US EPA Contract Laboratory Program Statement Of Work For Analysis Of Ambient Air, July 1991, Iair01 2


                            _„.  .           Publication 9240.1-29
            United States           Office of           EPA/540/R/95/040
            Environmental Protection      Solid Waste and        ~PB95 963537
            Agency             Emergency Response     March1995


            Superfund		
v»EPA      USEPA Contract Laboratory
             Program Statement of Work
             for Analysis of Ambient Air
             July 1991
             IAIR01.2

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

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V.

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                               STATEMENT OF WORK.


                               TABLE OF CONTEI


                                              V      ^
                                                                       Page No.



PREFACE	6  •  -\ •  •/•  /	i


EXHIBIT A  SUMMARY OF REQUIREMENTS  FOR ANALYSIS^ OF AMBJENT AIR	A-l


EXHIBIT B  REPORTING AND DELIVERABLES REQUIREMENTS >^ .  ~N^	B-l


EXHIBIT C  TARGET COMPOUND LIST  ./... T—r-^__^..  .  .  .^X	C-l


EXHIBIT D  PREPARATION AND ANALYSlk METHODTT~7 . /->_.  .  ./.	D-l


EXHIBIT E  QUALITY ASSURANCE/QUALITY C
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                                    PREFACE
      The purpose of this contract  is  to provide  the U.S.  Environmental
Protection Agency  (EPA) with chemical  analytical  services
procedures, and ah analysis structure  which will  generate
documented quality.  The Statement of  Work was developed
the air toxics workgroup to ensure that  the needs of  re
air pollution programs were addressed.
      The samples to be analyzed are of ambient  air
vicinity of known or suspected hazardous waste sit
potentially hazardous organic and/or inorganic ma
concentrations.  The Contractor should be aware  off
associated with the handling and analyses of  these
Contractor's responsibility to take all necess/ary
                                                                ity control
                                                                of known and
                                                              the guidance of
                                                                state and  local
                                                                       the
                                                     e potential hazai
                                                    amples.  It is the
                                                   leasures and precautions to
ensure the health and safety of its employees/  The Contjacbor is responsible
for providing a safe working environment and/malcing its/employees aware of the
potential hazards of working with and analyzing, these /ampUes,

      Procedures specified herein shall be used in^tfie Preparation and
analysis of air samples for the presence and quaiatitatr
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                                  EXHIBIT A
                           SUMMARY OF REQUI
                           ANALYS
July, 1991
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SECTION 1
SECTION 2
      2.1
      2.2

      2.3

SECTION 3
      3.1
      3.2
      3.3
      3.4
      3.5
                                   EXHIBIT A
              SUMMARY OF REQUIREMENTS FOR ANALYSIS OF
                                                                       Page No.
GENERAL REQUIREMENTS	/./....  >x^.  .  >x^   A-1
SPECIFIC REQUIREMENTS
Receive and Prepare Ambient Air  S
Analyze Samples for the Identifi^at
Quantitation of Specific Parame
A-2
A-2
Perform Required Quality Asst
Quality Control Procedures   .  .^S^.  . ^x/.  ./	A-4
DETAILED TECHNICAL AND MANAGEMENT
Personnel	^\-  • ^>	A-10
Facilities	/.  !^T~T~r—r-»^_^.  .  . >/	A-13
Instrumentation . .   . .\.  \T~~7—?•—~^..  .  .  .  .  77	A-14
Data Handling and Packaging  . \.  .././.. 7^	A-15
Laboratory Management Require^nehX^  /	A-15
July, 1991
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Exhibit A
                                                      SOW No.  XXX -  Ambient Air
                                   SECTION 1
    »

                             GENERAL REQUIREMENTS

   The Contractor shall employ procedures  specified in/thi4  Statement of Work
(SOW) in the preparation and analysis of the  ambient /ir  samp^i^s  for the
presence and quantitation of the organic and  inorganic  j^ontpoundsMjndicated in
Exhibit C.
   The Contractor shall use proven  techniques  to
organic and inorganic parameters presented  in
as specified in Exhibit C.  The Contractor  sh
and analysis procedures as prescribed  in Exh
preservation and holding time requirements.

   For all samples analyzed under this co
to the QA/QC protocols specified in Exhibi
protocols specified in Exhibit F.
   Following sample analysis, the Contractor  shall
shall report analytical activities, sample data, and
documentation as designated in Exh
and deliverables requirements for
reporting forms and a forms ins true
                                                    ^ntify and mea
                                                   parget  Compound List
                                                          sample  preparation
                                                              specified sample
   To ensure proper understanding of t'
contains a glossary of terms.  When a te
explanation, the glossary meaning shall be
do not replace or take precejiertesover
SOW text.
   The samples to be an,
hazardous waste sites .and
materials at high concen
potential hazards as/soc
It is the Contracto
the health and safety o

   In addition
the integrity
major decisio
addition,
potentiall
                                                          ractor shall adhere
                                                            the  evidentiary
                                                              _ta reduction and
                                                                 trol
                                                                   reporting
                                                           copies  of  the  data
                                                   in  this  contract,  Exhibit  G
                                                 d in the  text without
                                               Icable.  Glossary definitions
                                                information included in  the
                                   e i-Contr^ctor a^pe  from known or suspected
                                   in hazardo>is_organic and/or inorganic
                                  vel^s.  The Contractor should be aware of the
                                  tWe handling~4.nd analysis of these samples.
                                   ty to take all necessary measures to ensure
                                  yees.

                                lust be.  aware of the  importance of maintaining
                                    undeft this contract, as it is used to make
                                            environmental welfare.  In
                                ,his contract may be  used in litigation against
                                   the  enforcement of Superfund legislation.
July, 1991
                                                                       Page  A-l
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Exhibit A
                                                      SOW No.  XXX -  Ambient Air
                                   SECTION 2

                             SPECIFIC REQUIREMENTS

     For  each  sample,  the  Contractor shall perform the/fo^lowibg^tasks:

2.1   TASK I:    RECEIVE AND PREPARE AMBIENT AIR SAMPLES
2.1.1  The Contractor shall receive and handle sampl
custody and document control procedures describe^
                                        under the
                                      Exhibit F.
2.1.2  The Contractor shall provide the requi/ed/analytirfaKexpertise  and
instrumentation for analyses of the TCL analyte/ equal tto o£ lower than  the
quantitation limits specified in Exhibit C/ Iri Exhibi/ D/EPA provides  the
Contractor with the specific sample preparation\technique4 for ambient air
samples and an appropriate set of analyticalxproce^ces/that shall be  used.
2.1.3  The Contractor shall prepare and analyze samples
holding time specified in Exhibit D, even if these tie
maximum data submission time allowe<
                                                the  maximum
                                                  than the
2.1.4  The Contractor is advised tt
contract are usually from known or
contain high levels of organic and
hazardous nature and of unknown structui
handled throughout the preparation and ar
Contractor shall be responsible for all
                                           :sess
                                           .under  this
                                              sites  and may
                                            potentially
                                  entration,  and  should be
                                  ith appropriate  caution.   The
                                v measures and precautions to
ensure the health and safety^-oT"1raboratorv employees.
2.2   TASK II:
ANALYZE
SPECIFIC
                                     IE IDENTIFICATION AND QUANTITATION OF
                              STERE
2.2.1  For each sample received, /6he/Cont£ax^tor /shall be required to perform
the analyses described aVfollow6. /The documentation that accompanies the
sample(s) to the ContTsactor^xfa^lllCy shall indicate specific analytical
requirements for that sample or s^et of samples.

2.2.2  Exhibit D^spet^tfies the^analytteal procedures that shall be used.
Exhibit D contains instructions anaxrefeifences for preparation of ambient air
samples contadnin^Tow^tQ^edrum concentrations of organics for GC/MS analysis
and inorganics for ICP/AA analysis.   GC/MS may use automated computer programs
to facilitate ,che identification \^f organic compounds.

2.2.3  A/1 samples must initially be run undiluted (i.e., final product  of
sample prfepaxatban procedure)./ Wtyen an analyte concentration exceeds the
calibrated or\Mnear\range, appropriate dilution  [(but not below the contract
required quantit^ion rimit /CRQL) ]  and reanalysis of the prepared sample is
required, as specifi«4 iiiExhiVit D.
July,  1991
                                                                       Page  A-2
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Exhibit A
                                                 SOW No. XXX - Ambient Air
2.2.4  For the purpose of  this  contract,  a  full  sample  ana
analysis for all -of. the TCL constituents  identified  in  Ex
with the methods in Exhibit D and performance  of related
Exhibit D and Exhibit E.   Laboratory Control Samples
analyses shall each be considered a separate full samp
QA/QC requirements are considered an inherent  part o~
included in the contract sample unit price.
                                                         is is defined as
                                                           C in accordance
                                                        $C as specified in
                                                           spike sample
                                                       ilysis.   All other
                                                               are
2.2.5  The volatile and semivolatile compounds a
and initially identified shall be verified by anarayst competent  ih\the
interpretation of mass spectra by comparison of/the; suspect mass spectra^-
the mass spectrum of a standard of the suspected Compound.  This procedure
requires the use of multiple internal standards./ Two cr/&»ria must be
satisfied to verify the identifications.
     2.2.5.1  Elution of  the  sample  component
     retention  time  as  the  standard  componei
                                            the s4me/GC relative
2.2.5.2  Correspondence of the sample componei
mass spectra.
                                                     and
                                                                 component
2.2.6  For each sample analysis, the ConEta&tor^shall conduct/mass spectral
library searches of non-target compound-sample compoHenfcSL^to determine
tentative compound Identifications ag fallows:

     2.2.6.1  For each volatile fractiohv.  the  tfontrtactor shall conduct a
     search to  determine the  possible  idetoticy of up  to  10  organic  compounds
     of greatest concentration which are  no^ system monitoring compounds  and
     not  listed in  Exhibit
2.2.6.2  For each
search to determine
organic compoundsy
Exhibit C.

