure

                  4.3.5.3.1 "••-' j^eaafe Camples  are  extracted using a lot
                           '"?»; :of SPEsd£sfc;r   of reage*jt| water spiked with 1 mL of the
                {'         ~\  high initial calibration 1016/1260
                           I",;'1 standard  (to demonstrate adequate SPE
                 *• 4^3,5.3.2    The low and high SPE recovery check
                    :  '•'"•       standard solutions used to evaluate SPE
                        ,  '5'|,   disks  are prepared by diluting the
                          ;>st; ^original 1016/1260 stock calibration
                 "5  .-.,        "'^dilution in methanol.  The low and high
                    ;?          SPE recovery standard concentrations are
                     V|        equivalent to the low and high calibration
                      I        1016/1260 standard mix concentrations
                      ^"•'•i       respectively.   Laboratories shall prepare
                       ,.:,;       the SPE recovery check standards in
                      | f       methanol and add one mL of each 1016/1260
                     ,,,,        calibration solution to 100 mL of reagent
                    y •'         water.  If the Laboratory experiences
                               solubility problems in preparing the SPE
                               recovery check standard solution, the
                               Laboratory shall prepare the SPE recovery
                               check standards in methanol, add one mL of

                             D-8-PCB-Q                          08/23/94

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                                                               DRAFT

                          each calibration solution to 4 mL
                          methanol,  and add the resulting solution
                          to  100 mL of reagent; water. The recovery
                          check samples shall be prepared and
                          analyzed according;,-to the procedures in
                          Section IV.     '•:   "  .

             4.3.5.3.3    The SPE recovery check standard solutions
                          shall be analyzed in a valid vinitial
                          calibration ;or daily calibration
                          analytical sequence (see paragraph ;3.8.1).
                          Note: if-the SPE recovery check standards
                          are the ionly sample^ .analyzed in the
                          analytical sequences, the method blank
                          shall bW'&seplacedSwith an instrument blank
                          and the £6$  sl»2,l;be prepared by diluting
                          100 fiL of LCS ,^eck mixture into 5 mL of
                          hexane and concefecating to ImL using
                          nitrogen blowdown. "'"llbeJEPA identification
                                  for  standards as;;klescribed in
                                    .shall be used 'for the low and
                      " V;high '^PS''%s^Boi!rery
            '<        '"^
         4  'The reco^ry of the c&eek compounds spiked at the
         •tf   upper limp:  of  the calibration range must demonstrate
      ,,,. -:   recovery«elE,^3QsJJ,ft;,jpercent to establish that the SPE
         ••v'• floedia hSis^l^feiisapadtty to retain compounds at the
           ':?i3t|ji|*e,r end of the calibration range (i.e., no
             btfe^t^birough of target compounds is occurring) .   The
             recoveag^Jcheck  at the  low concentration level shall be
   <:JC;--.,\ ; v evaluate^|jo>!, ;-  "" ~"- ':.'J3uc$a levels ''!$&&'  does not  introduce method
:             "interferences.   If any compound recovery is less than
             SO^^ircent or greater  than 110 percent,  then that lot
             of dffisks shall  not be  used.
 4.3.5.5     Corrective Action
                   '
             If jt&s disks do not  exhibit acceptable recovery of any
             spiked compound at the low or high concentration
             J^rels, the entire lot shall not be used to extract
             Isamples, since the system cannot be demonstrated to be
             functioning at those levels.
                        D-9-PCB-Q                 •          08/23/94

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                                                                    DRAFT

      4.3.5.6     Documentation

                  All data  and related documentation for the SPE
                  recovery  check analysis  shall Ise maintained by the
                  Laboratory  during the term o-f ;'the contract and shall
                  be available to the  Agency .Surixig-.on- site laboratory
                  evaluations or if requested. ;by  the XPD or APO.

4.3.6 Extract Cleanup Cartridges - Florisil,  0.5  g solid' $hase glass
      extraction cartridges with stainless steel  or Teflon frits
      (Analytichem Florisil PR,  or equivalent) .   Bake the glass ilorisil
      cartridges at 140°C overnight te-activate (do not exceed 150°C).

      4.3.6.1     Florisil  Cartridge Check

                  Each lot number of Florisil -Cartridge must be tested
                  by the following procedure before the lot is used for
                  sample cleanup.   Add 1.0 mL 6€;the Aroclor 1016/1260
                  mid point calibration standard >ta»"the top of a
                  prewashedf^J. the ^aiiyi.ytlica3.! sequence ,  the method blank shall be
                 •:.ed  in Exhibit B shall be used for this
                  instilment blank and LCS.

                  Documentation

               ;  ..All data and related documentation for the florisil
                • j/asecovery check  analysis shall be maintained by the
                  Laboratory during the term of the contract and shall
                             D-10-PCB-Q                          08/23/94

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                                                                          DRAFT

                         be available to the Agency during on-site laboratory
                         evaluations or if requested by the TPO or APO.

4.4   Glassware  -  Sufficient glassware to meet contract requirements shall be
      reserved for exclusive use in support of this contract.

      4.4.1        Erlenmeyer Flasks - 125 mL.

      4.4.2        Beaker - 150 mL.                             !  ':

      4.4.3        Concentrator tubes - 10 mL.r

      4.4.4        Kimax concentrator tube (graduated) - 25 mL.

      4.4.5        Graduated test tubes - graiaiua,ted from 1 to 10 mL.

      4.4.6        Autosampler vials - appropriate for the GC system.

      4.4.7        Centrifuge tubes - 40 mL.            '

      4.4.8        Wide-mouth centr:ii«ge ;$afee&,,(optional).

      4.4.9        Powder funnel - 6vcn> <60°). .

      4.4.10       Pasteur Pipets.      ;     >-i

      4.4.11       20-mL screw-cap vials (fair sulfuric acid/permanganate
                   procedurel ;,;> •',              ;

      4.4.12       Si
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                                                                           DRAFT
      4.5.4       Microsyringe -  10-^L, 50-fiL, and 100-^tL.

      4.5.5       Spatula -  Stainless steel.

      4.5.6       Hot plate  stirrer.

      4.5.7       Teflon coated magnets.

      4.5.8       Glass  wool.                 ., -                    ,  ;,

      4.5.9       Vortex mixer .

      4.5.10      Whatman #42  filter  pape*.

      4.5.11      Whatman vacuum  holder.

      4.5.12      Nitrogen blowdown apparatus .

      4.5.13      Water  bath.     ;  . ,

5     Reagents                    ;••',      "'" '; "I   , -.   : , _
                                    >           ; .
5.1   Reagent water  - Reagent  water iss-;,.def ine4, .as water in which Aroclors or
      potentially interfering  compounds; do ise£ produce a signal greater than
      one -half the response  in the  corresjjosi&ing RRT window of the initial
      calibration low concentration standard.  Reagent water shall be
      generated by one of "tfeeifollowing methods .
                                   ,
      5.1.1 Reagent ^ter may be ^generated by* pas sing tap water through a
            carbon filter bed containing approximately 500 g of activated
            carbor*;,{$algon  Corp .:; 'ifeLl.tras.orb- 300, or equivalent).
                   -''"'•           -':. • "•£' " ;1, ;,; ' - - -.?
                     j   ,       .'»••••< ^ i i •>" ?-J\S ZS'-'*' '  f
      5.1.2 Reagent watsfer-aaay be generated using a water purification system
            (Millipore-O-FltiB with Organex Q cartridges, or equivalent).
      5.1.3 Rejageat water may be prepared by boiling for 15 minutes  then
          ^I>sift)"ling'-ci|>iit%minant-fr4fe !-inert gas through the water  for one hour
         /-jipwhile mainta'iafttllg the water temperature at 90°C.  While  still hot,
       ,{£,./  transfer the de^ssed water to a narrow-mouth screw- cap  bottle,
      ;|;J    seal with a TefUbtl- lined septum, and cap.

5.2  "^.I^ents - Hexane, mettottiol, acetone, and toluene.  Pesticide  quality,
      or
                  .
5.3   Sodium hydroxide soMtion (0.5 N) .
                   •~- '• ^.-'
5.4   Sulfuric acid  solistion (0.5 N) .

5.5   Concentrated sulfuric acid.

                                   D-12-PCB-Q                           08/23/94

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                                                                          DRAFT

5.6   Powdered Anhydrous Sodium sulfate.

5 . 7   Hexane/acetone  [ (50 : 50) (v/v) ] .

5.8   Potassium permanganate  (5 percent aqueous  solution).

5.9   5 : 100 methanol/water solution  (methanol  in water v/V) ,  ^

5.10  Corn oil.                                               " ••'.'••

6     Standards                                -'                       -  •'">

6.1   Stock Standard  Solutions
                                                      & >'
                                         ' ',            f- ~
      Stock solutions may be prepared f rom IpuSle  standard materials or
      purchased as certified solutions.  StandaJSd solutions  shall be prepared
      by dissolving pure standards in a suitable s^lyent in volumetric  flasks.
      When compound purity is assayed to be 96 percetst -^r greater, the  weight
      may be used without correction to calculate the  dtoCientration of  the
      stock standard.  Exhibit E, -Section V provides further  directions for
      preparing and verifying th^Vifftbgjd^p -j&f. .stock standard solutions.
6 . 3
6.2   Secondary Dilution Standards  :;          r

      6.2.1 Using stock standard solutions, ,|f&*epare  secondary dilution
            standards in hexane.         ,(";•"

      6.2.2 Secondary diiw^b^a:;standards shaitl be  stored at 4«C (± 2°C) with
            minimal head^pace anS^ichecked ff^jaently for signs of degradation
            or evaporation.  Theilikjprocedures'iaije  especially important just
            prior to preparing calibration  standards from them.
            NOTE: Standards shall linot*' fee .S^tored  in volumetric flasks,
            especially ^li^a they are prepared with solvents  with low boiling
            points.        ~?"-\
              single low ^^tcentration standard mixture  shall be prepared for
           ' each Aroclor an^g|toxaphene in hexane  as  specified in paragraph
            6.3.2.  A separa^, solution must be prepared for each
            multicomponent mficiEure with the exception  of Aroclors 1016 and
          > 1260, which shal| i^e combined.  The 1016/1260 mixture and the SMC
           f:s|iall also be pri^ared at three concentration levels,  the low
            concentration, jifS concentration at 5  times  the  low concentration,
            and '-t;b^, high oia^centration at 25-50 times  the low level.   The low
            conceritr^t^n-|si;andard, as specified  in  paragraph 6.3.2,  achieves
            the sample ^extract compound concentrations equivalent to  the
            sample compound CRQLs as listed in Exhibit C. The high
                                  D-13-PCB-Q                           08/23/94

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                                                                          DRAFT

            concentration level shall be near the upper end of the linear
            range .

      6.3.2 Low Concentration Multicomponent Calibration Solutions

      Multicomponent       Concentration       SMC    "           Concentration
      Standard               (ng/mL)                    '    -:        (ng/mL)

      Aroclor 1016/1260       100/100         Decachlorobiphenyl, ,      20.0

      Aroclor 1221            200            "Becachlorobiphenyl        20.0

      Aroclor 1232            100             DecachloEoMphenyl        20.0

      Aroclor 1242            100         -   ; /Decachlorobiphenyl        20.0

      Aroclor 1248            100             Decacfelorobiphenyl        20.0

      Aroclor 1254            100             Decachlorobiphenyl        20.0

      Toxaphene               500>;!   ,,, ;.  -   .Decachlorobiphenyl        20.0
                                   '    ~"   "' '
      6.3.3 All standards shall be stored at 4?£ (± 2°C)  in Teflon-sealed
            glass bottles.  Calibrations solutions shall be replaced after 6
            months, or sooner, if comparison -with check standards  indicates a
            problem.                       b

6.4   Calibration Check Standard/;

      The calibratiim^check is a -.daily one-point check of the Aroclor
      1016/1260 initial calibration^ ,, .The mid level Aroclor 1016/1260  standard
      used in the initial calihj&dfeexEis ";tfc#- calibration  check  standard.   The
      calibration check -slfcezulard shall be prepared in a volumetric flask and
      diluted to final volisae^ith hexane.
                             '"*":* , -
6 . 5   System Mcsaitar Compound
            '       ""  '  '         ' ''

                                  (SMC) is decachlorobiphenyl.  A stock
      so|^it€ion of the SMC ijiacetone shall be prepared as  described in
      ps|fcagraph 6.1, and a spiking solution at a concentration  of 2.0 jig/mL in
              shall be prepacefjl from the stock solution.   Each  field and QC
             must be spiked ^|th the SMC before analysis.   Water  samples (100
                be spiked w||tf 10 jiL of the SMC.  Soil/solid samples (6 g)
      shall "^jlssaked with,40- /iL of the SMC.  For oil analysis, prepare
      decachlofcfeiflienyl f.trla concentration of 0.2 jtg/mL and add  1.0 mL of
      this solutioni^al^ig-of oil sample (see Section IV.)  The SMC is
      employed to dete%t4Jshifts in retention time of eluting peaks.
      Additionally, the SMC will be used to monitor the  extraction efficiency.
                                  D-14-PCB-Q                           08/23/94

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                                                                          DRAFT

      Note: Reagent grade  acetone  shall be used to prepare the SMC stock and
      working solutions.   The  Laboratory shall ensure that the acetone used to
      prepare the SMC stock and working solutions is free of any
      contamination .

6.6   Performance Verification Standard             .  ,   \

      The Performance Verification Standard (PVS) shall be analyzed at least
      once during each analytical  sequence to assess system staibll^ty.  The
      PVS is two times the concentration of tip alow level Aroclor 3:t&l'6/1260
      initial calibration  standard.

6.7   Laboratory Control Sample

      Laboratory Control Samples  (LCS)  conrteaiifcfcing known amounts of Aroclors
      traceable to primary standards  will inl!t3^11y?lbe supplied by the Agency.
      Following receipt of these initial supplies-, liowever,  the Laboratory
      shall prepare its own LCS standards.   The LCS^s'&ail be spiked into a
      clean matrix and prepared using all steps of this^|fieotocol.   An
      appropriate amount of the LCS .shall be added to reageut water and
      analyzed with each Batch o^swafces-- sastpi^s.^  An appropriate amount of the
      LCS shall be added to clean "iffaartz skrii" .iapS 'analysed with each Batch of
      soil/solid samples.   An  appropriate amount of!'the,fI&j5erck "sHsKOfitaJJ^d solutions^jsecondary standard solutions,  and
         •:4 ^working stand^pc^ solutions  shall be stored at 4°C (± 2°C)  in
       3'i?' Teflon-lined s<§|pw-cap amber bottles (also see paragraph 6.3.3).

     J&I&.2  All standards shi||l be protected from light.

      6.&03..Samples, sample /extracts, and standards  shall be  stored
                                  D-15-PCB-Q                           08/23/94

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                                                                           DRAFT

                                  SECTION III


            INSTRUMENT QUALITY CONTROL PROCEDURES AND REQUIREMENTS


      Instrument Operating  Conditions

      The following are  the suggested  gas chromatographic analyti&al
      conditions.                             ^                     ,'•;

      Column:     J&W DB-1701,  DB-608  or DB-,5 (or equivalent), 15 m x 0.53 mm
                  ID, 0.25  to  1.0 (an film thickness fused silica capillary
                  column (FSCC).                      5  -
      Carrier Gas:
      Flow Rate:
      Injector Temperature:                    205«C
      Detector Temperature:                    300°C
      Initial Temperature:        ..,»,           140°C
      Initial Hold Time:         --|s>l; , -5:    -1 min
      Ramp Rate:                 '~&.      *' •'•
      Final Temperature:
      Final Hold Time:               <;
      * Cold  (ambient) on-column  injectoirs -!fcbat allow injection directly into
      0.53 mm ID column may be used for this method as long as peaks are
      gaussian, retention-*itimes^are stable,? and calibration criteria are met.

      NOTE: The typieal-:run time's&pader  these conditions is 25 minutes.  It may
      be necessary d& 'adjust GC c^pditions on individual instruments to
      optimize detection of ArocJ«!rstjpea.ks.   It may also be necessary to
      adjust  detectt)ir-capnditioni|i^|j<^t3^^e instrument sensitivity.

8     Calibration of the GC ."System -  Initial-Calibration

8.1   Summary -•• T.  :-              3 ,,„
      8. l^fJ-'-SPrior to ttie-ips^ilysis  of  samples and required blanks, each GC
       '4f;/ system must be^^Dltially  calibrated to ensure that the instrument
      J:v*   meets the minim^^performance requirements of the method.  The
     f^;"    initial calibrat^n is accomplished by analyzing the low level
     '* '-=1^-,  Aroclor and toxagllene  standards and the low, mid, and high level
        *^;$h4li be  used to establish the calibration factors used
            for Aroclor gaantitati-°11  an<^ to define the retention time windows
            for Aroclor identification.   Additionally, the low, mid, and high
            level 1016/1260 standards will be analyzed to assess instrument

                                   D-16-PCB-Q                          08/23/94

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                                                                          DRAFT

            linearity  and to  determine the mean SMC retention time for
            evaluating SMC retention time  shifts (RTS) during analyses.  All
            samples shall be  analyzed during the contract specified 24-hour
            analytical sequence.

      8.1.2 Aroclor identification shall be based on matching patterns of
            standards  with peaks  in samples and by RRT windows for 3-5 ,
            quantitation  peaks  for each Aroclor.  These RRT%iSdows will be
            established from  the  low level initial calibration &£jft*dards and
            must be used  in all field samples .wifaere the SMC recovelcy tis
            greater than  or equal to 10 percetit and less than or equal -to 200
            percent.                         ?
                                          ,'-if         /-•
      8.1.3 Aroclor identification shall ,b£Abased on gafttern recognition and
            the absolute  retention time windows established from the low level
            initial calibration standards  in^iail.fi^fl samples where the SMC
            recovery is less  than 10 percent,  greikt«ix than 200 percent, or if
            peak interferences  are present.         '"•••';

      8.1.4 Shifts in  the chromatojgraphic  peaks shall be evaluated by
            comparing  the RT  of €bfe.,^G;vfta.-all analyses with the mean RT of
            the SMC calculated  f roll th.e'i$l%$By&B -initial calibration
            standards.  The retention, time shJUSt'"is''r€f«cred to as RTS or
            RT %D (see paragraph  21.4il,).   Th£ltT of the SMC for field and QC
            sample analyses must  be witfein $3t:0 percent of the mean RT
            calculated from the 1016/126Q,;itiftial calibration standards.
8.2   Frequency
      8.2.1 An initiai-calibratilpishall be performed to  determine Aroclor
            patterns|l :RRT and RT Endows ,  calibration factors ,  and to assess
            instrument linear ity-lufiAjnew, initial  calibration is required
            wheneveT^jlciailibratioiiil^fe-^^^i^Srds  or  performance verification
            standards danzpt satisfy QC criteria.  A new  initial calibration
            is also requiiped'-whenever major instrument maintenance has been
            performed such asvcjegojLunm or detector  replacement.   An initial
            calibration must be performed  for  each GC and for each
                 '                 "       are used to perform these analyses.
                            '
            An analytical sequence is a contractually-defined sequence of GC
            analyses which c^psists of an initial  calibration or a valid
            calibration chec!^:: field samples, LCSs, method and instrument
            blanks, PVSs, an|>-'6ther QC samples run within a 24-hour period
           , j,s.ee paragraph l^Syfor the required sequence  of samples).
      8.2.3 Ana?iyMssof th«-'Initial calibration  shall begin with the injection
            of the^i^.lffrel 1016/1260 standard followed by  the mid level and
            low level''lpMf/1260 standards and the single  point  standards.
                                  D-17-PCB-Q                           08/23/94

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                                                                          DRAFT

      8.2.4 The analytical sequence concludes  with an acceptable analysis of
            an instrument blank and a PVS  (see paragraph 10) .

      8.2.5 Samples shall be analyzed only after meeting the technical
            acceptance criteria for the initial cali&ration or a valid
            calibration check standard.              ;   %,,

8.3   Procedure

      8.3.1 The GC system shall be set up  per,;tfee requirements of paragraph 7.

      8.3.2 Prepare calibration standard soiufrions containing the SMC and
            individual Aroclors using the  procedure lisced in paragraph 6.3.
                                         . > < •            *'"' *
      8.3.3 The calibration solutions shall -He,., equilibrated to ambient
            temperature before injection (app£O£i3iaJ|gly one hour).

      8.3.4 Inject between 1 and 5 /jL of each  calibration standard.  The same
            injection volume shall be used for all calibrations and field/QC
            sample analyses.     -s>c.

8.4   Calculations               "'; *-
      8.4.1 The quantitation of Toxap&ene  or,Jioclors  must be accomplished by
            comparing the heights or the areas  of three to five major peaks of
            the multicomponent compound iJiiatshe  sample  with the calibration
            factors for the same peaks established during the initial
            calibration ,,sequ*ia&e.  The following table lists the number of
            potential .^uantitatilon peaks f oEf-each Aroclor and Toxaphene.

            Aroc 1 or/%$xaphene    .^-           "~       No. of Potential
                   4,            ;,;1J ., .„„.,„,,,„..          Quantitation Peaks

            1016/1260 ^ \         ™"  ""  *  ""'                 5/5

            1221            'OV.,                            3



       |||i-' 1242         '' ^|.                                5

            1248            p'1                               5

               4           ;f;'                               5

                         , ;'i '•"                                 4
      8.4.2 The choicfe*!ibS"the peaks used  for multicomponent quantitation and
            the recognition of those peaks may be complicated by the
                                  D-18-PCB-Q                          08/23/94

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                                                                    DRAFT

      environmental alteration of  the Aroclors  or Toxaphene and by the
      presence of coeluting  compounds and/or matrix interferences.

8.4.3 Calculate the calibration factor  (ratio of the total peak area or
      height to the mass injected)  for  each quai&itaticm peak in the
      initial calibration standards and the SMC using equation .D.I (EQ.
      D.I):                                 /.    '    .
       Calibration Factor =  Total ^ea °^ak °* Pea* Hei?ht "" '  -  EQ.  D.I
                                  Mass--injected (ng)
8.4.4 Calculate the %RSD of  the calibration  faetoors  of the  low level,
      mid level, and high level Aroclof' 3&L6/1J2£0 standard  quantitation
      peaks and the SMC for  the initial caMbisation  using the following
      equation.
                                                             EQ.  D.2
                           V-  '*'"; •  '\': ,,  -,
                              %,           ' ' *,   ~
      where:  SD = standard deviation. .->

      Standard deviation is calculated-using the  following equation:
                                                             EQ.  D.3
      where:   x^' •= individual calibration factor  (per peak).

              x  = meatt >"sp£:'--|three initial calibration factors  (per peak)

           '"' 'if-' ;.-.<- -:munber of aa|i£bration s tandards.
      Equation D.4 is;'^he general formula for  the mean of a  set of
      values.
                                                           EQ. D. 4
                            D-19-PCB-Q                           08/23/94

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                                                                           DRAFT

            where:   X  = mean of values.

                     X^  = value.

                     N  — number  of values.           I-

      8.4.5 Calculate the RRT for each target compound using the following
            equation:

                                        PT                      ' '  °
                              RRT = 	•'"eagpo.K.Bt.,                EQil'D.'S
      8.4.6 Calculate  the  mean RRT and RT for each quaafcitation peak by using
            equation D.4.                            -I--'

8.5   Technical Acceptance Criteria               j  ~

      8.5.1 The %RSD of  the calibration factors for eacti Aroclor 1016/1260
            quantitation peak andft&e SMC in the initial calibration must be
            less than  or equal t
      8.5.2 The RT  of  the SMC  in the -standards gnust "be --within ±1.0 percent  of
            the mean SMC retention tisane calculated from the 1016/1260 initial
            calibration standards.    V

      8.5.3 The peak resolution of Aroclor/,,1016  and 1260 must be evaluated in
            the initial eaiilitation before 'proceeding with sample analyses
            (see paragraph ' 11 5 . -' ^           '-  ,
                     f-           < i '             ,'
      8.5.4 The chromatographic peaflc response for all quantitation peaks  in
            the loj? concentration >5s(t:andard must  be greater than 10 percent of
            full-scale *Jeflectisrur-jr t   -• !

8.6   Corrective Action   -  :
                              ."' "~\ "'
      8.6.1 If ;'the  SiRSD for any A3E*ciLor 1016/1260 quantitation peak or SMC in
            Sitfee initfaif calibration •!«  greater than 25.0 percent, the
         *--- ;instrument has;:i«Jt demonstrated adequate linearity to be used for
        ;':,••' this method.  SeJtrective action shall be taken and documented.
            If the  SMC RT  is ^t within ±1.0 percent of the mean SMC
            retention time casfcculated from the 1016/1260 initial calibration
            '^standards, the Laboratory shall perform corrective action which
            may ^include  a  new initial calibration.  DO NOT proceed with sample
            analysis ..until 'the RTS  is within ±1.0 percent.
      8.6.3 If the  respbi|ise  for  any quantitation peak in the low concentration
            standard  is not  greater than 10 percent of full-scale deflection,
            the Laboratory shall perform corrective action and make

                                   D-20-PCB-Q                          08/23/94

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                                                                           DRAFT
             appropriate adjustments before sample analyses  are  started,  to
             ensure that all quantitation peak responses  in  the  low
             concentration standard are greater than 10 -percent  of full-scale
             deflection.
       8.6.4  Corrective action may include optimizing'Isyste®. performance by
             adjusting gas flows, replacing the GC injector-liner,  column,  or
             the  precolumn,  or removing 0.5-1 m of the analytical column.

       8.6.5  All  initial calibration technical,«acceptance criteria s-hall be met
             before any samples or required blsaks are analyzed.   Any saifrples
             or required blanks analyzed when -Sthe initial calibration criteria
             have not been met shall require^tieanalysis ^"at no additional cost
             to the Agency.                 =            •';;

8.7    Documentation                            --;•'/ '*!<.>•-.
                                    ' -;,      "' ' :"' -;-fc- •'    -v
9.1    Summary                        '••• i         *~    ' •  '-•'•••  '-,

       A check of the initial calibration sequence shall be performed at the
       beginning  of every 24-hour analytical, ^sequence that includes field
       sample analyses.   This check of the;Initial calibration shall  be
       performed  using the'l|t^tXbsvel Arocldr,11016/1260 standard.   The percent
       difference (%D) JieiCween 'elser^alibratioiarlfactor in the calibration check
       standard and tibf^Kaverage calibration factor from the initial calibration
       is calculated i?&r each quaiit;l1:ation peak and the SMC, and  must meet  the
       technical  acceptance  criteii^.^lveA^in paragraph 9.5.  The  SMC RTS  and
       Aroclor peak re>s«skution nnlSti^Jigb''»6etf' - 'v                    ' ;-
      ^^,|1,  Each GC  used forgatoalysis shall be  checked to verify the initial
          1 ^calibration for|»ach twenty-four  (24) hour period of operation.
            TH^is .^procedure J$: to ensure that  the  instrument stability has  been
            maintained.    'j~
                   ''''' ^   •"-  ',
                    •- ,' \   Ay~
       9.2.2 An analytical; ^sequence is a contractually-defined sequence  of  GC
            analyses which  consists  of an initial calibration or a valid
            calibration check standard,  field samples, LCSs,  method  and

                                   D-21-PCB-Q                           08/23/94

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                                                                           DRAFT

            instrument blanks,  PVSs,  and other QC samples run within a 24-hour
            period  (paragraph 18).

      9.2.3 The analytical  sequence shall be concluded,.with an acceptable
            analysis of an  instrument blank and a FVS , >

      9.3.3 The calibration check solution shall be eqmiJ&ibrated to ambient
            temperature before  injection (approximately one tiour).

      9.3.4 Inject between  1  to fripL of tHe"iEi|leviel .,1016/1260 calibration
            standard.  The  same inj«j(Stion volutes"shall &b used for  all
            calibrations and  field/QGfsample analyses.
                                      "-:    _t 1 ;,'
9.4.  Calculations

      9.4.1 Calculate the•;fcafttferation factaaf ,(rat^° °f t^le total peak area or
            height to the mass;injected) for «ach quantitation peak and the
            SMC in t&e-'talibratrair.check standard analysis using the following
            equation:;            '-g            ':
                    < -            ''.-Js.,-,-,>«--.,,, .....
                  '>*''• ;.<         •., ;; ;;f<" ' "^ -;'C  t ^ . ,v\
                      ";'       J-?<. ~5;;^j'^;".g^, ~ ~?'"*n'%z--                             Tfr\  T\ c*
             calibration m*toz = Total Area of Peak or Peak Height       EQ-  D-6
                         ?  ,--.  ,.,           Mass injected (ng)
                           D betweiw,.76he calibration factors from  the
         ;,,,'fCalibration *<3Seck  standard and the mean calibration factors from
         ~.' the initial calaabiration using the following equation.   (NOTE:  For
         "   the SMC, calcul^lp the  %D between the calibration factor
            calculated from 4jne calibration check and the mean calibration
         r..s factor calculateitjfrom  the 1016/1260 standards analyzed during the
        '            calibraton).
                                   D-22-PCB-Q                           08/23/94

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                                                                          DRAFT
                                                                    D-7
                  where:   x  - mean initial calibration factor for the
                                appropriate quant i tat ion peak,,

                           xc  = calibration factor from current calibration
                                check standard .for the appropriate quaiatitation
                                peak.           '                       ;'

9.5   Technical Acceptance Criteria       , :            ,*•

      9.5.1 The %D between the calibration factors for> each Aroclor 1016/1260
            quantitation peak and SMC in the  calibration check standard and
            the mean  calibration factor for the quantitation peaks or SMC in
            the initial calibration must be within ±35,0 percent.

      9.5.2 All Aroclor 1016/1260..calibration check standard compound
            quantitation peak absolute;and relative retention times must be
            within the windows es'tdfelishe'd: 'frim^?tAat''^a^f-calibration standard
            during the initial calibration.  Report calibration check RT and
            RRT data  on Form  QIB-PCB^;see Exhibit B).

      9.5.3 The retention  time of the SMC in the calibration check standard
            must be within ±1.0 percent of
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                                                                           DRAFT

      9.6.3 If  the  SMC RT  is not within ±1.0 percent of the mean SMC RT
            calculated from the Aroclor 1016/1260 initial calibration,  the
            calibration  check standard shall be immediately reanalyzed.   If
            the RTS is still outside criterion upon reanalysis, corrective
            action  shall be performed,  which may inclttfle a new initial
            calibration.   DO NOT proceed with sample.analyses until the SMC
            RTS is  within  ± 1.0 percent.                   -K

      9.6.4 If  the  peak  resolution criterion is not met, the Laboratory must
            perform corrective action and demonstrate adequate resoitrtiion
            before  samples can be analyzed (see paragraph 11).        "<"

      9.6.5 All calibration check technical:|acceptance criteria shall be  met
            before  any samples or required Blanks are;,analyzed.  Any samples
            or required  blanks analyzed whe&pt&e calibration check criteria
            have not been  met shall require reaijalystis at no additional cost
            to the  Agency.                       '•'  -,;;,

9.7   Documentation

      Calibration check  standardj,r*i«$;j» jKee.jgeported on Forms QIB-PCB, QV-
      PCB, and QVI-PCB.  Reportingf^equire"mewfcss;jsr« listed in Exhibit B.

10    Performance Verification StandaM (PVSA '•
                                      ~€
10.1  Summary

      A performance verification standard ItJPVS) shall be analyzed at the  end
      of every 24-hour!analytie&|:, sequence.  ;i£he analysis of the PVS shall be
      started within^M  hours aftgtc the inject&on of the first initial
      calibration standard or the'lfcnstrument blank analyzed before a valid
      calibration, •;,'  ,:-.         ' \,,":;,,
                  e"TP$IS  jtefst be  anISgp&ed at the conclusion of the analytical
                 The PVSi!^^lysis  shall be  started within 24 hours after  the
                of  the firlfepinitial calibration standard or the instrument
            analyzed beforeXf|fvalid calibration check standard.  If a
     jligtfccessful PVS analysi^~as not obtained at the conclusion of the
     "atpfpiftical sequence,  ajji samples  analyzed since the last successful PVS,
      inililLjIl^calibration,  ci^lvalid calibration check standard shall be
      reinje'i^S'-.and reana^^ed  in a valid  analytical sequence at no
      additional^^g^ense jjbvfaie  Agency.   The Laboratory is encouraged to  run
      additional PVS ^SEaaljSses during an analytical sequence to minimize unpaid
      reanalyses.   If -^-"^cceptable PVS is  analyzed during an analytical
      sequence,  the  Laboratory may continue to collect data under the current
      calibration until  the conclusion  of the current 24-hour sequence.   If at

                                   D-24-PCB-Q                          08/23/94

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                                                                           DRAFT

      any time  an unsuccessful  PVS analysis is made,  the Laboratory shall stop
      sample analysis  and immediately reanalyze the PVS.  Up to two injections
      of the PVS  may be  used to satisfy the criteria.  If on reanalysis  the
      PVS is still  outside QC criteria,  the Laboratory shall take corrective
      action and  recalibrate the GC (run a new initial calibration) prior to
      reinitiating  sample analyses.   Recalibration wl.fl "begin a new analytical
      sequence.                                          '  ;
10.3  Procedure
      10.3.1
      10.3.2
      10.3.3
      10.3.4
The GC conditions shall be
analyzing samples.
                               same  as  those used for
The PVS is two times the ioncentration of the low level
Aroclor 1016/1260 standarxffrased  in ttlie initial calibration
(see paragraphs 6.3 and 6.6).     :

The PVS solution shall be equilibrated to ambient
temperature prior to injection (approximately one hour).
The same in
samples and sta
                                be used for all field and QC
                                     PVS.
10.4  Calculations                   ..        ^
                                      '•;     ,si „ :
      The amount of Aroclor 1016/1260 and-,the  SMC in the PVS shall be
      calculated using the following  equation.
                                    Obseived=
                                                -
                                              w*T m
                                                  EQ. D.8
            area or peak height of the appropriate PVS
          '^',,quantitation peak or SMC.
      where:
             ..,-, '."f&Pji  -,~     measbLtsalibration factor  established during the
           ,,;(,;;,''   :" •:-;-,-; ,  ;    initi&i;,yealibration  for  the appropriate
           !            -V£-|  quantisation peak.   (NOTE:  For the SMC
                          X'.-; calculation, use the mean calibration factor
                            '^calculated  from  the  1016/1260 initial
                             iealibration standards).

      An ic«B|sa.ge amount (avenge amount observed)  of the five quantitation
      peaks' l&i^fcoth 1016 &$&' 1260 are then determined using the following
      equation.'  [V; ^     Y; \,
                                  D-25-PCB-Q
                                                     08/23/94

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                                                                          DRAFT
                                   ~X= V -^                    EQ.  D.9
                                      ft *

      where:      X  = mean concentration.

                  X^ = individual  peak concentration.

                  N  = number of quantitation peaks .

      The amount recovered is calculated usis|j  the following equation
             Amount Recovered =  *™*9* ^1*               X 100    EQ. D. 10
                                                   (ncft
10 . 5  Technical Acceptance Criteria

      10 . 5 . 1      All PVS target eoopounds must have  a calculated recovery
                  (mean of the S^^attrilfca^iwa peaks)  of 75-125 percent to
                  report data witftoiat flags.1"-:,- •_- - , ,  -  ,
      10.5.2      If recovery of a PVS;; compound  is not within 75-125 percent
                  but still within an expanded recovery window of 50-150
                  percent, the associated ssaiaple analyses  results shall be
                  flagged "P" (see paragragih 10.6).

      10.5.3      All Areclor liQjljS/1260 compound quantitation peak absolute
                  andvj?elative retention times*»aist  be within the windows
                  established froa^-the low calibration standard during the
                  initial calibration.  Report PVS RT  and  RRT data on Form
                          (see               ''
      10.5.4      The SMC recovery criterion of  50-150  percent is advisory
                  only.  Reana%sis of the PVS is not performed if the SMC
              ;.  , jNeesevery is ou1^i.4e the advisory  recovery limts .   The SMC
          „ -!/;s -  ' reco^yy in the P^Srimust, however, be greater than or equal
         ...  *      to 20 peanut and less than or equal  to  200 percent.
      lfV5.5      The SMC RTf~fai the PVS must be within ±1.0 percent of the
      "": J"          mean SMC Rf-^alculated  from  the  1016/1260  initial
      '• ^<-.°/s       calibration-standards.
         "''$-i-*i,              ,!' ".
      10.5.6 i*s i The peak/Resolution for Aroclor  1016 and 1260 must be
                 : esraluated^in the PVS before  proceeding with sample analyses
                  ('see-rgaragraph 11).
                                  D-26-PCB-Q                           08/23/94

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                                                                           DRAFT

10.6  Corrective Action

      10.6.1      If recovery  of an Aroclor is not within 75-125 percent  but
                  still within an expanded recovery witKiow of 50-150 percent,
                  flag the Aroclor "P"  in all associated field sample results
                  generated  since the  last valid PVS,j iaaistial calibration or
                  valid calibration check standard: •'      ,; ,

      10.6.2      If either  (or both) Aroclor in the PVS is outiMe the
                  expanded recovery range,  thf .WS shall be reanalyze*!
                  immediately.   If,  on  reana^sls, either (or both) Ar«clor is
                  still outside the expanded^recovery range,  stop sample
                  analyses,  perform corrective action,jron a new initial
                  calibration,  and reanal^e, all samp Jabs run after the last
                  valid PVS, initial calibration or *Su.id calibration check
                  standard before proceeding with sample analyses.