2.2.6.3  In per
Institute of Standa
library must be used.
     NOTE:   Sul
     internal
                                  Le fraction,
   possible1
greatest/cone
                                        itrati
je  Contractor  shall  conduct a
  yn. of up to  20 non-surrogate
 tfhich are not listed in
                       ing'-se^a/ches,  the most  recent release of  the National
                                T/chnology  (NIST)/EPA/MSDC  mass spectral
                        espon,
                          require
            of^Less  than 10  percent of the  nearest
              :o be  searched in this fashion.
July,  1991
                              iparison of sample specta with the spectra
                               the mass spectral interpretation
                              identification.  If the compound does not
                              ia, it shall be reported as unknown.  The
                          hovild give additional classification of  the
                         ible (i.e., unknown aromatic, unknown
                           :ype, unknown chlorinated compound).  If


                                                                  Page A-3
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Exhibit A
                                                 SOW No. XXX - Ambient Air
    probable  molecular weights  can be distinguished, they/alsrb should be
    included.    •  •
2.3
     2.2.6.5  The-Contractor shall not  report as  semiv
     identified  compounds  (TIC)  any  target compound f:
     (i.e., late eluting volatile compounds shall no
     the  semivolatile  analysis).  However,  the Cont,
     target compounds  that appear as semivolatile
     compounds.
                                                         ^tentatively
                                                                  fraction
                                                                .TICs  in
                                                                   jticide
 TASK  III:    PERFORM REQUIRED QUALITY ASS
              PROCEDURES
                ICE AND QUALITY CONTROL
2.3.1  All specific QA/QC procedures presc/ibe^ in  Exhibits  D  and E shall be
strictly adhered to by the Contractor.  Re^ordsMocumenting  the  use of the
protocol shall be maintained in accordance wKh  the^^document control
procedures prescribed in Exhibit F, and shall be\report«d  in accordance with
Exhibit B requirements.

2.3.2  The Contractor shall establish-~aad_use on a  continuing  bfasis QA/QC
procedures including the daily or  f4s require3>—fflocgfrequent'use of standard
reference solutions from EPA, NIST\prT\5ec«n4gry standarcls—traceable thereto,
where available at appropriate concentrations (y-e./^-standard  solutions
designed to ensure that operating parameters of/equipment  and  procedures,  from
sample receipt through identification and qviaytitzation, produce  reliable
data).  Exhibits D and E provide specif ic\QA/QC/requirements.
2.3.3  Additional QA/QC sh
with each Case or Sample
Control Samples (LCS) foy
inorganics submitted to
verification of instr
                          be
                        ;anic:
                        for Coiitractor^
                   .ent parameters
 .quired quarterly or more frequently,  i.e.
Grtoup (SDG) ,\in the form of Laboratory
 aryd^fiejrformance Evaluation (PE) Samples  for
              sis,  and in the form of
               ed in Exhibit E.
jiesci
2.3.3.1  EPA has^provided tc
data (Exhibit B).
returning analysis datasheet
within the time specified\in
                                      Contractor  formats  for the  reporting of
                                  itor shall be responsible for completing and
                                       the format specified in this SOW and
                                      Contract Performance/Delivery Schedule.
                                         .ose  designated by EPA will be deemed
                             data are unacceptable.   Resubmission in the
                              dicional cost to the Government will be
     2.3
     packag^
     that the
     including fo
     columns, and
                               ms may be submitted in the hardcopy data
                              orms are  in exact EPA  format.   This means
                          merits  is the  same as on each  EPA  required  form,
                         d /cities, page numbers and  header  information,
July,  1991
                                                                  Page A-4
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Exhibit A
                                                      SOW No.  XXX -  Ambient Air
2.3.4  The  Contractor  shall provide  analytical  equipment  a
expertise for  this  contract as  specified  by  the following
                                          technical
     2.3.4.1  Gas. chromatograph/mass  spectrometer (GC/MS,?  data system capable
     of meeting all the terms and conditions of the Conrra^f with the
     following requirements:

       •   The GC/MS shall be equipped with a glass
          packed columns;

          The computer shall be interfaced by h
          spectrometer and be capable of acqui/in(
          the duration of the chromatographic

          The computer shall be equipped wi
          all data from the GC/MS runs;
                                                   using
                                ire  to the mass
                                continuous mass  scans  for
                                       devices  for  saving
          Computer software shall be availableXtp
          for specific ions and plotting the inte
          respect to time or scan number;
          A computer data system m
          continuous acquisition a
          all mass spectra obtained
          chromatographic program.
          allows  searching any GC/MS
          and plotting such ion abundancx
          type of plot is defiend as an
          Software must also
          abundance in any/EICP befeyeen
          Also,  for the non-j23r~£e£ c
          allows  for th
          library spec/ra
          spectral
          system
          edited  ma
                                    searching GC/MS  runs
                                      the ions with
             yailable t
                          sp<
                                    ory personnel;
          The  GC/MS  shall
                            si
                    to be~--3) mete
                        used slica
          The  C?C for pesticide a
           r vride bore capillary
                       :hat allows the
                  •eadable media, of
           duration7of the
                   software that
           ions of a specified mass
          time or scan number.  This
  t;ract^d Ion Current Profile (EICP)
         lows intergrating the
speciXied\time or scan number limits.
            .re must be available that
            a against reference
       .ease, of the NIST/EPA/MSDC mass
         eference library.  The data
         data files that have been
    2.3.4.
    the capabi"
July. 1991
                  with a GC to MS interface capable of
                   llary column into the ion source.  The
                      y 0.25 or 0.32 mm inside diameter,
                     uivalent; and

              lysis shall be equipped with packed columns
               lumns and a suitable detector as described
i,vely  coupZ.edyplasma  (ICP)  emission spectrophotometer with
           mentals sequentially or simultaneously.
                                                   Page  A-5
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Exhibit A
                                                      SOW No.  XXX -  Ambient Air
     2.3.4.3  Atomic absorption (AA)  spectrophotometer equi
    •furnace  and flame  analysis capabilities.
                                                           with graphite
    2.3.4.4  The. Contractor  shall  use  a magnetic tape ^tor4ge device  capable
    of recording data  and suitable for long-term, off/line stooge.   The
    Contractor  shall retain  all raw GC/MS data acquited/unb^r thrs^contract
    on magnetic tape in appropriate instrument manuTac/turer'ss§prma^>\The
    Contractor  is  required to  retain the magnetic 4a^es with associated"
    hardcopy tape  logbook identifying  tape conteirfts^(see Exhibit B)r®r 36!
    days after  data submission.  During that tinie,/the  Contractor shall
    submit tapes and logbook within seven days/of/request, as specified in
    the Contract Performance/Delivery  Schedu]
    2.3.4.5  The Contractor shall have  a  coApu/erized
    system capable of providing  a  forward
    spectra contained in  the  mass  spectral
    recent) release of  the NIST  library (conta
    used.
                                                      ibrary search
                                      Jomp^ison/us/ng  the standard
                                                     1985  (or most
                                                42^.261 spectra) must be
          The  system shall provide a.numerical ranking or
          most closely corresponding to~tHe~~sainpjie^spectra
      •    The  data system shall haveN
          signals  from spectra.

    2.3.4.6  The Contractor shall have, £t
    capable of analyzing purgeable organic*
                                                  of
           je  standard  spectra
               ined;  and

            rving background
                                             and operable,  a device
                                        as Described in Exhibit D; and
    2.3.4.7  The Contractor shall have, in-hoi
for all target compounds
samples from the Sample/Manage)]
EPA for use in the/Pre'award Pe
the target compounds/and thus
unless or until /they^have be
standard material
                                        Exhibit
                                         ice
  £he appropriate standards
    Lor to accepting any
      Standards provided by
  ition may not contain all
sed for routine analyses
with commercially-available
2.3.5  The minimum functionki^requl^ements necessary to meet the terms and
conditions of this^-eefttxact areN(istea\below.  The Contractor shall designate
and use qualifies key personnel to>erfor^n these functions.  The EPA reserves
the right to revi^r^ers«nneiN^ualifica
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Exhibit A
                                                      SOW No.  XXX -  Ambient Air
       Systems Manager;

       Programmer Analyst; .

     •  GC/MS Operators;

     •  Mass Spectral  Interpreter;

       Inductively Coupled Plasma  (ICP) Operators;
                                                r
       Inductively Coupled Plasma  (ICP) Spectro^coj

     •  Graphite Furnace Atomic Adsorption  (G!

     •  Sample Preparation Laboratory Supei

       Sample Preparation Specialists; anc

       Chemist (back-up).

NOTE:  The Contractor shall designate a Sample Custodian\and"a~>Document
Control Officer.
2.3.8  The Contractor s
control procedures deacriWed
therein, shall be requir
followed.  This docuroen
Purge (Exhibit B).

2.3.9  Sample shipments
coordinated by SMOi_acting on
(APO).   The Co
necessary thr/fughpj±e—ciie pro
data reporting,/to ensure^hat
2.3.6  The Contractor shall respono\wi
recipients for additional informatio
Government's inspection activities.

2.3.7  The Contractor is required  to reta
sample containers for a. period— o^  60 days
otherwise instructed in Exhibit B
                                                            ts  from  data
                                                           result from  the
                                                   sample volumes and used
                                                data submission unless
                                                  /-custody and document
                                              cumentation, as described
                                            procedures are being strictly
                                •/allbe reported in the Complete Case File
 Contractor's facility will be scheduled  and
 Lehalrxpf the Administrative Project Officer
     icate^with SMO personnel by  telephone  as
:ss of s^mt/le scheduling, shipment, analysis, and
  amples are properly processed.
                             co
     2.3.9/1  Af there are problem^ with  the samples  (e.g., mixed media,
     containers broken)  or sample  documentation/paperwork (e.g., Traffic
     Reports  no^with shipment J or/ sample and  Traffic Report  numbers do not
     corresp^snd)  the  Contracto/r sbiall  immediately contact SMO for  resolution.
     The  Contrafr
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Exhibit A
                                                      SOW No.  XXX -  Ambient Air
    reporting.   In particular,  the Contractor shall noti
    'advance  regarding sample data that will be delivere
    specify  the  estimated delivery date.
                                               site
2.3.10 Sample analyses will be  scheduled by groups  o
as a Case and identified by a unique  EPA Case  numbe
signifies a group of samples collected  at one
finite time period, and will include  one or more
blanks.  Samples may be shipped to  the  Contracto,
multiple shipments over a period of time,  depe
A Case consists of one or more  SDG(s).   An S

       Each Case of field samples received;

     •  Each 20 field samples within a Cas

     •  Each seven calendar day  period during wl
       are received (said period beginning with
       sample in the SDG).
                                                              !0 personnel in
                                                               and shall
ach defined
   IP.  A Case
        over a
          ated
2.3.11 Data for  all  samples in an S>DG must
package) in the  order  specified in
number of the first  sample  received
received together  in the  first SDG sh
sample number (considering  both alpha
group of samples received under the SDG.
data reporting forms.   The  SDG Receipt Dat
the SDG is received.
                                                           by the  following:
                                                       14 samples in a Case
                                                             of the first
                                                   Itted together (in one
                                                             r is the EPA
                                                      _several samples are
                                                             is the lowest
                                                   designations)  in the first
                                                   number is reported on all
                                               (the day that the  last sample in
2.3.12 The  Contractor is/responsible^
received, through  proper sample  dopi
communication with SMC/pe/sonnel.,
                                      fo_r identifying each SDG as samples are
                                                    Exhibit B) and
 2.3.13  Each sample ^eceiv^d by tfhe/Contractor will be labeled with an EPA
 sample  number,  and abs^mpanie^/by/a  Traffic Report (TR)  form bearing the
 sample  number and descriptive information regarding the  sample.   The
 Contractor shall complete aftd^sigrNt^ie TR, recording the date of sample
 receipt and sampj^e^-ctmd4^tion orf^receip-t^for each sample  container.

 2.3.14  The Coiitr^c'tor^shaj.l submit sigWd copies of TRs  for all samples in an
 SDG to  SMO v/ithln three ca!be.ndag. days following receipt  of the last sample in
 the SDG.   TELs/shall be submith:ed\in SDG sets (i.e., all  TRs for a SDG shall be
 clipped t/geoher) with an SDG ^ove^r Sheet containing information regarding the
 SDG,  as /pecr£ied in Exhibit B.
 2.3.15 EPA C
 be used by the
 both verbally and i
                 numbers (including SDG numbers) and EPA sample numbers shall
                   .tracbsr ir/ identifying samples received under this contract
                       eports/cprrespondence.
 July, 1991
                                                                        Page  A-8
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Exhibit A
                                                      SOW  No.  XXX  -  Ambient  Air
2.3.16 Samples will be routinely shipped directly  to  the  Contractor  through  a
delivery service,  .The Contractor shall be available  to rycewe sample
shipments at any cime the delivery service is operating,/ inoduding Saturdays
and holidays.  AS necessary, the Contractor shall  be  re,spoi^sible for  any
handling or processing required for the receipt of sample ^shipments,  including
pick-up of samples at the nearest servicing airport, /bus  stabion, or  other
carrier service within the Contractor's geographical/ar,ea>
                                             any/
2.3.17 The Contractor shall accept all samples set
that the total number of samples received in
exceed the monthly limitation expressed in the
Contractor elect to accept additional samples,/thf
bound by all contract requirements for analy<
jduled by SMO>provic
 Lendar month  does^npt
fract.   Should the
 Contractor  shall remain
        imples accepted.
July, 1991
                                                                      Page A-9
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Exhibit A
                                                      SOW No.  XXX -  Ambient Air
                                   SECTION 3

                 DETAILED TECHNICAL & MANAGEMENT REQUII

    The  Contractor shall have the following technica/ an^mana^gejnent
capabilities:

3.1 PERSONNEL

3.1.1  Project Manager

    Responsible  for all technical efforts of,
and conditions of the contract.

       Education:  Minimum of Bachelor's
       scientific/engineering discipline.

    •  Experience:  Minimum of three years  of  laboi
       including at least one year in a supervisory
3.1.2  GC/MS Laboratory Supervisor

    Responsible  for  all  technical  e
terms and conditions of the contract.
3.1.4
                           to meet all terms
     •  Education:  Minimum of Bachelor's
       scientific/engineering discipline.

                          /^^
     •  Experience:  Minimum of thre
       operating a GC/MS/ including alt
       position.
                           atory to meet all


               In chemistry or any
                        experience  in
                   r  in a supervisory
3.1.3  Inorganic Lab

     Responsible  for
all  terms and conditions

     •  Education
       scienti,
/efforts of the Inorganic laboratory to meet
jntract.

        degree in chemistry or any
                                 iree years of  laboratory experience  in
                              \including at least one year  in  a  supervisory
     Responsible r<}r ove~isseei/hg /fhe quality assurance aspects of data
generation and  reporting oirectfly  to  upper management.
July,  1991
                                    Page A-10
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Exhibit A
                                                      SOW No. XXX - Ambient Air
       Education:  Minimum of Bachelor's degree in c&emistr/v or any
       scientific/engineering discipline.
                                                            Derience,
                                                           Lth QA principles
     •  Experience:  Minimum of three years of laboraitor
       including at least  one  year of applied experift
       and practices  in  an analytical laboratory.

3.1.5  Systems Manager

     Responsible  for the  management and quality c/Shtr'pl of all compu^
systems (hardware, software, documentation,  and/procedures),  generating^
updating,  and performing quality  control  on automated deliverables.
       Education:  Minimum of Bachelor's  de
       intermediate courses  in programming
       management systems, or systems  req
                                             ree
                                           irer
                                          with  foiar  oT  more
                                         ormatiop  management,  database
                                         nts  ailaly/is.
       Experience:  Minimum of  three  years  ex"p^riencq
       management or programming  including  one  ^^^^
       used for data management and generation  of del

3.1.6  Program Analyst

    Responsible  for  the installati
and programs; generating, updating,
on analytical databases and automated
       Education:  Minimum of Bachelor's
       intermediate courses in-programming
       information systems'; or systems requi
                        tnu.
Experience:   Min
applications prpgr
software used /for/data manage:
    tW(
ling ir
                                                        n data or systems
                                                      xp'exj.ence with software
                                                      maintenance of software
                                                            control  procedures
                                                      four or more
                                                 rmatilon management,
                                                   s  analysis.
                                        s~^experieN5ic/e  in systems  or
                                   iluding  onfe^year of experience  with
                                                 eration of deliverables,
3.1.7  Gas Chroinato^
                                spe/trometer  (GC/MS)  Operator
       Education:  Minimunh^of Bachelor's  degree  in chemistry  or any
       scient:" "
       Experiences-—Minimum ~b€ one ye-ar^/£>f  experience  in operating and
       maintaining GC/MS  rr^struments  in  conjunction with the education
       requirement; or  in li\u o:E education requirement,  three additional
       vea^s /f experience in\>peVating  and maintaining GC/MS
3.1.8  Mass^^pectru^ Interprej/er

       Education:^^inimul8vyf  Bachelor's  degree  in chemistry or any
       scientific/engoMaeering/discipline  with specialized training in GC/MS.
July, 1991
                                                                      Page A-LL
-------
Exhibit A
                                   SOW No.  XXX -  Ambient Air
     •  Experience:  Minimum of two years of applied experXenjze with  GC/MS
       analysis of environmental samples.

3.1.9  Inductively Coupled Plasma (ICF) Spectroscopis

     •  Education:  Minimum of Bachelor's degree in
       scientific/engineering discipline and speci,
       spectroscopy.

     •  Experience:  Minimum of two years of
       analysis of environmental samples.

3.1.10 ICP Operator

     •  Education:  Minimum of Bachelor's
       scientific/engineering discipline.

       Experience:  Minimum of one year of applie
       analysis of environmental samples or in lieu o
       requirement, three additional^ears of experience
       maintaining ICP instrumental:ion
     Responsible  for
terms and conditions

     •  Education:
       scient
                                            with ICP
                                            onal
                                             ing and
3.1.11 Graphite Furnace Atomic Abso

     •  Education:  Minimum of Bachelor^
       scientific/engineering discipline\

     •  Experience:  Minimi
       analysis of enviro;
       requirement, thr
       maintaining AA

3.1.12 Sample Prepar
                         ,rjee  in chemistry or any
                               d experience with AA
                                u of educational
                                 ience operating and
 3.1.13
            :al/efforts of sample preparations to meet all
              Contract.

      ium of^BacheloxE\s  degree in chemistry or any
            discipline,!

              hree years of laboratory experience,
               r of supervisory experience.
        EducaT
        in gener
  Lnimum otf high school diploma and a college level course
chemistry/or (equivalent.
        Experience:   Mil
        analytical laborato^i
             six months of applied experience in an
 July,  1991
                                                   Page A-12
-------
Exhibit A
               SOW No.  XXX - Ambient Air
3.1.14 Technical Staff Redundancy

     In order  to  ensure  continuous  operations  to  accomplish ehe  required work
as specified by.the contract, the bidder shall have a minimum of one chemist
available at all times as a back-up technical person with 4he following
qualifications.

       Education:  Minimum of Bachelor's degree  in
       scientific/engineering discipline.

       Experience:   Minimum of one year of expei
       following areas:  GC/MS operation and m/intzenance; ICP operation and
       maintenance; AA operation and maintenance/ classiczSt^chemistry
       analytical procedures; and sample preparation fo/ inorganics analysis.
3.2 FACILITIES

    The  adequacy  of  the  facilities  and  equipmet
technical staff for accomplishing the required worl
contract.

3.2.1  Sample Receipt Area

    Adequate, contamination-free,
resistant bench top shall be available
samples.

3.2.2  Storage Area
                 important as the
                     ified by the  EPA
                       with chemical
                      handling  of  EPA
    Sufficient  refrigerator  space  £s  maintain\unu\ed  EPA  sample volume  for up
to 60 days after data subTOis/^Torrx^hal(l be provided.) Volatile samples must be
stored in a refrigerate
contract.  Samples mus
from all potential coy
stored separately.