      10.6.3      If the RT  or  RRT for  any Aroclor lOi^J.260 quantitation peak
                  is not within the RT  and RRT windows  ^isissblished from the
                  low calibration r'Sjtandard during the initial calibration,
                  reanalyze  the iSH$> JB££i%9*ff9 £,?analysis a compound peak  is
                  still outside tnf|v^indowsfs*^|H*w}il^j»al calibration must be
                  performed  before samples  can;be analyzed.  The instrument
                  must be recalibratelfl ;-as described in  paragraph 8.  Reanalyze
                  all samples run after'.:^he,3Utet valid  PVS, initial
                  calibration,  or valid calibration check standard before
                  proceeding with sample analyses.

      10.6.4      If tfcasL^MC RIPS.Criterion ispaot met for a PVS,  sample
                  analyses shalpite. stopped aiidxthe noncompliant PVS
                  imiiediately reanalyzed.   If the SMC RTS is still outside the
                  «xJ|terion  uponjjtaaanal.ysatsj..jcorrective action shall be
                  peiifojnied, wbiMiiS^JgiiiiciiSle a new initial calibration.  DO
                  NOT d^afcinue  with sample  analyses until the RTS is within ±
                  1.0 perce$,t;^,, Reanalyze all samples that were run between
                  the noncompliant; PVS  and  the last valid PVS,  initial
              ;I  ^-Calibration,  or :iml,id calibration check standard before
          ,J  '-   "proo^iiing with s^sle analyses.
         , .;!«            ^ \^{
         ' ••               ^..^
            5      The SMC 3e«overy criterion of 50-150  percent is advisory-
                  only.   The||aiC recovery in the PVS  must,  however, be greater
                  than or eq^il  to  20 percent and less  than or equal to 200
                  percent.
      10.6.6':"-V. |i ,,If the F^^SMC recovery is  less  than 20  percent,  greater
                       20(J^ercent, or if peak  interferences  are present, stop
                                   perform corrective  action,  and immediately
                  reanalyze the noncompliant PVS.   If  the  SMC recovery is
                  still but on reanalysis, perform  corrective action and start
                  a new analytical sequence.  All samples  analyzed since the

                                  D-27-PCB-Q                           08/23/94

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                                                                          DRAFT

                  last valid PVS, initial calibration,  or valid calibration
                  check standard shall be reanalyzed within a valid analytical
                  sequence.                             j

      10.6.7      If the peak resolution criterion  is,:-tiot met,  the Laboratory
                  shall perform corrective action andr-demonstrate adequate
                  resolution before samples can be^analyze*! (,see paragraph
                  ID.                            f          '  -.-:

      10.6.8      If all PVS criteria cannot bSkmet after having taken
                  corrective action, reanalyzes'(do  not  re-extract) the
                  associated field samples iti another valid analytical
                  sequence.  If on reanalyzes all QC ssaiple criteria are met
                  and the PVS criteria still cannot bfs  aet,  then submit all
                  sample data from both sequences.  The Laboratory shall
                  describe in the Batch narrat^^tdserproblems associated with
                  the PVS and how the field sample -matrix may have affected
                  the PVS analyses.  If the Laboratory  ij|jj?ys technical ^acceptance  criteria are not met,
                  more, *B?equenb|ajaalysis of "flse PVS is  recommended, especially
                  whelUnighly contaminated or?c«mplex samples are analyzed.

10.7  Documentation '            4 •>;;,'.„-,,,.,, ,„.,,,,

      Results of PVS ankjlyses are reported on Forms QIB-PCB, QIII-PCB, and
      QVI-PCB.  Reporting Requirements are listed in Exhibit B.

11    System EerfonaaTice - GC Reaol-ation

11.1
         Ititation of Aroclcep'lB. is primarily  accomplished using pattern
        iognition and matchiiigftRTs and RRTs  of  quantitation peaks.  Because
           Llary columns are i|S£d, peak resolution is  not usually a limitation
      of %fati»,',omethod.  The metticd does require  an experienced PCS analyst to
      make Ar%ft:®r identifis|iitions and to  establish that no significant change
      in Arocidr^|>at;terns^liis  occurred whenever a calibration check standard
      or PVS is ana^jj^eidxi^If  a change in  pattern is  seen,  identification and
      quantitation is~siiw«rsely affected and the Laboratory shall recalibrate.
                                  D-28-PCB-Q                          08/23/94

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                                                                          DRAFT

11.2  Frequency

      11.2.1      Initial calibration - The peak resolution  in the  PCB pattern
                  for the low level Aroclor 1016/1260 standard shall  be noted
                  by the analyst before proceeding with  sample analyses.

      11.2.2      Calibration check standard  - The peak resolution  for
                  Aroclors 1016 and 1260 shall be evaluated '  'f »*.. each
                  calibration check standard.  The analyst shall4establish
                  that the pattern has not changed before proceeding -irith
                  sample analyses .                                   : '  -

      11.2.3      Performance verification standard  - The peak resolution for
                  Aroclors 1016 and 1260 rshall be evaluated  for each  PVS  that
                  is analyzed in a. valid analytical .sequence.   The  analyst
                  shall establish that the pattern lias not changed  before
                  proceeding with sample analyses. '«

11.3  Technical Acceptance Criteria
      11.3.1      Any pair of adj^aet-j^aks.Jfully resolved in the  low  level
                  Aroclor 1016/12^.. iniHal-^ali^al&Qn standard must not
                  exceed 25 percent^valley in £he cMibr&tion check or
                  performance verification sta&dards.

11.4.  Corrective Action                  .   :

      11.4.1      If the /AirocSor,, pattern changes and any pair of adjacent
                          ily^r^olved in thejiiow level Aroclor 1016/1260
                          calibration standard exceeds the 25 percent valley
                  crierion in tHe> calibration check, corrective action shall
                  be .performed. 4% ;;vali,d, calibration check must be
                  deatei«strated,^^^e.^r)lp|3a|fcial calibration shall be performed
                  and 'doewented before proceeding with sample analyses.

      11.4.2      If the Aroetmrjifpattern changes and any pair of adjacent
                 jpe^ks fully re^oftsred in the low level Aroclor 1016/1260
            4  " ;^nl:t$^xcalibratiGii6.standard exceeds the 25 percent valley
         N1       criterlim -in the PVs , the PVS shall be immediately
         t;        reanalyze!^  If after reanalysis the PVS percent  resolution
                  is still ojafcside criterion,  corrective action shall be
                  performed and a valid calibration check demonstrated  or new
                  initial calibration performed. Reanalyze all samples  run
                  after the.|Last valid PVS, initial calibration, or a valid
            ' ;==   . calibrators check standard before proceeding with sample
               -ilaualyses; >-'*
                 '"''' •'• ;    i~
      11.4.3      LossV&£ i-column resolution (a higher percent valley) could
                  indicate injector contamination or column degradation;
                  therefore,  injection port and/or column maintenance may be

                                  D-29-PCB-Q                          08/23/94

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                                                                         DRAFT
                  required.  Maintenance may include replacement of the
                  injector liner and/or removing 0.5-1 m of the column.  If
                  these measures do not work, column replacement should be
                  considered.                         •

11.5  Documentation

      Percent resolution results are reported on Forms QII-BCB, QIII-PCB,
      and QV-PCB.  Reporting requirements are listed in Exhibit |k
                                  D-30-PCB-Q                          08/23/94

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                                                                          DRAFT

                                   SECTION IV


            SAMPLE ANALYSIS AROCLOR IDENTIFICATION AND QUANTITATION
12

12.1  This method  is  designed for use in the rapid analysis of
      soil/solid,  oil,  and  wipe  samples for PGBs measured as Arocloxsv  If,
      upon inspection of a  sample,  the Contractor suspects that the saa^le is
      not amenable to this  method,  contact tfee Regional TPO or the CLASS
      contractor for  instructions.   For Sujierfund emergency removal actions,
      contact the  Regional  TPO or the Hea&fuarters APO 'Jlor instructions.  If,
      for emergency response  actions,  the TfO'*»r APOsare not available,
      contact the  Regional  On- Scene Coordinator ^{OSCj: for instructions.  The
      Laboratory must remember that it shall follow "the requirements in this
      SOW without  deviation.

12.2  Before samples  or required b.ianks can be analyzed, t3te , instrument must
      meet initial calibration orC-j^YsOLJIl ©alibration check standard and
      column resolution technical" ;^ceptande''ei^t:eTcia^, ,All sample extracts,
      required blanks,  LCS, PVS,  anct calibration staiidards shall be analyzed
      under the same  instrumental conditions abet shall be allowed to warm to
      ambient temperature (approximately, one Kour) before preparation and
      analysis.                           , ; .

12.3  The laboratory  shaiil ;:p«tf<>rm sample extraction and cleanup of water
      samples utilizing Either 'Solvent (paragraph 14) or solid phase
      (paragraph 15) , l^traction  %«& cleanup. \"lfoe laboratory must meet all
      QA/QC requirements as stated/under this contract using either of these
      extraction/ cleanup techniqiSeifL ,,S! Ttie .solvent extraction procedures are
      recommended  for,: the cleanup land extinction of all samples; however,
      Aroclors SPE procedures for waters may be used if equivalency to the
      solvent extraction piroeedures can be demonstrated by the Laboratory.
      Solvent extraction and  tsitesjaup procedures shall be used for non- aqueous
      samples, <'•' '"••' ••           "  • ??  .,
         r  „:- -,,:<  •:,     >.         v--  ^-
           , V '^"  -'-'•• ,,f: i;,          - K
12.4  BlaBp^samples,  such;^  trip blanks and field blanks, supplied by the
      Rejgiion and included $£j3n a batch of field samples shall be prepared,
      aajtlyzed, and reportediss  water samples.   Occasionally,  a water QC
     ,$#nle (e.g., field anltitrip blanks) will be included with a batch of
          <-ssamples .   If the laboratory is not certain whether a water sample
      associated with a batcji of soil samples is a QC sample,  contact the
                    or the GEiisS  contractor.
      NOTE: If water",':1»$Lgaks provided by  the Region,  such as trip and field
      blanks are inclti^&dl.in a batch of  soil samples,  the Laboratory is not
      required to prepare and analyze  an associated water method blank or a
      water LCS.

                                   D-31-PCB-Q                          08/23/94

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                                                                          DRAFT

12.5  If unusual or high concentration samples  are  received,  see Exhibit D,
      Appendix B for general guidance on  screening  and sample preparation.

13    Phase Separation

      Multi-phasic samples shall be phase-separated ''£11120 ;their individual
      phases.  The phase separation techniques  employed will  vary according to
      the types of samples received.  Since  it  is impossible  to know the
      number and types of phases that will be present  in a sampfleg'-the choice
      of phase separation techniques is left tsa the professional ^Sgeaaent of
      the analyst.  Various techniques can be^femployed to separate tfbey/phases.
      These include pipetting off liquid  phases (decanting should not be
      done), centrifuging to remove suspended solids,  and use of spatulas to
      remove solids (wooden tongue depressors work  wellf).   Whenever possible,
      phase separation operations should  be.::pone with  disposable glassware.
      The phases should be separated into glasls -cxrajpslners with teflon-lined
      screw caps.  This allows for storage and  handling of the waste in a safe
      manner.                                       ','  «

      13.1  Samples received containing multiple phases stien  !as water, oil,
            and soil/solid in the |same sample jar shall be "phase separated"
            into individual phase'sft.      "•""•i"-!.-"£-r^;  '?/ .;;,

      13.2  Each individual phase is;-itaken tteBtogh  the procedure as a
            subsample.  Report analytical results for  each sample phase.
            Note: Each multi-phase sample! slsall be  identified using the EPA
            sample number convention for  multi-phase samples  as specified in
            Exhibit B.  .-: :;; g %
                             "'*% '•>           • r.
                     '"  -       '' , ^ '
      13.3  Do not aaalyze any pliise that represents less than 10 percent of
            the total-:sample volisife..

      13.4  In the -fallowing pi^^^B&,i--)f/^fe  applicable, references to
            "samples" explicitly mean "single phase units."

14    Solvent Extraction
14.1  Samp lelfareparat-ion "and Extraciii,^  - Water  Samples
                           .
      A ^d mL aqueous sam^i- is serially  extracted using two 10 mL portions
      efpiexane.  Extractior!|^:\are performed  in  125  mL Erlenmeyer flasks with a
               stirring bar.s*|Dne gram of  NaCl  is added to the aqueous sample
                after the  finsfc hexane extracting solvent is added. Extracts
                    filtered|;;*fand dried  through powdered anhydrous sodium
      sulf ate; >«bad concentrated to a  1 mL  volume using the nitrogen blowdown
      procedure". If^Hom-AroctSrs extractables  are removed from the extract with
      sulfuric aciTd^?fW!£af»iuni permanganate,  and florisil column clean-up
      procedures.  Fin43L extract volume  is 1 mL.

      14.1.1      Measure  100 mL of sample into a 125 mL Erlenmeyer flask.

                                  D-32-PCB-Q                          08/23/94

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                                                                           DRAFT

      14.1.2       Spike  the sample with 10 pL of the SMC  (2.0  ug/mL).

      14.1.3       Add teflon stirring bar.

      14.1.4       Add 10 mL of hexane.

      14.1.5       Place  the sample on magnetic stirring plate  and stir for
                   three  minutes.   The stirring rate should be/^tefficient to
                   mix hexane throughout the sample.              '.,

      14.1.6       Add 1  gram of NaCl to sample during stirring and stir for an
                   additional 3 minutes.     ":

      14.1.7       Remove stir bar and allow ,aqueous and*hexane layers  to
                   separate.                '    ,

      14.1.8       Transfer  the hexane layer by pastemr pipet to a 25 mL
                   concentrator tube.                    ~,

      14.1.9       Repeat steps 14**l»4 - 14.1.5 and 14.1.7 - 14.1.8.  Combine
                   extracts.   Dis-oard^iextract:ed aqueous sample.
      14.1.10     Prepare  a drying column by pltjgging; ttie bottom of a funnel
                  with  glass wool and" adding approximately 15 grams of
                  powdered anhydrous sodium salfate.  Pour extract  through
                  funnel and collect in a -25 ML graduated concentrator tube.
                  Rinse the extract contaiiier with minimal volumes  of hexane
                  and poar t3ir«Migh the funraeTL  Rinse sodium sulfate twice
                  with minimal 'volumes of hexane.
                     ;   ••         - :f,
      14.1.11     CoEscentrate extract to approximately 1 mL using the
                  ftitarogen-blowdo^.,,,EXO,ced!tire in a 30«C water bath.   To
                  minimize analyse?;:3.b;SS;:, occasionally rinse sides of
                  conceiitxatjor  tube with hexane during the blowdown procedure.
                  Do not tetvesxtract go dry during concentration.

      14.1.12,,,.-•;;' >fiSBQ»^ed  to extr£te£<.«clean-up step (paragraph 14.3).
            ^>;, -, "i vy,u\  /<"x.           ' ?• =
          ,/,;;» '"    '"''-tv|;/:i_,         • tf-
14.2  Sam|it* Preparation :^Eia Extraction - Soil/Solid Samples
          gram sample of sofl^is mixed with powdered anhydrous sodium  sulfate
         , is serially extract!^ with a 20 mL and a 10 mL portion of
             acetone (50:50)^sing an ultrasonic probe.  Extracts are
      combiaB<8^, filtered, ac^idried through powdered anhydrous sodium  sulfate,
      and coSleisit^rated withiltblvent exchange into hexane to a 1 mL volume
      using thev'mS:r.pgen bi^wdown  procedure.  Non-Aroclors extractables  are
      removed from''-tfeerTex£fact with sulfuric acid, potassium permanganate,  and
      florisil column'^tslLean-up procedures.   Final extract volume is  1  mL.
                                  D-33-PCB-Q                           08/23/94

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                                                                    DRAFT

14.2.1      Decant  and discard any water layer on a soil/solid sample.
            Mix samples thoroughly, especially composited samples.
            Discard any foreign objects such as sticks, leaves, and
            rocks.

14.2.2      Weigh approximately 6 grams of a araf»r«s;sentative sample to
            the nearest 0.1 g into a 150 mL beakerT

14.2.3      To the  weighed sample add a sufficient amount of; powdered
            anhydrous  sodium sulfate to prepare a free f lowing mass upon
            mixing.  Mix well.         ,,!' "                     *' <  •-

14.2.4      Spike the  sample with lO.ytt'of the SI4C (2.0 ug/mL) , mix
            further.                 "~:           ::;

14.2.5      Add 20  mL  of hexane/acetone (£0; 5,0)

14.2.6      Sonicate at microtip maximum power? -caecl the sample during
            sonication.   The sonicator must be set for 50 percent pulse
            action.  SonicatejEor 3 minutes.  The power output may have
            to be adjustedffslu-^s^e;, that the sample extract does not
            splash  excessively';  any ^ig%€icaafc JLoss of sample during
            sonication is notlfacceptable4 r XInseB--lCbe sonicator tip after
            each sample extraction with% mL of hexane/acetone (50:50).
            This rinse liquid shall be-combined with the sample extract.

14.2.7      Remove  and collect solvent: layer in a 40 mL centrifuge tube.

14.2.8      Add 10,  mil  of li^iane/acetone ,(50:5°) and repeat steps 14.2.6
            andC'£4.2.7.
14.2.9      Combine extra^ps^and^filter by gravity or vacuum filtration.
                                   -transferring entire sample contents
            to fuEibel and rinse with an additional 10 mL hexane/acetone
            (50:50)v.,t «;   centrifuge tube.  Rinse the extract container
             -~ i-.r,,,|f-     with minimal volumes of hexane/acetone (50:50)
                ;: -' |!     and pour through the funnel.   Rinse
                         filter/sodium sulfate with 10 mL of
                         hexane/acetone (50:50).

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                                                                           DRAFT

                   14.2.9.2    For vacuum filtration use  Whatman #42 filter
                               paper in a Buchner funnel.   Pre-wet the paper
                               with the hexane/acetone  £50:50)  solvent and
                               discard rinsate.  Transfer combined extracts
                               into funnel, apply vacusaa,  and collect filtrate.
                               Rinse filter with an IjO-iiL^of hexane/acetone
                               (50:50).  Pour filtered  extacact  through a powder
                               funnel plugged with glass  wo6l-,aiad filled with
                               powdered anhydrous sodium  sulfatfeiaiaid, collect in
                               a 40 mL centrifuge tube.   Rinse  the 'iext^r-act
                               container with pinimal volumes of hexane/aeetone
                               (50:50) and pour through the funnel.   Rinse
                               sodium sulfate;with an additional 10  mL
                               hexane/acetcpe (50:50).jf
                                          ? ' \        : "^''
      14.2.10      Concentrate extract to appraxlatatssly 25 mL using  the
                   nitrogen-blowdown procedure in^a. i300C  water  bath.   Transfer
                   extract concentrate to a 25 mL coticieiitrator  tube  and
                   concentrate further to approximately 18 «'S mL.   Add 5 mL of
                   hexane to conceiijxator tube and mix  vigor0«sly.
                   Reconcentrate <6^^pfHDaSiwately 1 mL.   To minimize analyte
                   loss,  occasionally rinse"-siSSes sd? centrifuge and
                   concentrator tubes s>with hexafte durii% ihe  blowdown
                   procedure.   Do not'.allow extract to  go  dry during
                   concentration.      ;'••     ~> ,

      14.2.11      Proceed to  extract cleaii4ip step  (paragraph  14.3).

14.3  Sulfuric Acid Cleatnip   ->  ~           \-,,
      14.3.1      Using a syringe] • . _ , s .
      14.3.6      If avSilean phase  separation is achieved, proceed to  step
                  14 . 3 .V.
                                   D-35-PCB-Q                           08/23/94

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                                                                          DRAFT

      14.3.7      If the hexane layer  is  colored or the emulsion persists for
                  several minutes, remove the sulfuric acid layer from the
                  vial and dispose of  it  properly.   Add another 5 mL of the
                  clean concentrated sulfuric acid.

                  NOTE:  Do not remove any hexane at: this stage of the
                  procedure.

      14.3.8      Vortex the sample and allow the phases to separate.

      14.3.9      Transfer the hexane  layer to'a clean 20-mL vial.   :  ;
                                            -s
      14.3.10     Add an additional 1  mL  oJr'lhexane to the sulfuric acid layer,
                  cap and shake.  This second extraction is done to ensure
                  quantitative transfer oifrdphfe. Aroclots and Toxaphene.
                                              '"•- \ * ,   v'
      14.3.11     Remove the second hexane layer and combine with the hexane
                  from step 14.3.9.                  :

      14.3.12     Add 1 mL of reayge^t  water to the combine*! feexane extracts to
                  remove excess -Spkisiricvaicid .that may still he present.
      14.3.13     Vortex and allow ^Hte phases Mo -'separate ''.
                                    * ±. -^?r       ' -
      14 . 3 . 14     Transfer the hexane iayer ;fco a clean 20 -mL vial .
                                           , f: :

      14.3.15     If a water layer is evSidtent in the eluate,  remove by the
                  additi
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                                                                           DRAFT

      14.4.2       CAUTION:   Make sure that there is no exothermic  reaction nor
                   evolution of gas prior to proceeding.

      14.4.3       Cap  the vial tightly and vortex for 1 minute.  A vortex must
                   be visible in the vial.

      14.4.4       CAUTION:   Stop the vortexing immediately if the  vial leaks.
                   AVOID SKIN CONTACT; POTASSIUM PERMANGANATE BURNS.

      14.4.5       Allow the phases to separate sf or at least 1 minute.  s Examine
                   the  top (hexane) layer, it ;ssTiould not be highly  colored nor
                   should it have a visible eaulsion or cloudiness.
                                            ;
      14.4.6       If a clean phase separation is achieved  proceed  to  step
                   14.4.9.                 '  '"'

      14.4.7       If the hexane layer is colored or-t^fcie emulsion persists for
                   several minutes, remove the permanganate solution from the
                   vial with a glass pipet and dispose of *4&, properly.   Add
                   another 5 mL oftaeiean aqueous permanganate; -solution.
                                  ,''»•  '" !";,-*
                   NOTE:   Do not resaove any'ttessaiae ••-afc -*;his,  stage  of the
                   procedure.         ?          .:     ! '"'

      14.4.8       Vortex the sample and allow the phases to separate.

      14.4.9       Transfer  the hexane layer to a clean 20 -mL vial.

      14.4.10      Add ,311" additional 1 mL of ttexane to the  permanganate layer,
                   ca£>j£he vial securely and s&ake.  This second  extraction is
                   dojoe to ensure Jej: '|,;  , „. ,, ...

      14.4.11      Remove the second hexane layer and combine  with  the  hexane
                   from step;,';34-.4.9.

14.5  FlorisiJ, r©B«iprldge Proceduife;  '.
      14. 5s,.!      Reduce^^fifefe volume of the combined hexane layers to  1.0 mL
        ^=t*        under a  stream of dry nitrogen.

     "|&i,5.2      Attach thefH&c Elute vacuum manifold to a water aspirator or
      '^fft -•;       vacuum pumg;.1with a trap installed between the manifold on
         ' '--v/J,,-    the vacuum*. ^Source.  Adjust the vacuum pressure in the
            '^ =', ^manifold/tai' between 5 and 10 pounds of vacuum.
               "':;  .$••    j':;
      14.5.3      Pl«c«s;«»e Florisil cartridge into the vacuum manifold for
                  each-sample extract.
                                   D-37-PCB-Q                           08/23/94

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                                                                           DRAFT

       14.5.4      Prior to cleanup of samples,  the cartridge must be washed
                   with hexane.  This is accomplished by placing the cartridge
                   in the vacuum manifold pulling a. vacuum and passing 5 mL of
                   the hexane solution through the cartridge.  While the
                   cartridges are being washed,  adjustSfhe vacuum applied to
                   each cartridge so that it is  appr'
                                                f'.. ••    \ ~\
       14.5.6      After the volumetric flasks are-, ini place,  vacuum to the
                   manifold is restored and the  extract: sfor each field and QC
                   sample solution is transferred to thef,tap frit of the
                   appropriate Flq^sil cartridge.
                                             :<•>':•-„
      14.5.7       The PCBs in theV^tract etteciepfcrAtres-.sare then eluted through
                   the column with 95:JffiL of hexaaei-and'cbllsected into the 10 mL
                   volumetric flasks liB&d in tfefe rack  inside of the vacuum
                   manifold.            's     .-*'?*

      14.5.8       Transfer the eluate in each volumetric flask to a clean
                   centri;:R%e'|t3ibe or 10 mLVial.  Use two additional 1 mL
                   hexaaai| rinsesl8«^ the flask:*fao ensure quantitative transfer
                   ofjtbe cartridgfe seluate.    '~K,
      14.5.9       Concentrate thf^do^ititp^,,to a 1.0 mL volume using either
                   nitrijgen blow^»iBa,l^:''S|pU?»tf,"Snyder column.   Measure the final
                   volume iwith a clean syringe or by transferring the extract
                   to  a cleaa?'SEolumetric flask.
                             ' % %
      14.5.10 .,« "'If; crystals of%ap£fur are evident or the presence of sulfur
            ,Th !    Is %S3Bfiected, proved to paragraph  14.6.   Sample analyses
         r f         showiri|^|||ie presence of sulfur are  not  acceptable and must
       .';?-         be  reanalpsed after sulfur removal.

        i5.11      If  sulfur IB,not expected to be a problem,  transfer the 1.0
          ;!>,       mL  of samplpe;.: to a GC vial and label the vial.   The extract
         'xir:;,  .,     is  ready fjjj£ GC/ECD analysis; proceed to paragraph 18.
             \|i; HE,  Store thetjextracts at 4°C (± 2°C) in the dark  until analyses
               '••f  «r-e perfoianed.
                   '<*._,-j^ ^j:t-
14.6  Sulfur Removal  '-:-<; ''•"•*
                                   D-38-PCB-Q                           08/23/94

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                                                                           DRAFT

      14.6.1      Bright (unoxidized)  granular copper is used to  remove  sulfur
                  contamination.   Add one to three granules of copper  to each
                  hexane extract  in a clean vial.  Tighten the top on  the vial
                  and shake for 30 seconds.   Filter or)centrifuge and  then
                  decant the solution to remove all solid precipitates.   If
                  copper appears  bright, go to paragraph 18.  If  copper
                  changes color,  repeat sulfur removal as necessary.

      14.6.2      If  only a partial set of the samples in the Battels- require
                  sulfur cleanup,  an additional- reagent blank of  hexane  spiked
                  with the appropriate amountf'of the SMC solution and':<£Leaned
                  with the copper is required.

      14.6.3      Proceed to paragraph 18 .tor GC/ECD analysis.

15    Solid Phase Extraction and  Cleanup of Water Samples

      Solid Phase Extraction using nonpolar Cg (or equivalent) or C^g  disks
      may be used to  extract water samples (Note: an alternative  phase may be
      used if the new phase can be:; demonstrated to meet the'KJA/QC requirements
      of this method.)   An additi«ndl.-^li.t«r 4i?H *-s required when water
      samples contain particulates?;; Upon'o'peiiiB^ tUT'.package of disks,  they
      shall be used immediately or 'stared in aJdesiccator, (over Drierite, or
      equivalent).  For reproducible extraction efficiencies, all directions
      given below shall be followed as closely as possible.  Note: The
      laboratory shall not use  SPE for non,~agueous samples.

15.1  Sample Filtration -T : •: '•':-•,.,          '•
                       £ ,< -- " - % <-' '">:•          s   s
                               -•:%,*            ..{,-
      All water samples shall be ifiltered. When disk extractions  are performed
      the filtratiojsrsstep  may be iioabined with the extraction by  placing a
      filter disk ,4el»igned to fi^M^ide..,tfhe.. neck of the sample reservoir and
      proceeding wiiili'.iiise  water y&ap&gcl&aii&p and extraction as  specified in
      paragraphs 15.2 '-a,3

15.2  Sample Preparation -
                                CRQDfc|pte  the same as the solvent extracted
          '^sample CRQLs-•«£(' 'ftated in Exhibit C.
      ^-82.1      Pour 100 mfp«f water  sample into a clean erlenmeyer flask,
      f;::           fleaker beater,  separatory funnel, or any other suitable
      *"'*»- ?\ •',       mixing chan&er.
         '*-+i%...               -7!
      15.2.T' \|r; .Adjust thg^pH of the  sample to 5.0 - 7.0 using 0.5 N sodium
              'X-:;jbydroxidi|>
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                                                                          DRAFT

      15.2.5       Shake  sample  vigorously to mix thoroughly.

      15.2.6       Proceed with  sample  cleanup and extraction utilizing SPE
                   disk procedures  (paragraphs 15.3 -  15.'5).

15.3  Disk Set-up  and Conditioning                      \

      15.3.1       Place  the  disk onto  the frit on'the vacuum-head,  place the
                   reservoir  on  top of  the head and clip together.-
                                              <'','•                    ''
      15.3.2       When filtration  is required!*-a filtration disk or :5t>0 mg of
                   Celite will be placed on taop of the extraction disk.

      15.3.3       Turn vacuum pump on  and;|f$et pump vacua™ to 10 inches of
                   mercury.   Do  not exceed : the manufacturer's recommendation
                   for manifold  vacuum.   Flow'-r^es eari be controlled by
                   opening and closing  vacuum manifold valves or pinch clamps.

      15.3.4       Wash each  disk with  four 5 mL aliquotss^of hexane.  SLOWLY
                   open vacuum valxsff to allow the hexane to jpass through the
                   disk after
      15.3.5      Wash  each  disk wilfh, four  5  mL,4«lIqti«fcs'(of methanol (MeOH).
                  Let disks  drain after  each  Wash.  Do not allow the disks to
                  drain dry  between washes. -, /
                                         ' {•"* ' ^
      15.3.6      Wash  the disks with two/S.':mL aliquots of methanol/water
                  (5:100),   &ll»w the firstiS mL portion to wash through;
                  however, do'mofirAllow  the ':$$fsik to drain dry.  Next wash the
                  last  5 mL  portion through,  keeping the disk wet.   Each disk
                  must  remain moi|s»|- until the entire sample volume is
                  extracted.  DTpfb^CONDITIONING,  DO NOT ALLOW DISKS TO DRY.
                  THIS  STEP  IS J^^^||^KpoOD RECOVERIES.

15.4  Compound Extraction Basing Disks
      15.4.1  ,,,,   JSwirl  the  sample|J.(from paragraph 15.2) for 20 seconds and
                             decants*^»' sample  into the sample reservoir.
                                    '•••&-'•     *                *
                  Open manl3|ald valves  to  allow samples to pass through the
                  disks  at approximately 3-8  mL/min.   The flow rate must not
                  exceed 10 ips/min.   If the flow rate slows because of
                  particulatfe;buildup on the  disk or filter, increase the
                  vacuum to Jatsiintain  3-8 mL/min.  flow.
                           'v&f- ,
                          JSe'
                  HOTE:   ItSfflust  take at least ten minutes for the sample to
                  pass through the  disk.
                                   D-40-PCB-Q                          08/23/94

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                                                                           DRAFT

       15.4.3       Rinse the sample container with 5-10 mL of methanol/water
                   (5:100) into the sample reservoir to transfer any remaining
                   compounds.                            :

       15.4.4       When the entire sample volume has passed through the disks
                   (approximately 15 minutes),  rinse ti& saaple reservoir with
                   an additional 5-10 mL methanol/w4t:er (5i:J0S) into the disks.

       15.4.5       Wash the disks with an additional 5 mL methanbl/srater
                   (5:100), continue to apply vacuum until the top &£»£iie disk
                   is dry.  Turn off vacuum.  *-:,                       '  ;

       15.4.6       Wipe the reservoir dry wit3i  clean lab/'lzissues (Kimwipes, or
                   equivalent) .            ,  >             • •
                                            v  <        ^
15.5   Compound  Elution using Disks           " :-   , ;

       15.5.1       Release the vacuum on each filtration,-device, dispose of the
                   water eluate in the large receiver.   fflD.UOT UNCLIP THE
                   RESERVOIR FROM THE VACUUM HEAD.
                                 -;;  ,"-.  ,'l''  "•••
       15.5.2       Place a clean solvent recelwr^lover;-.the drip tip of the
                   vacuum head.      ~-           -    -:   ',-,'

       15.5.3       Add 5 mL hexane to e&iah d±§k~. If  additional filtration media
                   were used,  allow the hexaile  to  stand in the reservoir for 2
                   minutes prior to applying.-vacuum.

       15.5.4       Turnf*7acuum pump on.  Adjust,;pump pressure to 5 inches of
                   mer^mry.      '}%           '-"•
      15.5.5       SLOWLY open the;|»anifp;lds valves to  allow hexane to soak into
                   the /s&rbent b^dfj";'I&SJ'WSSt AUJ3W THE  HEXANE TO EUDTE AT THIS
                   TIME.   Close valves and allow disks to  soak for 2 minutes.

      15.5.6       After  2 mitra^es^, slowly open the manifold valves and collect
              ;  ;,:'S'fNtjtMnat into tfielr^ceiver tube.   APPLICATION OF EXCESSIVE
            f  !  ""  VAGOOH MILL RESULTpf ANALYTE LOSS.
         .'. f             ' 't:'^
      15|4S;7       Add a  secdppd volume of 5 mL hexane  to each disk and elute
      , J<-          under  vacu^an until the disk is dry.

           &       Proceed wim^cleanup of the hexane  extract as described in
              ;     paragraphs§3;5.6 to 15.9.
           "'•%  '* ^           '.Yt
             •-«.:a's.        "1;|
15.6  Sulfuric AcM =Cleanxij»:

                      ' ',r' ?'
      15.6.1       Usiiig4ia.isyringe or a volumetric pipet,  transfer the hexane
                   solution to  a 20-mL vial and carefully  add 5 mL of the
                   concentrated sulfuric acid in a fume hood.

                                   D-41-PCB-Q                           08/23/94

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                                                                    DRAFT

15.6.2      CAUTION:  Make  sure  that there is no exothermic reaction nor
            evolution of  gas before proceeding.

15 . 6 . 3      Cap the vial  tightly and vortex for one minute .  A vortex
            must be visible in the  vial.

15. 6. A      CAUTION:  Stop  vortexing immediately if the vial leaks.
            AVOID SKIN CONTACT;  SULFDRIC ACID BURNS.  "-

15.6.5      Allow the phases to  separate for at least 1 minute.  Examine
            the top (hexane) layer;  it &pould not be highly colored nor
            should it have  a visible einsulsion or cloudiness.
                                     .&
15.6.6      If a clean phase separation is achieved, proceed to step
            15.9.9.                ''M "V-      -:'

15.6.7      If the hexane layer  is  colored or: the emulsion persists for
            several minutes, remove the sulfurte'^acid layer from the
            vial and dispose of  it  properly.  Add [another 5 mL of the
            clean concentrated,, ,sulf uric acid.
                          "'* '''  "
                                            ,
            NOTE:  Do not  refiove  any'^sestoe/la-t tbis, stage of the
            procedure.       ::  .         -•" -'"     -:;;•''
                                ;,
15.6.8      Vortex the  sample aim allow *he phases to separate .
                                 ' ";'•• • '''3 '
15.6.9      Transfer the hexane layers to a clean 20-mL vial.

15.6.10     Add,«B.'additt«Aal 1 mL  of'ljfxane to the sulfuric acid layer,
            cap; and shake. :-|::^fhis  second'le&traction is done to ensure
            quantitative trsjfasfer of the^roclors and Toxaphene.
             -             ^ "xf

15.6.11     Reac^es the  sefee^-^^teslliyer and combine with the hexane
                '      15.9.9.
                         -
15 . 6 . 12     Add 1 mL of l||ift«|gent water to the combined hexane extracts to
        ; ; , ;r'-'-E«no>ve  excess "i;«^M&iric acid that may still be present.
            Vortex iand allow  the  phases to separate.
                    "its-
            Transfer tfcfc hexane layer to a clean 20-mL vial.

            If a water,||ayer  is evident in the eluate, remove by the
            addition dlflsodium sulfate as follows:  (Note: water
            injected/Jilto  the GC  may strip the analytical column phase
           :^afid may fjause  retention time shifts.)
           '•3< "' "•"?    •,, ,1'$

            15:6'j|5/l   Add 5 g Na2S04 to the eluate.
                             D-42-PCB-Q                          08/23/94

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                                                                           DRAFT

                  15 . 6 . 15 . 2    Decant the eluate and quantitatively recover the
                               Aroclors by adding additional hexane to  the
                                        Combine this hexane with the  eluate.
      15.6.16     Continue with  the potassium permanganate (paragraph  15.10)
                  and florisil  (paragraph 15.11)  clfsajftaps.iAs described below
                  if the  sample  is  heavily contaminated. :~ilf ,s,the sample  is not
                  heavily contaminated,  the potassium permanganate cleanup may
                  not be  necessary  and the laboratory may skip !pai|agraph 15.10
                  and shall  continue with the JEborisil cleanup (paragraph
                  15.11).                     ,-                      '•   ;

15.7  Potassium Permanganate Cleanup        -           ;

      15.7.1      Add 5 mL of the 5 percent ^aqueous jkjptassium permanganate
                  solution to the combined hexstie. fractions from step  15.9.14.

      15.7.2      CAUTION:   Make sure that there  is no exothermic reaction nor
                  evolution  of gas  before proceeding.   :?'\  ,.
      15.7.3      Cap the vial  t|ghl^;;ai»5j|ro|:tfx for 1 minute.  A vortex must
                  be visible  in thepvial'. ^''1^ X=';-- <;  -
                                   ,P •          |"g    ••", .;$' , •>'
      15.7.4      CAUTION:  Stop  the wrtexingJIaramediately if the vial leaks.
                  AVOID SKIN  CONTACT;  MTASSUM PERMANGANATE BURNS.