3.2.3  Sample Preparatr

     Adequate,
provided with:
             olatile  samples  from  this
          ,e  demonstrated  to  be  free
          ts,   and standards must be
.^ventilated work space shall be
                                  /in which to prepare standard materials;

                              de^iineralized organic-free water; and
Julv, 1991
                               Page A-13
-------
Exhibit A
                                              'SOW No. XXX -  Ambient  Air
Analytical balance(s) located away  from draft  and  r
temperature.
3.3  INSTRUMENTATION

     At a minimum,  the  Contractor  shall have the
operative at the time of the Preaward  Site  Evaluati
full duration of the contract.
3.3.1  100 Samples/Month Capacity Requirements
                                                                change  in
                                No.  of
                             Instruments')
  Fraction

  VOAs
  Semivolatiles,  Pesticides,  PCBs
  Inorganics
NOTE:  The Contractor shall have the following  inst
(operational) at all times as a back-up system:
                          Quantity
                                      Type of
                                    Ins trument

                                       GC/MS
                                       GC/MS
                                        ICP
                                       GFAA
                                                      ;ailable
                                                iinents
   These instruments must be included in
In addition, the Contractor shall have an\in-no
and circuit boards to ensure continuous ope
holding and turnaround time

3.3.2  200 Samples/Month/CapXcity^ReqWrements
                                        dd^r's inventory of equipment.
                                          e stock of  instrument parts
                                           to meet contract-specified
                                        No.
  Fraction

   VOAs
   Semivolatiles,  Pest:
   Inorganics
                 Ldes ,
JBs
 Type of
Instrument

  GC/MS
  GC/MS
    ICP
   GFAA
NOTE:  The Sec?
one GFAA.
         idarv_Instrume-nt Requireme/it  for  200  Samples/Month  Capacity  is
     These instruments must be Nincluded in the bidder's inventory of
equipment/  In  addition,  the  Contractor  shall have  an in-house  stock of
instrumeiz(t  par^s  and  circuit  boards  to ensure continuous  operation to meet
contract-sp~e^if ietikholding and/turnaround times.

3.3.3   Instrument

     Further information^on instrument specifications and required ancillary
equipment may be  found in Exhibit D  and  other Exhibits in this  SOW.
 July,  1991
                                                               Page A-14
-------
Exhibit A
                                                     SOW No. XXX  -  Ambient Air
3.4  DATA HANDLING  AND  PACKAGING

     The  Contractor shall be  able  to  submit  reports  and
specified in Exhibit B.  To complete this task, the Co
required to:
                                                            /packages as
                                                            :or shall be
     •  Provide space, tables, and copy machines to
       requirements; and

     •  Designate personnel responsible for repor

3.5  LABORATORY MANAGEMENT CAPABILITY

     The  Contractor shall  have an organizati
responsibilities for each individual in the/m
sufficient resources for EPA contract(s)
operation.  To establish this capability,
personnel to carry out the following responsib^
Functions include, but are not limited to, the fo

3.5.1  Technical Staff

     Responsible  for all technical
preparation, sample analysis, sample
instruments.
                                                                            n
                                                            ined
                                                              to ensure
                                                         a successful
                                                         shall designate
                                                          the EPA contract.
                                  s of EPA oontract(s) (from sample receipt
                                 be\the primacy contact for EPA Headquarters
                                               logging, handling, and
                                                           act such as  sample
                                                            -shooting of all
3.5.2  Project Manager

     Responsible  for  overal
through data delivery) an
APO and Regional Technical

3.5.3  Sample Custodi

     Responsible  for/rec
storage).
3.5.4  Quality Assurance 0

     Responsib
reporting di

3.5.5  Doc;

     Res
Complete
Region or ot
                                         y assurance aspects of  the  data  and
                                   all  documents  generated are placed  in  the
                                  d are delivered to the appropriate EPA
                                 [nated by EPA.
July, 1991
                                                                     Page A-15
-------
                                  EXHIBIT B
                          DELI
July, 1991
-------
                                   EXHIBIT B
                    REPORTING AND DELIVERABLES REQUI
SECTION 1  CONTRACT REPORTS/DELIVERABLES  DISTRIBl

SECTION 2  REPORTING DESCRIPTIONS AND  ORDER  OF
      2.1  Updated Standard Operating  Procedu/es,
      2.2  Sample Traffic Reports
      2.3  Sample Data Package Summary (Oi
      2.4  Sample Data Package
      2.5  Results of Intercomparison  Study/
              Preaward Performance Evaluation (PI
      2.6  Complete Case File (CSF) Purge
      2.7  GC/MS Tapes (Organics
      2.8  Verification of Instrumfc
      2.9  Quality Assurance Plan
                                                                       Page  No.
                                                                        -1
                               tion Guide
                                 g Forms
SECTION 3  FORM INSTRUCTION GUIDE/DATA
      3.1  Volatiles-Canister
            3.1.1  Form Instruction
            3.1.2  Data
           Volatiles-Tjena:
            3.2.1  F
            3.2.2  Pata<
           SemivolatiT
            3.3.1  Form
            3.3.2_J)ata Repor"
      3.4
      3.2
      3.3
July, 1991
-------
Exhibit B
                                        SOW No. XXX  - Ambient Air
                                   SECTION  1

                  CONTRACT REPORTS/DELIVERABLES DIS
      The following Cable summarizes the contract
requirements specified in the Contract Schedule an
of each deliverable.  NOTE:  Specific recipient
to change during the term of the contract.  The
Contractor in writing of such changes when they/ oc£ur
                                                    eliverables
                                                        ribution
                                                      are^subject
                                                              the
           Item
               No. of
               Copies
  Schedule/and De Lively
                                                                 Distribution
                                                                (1)
                                                        (2)
                                       (3)
Updated Standard
Operating Procedures
(SOPs)
                                                         X
                                       X
*Sample Traffic Reports
                       ***3 days after
                       of last sample in
                   eipt
**Sample Data Summary
Package (Organic Only)
**Sample Data Package
including the Performance
Evaluation Sample (PES)
Results of
Intercomparison
Study/Preaward
Performance Evaulation
(PPE) Sample
                       35 days
                       last s
              receipt of
               SDG
Complete SDG File
                                    receipt
                                    SDG.
                                     data
                                  last sample in
*Verif ication of .
Parameters  (Metals Only)
                       15th day of January,
                      ^April, July, and October.
                                  X
GC/MS Tapes
Only)
(O
Retain for 365 days after
i^tar submission, or
submit within 7 days
after receipt of written
request by APO.
                                                                 As Directed
 ****QuaLity ^Assurance
 Plan   <^
                        Submit copy within 7 days
                        by written request by
                        APO.
                             As Directed
July,  1991
                                                       Page B  -  1
-------
Exhibit B
                                                SOW No
                                                                  - Ambient  Air
Distribution

(1)   Sample Management Office
(2)   Environmental Monitoring Systems Laboratory-La
(3)   USEPA Region

*     Also  required  in each Sample  Data Package.

**    Concurrent  delivery  of these  items  to all/recipients is required.

***   SDG is  a  group of samples within a  Case',  received /veir a period of seven
      days  or less and not exceeding 20 samp/les/   Data >£or/all samples in the
      SDG are due concurrently.   (See Exhibit A><£ask/lII/ for further
      descrip*-on).

****  See Exhibit E  for description.

NOTE:  As specified in the Contract
Supplies and Materials), unless ot
shall dispose of unused sample vol
earlier than 60 days following submi
Address
(1)
(2)
                                       edule in the IFB (
                                                     by
                                                           :ent Furnished
                                                          ,e Contractor
                                                        /containers no
USEPA Contract Laboratory Program
Sample Management Offj
P.O. Box 818
Alexandria, VA  222

For overnight deprive,

300 North Lee
Alexandria, VA

USEPA Environmental Mo
Systems Lab
P.O
Las
ATTN: /Dat?& Audit
                                                  ddress:
      For
                             e, use street address:
                                   er
July,  1991
                                                               Page B - 2
-------
Exhibit B
   SOW No. XXX - Ambient Air
(3)  USEPA  REGIONS:

     SMO, acting  on behalf  of  the  EPA APO, will provi.
     the  list of  addresses  for the 10 EPA Regions.
     Contractor with updated Regional name/address
     throughout the period  of  the  contract and
     recipients on a case-by-case  basis.
NOTE:  Specific recipient names and addresses
term of the contract.  The APO will notify th;
changes when they occur.
        le Contractor with
           provide the
                         the
tractor in writing of such
July, 1991
                  Page B -  3
-------
Exhibit B
                                                      SOW No.  XXX - Ambient Air
                                   SECTION 2

              REPORT DESCRIPTIONS AND ORDER  OF  DATA

    The  Contractor  shall  provide reports and other/de
the schedule specified in Section F of  the IFB,  "
required content and form of each deliverable is

    All  reports  and documentation shall be:

    •  Legible;

    •  Clearly labeled and completed in a^cor&ance  w|/£h /nstructions in this
       Exhibit;

    •  Arranged  in  the order specified  in this

    •  Paginated; and
     •  Single-sided.

     If submitted  documentation does \\pt\onfornf td tKe~-aWve criteria,
Contractor will be required to resubmite. sufctfi  documentation with
deficiency(ies) corrected, at no additioxialNzfostr  to  the  Government.
                                                           the
    Whenever  the  Contractor's—enquired to^submat or resubmit data as a
result of an on-site laboratory evaluation o\thrpugh  an  APO/TPO action,  the
data shall be clearly ma/ked^as^ADlkTIONAL DAtA" \nd  shall  be  sent to all
three contractual data /recipientsVs»e)\~Ta4SL-LV\and Region) .   A cover Letter
shall be included that/describes which  dataa^ebeing  delivered,  to which EPA
Case(s) the data pertZaiiy; and who^ rejjfuestTfed the/data.
     Section 3  of tfiis  Exhib^ yton]
properly completing allxdata  repc
required documentation ano^-cpntari
format.
                      ains  instructions to the Contractor for
                     ting forms to provide the EPA with  the
                       the required data  forms in EPA-specified
                                          each deliverable item cited in the
Contract Performance/Delivery Schedule  (see  Section F  of the  IFB "SCHEDULE
INFORMATION")/are specified\s  fallows  in this  Section.   Items submitted
concurrently/must be arrangedXin Vhe order listed.   Additionally,  the
components o^ each  item must b£ arranged  in  the order  presented herein.
2.1  UPDATE!
STAND?
OPERATIC
toCEDURES
2.1.1 The Contractor  sha^tiw/subjdit  updated copies of all required Standard
Operating Procedures  cSQPs)  t^nat were  submitted with the prebid Performance
 July,  1991
                                                        Page B -  4
-------
-\
       Exhibit  B
                                                 SOW No. XXX  - Ambient  Air
       Evaluation  (PES)  sample  results.   The updated SOPs must-addr^ss any and all
       issues  of laboratory performance  and operation identified fey the Contractor in
       the review  of  the  PES sample data and the evaluation
       Documentation.
                                                       der-Supplied
       2.1.2 The Contractor  must supply SOPs for the foll(

            2.1.2.1  Evidentiary SOPs.

            2.1.2.2  Sample receipt and logging.

            2.1.2.3  Sample and extract storage are/.

            2.1.2.4  Preventing sample  contamination/

            2.1.2.5  Security for laboratory and samp]

            2.1.2.6  Traceability/equivalency of standards
                                          /—»~^^^^
            2.1.2.7  Maintaining instrument  records—azyibound logboi

            2.1.2.8  Glassware cleaning.

            2.1.2.9  Technical and managerial Kevrs^w iof laboratory operation and data
            package preparation.
            2.1.2.10 Internal  revi<
            individual data package.
                            tontractuariy-r>auired QA/QC data for each
            2.1.2.11 Sample  anauys/s,  dat\ hkndTitig.  and\/ata reporting.