      15.7.5      Allow the phases to  separate for at least 1 minute.  Examine
                  the top = XheXj&ae) layer, it should not be highly colored nor
                  should' It have jk visible  en&lsion or cloudiness.
                     " *-           •£            •••• ,
                    •-tf>           • •;:           '•''•
      15.7.6      If a clean  phase^separation is  achieved proceed to step
                  ,15.10.9.       - Jr. .  „, , .....
      15.7.7      If tM; fejsxane layer  is  colored or the emulsion persists for
                  several -misates, remove the  permanganate solution from the
                  vial with a-,jglass pipet and  dispose of it properly.  Add
             , :  -.';• another 5 mL otf c&ean aqueous  permanganate solution.

                  NOTE: '%*-;:not remove  any hexane  at this stage of the
                  procedure.^-

     f^.7.8      Vortex the:,isample and allow  the  phases to separate.
     ' •'•*, - :A                   . I
       X.3&. ' -,                 ••'*•'
      15 '.J-^,.,,,   Transfer dberhexane layer  to a clean 20-mL vial.
      15.7.10   '^,'AQd an awitional 1 mL of hexane  to  the permanganate layer,
                  cagii;t:h^:;;Vlal securely and shake.   This  second extraction is
                  done^i^':ensure quantitative  transfer of the Aroclors and
                  Toxaphene.
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                                                                          DRAFT

      15.7.11     Remove the  second hexane layer and combine with the hexane
                  from step 15.10.9.

15.8  Florisil Cartridge Procedure

      15.8.1      Reduce the  volume of the combined:|jex«Jpe layers to 1.0 mL
                  under a stream  of dry nitrogen.   >'    :

      15.8.2      Attach the  Vac  Elute vacuum manifold to  a water aspirator or
                  vacuum pump with  a  trap installed between the manifold on
                  the vacuum  source.   Adjust.-tlbe vacuum pressure in the
                  manifold to between 5 and^O pounds of vacuum.
      15.8.3      Place one Florisil  cart£$4ge into the vacuum manifold for
                  each sample extract.      >\.i;.       :

      15.8.4      Prior to cleanup  of samples,  the cartridge must be washed
                  with hexane .  This  is  accomplished feynplacing the cartridge
                  in the vacuum manifold pulling a vacuum and passing 5 mL of
                  the hexane solution, through the cartridge..  While the
                  cartridges are S|sl:s%,-^ste4t ia tb&pJnanifold are washed the vacuum
                  is released and a racfe obtaining labeled 10 mL volumetric
                  flasks is placed  inside $&e manifold.  Care must be taken to
                  ensure = that the solvent guide from each cartridge is placed
                  ins jje SB£ the.iapipropriate ^fslumetric flask as the manifold
                  topj3i,s replacel|iiEnd that thVsorbent beds do not go dry
                        they havdifbeen conditioned.
                                       .
      15 . 8 . 6      Af^fefer-'-the voldaa^tacfcRi'^La^fess  are in place ,  vacuum to the
                              restored and the extract for each field and QC
                  sample scillxEtion  is  transferred to the top frit of the
                  appropriateilfl&risil cartridge.
                               '
      15.8.7;  ':  "The H^R in the  eibgi&ct concentrates are then eluted through
         £•'„?"      the cdl«aia with  9 mL of hexane and collected into the 10 mL
        j5         volumetrlfegflasks held in the rack inside of the vacuum
      _,  1:         manifold. ^
      i\ ;•.                    "t
      *l5,|f8*;8      Transfer t&e eluate  in each volumetric flask to a clean
        '<~ !>",:,:    centrifug^ftube  or 10 mL vial.  Use two additional 1 mL
            ' V":-:,rE, hexane rinses of the flask to ensure quantitative transfer
                -vJ>,o£, the cartridge eluate.
                   ';.     'A*  '

      15.8.9      Concentrate the  solution to a 1.0 mL volume using either
                  nitrogen blowdown or micro-Snyder column.  Measure the final
                                   D-44-PCB-Q                          08/23/94

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                                                                           DRAFT

                   volume with a clean syringe  or by transferring the extract
                   to a clean volumetric flask.

       15.8.10      If crystals of sulfur are evident or./the  presence of sulfur
                   is suspected, proceed to paragraph 15.12.   Sample analyses
                   showing the presence of sulfur are iw>t/;a.cceptable and must
                   be reanalyzed after sulfur removal.

       15.8.11      If sulfur is not expected to be a problem,  trscasJer the 1.0
                   mL of sample to a GC vial an«tMabel  the vial.   The"' extract
                   is ready for GC/ECD analyses; proceed to  paragraph 18.
                   Store the extracts at 4«C *|± 2°C) in the  dark  until analyses
                   are performed.                       ,.;

15.9   Sulfur Removal                                :
                                              >/ 1    *;-:
       15.9.1       Bright (unoxidized) granular copper  is used to remove sulfur
                   contamination.  Add one to three granules of copper to each
                   hexane extract in a clean vial.  Tightie»  the top on the vial
                   and shake for 3@; s^ecpnds.  Filter or centrifuge and then
                   decant the solt3GC:i«4'V«tjd,peespve, all solid precipitates.  If
                   copper appears b^ght/'lti^olfiaragraph^lS.   If copper
                   changes color, repeat sulfur^fas&moval -as: necessary.

       15.9.2       If only a partial set;of tile samples in the Batch require
                   sulfur cleanup, an additional reagent  blank of hexane spiked
                   with the appropriate amoamt  of the SMC solution and cleaned
                   with the copper is required.
                         K '    ^M, ,';';          '  i-
       15.9.3       Proceed to paragraph 18 f or!  0C/ECD analysis.

16     Sample Preparation and Extaeajcttion. -	Oil  Samples
      NOTE: The Aroclors tsarlet compound CRQL for oil samples  is  2000 jtg/k§
            for 1221;  5006.?j£g^kj for toxaphene; and 1000 fig/kg for  the other
            Aroclors.        " ;2i,
16.1  Add li,§%"bf 'saofft^j-jto a 10 iSD,g86olumetric flask.   (Oily mixtures should
      be phase -separated according to the procedures in  paragraph  13 of the
                               ,
16.2      1.0 mL  of  SMC (0.2|pg/mL) to the sample.
     '~~'r ?',;: -                   ^ / ,
        A  ',,,_                 f',t
16.3  Add'tjfiJRane  to  the volumetric flask until reaching the  10 mL meniscus
      mark.'"'-"-\^:         . £•
                *''**•  "'- *     •'.''•/*•
16.4  Cap with  stoppeafiarast'mix for one minute.
                      • • ;'; S,

16.5  Pipet exactly  1.0 mL out and proceed with clean-up and final
      concentration  as  specified in paragraphs 14.3 - 14.6.

                                   D-45-PCB-Q                           08/23/94

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                                                                           DRAFT

17    Sample Preparation and Extraction - Wipe Samples

      A wipe sample  containing PCBs is serially extracted with  two  portions of
      hexane using an  ultrasonic probe.  Extracts are combined,  filtered,  and
      dried through  powdered anhydrous sodium sulfatfis,'and concentrated to a 1
      mL volume using  the nitrogen blowdown procedure. ,

      NOTE: The target compound CRQLs for wipe samples will %e  specified by
            the Agency.                                            >f,
                                              •*'                      ~*
17.1  Pour off any free solvent from the sample jar into a clean Erletsaeeyer
      flask of appropriate size.            =

17.2  Spike the sample with 10 uL of the .SHE, (2.0 ug/mL).
                                            , "*"'> \
17.3  Add enough clean hexane to the sample jax*to ;ce  '
17.4  Sonicate at microtip  maximum *f«»wer;  cool'-ftie 'sastple during  sonication.
      The sonicator must be set for SIKpercenii pulse action.  Sonicate for 3
      minutes.  The power output may have  to^lse adjusted to ensure  that the
      sample extract does not splash excessively; any significant loss of
      sample during sonication is not acceptable.  Rinse the sonicator tip
      after each sample , -extraction with 1  mL spf hexane.
                        '      '  - -"-           ",' 5-
                       - \'        V -v'V          "-•"^ ^
17.5  Remove the hexase' layer frcfflC,the sonica~€pon and combine it  with the
      hexane in the ?i!rlenmeyer fl^jsk.         '

17.6  Repeat steps' 1?. 3 v- 17 . 5»,C"?W •Jf-L'-",^- ,r '

17.7  Filter the combined '«4*a**cts by gravity  filtration.
                               -, <
      17.7.1  A "^Frepare  a fil't^tsiojti/drying bed with Whatman #42  filter
           ..i/-f*r ""'"~tia'Pie*-<-Silled with^'Aproximately 15 grams of powdered
          •™-.Jg^--     * *  s«\ Jf & •.          ^@,^l; ,r    mL hexane /?mn& transfer rinse solvent to powder funnel.
            ^''H:'^. Rinse powl®: funnel with 10 mL hexane.
17.8  Concentrate «etag*c*^*»  approximately 20 mL using the nitrogen blowdown
      procedure in a'3&HJ*water bath.   Transfer extract concentrate to  a clean
      25 or 30 mL concentrator tube,  and rinse concentrator tube  (from
      paragraph 17.7.1) with  5 mL hexane.  Transfer the rinse  solvent to the

                                   D-46-PCB-Q                          08/23/94

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                                                                           DRAFT

      25 or 30 mL concentrator tube,  and concentrate further to approximately
      1 mL.  To minimize  analyte loss due to volatility, occasionally rinse
      sides of centrifuge and concentrator tubes with hexane during the
      blowdown procedure .

17.9  Proceed to extract  clean-up steps (paragraphs 14,3 - 14.6).

18    Instrumental Analysis

18.1  Set up the GC system per the requirements, in paragraph 7.   !-   '
                                             ir  '                        • ;
      18.1.1      Solvent-flush manual injection or automated sample injection
                  is recommended for  analysis.

      18.1.2      An analytical sequence consists of field sample analyses and
                  all associated standards,  b'laaoks , , and QC analyses performed
                  within  a 24 -hour period on one instrument.   There are two
                  (2) types of analytical sequences* «» initial calibration
                  analytical  sequence and a  daily califerat&on check analytical
                  sequence.  All samples shall  be analyzed within one of these
                  analytical
                  • 18.1.2.1    An  iiiicial  calibration • -analytical sequence
                              begins qsfith a  t&fjsee-point calibration of Aroclor
                              1016/1260.;:followed by single-point analyses of
                              the other :Ax®c3x»rs and toxaphene,  an instrument
                              blank, an 1CS, and a  method blank.   The initial
                         r..  -^calibration analytical sequence is as follows:

                    >; <:'f      • 'r ,:, Initial  Calibration (analysis of the high
                    ?>              ~ 1016/1260  standard proceeded by the mid
                  I  "           r. ; ^and^lpw, v1016/1260  standards followed by
                   ; =•  ;-,-        ,:;:a'-';-l!:^|33^1s^ipoint analyses of the other
                       s   ~          Aroclors and toxaphene) ;
                             *•
                             "• : ;* ;(/;   Instrument Blank ;
                  "'*.  •' m         "' „ ; - ,
                  "'  ; - {; j -^    •   Ji1I*aiboratory Control Sample(s);
                       ^ '*$$<-
                         ^;1S •     Method Blank(s);

                             ^*     Field Sample(s);
                             Si^
                            jv5:-     Instrument Blank(s) ;  and
                          .-'K
                  .]:>•     ,A    '     Performance Verification Standard(s) .
                   s'-  "$.' *"
                  18.li~2.vl    A daily calibration check analytical  sequence
                              begins with an instrument blank, a valid
                              calibration check standard,  a method  blank,  and

                                  D-47-PCB-Q                           08/23/94

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                                                                    DRAFT

                        an LCS .  The  daily  calibration analytical
                        sequence is as  follows:

                        •      Instrument  Blank; ;,

                               Calibration Check 'Standard (1016/1260);

                               Method  Blank(s);         .   ,

                        •      LaboratorydGontrol  Sample(s);    ;

                               Field Sample (s) ;
                                    A"'           :
                               Instrument  Blank(s);;  and
                                   : ;           s; - ,
                        •      PerformaneeSerJJIication Standard(s) .

18 . 1 . 3      If all acceptance  criteria for  thesi?  -analyses are met , then
            the Laboratory may proceed with sample. analyses .
                            , ••    i.
18.1.4      All analytical :;sie<|u4p«^ '^nclude with an acceptable
                                   >
' ^ -' V '< -
 '*'•;>'
     -i
            instrument blanM^iand a'sfW>ssaitysis. , , The PVS shall be
            started within 2&: hours  afte^^hen Injection of the first
            initial calibration|s,tandarjdllor the first instrument blank
            in the daily calibration sequence.  NOTE: If a PVS
            reanalysis is required ^because of a non-compliant initial
            PVS analysis, the PVS reanalysis must  be started within 26
            hours ,a!f teethe start of-'-Ejte current analytical sequence.
               ,.r;  " :'-|           '£
18.1.5      The.'isethod blall:~and all associated samples shall be
            asllyzed in th^issame analytical sequence.  If samples from a
            fetch are anal|^d^J.n,,jtiqr.e,, than one analytical sequence, the
            associated m«tMiSifta^«si&t also be analyzed in the same
            analytical sequence .  If a  method blank extract is used up
            because : 03| stai^ltiple analyses,  the Laboratory shall
            substitute' ' #j& instrument blank in place of a method blank in
           : -all ^subsequent ,&3Balytical sequences.   The Laboratory shall
      v-'"-   'hbt«^as4.s in the"1ESj|fech Narrative and shall use the EPA
   J'l  "'      identiMoation number as described in  Exhibit B for this
  C'ti        instrumei&^blank.
  .1.6      The LCS shfH be  analyzed with all associated samples in the
            same analytical sequence.   If samples from a batch are
            analyzed ik*more  than one analytical sequence, the
            associatecUSLCS shall  be analyzed in the same analytical
         s< - i;sequencei;: If an  LCS  extract is used up because of multiple
            aofli;Lys«s;  the Laboratory shall dilute the LCS standard
            mixta«Ci£ (the original stock mix) and use this solution in
            place of the original LCS sample in all subsequent
            analytical sequences  (see paragraph 27).  The Laboratory

                            D-48-PCB-Q                          08/23/94

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                                                                           DRAFT

                   shall note this in the Batch Narrative  and shall  use the EPA
                   identification number as described  in Exhibit  B for this LCS
                   solution.

18.2  Computer  reproductions of chromatograms that ascei- attenuated to  ensure
      that all  peaks are on scale over a 100-fold range are  acceptable.
      However,  post analysis attenuation shall be n6  greater than a 100-fold
      range.  This is to reduce the potential for RTSs of quantitation peaks
      due to  column overload and to ensure that the detector is"  ojpexating
      within  the  calibration range.  If any sample quantitation  peaJfcs^>exceed
      the calibration range (greater than the''high concentration level; of the
      1016/1260 initial calibration),  they shall be diluted  according to
      paragraph 19.                        ,  i:

18.3  If any  saturated non-target compound f^sjsomatogjraphic peaks are  evident
      or if any chromatographic peaks overlap -mate -titan one  RRT  and/or RT
      target  compound quantitation windows, the Laboratory shall use  the "E,N"
      flags on  Form QIA-PCB to indicate this situation.

      18.3.1       If saturated chr^aaatographic peaks  outside target compound
                   quantitation RSSSi^a^/fOt-Bf .-windows  are  evident, flag the
                   nearest target compound *&ylf* MH^forja QIA-PCB.

      18.3.2       If chromatographic |»eaks overlapping more  than one  target
                   compound quantitatiowiSRT^aikl/or RT windows are evident,
                   flag the corresponding 'target compound  quantitation peaks
                   "E,N" on Form QIA-PCB.  :>.
18.4  Chromatographic peak response of the quantitation peaks must be
      greater than  Iphpercent aridVilbess than tdQ percent of full-scale
      deflection to;*nsure that iralividual quantitation peaks and
      Aroclor patterns  will be visible^duri^n^ data review.
                    > -  ' •..•.          ^' ''^ ••  "f -.  * ,' .. '**'"'
                       '•'••>;<•-       ''?. iff""- -„••:!-,.  "N  „*" 'ia
19    Dilutions       "r  ;  =

19.1  Samples with  quantitati%irifj»eaks larger than high level 1016/1260  initial
      calibrat356li:~:;$pafes must be"5si^NEp:,ted with the "E" data flag as described
      in ExMiMt:f
-------
                                                                          DRAFT
20
20.1
      concentration that exceeds  five  times  the  concentration of the low level
      initial calibration standard,  then the undiluted sample shall be
      reextracted and/or reanalyzed at no additional  cost to the Agency.
      19.2.1
      19.2.2
      19.2.3
      19.2.4
      19.2.5
                  At the request  of the  Region,  sample dilution may be
                  required prior  to the  initial  extraction and analysis.  If
                  no Aroclors  are detected in the  diluted sample above five
                  times the  concentration of the low initial calibration
                  standard,  then  the undiluted sample shall be-cefeattracted and
                  reanalyzed as an additional paid sample.         , „  „,

                  Dilutions  -  Solvent extracted, oil,  and wipe samples
                  19.2.2.1
                              Dilutions  of/.solvent  extracted,  oil,  and wipe
                              samples  shall be .made by using an appropriate
                              aliquot  of the 'iaptBact? diluted in hexane.
                              After making a  dil^rti^n.^  add sufficient SMC
                              solution to bring  up  lid -Spc0per concentration (20
                              ng/mL).                    :  .
                  Dilutions  -  SPJJvextr«cted -samples
                                 ,-•' •    * "'"• '•'  ".'" . ,"•,',"•' •. *
                  19.2.3.1
                              Dilutions  of water  samples shall be made by
                              using a»,;rapprop3:Jiate  aliquot of sample diluted
                              to  100 T&L with-«ethanol/water (5:100)  (see
                              paragraph 1S^2).  Continue with sample
                              extraction and cleanup  as  described in paragraph
                                      Dilute samples  prior to the addition of
                  Saatple diluti«ys5jihill be analyzed in a valid analytical
                  sequence which  includes the  associated method blank and LCS.
                           j *
                  If sample r«ea:^.r.actions and  reanalyses are required, the
                  laboratory  shi^^lso  reextract  and reanalyze an associated
                  method jolank
      Identification of Ar'ajjsprs
          analyst shall conster  the Aroclor pattern in addition to specific
                   peaks.  T^e: choice of the peaks  used to identify and
                 Aroclors may-Sbe  complicated by the environmental alteration
      of the v$*a,tstern and byf'Sje presence of co-eluting compounds or matrix
      interferetobess^  The.diEnre highly chlorinated components of Aroclors are
      more stable lia ;|sbe#;|%svironment.   Therefore, the analyst should emphasize
      the later eluting«.^eaks  of  a pattern in identifying weathered Aroclors.
                                   D-50-PCB-Q
                                                                       08/23/94

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                                                                          DRAFT

20.2  Retention Time  Standard -  The  SMC  shall be used as the RT marker for
      compound identification.   The  SMC  shall also be used to monitor
      extraction efficiency.

      20.2.1      The SMC  shall  be added to  all field and QC samples prior to
                  extraction.                        , -  "

      20.2.2      In  each  analysis,  the  SMC  RT must be  within! $ 1.0 percent of
                  the mean RT of the SMC calculated from the 1014^3,260 initial
                  calibration standards.      ,,                    '\

20.3  Aroclor identification  when SMC recovery is greater than or equal to 10
      percent and less than or equal to  200 percent.   ; ;

      20.3.1      Quantitation peaks shall;%e identifijed on the basis of RRT
                  in  all field samples for whicil the.JSMC recovery is greater
                  than or  equal  to 10 percent and' less  than or equal to 200
                  percent.                            i

      20.3.2      Peaks in samplefcbromatograms shall be identified as
                  quantitation pessfcs:J£;£toef*,£&? is within ± 0.005 RRT units
                  of  the RRT  established ftom-aatee-lotir calibration standard
                  during the  initial!' calibration.   ;   "  !
                                      :-        8
20.4  Aroclor identification  when SMC *e«overf is less  than 10 percent,
      greater than 200 percent,  or if peak (interferences are present.

      20.4.1      Quantitatlsn ;pe,aks shall "fee identified on the basis of
                  absolve RT la/|all field sapples for  which the SMC recovery
                  is-..less  than ioftfercent, greater than 200 percent, or if
                  peak interferences are present.
                  -;-,"            &>i:
      20.4.2      Peaks in samplfesiiarda3iog3rams shall be identified as
                  quantisation peaks if  their absolute  RT is within ±1.0
                  percent  ^f\ii|jhe RT  established from the low calibration
                  standard difrlt*g,-,the initial calibration.
                              identified on  the basis  of absolute RT shall be
                  flagge&p££h the qualifier "T"   (See Exhibit B) .
                           -'-A'
                  If the recovery of the SMC is less than 10  percent,  greater
                  than 200 p^cent, or if peak interferences  are present for a
                  sample, acceptable recovery of  the SMC must be obtained in
                  the assocMjfaed method blank and LCS  (see paragraphs  25 and
20.5  If multiple p!eakSyar« within the identification windows  (target compound
      and SMC) ,  the La&fostory shall use professional judgement to properly
      identify the appropriate peak.  The Laboratory  should  consider the
      inherent matrix effects of the sample on peak shifting,  masking,  and

                                  D-51-PCB-Q                           08/23/94

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                                                                           DRAFT

      overlaps  when making identification determinations.  The Laboratory
      should take  into consideration the mean RT and RRT from the initial
      calibration,  RT and RRT from the calibration check standard, and  the  SMC
      RT  from relatively clean samples analyzed beforehand after the sample in
      question  as  a basis for selecting the most appropriate peak.  The
      Laboratory shall describe in the Batch Narrative-- the rationale used for
      choosing  a particular peak (e.g., chose peak Closest: lap the RT of the
      peak in calibration check standard) as the target com£oo»d or SMC and
      how the field sample matrix may have affected peak identification.

21    Calculations                           :, ""•                      ':'  ;

21.1  Calculate the RRT of a sample component or a standard using the
      following equation:
                              DOT* —        CCrapODfiDt  ;<             T?O  T\ 11
                              .fuv J ™ ' *•" ••   ••  "     'ff^             *^^ • *^ • J» J.
                                          ***•          f.^  ^ .

                                   •^
      Where:                     ,JJ-^-^V:3-  V  ,-

      RRT = relative retention time - -         , ' ,'    •'; '

      RTcomponent = retention time of 4ftie target compound

      RTSMC = retention time  of the SMC

21.2  Samples will be^xmntitatagd^using the 'Calibration factors determined
      from the low co^teentration|&oclors standards from the initial
      calibrations. ,1|(NOTE:   The l^pc concentration shall be calculated using
      the mean SMC,,-calibration f^^o^  calculated from the  1016/1260 initial
      calibration standards) .   ,:;Jilf,»;S-;;141  , i;y

21; 3  Quantitation of PCBs sjas.jAroclors

      21.3.1    ,  "Tlie concentra'ti^j^pf an Aroclor in a sample is calculated by
           ,;|-,;  '''-av£ra||Hp,g the conjurations of the individual quantitation
          ;,-/!-      peaks/"-pfee response  of each peak can be measured by either
        ,r,|-       peak heigpfc. or integrated peak area measurements.  Because
      ,^7'         the quantisation peaks  are not specified by the method, it
     4-;,;A          ^s require
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                                                                     DRAFT

             peak common to both compounds present  in  the  sample must not
             be  used to quantitate both compounds.

21.3.3       Water


                Concentration (pg/L]  = .__ */^v*  .    >-•      EQ- D-12
            where :                      ,                          •••

            AX    =     response for the peak to Jbe measured

            CFm   =     calibration factor of ,fisantitation peak
                         established from -fjfee,, Low concentration standards
                         calculated during the Initial calibration.
                                                   . .
            Vt     =     volume of total extract (;^L) r(take into  account
                         any ••'dilutions ) .              :
                                         .
            Vi     =      volume, of ext±set^ injected

            Vs     =      volume j,«sf, water ^attracted (mL)
                                       '•!-.
21.3.4      Soil/Solid (Wet- weight basis)  and Oil
                                                                .  D.13
              ,, CFm, "Vj,/"* sesame  as  given in Equation D.12

              :-L-:T     voluae;;=
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                                                                           DRAFT

                  An average concentration of the three to five quantitation
                  peaks  for the Aroclors is then determined using  the
                  following equation:
V* 2i
h «
                                                                  EQ.  D.14
                  where:                       -.'

                  Concavg = mean concentration.
                                            '""*'
                  Xi      = individual pea$| concentration.

                  N       = number of peaks.
21.4  Calculate the  SMC  amount observed and amount (pef-cetit) recovered  using
      equations as described in paragraph 10.4.
21.5  RTS shall be monitored usingfthe SMC'^^SilagEaph :2fl.2) .  The RTS  shall be
      measured for all  analyses.   Y" '    .      ,-S

      21.5.1      Calculate the retention tiae percent difference (RT  %D)
                  between the RT of the SHCj/in the field and QC samples  or
                  subsequent standards analyzed and the mean SMC RT from the
                  most  reeftst 1016/1260 initial calibration standards  using
                  the £«.llowingi! equation:    ~
                                                                      . D.15
                  where:    '" <\ "

                  ^^£I!M'«-_i    retefit^>n time percent difference.
                        *•" ;^' •
                  RTS   = %; r;v retention time of the SMC in a field and QC
                             ?;-sample or subsequent standard.

                  RTC   =    ;,,|JBean retention time of the SMC from the  most
                            -i ?recent initial calibration (mean RT of the
                           _.-;'-H: 1016/1260 SMCs analyzed during the initial
                  :•'••.     (•'•''  calibration).
                                   D-54-PCB-Q                           08/23/94

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                                                                           DRAFT

 22     Technical Acceptance Criteria

 22 . 1   Each sample within a Batch shall be analyzed on a -€C  system meeting the
       initial  calibration or valid calibration check standard technical
       acceptance criteria (paragraphs 8 and 9).     ,  I

 22.2   Each sample within a. Batch shall be analyzed after an acceptable method
       and instrument blank,  (paragraphs 25 and 26) and after- ass -^acceptable LCS
       (paragraph 27) is analyzed.                              :', „;:

 22.3   Each sample within a. Batch shall be run.fwi.thin a valid  initial   ;
       calibration or daily calibration check analytical sequence that
       concludes with an acceptable instrument blank (paragraph 26)  and an
       acceptable PVS (paragraph 10).     "\           ,*;

 22.4   Each sample within a Batch shall be analyzed and results reported within
       the contract required turnaround times .      'i

 22.5   Each sample matrix within a Batch shall have an acceptable method blank
       analyzed during the same analytical sequence.
22.6  The RTS  for  the  SMC RT must*%«; within- iv^Sspercent;, between  any sample
      in a Batch and the mean RT of -jiiie SMC cal^iated -ficiom the  1016/1260
      standards analyzed during the iialtial calibration.  The RTS  is  not
      evaluated if the SMC is not recovered s&r' if peak interferences  are
     . present.

22.7  The advisory recovexjr.l&it for the S&C is 50-150 percent.   Reanalyses
      of field samples, aire not made if the SHG .recovery is outside the
      recovery lirnts,,^/'.         "', ;            ,
                    '''••           j ,,v
22.8  The SMC  recoyer^ must be gJpesSLte, r,,ghan, or equal to 10 percent and less
      than or  equal '>«fe 200 perce&'SHt.-oic^fcfco use RRT for identification
      purposes.  The idiatitfification window is ± 0.005 unit of the  RRT for each
      quantitation peak in'it&e low concentration standard analyzed during the
      initial  calibration,  it fhe^ recovery of the SMC is less than 10
      percent^, ,!^r^ac«sr.- than 200 ipeajfeent,  or if peak interferences  are present
      (but is ^aldequa1Sfe^;|secovered sin -the method blank), the absolute RT of
      the |c«mpounds shaiiv|je used for identification purposes.   The
      id«Bitification windowV;ts ±1.0 percent of the absolute RT  for each
      q^fititation peak in tltet, low concentration standard analyzed during the
        ttial  calibration.  ;-'i<\
23    Corrective Action      ?"
               ••A, 'i           ' '''
23.1  Flag all'sample results  "S"  if the SMC is outside the advisory recovery
      limits of 50'--ljto gjesrbent.

23.2  Flag all sample results  "T"  if the absolute RTs are used for
      identifications.

                                   D-55-PCB-Q                          08/23/94

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                                                                          DRAFT

23.3  An SMC recovery of less than 20 percent in the method blank  or LCS
      associated with a sample Batch is an indication  that serious problems
      may have occurred during the extraction process . ^Corrective action
      shall be performed and the unacceptable method MLank and/or  LCS and all
      samples associated with the unacceptable method  blank and/or LCS shall
      be reextracted and reanalyzed at no additional %xp"esse  to  the  Agency.

23.4  If the SMC RTS criterion is not met for any 'field sample, «sample
      analysis shall be stopped and the noncompliant sample rer^d^s  If the RTS
      criterion is still out upon reanalysis analyze an instrumenC!4"biank.   If
      the instrument blank SMC RTS is. outsidefFtihe criterion,  perform  '
      corrective action which may include a _,^sste4,jiniJExhibit B.
                     '
                                  D-56-PCB-Q                           08/23/94

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                                                                          DRAFT

                                   SECTION V

              SAMPLE QUALITY CONTROL PROCEDURES AND REQUIREMENTS

                                                       \
25    Method Blank Analysis                        , •-••

25.1  Summary - A method blank for water samples is 100 mL o€ reagent water
      spiked with the  SMC  and carried through the entire analytical scheme.  A
      method blank for soil/solid samples is  6v.j* of clean quartz saaiol spiked
      with the SMC and carried through the  entire analytical scheme/ 'A- 'method
      blank for oil samples is 1  g of clean eorn oil spiked with the SMC and
      carried through  the  entire  analytical scheme.  Method blanks shall be
      carried through  the  entire  analytical .procedure J ;

      NOTE: The Agency will provide  the LaboraifcsKegr .srith further instructions
            for the analysis of method blanks for »%e samples .

25.2  Frequency                                         !

      A method blank analysis sbeM-'-ft^-^ea^B^Bked for each matrix type (water,
      soil/solid, or oil)  and wittii/
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                                                                          DRAFT

      25.2.4      Criteria  for  an acceptable  method blank is  defined in
                  section 25.4.

      25.2.5      If all  field  samples  in a Batch  are filtered,  the associated
                  method  blank  shall  also be  filtered.  If only  a partial set
                  of samples  in a Batch are filtered,:$ken a  separate method
                  blank shall be run  through  the filter,  extracted,  and
                  analyzed.                                 L ',

25.3  Procedure for Method  Blank Preparation  ,-/-,                  : :
                                            ,!«-,!'"                    '  $"
      25.3.1      Prepare the method  blanks^Af the frequency  listed in
                  section 25.2.           ^ '"          /

      25.3.2      Measure out 100 mL  of reag«nt wate;r for each water method
                  blank sample  aliquot.
      25.3.3      Soil/solid method blanks are  6 g '-of clean quartz  sand.

      25.3.4      Prepare water  and soil/solid  method blanks' as  described in
                  section 14 or  l3;^i|^e^B|i^g«,on whether  solvent  or  solid phase
                  extraction is          '        *
                                               . ,
      25.3.5      Spike 1.0 g of corsk oil withll.O mL of SMC  (0.2  /ig/mL)  and
                  proceed with the Aroelors/jftEocedure (sections  16.3  -  16.5).
                                        ,,  ,, i '•*/;
      25.3.6      Analyze the method blaflk^sxtracts .   Calculate  the results
                  according t&. ^section 2 IT;. ,
                      ••       '" * f          ''1\>S",
25.4  Technical Acceptance Criteria          '";=;
                   >•'-''           & ,
      25.4.1      J&.1 method blaj^ks shall be analyzed within  an  acceptable
                  aloaiiy^ical sg^^^j^^t^^  system  meeting  the initial
                  calibration (section 8) or valid calibration check  standard
                  (section ^^ criteria, and the PVS acceptance criteria
                  (section
                          RT in the^thod blank must be within ±1.0 percent
                  of th^liiean SMC RT ' calculated from the 1016/1260  initial
                  calibrafci|op,, standards.
                  The SMC re^^ery criterion of 50-150 percent  is  advisory
                  only.  The|-J|IC recovery in the method blank must be greater
                  than or eq^il to 20 percent and less than or  equal  to 200
                  percent. i*'%'
                  *       f" ^ -
      25.4.4      %sttt^,«ftion peaks or potential  interferences  in the method
                  blanfejj, aiust have a response less  than  one -half the  response
                  in the corresponding RRT window  of  the initial calibration
                  low concentration standard.

                                  D-58-PCB-Q                           08/23/94

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                                                                          DRAFT

      25.4.5      A method blank may contain a detectable but acceptable
                  concentration of a target compound,  quantitation peaks, or
                  interferences (less than one-half the response of the
                  initial calibration low concentration standard) .

      25.4.6      If all criteria are satisfied,  the 'teethed blank analysis is
                  acceptable and samples  may be analyzed.  :If the method blank
                  is unacceptable, corrective action shall "be, taken and an
                  acceptable method blank must be analyzed priorVlto analyzing
                  the associated samples.     ,                    '    ;
                                              X
25.5  Corrective Action                       '•'

      25.5.1      If a method blank does  **$£ meet the .technical acceptance
                  criteria, the Contractor' jsifaiall  consistler the analytical
                  system to be out of controli° jitlt its" the Contractor's
                  responsibility to eliminate m£tho& interferences  caused by
                  contaminants in solvents,  reagents^&artridges, disks,
                  glassware, and other sample storage  iitd processing hardware
                  that lead to discrete artifacts and/or elevated baselines in
                  gas chromatogramsl :;.|fe j^oatamination is a problem,  the
                  Contractor shali^|fi,nvest;fga*«Mfp»>, source of the
                  contamination, anil; appropriate  corrective measures shall be
                  taken and documented before further  sample analysis
                  proceeds.           s ,     ,->>,-
                                            ' * *':-
                                         \'  t
      25.5.2      If a compound is found •;!«; the method blank (less  than one-
                  half the;=i3ispaiise in the -.Corresponding RRT window of the
                  initial calibration low concentration standard) and is also
                  detected in an Associated field sample at less than the
                  CJKgL', the compo^ad shall be reported as a nondetect,  i.e.,
                  with a "U"
      25.5.3      If the SMC recovery in the method blank is  less  than 20
                  percent, , greater than 200 percent,  or  if peak interferences
                  are present., '^"ttxe method blank shall be immediately rerun.
             ;    ?,J.£ -:an reanalyslpithe method blank SMC  recovery is  still
            .j     cmtsxidte the recovery- limits, the method blank and  all
         >'  "'     associated samples shall be reextracted and reanalyzed at  no
         :         additional -.cost to the Agency.

      =25.5.4      Flag all m6pbod blank results "S" if the SMC does  not meet
     '• ,/ts         the adviso^ recovery criterion of  50-150 percent.

      25.5.5'  v, r,If the R^S,^briterion is not met for a  method blank,  sample
               '•'  analysesjMiall be stopped and the noncompliant blank rerun.
                  llE L*jae$GfcS criterion is still out on reanalysis, perform
                  corrective action which may include a  new initial
                  calibration.  DO NOT continue with  sample analyses until the
                  RTS is within ±1.0 percent.

                                  D-59-PCB-Q                           08/23/94

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                                                                          DRAFT

      25.5.6      Any samples processed with a method blank  that  is  out of
                  control  (i.e., does not meet any of the  technical  acceptance
                  criteria) shall be reextracted and/or .reanalyzed at  no
                  additional expense to the Agency.

25.6  Documentation                                    '.  ,

      Method blank results are reported on Forms QIA-PCB,  QIB-f£B, and QVI-
      PCB.  Reporting requirements are listed in Exhibit B.

26    Instrument Blank Analysis

26.1  Summary

      An instrument blank  is 1 mL of hexarie jspiked witHi 10 ^L of  SMC (2.0
      jig/mL).  At least two acceptable instrument blanks shall be analyzed
      within an analytical sequence, one preceding Sample  analyses and one
      following sample analyses.                    "!
                                                       ™<
26.2  Frequency                  ,•• ,                         ;<
      An instrument blank shall b% Analyzed 'A^iteast , twice during  the
      analytical sequence to ensure ijtiiat the i^tst:rumeifc ,is free from potential
      contaminants.  The first instrument bla^fe analysis shall be  performed
      after the initial three -point caM.brafci.dn in the initial calibration
      analytical sequence or as the first; analysis in a daily calibration
      check analytical sequence.  The seebnil instrument blank analysis  shall
      be performed immed^^eslyjbefore the BKS analysis.  The Laboratory is
      encouraged to run-SsdaitrtSjBBStJ instrument:! blanks during the analytical
      sequence, especially when ^ghly contaminated or complex samples  are
      analyzed.  Instrument blanks must be analyzed after analysis of samples
      with high levels of targe t^i&Dmpounds or interferents (see section
      26.5.6).    ''•'   y       .:iM;:^~,tki. ?''-•'

26 . 3  Procedure for Instrutteftt Blank preparation

      An instrjpeent fclank is I'mL^.hexane spiked with 10 /iL of SMC (2.0
         ,•.,
26 . 4  Calxsalations
     /f&mcentrations of the ^tC and any quantitation peak in the  instrument
     4tta$k, are calculated ai^eording to the procedures described  in  section
      21". '-tlto^e: The target ^dmpound concentrations (detected concentrations
      and CRXlif^alues) in ti^ instrument blank shall be  reported  in  the
      appropri^tseKeoncentss&tiion units  (e.g., report in /*g/L if  the associated
      samples are water and in fig/Kg if the associated samples  are soil).
                                  D-60-PCB-Q                           08/23/94

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                                                                           DRAFT

 26.5   Technical Acceptance Criteria

       26.5.1      A minimum of two (2) instrument blanks ;shall be analyzed
                   during an analytical sequence  on a GfC system meeting the
                   initial calibration (section 8)  or *i?win^aks,  or interferences at
                            up to twice :,the CRQL (2x CRQL).
                       - "*        "~£           -<<
      26.5.6       Following the Sfaalysis of a -field sample  containing high
                   legjl&ls of target compounds or interferents ,  an instrument
                   ,b!6nk shall beJjiaSfalyzed^and must meet  acceptance criteria
                                                 analyses.   If  an autosampler
                   is utilized, then the field samples run after a high level
                   sample i*uft:,;;ibe carefully evaluated for  carryover.   The field
                   sample imme^KLki^ely following the high level  sample shall be
                 , -pesanalyzed, a5«bg-;.with any other samples analyzed after the
            ,U.:  • ' "M'gttfJLi^wel sample!--isS|ich shows evidence  of carryover.

      26.;S,7       High levfei'^samples are defined as being field samples that
       s»f the nearest target compound or quantitation
26.6  Corrective Action
                                   D-61-PCB-Q                           08/23/94

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                                                                     DRAFT

 26.6.1      All  groups of samples analyzed shall be bracketed with  two
            acceptable instrument blanks.   If either instrument blank is
            unacceptable,  corrective action shall "be taken and all
            samples  not bracketed by two valid instrument blanks  shall
            be reanalyzed at no additional expense to the Agency.

 26.6.2      If the response of any target compound «or «|uantitation  peak
            in an instrument blank analyzed after the initial
            calibration or before a valid calibration cheek standard  is
            greater  than or equal to one;-1ialf the response i« tfae
            corresponding RRT window of itshe initial calibration low
            concentration standard, corrective action shall be performed
            and  the  system shall be .demonstrated, tso be clean by the
            analysis of additional j&strument blraiiiks until all target
            compounds and/or quantitatgton peaks'ikre within QC limits.

 26.6.3      If any target compound and/or quaatitation peak in an
            instrument blank analyzed after fieSJi^QC sample analyses  is
            greater  than two times the CRQL, anotis&r .instrument blank
            shall be analyzed*  If, on reanalysis, contamination  still
            exceeds  the crJi|e-M*^r -Cjjarxaectiye action shall be performed
            and  the  system aiei»onstrasi!eifeS^,i*e::clean.  Then, all
            associated field/I^C samples Analyzed since the last valid
            instrument blank or method jjjarik which contain those  target
            compounds, quantitafilon peafes, or interferents found  in the
            instrument blank at iWels ^greater than twice the CRQL  shall
            be rerun.              ' ;'„;''

 26.6.4      If a?l itistrumesiit blank (ot&er than the first instrument
            blaaafc in the analytical seqifiepice) contains target compounds,
            qaaatitation peilSS, or interferents between one-half
            response and tjKM^uaejs J^he. ,CRQL, all positive results
            (resa3.£s greattwd^aTOt^'^iual to the CRQL) for those
            compotsEBJs in samples analyzed after the last valid
            instrumeaty&lank shall be flagged with a "B".
                        '-. 'f '""
 26 .6.5 ,  „;; lElsig all instrtaaiaaait blank results "S" if the instrument
      |;:; -:  T>'laiSK;^SpttC does notlipeet the advisory recovery of 50-150
    :-~' "*     percent^;; _

 2&.S'. 6      If the ins^kument blank SMC recovery is less than 20
;;:,          percent, gEfkter than 200 percent, or if peak interferences
•'%- "i0•••       are  preseng^l sample analysis shall be stopped, corrective
     ; :, <     action pei^«rmed, and another instrument blank shall  be
      *"K*£~' analyzed.;|'§If the SMC is still outside the criterion  upon
                      I', corrective action, which may include a new
                   l;,,ealibration shall be performed.  All samples
                      since the last valid method or instrument blank
            shall be reanalyzed after a valid instrument blank has  been
            demonstrated.

                             D-62-PCB-Q                          08/23/94

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                                                                          DRAFT

      26.6.7      If  the RTS criterion is  not met for an instrument blank,
                  sample analyses  shall be stopped and another instrument
                  blank shall be analyzed.   If the RTS smtside recovery limits
                  on  reanalysis , corrective action which may include a new
                  initial calibration shall be performed.  DO NOT continue
                  with sample analyses until the RTS "is *i thin ±1.0 percent.

      26.6.8      Any samples not  bracketed by valid ins tumet«:> iblanks or a
                  valid instrument blank and a method blank and shall be
                  reanalyzed at no additional expense to the Agency!.'

26 . 7  Documentation

      Instrument blank results are reported >on Forms Q1&-PCB, QIB-PCB, and
      QVI-PCB.  Reporting requirements are -l^Sfted irvllxhibit B.
                                              ' ', , *    >>"
27    Laboratory Control Samples                     j ,

27.1  Summary
                                 *  -•

      NOTE: The Agency: -Mil pr6%S||e  the Labo«|tory with further instructions
            for the aaaiysis of IpSs  for wipe\ssmples .
                   ...  ''•           \.
27.2  Frequency   „' ; -  ,           |§ B,e,, ..... ,,_„
                   ; -~~\        «,JJl.;^mi i'^Jr
      An LCS shall be atisHyzed once  per matrix per analytical sequence (24
      hours) per instrument, ivXhe  LCS shall be analyzed after the first
      instrument blank in the-ifpsifcLal calibration analytical sequence or after
      the method;' Jjlaoik; in the dkilty, Calibration analytical sequence.
                        '
                  An LCS'all be analyzed with  each:
                  Set of wa^T field samples  (LCS prepared from reagent
                  water) ;   :/,,t
                             ' '-
                  Set of soij/solid field samples (LCS  prepared with quartz
                 ,sand) ;
                   '•   ,   .
            •     "Set:: :M:- »lly field samples  (LCS prepared with corn oil) .

      27.2.2      The LCS shall be analyzed with all  associated samples in the
                  same analytical sequence .  If samples  from a batch are

                                  D-63-PCB-Q                           08/23/94

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                                                                          DRAFT

                  analyzed in more than one analytical sequence, the
                  associated LCS  shall be analyzed in the same analytical
                  sequence.   If an LCS extract is used "up because of multiple
                  analyses,  the Laboratory shall use the original stock mix
                  diluted into hexane in place of th.-       /:
                                       *'' ,   * •
            27.3.1.2    Spike 100 mL of aseagfent water with 100 /iL of the LCS
                        standard  mixture Vagi described in the instructions
                        ,f»rovjaeied  with  the I|CS mixtures.   Use syringes to
                       ,;3Jerfbrffl5,,|ifae spiking ,:fee ensure accuracy.  Add the SMC
                        and mix and carry through  the extraction and clean-up
                        process as! described in section 14 or 15, depending on
                        whether ^^.vent^or solid phase extraction is utilized.
                                                   as  described in section 18.
            27.3.1.3    Nominal  aqueous  LCS  target compound concentrations are
                        as  follows:
                        Aroclor  1224;:,           25 pg/L
                        -Amclor  1254  '            3 Mg/L
                        HefECachlor  epoxide    0.5 /*g/L
         ••
        .3.2      Soil LCS  'n*-
                        AlloJBr.:the  LCS  mixture ampules to reach room
                        tenip/erature before opening.   The ampules must not be
                        o|*eaied until preparation/ analysis is to occur.
                        Exercise care  in breaking the ampules open to avoid
                        : injury.
                                   D-64-PCB-Q                          08/23/94

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                                                                           DRAFT

             27.3.2.2    Spike 6 g of quartz  sand with 100 /xL of the LCS
                         standard mixture as  described in the instructions
                         provided with the LCS mixtures/'  Use syringes to
                         perform the spiking  to ensure Accuracy.   Add the SMC
                         and mix and carry through  the. .^extraction and clean-up
                         process as described in section. ,14.   Proceed with the
                         analysis as described in section :18,;

             27 . 3 . 2 . 3    Nominal LCS target compound  concentrations,, are as
                         follows:              /"',,                    V •
                         Aroclor 1221        vi   417
                         Aroclor 1254        V:    50  pg/ikg
                         Heptachlor epoxide  ,       8
       27.3.3       Oil LCS                           '-
                                                   ,' ;.
                   This section has not been finalized. ? The  LCS  composition
                   and concentrations for oils are currently  being
                   investigated.   ,t.;  ,
                                 !-! ,'•"" '; • '-•<  •;:"-.. U;\, ,-,
            27.3.3.1    Allow the pCS mixture ampules to reach room
                         temperature :feefore openlsig. -"The .ampules must not be
                         opened until -preparation/ analysis is to  occur.
                         Exercise care in breaking the ampules open to avoid
                         injury.         '   ;- ' •'.:
             27.3.3.2     f|>fk^|l;-g of corn oi^ with 1 mL of the  LCS  standard
                       -,  Itixtuffr^s described?^ the instructions  provided with
                     ?£  'the LCS fejstures.  Usfe- syringes to perform  the spiking
                     ',  '  to ensur6| Accuracy.  Mix and carry through  the
                    :  s   extracti^fc^nd cleanup process adding 1.0 mL of SMC
                   ' ' ; r^v(°-2 /igJiE|l;--«S«i|i»^EBe and further prepare  as
                         ;*tescribed in sections 16.3 to 16 . 5 .
            27 . 3 . 3 . 3     Nominal: rfljCS target compound concentrations  are  as
                                 1221            25,000 /ig/kg
                              >r 1254             3,000
                         Hep tailor epoxide         500
27.4  *e9|snical Acceptance Cliteria
               .^ ,,All  LCS offi^iounds must have recoveries between  30  and 130
               ''
      27.4.2      All%08'-"target compound absolute and relative retention
                  times  must be within the windows established from  the  low
                  concentration standard during the initial calibration.

                                   D-65-PCB-Q                           08/23/94

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                                                                          DRAFT

      27.4.3      The RT of the  SMC must be within ±1.0 percent of the mean
                  SMC RT established from the  1016/1260  initial calibration
                  standards.

      27.4.4      The SMC advisory recovery criterion:is 50-150 percent.  The
                  SMC recovery in the LCS must, however, be greater than or
                  equal to 20 percent and less thaa or eqaal to 200 percent.

27.5  Corrective Action                                          -,; -.<

      27.5.1      If an LCS compound recovery;i:s outside the criterion,
                  reanalyze the  LCS.  If upon  reanalysis an LCS compound
                  recovery is still outsider'the criterion,  the LCS and all
                  associated field and QCCamples  shall) be  reextracted and
                  reanalyzed.             •".''•'

      27.5.2      If the SMC is  less than 20 percent,.greater than 200  ,
                  percent, or if peak interferences luce.-present in the LCS,
                  sample analyses shall be stopped and tiie  LCS reanalyzed.  If
                  the LCS SMC recovery is still outside  QC '.criteria upon
                  reanalysis, coireaci3re|;iac|4^n shall be performed and the LCS
                  and all associated samples sliall be reextracted and
                  reanalyzed.      ,'          ,,, '••      ;  •

      27.5.3      If the RT or RRT fof^any |£S compound  is  not within the RT
                  and RRT windows establishes  from the low  concentration
                  standard during the initial  calibration,  reanalyze the LCS.
                  If uppii aseabalysis a compound is still outside the windows,
                  a ney l£nitiails^alibration'«ast be performed before samples
                  can &e analyzed^  The instroaent must  be  recalibrated as
                  described in session 8.
      27.5.4      I^stfee RTS crit^iojiMs SB»t met  for  the  LCS,  sample analyses
                  shall} tf& ^stopped and the noncompliant LCS  reanalyzed .   If
                  the RTSi' "i,s still outside the criterion upon reanalysis,
                  corrective ^ition which may include  a new  initial
              :<  T.calibration shall be performed.  DO  NOT  proceed with sample
          ,:;i-  rs- "  'analyses until tKe||RTS is within ± 1.0 percent.
                          . ~
      27415/5      Any samply^ processed with an LCS that  is  out of control
      ;;  *$,         (i.e., does snot meet any of the  technical  acceptance
     ,,*f,l          criteria) ijiall be reextracted and/or reanalyzed at no
     * -^, , s       additional; jekpense to the Agency.

          X1'!~! '             ';'
27.6  Docume'misaPCiQn       ,-:
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 EXHIBIT D



APPENBKBS

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                         APPENDIX A - DRY WEIGHT CALCULATIONS
If concentrations of target analytes in soil/solid samples are to be calculated on a dry weight basis the
percent moisture and reported concentrations shall be calculated as follows:

1.     Immediately after weighing the sample for extraction, weigh 5-10 g of the soil/solid into a tared
       crucible. Determine the percent moisture by drying overnigh^at I05:,- ,100

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                   APPENDIX B - GENERAL GUIDANCE FOR UNUSUAL OR
                              HIGH CONCENTRATION SAMPLES

Difficulties may be encountered when using the QTM methods for the analysis of unusual matrices (e.g.,
sludges, solvents, paint chips, etc) and samples containing high concentrations of target and non-target
compounds. The following suggestions and general guidance may be useful when such samples are
analyzed using the QTM methods.

1.      A screening device such as a PID organic vapor analyzed (OVA) may be ased if samples are
        suspected to contain very high levels of volatile organics. Such a screening device would allow the
        analyst to approximate sample dilutions to protect instrumentation and to minimize unnecessary
        samplereanalyses.                                ,,;                      ' '   \>,

2.      For highly contaminated samples, the laboratory may consider using smaller injection volumes to
        protect the instrumentation. If a smaller injection volume is used, toe instrument sensitivity may
        need to be increased so that the contract required ->
4.      Some types of soil/solid samples (e.g^i paiatj^ai|») laay need to be agitated prior to headspace
        analysis.  Agitation through techniques $uch as sdmcit^i will aelp to fractionate and disperse
        these types of matrices for more effective extractions and headspace analysis.

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           APPENDIX C - MODIFIED SOLID PHASE EXTRACTION PROCEDURES
                               FOR PESTICIDES AND PCBS
The following modified disk extraction procedure for water samples may be used in place of the
corresponding SPE procedures in the QTM SOW for pesticides and PCB& ;-The procedure has been shown
to be effective in the extraction and cleanup of water samples for pesticides and PCBs. However, this
procedure has not been validated by the EPA, therefore, if these procedures are used, the Laboratory must
demonstrate equivalency by meeting all methods QC requirements.   :      :   ;
                                                                      " <
Because many disk extraction vacuum hardware components are available commerciaBy, the Laboratory
should follow the manufacturers  directions for the proper use of these devices. The Laboratory should
also refer to the extraction disk package inserts for additional details on the proper use of the disks and
disk vacuum apparatus.

15.6    Disk Extraction Set-up and Conditioning (Optiatt'lp         /
                                               " -f '*'' • •
       15.6.1   Place a 47 nun C-18 Empore™ disk onto the base unit of a glass filtration assembly.
              Gentry pinch the clamp to assure even pressure around the disk. Use of a manifold for
              multiple extractions is acceptable.                   : ,

              NOTE: If the sample contains particulates, use an in-situ prefiltration media such as
              Filter Aid 400 or other  conaaerdaBy Available membrane-type filter may be advisable.
              The prefiltration media shouMfce placed p^M to the wash step. (When using Filter Aid
              400, adjust solvent volumes to aBow bed submelston tntwtghout the procedure.)

       15.6.2   Wash the extraction apparatus and disk by adding 5 ml of methylene chloride to the
             reservoir, rinsing down the sides of the reservoir in the process. Draw a small amount
              through the disk with a vacuum; turn off the vacuum and allow the disk to soak for
              approximately one miaate. Pull the remaining solvent through the disk and allow the disk
              to dry.     ,/  • '  ""''v  ,-:             S|
                       •' '°V '          * W"             £J
                        f <'            .>£ y
       15.6.3   Condition the disk by addin|fpproximately 5 mL of methanol to the reservoir, drawing a
              small amount through the dM: then letting it soak for approximately one minute.  Draw
              most of the remaining methaii0l ^apugfe ie disk, leaving 3-5 mm of the methanol on the
              surface
              NOTE: THE DISK SMQIIfeD NOT BE ALLOWED TO GO DRY FROM THIS POINT
              UJO3L 'Pffi.END OF SA!fflJ3E. EXTRACTION. RESIDUAL VACUUM IN THE
             eXfRAetl^S^EVICE MttSf&E VENTED TO PREVENT THE DISK FROM
              DRYING OUT.t|M|pST VACUUM MANIFOLD DEVICES AUTOMATICALLY
              VENT WHEN THW«ACUUM IS TURNED OFF. THE VACUUM LINE MAY
              NEED TO BE DISCONNECTED IN ORDER TO VENT THE RESIDUAL VACUUM
              IF SUCTION FLASKlfi&RE USED.  SHOULD THE DISK ACCIDENTALLY GO
              DRY, SIMPLY REPEllr THE METHANOL CONDITIONING STEP.
       15.6.4 Add 10 mL of reageat!*vater to the disk. Using the vacuum, pull most of the water
                               7 3-5 mm of water on the surface of the disk.
                       ' V ,' -¥
15.7    Compound ExtractioHiaaS Elution Using Disks (Option 2)

       15.7.1   Add 0.5 mL of methanol to the water sample and mix well.

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15.7.2   Add the water sample to the reservoir and filter as quickly as the vacuum will allow.
        Drain as much water from the sample bottle as possible.

15.7.3   Remove filter assembly and insert suitable sample tube for eluate collection.

15.7.4   Add 5 mL of methylene chloride to sample bottle. Rinse bottle thoroughly and set aside
        momentarily.

15.7.5   Wet the disk with a small amount of acetone - just eaough to wetthe surface
        (approximately 0.5 mL) and  immediately transfer the methylene chloride from the sample
        bottle to the disk with a disposable pipette, rinsing sides of the filtration reservoir in the
        process.

15.7.6   Draw half of the solvent through the disk then release the vacuum. Allow the remaining
        methylene chloride to soak the disk for approximately 1 minute then  draw remainder
        through under vacuum.

15.7.7   Repeat the solvent rinse of the sample bottle using 5 ttL of methylene chloride and
        transfer to the apparatus, rinsing down the sides of the reservoir. Add 5 mL of methylene
        chloride directly on the disk, let soak for approximately 1 minute, and draw through under
        vacuum.                                                :

15.7.8   Add 8 g of anhydrous sodiu^.dd£ateK},l|cy^e,,eluate.  Pipet the eluate into a
        concentrator tube. Rinse the ^collection tubl and sodiian sulfate with two 5 mL portions
        of methylene chloride and combine the rinsatesiwfth the sample eluate in the concentrator
        tube. NOTE: If large clumps form on addition of the sodium sulfate to the sample
        eluate, break up the clumps before adding the rinses.

15.7.9   Pesticides - Concentrate extract to approximately 2 mL under gentle stream of nitrogen
        (may be wanned gently - approximately 30 degrees C) Add hexane/acetone (9:1) to bring
        volume to 10 ml, then blowliown to 1 ml. '»

        PCBs - Coficentrate extract to approximately 2 mL under gentle stream of nitrogen (may
        be wanned gently - approximately 30 degrees C.)  Add hexane to bring volume to 10 ml,
        then blow down  to approxsnitefy 4 ;ntl and- adjust to 10 ml final volume with hexane.

        NOTE: To minimize analyte loss due to volatility, occasionally rinse sides of centrifuge
        and concentrator tubes witli methylene chloride, hexane/acetone, or hexane, as
        appropriate, during the blowdown procedure.
    ;'-J               *  Y*            ^  '
15.7.10 Continue  with the florisil cleanup procedure for pesticides analysis or sulfuric acid and
  ;      florisil procedure fot|l?CB analysis as described in the methods.

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                                                  DRAFT
            EXHIBIT E

QUALITY, ASSURANCE/QW&LITY CONTROL
       F   .^.REQUIREMENTS,

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                                                                           DRAFT
                               TABLE OF CONTENTS


SECTION


Overview  	


I     Introduction   	,,.


II    Good Laboratory Practices  	»,;,. .


Ill   Quality Assurance Plan 	,', ....


IV    Standard Operating Procedures   	„•,'„


V     Analytical  Standards Requirements   	


VI    Contract Compliance Screening	

                                 'it,'  -^  ;.
VII   Regional Data Review   	<*;;'	


VIII  Performance Evaluation Samples   ....


IX    Data Package Audits   	.,..».


X     On-Site Laboratory, Evaluations   ....
XI    Quality Assurance And  Datat'^ferend Analysis
XII   Data Management
PAGE



E-3



E-4



E-6



E-7



E-12



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E-25



E-27



E-28



E-31



E-33



E-36



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                                                                          DRAFT

                                    OVERVIEW

A comprehensive quality  assurance and quality control program is an integral
part of the Environmental Protection Agency's (EPA's) Contract Laboratory
Program (CLP).  The quality assurance (QA)  component includes management
review and oversight at  the planning,  implementation;, and completion stages of
the environmental data collection activity  to ensure that data provided are of
the quality required.  The quality control  (QC)  system includes- those
activities required during data collection  to produce the data <y,.ihe QC system are
corrected.  After environmental data are collected:, ;(JA activities focus on
assessing the quality of data obtained to determine ffcs .suitability to support
enforcement or remedial  decisions.                      *  :.

This Exhibit describes the overa^s'tppStr^iias^urance/quality control
operations and the processes by witipeh tne tJEBi^eifc*Jthe QA/QC objectives
defined above.  This contract requiases a varief^^of'QSI/IJC activities.  These
contract requirements are the minimum'^JA/QC activities necessary to satisfy
the analytical requirements associated with :;the  determination of the different
method analytes.  The requirements are designed  to  facilitate laboratory
comparison by providing  USEPA with data from all Contractors.  These
requirements do not release iflie >analytical*45©ntractor from maintaining their
own QC checks on method;and insfcctiment performance.
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                                                                          DRAFT

                                   SECTION I

                                  INTRODUCTION

Appropriate use of  data  generated under the  wide range of analytical
conditions encountered in environmental analyses requires .reliance on the QC ,
procedures and criteria  incorporated into the methods.   Thai methods in this
contract have been  validated  on samples typical of-those received by the
laboratories participating in the CLP.   However, the validation, f§£ these
methods does not guarantee that they perform equally well for all-:saiBple
matrices encountered.  Inaccuracies  can also jifce'sult from causes other-,tfean
unanticipated matrix effects,  such as samplMg artifacts, equipment
malfunctions, and operator error.  Theref a-^tlfede to cons'fcpscting  quality assurance project plans,
quality c^tstrol programs^ *%£  a quality assurance organization.  It is,
however,",-aai explanation  ofttta&e QA/QC requirements of the program.  It also
outlines some minimum standards  for  QA/QC programs and includes specific items
that .jSf-e required in a QA Pl^O-   Delivery of this documentation provides the
Agency*iiSffch, a complete data package  which will stand alone,  and limits the
need for *GbjStact with the Cajatractor or with an analyst, at a later date, if
the analys is:"fe j-Ques tioned> S;
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                                                                          DRAFT

To assure that the product delivered by  the  Contractor  meets the requirements
of the contract and allows inter- laboratory  data  comparison, the Agency has
established the following contract requirements.

•     Preparation of and adherence to a  written Qualitf- Assurance Plan,  the
      elements of which are designated in Section I-IIJi  ~u

*     Preparation of and adherance to QA/QC  Standard Operating- procedures
      (SOPs) as described in Section IV.                       ";?  =,
                                              i ?*                   *
                                              , ;-:«                      > '
•     Adherence to the QC and analytical methods  specified in the contract.

•     Verification of analytical standards ,ahd documentation of  the  purity of
      neat materials and the purity and  a«*airacy  of so;itttions obtained from
      private chemical supply houses.     " '•*} -;,,      ;j,
                                             ''•• , :-2 -    , ,;••
•     Participation in the analyses of Laboratory, ^valuation Samples,
      including adherence to corrective  action
      Submission of all raw data and pertinent documentation, "for Regional
      review.
      Participation in on-site laboratory evalyajcibns^ 'including adherence  to
      corrective action procedures. "'; ;       v|:'

      Submission of all original documentation generated during sample
      analyses for Agency review.          -;'
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                                                                          DRAFT

                                   SECTION II

                           GOOD LABORATORY PRACTICES   .

      Good laboratory practices  and good automated laboratory practices are
defined as those common sense procedures carried o«,t fey qualified laboratory
personnel to ensure the quality  and integrity of die analytical data being
produced.  By following the  specific  analytical and reporting procedures
outlined in this SOW, the  Contractor  will produce analytical daibaiof known and
documented quality.  Data  integrity is  defined,*as ensuring that data,are
complete, consistent, and  without  errors,  and>|ensuring the prevention, of
information corruption and unauthorized data modification.
                                          .: v"
      Good laboratory practices  and good aSatomated laboratory practices are
managerial concepts covering the organizat^^^al procefes and the conditions
under which laboratory studies are planned,  periorjp*e4, monitored, recorded,
and reported.  Good laboratory practices and good;aatomated laboratory
practices include but are  not necessarily limited to procedures,  programs, or
statements regarding schedules,  plans,  standard operating procedures,
inspections (procedural, process,/«andsfacility),  audits (data, report, and
computer), quality assurance sta§ejii»i:||;^Qbiyes,  and staff records.  Good
laboratory practices and good autoinated. l5iboisa.to;ry: practices also include but
are not limited to classification  !&:•-.work (such-'!as'"R&S'4?S SAS, government vs
private), sample retention procedures^,^equipBSSSt calibration and maintenance,
characterization requirements of samplje^ (st»efti as identification and
stability), method and software  validatieaq,'^^approval of supplies and
standards, traceability of standards  bacfc'.tsb their origin, sample and data
chain-of-custody, inspec1iitm:fis£>,electronic sand hardcopy data and data
packages, computer and'facilityjjkecurity,  stskff training, and monitoring by
the laboratory's quality assurafsleV officer.  * ;,
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                                                                          DRAFT

                                  SECTION III

                             QUALITY ASSURANCE PLAN

      Overview                                      ,,'  /

      The Contractor shall  design and implement a Duality assurance program
      with the objective of providing sound analytical chemical measurements .
      This program shall specify the quality control procedures , ,»e©rrective
      action procedures, and all documentation required during data  ;
      collection, as well as the quality assessment measures performe4',by
      management to ensure  acceptable data  production.  As evidence of such a
      program, the Contractor shall prepare ',-& written  Quality Assurance Plan
      (QAP) which achieves  the following. :

      •     Maintains data  integrity,  validity, Jand''-tjsability.

      •     Ensures that analytical measurement systep&s ,,are maintained in an
            acceptable state of stability and reproducli>ili.ty .
      •     Detects problems  t&rmjp^^^''.!*8^5313161^ and establishes
            corrective action procedures whl«.1S,lSes*|>;t^|e analytical process
            reliable.               ,             "    '•'••'•

      •     Documents all aspects  of  tiie measurement process in order to
            provide data which are technically sound and legally defensible.

      The QAP shall presetit^in specific t%rms,  the policies,  organization,
      objectives, functional  gtai4$lines» and Specific QA and QC activities
      designed to acM&ve the dalpt; quality requirements in this contract.
      Where applicable, SOPs  pertaining to each element shall be included or
      referenced a^lgart of the ^^f.^^The ,,,QAP  shall be available during the
      on -site laborietary evaluat^eStl.^aM^bwtf  be submitted within seven days
      of written request/|»y the TPO,  EMSL-LV,  and/or NEIC.   Additional
      information relevant/ib,- the  preparation  of a QAP can be found in EPA and
      ASTM publications.    ' V  ,

2     Elemeects'- cff " a:s-QqilttV Assurance JP Ian
         \- ' '              ****< "'>-
2 . 1   Onganization and PerSs^onel
      ,  ::                  VM
     /r|;.;l.l QA Policy and Ob^ctives

        *       Management   ^:
                  Assigboent of QC and QA Responsibilities

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                                                                           DRAFT

             •      Reporting Relationships

             •      QA Document Control Procedures

             •      QA Program Assessment Procedures   "

      2.1.3  Personnel                                      =

             •      Resumes                                        '"- .

             •      Education and Experience Pertinent to  This  Contract -^nd as
                   Specified in Exhibit A      '

             •      Training Programs        >

2.2   Facilities  and Equipment                 ':'••  „  ;:

      2.2.1  Instrumentation and Backup Alternatives    -

      2.2.2  Maintenance Activities-and Schedules
                                 ''"" *-»." X'V ,;-"'.  f  ,,
2.3   Document  Control          '*;.,    "' *-'"".;ts"      /

      2.3.1  Laboratory Notebook Policy        J

      2.3.2  Sample Tracking/Custody Proe<&&ures

      2.3.3  Logbook  Maitg&esgai$e,-and Archivia^ Procedures
                      ;./7 " '"'^i,          'V-
      2.3.4  Case  Fil£,!®rganizati%liv Preparatieb, and Review Procedures

      2.3.5  Procedures for Prepaf4fe^n-'-A!5P-3roval' Review> Revision,  and
             Distribidbm of         '         '~
      2.3.6 Process  for ReVisipn of Technical or Documentation Procedures

2.4   Analytical'IKetfeed.ology  Si  j ,

      2.4,/l!-Calibration'Procedures  and Frequency

      2;*|s=.2 Sample Preparation/Extraction Procedures

     '"Si"|4«'Ji Sample Analysis It|?ocedures

      2.4.4 ^taaiiards  Preparation Procedures
            Initiatioti>i>i^ 'Corrective Action
2.4.5 Decisiob.^roc^ses,  Procedures and Responsibility for
                                Act!

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                                                                           DRAFT

2.5   Data Generation

      2.5.1 Data Collection Procedures

      2.5.2 Data Reduction  Procedures

      2.5.3 Data Validation Procedures             :      -,:

      2.5.4 Data Reporting  and Authorization Procedures          l'!
                                               •

2.6   Quality Control                        f

      2.6.1 Solvent, Reagent,  and AdsorbentJgheck Analysis

      2.6.2 Reference Material Analysis     (

      2.6.3 Internal Quality Control Checks

      2.6.4 Corrective Action and Determination of QC Iand.£ Procedures
                                  V*  ,
      2.6.5 Responsibility  Designa££$&';-  ,; *~
                                  '- /    '  'v %/* '"•-  >.
2.7   Quality Assurance              ;•••

      2.7.1 Data Quality Assessment    f    :;=

      2.7.2 Systems/Internal Audits

      2.7.3 PerformanpBii^xtenialll&udits     ; ,.;
                     .: h          •$,            ''-I
                     : ;           t*            ' ( -
      2.7.4 CorrectiveAction Procedures
                  >;              ;;-^  , ,
      2.7.5 Quality*A|sESurance

      2.7.6 Responsibility^l)«|ignation

3     Updating-^aad-ISti&mitting the JQAg
3.1   Initial Submission"'-,
       /.: C                   ,j-
          ".ng the contract solicitation process, the Contractor is required to
         unit their  QAP to EMSt-LV and NEIC.  Within 60 days after contract
           , the Contractor Shall revise the QAP to be in full compliance with
      the!4*ejfuirements of thfbs contract.  The Contractor shall maintain the
      revised-^|HP, on file atffsthe Contractor facility for the  term of the
      contract/  :4&e>;revise
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                                                                          DRAFT

      3.1.1 Changes resulting from 1) The Contractor's  internal review of its
            organization, personnel, facility,  equipment,  policy and
            procedures; and 2) The Contractor's implementation of the
            requirements of the contract; and          :

      3.1.2 Changes resulting from the Agency's review io.f - the laboratory
            evaluation sample data, bidder  supplied documentation,  and
            recommendations made during the pre-award on-site; laboratory
            evaluation.                                         -''. •

3.2   Subsequent Updates and Submissions     •"                         ?

      During the term of the contract, the,i@bntractor stiall amend the QAP when
      the following circumstances occur:,(  :s          ;|

      •     The Agency modifies the contract; '•>« >,  -  "

      •     The Agency notifies the Contractor  of deficiencies in the QAP;
            The Agency notifies the- Contractor  of  deficiencies resulting from
            the Agency's review e£Iftlife r£&a£factor's performance;
      •     The Contractor identifies deficiencies  resdlting from its internal
            review of its QAP;       '•"'        i
                                       'j, '    £*••''
      •     The Contractor's organization, ^personnel,  facility,  equipment,
            policy, or procedures change;  and

      •     The Contractor identifies deficiencies  resulting from the internal
            review of_'S±s organi'faition, persofinbl,  facility, equipment,
            policy, br procedures Jehanges.

      The Contractonslmll amerailiJfeeJ^illMl^iiin  30  days  of when the
      circumstances lis?te*t above result in a  discrepancy between what was
      previously describee! ,.iiiv>the QAP and  what is presently occurring at the
      Contractor's facility. : f^ .

                ATP"is-i^«^aded,  ali'*'-ekinges in the QAP  shall be clearly marked
             a bar in thtejajargin indicating where the  change is found in the
                or highligHfclkig the  change by underlining the change, bold
         tting the change, o&using  a different  print  font).  The amended
        :tion pages shall hai|i&>  the date on which the changes were implemented.
     vt&g]Spntractor shall iiieorporate all amendments  to the current QAP
      docMa^at.  The Contractl&r shall archive all amendments to the QAP
      document:^«>r future x^lerence  by the Agency.
              " «  'i^       -^'.
      The Contractor is3mpl^ send a copy of  the current  QAP to the designated
      recipients withiiS 'Seven days of a request  by  the TPO or NEIC.

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                                                                         DRAFT

3.3   Corrective Action:

      If the Contractor fails to adhere to the requirements listed in this
      section, the Contractor may expect, but the Agency is not limited to the
      following actions:  reduction of numbers of samples sent under this
      contract, suspension of sample shipment to the'-Contractor, data package
      audit, an on-site laboratory evaluation, remedial laboratory evaluation
      sample, and/or contract sanctions, such as a Cure Notice,';
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                                                                    DRAFT

                             SECTION IV

                   STANDARD OPERATING PROCEDURES

Overview

In order to obtain reliable  results,  adherence to prescribed analytical
methodology is imperative.   In any  operation1- that is peaSfbrmed on a
repetitive basis, assurance  of data quality and reproduci-bllity is best
accomplished through the use of SOPs.   As,=!defined by the EPAi .an SOP is
a. written document which details an operation,  analysis, or action which
is commonly accepted as the  method  fpri performing certain routine or
repetitive tasks.                    ; „
                                    %* s"            ^ '
SOPs prepared by the Contractor shall! j»y the TPO atip^sr NEIC;

•  , ~'. '^Capable of providing for the  development of documentation that is
  ,,   '' sufficiently c^^lete  to record the performance of all tasks
,;; .    required by the
      Capable of demonstrating the validity of data reported by the
     "^Contractor and ej^lain the  cause of missing or inconsistent
                                E-12

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                                                                          DRAFT

      •     Capable of  describing the  corrective measures and feedback
            mechanisms  utilized when analytical results do not meet protocol
            requirements;

      •     Reviewed regularly  and updated as necessary when contract,
            facility, or Contractor procedural modifications are made;

      •     Archived for future reference  in useability or evidentiary
            situations;                                         - ,,'

      •     Available at specific work stations as appropriate;  and

      •     Subject to  a document control  piNocedure which precludes the use of
            outdated or inappropriate  SOBs,

2     SOP Format:

      The format for SOPs may vary depending upon the kind of activity for
      which they are prepared.  At a minimum,  however,  t&e following sections
      must be included:           , ,

      •     Title Page;           1.•'        "'-",  ;  .,

      •     Scope and Application;

      •     Definitions;

      •     Procedures;

      •     QC Limits;?'          '>

3     SQ? Requirements:     .-• J
      :;-                     '-. c.
      'me:pontractor shall maintain  the following SOPs:
         '-V-,v              4K-
3.1   Evidentl^cy,, SOPs:    -\/,.
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                                                                            DRAFT

      Evidentiary  SOPs for required chain-of-custody and document control are
      discussed  in Exhibit F, "Specification for  Written Standard Operating
      Procedures."

3.2   Sample Receipt and Storage:

      •     Sample receipt and identification  logbooks;

      •     Refrigerator temperature logbooks;                  E: ,


      •     Extract storage logbooks; and   ,, ,s.                       -  '.''

      m     Security precautions.          , ':'            ~

3.3   Sample Preparation:                    -;"-,-

      •     Reagent purity check procedures  and iSQCtaaentation;


      •     Extraction procedures;                      •';=


      •     Extraction bench she&£s'; \%BQ&;^. •-., ,,
                                  '"'..(?.   ' "::-  *'•'""!;V "  =
      •     Extraction logbook maintenance.    • / " ' '•- '••'-,


3.4   Glassware  Cleaning              !;;    -;'"':


3.5   Calibration  (Balances):              :
                          '  •  '"";  ",
      •     Procedures; V     "'  fc-            •'* •-
                     •f~: '        V,            •'•;

      •     Frequency-requiremenisi;

      •     Acceptaheeacriteria£SaSj,-,^EK||^ctiTre actions;  and
                       ~  ; ,v J,
      •     Logbook maintenaac^ authorization.

3.6   Analyticjal>!r«pedures  (£or'f&&i$h analytical  system):

      •   ';? -i"Instrument pe^^rmance specifications;

       ,^4'-                 'f|,.
      pi:.'s   Instrumental operating procedures;
      il">'                     '-"-',!
     ,*£/-..             . .  .  "••'!
      "* ,~S|Q,, Data acquisition;afystem operation;

      •     '!KjE»efedures whe^islutomatic quantitation algorithms are overridden;


      •     QC - req^red ^g^rameters;



                                      E-14


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                                                                           DRAFT

       •      Analytical run/injection logbooks;  and

       •      Instrumental error and editing flag descriptions  and resulting
             corrective actions.