                                          documentSvCpntrol,  including case file
2.1.2.12 Chain-of-c
preparation.
; tody  ar
                               chain-(
                            [on/Self-inspection system, including:

                            -command for  data review;
                                      ring prfe-sjJsion and accuracy;

                  .Taxation parameters fpr identifying systematic errors;

                 Procedures to ensure jthat hardcopy data are complete and compliant
                       le requirement/ im Exhibit B;
       July, 1991
                                                                Page B - 5
-------
Exhibit B
                            SOU
                                                                  -  Ambient Air
          Demonstration of internal QA inspection procedi
          supervisory sign-off on personal notebooks,  in'te
          etc.);

          Frequency and type of internal audits (e.
          checks,  perceived trouble areas);
                                   [demonstrated by
                                   il  PE  samples,
          Demonstration of problem identification
          resumption of analytical processing
          (i.e.,  QA feedback);  and

          Documentation of audit reports (i
          corrective action,  etc.

    2.1.2.14 Data Handling.
                                                 spot
                          ing  from  internal  audit


                               xteftrnal) ,  response,
      2.1.2.14.1  Data Management procedures defined a^writt^tn procedures
      that are clearly defined for aLldatabases and file's-xused/'to generate  or
      re-submit deliverables specif;
      correction, deletion, storag
      and files.  Key areas of conce
      personnel and security,  demonst
      quality control.

      2.1.2.14.2  Data manually entered fr
      quality control proceclj*re'5-~snd error

      2.1.2.14.3  The re
      to data originally
      documented to al
      the following i
                                      y,  update,
                                     readable data
                                    ization including
                                  aceability, and
                       dcopy  must  be  subjected to
                         stimated.

                           f corrections  and updates
                         'or  resubmitted must be
                           Documentation must include
             Justifi
             Initials of ttv
             changes—aust be
             The
             submitted
           ale for the change;

                  the changes or changes.   Data
                when generating the deliverables;

      ion mus^Jie retained according to the schedule
       ^.verable;

          es must be reinspected as a part of the
          inspection process prior to submission.
           and not just the changes must be
       ger must approve changes to originally
liverables;  and
July, 1991
                                           Page B - 6
-------
Exhibit B
                                                SOW No.  XXX -  Ambient Air
              Documentation.of data changes may be reque
              auditors.

      2.1.2.14.4  Life  Cycle  Management procedures mu4t
      systems used to generate  and edit contract  de/i
      must be thoroughly  tested and documented pri

      2.1.2.14.5  A software  test  and acceptanc
      requirements, test  results,  and acceptance  c;
      followed, and available in written form
                                                       by laboratory
                                                              to  computer
                                                               systems
2.1.2.14.6  System changes shall not
systems generating deliverables.  Changj
development system and tested prior/to
                                                   directly^  to  production
                                                must b4 made  first  to  a
                                                lemefitatXion.
      2.1.2.14.7  Each version of the produc^iqn system will be  given  an
      identification number, date of installatiohxjdate^qf  last  operation,  and
      archived.
      2.1.2.14.8  System and oper
      maintained for each system.
      and an operations and mainte

      2.1.2.14.9  Individual(s) respo
      be identified:

          •   System operati
             training; a
                                       icntation shal
          •   Database

      2.1.2.14.10 Da/a

2.2 SAMPLE  TRAFFIC
       developed and
.elude a user's manual
                                            ,e following functions shall


                                          .eluding documentation and
                                            ry, data updating and QC.

                                      backup,  and archiving.
2.2.1  The original sample^-TO pag^^marked "Lab Copy for Return  to SMO" shall be
submitted  to  SMOwi t.bl.abora'Eqry  receipt information and  signed  in original
Contractor signature, for-^ach samgle ih> the SDG.

2.2.2  TRs /hall be submitted In SDG sets (i.e., TRs for all samples in an SDG
shall be c/iippCed together) ,\/ith\ an SDG Cover Sheet attached.
         /   7               \   \
2.2.3  The S4JG Cover Sheet shajll Contain  the following items:

     •  Labol

     •  Contract nv
July, 1991
                                                              Page B -  7
-------
Exhibit B
                                                      SOW NOxXXX - Ambient Air
       Sample Analysis Price  -  full  sample  price from contract;

       Case Number; and

       List of  EPA sample numbers of all  samples
       first and last samples received,  and their
                                                                        ing the
NOTE:  When more than one sample is received in/the/first or last SDG shipment,
the "first" sample received would be the, lowes/ sample number (considering both
alpha and  numeric  designations),  and the  "Ia4t'/sample/received would  be the
highest sample number (considering both alp)*a  and numeric /iesignati°ns) •
2.2.4  Each TR shall be  clearly marked w^th th« SDG
number of the first sample in the SDG.
the laboratory receipt date on  the TR.  The  TRNfor  the
the SDG shall be clearly marked  "SDG -  FINAL SAMPl
                                                         er  and  the  EPA sample
                                                         shall be entered below
                                                       j-ast  sample received in
2.2.5  If samples are received at thej.aboratory with mutt-i^-sample TRs, all the
samples on one multi-sample TR may/not nec~e"s-»acaj.ybe in the^same SDG.  In this
instance, the laboratory shall make, tha^«p4iropriate~niMye«-jjf photocopies of the
TR, and submit one copy with each SDG cVversRe^t.

2.3  SAMPLE  DATA  SUMMARY PACKAGE (Organ\c A\a^se^ Only)

2.3.1  As specified  in  the  Delivery Schedule, 
-------
Exhibit B
                                                      SOW No.  XXX - Ambient Air
                                                   cons
2.4 SAMPLE  DATA  PACKAGE

2.4.1  The sample data package shall be complete,
shall include data for analysis of all samples in an

    2.4.1.1  For  VOA  and SV,  these  samples inc
    reanalyses, blanks,  and  laboratory control s

    2.4.1.2  For inorganics,  these samples include analytical and field
    sample  reanalyses,  blanks,   spikes,  dupl/ca^es,  and  laboratory  control
    samples.
          This  document
      shall contain:
      Number;  SDG Numb
      numbers in alpharv
      with  laborato
      problems enco
2.4.2  The sample data package  is divided  ^

       Cover Page;

     •  Sample Data (Results);

     •  Quality Control Summary;

     •  Raw Data;

     •  Preparation Logs;  and

     •  Sample TRs.

     2.4.2.1  Cover Page
                                                          s follows:
                                                   sver Page."  The Cover Page
                                                  /code;  contract number; Case
                                              ?n cover page of SOW); EPA sample
                                            EPA/sample number cross-referenced
                                               its,  describing  in detail  any
                                  £ssing the samples in the data package.
          The Cover Page  snail contain the following statement,  verbatim:

      "I certify" that  tnTts^data "packages is  in compliance with  the terms and
      conditions o^~tA«^conttact,  both^/technicaliy  and  for  completeness, for
      other /tharf the condr&ions\detailed above.  Release of the data contained
      in  tnis /hardcopy  dataV package  has been  authorized by  the Laboratory
      Manager/ or  the  Manage^'s\, designee,   as  verified  by  the  following
      signature."
               star
      Laborato^
      the signer's""
                         shall bd  directly followed  by the signature  of the
                         or mis /designee with a typed line below it containing
                           'tittle,  and the date of signature.
July, 1991
                                                                    Page B - 9
-------
Exhibit B
 SOW No^XXX -  Ambient Air
      In the event that the Laboratory Manager cannot va
     for each sample, he/she must provide a detailed
     associated with the sample(s)  on the Cover Page.

     2.4.2.2  Sample  Data
    Ldajze all data reported
            of the problems
       2.4.2.2.1  Volatiles  Sample data  shall be'abranged in packetsNwith "
       Organic  Analysis Data  Sheet  (FORM  I  VGA, /including  FORM I
       followed by  the raw data  for  volatile/samples.   These sample  packets
       should then be placed in increasing EP£( sample numjz^el^order,  considering
       both letters and numbers in ordering
       NOTE:  FORM I VOA-TIC is  the tabulat
       for  up  to  10  organic compounds  that
       standards  and are  not  listed  in  Exhil
       Chemical    Abstracts   Service    (CAS)
       identification, and  estimated concentration.

          2.4.2.2.1.1   Reconstruc
          sample or sample extract!1

          2.4.2.2.1.2   RICs  must be\ normalized
          component, and must contain tne fVlLowi

             •   EPA sample number;
                          /^^^,
             •   Date and/rime of a
      ighest probable match
     rrogates and  internal
           It includes  the
       Number,    tentative
            (RIC)  for  each
        largest  nonsolvent
header information:
          2 .4.2 .2 .1. 3\Intfecna4.  standards and surrogate  compounds are  to  be
          labeled with tke names/of compounds, either  directly out from  the
          peak, or  on a print-out\Qf retention times  if retention times  are
          printed^-ever—the peak>

          2.4/2.2/rl74~~~~~"Quanti>t^.tion Report:   The complete data  system report
          must /be includedXin  aJ-1  sample data packages,  in addition  to  the
           Reconstructed  ion  chromatogram  for prelimiary  identification and/or
          /qua/htitation using  ^either  the  automated  or  manual  data  system
          pros^dures.  The complLet^ data system report shall include all of the
                    n listed belo*
                  iPA sample Dumber;

                  Date ahd time  of analysis;
 July,  1991
                Page B - 10
-------
Exhibit B
                              SOW No. XXX - Ambient Air
                 RT or scan number of identified target

                 Ion used for quantitation with measur

                 Copy of area table from data syste

                 GC/MS instrument ID; and
             •   Laboratory file ID.

          2.4.2.2.1.5   In all instances wher;
          edited,   or  where  manual  integ
          performed,  the  GC/MS  operator  s
          procedures  by initialing and da

          2.4.2.2.1.6   Target Compound Mass
          compound identified,  the following
          package:
                                    tern report has been
                                    titation  has  been
                                  'uch  edits  or  manual
                              geat made  to  the report.

                                'or each sample, by each
                                 included  in  the  data
                 Copies of the raw i^pecB?a-^and^copies  of background substracted
                 mass spectra of t4rge^cpMounds~~tts-e«d_in  Exhibit C that are
                 identified   in   ttte \ampTe~~-~-and  corresponding   background
                 subtracted target compouhd•stanaaEcmasS-s^ectra.  Spectra must
                 be labeled with  EPA  sampleNnumoer/ laboratory file ID, date and
                 time of analysis,  and GC/MS\Lnslcrument ID; compound names must
                 be clearly marked on all^pect?ra.
          2.4.2.2.1.7
          Matches:   For
          shall be  incli/de
Te^tativelyNIdentifieck Compound Mass Spectra and Library
  ch/s'amp4ve, \>y each compound identified,  the following
    in the\ dalta~~pa^jcage:
                         )f  mass /speieftra  ^af  org'anic  compounds  not listed  in
                            Tentatively  Identified Compounds, with associated
                                :tr/ (three best matches), labeled as above.
       2.4.2.2.2  "Volatile
            Data:
                              l Calibration:  All initial calibration data must
                          all^analysesxaysociated with the SDG.   When more than
                mitial   ca^iibration  is  performed,   the  reconstructed  ion
                        and quanoitation reports and each  type  of  form must be
             'in chronological\order,  by instrument.

                 ;ial Calibratin  ^ummary (FORM VI );

                        -andaxd Area and Retention Time Summary (FORM VIII);  and
July, 1991
                                            Page B - 11
-------
Exhibit B
                          SOW No/tv^XXX  - Ambient  Air
             Volatile   standard(s)   reconstructed   ic
             quantitation reports  (or legible facsimiled)
             point)  calibration are labeled according tc
             2.4.2.2.1.4.   Spectra are  not required.
                                /chromatograms    and
                                   the  initial  (five
                               parfc\2.4.2.2.1.2  and
          2.4.2.2.2.2   Continuing Calibration:
          calibration  is  performed,  the reconst
          quantitation  reports  and   each  typ/i
          chronological order,  by instrument /Lf
          used.
                           more than
                         :ed  ion  chromatog^ams
                        if   form  must  be  p\}t    n
                       acre than  one  instrument  is
              •   Continuing Calibration Sv
                     (FORM /II/;
                 Internal Standard Area and TRe^ent^W Tj/me Summary (FORM VIII);
                 and
                 Volatile  standard(s)
                 quantitation  repor
                 (five point)  cali
                 and 2.4.2.2.1.4.
             reconstructed\4on  tbroma to grams   and
            or  legible  facsim^i^s) /for the  initial
         ation~~are--lalieled accordirr4  to 2.4.2.2.1.2
                        ~reqt
       2.4.2.2.3  Semivolatiles:  Sample data sWall: be arranged in packets with
       the  Organic  Analysis Data SheetVFORMA SV,  including  FORM I SV-TIC) ,
       followed by  the raw data for semivblatlle/samples.  These sample packets
       should then  be placed in increasing\PA smple number order, considering
       both letters and  nunjkefs~"iTi ordering
        NOTE:  FORM I SV-
        for up  to  10 o
        s tandards  and are
        Registry Numb

           2.4.2.2.3.'
           sample or  samp

           2.4.2.
           comp
                  lis
                    are
    cuc^ed  total  ion chromatograms
extrac/l
    ta
comppu
    d  In—£xhib
    identif iea.tio
  the highest probable match
/not surrogates  or internal
 (TCL) -   It includes the CAS
and estimated concentration.
                                  (RIC)  for each
         be\normalized  to  the  largest  nonsolvent
   contact*} the^ following header  information:
 July, 1991
                                         Page B - 12
-------
Exhibit  B
                                                      SOW No. XXX - Ambient Air
          2.4.2.2.3.3   Internal  standards and  surrogate7 compounds are  to  be
          labeled with  the names  of  compounds, either/directly out from  the
          peak, or  on a print-out  of retention times/if Cre tent ion times  are
          printed over the peak.

          2.4.2.2.3.4   Quantitation  report:   The
          must be  included in  all sample  data p^
          reconstructed ion chromatogram for pre
          quantitation utilizing  either  the  automated
          procedures.  The complete data systei/re/port shall include all of  the
          information listed below:

              •   EPA sample number;

                 Date and time of analysis"?

              •   RT or scan number of identified

              •   Ion used for quantitation with measure
                                  r
                 Copy of peak area< tabJLe_ from data"

                 GC/MS instrument ID\ani

              •   Laboratory file ID.

          2.4.2.2.3.5   In ali—instances whexe "hhe data  system report has been
          edited,   or  wheafe  manual  integra\ion\ or  quantitation  has  been
          performed,  the/GC/MS~^QperYtor  must\ide\tify  such edits  or  manual
          procedures by/initial ing^ arid^d^Cing thk/hanges made to the report.
          2.4.2.2.3.6,
          compound vuent
          package:
        Target Codpoyfid M>&sSpactra:  For each sample, by each
        Lfied,  /he/followin^fehall be  included  in  the data
                 ma
July, 1991
Copies or^She rawxspectra and copies  of background substracted
       ectra oC tar^at compounds listed  in Exhibit C that are
                   e  sample   and   corresponding  background
                  com^ojand standard mass spectra. Spectra must
                    sample  number, laboratory file ID, date and
                  and GC/MS instrument ID.  Compound names must
                  on all spectra.

                   Identified Compound Mass Spectra and Library
                  ,  by each compound  identified,  the following
                  data package:
                                                  Page B  -  13
-------
Exhibit B
                                            SOW
                                                                  -  Ambient Air
          2.4.2.2.3.8   Copies of mass spectra of organic Compounds not  listed
          in Exhibit C,  Tentatively Identified Compounds,  w-^h  associated best-
          match spectra (three best matches), labeledas/^above
       2.4.2.2.4  Semivolatile Standard Data

          2.4.2.2.4.1   Initial Calibration:  A
          be included for all  analyses  associa
          one  initial   calibration   is  per
          chromatograms and quantitation reports'' and
          put in chronological order,  by i
                                       Bed,   the
                                      nent
                 Initial Calibration Si

                 Internal Standard Area and
                 SV);  and
                                   0
initial calibrationMata Must
 ith the SDG.   When morfe/than
          reconstructed   ion
           e  of  form must be
         lows:
                                                 Summary  (FORM VIII-
          2.4.2.2.4.2   Semivolatil
          and quantitation reports Aor
          point)   calibration  are\ lal
          Spectra are not required.
                             Tjdard(s) reconstructed ion chromatograms
                            legiBTe—§acsjLmiles) fc^irthe initial (five
                                      2747272T3-T-2, and  2.4.2.2.3.4.
          2.4.2.2.4.3   Continuing Cali'bra
          calibration is  performed,  the\ reconstructed
          quantitation  reports  and  each
          chronological  orj%€r~, "By-^ instrume
          used,  as follow>
                                       When more than one  continuing
                                              ion  chromatograms  and
                                     e   of   form  must  be  put   in
                                        more than  one  instrument  is
                 Contii
                 Internal Standard
                  Calibration Sumsoary f^ORM VII-AASV);

                          :ea anaKfletfention Time Summary  (FORM VIII-
2.4.2.2.4.4  ^5«mivola
and quantitation r
point)
2.4
     2.4.
       2.4.2.3. I>xVola
       following fo
July, 1991
                                 ile standard(s) reconstructed ion chromatograms
                                      legible facsimiles) for the initial  (five
                                        eled  according   to   2.4.2.2.3.2   and
                                are\not required.

                                 ample data  shall  be submitted  with  FORM  I  -
                                    samples  in the SDG, arranged in increasing
                                  tber order.
                         The quality control summary shall contain the
                                                          Page  B -  14
-------
Exhibit B
     SOW No. XXX - Ambient Air
       NOTE:   If more  than one  form is  necessary,  duplicate forms  must be
       arranged-in chronological order by date of analysis/or instrument.

             Surrogates Summary  (FORM II-VOA);

             Method Blank Summary  (FORM  IV-VOA);

             GC/MS Instrument Performance Check/(F

             Internal Standard Area and  RT Si

          The quality control summary  shall,

          NOTE:   If more  than  one form
          arranged in chronological order

             GC/MS Tuning Data:
   (FORM_VIII-VOA)

           e  following:

      dj/plicate  forms  must be
        lysis or  instrument.
                 GC/MS Tuning  -  BFB-4ata^  for  each 12-{
                 arranged in chronological
                 system utilized;

                 GC/MS Tuning and Mas
                 Bar graph spectrum,  labe
                 and
               riod,  shall  be
                for  each GC/MS
          'ORM V) ;

,n 2.4.2.2.1.2 and 2.4.2.2.1.4;
             Blank Dat
             by instr;
             both o
             Laboratory
   2.1.2.  and 2.4.2.2.1.4.

   .ged  in chronological order
 1  be  arranged in packets with
Sheets (FORM I VGA  and  FORM I
for volatile samples;  and
                                        heet for target compound results (FORM
                                         is not required.
                                    chromatograms  and quantitation  reports  or
                                   (GC/MS), labeled according to 2.4.2.2.1.2 and
                                  ctra are not required.