3.7    Maintenance Activities (for each analytical system)i

       •      Preventive maintenance schedule and procedures;

       •      Corrective maintenance determinants ^and procedures;  arid,:

       •      Maintenance authorization.      :- ;'

3.8    Analytical Standards:                ,  ;

       •      Standard coding/identification arid, :i.syentory system;

       •      Standards preparation logbook(s);

       •      Standards preparation^procedures;

       •      Procedures for equiva%ency/trIc^&Eiiity sanalyses  and
             documentation;         ' =;;:          :   "     '

       •      Purity logbook (primary standards-iand solvents);

       •      Storage,  replacement,  and labeling  requirements;  and
                           '• ;•' r            ''• '
       •      QC  and corrective" action measures.?.

3.9    Data Reduction ^Procedures: =:,

       •      Data pro«&sssing  sys4©aei,:'o|idRat;f«n;
                      ":  j'; •
       •      Outlier identification methods;

       •      Idemttficajtion of data-icequiring corrective action;  and

       •  .JjJfrocedures  f6^;fpormat  and/or forms  for each operation.
3.10  O^^imentation Policy/Pj^cedures:

     •:-JT                    f*
      m^J, 4>, Laboratory/analyses'  notebook policy, including review policy;
          ' '.5*5  *!              '''-'i'
                     Batch, &.e  (CBF)  contents;
            Complete^ ;Sat
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                                                                          DRAFT

      •     Document inventory procedures,  including review policy.

3.11  Data Validation/Self Inspection Procedures:

      •     Data flow and chain-of-command for data .review;

      •     Procedures for measuring precision and accuracy;

      •     Evaluation parameters for identifying  systematic errors;

      •     Procedures to assure that hardcopy and electronic deliverable are
            complete and compliant with  the ilr-equirements in SOW Exhibits B and
            H;                            ,               ,

      •     Procedures to assure that hardcopy deliverables are in agreement
            with their comparable electronic SfeMveirables;

      •     Demonstration of internal QA inspection ptsscedure (demonstrated by
            supervisory sign-off on personal notebooks,  -internal laboratory
            evaluation samples, ete,).J
            Frequency and type of ijtetiternaT TatiilJBS -;fe^g. «, xandom,  quarterly,
            spot checks, perceived^t^puble areas};   '•''•  *

            Demonstration of problem  Hfeutifieation-corrective actions and
            resumption of analytical  processing.   Sequence resulting from
            internal audit  (i.e., QA  feedKack);  and

      •     Documentation of 'a&ft$£ reports 'Cisternal and external) ,  audit
            response^ -corrective'^action,  etc-;

3.12  Data Management  and Handlifi^ ,,„„ -,^-, -,-„,,

      •     Procedures 'for -.controlling  and estimating data entry errors.

      •     Procedures for revj,e»ing changes to data and deliverables and
            ensttrla&g- tcaceabilityJ^fe.updates .
           I.   "       "*,-': ;_         "*i""'
      •   ,,<;!-Lifecycle  manj|gi^ment procedures for testing,  modifying,  and
       ;-f  '•  implementing clffii^es to existing computing systems including
      .-!*    hardware,  softwai^i, and documentation or installing new systems.
      - -K                     5
     : ' &,-,                   ,^
      ~»|:;j, j,- Database securitj^ backup and archival procedures including
                     from system failures .
               u ,
            System jffiaintenance procedures  and response times .
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                                                                           DRAFT

      •     Individual(s)  responsible for system operation, maintenance,  data
            integrity and  security.

      •     Specifications for staff training procedures.

4     Delivery Schedule: Updating and Submitting SOPs  -;•  ;=

4.1   Initial Submission                                     :  ;  :.
                                                               "" ! i, s,.
      During the  contract  solicitation process £ the Contractor is "igeqwired to
      submit their  SOPs to EMSL/LV and NEIC.jT Within 60 days  after contract
      award, the  Contractor shall revise thesset of SOPs to be in full
      compliance  with the  requirements of this contract*  The Contractor  shall
      maintain the  revised set of SOPs on^file at the ^Contractor  facility for
      the term of the contract.   The revised lSSQ.Ps will 'become the official
      SOPs under  the  contract  and may be used 'IftJasLgg; 'legal proceedings.   The
      revised SOPs  shall include:                 ';' •

      4.1.1 Changes resulting  from A) The Contractor ' s :?i^t.ernal review  of its
            organization,  personnel?, facility, equipment, -policy  and
            procedures, and B) T&:^x^r3aet:o|:,',s implementation of the
            requirements  of  the  extract;
                                   - -s'-          .-;;     " '  '  • '
                                   'I          ••>'' •        •  '
      4.1.2 Changes resulting  from the: -Agency ^i review of the laboratory
            evaluation sample  data,  bidder supplied documentation, and
            recommendations  made during the ?||>re- award on-site laboratory
            evaluation.                  :" :

4.2   Subsequent Updates "and Stibsiissions    :  ,
                      - * > '         ^ .           v - ,
                     ; . '          ~*i*
      During the tesm. of  the contract,  the Contractor shall amend the  SOPs
      when the f clipping  circums^Ssieices, .occur:

            The Agency%edifies  the  contract;

            The Agency notifi!es::$lie  Contractor of deficiencies  in  its  SOPs;

           ?5pp6 "^getey^'^^if ies  thtf '<5j?ntractor of deficiencies  resulting from
            the Agency 's«i^wiew  of the Contractor's performance;
           '               "1;^
                           y,~n
            The Contractor ' sjljprocedures change;

            The Contractor  identifies  deficiencies resulting from  its  internal
           ; review of its SOfbjS documentation;  or
           '" ' ' 5 f •*            ' ; '
            The y3B$t,ractoip3;dentif ies  deficiencies resulting from  the  internal
                     ";; i,ts procedures .


                                     E-17

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                                                                          DRAFT

      The Contractor shall amend  the  SOPs  or write new SOPs within 30 days of
      when the circumstances  listed above  result in a discrepancy between what
      was previously described  in the SOPs and what is presently occurring at
      the Contractor's facility.  When the SOPs are ajasnded,  all changes shall
      be clearly marked (e.g.,  a  bar  in  the margin indicating where the change
      is found in the document, or highlighting the ehauge by underlining the
      change, bold printing the change,  or using a-diffeBBsrt^print font).  The
      amended/new SOPs shall have the date on which the changes were
      implemented.                                                h

      When the SOPs are amended or new SOPs ar« written,  the Contractor:shall
      document in a letter the  reasons for £he changes,  and submit the amended
      SOPs or new SOPs to the TPO, EMSL-LVs^f^uality assurance/technical SOPs),
      and NEIC (evidentiary SOPs).  The  G|ji$|ractor shajll send the letter and
      the amended sections of the SOPs or'ia^r ,SOPs witfein seven days of the
      change.  An alternate delivery  schedule 'ifOT £tar submittal of the letter
      and amended/new SOPs may  be proposed by the ;J©b&tractor,  but it is the
      sole decision of the Agency, represented either"by the TPO or APO, to
      approve or disapprove the alternate  delivery schedule.   If an alternate
      delivery schedule is proposed.,,  the Contractor shall describe in a letter
      to the TPO, APO, and the  C4o3ftii^:^|g^>^£lcer why he/she is unable to
      meet the delivery schedule lifted *i!itf'%lfe;Be«fci,O3tt,,   .The TPO/APO will not
      grant an extension for greateifkthan  30 dffs for amending/writing new
      SOPs.  The TPO/APO will not gr^st,  an extension for greater than 14 days
      for submission of the letter doctoaenting the reasons for the changes and
      for submitting amended/new  SOPs. St&^i6ontractor shall proceed and not
      assume that an extension  will be gristed until so notified by the TPO
      and/or APO.       ,, -   .,
      The Contractor Miall send 'j^eomplete set? -of current SOPs or individually
      requested SOPsf=,%o the reci^p&its he/she designates within seven days of
      a request bjri^e TPO, APO ^0J;,,J|E JC ,,^ Documentation of the reasons for
      changes to the'^Es shallf^tlSi^i/r^Wipitted along with the SOPs.
4.3   Corrective Action:  =:
                            •' ' ; 5 '.'

      If the ,jpo3Etr«HStQr fails tc* ISJiiere  to the requirements listed in this
      sectieaii; •'ttie^Contxa^tor may fe«|H^ct,  but the  Agency is not limited to the
      folii»n.ng actions : %«i«iuction of numbers of samples sent under this
      copeieiract, suspension '^1 sample shipment to the Contractor,  data package
        pl.t, an on-site laboimtory evaluation,  remedial laboratory evaluation
              and/or contracd||$anctions ,  such as a Cure Notice.
                              *
                                     E-18

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                                                                          DRAFT

                                   SECTION V

                       ANALYTICAL STANDARDS REQUIREMENTS

      Overview

      The U.S. Environmental Protection Agency (EPA)'will™tM>;t supply
      analytical  reference standards either for direct analytical measurements
      or for  the  purpose of traceability.   All contract laboratories will be
      required to prepare from neat  materials -a* purchase from private
      chemical supply houses those standards .necessary to successfully
      accurately  perform the analyses required in this protocol.

      Preparation of Chemical Standards fffom the Neat Sigh Purity Bulk
      Material                           '- .•>*• >     -1 <
      A Contractor may prepare  their chemical standards from neat materials.
      Commercial sources  for neat  chemical standards pertaining to compounds
      listed on the  Target  Compound List (Exhibit C) axe -given in Appendix C
      of the "Quality  Assurance Materials Bank:  Analytical;Reference
      Standards" Seventh  Edition^  3®xsijigK$/;]L9&&,.   Contractors shall obtain the
      highest purity possible whetti^urchaiittg^^j£fcj:j:i|emical standards; when
      standards are  purchased at less than 97%^piri"sfcyv'i'he Contractor shall
      document the reason why a higher puritylicould not be obtained.

2.1   Neat chemical  standards shall be kept; Tefrigerated when not being used
      in the preparation  of standard solutions.   Proper storage of neat
      chemicals is essential|ia order to safeguard them from decomposition.

2.2   The purity of  a>eompound  cam sometimes  %e.misrepresented by a chemical
      supply house, ulgince  knowleU|j;e of purity :is needed to calculate the
      concentration^f solute ia^rsplution, standard, it is the laboratory's
      responsibilitys;CO(...have an^jifet^&t.sliqsgtimentation ascertaining that the
      purity of each compound is correctly stated.   Purity confirmation, when
      performed, should use,|tei|her differential  scanning calorimetry, gas
      chromatography with fllsaa^ SLonization detection, high performance liquid
      chromatogr^pf^i :JLnfrared  spfjBCtarometry,  or  other appropriate techniques.
      Use ptf,: &^}"o™f"Tie^efe1iindependehieri«ethods  is  recommended.   The correction
      fao|%r for impurity|^feen  weighing neat  materials in the preparation of
      solution standards  is-:

Equati&f 1                  \g,
             , weight of impuM compound = ^eigrht of puze compound
             ,;=  •.,             ;,               (percent purity/100)
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                                                                          DRAFT

      where "weight of pure compound" is that  required to prepare a specific
      volume of a solution standard of a specified concentration.

      When compound purity is assayed to be  97 percent5, or greater, the weight
      may be used without correction to calculate the/;eoncentration of the
      stock standard.  If the compound purity  is  assayed -to De less than 97
      percent, the weight shall be corrected when cu'lculatfkig, the
      concentration of the stock solution.                    •/'-•
2.3   Mis -identification of compounds occasionally occurs and it
      that a mislabeled compound may be received from a chemical supply house.
      It is the laboratory's responsibility :;|E0 have analytical documentation
      ascertaining that all compounds used lin the preparation of solution
      standards be correctly identified. ^t^pLentificatjipa confirmation, when
      performed, shall use gas chromatograplij'J^aass spectrometry analysis on at
      least two different analytical columns , *<**:• lotSer appropriate techniques.
2.4   Calculate the weight of material to be weighted; iNit for a specified
      volume taking into account the purity of the  compound and the desired
      concentration.  A second person,,, shall verify  the accuracy of the
      calculations .  Check balan4fg^1Bfec^i^a^ac^, with a set of standard
      weights.  All weighing shoul^be pe^fia"iaifei:-<
      Soluti6%s'|of analytic^ reference standards  can be purchased by
                                meet the following criteria:
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                                                                          DRAFT

3.1   Contractors shall maintain the following documentation to  verify the
      integrity of the standard solutions they purchase:

      3.1.1 Mass spectral identification confirmation of  the neat material;

      3.1.2 Purity confirmation of the neat material»  arid

      3.1.3 Chromatographic and quantitative documentation that  the  solution
            standard was checked according to the following section.

3.2   The Contractor shall purchase standards! for which the quality  is
      demonstrated statistically and analytically.  One way this can be
      demonstrated is to prepare and analyse three solutions;  a  high standard,
      a low standard, and a standard at tfe^ target concentration (see  3.2.1
      and 3.2.2 below).  The Contractor shall have documentation that  the
      analytical results for the high standard and -law standard  are  consistent
      with the difference in theoretical concentrations.   This is done by the
      Student's t-test in 3.2.4.  If this is achieve*!, 'She Contractor  shall
      then demonstrate that the concentration of the  target standard lies
      midway between the concentrations of the low and high standards.   This
      is done by the Student's twfses*,!.$ix 3L.2-.j5... Thus  the standard is
      certified to be within 10 percent o£ IfKe {$axgga%  concentration  using the
      equations in 3.2.6.

      If the procedure above is used, tihe Contractor  shall document  that the
      following have been achieved:

      3.2.1 Two solutions-of .Identical concentration  shall be prepared
            independently from ssefat materials,. An aliquot of the first
            solution^sKall be di&fced to the Intended concentration  (the
            " target ^standard"). p^as aliquot is taken from the second  solution
            an diluted to a concfBtxation.jten percent  greater than the target
            standard, j^fbis is .^llktfcttfce^liigh standard".   One  further
            aliquot is '"t^kesn from the second solution and diluted to a
            concentration 10:f^ercent less that the target standard.  This is
            called the " low
              k replit^t^jjanalyses ofiseach standard  (a total  of 18  analyses)
          y-shall be per'fl^aed in the following sequence:  low standard,  target
          * standard, high^i^andard, low standard, target  standard, high
            standard, . ..   :sr
                            1:
          \, The mean and varjkpice of the six results  for each solution shall
               calculated.  ,'!'
                                     E-21

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                                                                     DRAFT

                 MEAN = (yx + y2 + y, + y4 + ys + y6) /e

      Equation 3                                >

                    (y? + y22 + y| + yt2 + y| + if - 6*;{«EAW) 2/s
      The values  Y, ,  Y2, Y3 .....  represent the results of :ttte six
      analyses  of each standard.  The means of  the  low,  target!,; .and high
      standards are designated M.,, Mj,  and Mj,  respectively.  The'?*'
      variances of the low,  target, ab4':-high standards  are  designated
      Vv V2, and V3, respectively.  .additionally, a pooled variance,
      V , is calculated.              ,            ,

      Equation  4                        ':: '     ''',
      If the  square root offi^Las less than one percent of Mj, then
                 is to be ti^Jdbte s^fiLue of v  in all subsequent
      calculations.         *"        "  "    ''

3.2.4 The  test  statistic shall ^ calcxiated:

      Equation  5                   ,   -

            ZEST STATISTIC = ] (M3/l . 1 )  - .(A^/0 . 9 ) |/ ( V3 )°'S
                   •"   '  .''"":;           V

      If the  tesjt  statisticjiexceeds 2.i3;4then the supplier has failed to
      demonstrate  a  20 percjarit differences between the high and low
      standards .   In such 4i*«as^*- -fcb£ standards are not  acceptable.
                i '           ''" - ''    " '
3.2.5 The test  statistic shall be calculated:

      Equation  6        ,;

                                    . s)  -  (#3/2.2) | / (Vp/4) ° •s
.-ir:
< ••
      If the  test  stata&tic exceeds 2.13, the supplier has  failed to
      demonstrate  that|fSie target standard concentration  is midway
      between the highiftid low standards.  In such a case,  the standards
          not acceptabfte'.
                        '
3.2.6 The ~ $>$ -percent Confidence intervals for the mean  result of each
      standard ^shaiij-'be calculated:
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                                                                          DRAFT

            Equation  7

                 Interval for Low Standard = M^ ±  (2.13) (V^/6)0-5

            Equation  8

                Interval for Target Standard = A^ ± (3U13 )!;:

            Equation  9                                           :-s ::

                 Jnterva-Z for High Standard = A£ * (2 . 13) { V6) °'5         :

            These intervals shall not  overiap.   If  overlap is observed, then
            the  supplier has  failed  to deafcrastrate  the Ability to discriminate
            the  10 percent difference  in concentrations .   In such a case ,  the
            standards are not acceptable.     '•• : ;• ,,   ;;r

            In all cases, the Contractor is  responsibly ~f or the quality of the
            standards employed for analyses  under this sboatract.

4     Requesting Standards f rom -tabs Slfefif "Staandards Repository

      Solutions  of analytical refer«ace materials can =b«  ordered from the U.S.
      EPA Chemical Standards  Repository,  depending  on availability.   The
      Contractor can place an order  for staialards only after demonstrating
      that these standards are not available' from commercial vendors either in
      solution or as a neat material.      ;~
      Documentation oft tAie VerMtpation  and gre-paration of Chemical Standards
      It is the responsibility ofljeach laboratory  to  maintain the necessary
      documentatiah!;;to show tha£ '^Jig s chemical  standards they have used in the
      performance of^Cfcl' analyg§S^MBfec«b| 3» the requirements previously
      listed.  Weighing lo,gbooks , calculations, chromatograms ,  mass spectra,
      etc. , whether produee«catory evaluations.   Documentation of
      standards "prepasaiipn may be c«guired to be  sent  to EPA for verification
      of jttotitract complimif;^.  In those cases  where the documentation is
      s^|5j»ortive of the aiiajjjrtical results of  data packages sent to EPA, such
      j3»Sumentation is to be|&ept on file by the laboratories for a period of
          year.             ^-:f
                   by the TpKor APO, the Contractor  shall submit their most
      resent *ptee?rious year.'lUdocumentation  (12 months)  for the  verification
      and preparation of iisibemicals standards within 14  days of  the receipt of
      request to tfeejr^cifjients he/she designates.
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                                                                    DRAFT

The Agency may generate a report discussing deficiencies in the
Contractor's documentation for  the verification and preparation of
chemical standards or may discuss the  deficiencies during an on-site
laboratory evaluation.  In a detailed  letter to t&e TPO, APO, and EMSL-
LV, the Contractor shall address the deficiencies and the subsequent
corrective action implemented by the Contractor-t»-,cprrect the
deficiencies within 14 days of  receipt of the-report ;«r the on-site
laboratory evaluation.  An alternate delivery schedulejinajr be proposed
by the Contractor, but it is the sole  decision of the Ageaaisgr,,,
represented either by the TPO or APO,  to,lapprove or disapprove ^he
alternate delivery schedule.  If an alternate delivery schedule'is
proposed, the Contractor shall  describe! in a letter to the TPO, APO, and
the Contracting Officer why he/she is ,i*mable to meet the delivery
schedule listed in this section.  Tt^TPO/APO will not grant an
extension for greater than 14 days reatfllJie Contractor' s response letter
to the standards documentation  report. :<33isa Contractor shall proceed and
not assume that an extension will be granted ?until so notified by the
TPO and/or APO.                                 '  ,.

If new SOPs are required to^he  written or SOPs are recjuired to be
amended because of the defi-.'*     ~
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                                                                           DRAFT

                                   SECTION VI

                         CONTRACT COMPLIANCE SCREENING.

Contract Compliance  Screening (CCS) is one aspect of ; the Government's
contractual right  of inspection of analytical data,, /-CCS -^examines  the
Contractor ' s adherence  to  the contract requirements based  I    "" '"'" :'^  i •'•<- - -
The Agency may generate a  CCS trend; report whibn; summarizes  CCS results  over a
given period of  time.   The Agency may; send tbe CCS trend report or discuss the
CCS trend report during an on-site laboratory-evaluation.   In a detailed
letter to the TPO  and APO, the Contractor shall address the  deficiencies  and
the subsequent corrective  action implemented by the Contractor to  correct the
deficiencies within  14  days^slf; receipt of tfee, report or the  on-site  laboratory
evaluation.  An  alternate  delrasejcy schedule i^say be proposed by the Contractor,
but it is the sole des&ision of tUifi,, Agency , represented either by the TPO  or
APO, to approve  or, disapprove the Alternate delivery schedule.  If an
alternate deliverytschedule is paf^o^ed,, the Contractor shall describe in a
letter to the TPO,sAIp^,,and thei'fclibtKme£3Jgg 'Officer why he/she is  unable  to
meet the delivery  sche1&kl« listed in this section.   The TPO/APO will not  grant
an extension for greater ttta^a.14 days  for the Contractor's  response  letter to
the CCS trend report.   The Comix-actor  shall proceed and assume that  an
extension willi..t>^|;^j*asited  until '-ioptified  by the TPO and/or APO.

If new SQfs>are  required.;^, be written or SOPs are required to be  amended
because «&£ the def iciencies,,f£ind the subsequent corrective action implemented
by the, Contractor , the  Contractor  shall write/amend and submit the SOPs per
the requirements listed in EMttibit E,  Section IV.
     '                         "
If the Ccmtgsac.tor fails  to  alhere to the requirements listed in this section,
          ' -V '5-V1-              A t .....
the Contracfcesr.pssay expect, ,;feut the Agency is not limited to the following
actions: reduction yof numbers of samples sent under this contract, suspension
of sample shipment *laa; p£h» 'Contractor,  data package audit, an on-site


                                      E-25

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                                                                         DRAFT

laboratory evaluation, remedial laboratory evaluation sample,  and/or contract
sanctions,  such as a. Cure Notice.
                                     E-26

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                                                                          DRAFT
                                  SECTION VII

                             REGIONAL DATA REVIEW

Contract laboratory data are generated to meet the,-specific needs of the EPA
Regions.  In order to verify the useability of data ;for the intended purpose,
each Region reviews data from  the perspective of the end-user,:«'*ad based upon
functional aspects of data quality.   General guidelines for data'sSfeview have
been developed jointly by the  Regions and the,national Program Offiise..,  Each
Region uses these guidelines as  the  basis for 4ata evaluation.  Indivfdiial
Regions may augment the basic  guideline review process with additional review
based on Region-specific or site-specific £oticerns.   Regional reviews, like
the sites under investigation, vary  based^jWl the natuj?4 of the problem under
investigation and the Regional response appropriate JC0""the specific
circumstances.                                '•?''>•  ^

Regional data reviews, relating  useability of the da£a>vito a specific site, are
part of the collective assessment process.   They compieiffieat the screening
performed by the CLASS contractor^ .which is designed to identify contractual
discrepancies, and the review  pe3E£oiBfe8>--ft• S&SL-LV which is designed to
determine technical quality and  c«nssisteiicy."S i^^e|si,3^diyidual evaluations are
integrated into a collective review; tabiat is necessary'-Coar program and
laboratory administration and  managemfemt and way be used to take appropriate
action to correct deficiencies in the;Gontra<5tbr's performance.
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                                                                          DRAFT

                                  SECTION VIII

                        PERFORMANCE  EVALUATION SAMPLES  ,
      Overview
      Although intra-laboratory QC may demonstrate =€ontxactor and method
      performance that can be  tracked over time,  axi external performance
      evaluation program  is  an essential feature  of a QA program.  As a means
      of measuring Contractor  and method performance,  Contractors-participate
      in inter-laboratory comparison studies cpaducted by the EPA'51; '-litesults
      from the analysis of these  performance^Valuation samples (PESV<«>111 be
      used by the EPA to  verify the  Contrac,6»rfs  continuing ability to produce
      acceptable analytical  data.  The results are also used to assess the
      precision and accuracy of the  analytical methodspiror specific analytes.

      Sample sets may be  provided to participating .Contractors as frequently
      as on a Batch-by-Batch basis as zero blind  (recognizable as a QC sample
      of known composition); single  blind (recognizable as a QC sample and of
      unknown composition);  or double blind (not  recografcisable as a QC material
      and of unknown composition) samples.   The laboratory evaluation samples
      may be sent to either  by t^^^jra^t^ljent or the National Program
      Office, and may be  used  for*v«bgntrac€"-&tS;'c^iv :-,--;,,-
                                   SV;          /;•'•"  •" -K.''
      Contractors are required to analyze the-Camples and return the data
      package and all raw data within aihe contract required turnaround time.

      At a minimum, the results are  evaluated for compound identification,
      quantitation, and saffij)i$neontand.natioxit;,.  Confidence intervals for the
      quantitation of ;£aa*get coagbunds are t*a*S|ed  on reported values using
      population statistics.   ThijS&gency may aifcjust  the scores on any given
      PES to compensate for  any unexpected difficulties with a particular
      sample.  The Agency will n^^tf^y^b.e^,Contractor of unacceptable
      performance. ''" v>\"  ,      -i3;"T-'i <;s'»',-fe- ';s'

2     Contractor Performance ;,t

      A Contrac-tiOXl-jS results on ^Itefe-, laboratory evaluation samples will
      deteraiije''tKe t^iwaeactor's  peTHljsrmance as follows:

2.1   Ac»«ff>table, No Response/  Required (Score greater than or equal to 90
      l^rbent):             '/f
     /yh                     %-;
        fctj^meets most or  all|«ff the  scoring criteria.   No response is


2.2   Acceptabiel./IResponsel-Bxplaining Deficiency (ies)  Required (Score greater
      than or equal,to 75" percent but less than 90 percent ):


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                                                                          DRAFT

      Deficiencies exist  in the Contractor's performance.

      Within 14 days  of receipt of notification from tHe EPA, the Contractor
      shall describe  the  deficiency(ies) and the actioin(s) taken to correct
      the deficiency(ies)  in a letter to the APO, TEOj-'and EMSL/LV.
                                                     ' *;?
      An alternate delivery schedule may be proposed by tfce^.Contractor, but it
      is the sole decision of the Agency, represented ei their-by, the TPO or
      APO, to approve or  disapprove the alternate delivery scK«dt&e.  If an
      alternate delivery  schedule is proposed,,-*8;he Contractor shall?;describe
      in a letter to  the  TPO,  APO,  and the Contracting Officer why hej|&bs is
      unable to meet  the  delivery schedule lasted in this section.  The
      TPO/APO will not grant an extension ;fjear greater tfean 14 days for the
      Contractor's response letter to the ^laboratory ,<^luation sample report.
      The Contractor  shall proceed and not.a&sume thai an extension will be
      granted until so notified by the TPO at&Hfm- ,Af€K

      If new SOPs are required to be written or SOPs'Jare required to be
      amended because of  the deficiencies and the subsequent corrective action
      implemented by  the  Contractor,,,  the Contractor shall -write/amend and
      submit the SOPs per  the requpc^ns^acs listed in Exhibit E,  Section IV.
2.3   Unacceptable Performance, Response ExplaJtoing:Ife£t;eiency(ies) Required
      (Score less than 75 percent):           >j

      Deficiencies exist in  the Contractorf?s performance to the extent that
      the National Program Office has  determined that the Contractor has not
      demonstrated the capaMlity to meet the contract requirements.
                       '•$• "   '  ": ."            ; ,"*
      Within 14 days4^f receipt of: notification from EPA, the Contractor shall
      describe the deficiency(iesj^ and the actftm(s) taken to correct the
      deficiency (ies) in a letter:ito the APO, TPO,  and EMSL-LV.
                  '.;',            - •'$  %•'.' is;"'v:-r
      An alternate delivery,,  schedule may be proposed by the Contractor, but it
      is the sole decision,-,df :>the Agency, represented either by the TPO or
      APO, to approve or dis^^arjpye the  alternate delivery schedule.   If an
      alterna^ s?etel35|ery scheduler,is,.,proposed,  the Contractor shall describe
      in a Mfctir-fe»«iJie*a;PO, APO/4i*a the Contracting Officer why he/she is
      unable to meet the^ft^Livery schedule listed in this section.   The
      TEQ-/APO will not graS&ran extension for greater than 14 days for the
      .Qbijtrac tor's response '^letter to  the laboratory evaluation sample report.
          ew SOPs are require^ to be written or SOPs  are  required to be
      ametidejd. because of the|deficiencies  and the  subsequent corrective action
      impleiH|ilfe4 by the Cottfcractor, the Contractor shall write/amend and
      submit tHe\1S©Es per^tfee requirements listed  in  Exhibit E,  Section IV.
                                     E-29

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                                                                    DRAFT

The Contractor shall be notified by the TPO, APO,  or  Contracting Officer
concerning the Contractor's remedy for the Contractor's unacceptable
performance.  A Contractor may  expect, but the EPA is not  limited to,
the following actions: reduction of the number 
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                                                                      DRAFT

                              SECTION IX

                          DATA PACKAGE AUDITS

  Overview                                      :,
                                              •  I - I ' '
  Data package audits are performed by the Agency f or jprpgram overview and
  specific Regional concerns.  Standardized procedures have been
  established to assure uniformity of the auditing process., i I>ata  packages
  are periodically selected from recently -;t?eceived cases.  They-ar-e
  evaluated for the technical quality of %ardcopy raw data, qualifrjjr
  assurance,  and the adherence to contractual requirements.  This  function
  provides external monitoring of progacam QC requirements .
                                       " „         - , ;c
  Data package audits are used to assess the technical quality of  the data
  and evaluate overall laboratory perforrfajje«,. 'Ufiey provide the Agency
  with an in-depth inspection and evaluation of Ithe Case data package with
  regard to achieving QA/QC acceptability.   A thorough review of the  raw
  data is completed including: a check of ins truments, printouts,
  quantitation reports, chromatograms , deviations f rom tt&e contractual
  requirements,  a check for -iteabsiKci|»B;ioj8«,and calculation errors,  a review
  of  the qualifications of th&^laboratoTyi^rseaiJel -involved with  the
  case,  and a review of all current SOPs on/ifile.  •  ,

  Responding to the Data Package Atidit Report:

  After completion of the data package "audit , the Agency may send  a copy
  of  the data package %-attdJbt .report to *the  Contractor or may discuss the
  data package audit. -report, 4aring an oiifsate laboratory evaluation.   In a
  detailed letter ''lo the TP0|sJAPO,  and EHSJJL-LV,  the Contractor shall
  discuss the corrective actions implemented to resolve the deficiencies
  listed in ths;;data package Japdit^ report  within 14 days of receipt of the
  report.   An attenuate delfeidiy ittih£$u&e  may be proposed by the
  Contractor,  but i£ Js the sole decision  of the Agency, represented
  either by the TPO or.&BD,  to approve or  disapprove the alternate
  delivery schedule.   I f: -in (alternate delivery schedule is proposed,  the
  Contr actor I shall describe"%»'^a letter to  the TPO,  APO, and the
  Contracting "Ofeflgserpwhy he/sBeJis unable  to meet the  delivery schedule
  lis^taila in this secAosa.   The TPO/APO will not grant an extension for
  gzt^ater than 14 days '^fer the Contractor ' s response letter to the
  laboratory  evaluations-sample report.  The Contractor  shall proceed  and
/:aot  assume  that an extiejitsion will be granted until so notified by the
     ;; -and/or  APO.        ~:\,
 If new jSJDBs are  required to be written or SOPs are required to be
 amended t>ecat^se  of  tijte  deficiencies and the subsequent corrective action
 implemented fcyJiaiej'Gbntractor,  the Contractor shall write/amend and
 submit the SOPs 'per the requirements listed in Exhibit E, Section IV.

                                 E-31

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                                                                   DRAFT

Corrective Actions

If the Contractor fails to adhere to the requirements listed in this
section, the Contractor may expect, but the Ageaey is not limited to the
following actions: reduction of numbers of samples sent under the
contract, suspension of sample shipment to the Contractor, data package
audit, an on-site laboratory evaluation, re»e4ial lafeeratory evaluation
sample, and/or contract sanctions, such as a'Cure Notitee,.
                               E-32

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                                                                      DRAFT

                               SECTION X

                    ON-SITE LABORATORY EVALUATIONS ;

  Overview                                        .

  At a frequency dictated by a contract laboratory's1 performance, the APO
  or his/her authorized representative will conduct an' tm»nsJ.te laboratory
  evaluation.  On-site laboratory evaluations  are carried"traSs-sto monitor
  the Contractor's ability to meet selected terms and conditioiss ;&pecif ied
  in the contract.  The evaluation process incorporates two separate
  categories:  Quality Assurance Evaluation and an Evidentiary Audit.

  Quality Assurance On-Site Evaluation ,          ,;" ,:

  Quality assurance evaluators inspect the Contractor's facilities to
  verify the adequacy and maintenance  of instrumentation,  the continuity
  of personnel meeting training requirements,  sajji^the acceptable
  performance of analytical and QC procedures.   The,:;|Cmtractor should
  expect that items to be monitored will include,  but ~m>t. be limited to,
  the following items:      , -'1.  ;~ f'   ,Si, ,

  •      Size and appearance of!?£he facility;

  •      Quantity,  age, availability, scbe«tuled maintenance and performance
        of instrumentation;            •;

  •      Availability,,, a|fftsf>riateness,|,-Review of tneAj€pntractor's sample  analysis/data package
   --"-,->'  inspection/dat» management procedures.

~^ior  to an on-site evaluation, various  documents pertaining to
"-^^gprmance  of the spe&jbfic Contractor  are integrated in a profile
 pac1skge,,for  discussio^iiluring the evaluation.   Items  that  may be
  incluctei,|$re previous>>iarh-site reports,  laboratory evaluation sample
  scores, R'i^ijopal re-s|^w of data,  Regional QA materials,  data audit
 reports, ana;-^ata,s-alend reports.


                                 E-33

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                                                                           DRAFT

3     Evidentiary Audit

      Evidence auditors  conduct an on- site laboratory evaluation to determine
      if laboratory policies and procedures are in place to satisfy evidence
      handling requirements  as stated in Exhibit F.  \The evidence audit  is
      comprised of the following three activities .     ;  ;>

3.1   Procedural Audit:                                        ;f

      The procedural audit consists of review jaiid examination of actual  SOPs
      and accompanying documentation for the iipBllowing laboratory ope^rations :
      sample receiving,  sample storage, sanfrjfce identification, sample
      security, sample tracking (from recent to completion of analysis)  and
      analytical project file organizatiottJ|4nd assembl^,

3.2   Written SOPs Audit:                      "'•• •'•,  '{
                                                 ' ^ ,,  ,<' '
      The written SOPs audit consists of review and examination of the written
      SOPs to determine  if they are accurate and complete for the following
      laboratory operations:  sampl«|8-r,^ceiving, sample storage, sample
      identification, sample secwi%jj£j*saaif*l*| Bracking (from receipt to
      completion of analysis) and:^tolytica'f>*^«J0|Ct 'tfiZLe organization and
      assembly.                    ^"-i-_         ,-"'!' ""'"' -••'
                                      '         '• '
3.3   Analytical Project File Evidence. &.udit^

      The analytical project file evidenc*:§audit consists of review and
      examination of the ^nai^tical proj ectffile documentation.  The auditors
      review the files ,to:  dete'rsti^e:
      m
    The accuracy of the  cl^seument inventory;

    The compi*taeness ofi'tt^f^leV]j'"'

    The adequacy df&tiUftccuracy of the document numbering system;

    Tr-ae^eSblli-ty of samp'le'-Mfc^tivity;

 / rjfltdentif icat£d»i>**f activity recorded on the documents; and

;--   Error correctiong^ethods.

         of the On-SJjte  Team's Findings
                                  auditors present their findings and
      recommendations  for ^errective actions necessary to the Contractor
      personnel.    -   : ,_-
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                                                                          DRAFT

5     Corrective Action Reports  For Follow-Through to Quality Assurance and
      Evidentiary Audit Reports

5.1   On-Site Laboratory Evaluation

      Following an on-site evaluation,  quality assutiance and/or evidentiary
      audit reports which discuss  deficiencies found during £he on-site
      evaluation may be sent  to  the Contractor.   In a detailed ietter, the
      Contractor shall discuss the corrective actions implementfedtfco resolve
      the deficiencies discussed during the  onisite evaluation aridb«J,i&cussed
      in the reports to the TPO, APO,  EMSL-LV;?(response to the qualrtejfe;
      assurance report), and  NEIC  (responseyfeo the evidentiary report) within
      14 days of receipt of the  finding or ftthin the tiaae agreed upon between
      the APO/TPO and the Contractor.   Apyaftemate delivery schedule may be
      proposed by the Contractor,  but  it i«,jjtt»e sole,«ecision of the Agency,
      represented either by the  TPO or APO,  tsb,:,<4ppr^e or disapprove the
      alternate delivery schedule.   If an alternate'-^delivery schedule is
      proposed, the Contractor shall describe in a'lefcfcer to the TPO, APO, and
      the Contracting Officer why  he/she is  unable to' ime£-the delivery
      schedule listed in this section.   The  TPO/APO will 'nott-grant an
      extension for greater than'^.^^.^ipc^t^e Contractor's response letter
      to the laboratory evaluatic^sample'^SjSdlSfc.; "1S»e. Contractor shall
      proceed and not assume  that  ati!-sextensionw£il:%e«£;kanted until so
      notified by the TPO and/or APOi        _-/:

      If new SOPs are required to  be wfittejror SOPs are required to be
      amended because of the  deficiencies aild the subsequent corrective action
      implemented by the Costlcactor, the Contractor shall write/amend and
      submit the SOPs ,;p«r the'*requirements lifted in Exhibit E, Section IV.

5.2   Corrective Actions          -j
                  f\. •            '•• •'--
      If the Contfactas^,fails ^.i^bife«l-|t4*yie requirements listed in this
      section, the Contractor may  expect, but the Agency is not limited to the
      following actions: ±»
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                                                                     DRAFT

                             SECTION XI

             QUALITY ASSURANCE AND  DATA TREND ANAJSSIS

Overview

Data submitted by laboratories are subject C© revlewrficpm  several
aspects:  compliance with contract -required QC, useabHSjjty,  and full
data package  evaluation.   Problems resulting from any of>these  reviews
may determine the need for a on-site laboratory evaluation *a%d/pr a
remedial PE sample.  In addition,  QC paafsiscribed in the methods'^arovides
information that  is continually used Jsj&'the Agency to assess sample data
quality, Contractor data quality,  ani&rogram da^.; quality via  data
trend analysis.   Trend analysis is.~l^omplished;%y entering  data into a
computerized  data base.   Statistical-'|p4j*prts ty& evaluate specific
anomalies or  disclose  trends in many affeks,, including the  following, are
generated from this data base:              ;  ;

•     System  Monitor Compound Spike Recovery;   "-•-  .-,,

•     Laboratory  Control S^«tei,iM^sis?»i:y;
                           'i ,•    --&;/'«!  "'• ':.  ,
                            "-• ?-        ' " *'& ;&' ';.
                             ••••:-            s?    ;'•  ""
m     Method  Blanks;         -:-«-         '•">    •"-•"-
                                        ;?.".
•     Initial Calibration and Calibration Check Data;  and

•     Other QC and Method Parameters-/
                    s   N^             *'
Program Benefits  •;.      •?' /,           '\S,
  ~ ~          ,;,'  ,"        ',,".'•'            ;'," ',

Program-wide  Statistical results are usei to rank laboratories  in order
to observe die,.relative peieSo^Bjancie, of  each Contractor in  a  given
protocol agai-ijiS.fciI.ts pee^9»';^||(^i{g|^%s are also used to  identify
trends within la&sratories.  The results of many of these  trend analyses
are included  in ovelrafiL:.evaluation of a Contractor's  performance,  and
are reviewed  to de termini if corrective action or an  on-site laboratory
evaluatioH'itsRadicated iri.jteder to meet the QA/QC requirements of the
contra&tfe :' '-'•'"•* ^ll, ,*-,        '-J-V .'
                 -\ '*
                   'Cri
           performairat%.over time is monitored using these  trend analysis
           to detect cppiartures of Contractor output  from  required or
        levels of qual||jfy control, and  to provide an  early-warning of
           QA/QC  probljrais which may not be apparent from the results of
              case.   fit
                     i'>' "
As a furtfesr  :||enefit)j3fco the Program,  the database provides the
information n^ededfcb  establish performance-based criteria in updated
analytical proto&olis,  where advisory criteria have been previously used.

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                                                                   DRAFT

The vast empirical data set produced by contract laboratories is
carefully analyzed, with the results augmenting theoretical and
research-based performance criteria.  The result -is a continuously
monitored set of quality control and performance ^criteria specifications
depicting what is routinely achievable and expected of environmental
chemistry laboratories in mass production analyses ;of environmental
samples.  This, in turn, assists the Agency in meeting dts objectives of
obtaining data of known and documented quality.
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                                                                    DRAFT

                            SECTION XII

                          DATA MANAGEMENT

Overview

Data management procedures are defined as  pr«. .'"  ",,,/_

The record of changes in the form of corrections and updates to data
originally generated, submitted,9 lland/aa; resubmitted  shall be documented
to allow traceability of updates.  Be'cotnentation shall include the
following for each change :

•     Justification or rationale for t&ie change.
               . ;; - "        ^;P           ---
                           ^
•     Initials <-of the persotv.inaking the change  or  changes .  Data changes
      shall fee implemented(46^d, reviewed by a person  (or group)
                   >f the ^M^y^^^ting, the  deliverable .
      Change documenfcatS.on shall be  retained according to the schedule
      of the original
              «e)d electronic v^j|t^a or  other  deliverables  shall be
      reinspected as ---a part of the laboratories'  internal inspection
      process prior fe&^fe submission.   The entire  deliverable, not just
      the changes, sha^t be inspected.
      The Laboratory Mfaager shall approve  changes  to originally
                delivei^les.
                      "
      DocomenSation of data changes may be  requested by laboratory
      auditors ^ •' J,
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                                                                    DRAFT

Lifecycle management procedures  shall be  applied to computer software
systems developed by the  laboratory to be used to generate and edit
contract deliverables.  Such systems shall be thoroughly tested and
documented prior to utilization.

•     A software test and acceptance plan inclwliijg test requirements,
      test results and acceptance  criteria shall be Developed, followed,
      and available in written form.

•     System changes shall not be  made disectly to production, .systems
      generating deliverables.   Changes^shall be made first to '-a.'""
      development system  and tested prior to implementation.
                                      V            '"
m     Each version of the productions system will'Jje given an
      identification number, date  of siestallatlon,  date of last
      operation, and archived.         " \     \

•     System and operations documentation shall.- "be developed and
      maintained for each system.   Documentation 'Shall include a users
      manual and an operations, and maintenance manual.

•     This documentation  shajll be  avaliiaKle' for on-site review and/or
      upon written request by^fehe  TPO orJHEIC. '

Responsibilities                 ' ;

Individual(s) responsible for the  following functions shall be
identified:       _: » -'  ; ,-

•     System o^ration and'iftaintenance "Including documentation and
      trainings/'           \ , -
            ^ -  ,_          .-' t^. ,,.,.,.„,,,,	
•     Data base!~iaitegrity^,ilsc1atfli^-,data entry, data updating,  and
      quality contxoi,

•     Data and system Searsucity,  backup, and archiving.
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                                                     DRAFT
CHAJN*C^-,CUSTODY, DOCBltENT CONTROL,
              OPERATIRg PROCEDURES
                                                 08/23/94

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                                                                          DRAFT
1.0   Sample Chain-of-Custody

      A sample  is physical  evidence collected from a facility or from the
      environment.  Controlling  evidence is an essential .part of the hazardous
      waste investigation effort.   To accomplish tills,  Contractors are
      required  to develop and implement the following sample identification,
      chain-of-custody, sample receiving,  and sample tracking procedures.

1.1   Sample Identification                  -                       '

      To assure traceability  of  the samples while in possession of the
      Contractor, the Contractor shall ha*<6,,a specified method for maintaining
      identification of samples  throughout^tfee^laboratory.

      Each sample and sample  preparation container,shall be labeled with the
      EPA number or a unique  laboratory identifier.   If a unique laboratory
      identifier is used, it  shall  be cross-referenced "'to., the EPA number.

1.2   Chain-of-Custody Procedure^i.-ss;'-.^;,'.1;'-,;" ?„  _,

      Because of the nature of the^data being .collected, :;the custody of EPA
      samples must be traceable  from 3jj^e time itihe samples are collected until
      they are  introduced as  evidence'!gaa legpal proceedings.  The Contractor
      shall have procedures ensuring that EJ?& sample custody is maintained and
      documented.  A sample is under custody if:
                        '"'   ;8J, i „           ' i
      •     It  is in your possession;  or     ^
                     ,;           'if",,i           'i-,
      •     It  is in your view afifeer being in your possession; or

      •     It  was in your  possession:;saiKi'jioti locked it up; or

      •     It  is in a designated secure area.  (Secure areas shall be
            accessible only to.|authorized personnel.)
1.3  Sample |fe«lvitig- feeocedures   • *}_ '•

                  The Conttidctor  shall  designate a sample custodian
                  responsib&,ifor receiving all samples.
                            ' ,'•-"";
                             '" "
                  The Contracstor  shall  designate a representative to receive
             ;.;     samples  icifMie  event  that the sample custodian is not
           "':^ available:.-'

      1.3.3       "TStejslcoaiSition of the  shipping containers and sample bottles
                  shaXl".ibe inspected upon receipt by the sample custodian or
                  his/her  representative.
                                      F-2                              08/23/94

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                                                                     DRAFT

1.3.4        The condition of the custody seals  (intact/not intact)  shall
             be inspected upon receipt by the  sample  custodian or his/her
             representative.

1.3.5        The sample custodian or his/her repiesentative shall check
             for the presence or absence of the ^following documents
             accompanying the sample shipment:.;       :

             • Airbills/airbill stickers;                '"•'

             • Custody seals;          ;!=,                       '  -

             • Quick Turnaround Method CQTM) Traffic  Report/Chain-of-
             Custody (TR/COC) records,;,           s  •

             • SAS  packing lists,  if appli,eabj|e* and

             • Sample tags.                     ,,
                                                 '*  -,
1-3.6        The sample custodian or his/her represeiitafcive  shall sign
             and date all f^Es^^|e^,g,||TM TR/COC records  or packing
             lists,  and air&tils) "accicHBpii^fia^;-,t%e samples at  the time  of
             sample receipt.  ''%«         »?-   ~  f 'I/
                              ''*••         •• sare,,,received

                             of the  shipping container;
                     ' ~"j
                     ^il'
                  Preface or  absence  and condition of custody seals on
                  shipfflng and/or sample containers;
                       < >-.-'•
                      '2J'
                  Cust^ay seal numbers,  when present;

             i^    CoMition  of the  sample bottles;

              ' : -f-Pxesence or  absence  of airbills or airbill stickers;

                  Airbill or airbill sticker numbers;


                                F-3                               08/23/94

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                                                                          DRAFT

                         Presence  or absence of QTM TR/COC records;

                         Presence  or absence of EPA SAS -packing lists;

                         Presence  or absence of sample tags;

                         Sample  tag  identification ••numbers across-referenced to
                         the  EPA sample  numbers;                .

                         Verification of agreement or non-agreement ȣ ,
                         information recorded |:on shipping documents and sample
                         containers;  and -
                  •     Problems  or  discrepancies.     •

1.4   Sample Tracking Procedures             *  •;;;'  , "*

      The Contractor shall maintain  records  documentit^ all phases of sample
      handling from receipt  to  final analysis.
                                 $"'V
2.0   Document Control Procedure^ ' • 14 £jy~ %:,.: -,,;;/> ^,
                                 »<'*. ;*   ' 'V'S'K*V' I''; ,>4lT *',/
      The goal of the laboratory  doiraaanent control program is to assure that
      all documents for a specified  B^ch wili^be accounted for when the
      project is completed.  Accountably, dofisaents  used by contract
    .  laboratories shall include,  but nctib^flimited to, logbooks, QTM TR/COC
      records, sample work sheets, bench %££ets, and other documents relating
      to the sample or sample:;:analyses.   Tbse^following document control
      procedures have been estat>|.;ished  to ashore that all laboratory records
      are assembled aaw! stored  fi|r
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                                                                    DRAFT

            for performing the  activity  at  the  time an activity is
            performed.

2.1.4       Logbook entries shall  contain the time of analysis (in
            military time) and  be  dated  (montfa/ltay/year)  and signed by
            the person responsible for performing; "the activity at the
            time an activity is performed.   ,

2.1.5       Logbook entries shall  be  in  chronological order.;, Entries in
            logbooks, with the  exceptioji -of instrument run lt>gs -and
            extraction logs , shall include  only one Batch per page .

2.1.6       Pages in both bound and unbound logbooks shall be
            sequentially numbered.  --\          •"•

2.1.7       Instrument run logs shall be laBsiBrfeained so as to enable a
            reconstruction of the  run sequence  of individual
            instruments.                        •';  ••.

            Because the laboratory must  provide copies of the instrument
            run logs to EB&., *3th$ tla^mtpry^ may exercise  the option of
            using only labbnitory  or!H^<«asg»l^, identification numbers
            in the logs for Staple ID ratfher than government agency or
            commercial client tiames to ^reserve the confidentiality of
            commercial clients. • ••>   ,.'; /

2.1.8       Corrections to supporting documents and raw data shall be
            made iy-^b?aw^Bg a single ;l'ine through the error and entering
            the.; correct i'^alormation.  Corrections  and additions to
            supporting dociaents and  raw; data shall be dated and
            initialed.  No,|i6aformation shall be obliterated or rendered
           , Unreadable .  J:»:L. ,  ,„ ....... ,,
            •*:&,.      .'•£'&&}:.•&,$*
            All notations shall be recorded in  blue or black ink.
                     ^ '; ^ *
                      .;
            Unused portions of  documents shall  be "z'd" out.
2 . 1 . 9\ is -- ' ''" "Tb^ltS^aXiractor sM'll. assign a numerical  identifier to each
            electrojiis transfer of EPA data.
                    '-•?
            All data 6j|£nsferred using direct  electronic  transfer
            technology:||o the data user shall  be printed  in hardcopy and
            filed in t^ CBF.  The Contractor  shall  record  the following
            informatLMl?on the hardcopy or on  a separate  piece of paper
            attachedflSo the hardcopy, as well  as a sequentially-numbered
            ^ - /! *,$,;•*
            m  "-'Ts-flfche laboratory individual responsible  for  the
                  electronic transfer;

            •     The date and time of the electronic  data transfer;

                                F-5                          .    08/23/94

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                                                                          DRAFT

                  •      The  individual  for whom the data was electronically
                         transferred;

                  •      The  status  of the data that was; electronically
                         transferred (e.g.,  first subaifctal or second
                         submittal);  and            ,;  ,';   ,

                  •      The  numerical identifier of the eleetSPomc transfer.

      2.1.11      If an  RPM  authorizes  the Contactor to transmit;preliminary
                  form 1 or  raw data to the d«ta user via & fax (or fao?)
                  machine, then the Contractor shall:
                                          ,-£•<          ,*•
                  •      Assign a numerical ,identifier :£o each fax;

                  •      File the fax originals*fn title CBF;

                  •      Record the  information identified in paragraph 2.1.10
                         on the fax  originals;            ;:,
                        Record  taB^&B!C^^8aBfe|ej,,of EPA data in a
                        sequentially-numbered logbook;  and
                                   ''"'¥•        -»•' '•    ""' '•'''
                        Record  the  aij|torizat3ym information (e.g., Regional
                        Program Managers  name,  date,  time, and reason for
                        facsimile transmission).
2.2   Consistency of

      The Contractor &hall assigi|t|k Document 'patrol Officer (DCO) responsible
      for the organisation and  assembly  of the CBF.

      All copies of laboratory ::*yjiiuments::isfciill be  complete and legible.
      Original documents wfctl.«3|,. include  information relating to more than one
      Batch shall be filed in%tsst; CBF of  the  lowest batch number.  The
                         placed:it|K,|e%e  other  CBF(s) and the Contractor shall
                      iyijf^ informatS^if  on the copy(ies) in red ink:
                        • i. .
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                                                                           DRAFT

2 . 3   Document Numbering and Inventory Procedure

      In order to  provide document accountability of the completed  analysis
      records, each item in the CBF shall be inventoried and assigned a
      serialized number as described in Exhibit B.

      All documents relevant to each sample Batch, sinclucybtjg logbook pages ,
      bench sheets,  chromatograms ,  re -preparation records, 'reaaalysis records,
      records of failed or attempted analysis, custody records", 1 «£c. ,  shall be
      inventoried.                             -,                   "•':•• -

      The DCO shall be  responsible for ensuring that all documents  generated
      are placed in the CBF for inventory and are delivered  to  the  appropriate
      EPA Region or other receiver as designated by EFA:.:  The DCO shall place
      the sample tags in plastic bags in tlj.e'Vfile .

2.4   Storage of EPA Files                       :-  -

      The Contractor shall maintain EPA laboratory documents  in a secure
      location.                   »-  .
                                  .   -•*  ,
2.5   Shipment of Hardcopy  Data De|iverabTe'^' 4'fJ   v  , ,.
                                  "i ^         <•''•;-  '   ,  ;
      2.5.1       The Contractor shall documejate shipment of hardcopy
                  deliverables  packages; to tihe recipients .  These shipments
                  require custody seals1 it:he containers placed such  that
                  they cannot be opened wil&out damaging or breaking the  seal.
                  The Contractor shall document what was sent, to whom, the
                  date,,; and fiherfflethod (carrier) used.
                          of  the  tiansmittal letter for the CBF shall be  sent
                  to,,NEIC/CEAT a»t: the, .CLASS contractor.
                  •                "•• '- "   "' ' '
      2.5.2       Authorised Alternative Transfer Methods
                  If the Regi^a^a.  Program Manager authorizes the Contractor  to
               ,; : '-^-latswisfer EPA ;is^||i^C,o the data user by mailing the diskette
          ,  ,}'. '' "ratfeejTs -t;han via  aiir«fct electronic transfer technology, then
         »;,; -       the CbtttsCactor shall follow the procedures described in the
        *'--        above patibsferaph  2.5.
        .ij                 ^T?
      .&1'                   '%t.
3.0  ,J1gi?ecifications For Writan Standard Operating Procedures
      The Soiitractor shall IpD^e written standard operating procedures  (SOPs)
      for retMsi|>;t of sampleji|, maintenance  of custody, sample identification,
      sample stfeage,3 sam|ii tracking,  and assembly of completed data.

      An SOP is defiri«4|ias a written narrative step -wise description of
      laboratory operating procedures  including examples of laboratory
      documents.  The SOPs shall accurately describe the actual procedures
      used in the laboratory, and copies of the written SOPs shall be

                                      F-7                              08/23/94

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                                                                          DRAFT

      available to the appropriate  laboratory personnel.   These procedures are
      necessary to ensure that  analytical data produced under this contract
      are acceptable for use  in EFA enforcement case preparation and
      litigation.  The Contractor's SOPs shall provide mechanisms and
      documentation to meet each of the following specifications and shall be
      used by EPA as the basis  for  laboratory evideaa

3.2   The Contractor shall have written SOPs :fesr receiving and logging' in of
      the samples.  The procedures  shall ine&ikde but not be limited to
      documenting the following i
            Presence or absence  of QTM TR/IPC; records ^'
                                             : "-; " ,_  if-
            Presence or absence  of airbills/airbillAStickers;

            Presence or absence  of SAS packing  lists, HE applicable;

            Presence or absence  of:          (.

            Condition of the  shi^ptng container;

            Condition tljp'.•£&&  sample bottles;

            Verification of aipaesement or non-agreement of information on
                      Documents^B«4i,sample containers;
            iResolution oW^aroblems of discrepancies with the CLASS contractor;
            and           \'-',~
                              ,
            The definition  otl^any terms used to describe sample condition upon
            receipt  (e.g.,  g0^Ai,  fine,  ok).
3.3   The C6^fc«|c;tor shall,|^ve  written SOPs for maintaining identification of
      EPA sanp^^K^ja^roughjMtib the laboratory.

      If the Contracdefellassigns  unique laboratory identifiers, written SOPs
      shall include a  description of the method used to assign the unique
      laboratory identifier and  cross-reference to the EPA sample number.


                                       F-8                              08/23/94

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                                                                          DRAFT

      If the Contractor uses  prefixes or suffixes in addition to sample
      identification numbers,  the written SOPs shall include their
      definitions.

3.4   The Contractor shall  have written SOPs describing all storage areas for
      samples  in the laboratory.   The SOPs shall include ,a list of authorized
      personnel who  have access or keys to secure storage areas.

3.5   The Contractor shall  have written SOPs describing the meliioa by which
      the laboratory maintains samples under custody.             :;
                                             ,-.'. ''                     "-'
3.6   The Contractor shall  have written SOPs*Describing the method by which
      the laboratory maintains the securityjbf any areas identified as secure.

3.7   The Contractor shall  have written SGf^gfor traciking the work performed
      on any particular sample.   The tracking SOP skill include:

      •     A  description of  the documents used to record sample receipt,
            sample storage, sample transfers,  sample preparations,  and sample
            analyses;             r,                          ;
      •     A description  of  the^lfecuments'-^yle^,;*^ «ecprd calibration and
            QA/QC laboratory  work;*;         />        I

      •     Examples of document  formats and laboratory  documents  used in the
            sample receipt, sample  storage,  sample transfer,  and sample
            analyses; and

      •     A narrative*step-wCsfe, description*of how documents  are used to
            track samples.      !';|];           '  =:

3.8   The Contractpy of the  electronically  transferred  data.
               '*•'*•%,">.    - f"
            Ensuring:gehad: ;;fche hardcopy is placed  in  the CBF.

            Recording the following information on the  hardcopy or  on a
            separate piece of paper attached  to the  hardcopy,  as well as  in a
            sequentially numbered logbook:

                                      F-9                              08/23/94

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                                                                           DRAFT
                   The laboratory individual responsible  for  the electronic
                   transfer ;

                   The date and time of the electronic ^data transfer;
                   The individual for whom the data !«ras>!; electronically
                   transferred;                      ;      •'   ;;,

                   The status of the data that was electronically transferred;
                   and                          s,                  -' •:.

                   The numerical identifier of'-the electronic transfer.

3.9   The Contractor shall have written SCSSfs for the ase of a fax machine to
      transmit  EPA data or preliminary foTf^-^-or raw'-lfata  results to the data
      user.  The written SOPs shall include the*ffQlio*ring.

      •     Assigning a numerical identifier to each fax;

      •     Filing of fax originalss,4n the CBF;

      •     Recording the information ideni*i^li^l''ixi-^zaigraph 2.1.10 on the
            fax originals;         ':'V;          !V  '< •>

      •     Recording the fax transferikiuf E1E|&. data in a sequentially numbered
            logbook as described in paragraph 2.1.11; and

      •     Recording the,:autl$M:ization information (e.g.,  Project Officer's
            name,  date,' ;*trlme,"aj^t reason fordjlfacsimile transmission).

3.10  The Contractor Ssrhall have vafitten SOPs for organization and assembly of
      all documents,-:arelating to «&eh Batch. ^Doctoments shall be filed on a
      batch-specifre/J^iaesis.  Th4i^||t*dMll^s<:i*hall ensure that all documents
      including logbook -|Mg§es,  sample tracking records, chromatograms,
      computer  printouts, s^aif .data summaries, correspondence,  and any other
      written documents having.Vjseference to the Batch are  compiled in one
      location  fiorj'StiJiHiiission €b-:>|8?Ai   The written SOPs shall include:

      •  ,-j; >4 description;--^ the numbering and inventory method;

      • f"   A description ofps^he method used by the laboratory to verify
     .|3 ; '*   consistency and igmpleteness of the CBF; and
       '• "*:C  .                 1 •
      • '" "'."^Procedures for tl&6 shipment of deliverables packages using custody
4.0   Handling Of t^gMgiteial Information
                       >I'~*,A
      A Contractor  conducting work under this contract may receive
      EPA-designated confidential information from the Agency.   Confidential
      information must be handled separately from other  documentation

                                      F-10                              08/23/94

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                                                                          DRAFT

      developed under this  contract.  To  accomplish  this,  the following
      procedures for the handling of confidential  information have  been
      established.

4.1   All confidential documents shall be under  the  supervision of  a
      designated DCO.

4.2   Confidential Information

      Any samples or information received with ,a request of  confidentiality
      shall be handled as "confidential."  A Separate locked file shaM be
      maintained to store this information and shall be segregated  from other
      nonconfidential information.  Data  generated from Confidential samples
      shall be treated as confidential,  l^on receipt o£ confidential
      information, the DCO will log these ;*J®#uments JLnto a Confidential
      Inventory Log.  The information will theft "i»e available to authorized
      personnel but only after it has been signed  oat to that person by the
      DCO.  The documents shall be returned to the locked file at the
      conclusion of each working day.  Confidential  inf«i»ation may not be
      reproduced except upon approyal by  the EPA APO.  The ,B|CO will enter all
      copies into the document aeiatxolJL -ssjgrsfsenk described above.  In addition,
      this information may not be^Stispos'ed^l^cftt upon approval  by the EPA
      APO.  The DCO shall remove aaflDetain thjfe-icovei'-page of any confidential
      information disposed of for one^year adS {shall keep a  record  on the
      disposition in the Confidential Inventory  Log.
                                     F-ll                             08/23/94

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GLOSSARt &F
AND ACROSUJ 11ST
                                         DRAFT
                                        08/23/94

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                                                                         DRAFT
                              TABLE OF CONTENTS
SECTION I:     GLOSSARY OF TERMS	




SECTION II:    ABBREVIATIONS AND  ACRONYMS.
PAGE






G-3




S-8
                                     G-2
    08/23/94

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                                                                           DRAFT

                                    SECTION I

                                GLOSSARY OF TERMS

 ALIQUOT -  a measured portion of a sample  taken for  analysis.

 ANALYSIS DATE/TIME - the date and military  time of ,,£he "itijecfeion of the
 sample,  standard,  or blank into the GC system.                -,,

 ANALYTICAL SEQUENCE - an analysis sequence  consisting of an initial? - ,
 calibration or a daily calibration check  standard,  method blank(s),  laboratory
 control sample(s)  (LCS),  field sample(s), iaasttrument  blanks,  and a performance
 verification standard(s).   There are two  ty|»es  of analjtecal  sequences:  an
 initial calibration analytical sequence au&i.a  daily calibration  check
 analytical sequence.  An analytical sequence''saaist not exceed  24  hours.
                                              *  < \ ',   ' ^s,
 AQUEOUS  NON-MISCIBLE OIL SAMPLE - Oil sample that ii.not miscible with  water.

 AQUEOUS  MISCIBLE OIL SAMPLE - Oil sample  that  is miscitlLe swith water.

 BATCH  -  a  unit within a sample C£^;t^t:U«,r.used to identify  a group of
 samples  for delivery.   A Batch is'-.jl^roup o^ii&ld:. Samples  (up to 30
 fractional analysis) within a Case ^received in>bne SaylS"Data from all  samples
 in a Batch are due concurrently withfaa the specified  turnaround  time.
                                      s      ^ •: ,
 BLANK  -  for the purpose of this SOW, there iare  three  required blanks: method,
 instrument,  and cleanup.   All protocols (.1,*.,  volatile,  PAH, phenol,
 pesticide,  and PCS)  require saefihod and installment blanks.  A  method blank must
 be performed with  each' ftetchT -f|q&*,each samplS|;ifraction,  and for  each matrix.
 In addition,  the pes4Sici.de and P&ijj£protocols ^6quire  the  analysis of a  cleanup
 blank  if the optional, sulfur cleapop step is employed.  Also, an additional
 method blank shall;lie analyzed alfttjg.m^h,samples that are filtered.
CALIBRATION CHECK  -  a dSeek standard analyzed at the start of each daily
analytical sequence  to deteigttine if the initial calibration is still valid.
                            ;, 1 C1;

CALIBRATION FA^T<|B..-f -the total*'adjja>,of a peak(s) divided by the mass injected
(in             ''"''' ' "           "
CASE - apEtnite, usually predetermined number of samples collected over a
given -SipSe period from a paSplcular site.  Case numbers are assigned by the
Samplej^anagement Office.   A|i^ase consists of one or more Batches.
     "!-\||?:-,                 Zil
CLP Analytical Services Supgi&rt (CLASS) contractor - At times during the
length of tftli.^ntract,  tfe^JcLASS contractor acting on behalf of the
Headquarters AP%Jafsd/or R.ejg|6nal TPO,  will provide directions to the
Contractors.      '«¥ 1*^,4'"
                                      G-3                              08/23/94

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                                                                           DRAFT

CLEANUP BLANK-  1 ml  of hexane carried through the pesticide or PCB sulfur
cleanup procedures to  determine whether contamination was introduced during
cleanup .                                                :

CONTRACT REQUIRED QUANTISATION LIMIT (CRQL) - target compound quantitation
limits as  specified  in Exhibit C.                     ''I

CONTRACTOR - synonymous with Laboratory as used herein.      ?;
                                                              -;    , ,

DAY - unless otherwise specified,  day shall me^sa calendar day.     -
                                             J>'                     'J- ..-
                                             ,>                         •£-.
DATA SYSTEM - for the  purpose of this SOW, ^/integrator/computer system that
allows the continuous  acquisition and prin^SSCt of timers, intensity data
throughout the  chroma to graphic program.  ,  |^/         , |5'
                                           *"*; ***,'.&        ** " •
                                           "•" f" -,      " ,
DILUTION FACTOR - a  dilution factor (i.e., a sjh|gj.e|whole number, such as
"100" for  a 1 to 100 dilution of a sample) must fee .^ported for all samples
which are  diluted.   A  sample dilution considers all: factors which affect the
sample CRQL.  Some common examples include: extraction or analysis of a
smaller sample  aliquot; dilution of.a sample or sample extract; and dilution
of a smaller aliquot of a methanoll «X§i^f:";f or volatile s analysis.
                                 v \'%    '"'''' '~^\^^ !? <.
ELECTRON CAPTURE DETECTOR (ECD)  -  director use^in'lihersanalysis for pesticides
and PCBs in this SOW.                .1        ,;?

ELECTROLYTIC CONDUCTIVITY DETECTOR (ELCS:JC%<1|1ALL)  -  detector used in series
with photo-ionization  detector (PID)  in tfbel analysis for volatile organics in
this SOW.               r-^-^            ^-:"-
                             ~"
                                             i> '£_
EASTERN STANDARD TIME?f?EST)  or ElipSERN TIME -^ifee time of the fifth time  zone
west of Greenwich  thitt  includes
EXTERNAL STANDARDS' ^jTaogget com^i^is|^iii^i.^€d at a known concentration prior
to sample analysis  to  determine calibration factors.
FLAME IONIZATION DETECTOR (FH3_,;r^ detector used in the analysis for PAHs  and
phenols in
GOVERNMENT]/ the  terms G^^piment and Agency are used synonymously in  this SOW
and refefisjrto the US Goverlsi^at or the US Environmental Protection Agency
         •tf'                  'ik'.
(EPA).^-^
HEATED' 4|P|KPSPACE  SAMPLER -  device for sampling the headspace gases and  for use
in direclf^i^^ption  GC volatl^fces analysis.
                            '
HIGH LEVEL SAMPlJESs'%, field':^amples that contain target compounds at
concentration levels that exceed twice the high calibration standard and/or
interferents that are :!i&|lected at levels greater than the mid level initial
calibration standard concentration response of the nearest target compound.
                                      G-4                               08/23/94

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                                                                           DRAFT

 IN-HOUSE - at the Contractor's facility.

 INITIAL CALIBRATION - Analysis of three analytical  standards at the beginning
 of the contract and whenever specific quality  control criteria are not met.
 Initial calibration defines the linear and  dynamic  range of response of the
 instrument to the target compounds.                  " .  •„

 INSTRUMENT BLANK - reagent water (for volatiles)  or solvent ;<;for PAH, phenols,
 pesticides, and PCBs) analyzed to determine whether carry-over iScom a previous
 sample has occurred.                           ;,                   -4-,"'>'
 LABORATORY -  synonymous with Contractor as ve|ed herein.

 LABORATORY CONTROL SAMPLE (LCS) - sample prepared  andrfOTtified (spiked) with
 known quantities of specific compounds anS stibj ecteds-ifco  the  entire analytical
 procedure by  the Contractor in order to assess*' tile .accuracy  of the method and
 to  demonstrate that the analytical system is in tsoratsjol  and  producing
 consistent data.                                   '  ;,l- ,
                                                        •i • .';/,
 MATRIX -  the  predominant materiaLjof .which the sample  to Be' Analyzed is
 composed.   For the purpose of this 30&,:;;i*%e;; sample matrix is either water,
 soil/solid, oil, or wipe.        "::* ',     '  •'• '':-,;,;j  ,:;- •-.-

 METHANOL  NON-MISCIBLE OIL SAMPLE - Oil sample:j|hat is  not miscible with
 methanol.   Used synonymously with metfoanpl eaitractable oil sample.

 METHANOL  MISCIBLE OIL SAMPLE - Oil sample' t&at is  miscible with methanol.
 Used  synonymously with met&apol jion-extractable oil sample.
METHOD BLANK -  an analytical conical consisting ;!of all reagents  and the SMC
carried  through the^ame analytic^, procedures =as the field samples.   The
method blank is usect to define t^s level of laboratory background
contamination.      •-;•%,.,      , ,--
PHOTO- IONIZATION DEf1^|,,pID)  -  detector used in series with electrolytic
conductivity detector '-''QEiCD  or HALL)  in the analysis for volatile organics.
The PID may also be used : for the analysis of phenols in this SOW.
                                      G-5                              08/23/94

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                                                                           DRAFT

PROTOCOL  - describes  the  exact procedures to be followed with  respect to
sample receipt and handling,  analytical methods, data reporting and
deliverables, and document  control.   Used synonymously with SOW.

QTM TARGET COMPOUND LIST  (QTCL) -  a list of compounds,.Designated by the SOW
(Exhibit  C) for analysis.                            '=: . ;

Quick Turnaround Method (QTM)  TRAFFIC REPORT/CHAIN-OF-CUSTOirry(m/COC)  - an
EPA sample identification form filled out by the sampler which acbompanies the
sample(s) during shipment to  the laboratory andwhich documents sample.
condition and receipt by  the  laboratory.     T '                         !

REAGENT WATER - water in  which a target compound or int«rferent does not
produce a signal greater  than one-half tht&icesponse intifNEhe corresponding RRT
window of the initial calibration low concecBtifation sjtsandard.

REGIONAL  PROGRAM MANAGER  -  Regional EPA official; -|w*cih as the  Regional
Technical Project Officer (TPO) or Regional Site Manage^,  Regional Site
Managers may be Site  Assessment Managers (NPL listings)-; 'fi»-Scene Coordinators
(emergency response(s)),  or RemedJLs%J,.;P.roject Manager (site *remediations).
                                 /.,',|BV4|fo/ ^jif'<,;••/,, , ,,,(
RECOVERY  - a determination  of the ;4^curacy" o%'-ffl^ '|aBaly,tical procedure  made by
comparing measured values of  a fortified (spikect) 'sample..against the known
spike values.  Recovery is  determinedly the Billowing equation:
                         %Rec = measured ^•yalue  x 100%
                                  known
                        '   - 'S1;  * ;-            -,
REANALYSIS  - reanalysis,-
         ™                   "
RESOLUTION  'C&Ltfar termed per^sht valley)  - the separation between peaks  on a
chromatogram, calbeaiilated by -Dividing the height of the valley between the
peaks by the peak h«iL^l^^ the smaller peak being resolved, multiplied by
100.                 ~ ".'"-V-
                                      G-6                               08/23/94

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                                                                          DRAFT

RETENTION  TIME MARKER -  standard compound (SMC)  used to assess GC system
stability  by quantifying shifts in retention time for all analyses.

SAMPLE  - a portion of material to be analyzed that is contained in single or
multiple containers and  identified by a unique sample number.

SAMPLE NUMBER (EPA Sample Number) - a unique identificatiab, number designated
by EPA for each  sample.   The EPA sample number appears on the  sample QTM
TR/COC form  which  documents information on that sample.       H-  J,

SOLID PHASE  EXTRACTION (SPE) - a procedure commonly utilizing  a cartridge or
disk containing  a  solid  matrix coated with amended organic phase used to
extract and  cleanup field and QC water samples.

SOLVENT EXTRACTION -  liquid- liquid and liquid-solid ea&raction procedures used
to prepare field and QC  samples.                 .  -1

STANDARD ANALYSIS  -  an analytical determination made sssith known quantities of
target compounds;  used to determine calibration factofs^'^eJEine identification
windows , and establish linearity $v@r, the calibration range»
SYSTEM MONITOR COMPOUND (SMC)  -  aSeampound aiMfed^to^every blank,  sample,
laboratory control  sample,  and standard;  used -to. evkluatje analytical
efficiency and stability by evaluatittg recover^ and retention time shift.
These compounds are  typically  brominafeed,  flxisrinated,  isotopically labelled,
or compounds not expected to be  detected ,ia • environmental media.
TECHNICAL PROJECT OFFICER; (t£H>|= _-  Regional ^fficial  responsible for monitoring
the technical requireipe»t:s of'1^^;Laboratory*^ contract;  the TPO is the first
line of contact when^^te  Laboratory requires ^echnical assistance,  and along
with the Administrative Project OJficer (APO),  is  the only person that can
provide instructions,"or clarifications  to  the  Laboratory  regarding the SOW.
                  •• \  ,»?•.         :;-%~&^>?''~: ''-.-} •"
TELEFACSIMILE (fax or'%yps)  -  a system  of  transmitting and reproducing fixed
graphic material (as printing;}  by  means of signals transmitted over telephone
lines.                       ' •; ,;

TIME - when.'.petjdfred^feo.i-.irecord time-jm  any deliverable item,  time shall be
expressedi&r Military  Tim|^  i.e.,  a 2'"4-hour clock.
        •ft
VALIDATJ<$ TIME OF SAMPLE RE^||PT  (VTSR)  -  the  date  and time on which a sample
is re&gifaed at the Contractolfes facility,  as recorded on the shipper's
delive^l^rsceipt and QTM TR/SOfC Record.  NOTE:  The  VTSR date/time is adjusted
for sanipSwitjgeceived during jjpeni-routine  working hours (see  Exhibit A,  Section
III, paragrlpiti^.S, for details).
                                      G-7                              08/23/94

-------
                                                                           DRAFT
                                   SECTION II

                           ABBREVIATIONS AND ACRONYMS
APO
CADRE
CBF
CCS
CF
CLP
CLASS
CRQL
%D
DCO
DF
ECD
EOT
ELCD
EMSL-LV
EPA
EST
FAX or FACS
FID
FSCC
GC
1C
LCS
NCC
NEIC
NPL
OSC
PAH
PCB
PE
PEST
PHE
PID
PRP       -ft
PVS     ;!J'
QA    ,f.""
OAP  ,;0'
QATS  :
QC
QTCL
QTM
RAS
%REC
RPM
RSCC
Administrative Project  Officer
Computer-Aide Data Review and Evaluatisto
Complete Batch File
Contract Compliance Screening
Calibration Factor
Contract Laboratory Program
CLP Analytical Services Support;
Contract Required Quantitationtllimit
Percent Difference           j-, *,*A
Document Control Officer      - '*<-t
Dilution Factor
Electron Capture Detector
Electronic Data Transfer
Electrolytic Conductivity Detector
Environmental Monitoring Systems Laboratory - las Vegas
Environmental
Eastern Standard Time'ie ,
Telefacsimile
Flame lonization Detector*'-! -
Fused Silica Capillary  Column
Gas Chromatograph           \  '
Initial Calibration
Laboratory
National Computer
National JSoforcement
Nationa2*3»riorities
On- Sce3BB'sCoordinator
Polynuclear Aromatic
Polychloriniifeecl,, Biphenyls
Performance Evaliuation
Pesticides      "^ '='11:
                         •estigatioa Center
            _    Detecto?- ^'
Potential Responsible Parties
              te "^ -*"1-.
Performance Vefep|Lcation Standard
Quality AssuraniSsh-
Quality Assurancef-^lan
Quality Assuranc||fechnical Support
•J^oality Control jjJ!
      Turnaroun^^Target Compound List
      J Twnaroiajdf5 Method
Routine i-3ftjastlyt|ical Services
Percent Rec&fefaery
Regional Project Manager
Regional Sample Control Center
                                      G-8
                                                            08/23/94

-------
                                                                          DRAFT

%RSD        Percent Relative  Standard Deviation

RT          Retention Time
RT ZD       Retention Time Percent Difference
RRT         Relative Retention Time                  ;
RTS         Retention Time Shift
SAS         Special Analytical Services
SD          Standard Deviation
SMC         System Monitor Compound                              v
SPE         Solid Phase Extraction
SOP         Standard Operating Procedure     >;!
SOW         Statement Of Work
TCL         Target Compound List          ,/
TPO         Technical Project Officer     ,1
TR/COC      Traffic Report/Chain-of-Custody?
VOA         Volatiles                         1.    f; -
VTSR        Validated Time of Sample Receipt     .  '\
                                     G-9                              08/23/94

-------
                EXB3BIT H, ; "

   DATA DICTIONARY ANB/fGBMAT FOR DATA
DELIVERABLES IN COMPUTER-READABLE FORMAT

-------
                                    SECTION I

                             FORMAT A SPECIFICATIONS

1.   DATE

            Dates  are to be YXMMDD format with  all  characters filled; no
            slashes,  dashes, or spaces.