                                  ta:  The quality control summary shall contain
July, 1991
                   Page B - 15
-------
Exhibit B
                                              SOW No^XXX  - Ambient Air
                                                                 forms must  be
                                                         iplicate forms must  be
                                                              or instrument.
                                                               eriod,  shall  be
                                                            :ent for  each GC/MS
NOTE:   If more  than one  form  is necessary,  di,
arranged .in chronological order.

      Surrogate Percent Recovery Summary  (FOE

      Method Blank Summary  (FORM IV  - SV);

   •   GC/MS Instrument Performance Check/(FG

      Internal Standard Area and RT  Sutoma/y  (FORM/

   The quality control summary shall
                                  t
   NOTE:   If more  than  one form is
   arranged in chronological order by dat

      GC/MS Tuning Data:

          GC/MS Tuning - D
          arranged in chrori
          system utilized;

          GC/MS Tuning and Mass
                 Bar graph spectrum, label
                 and
                 Mass

              Blank Da#a
              by ins t
              both o
              TIC) ,
    - DFTPP  (FORM V  SV);

in 2.4.2.2.1.2 and 2.4.2.2.1.4;


     1.2  and  2.4.2.2.1.4.
        2.4.
        following^forms^
 July, 1991
                                          cranged in chronological  order
                                         fi.1 be arranged in packets  with
                                        sheets (FORM I-SV  and FORM  I-SV-
                             raw data for semivolatile samples;  and
                                  feet  for  target  compound results (FORM
                                   not required.

                             chromatograms  and quantitation  reports  or
                            (GC/MS),  labeled according to 2.4.2.2.1.2 and
                        jSpelctra  are  not  required.

                            The quality control summary shall contain the
                                                             Page B - 16
-------
Exhibit B
                                        SOW No. XXX  - Ambient Air
       NOTE:   If more  than one  form is  necessary,
       arranged .in chronological order.
                                         du'
Initial and Continuing Calibration Verif
CRQL Standards/Linear Range Standards
Blanks [FORM IV - AAIN]
ICP Interference Check Sample  [FORM/V^ AAIN]
Spike Sample Recovery  [FORM VI -
Analytical Spike Sample Recover;
Duplicates [FORM VIII  - AAIN]
Laboratory Control Sample  [F0RM
Method of Standard Additions [
ICP Serial Dilutions [FORM XI  - AAI
Instrument Quantitation Limits (Quar
ICP Interelement Corr£ction~-Fa«£Qrs (Annual)
Analysis Log (A) [FORK Xl
Analysis Run Log (B) [FORM XV  - AA1N]
Linear Range Standards (Qu\rte\l^) /FORM XVI  - AAIN]
                              forms must  be
                                                              [FORM II -  AAIN]
                                                                II -  AAIN]

                                                                 XIII -  AAIN]
      2.4.2.4
    Raw Data
       2.4.2.4.1  For eacft reported
       data from the ins/crugient us^ed
       data for  quart
       shall  contain
       including tho^e
       Limit  (IQL).
 falue, the\Conbractor shall include all raw
      Itain the sample values (except for raw
tions oiXinstrument  parameters).   Raw  data
               ed  for  the  sample  results,
 'may faH^b^low the  Instrument Quantitation
   and ICP instruments  must provide legible
                     tent/
       hard copy of tf
       printer tapes, etc
       readout must be inclui
                     .-time  instrument readout  (i.e., stripcharts,
                    photocopy of the direct sequential  instrument
       2.4.2.4^2  The^orderxof  r^w  dd'ta  in  the  data  package  shall  be:
       Volatiles/^Semivol^atiles,  and Inorganics.    All  raw data shall  include
       concentration units tor I<^C/MS and  ICP  and absorbances  or concentration
       unyts /or GFAA.

                  Organic and ilnorkanic raw data must be labeled with EPA sample
              ancl-Nappropriate codas as shown in Tables B-l and B-2 respectfully,
                Lfy un^cjuivoc^lly/the following:
July,  1991
                                                       Page  B -  17
-------
Exhibit B
                    SOW Nov^XXX - Ambient Air
       •  Calibration standards,  including source and preparation date;

       •  Initial  and continuing  calibration blanks a^id prepa>ation blanks;
          Initial    and   continuing   calibratioi
          interference  check samples,  CRQL standa;
                    .rerificat
                   iud linear rat
                   st
^ndards,
    .ard;
          Diluted and undiluted  samples  (by  EPA/sample number) and all weights,
          dilutions,  and volumes used  to obtain /the reported values.   If the
          volumes,  weights,  and dilutions, ar/ cctasistent^fsr  all samples in a
          given  SDG,   a  general  statemen/  outlining'  t^hese  parameters  is
          sufficient;
          Duplicates;

          Spikes    (indicating   standard    solut^
          concentrations,  volumes given SDG, a general
          parameters  is  sufficient;

          Instrument used, any ins
          apparent  anomalies  on th\  m<
          voided  or data not used to
          explanation;
          ana
                                final    spike
                      statement outling these
                          orrections or other
                          Including all  data
                          and a brief written
          Data and EPA sample  number for
          and sequentially xitlenTrified on
          All  calculati
          percent reco
          linear  fit;

          Time and date
          if they  c
          automatically
          on all  raw data
          and  blanks-;—as well
               ICP,  and GFAA analyses clearly
               data;
                  cal  spike  data,  including
                   ,  slope  and  y-intercept of
                              and
on
         Instrument run logs can be submitted
 nformation.    If  the  instrument  does  not
me of analysis,  these must be manually entered
  al  and  continuing calibration verification
      ference  check samples and  linear  range
                            for\GFAA analysis.
                                   following:
July, 1991
                                  Page B - 18
-------
Exhibit B
SOW No. XXX - Ambient Air
                                   Table  B-l

                       Codes for Labelling Organic
                                  	/s
                                                                       x/
Sample	/./.... /\ .  .   .  XXXXX
Re-analyzed Sample	/./..././..   XXXXXRE
Sample Analyzed at a Dilution	/. ./..../../...   XXXXXDL

Laboratory Control Sample Number  .  .  .   • >x. •  /X/.  / .  .  .  .    FLCS##
  Fraction  (V for volatile and S for semivolabile)
  LCS   	-^X  '^X •  •   •  •  LCS
  Suffix  (Characters/Numbers of EPA Sample Number)  X\ .  /X^.   .  .   ##

Blank
  Volatile Method Blank   .  .  .  A  . V--*^.  •  r~7^T~^-^^.^ .  .    VBLK##
  Volatile Storage Blank  ....  .V  \. ^^^77.  -^_^^-  7 •  •   VSBLK##
  Volatile Instrument Blank   .  .  .  \-" \ • •  / ./^~~^~rj.  .  -   VIBLK##
  Semivolatile Method Blank   ....  \  . \ •/•  /	    SBLKy/#
  Semivolatile Instrument Blank   .  .  . \ .V ./	SIBLK##
Standards 	
  Fraction (V for volati^s
  Standard  ....
  Concentration (/i{
                 inje
                             and S for semivoratiles)
                           •olatilfis and
                           for s
           FSTD###
           .  .  .  F
           .  .  STD
July,  1991
              Page B - 19
-------
Exhibit B
                                                      SOW No/xXXX -  Ambient Air
                                   Table B-2

                      Codes for Labelling  Inorganic
Sample
Duplicate
Sample Spike	/• /	XXXXXX?
Analytical Spike	-..././...  .^.  .  .  XXXXXXA
Instrument Calibration Standards:
  ICP and GC/MS    	/  S/or SO f/r blank standard
  Atomic Absorption   	/./.../  SO,  S10,    etc.
  Initial Calibration Verification  .  .  . ^ .  :\^ .  / ./.	ICV
  Initial Calibration Blank    	-^X.  .>A  /	ICB
  Continuing Calibration Verification   .  . .  /X.  .  . C .	CCV
  Continuing Calibration Blank	;-\  .  /X^ ....  CCB
Interference Check Samples:
  Solution A	
  Solution AB   	.  .          —-^ •  •  •  •  •  •  ICSAB
  CRQL Standard for AA	\  . \~-r-^__.  . T^T^T"-:--^.  .  .  .  CRA
  CRQL Standard for ICP    	\  A.  .T~"?7. /-»-^_- / •  •  .  '  CRI
Laboratory Control Samples	\  \. . / . /.    .  ^~^.          LCS
Preparation Blank	"	\  \ . /  /	   pg
Linear Range Analysis Standard   .  .  .  . \ . ;  ./.	LRS
Notes:
  1.
When an analyticay
samples, the  "A"/
added to the  E
duplicate mus
  2.
  3.
The numeric su
the true value of
                                          erformed/on samples other than field
                                               surfixes  must  be  the last to be
                                                 .nee,  an analytical spike of a
                                     the "S" suffix for the standards indicates
                                 mtration  of  the  standard in
ICP ca 1 ibra-CTon
concentration
calibpationstanda^ds unless all'
at tfre sXme concentration^
                                        pnsist of several analytes at different
                                         'numeric  suffix  can  follow  the  ICP
                                         e analytes in the standard are prepared
  4.
    CRQL standard for AA\is \considered to be a calibration standard if it
    a frart of the calibration  curve,  thus  it  must be formatted like any
       AA  is  nt>4;  useJ
                 The  "C^A"/format must  be  used if the CRQL standard for
               spo establish the calibration curve.
July, 1991
                                                             Page B - 20
-------
 Exhibit B
                                                      SOW No. XXX - Ambient Air
        •   Sample weights  and volumes;

        •   Sufficient  information  to  identify  unequivocally which  QC samples
           (i.e.,  laboratory control  sample,  preparation blank)  correspond to
          each batch prepared;  and

          Comments describing any significant sam
          occur during preparation.
     2.4.2.6  Sample Traffic Report

          A legible copy of the sample TRs a:
        as  described in part 2.2 of this E:
        SDG.   The  TRs shall be arranged i
        considering both alpha and numeric'

2.5  RESULTS OF INTERCOMPARISON/PERFORMANCE EV,

2.5.1   The  reporting of analytical results for
Performance Evaluation (PPE) sample/a
in  part 2.3 for  reporting of sample^ data.
through the exact  same  process as
                                                                          which
                                                             shall be submitted
                                                             the  samples  in the
                                                           sample number  order,
                                                           'LE ANALYSES