            Example:   March 19, 1989 will be expressed as ^890319".

2.   TIME                                                          y:

            Times  are to be expressed in HHMK'rJBormat with all characters
            filled, no colon.               - !,

            Example:   1:30 pm will be expressed as  "UfO" .

3.   CHARACTER                                   -'-  ,  "

            Character data are to be left-justified-udeth all letters
            uppercase.

4.   NUMERIC                      =;','! -:', ^ i  ,,.
            Numeric data are to be%ight-justified wiS&out a positive sign
            (+),  leading zeros, commas, or exjabirients.  Right-justified,
            leading zeros not necessary, length  includes  decimal points and
            signs.   Negative signing (-}.;, -although unlikely, will decrease the
            range of values by one order -«£* magnitude.

            Example:   Iftimeric'!i6,v3*will accommodate from  -9.999 to 99.999.
                     -•,<:        '--t|:          '•  ,.
5.  SPECIAL CASES   ",            I';
                                  ;s«*'
                    ;            ^^f1-? .-•        ''"-I? -
         &•'"           J;t.
        >•%,  Form  numbers u*s^|--£hree characters, the first  character is a 'Q',
        11  the second char^i^er identifies the  form type (1= Form QI, 2- Form
     ,4>;"-e'   QII,  3= Form QIlt|| 4= Form QIV, 5= Form  QV,  6= Form QVI, and 7=
     ' ^-.-1(1 , Form  QVII) ,  and ^Ipfc third character  denotes  the fraction (A= VOA,
        ''&-•;jr&=, PAH,  C= Phenq^, D= Pesticides, E= Aroclors).
                              '
                                       H-2                              05/01/92

-------
Z6/TO/SO
                                  aiu mod

-------
                                                                         •MI*
                                 FORM QI  - VOA
                        VOLATILES ANALYSIS  DATA SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-19
20-44
45-55
56-61
62-66
67-74
75-76
77-82
83-92
93-104
105-109
110-113
114-118
119-126
127-136
137-142
143-146
147-152
153-156
157
158-167
168-174
175-177
178
179-187
188-193
194-199
200-204
205
LENGTH
3
2
2
12
25
11
6
5
8
2
6
10
12
5
4
5
8
10
6
4
6
4
1
10
7
3
1
9
6
6
5
1
 CONTENTS
 Form number
 Form suffix
 Record  type
 EPA sample no.
 Lab name
 Contract
 Lab code
 Case no.
 Batch no.
 Sequence no.
 SAS no.
 Matrix

 Lab sample ID
 Sample  wt/vol
 Sample  wt/vol units
 Units    > M
 D ilutionl Jact^r - •;;.
 Instrumen%-]ID
 Date received
 Time received;
 Date analyzed  -
 Time analyzed
 Quantitation type
 SMC '•pAS', no.
1 SMC cokeeatration
•SMC % redo^ery
 SMC % rec. pout flag
 SMC area--'|\ ,,	,	
•- SMC RT  _;'l^-i:'::>-;>:' ;l
! sac ic  RT
 RT';'-3SD:;
 SMC fti, ;%B, out flag
                                                  FORMAT/CONTENTS
                                                  "QL4"
                                                  "AA* - "ZZ"
                                                  "Hi*
                                                  ^Character
                                                  Character
                                                  Character
                                                  Character
                                                  Character            :
                                                  Character
                                                  Character
                                                  Character
                                                  "SOIL/SOLID",  "WATER",  or
                                                  sfifccified other
                                                  Character
                                                  Ntamexic 5.1
                                                  "G" , ^HL" , other
                                                  "UG/L" , '< "1S?/KG" ,  or  other
                                                  Numeric 8.0
                                                  flhaa^-acter
HHMM
YYMMDD
HHMM
Character  (1, 2,  or  3)
Character
Numeric 7 .
Numeric 3 .
"*" or blank
Numeric 9.0
Numeric 6.3  (minutes)
Numeric 6.3  (minutes)
Numeric 5 . 1
"*" or blank
                                                            . 3
                                                            . 0
                                      H-4
                     05/01/92

-------
DETAIL RECORD
            LENGTH
            3
            2
            2
            10   '
            13
            1
            8
            8
            6
            1
            6
            6
            1
            6
                           FORM QI - VGA (Continued)
                         VOLATILES ANALYSIS DATA SHEET
CONTENTS
Form number
Form suffix
Record type
CAS no.
Concentration
"U" flag (non-detects)
Qualifiers
Reserved for EPA use
RRT
RRT_flag
1C RRT (STDS)
RT                '  ;
RT flag
1C Rf (STDS)
 FORMAT/CONTENTS
 "QIA*
 "AA1? -  "ZZ"
          ^
'Numeric 13,, 3
 "U"  or blank
 Character
 Character
 Numeric 6 . 3
 "*"  0r blank
 Numeric 6 . 3
         6.3
     or blank
•fftaaaeric 6 . 3
                                     H-5
                                              05/01/92

-------
                                 FORM QI -  PAH
             POLYNUCLEAR AROMATIC HYDROCARBONS ANALYSIS DATA SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-19
20-44
45-55
56-61
62-66
67-74
75-76
77-82
83-92
93-104
105-109
110-113
114-118
119-126
127-136
137-142
143-146
147-152
153-156
157
158-164
165-174
175-181
182-184
185
186-194
195-200
201-206
207-211
212
LENGTH
3
2
2
12
25
11
6
5
8
2
6
10
12
5
4
5
8
10
6
4
6
4
1
7
10
7
3
1
9
6
6
5
1,,, <;•• ;
                        CONTENTS
                        Form number
                        Form suffix
                        Record type
                        EPA sample no .
                        Lab name
                        Contract
                        Lab code
                        Case no .
                        Batch no .
                        Sequence no.
                        SAS no.          - :';
                        Matrix            -',

                        Lab sample ID
                        Sample wt/vol
                        Sample wt/vol units
                        Units
                        Dilution^fs&tefT : „ ,
                        Instrument fo" "''' ' ^
                        Date received
                        Time received \
                        Date analyzed ; ,
                        Time analyzed
                        Quantitation type
                        I&txaction type
                            '
                        SMC concfjtration
                        SMC %
                        SMC %
                        .SMC
                        s»e RT
                        SHC&G Rf
                        RT xfr.K' ?; ,
                        SMC RT10B|»at flag
FORMAT/CONTENTS
"Q1B"
"AA* - "ZZ"
•at*   ,
Qaaracter
Character ,
Character
Character         ;
Character
Character
Chara«tser
Character
"SGlt/SOLID", "WATER", or
          other
Numeric 5.1
"G" , ' "^HL"., or other
"UG/L", "UG/KG", other
Ntimeric 8 . 0
HHMM
YYMMDD
HHMM
Character (1, 2, or 3)
"SOLVENT" or "SPE"
Character
Numeric 7.3
Numeric 3 . 0
"*" or blank
Numeric 9.0
Numeric 6.3 (minutes)
Numeric 6.3 (minutes)
Numeric 5.1
"*" or blank
                                      H-6
                     05/01/92

-------
                           FORM QI - PAH  (Continued)
             POLYNUCLEAR AROMATIC HYDROCARBONS ANALYSIS DATA  SHEET
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17

18-30
31
32-39
40-47
48-53
54
55-60
61-66
67
68-73
13
1
8
8
6
1
6
6
1
6
CONTENTS
Form number
Form suffix
Record type
CAS no.

Concentration
"U" flag (non-detects)
Qualifiers
Reserved for EPA use i
RRT                I
RRT_flag        ,  {
1C RRT (STDS)      ,  ;
RT                   '-•
RT flag
1C RT (STDS)
                                       FORMAT/CONTENTS
                                       "Q1B"
                                       "AA»  -  "ZZ"
 Gfearactet,  "COMBINEA" for
 coeluter '•   .;-
 Numeric 13. 3 : ::
 "U"  or blank   ••' ',,
 Character           »-
 Character
 Numeric 6.3
 "*",:«r blank
 Numsaric 6 . 3
 Nttmeric 6.3
.t*&  or blank
 Numeric 6.3
                                      H-7
                                                           05/01/92

-------
                                                                         DfeAlt
                                 FORM QI - PHE
                          PHENOLS ANALYSIS DATA SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-19
20-44
45-55
56-61
62-66
67-74
75-76
77-82
83-92
93-104
105-109
110-113
114-118
119-126
127-136
137-142 "
143-146
147-152
153-156
157
158-164
165-174
175-181
182-184
185
186-194
195-200
201-206
207-211
212
LENGTH
3
2
2
12
25
11
6
5
8
2
6
10
12
5
4
5
8
10
6
4
6
4
1
7
10
7
3
1
9
6
6
5
1 '- ~-i
CONTENTS
Form number
Form suffix
Record type
EPA sample no.
Lab name
Contract
Lab code
Case no.
Batch no.
Sequence no.
SAS no.
Matrix            ' ^

Lab sample ID
Sample wt/vol
Sample wt/vol units
                                                  FORMAT/CONTENTS
                                                  "QIC*
                                                  "Aft.* -  "ZZ"
                        Instrumeritfpp)     '
                        Date received
                        Time received
                        Date analyzed
                        Time analyzed
                        Quantitation type
                                   type
            ation
                          Character : ;
                          Character
                          Character    :  '••-*'
                          Character
                          Character
                          Character
                          Character
                          Character
                          "S0iL/SOLID", "WATER" , or
                          sfefecified other
                          Character
                          N«met3ic 5.1
                          "G"', '^Ht«, or other
                          "UG/L", '"US/KG", or other
                          Numeric 8.0
                          Character
                                    (1,
                                        2, or  3)
                                        SPE"
                       'l SMC conc
                        SMC 2
                        SMC
                       --.-SMC
SMC
                                      flag
HHMM
YYMMDD
HHMM
Character
"SOLVENT" or
Character
Numeric 7.3
Numeric 3.0
"*" or blank
Numeric 9.0
Numeric 6.3 (minutes)
Numeric 6.3 (minutes)
Numeric 5.1
"*" or blank
                                      H-8
                                              05/01/92

-------
                                                                          DfcAft
                           FORM QI - PHE (Continued)
                          PHENOLS ANALYSIS DATA SHEET
DETAIL RECORD
            13
            I
            8
            8
            6
            1
            6
            6
            1
            6
CONTENTS
Form number
Form suffix
Record type
CAS no.

Concentration
"U" flag (non-detects)
Qualifiers          .!?
Reserved for EPA use?-'
RRT              J' •
RRT_flag           ;
1C RRT (STDS)       !
RT                  '•:.
RT flag
1C Rf (STDS)
                                                   FORMAT/CONTENTS
                                                   "QlCf
                                                   "A&*: -  "ZZ"
           "COMBINED" and
"COMBINEE1 :,for coeluters
Numeric 13. 3 "  •"
"U" or blank       ;
Character          "
Character
Numeric 6.3
"*" asr blank
Numeric 6.3
liuffleric 6 . 3
*^* or blank
Numeric 6.3
                                      H-9
                                               05/01/92

-------
                                 FORM QI - PEST
                         PESTICIDES ANALYSIS DATA SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-19
20-44
45-55
56-61
62-66
67-74
75-76
77-82
83-92
93-104
105-109
110-113
114-118
119-126
127-136
137
138-143
144-147
148-153
154-157
158
159-165
166-175
176-182
183-185
186
187-195
196-201
202-207
208-212
213
LENGTH
3
2
2
12
25
11
6
5
8
2
6
10
12
5
4
5
8
10
1
6
4
6
4
1
7
10
7
3
1
9
6
6
5
i ;,r.
                         CONTENTS
                         Form number
                         Form suffix
                         Record type
                         EPA sample no.
                         Lab name
                         Contract
                         Lab code
                         Case no.
                         Batch no.
                         Sequence no.
                         SAS no.
                         Matrix
                         Lab sample ID
                         Sample wt/vol
                         Sample wt/vol units
                         Units
                         Dilution factor
                         Instrument .lib.,! .,_;'_ ;
                         Additional -cleanup
                         Date received
                         Time received
                         Date analyzed
                         Time analyzed
                         Quantitation type
                         BjctcaeStion type
                        "SMC CA'S,a|o.
                         SMC conceiStratipn
                         SMC % recs»irery
                         SMC y, reje,sbu|; flag,
                         SMC area^;"5<'-.lv - ••  -'•
                             RT
                             1C Rf
flag
            FORMAL/CONTENTS
            "Q1B*
            "A&* - "ZZ"
            "Hi'*'   ,:
            Character
            "Character5-   ;:
            Character       ;
            Character       :  :'
            Character            :
            Character
            Character
            Character
            "S0IL/SOLID" or  "WATER"
            Character
                    5.1
                   "ML"
                   :pr "UG/KG"
            Numeric 8,'D
            Character
           ". nn or "N"
                        RT
                        SMC
HHMM
YYMMDD
HHMM
Character  (1,  2,  or 3)
"SOLVENT"  or  "SPE"
Character
Numeric 7 . 3
Numeric 3.0
"*" or blank
Numeric 9 . 0
Numeric 6.3 (minutes)
Numeric 6.3 (minutes)
Numeric 5 . 1
"*" or blank
                                      H-10
                                 07/30/92

-------
                                                                          UNI-
                                QI - PEST (Continued)
                         PESTICIDES ANALYSIS DATA SHEET
DETAIL RECORD
            13
            1
            8
            8
            6
            1
            6
            6
            1
            6
CONTENTS
Form number
Form suffix
Record type
CAS no.

Concentration
"U" flag (non-detects^
Qualifiers           -'
Reserved for EPA use ';;
RRT                -:•/
RRT flag          '•";
1C RRT (STDS)      ;  >- ,
RT                     :
RT flag
1C RT (STDS)
 FORMAT/CONTENTS
 "QIC*
 11AA" - "ZZ"
 TEL*;,
 Character;, " COMBINES'
 eoeluters  .,->:
 Numeric 13.V'-;:j ,,
 "U" or blank    T
 Character
 Character
 Numeric 6.3
 "*"lor blank
 NuaJric 6.3
 Nuateric 6.3
.«*" or blank
 Numeric 6.3
                                                                         for
                                     H-ll
                                               05/01/92

-------
                                 FORM QI - PCB
                         AROCLORS  ANALYSIS DATA SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-19
20-44
45-55
56-61
62-66
67-74
75-76
77-82
83-92
93-104
105-109
110-113
114-118
119-126
127-136
137
138-143
144-147
148-153
154-157
158
159-165
166-175
176-182
183-185
186
187-195
196-201
202-207
208-212
213
LENGTH
3
2
2
12
25
11
6
5
8
2
6
10
12
5
4
5
8
10
1
6
4
6
4
1
7
10
7
3
1
9
6
6
5 r; LJ
-i *'~ '"*"'
DETAIL
COLUM^y
1-3 '"' Ijjh'i ; :
4-5 ""^
6-7
8-17
18-30
31
32-39
40-47
LEK
3
•<%
"l^''
10
13
1
8
8
                         CONTENTS
                         Form number
                         Form suffix
                         Record type
                         EPA sample no .
                         Lab name
                         Contract
                         Lab code
                         Case no.
                         Batch  no .
                         Sequence no.        i
                         SAS no.
                         Matrix          " -'4

                         Lab sample ID
                         Sample wt/vol
                         Sample wt/vol units
                         Units    ,, ,
                        Instrxunerift'-iLD
                        Additional --ipleanup
                        Date received^,
                        Time received ;a
                        Date analyzed
                        Time analyzed
                        ,/<3taast.||IEation type
                        'SExtratffeifp  type
                        SMC CAS iffe.
                        SMC concentration
                        SMC %
                        ;,SMC
                            area
                        RT %D   ' S
                        SMC RT  %DXout> flag
                              uffix
                                type
                         C&S, >no.
                        .^caicentration
                        :tfc" flag (non-detects)
                         Qualifiers
                         Reserved for  EPA use
FORMAT/CONTENTS
"Q1E*
"AA";-  "ZZ"
'Character  ;
Character   '• ' ',
Character         \
Character
Character
Character
Character
"S0IL/SOLID", "WATER",  or
specified other
Character
numeric 5.1
"G",^WML"( or other
"UG/L", "UG/KG",  or  other
Numeric 8 . 0
-Character
"Y* •&£ '"N"
YYMMDD
HHMM
YYMMDD
HHMM
Character (1, 2,  or  3)
"SOLVENT" or "SPE"
Character
Numeric 7 . 3
Numeric 3 . 0
"*" or blank
Numeric 9.0
Numeric 6 . 3 (minutes )
Numeric 6.3 (minutes)
Numeric 5 . 1
"*" or blank
FORMAT/CONTENTS
"Q1E"
"AA" -  "ZZ"
"Dl"
Character
Numeric 13.3
"U" or  blank
Character
Character
                                      H-12
                     07/30/92

-------
                                                                          itiit
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17
18
19-24
25
26-31
32-37
38
39-44
                           FORM QI - PCB (Continued)
                         AROCLORS ANALYSIS DATA  SHEET
CONTENTS
Form number
Form suffix
Record type
CAS no.
Peak
RRT
RRT flag
1C RRT (STDS)
RT
RT flag
1C RT (STDS)
FORMAT/CONTENTS
"QlEf
"M* - "ZZ"
"B2" ;  . ,
Character
Numeric 1.0;
Numeric 6.3   ,\-*
"*" or blank
Numeric 6.3
Numeric 6.3
"*" or blank
Numeric 6.3
                                     H-13
                                              05/01/92

-------
                                                                         •Ml*
HEADER RECORD
                                FORM QII - VGA
                VOLATILES LABORATORY CONTROL SAMPLE DATA SHEET
                                                  FORMAT/CONTENTS
                                                  "Q2A*
                                                  "AA*' - "ZZ"
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-114
115-120
121-124
125-134
135-141
142-144
145
146-154
155-160
161-166
167-171
172


LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
10
6
4
10
7
3
1
9
6
6
5
1

*,
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no.
Batch no . >
Sequence no. ;,
SAS no. <;'
Instrument ID /" ;
EPA sample no. ;J
Lab sample ID
Matrix
Date analyzed
Time analyzed
SMC CAS «»Jl : ,,••';-• n
SMC conce&feation" H;
SMC % recovery
SMC % rec out .flag
SMC area ' ,:
SMC RT ,
SMC 1C RT
,-KaT?t: ,,.
?!SMC*RT-1CI>,?out flag .•
V " f ; '"
st''.f', " "'
DETAIL RECORD ..* . ,'A>
COLUMN
1-3
4-5
6-7
8-17

18-26 /.
27-39 ,r<>
40-42 , "k~
43 , i }f
LENGTH ::|i =
3
2
2
lO;;;;;/;^

?$'
"13
3
1
^-Kt'-. ' '
j r^owTiPwn^f ^ ~~f''f^'' --^ •• -.''"'
K'-T
-------
                                FORM QII  - PAH
    POLYNUCLEAR AROMATIC  HYDROCARBONS LABORATORY CONTROL SAMPLE DATA SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-114
115-121
122-127
128-131
132-141
142-148
149-151
152
153-161
162-167
168-173
174-178
179
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
10
7
6
4
10
7
3
1
9
6
6
5
1
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17

18-26
27-39
40-42;
43   '"
            LENGTH
            3
            2
            2 -  •:
9
13
3
1
                         CONTENTS
                         Form number
                         Form suffix
                         Record type
                         Lab  name
                         Contract
                         Lab  code
                         Case no.
                         Batch no.
                         Sequence no.
                         SAS  no.            ;
                         Instrument ID
                         EPA  sample no.     :
                         Lab  sample ID
                         Matrix

                         Extraction type
                         Date analysed
                         Time anaij|pB$ ':-,4, v: 1
                         SMC  CAS n<£?  ""'"  ":
                         SMC  concentration
                         SMC  % recovery f
                         SMC  % rec out^lag
                         SMC  area
                         SMC  RT
                        , sac  ;ic |T
                         ftT %D -;A
                         SMC  RT Xfti.out flag
            Form-' &&££i'x.
            Record't^e
                no.
                             ,,^concentrat ion
                         Obser| concentration
                         % reisibvery
                         % rec|;out flag
FORMAT/CONTENTS
"Q2B*
»AA* -  "ZZ"
Character  .,
Character  "
Character
Character       ••
Character
Character
Character
Character
Character
Cilaracter
"SOIL/SOLID", "WATER", or
spJeeaLfied other
"SOLfBIT" or  "SPE"
YYMMDD    ;
HHMM
Character
Nomekic 7.3
Numeric 3.0
"*" or blank
Numeric 9.0
Numeric 6.3  (minutes)
Numeric 6.3  (minutes)
Numeric 5.1
"*" or blank
FORMAT/CONTENTS
"Q2B"
"AA"  -  "ZZ"
"Dl"
Character,  "COMBINEA"  for
coeluters
Numeric 9.3
Numeric 13.3
Numeric 3.0
"*" or  blank
                                      H-15
                     05/01/92

-------
                                FORM QII  - PEE
                 PHENOLS LABORATORY CONTROL SAMPLE DATA SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-114
115-121
122-127
128-131
132-141
142-148
149-151
152
153-161
162-167
168-173
174-178
179
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
10
7
6
4
10
7
3
1
9
6
6
5
1
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17
18-26 f.
27-39 ,y
40-42, •}'••
43 s'«^.-j
LENGTH
3
2
2 ,- ,;
rf°f!" :
V.%
13
3
L.' -^
                        CONTENTS
                        Form number
                        Form suffix
                        Record type
                        Lab name
                        Contract
                        Lab code
                        Case no .
                        Batch no.
                        Sequence no.
                        SAS no.
                        Instrument ID
                        EPA sample no .
                        Lab sample ID
                        Matrix

                        Extraction type
                        Date analyzed
                        Time analyze*!, j«  :,
                        SMC CAS ri©.-,  "'""  '"'
                        SMC concentration
                        SMC % recovery,
                        SMC % rec out ;€lag
                        SMC area
                        SMC RT
FORMAT/CONTENTS
                        -KT %D *'.. ...
                        SMC RT %Bsiout flag
                        Felpitiumber
                        Record
                        ?CAS no.
                             ^concentration
                             u concentration
                                   flag
"AA"; - "ZZ"
"ttL"
Character
"Character
Character   v   •>
Character       f~ •:
Character            :.;
Character
Character
Character
Character
Character
*^)IL/SOLID" ,  "WATER" ,  or
specified other
"SOttfEST" or  "SPE"
YYMMDD
HHMM
        7.3
Numeric 3 . 0
"*" or blank
Numeric 9.0
Numeric 6.3 (minutes)
Numeric 6.3 (minutes)
Numeric 5 . 1
"*" or blank
FORMAT/CONTENTS
"Q2C"
"AA"  -  "ZZ"
"Dl"
Character,  "COMBINED"  and
"COMBINER"  for coeluters
Numeric 9.3
Numeric 13.3
Numeric 3.0
"*" or  blank
                                     H-16
                     05/01/92

-------
                                                                          MBit
                                FORM QII - PEST
                PESTICIDES LABORATORY CONTROL SAMPLE DATA SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-114
115-121
122-127
128-131
132-141
142-148
149-151
152
153-161
162-167
168-173
174-178
179
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
10
7
6
4
10
7
3
1
9
6
6
5
1
DETAIL RECORD
18-26
27-39 ,,:
40-42;>:-
43   ~'<
            LENGTH
            3
            2
            O    ,"
9
13
3
                        CONTENTS
                        Form number
                        Form suffix
                        Record  type
                        Lab  name
                        Contract
                        Lab  code
                        Case no.
                        Batch no.
                        Sequence no.
                        SAS  no.
                        Instrument ID
                        EPA  sample no.
                        Lab  sample ID
                        Matrix

                        Extraction type
                        Date analyzed
                        Time ana|5«e^;, • \; ;
                        SMC  CAS noj;    '  ; u
                        SMC  concentration
                        SMC  % recovery
                        SMC  % rec out'J£Lag
                        SMC  area        ;
                        SMC  RT
                                                   FORMATCONTENTS
                        SMC RT 5£0,,;:out  flag

                                ,", % '4,
           • -GparrENTs
            Fo»i aaumber
            Form *a££ix
            Record trjspe s
                no.   "v-'
     •> concentrat ion
     t> concentration
% recovery
% reO'-out flag
                                                   "AA* - "ZZ"
                                                           _
                                                   Character
                                                   Character
                                                   Character
                                                   Character
                                                   Character
                                                   Character
                                                   Character
                                                   Character
                                                   Character
                                                   i^ OIL/SOLID" ,  "WATER", or
                                                             other
                                                             or "SPE"
                                                   YXMMDD :   r
                                                   HHMM
                                                   Numeteie 7.3
                                                   Numeric 3 . 0
                                                   "*" or blank
                                                   Numeric 9.0
                                                   Numeric 6 . 3 (minutes )
                                                   Numeric 6.3 (minutes)
                                                   Numeric 5.1
                                                   "*" or blank
                                                   FORMAT/CONTENTS
                                                   "Q2D"
                                                   "AA"  -  "ZZ"
                                                   "Dl"
                                                   Character,  "COMBINES" for
                                                   coeluters
                                                   Numeric 9.3
                                                   Numeric 13.3
                                                   Numeric 3.0
                                                   "*" or  blank
                                     H-17
                                                                       05/01/92

-------
                                                                          Wfft
                                 FORM QII -  PCB
                 AROCLORS LABORATORY CONTROL SAMPLE DATA SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-114
115-121
122-127
128-131
132-141
142-148
149-151
152
153-161
162-167
168-173
174-178
179
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
10
7
6
4
10
7
3
1
9
6
6
5
I
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17
18-26
27-39
40-42
43
                        CONTENTS
                        Form number
                        Form suffix
                        Record type
                        Lab name
                        Contract
                        Lab code
                        Case no.
                        Batch no .
                        Sequence no.
                        SAS no.
                        Instrument ID
                        EPA sample no.
                        Lab sample ID
                        Matrix
                        Extraction type
                        Date analyzed
                        Time analyzed
                        SMC CAS 4BCfc,',,;:; J / ,
                        SMC concesferation
                        SMC % recovSwey
                        SMC % rec out flag
                        SMC area
                        SMC RT
                        SMC 1C RT
                               , „
                            KT;fU;-out flag
                        CONTENTJS- ;•.-:' S;^ ,,-•':'" .': <"
                             number
                             suffix
                        RecorSSWtype
                        CAS not^Yl
                             concentration
                               concentration
 FORMAT/CONTENTS
                              out flag
 "A&*  -  "ZZ"
 "HI*
 Character
 Character     =,
 Character     -::  *,
 Character        >:
 Character          "•  • •
 Character
 Charauter
 Character
 Chaa-acter
, CMaracter
.-"^OIL/SOLID"  or "WATER"
 •^S&BfENT"  or  "SPE"
 YYMWffift   .
 HHMM     "
 Character
 '-fomeric 7.3
 'Ntmeric 3.0
 "*" or blank
 Numeric 9 . 0
 Numeric 6.3 (minutes)
 Numeric 6.3 (minutes)
 Numeric 5 . 1
 "*" or blank
 FORMAT/CONTENTS
 "Q2E"
 "AA" - "ZZ"
 "Dl"
 Character
 Numeric 9.3
 Numeric 13.3
 Numeric 3.0
 "*" or blank
                                     H-18
                      05/01/92

-------
                                FORM QIII - VGA
            VOIATILES PERFORMANCE VERIFICATION STANDARD DATA SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-110
111-114
115-124
125-131
132-134
135
136-144
145-150
151-156
157-161
162
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
6
4
10
7
3
1
• 9
6
6
5
1
                        CONTENTS
                        Form number
                        Form suffix
                        Record  type
                        Lab name
                        Contract
                        Lab code
                        Case no.
                        Batch no.
                        Sequence no.
                        SAS no.            ;
                        Instrument ID     ;,
                        EPA sample no.    0
                        Lab sample ID
                        Date analyzed
                        Time analyzed
                        SMC CAS no.
                        SMC concentration
                        SMC % re&4®&3^?. ~'<' T
                        SMC % ree:-Npit flag:
                        SMC area  "f
                        SMC RT __    :
                        SMC 1C Rf
                        RT ZD
                        SMC RT %D out flag
                                        FORMAT/CONTENTS
                                  "ZZ"
                                        "AA*
                                        tJKaractrer
                                        Character :
                                        Character
                                        Character
                                        Character
                                        Character
                                        Character
                                        Chacacter
                                        CbaBteacter
                                        Character
                                        Character
                                        Numeric 7 .'3
                                        Numeric 3.0
                                               blank
                                                9.0
                                        Numeric 6.3 (minutes)
                                        Numeric 6.3 (minutes)
                                        Numeric 5.1
                                        "*"  or blank
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17
LENGTH ,r"?
3
2 "•: ;:
2
10
CONTENTS P -|:
Form number
..Form suffeb£:
• -;|8.«c.ord type
CAS no .
18-26
27-39
40-42
43
44-49
50   f.
 9,.
-••&
•'''3
 1
 6
 1
True cora(3«n|:ration
X'%e^s out flag
Res6$yt % valley
ResoljlL % valley out flag   "*"  or blank
FORMAT/CONTENTS
"Q3A"
"AA" - "ZZ"
"Dl"
Character, "COMBINEC" for
coeluter
Numeric 9.3
Numeric 13.3
Numeric 3.0
"*" or blank
Numeric 6.2
                                     H-19
                                                            05/01/92

-------
                                                                          IMft

                                FORM QIII -  PAH
FOLYNOCLEAR AROMATIC HYDROCARBONS  PERFORMANCE VERIFICATION STANDARD DATA SHEET
HEADER RECORD
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
6
4
10
7
3
1
9
6
6
5
1
                         CONTENTS
                         Form number
                         Form suffix
                         Record type
                         Lab name
                         Contract
                         Lab code
                         Case no.
                         Batch no.
                         Sequence no.
                         SAS no.
                         Instrument ID    ;,
                         EPA sample no.
                         Lab sample ID
                         Date analyzed
                         Time analyzed
                         SMC CAS no.
                         SMC concentration
                         SMC % ree«*(r«%>-7;. •
                         SMC % rec'laut fla|
                         SMC area
                         SMC RT  _   •;:,
                         SMC 1C RT    !;
                         RT %D
                         SMC RT %D out flag
 FORMAT/CONTENTS
 "Q3&*
 H A &£t" _ « 7 7 *t

 Character
 Character\_ s  ,
 Character    ;v
 Character
 Character
 Character
 Character
 Character
 Character
 Character
 ItXMMDD
 Charsfeter
 Numeric 7.3
 Numeric 3.0
•t*Z< or blank
•Nuaesdfc 9.0
 Numeric 6.3 (minutes)
 Numeric 6.3 (minutes)
 Numeric 5.1
 "*"  or blank
DETAIL RECORD
                         CONTENTS'.
                         Form
                         Form
                       .Mtecord type
                        True
                               coneesifcration
                            covery
                              out flag
                               % valley
                        Reso^j- % valley  out
 FORMAT/CONTENTS
 "Q3Bn
 "AA"  - "ZZ"
 "Dl"
 Character,  "COMBINEA" for
 coeluters
 Numeric 9.3
 Numeric 13.3
 Numeric 3.0
 "*"  or blank
 Numeric 6.2
 "*"  or blank
                                      H-20
                     05/01/92

-------
                                FORM QIII  - PHE
             PHENOLS  PERFORMANCE VERIFICATION STANDARD DATA SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-110
111-114
115-124
125-131
132-134
135
136-144
145-150
151-156
157-161
162
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
6
4
10
7
3
1
9
6
6
5
1
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17
18-26
27-39
40-42
43 :.i
44-49 ,;;| ;
50 *ff.
LENGTH
3 ':
2
2
10
9 x .. -s •
,:Ui3H" •'•
sV'3
= " 1
6
1
                         CONTENTS
                         Form number
                         Form suffix
                         Record type
                         Lab  name
                         Contract
                         Lab  code
                         Case no.
                         Batch no.
                         Sequence no.
                         SAS  no.
                         Instrument ID
                         EPA  sample no.
                         Lab  sample ID
                         Date analyzed
                         Time analyzed
                         SMC  CAS no.
                         SMC  concentration
                         SMC  % recsjwwcyj^". f;:
                         SMC  % rec'%«sut flag"1
                         SMC  area
                         SMC  RT __
                         SMC  1C RT     -J
                         RT %D
                         SMC  RT %D  out flag
                        CONTENTS;;':
                        Form nuni&fer^ m, ^
                        Form sy£@&; V'^,;';'' '/'
                        '^Record  type
                        CAS BO.

                        True co'iicjeaatxation
                        .flbser.  coiibeiieration
Rese
                           FORMAT/CONTENTS
                           "QSC"
                           "A&*  -  "ZZ"
                          •Qhara'ctei: .
                           Character
                           Character
                           Character
                           Character
                           Character
                           Character
                           Character
                           Character
                          .CJB&racter
                              out  flag
                               % valley
                               % valley  out
                           Character
                           Numeric 7/3
                           Numeric 3 . 0
                           "*"!;. or blank
                           Numeric 9.0
                           Numeric 6.3 (minutes)
                           Numeric 6.3 (minutes)
                           Numeric 5 . 1
                           "*" or blank
FORMAT/CONTENTS
"Q3C"
"AA" - "ZZ"
"Dl"
Character, "COMBINED"  and
"COMBINEE" for coeluters
Numeric 9.3
Numeric 13.3
Numeric 3.0
"*" or blank
Numeric 6.2
"*" or blank
                                     H-21
                                               05/01/92

-------
                                                                         •Mtt
            PESTICIDES
         FORM QIII - PEST
PERFORMANCE VERIFICATION STANDARD DATA SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-110
111-114
115-124
125-131
132-134
135
136-144
145-150
151-156
157-161
162
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
6
4
10
7
3
1
9
6
6
5
1
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17
18-26
27-39
40-42
43
44-49
50 ?;, •
~:^l
r s--. . %
LENGTH
3
2
2
10
9
13-*; ^q,
/•'B - • : " '"""
'" ^^\
;•;•' 6
1

 CONTENTS
 Form number
 Form suffix
 Record type
 Lab  name
 Contract
 Lab  code
 Case no.
 Batch no.
 Sequence no.
 SAS  no.
 Instrument ID     :
 EPA  sample no .
 Lab  sample ID
 Date analyzed
 Time analyzed
 SMC  CAS no.
 SMC  concentration
 SMC  %
 SMC  %
 SMC  area
 SMC  RT __   '  •< ;
 SMC  1C RT     V
 RT %D         '
 SMC  RT %D out flag,
                        CONTENTS • .
                        Form numf»e|r .
                       -JForm sv^fii,
                       %-eeprd type
                           '
                                      _
                                      flag"
                        True '-eseaeentration
                        Obser. cdlipentration
                                  '    '
                                                  FORMAT/CONTENTS
                                                  "Q3D"
                                                  "AA* - "ZZ"
                                                  "Hi*-;  .
                                                  Character
                                                  Character
                                                  Character
                                                  Character
                                                  Character
                                                  Character
                                                  Character
                                                  Character
                                                  Character
                                                  Character
                              out flag
                             , % valley
Chariaceer
Numeric 7.'3
Numeric 3.0
*P" ^ors blank
Ntimerib 9.0
Numeric 6.3 (minutes)
Numeric 6.3 (minutes)
Numeric 5.1
"*" or blank
                            FORMAT/CONTENTS
                            "Q3D"
                            "AA"  -  "ZZ"
                            "Dl"
                            Character
                            Numeric 9.3
                            Numeric 13.3
                            Numeric 3.0
                            "*" or  blank
                            Numeric 6.2
                        ResSfLv % valley out flag  "*" or blank
                                     H-22
                                                05/01/92

-------
                                FORM QIII  -  PCB
             AROCLORS PERFORMANCE VERIFICATION STANDARD DATA SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-110
111-114
115-124
125-131
132-134
135
136-144
145-150
151-156
157-161
162
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
6
4
10
7
3
1.
9
6
6
5
1
DETAIL RECORD
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no.
Batch no.
Sequence no.
SAS no.
Instrument ID
EPA sample no.
Lab sample ID
Date analyzed
Time analyzed
SMC CAS no.
SMC concentration
SMC %
SMC % rec
SMC area  "4:~-.
SMC RT  _   '•:•;.,
SMC 1C RT     .- =
RT %D
SMC RT %D out flag"
J -f,s   f*-t '!* -.. -
•iswt flag -
COLUMN
1-3
4-5
6-7
8-17
18-26
27-39
40-42
43
44-49 f ~
50 ;-'£
< .A'i
LENGTH
3 f
2
2
10
9
13- .> -'jt
//3i; ••" •'"'•
n:i
6
1
,'J:: CONTENTS :,i-l
:•""'. Form nunfoir.
'-;;;'f ^ ..Form su£xi^^^ *''\ ^ t '% .
•Sfefeord type
CAS >;»0s.
True: «^«a^entration
% 'j Obser . c?&$i€&&x3,tration
'" :t:-< ^.recovery' --i-g; '
'%;->irec out flag
Reioi. % valley
Resell % valley out
                                                   FORMAT/CONTENTS
                                                   "Q3R"
                                                   "&&?• - "ZZ"
                                                   Cjharact:er ,
                                                   Character   f
                                                   Character
                                                   Character          ;;
                                                   Character
                                                   Character
                                                   Character
                                                   Character
                                                   Character
                                                   .GSaracter
                                                   YSMMDD
                                                   mass.
                                                   Character
                                                   Numeric 7,3
                                                   Numeric 3 . 0
                                                   •f*5 &X blank
                                                   Wumeuic 9.0
                                                   Numeric 6.3 (minutes)
                                                   Numeric 6.3 (minutes)
                                                   Numeric 5.1
                                                   "*" or blank
                                                   FORMAT/CONTENTS
                                                   "Q3E"
                                                   "AA"  -  "ZZ"
                                                   "Dl"
                                                   Character
                                                   Numeric 9.3
                                                   Numeric 13.3
                                                   Numeric 3.0
                                                   "*" or  blank
                                                   Numeric 6.2
                                                   "*" or  blank
                                      H-23
                                              05/01/92

-------
                                FOKM QIV  - VGA.
                      VOIATILES INITIAL CALIBRATION SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-110
111-114
115-123
124-135
136-147
148-153
154-157
158-166
167-178
179-190
191-196
197-200
201-209
DETAIL
COLUMN
1-3
4-5
6-7
8-17
18-25
26-33
34-41
42-49
50-54 ,
55 «£
56-61't?
62
63-68
69-74
75-80
81-86
87-92
93-98
99-104
105-110
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
6
4
9
12
12
6
4
9
12
12
6
4
9
RECORD
LENGTH
3
2
2
10
s ;s> ?;
i.$J i;; ' '• •"
•^i£
•',' ?' 8
,.,-,<: ' 5
<-' 1
:- $., 6
;1||X'..i
'''- 1|6>|,'8!,
6 ~ -i>^ * ,
6 X~'V,
6
6
6
6
6
                        CONTENTS
                        Form number
                        Form suffix
                        Record type
                        Lab name
                        Contract
                        Lab code
                        Case no.
                        Batch no.
                        Sequence no.
                        SAS no.             :
                        Instrument ID       ;:;
                        CAL #1 EPA sample ago,,
                        CAL #1 lab sample IB
                        CAL #1 date
                        CAL #1 time
                        CAL #1 standard cone.
                        CAL #2 EPA sample no.
                        CAL #2 lab, sample ID
                        CAL #2
                        CAL #2
                        CAL #2 sta&lard cone.
                        CAL #3 EPA sample no.
                        CAL #3 lab sample IDj
                        CAL #3 date     .   .,'..;
                        CAL #3 time     :v, .'•
                        CAL-||t3 .standard cone.
                        CONTENTSj"V
                        Form numfcei;
                        Form su^E^st/
                        leeord type
                        Low
                        Resoff  % valley
                        ResqJ;;;  % valley out  flag
                        RT
•ritQf Mean
llRT Low
 RRT Mid
 RRT High
 RRT Mean
FORMAT/CONTENTS
"Q4A*
"A&",,- "ZZ"
^Character
Character
Character
Character
Character
Character
Character
Character
Character
Numeric 9.0
Character
Character
YYMMDD
fKaaedcJ-c 9.0
Character
Character
YYMMDD
HHMM
Numeric 9.0
FORMAT/CONTENTS
"Q4A"
"AA" - "ZZ"
"Dl"
Character
coeluter
Numeric 8.0
Numeric 8 . 0
Numeric 8 . 0
Numeric 8 . 0
Numeric 5 . 1
"*" or blank
Numeric 6 . 2
"*" or blank
Numeric 6 . 3
Numeric 6.3
Numeric 6 . 3
Numeric 6 . 3
Numeric 6 . 3
                                                              "COMBINEC" for
                                                  Numeric 6 . 3
                                                  Numeric 6 . 3
                                                  Numeric 6 . 3
                                     H-24
                     05/01/92

-------
                                FORM QIV  - PAH
          POLYNUCLEAR AROMATIC HYDROCARBONS INITIAL CALIBRATION SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-110
111-114
115-123
124-135
136-147
148-153
154-157
158-166
167-178
179-190
191-196
197-200
201-209
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
6
4
9
12.
12
6
4
9
12
12
6
4
9
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17
26-33
34-41
42-49
50-54
55
56-6K ' ,
62 ' "< ;-
63-68
69-74
75-80
81-86
87-92
93-98
99-104
105-110
LENGTH r'T
3 /" ';•
2 !
2
10
8^ , '
, < , , ;
>• 8
5
1
6
,?:,1
• 16:-
6'V-- ,
6 ' ' * :
6 :-;-
6
6
6
6
                        CONTENTS
                        Form number
                        Form suffix
                        Record type
                        Lab name
                        Contract
                        Lab code
                        Case no.
                        Batch no.
                        Sequence no.
                        SAS no.
                        Instrument ID
                        CAL #1 EPA sample ,no.
                        CAL #1 lab sample W ~
                        CAL #1 date          =
                        CAL #1 time
 FORMAT/CONTENTS
 "Q4B*
 "AA*. -  "ZZ"
 "SI*
 Character
- Character,
 Character
 Character      :
 Character
 Character
 Character
 Character
 Character
 Chracter
CAL #1 standard cone.
CAL #2 EPA sample no.
CAL #2 lab,, sample ID
CAL #2 date" ';/ -
CAL #2 ti»e "°~ -'- ,< o -,-i-;'
CAL #2 standard cone. ' !'
CAL #3 EPA staple no.-!
CAL #3 lab saigple ID; '
CAL #3 date -\.
CAL #3 time
CAL ;#3 standard c«nc.
CONTENTS ' ;
Form Tn intf%j&y , , , „ , ,
•Form sUiiSs; s ~i~ •-, •, . ~
^RBDord type
CAS -Sao,.

LOW :, ;;
; Hid 
-------
                                FORM QIV  - PHE
                       PHENOLS INITIAL CALIBRATION SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-110
111-114
115-123
124-135
136-147
148-153
154-157
158-166
167-178
179-190
191-196
197-200
201-209
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
6
4
9
12
12
6
4
9
12
12
6
4
9
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17
18-25
26-33
34-41 -7
42-49 .-••• '*"
50-54 ^V
55 .<••§:••
5 6 - 6 1- 1|^ ''.?, r
/TO '**-* V$
\jt. ••> «-•
63-68
69-74
75-80
81-86
87-92
93-98
99-104
105-110
LENGTH
3
2
2
10
8-. S",
o *- >• < -^> **>';
*$, - -
: v-8
8
5
1
6
~!A
•sjjji ?
Vlk-
6 "4
6
6
6
6
6
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no.
Batch no.
Sequence no.         ;,
SAS no.
Instrument ID     •,
CAL #1 EPA sample'$ao,
CAL #1 lab sample"IDS
CAL #1 date
CAL #1 time
CAL #1 standard cone.
CAL #2 EPA sample no.
CAL #2 lab sample ID
CAL #2
CAL #2
CAL #2 staa&ard cone. /
CAL #3 EPA sample no. r
CAL #3 lab sample ID-/
CAL #3 date   -:'   '; ;
CAL #3 time     ,   =
CAL #3 standard cone.
                        CONTENTS .
                        Form
                       -: Form
                       '•"Bsecprd type
                        Low
                       'Hid
                                                  FORMAT/CONTENTS
                                                  "Q4CT?
                                                  "AAV-  "ZZ"
                                                  "HI*  ,,
                                                  Character
                                                  Sharacter ."
                                                  Character  •  .
                                                  Character
                                                  Character
                                                  Character
                                                  Character
                                                  Character
                                                  Character
                                                  Character
                                                          9.0
                                                  Chara^tser
                                                  Character
                                                  YYMMDD
                                                          9 . 0
                                                  Character
                                                  Character
                                                  YYMMDD
                                                  HHMM
                                                  Numeric 9 . 0
                          FORMAT/CONTENTS
                          "Q4C"
                          "AA" -  "ZZ"
                          "Dl"
                          Character, "COMBINED"  and
                          "COMBINEE" for coeluters
                          Numeric 8.0
                          Numeric 8.0
                                    0
                                    0
                        % RSl%flag
                        Reso|L»; % valley
                        RescjJLy % valley out flag
                           Mean
                         RT Low
                        RRT Mid
                        RRT High
                        RRT Mean
Numeric 8.
Numeric 8.
Numeric 5.1
"*" or blank
Numeric 6.2
"*" or blank
Numeric 6.3
Numeric 6.3
Numeric 6.3
Numeric 6.3
Numeric 6.3
Numeric 6.3
Numeric 6.3
Numeric 6.3
                                     H-26
                                               05/01/92

-------
                                FORM QIV  - PEST
                      PESTICIDES INITIAL CALIBRATION SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-110
111-114
115-123
124-135
136-147
148-153
154-157
158-166
167-178
179-190
191-196
197-200
201-209
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
6
4
9
12
12
6
4
9
12
12
6
4
9
                         CONTENTS
                         Form number
                         Form suffix
                         Record type
                         Lab  name
                         Contract
                         Lab  code
                         Case no.
                         Batch  no.
                         Sequence no.         ;
                         SAS  no.
                         Instrument ID
                         CAL  #1 EPA sample IM>,
                         CAL  #1 lab sample f$
                         CAL  #1 date
                         CAL  #1 time
                         CAL  #1 standard cone.
                         CAL  #2 EPA sample no.
                         CAL  #2 lab -sample ID
date;!:.
                        CAL #2
                        CAL #2
                        CAL #2  standard cone.
                        CAL #3  EPA Jlaaple no.
                        CAL #3  lab sample ID
                        CAL #3  date    n
                        CAL #3  time        ,'.!':
                        CAL- #3, standard coac.
FORMAT/CONTENTS
"Q4D*
"AA».  -  "ZZ"
"HI"
Character
Character
Character  -  • t.
Character
Character
Character
Character
Character
Character
Character
YSfflMDD
HHMM
Numeric 9.0
Character
Character
YYMMDD
HHMM
Numeric 9.0
Character
Character
YYMMDD
HHMM
Numeric 9.0
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17

18-25
34-41
42-49 ,r
50-54 .'V

55 ,;..;-"
56-611*-! '«,
62 :
63-68
69-74
75-80
81-86
87-92
93-98
99-104
105-110
LENGTH.
3
2
2
10

8- : ;.'
8'!, ;!' • .1!
.," ''
• v 4^0
f 8
5

1
6
;CJ-1
'"••;,€ -,;'
6"'';--.fo ' ,
6 "' /•
6
6
6
6
6
•';r CONTENTS I8
Form nuisi3NE$3r - ? ^ • *
-< -, 4fFprm suffiM.'li',::/^-: >; ,-,
' "Rsfeeord type
CAS no.
' " ";\:
°- - LOW """ ,"; *:
, A* • J v ^ v: -..
•*-!„ ,;Hld •!; *>
:*|JB»

% R>|>
"s "
% R£%.fcflag
Resol i % valley
Resci-1 % valley out flag
RT Low
RT'?!Cid
'•.. RflHigh
: -D ,«P Mean
'l %8RT Low
RRT Mid
RRT High
RRT Mean
FORMAT/CONTENTS
"Q4D"
"AA" - "ZZ"
"Dl"
Character, "COMBINES"
for coeluter
Numeric 8.0
Numeric 8.0
Numeric 8.0
Numeric 8 . 0
Numeric 5 . 1

"*" or blank
Numeric 6 . 2
"*" or blank
Numeric 6.3
Numeric 6.3
Numeric 6 . 3
Numeric 6 . 3
Numeric 6.3
Numeric 6 . 3
Numeric 6.3
Numeric 6 . 3
                                     H-27
                    05/01/92

-------
                                                                         IMP*
                                FORM QIV  - PCB
                      AROCLORS INITIAL CALIBRATION SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-86
87-92
93-98
99-104
LENGTH
3
2
2
25
11
6
5
8
2
6
10
6
6
6
6
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no.
Batch no.
Sequence no.
SAS no.
Instrument ID
RT Low
RT Mid
RT High
RT Mean
FORMAT/CONTENTS
"AA", - "ZZ"
"HI*
Character
Character
Character
Character
Character
Character
Character
Character
Numeric 6.3
Nuiferic 6.3
Numeric 6.3
        6 . 3
HEADER RECORD
COLUMN
1-3
U-5
6-7
8-19
20-31
32-37
38-41
42-50
51-62
63-74
75-80
81-84
85-93
94-105
106-117
118-123
124-127
128-136
137-148
149-160 /
161-166 i
167-17DV
171- It9;r
LENGTH
3
2
2
12
12
6
4
9
12
12
6
4
9
12
12
6
4 ,; •;;..
;?9 ;';' ^::-
'i!2
1 ; "' 12
6
4
9
            CONTENTS If,
            Form number
            Form suffix
            Record type
            CAL #1 EPA ss
            CAL #1 lab sample
            CAL #1 date
            CAL-$!„ time      ;   ;
            CAL $1. standard conc»
            CAL #2"^jjjk sample noi
            CAL #2 ifb -sample ID
            CAL #2 dlbe
            CAL #2 tifite,
            CAL #
            Cfii, #3 EPA sample no.
            CAT, $3 lab sample ID
            CAL $
            CAL #
                #3 staijdakd cone.
                 lene EPA sample no.
            toxaphene lab sample ID
            toxa|>hene date
            toxapMene time
            toxaphene standard cone.
                                                  FORMAT/CONTENTS
                                                  "Q4E"
                                                  *JBt«> "ZZ"
                                                  MH2"
                                                  Character
                                                  Character
                                                  YYMMDD
                                                  HHMM
                                                  Numeric 9.0
                                                  Character
                                                  Character
                                                  YYMMDD
                                                  HHMM
                                                  Numeric 9.0
                                                  Character
                                                  Character
                                                  YYMMDD
                                                  HHMM
                                                  Numeric 9.0
                                                  Character
                                                  Character
                                                  YYMMDD
                                                  HHMM
                                                  Numeric 9.0
                                     H-28
                                                          05/01/92

-------
                          FORM QIV -  PCB (Continued)
                      AROCLORS INITIAL CALIBRATION SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-19
20-31
32-37
38-41
42-50
51-62
63-74
75-80
81-84
85-93
94-105
106-117
118-123
124-127
128-136
137-148
149-160
161-166
167-170
171-179
180-191
192-203
204-209
210-213
214-222
LENGTH
3
2
2
12
12
6
4
9
12
12
6
4
9
12
12
6
4
9
12
12
6
4
9
12
12
6
4
9
DETAIL RECORD '"
COLUMN
1-3
4-5
6-7
8-17
18
19-26
27-34
35-42 ,i.
43-50 I-/'
51-55^ ';
56
57-62
63-68
LENGTH '" ;,
3
2
2
10s !: -?'•;
, ill'1'-''' ' """ :"
> /.-&B"
^ 8
8
8
4-, 5
"|;" JL
•4f5- 1
6-CV , /
                        CONTENTS
                        Form number
                        Form suffix
                        Record type
                        1221 EPA sample no.
                        1221 lab sample ID
                        1221 date
                        1221 time
                        1221 standard  cone.
                        1232 lab sample no.
                        1232 lab sample ID
                        1232 date
                        1232 time        :
                        1232 standard  concr.
                        1242 EPA sample no.
                        1242 lab sample ID
                        1242 date
                        1242 time
                        1242 standard  cone.
                        1248 EPA.i sample no.
                        1248 lab Sample'IS
                        1248 date'  ;
                        1248 time
                        1248 standardseonc.
                        1254 EPA sample-no.
                        1254 lab sample ID".;
                        1254-.-date         •<
                        ,'1254 dtitae         ' '••.
                        1254 stasjpard  cone.
                             number
                            s' suffix
                        CAS no. •'..
 FORMAT/CONTENTS
 "Q4E"
 "AA"  -  "ZZ"
 "S3"
 Character
•Character -
 YYMMDD
 HHMM          '"  .
 Numeric 9.0
 Character
 Character
 YYMMBB
 HHMH ,
 Numeric 9.0
 Character
 Character
                        LofelllRT
Numeric  9.
Character
Character
HHMM
Numeric  9.0
Character
Character
YXMMDD
HHMM
Numeric  9.0
FORMAT/CONTENTS
"Q4E"
"AA"  -  "ZZ"
"Dl"
Character
Numeric  1.0
Numeric  8.0
Numeric  8.0
Numeric  8.0
Numeric  8.0
Numeric  5.1
"*" or blank
Numeric  6.3
Numeric  6.3
                                     H-29
                     05/01/92

-------
                                                                           MM*
                                  FORM QV - VGA
                       VOLATILES  CALIBRATION CHECK SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-113
114-119
120-123
124-133
134-142
143-148
149-154
155-159
160
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
9
6
4
10
9
6
6
5
1
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17
18-25
26-33
34-38
39
40-45
46
LENGTH
3
2
2
10
8
8
5
1 -;
$M ;'"
• "~ JL








.'•-,.. ...

                         CONTENTS
                         Form number
                         Form suffix
                         Record type
                         Lab name
                         Contract
                         Lab code
                         Case no.
                         Batch no.             '
                         Sequence no.
                         SAS no.            -';:
                         Instrument ID    ,  ;,
                         EPA sample no.     ;,—  ,
                         Lab sample ID
                         Standard concentration
                         Date analyzed
                         Time analyzed
                         SMC CAS no,;<
                         SMC areaA-J ,• A.  '
                         SMC RT  '«;,._"""  •*! -~hj'
                         SMC 1C Rf  •'          ,i
                         RT %D      " :'.-,      ,:j
                         SMC RT %V out'yElag , i'-
                         Form
                         Form sufflas
                         Record t^e
                             no ^i|-; ,&j
                                 CF
                                 v..
                           D out "Sag
                                % vallky
                                % valley  out  flag
 FORM&t/CONTENTS
 "Q54!"'
 "AA*; - "ZZ"
 "11*;  ,-
 Character
 Character  ,;•  .
 Character     ]•]
 Character
 Character
 Character
 Character
 Character
 Character
 .GiSaaracter
         9.0
 Character «
 Numeric 9.0
* .Hosier ic 6.3  (minutes)
"^Numeric 6.3  (minutes)
 Numeric 5.1
 "*" or blank
 FORMAT/CONTENTS
 "Q5A"
 "AA" - "ZZ"
 "Dl"
 Character
 Numeric 8.0
 Numeric 8.0
 Numeric 5.1
 "*" or blank
 Numeric 6.2
 "*" or blank
                                      H-30
                      05/01/92

-------
                                 FORM QV  - PAH
           POLYNUCLEAR AROMATIC HYDROCARBONS CALIBRATION CHECK SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-113
114-119
120-123
124-133
134-142
143-148
149-154
155-159
160
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
9
6
4
10
9
6
" 6
5
1
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17

18-25
26-33
34-38
39
40-45
46
LENGTH
3
2
2
10

8
8
5,;  •  ;.
                         CONTENTS
                         Form number
                         Form suffix
                         Record type
                         Lab name
                         Contract
                         Lab code
                         Case no.
                         Batch no.            .  :
                         Sequence no.
                         SAS no.           .  :
                         Instrument ID    y
                         EPA sample no.    - 'f.
                         Lab sample ID       '  |;
                         Standard concentration
                         Date analyzed
                         Time analyzed
                         SMC CAS  no..:
                         SMC area-"  -"' '*• •-.? v
                         SMC RT  ^ •   '  '' ::  &••#
                         SMC 1C RT   f           ,{
                         RT %D
                         SMC RT %D  out
fs" Form number
:  Form suffix
  Record
^ CAS  no*

  iUifcba  el-
  Mid' '• s V,,
  % D     =; ,. ;£;
5; % D  out  flasgli-
       .. % valley
                     FORMAT/CONTENTS
                     "Q5B"
                     Character ,
                     Character
                     Character
                     Character
                     Character
                     Character
                     Character
                     Character
                     Character
                     Character
                     Htuneric 9.0
                     HHMM
                     Character
                     Numeric 9.0
                             6.3 (minutes)
                             6.3 (minutes)
                     Numeric 5.1
                     "*" or blank
                     FORMAT/CONTENTS
                     "Q5B"
                     "AA" - "ZZ"
                     "Dl"
                     Character, "COMBINEA" for
                     coeluter
                     Numeric 8.0
                     Numeric 8.0
                     Numeric 5.1
                     "*" or blank
                     Numeric 6.2
.  %  valley out flag  "*" or blank
                                     H-31
                                         05/01/92

-------
                                 FORM QV -  PHE
                        PHENOLS CALIBRATION CHECK SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-113
114-119
120-123
124-133
134-142
143-148
149-154
155-159
160
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
9
6
4
10
9
6
6
5
1
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17
18-25
26-33
34-38
39
40-45
46
LENGTH
3
2
2
10
8
8
c
PL': {-I.'-"*
v '™S>'
' V=" '" 1
                         CONTENTS
                         Form number
                         Form suffix
                         Record type
                         Lab name
                         Contract
                         Lab code
                         Case no.              ^
                         Batch no.             ;•*•
                         Sequence no.       <  ,.,;'
                         SAS no.            .°|
                         Instrument ID    . ;
                         EPA sample no.     'I  ;,,;
                         Lab sample ID         :
                         Standard concentration
                         Date analyzed
                         Time analyzed
                         SMC CAS no«^
                         SMC areaj;-';'* f,,  v.,r
                         SMC RT  
-------
                                                                          wait
                                FORM QV  - PEST
                      PESTICIDES CALIBRATION CHECK SHEET
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-113
114-119
120-123
124-133
134-142
143-148
149-154
155-159
160
DETAIL
COLUMN
1-3
4-5
6-7
8-17
18-25
26-33
34-38
39
40-45
46
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
9
6
4
10
9
6
6
5
1
RECORD
LENGTH
3
2
2
10
8
8
5
1 , •!, ;; _
,*-j6,,, ''' •:'""
.- all
                        CONTENTS
                        Form number
                        Form suffix
                        Record type
                        Lab name
                        Contract
                        Lab code
                        Case no.
                        Batch no.            ;;
                        Sequence no.
                        SAS no.             :
                        Instrument ID    ,•-.
                        EPA sample no.     ,  .:,,,
                        Lab sample ID        "'•;
                        Standard concentration
                        Date analyzed
                        Time analyzed
                        SMC CAS no..,,
                        SMC area'; 7- ;•',;;,  "''
                        SMC RT   r >;'   ""':~'  f'-'-\
                        SMC 1C RT ;:           f
                        RT %D         .,        1!
                        SMC RT ZD out;tlag  < .':
                        Form number
                        Form suffStx
                        Record
                        -ntitial CF
FORMAT/CONTENTS
"ZZ"
"A&*
•m*
Character  :.
Character
Character
Character
Character
Character
Character
Character
GSkracter
         9.0
                        % D '••;;;
                        % D out'
                        Resol. %
                               % valley out flag
Character
Numeric  9.0
         6.3  (minutes)
         6.3  (minute s)
Numeric  5.1
"*" or blank
FORMAT/CONTENTS
"Q5D"
"AA" - "ZZ"
"Dl"
Character
Numeric 8.0
Numeric 8.0
Numeric 5.1
I1*n or blank
Numeric 6.2
"*" or blank
                                     H-33
                    05/01/92

-------
                                                                          ttftlt
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-92
93-104
105-113
114-119
120-123
124-133
134-142
143-148
149-154
155-159
160
LENGTH
3
2
2
25
11
6
5
8
2
6
10
12
12
9
6
4
10
9
6
' 6
5
1
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-17
18
19-26
27-34
35-39
40
41-46
47
LENGTH
3 ,;
2 ,' -'
' .,K
2 ,"- -
10 ''-'> |
1
8
8
5,.,;W
.^.^^
,;V'V^
§,~?;": 1
                                 FORM QV  - PCS
                        AROCLORS CALIBRATION CHECK SHEET
                         CONTENTS
                         Form number
                         Form suffix
                         Record type
                         Lab  name
                         Contract
                         Lab  code
                         Case no.
                         Batch no.
                         Sequence no.        .;
                         SAS  no.            ;  ,
                         Instrument ID    ; «= \
                         EPA  sample no.     -":-•„
                         Lab  sample ID
                         Standard concentration
                         Date analyzed
                         Time analyzed
                         SMC  CAS nQ.,,
                         SMC  area "|H',;:'>,: , »v
                         SMC  RT  't-   "  ' ^^t{' '
                         SMC  1C RT  " '
                         RT ZD
                         SMC  RT %D  out-flag
                         Form
                         Form suffix
                         Record
                             no,
                                 CF
 FORMAT/CONTENTS
 "Q5E*
 "Mwi - "ZZ"
 "HI"*,
 Gtxaracter
 Character S!
 Character      •;
 Character
 Character
 Character
 Character
 Character
 Character
 Character
 Ktsaeric 9.0
                             out
                             1 . % valley
                               % valley out flag
 HHMM"   ,<
 Character
 Numeric 9.0
: ^eperic 6.3 (minutes)
 Nisaefclc 6.3 (minutes)
 Numeric 5.1
 "*" or blank
 FORMAT/CONTENTS
 "Q5E"
 "AA" - "ZZ"
 "Dl"
 Character
 Numeric 1.0
 Numeric 8.0
 Numeric 8.0
 Numeric 5.1
 "*" or blank
 Numeric 6.2
 "*" or blank
                                      H-34
                     05/01/92

-------
                                FORM QVI - VOA
                     VOIATILES ANALYTICAL SEQUENCE  STMMARY
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-86
87-90
91-96
97-100
101-106
LENGTH
3
2
2
25
11
6
5
8
2
6
10
6
4
6
4
6
                        CONTENTS
                        Form number
                        Form suffix
                        Record type
                        Lab name
                        Contract
                        Lab code
                        Case no.
                        Batch no.
                        Sequence no.
                        SAS no.            ;
                        Instrument ID    V  :
                        Start date
                        Start time
                        Stop date
                        Stop time
                        Initial calibration
                        date
                          FORMAT/CONTENTS
                          "Q6A*
                          "AA*  -  "ZZ"
                          -si*
                         > Character.
                          Character   |
                          Character     : ,
                          Character
                          Character
                          Character
                          Character
                          Character
                          YHBBiDD
                         .YXHMDD
                          YXMMD1)
DETAIL RECORD
COLUMN
1-3
4-5
6-7
8-19
20-31
32-37
38-41
CONTENTS
Form number
Form suffix
Record type
EPA:sample no.
Lab samp|e ID
Date analyzed
Time analyzed
FORMAT/CONTENTS
"Q6A
"AA" - "ZZ"
"Dl"
Character
Character
YYMMDD
HHMM
                                      H-35
                                              05/01/92

-------
                                 FORM QVI  -  PAH
         POLYNUCLEAR AROMATIC HYDROCARBONS ANALYTICAL SEQUENCE SUMMARY
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-86
87-90
91-96
97-100
101-106
DETAIL
COLUMN
1-3
4-5
6-7
8-19
20-31
32-37
38-41
LENGTH
3
2
2
25
11
6
5
8
2
6
10
6
4
6
4
6
RECORD
LENGTH
3
2
2
12
12
6
4
                         CONTENTS
                         Form number
                         Form suffix
                         Record type
                         Lab name
                         Contract
                         Lab code
                         Case no.
                         Batch  no.
                         Sequence no.
                         SAS no.             ;
                         Instrument ID    .,}
                         Start  date        '  •:
                         Start  time
                         Stop date
                         Stop time
                         Initial calibration
                         date     ,  „
                         CONTENTS     !
                         Form number
                         Form suffix
                         Record type
                         EPA sample no.
                         Lab sample ID
                         Date analyzed
                         Time analyzed
FORMAT/CONTENTS
"Q6B"
"A&* -  "ZZ"
^Character
'Character
Character
Character
Character
Character
Character
Character
YXHKDD
YYMMDB
FORMAT/CONTENTS
"Q6B
"AA"  -  "ZZ"
"Dl"
Character
Character
YYMMDD
HHMM
                                      H-36
                     05/01/92

-------
                                FORM QVI - PHE
                      PHENOLS ANALYTICAL SEQUENCE SUMMARY
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-86
87-90
91-96
97-100
101-106
DETAIL
COLUMN
1-3
4-5
6-7
8-19
20-31
32-37
38-41
LENGTH
3
2
2
25
11
6
5
8
2
6
10
6
4
6
4
6
RECORD
LENGTH
3
2
2
12
12
6
4
                        CONTENTS
                        Form number
                        Form suffix
                        Record type
                        Lab name •
                        Contract
                        Lab code
                        Case no.
                        Batch no.
                        Sequence no.
                        SAS no.
                        Instrument ID
                        Start date
                        Start time
                        Stop date
                        Stop time
                        Initial calibration
                        date     <.  .
                        CONTENTS
                        Form number
                        Form suffix
                        Record type
                        E£A sample no.
                        Lab sample ID
                        Date analfized
                        Time analyzed
FORMAT/CONTENTS
"Q6C"
"AA" - "ZZ"
•Mil* >
Character
Character
Character     '"
Character
Character
Character
Character
Character
1SMMDD
FORMAT/CONTENTS
-Q6C
"AA" - "ZZ"
"Dl"
Character
Character
YYMMDD
HHMM
                                     H-37
                    05/01/92

-------
                                FORM QVI - PEST
                    PESTICIDES ANALYTICAL SEQUENCE SUMMARY
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-86
87-90
91-96
97-100
101-106
DETAIL
COLUMN
1-3
4-5
6-7
8-19
20-31
32-37
38-41
LENGTH
3
2
2
25
11
6
5
8
2
6
10
6
4
6
4
6
RECORD
LENGTH
3
2
2
12
12
6
4
                        CONTENTS
                        Form number
                        Form suffix
                        Record type
                        Lab name
                        Contract
                        Lab code
                        Case no.
                        Batch no.
                        Sequence no.
                        SAS no.           ;'
                        Instrument ID    ;
                        Start date
                        Start time
                        Stop date
                        Stop time
                        Initial calibration
                        date
                        CONTENTS
                        Form number
                        Form suffix
FORMAT/CONTENTS
"Q6B"
     '- "ZZ"
Character °
Character
Character
Character
Character
Character
Character
YXUHDDD
HHMM
YXMHDP
                                   no.
                        Lab sample ID
                        Date anal
                        Time ar
FORMAT/CONTENTS
"Q6D
"AA" - "ZZ"
"Dl"
Character
Character
YYMMDD
HHMM
                                     H-38
                     05/01/92

-------
                                FORM QVI - PCB
                     AROCLORS ANALYTICAL SEQUENCE SUMMARY
HEADER RECORD
COLUMN
1-3
4-5
6-7
8-32
33-43
44-49
50-54
55-62
63-64
65-70
71-80
81-86
87-90
91-96
97-100
101-106
DETAIL
COLUMN
1-3
4-5
6-7
8-19
20-31
32-37
38-41
LENGTH
3
2
2
25
11
6
5
8
2
6
10
6
4
6
4
6
RECORD
LENGTH
3
2
2
12
12
6
4
                        CONTENTS
                        Form number
                        Form suffix
                        Record type
                        Lab name
                        Contract
                        Lab code
                        Case no.
                        Batch no.
                        Sequence no.
                        SAS no.
                        Instrument ID    >
                        Start date        "
                        Start time
                        Stop date
                        Stop time
                        Initial calibration
                        date     ,  ,,
                        CONTENTS   '•'•„
                        Form number   i
                        Form suffix
                        Record type
                        EPA sample no.
                        liab sample ID
                        Date analyzed
                        Time analyzed
FORMAT/CONTENTS
"Q6B"
"A&"?  -  "ZZ"
•Wt-
Character
Character
Character
Character
Character
Character
Character
Character
YXM8DD
YYMMDB'
FORMAT/CONTENTS
"Q6E
"AA" - "ZZ"
"Dl"
Character
Character
YYMMDD
HHMM
                                     H-39
                                                                      05/01/92

-------
                                                                         tttttt
                                FORM QVII  - VOA
                             VOIATILBS NARRATIVE
HEADER RECORD
COLUMN      LENGTH      CONTENTS                  FORMA3VCONTENTS
1-3         3           Form number               "Q7A"
4-5         2           Form suffix               "A&*
6-7         2           Record type               "HI"  -
8-32        25          Lab name                  Character
33-43       11          Contract                  Character
44.49       6           Lab code                  Character
50-54       5           Case no.             :     Character
55-62       8           Batch no.            ,;;     Character
63-68       6           SAS no.              ,     Character
DETAIL RECORD
                        CONTENTS             ': :  .PQBMAT/CONTENTS
                        Form number              ;*Q?Alf
                        Form suffix               "A&* - "ZZ"
                        Record type               "Dl" f
                        Comment line #            Numeric 3.0
                        Comment  „  
-------
                                FORM QVII  - PAH
                  POL7NUCLEAR AROMATIC HYDROCARBONS  NARRATIVE
HEADER RECORD
COLUMN      LENGTH       CONTENTS                  FORMAT/CONTENTS
            3            Form number               "Q7JJ*
            2            Form suffix
            2            Record type
            25           Lab  name                  Character
            11           Contract                  Character':   •,.,
            6            Lab  code                  Character    '- ':•
            5            Case no.                   Character
            8            Batch no.            s      Character
            6            SAS  no.             .       Character

DETAIL RECORD                             :             !

COLUMN      LENGTH       CONTENTS             '  f   FJORftAT/CONTENTS
1-3         3            Form number             ;; '^7Bn
4-5         2            Form suffix               "M? - "ZZ"
6-7         2            Record type               "Dl"
8-10        3            Comment line  #            Ntuneric 3;~0
11-75       65           Comment-|1 '••'J.i   ;         Character
                                     H-41                              05/01/92

-------
                                                                          DfcAJt
                                FORM QVII - FHE
                               PHENOLS NARRATIVE
HEADER RECORD
COLUMN      LENGTH      CONTENTS                   FORMAT/CONTENTS
            3           Form number                "Q7C*
            2           Form suffix                "AA,"
            2           Record type                *?B1" :
            25          Lab name                   Character
            11          Contract                   Character
            6           Lab code                   Character
            5           Case no,                '..   Character
            8           Batch  no.            ^     Character
            6           SAS no.              ',"     Character

DETAIL RECORD                                         , •'.

COLUMN      LENGTH      CONTENTS              '  f   F<3BMAT/CONTENTS
1-3         3           Form number                fQ^C"
4-5         2           Form suffix                *A£" -  "ZZ"
6-7         2           Record type                "Dl" \\
8-10        3           Comment TJupG #             Numeric 3,0
11-75       65          Comment ,;,;j,;;;s!,''','    ,      Character
                                      H-42                             05/01/92

-------
                                FORM QVII - PEST
                              PESTICIDES NARRATIVE
HEADER RECORD
COLUMN      LENGTH       CONTENTS                  FORMAT/CONTENTS
            3            Form number               "Q7B*
            2            Form suffix               "M*
            2            Record type               nJ£L*
            25           Lab name                  Character
            11           Contract                  Character    ;,
            6            Lab code                  Character    '-* [•,
            5            Case no.             .  v;  Character      :;
            8            Batch no.           :     Character
            6            SAS no.                   Character
DETAIL RECORD
                         CONTENTS               ;•<  FilgMAT /CONTENTS
                         Form number               :::*Q7D"
                         Form suffix               "A&* - "ZZ"
                         Record type               "D1H> ;
                         Comment line, #            Numeric 3;0
                         Comment --; - '>• }'• • -'f          Character
                                      "
                                      H-43                              05/01/92

-------
        HEADER RECORD
                                                                                  nut
                                        FOKM QVII - PCB
                                      AROCLORS NARRATIVE
        COLUMN
LENGTH
3
2
2
25
11
6
5
8
6
CONTENTS
Form number
Form suffix
Record type
Lab name
Contract
Lab code
Case no.
Batch no.
SAS no.
FORMAT/CONTENTS
"Q7I"
"AA;*
                                                           Character
                                                           Character
                                                           Character
                                                           Character
                                                           Character
                                                           Character
        DETAIL RECORD
        COLUMN
        1-3
        4-5
        6-7
        8-10
        11-75
LENGTH
3
2
2
3
65
CONTENTS
Form number
Form suffix
Record type
Comment line #
Comment s-'_  til? V,i
F0SI1AT/CONTENTS
"SQJE"
"ML* - "ZZ"
"Dl" > .:   , _
Numeric :3»0
Character
U.S. Environmental Protection Agency
Region 5, Library (PL-12J)
77 West Jackson Boulevard, 12th Floor
Chicago, IL  60604-3590
                         H-44
                                               05/01/92

-------