                                                         jarisdja  Study/Preaward
                                                              rements specified
                                                       sample  shall be  carried
                                                .and fieldsample.
2.6  COMPLETE  CASE  FILE  PURGE

2.6.1  The Complete SDG  File
or generated for a specific
as a deliverable.   These ite"ms
items shall be submitted/aid*
(see Exhibit E for desc/ip
These items include, b
tracking records,  analysts'  log!
records,  computer  priivtputs,
(including instrument coridi^tio
                              package includes/all laboratory records  received
                                 that have not been previously submitted to EPA
                              shaPlbe submieted\o EPA as a deliverable.  These
                                j.th\their DocuBjentVInventory Sheet FORM AADC-2
                                           numberi/ng and inventory procedure) .
                                               le tags,  custody  records, sample
                                             bepch sheets,  instrument  readout
                                               ies,  instrument  logbook  pages
                                   correspondence, and the document inventory.
                            on
                            not limited to,
                                      Pag
                                aw /data si
2.6.2  Shipment of the Cot
courier, priority mail or
provided
and transmitt?
documents
however,
transmits

2.7 GC
                           Lete
                          eqx
2.7.1
tape,  in
       The
         appropri
July, 1991
                                    File package by first class mail, overnight
                                     ^is acceptable.   Custody seals, which are
                                   shipping containers and a document inventory
                                 The^oi/tractor is not required to maintain any
                                  submission of the Complete SDG File package;
                                Maintain  a copy of the  document inventory and
                                  all  raw and processed GC/MS data on magnetic
                                manufacturer's format.  This tape must include
                                                                   Page B  - 21
-------
Exhibit B
                                                     SOW No/^XXX  - Ambient  Air
data  for  samples, blanks,  laboratory control  samples,/initial calibrations,
continuing calibrations,  BFB,  and DFTPP, as well  as all laboratory generated
spectral  libraries and  quantitation  reports  requir/d £p  ge~nerate  the data
package.  The Contractor shall maintain a written refe^en/e rragboolc^Gf tape files
to EPA sample number, calibration data,  standards, blanks, and la^pratcJtv control
samples.  The logbook should include EPA sample numbers and standard andxljlank
ID'S, identified by Case and SDG.

2.7.2  The Contractor is required to retain th4 Gtf/MS tapes for 365 days  after
data  submission.   During  that  time,  the Contractor  sh£!ti submit  tapes and
associated logbook pages within  seven  days  .after receipt or a written request
from the APO.
2.8 VERIFICATION  OF  INSTRUMENT PARAMETERS

2.8.1  The Contractor  shall  perform and report
by methods  specified  in  Exhibit D  and  E for
instrument used under  this contract,—J'or the
the  Contractor  shall  also  repo:
(including method of  determination^
Annual Verification of Instrument Pa]
submitted in  each SDG data  package.
Quarterly Verification of Instrument Pal
to determine those values reported.

2.9 QUALITY ASSURANCE PLAN
quas^erly
each ty$e
   instrum
2.9.1  The Contractor
describes the procedure
data  integrity,  vali
systems are maintain*
detect  problems  t'
procedures which keep"1
of the measurement proce
and legally  defensible.

2.9.2  The  QA
obj e c t ive s,  /un
achieve the
pertainin
The QAP
request
                                                           erification of  IQLs
                                                          anoXmodel  number  of
                                                           tation and methods,
                                                           correction  factors
                                                            integration  times.
                                                          current year shall  be
                                                          rms.   Submission  of
                                                      include  the raw data  used
                                                     Assurance Plan (QAP) which
                                                  ieve the following:  maintain
                                                   that analytical measurement
                                                'stability and reproducibility;
                                           and" established  corrective  action
                               ~icAl process  reliable;  and document all aspects
                                 ;r to provide  data which are technically sound
                               in s>ecifi7c terms,  the  policies, organization,
                                .es,  and/specific  QA/QC  activities  designed  to
                                 :ents in this contract.  Where applicable,  SOPs
                                  be  included or referenced as part of the  QAP.
                                   -site laboratory evaluation and  upon written
 July,  1991
                                                                    Page B -  22
-------
FORM INSTRUCTIONS GUIDE,
ORTING FORMS
-------
Exhibit B
                       SOW No. XXX - Ambient Air
                                   SECTION 3
3.1   VOLATILES - CANISTERS

      This section includes specific instructions/for,
required forms for volatiles utilizing canister.
specific to a given function.  These instruction's
following order:
            General Information and Header

            Cover Page [COVER PAGE - AAVC

            Analysis Data Sheet [Form I -

            Tentatively Identified Compounds  [Form, II ^

            Method Blank Summary [Form III - AAVC]
            GC/MS Instrument
            AAVC]
            Initial Calibration Data
            [Form V - AAVC]
            Internal Stand
            AAVC
                           alibration [Form IV -


                   ng Calibration Check


                   Times Summary [Form VI -
            Canister C^rt

            Sample

            CompletT

3.1.1 General Information
                    •c]

                    AADC-1]

    ) Document Inventory Sheet [FORM AADC-2]

    ,er Information

     ^prms^presented in Section IV have been
with the^ycomputer-readable data format specified
 iary and Format for Data Deliverables in
   The specific length of each variable for
  ^smission purposes is given in the Data
    :ormation entered on these forms must not
     given on the form, including such
   as Lab Name and Lab Sample ID.
July,  1991
                                     Page B-l/VC
-------
Exhibit B
                                                SOW
                                                            rtv
                                                                  - Ambient Air
      3.1.1.2  Note that on-the hardcopy  forms  (Section
      provided for entries is greater  in  some  instance, '
      prescribed for the variable as written to  disk
      Greater space is provided on the hardcopy  fo
      clarity.
3.1.1.3  Values must be reported on  the ha/dc
individual form instructions  in this Sect/on
concentrations of volatile organic targ
two significant figures if the value i
Values can be written to the  diskette
exceed the field specification as gi
discussed in "Record Structure", pa^agrapii  5 of/ExKibit
                                                        the  space
                                                        the  length
                                                          chibit H).
                                                                 visual
                                           en
                                              iLe  in
                                                  the
                           e
       example,  results\£or
impounds must be  reported to
          r equal  to  10.
      format that  does  not
        d specifications and
            H.
                                              gr/ater  tha
                                              any/
                                                       iCOJ
      3.1.1.4  All characters which appear on the data
-------
Exhibit B
                                                      SOW No. XXX - Ambient Air
            3.1.1.6.2   The  -"Contract"  is the number of t.
            which  the  analyses  were  performed.   In the
            laboratories  operating under a corporate-w,
            contract number entered  shall be that of /he
            regardless  of the facility performing t
            3.1.1.6.3  The  "Lab  Code"  is  an alpha
            6 letters, assigned  by  the EPA,  to
            in data processing.   This  lab code
            the time a contract  is  awarded,  a;
            Contractor, except at the  direct!,
            name or ownership occurs at the
            remain the same until the  cont
            another lab code assigned  by
                                       contract under
                                    of multiple
                                  Contract,  the
                                           contract,
                                         5.e  Lab Code) .
            3.1.1.6.4  The  "Case No."  is  the
            associated with the sample, and
                                                    to
                                                    id
                                                    at
                              not be  modified by the
                                     If a change of
                                   lab code will
                                     by the  EPA to use
                   repor
Case number
,e Traffic Report.
            3.1.1.6.5  The  "SDG No."  is  the  Sample  Delivery  Group number.   The
            Sample Delivery Group ^SDGT~itttmber^ist;he  EPA  Sample  Number of the
            first sample received 4n  Ghe__SDG.  WherT~sw«tal  samples are
            received together  in thk  frrTTlJDe-shipment, th£ SDG  number shall
            be the lowest sample numb\r  (^consideri^(g~Tx>ttr--alpha and numeric
            designations) in the first^roo^ o/f s/amples received  under the
            SDG.
               \   \7  7
            3.1.1.6.6  The
            performed und'
            to be analyz
            enter SAS
            according
            have addi/tio?
            on all
            "SAS N
            No.  while o
            is the>EPA^assigned number for analyses
   Specia^XAnalytical Services (SAS).  If samples  are
         ;AS\only and Reported on these forms,  then
   id leavte GdseTkK blan^/  If samples are analyzed
   2 "Routine Analytical Services" (IFB) protocols  and
   SAS r^quifremehi^, U/st both Case No. and  SAS No.
   If th4 analyses haver no SAS requirements,  leave
             Some samples in an SDG may have a SAS
,ers do not.
                                        number of the SOW by which  the
            coptract laboratory  is\analyfcing the samples.

                 ie "EPA Samole No." is the other information common to  most of
                . This number NappeNars either in the upper righthand  corner of
                or as the leftNcolumn of a table summarizing data from  a
         :>er
-------
Exhibit B
                                                                                    r
                                   SOW
                                                                  - Ambient  Air
            3.1.1.7.1  All samples, spikes, blanks, and/standards  shall  be
            identified with an EPA Sample Number.  For/fieid^ samples,  the EPA
            Sample Number is the unique identifying
            Traffic Report that accompanied that st

            3.1.1.7.2  In order to facilitate dat
            sample suffixes must be used:
            XXXXX

            XXXXXRE

            XXXXXDL
            EPA sample numb

            Reextracted a

            Sample anal
            3.1.1.7.3  For standards, the foll>
            be used as the "EPA Sample No."

            •     VOC standards prena^ed in canisters
                  VCSTD###, where 0# is
                  standards in can
        le

    ary dilution

   tification scheme must
                               entration
           Identified as
      irt^ppb of volatile
       ', 050, and 100) .
                  For volatiles-caniscer
                  shall be used to
                                  the
      lowing scheme
Number".
  Name
CAL 1 Poij
CAL 2 Point
CAL 3 Poit
CAL
CAL
    '  /
       .4  As
                                                            EPA Sample Number
                                                                VCSTD1###
                                                                VCSTD2###
                                                                VCSTD3###   '
                                                                VCSTD4###
                                                                VCSTD5###

                                 :or/the blank identifiers, these designations
                                ie jcombined with other information to uniquely
                                  :andard.
                       :il.e s - c anis^t e r
                  The  "EPA^Sample
                          ie l^boratoi
                  two - charaxte r\' ## "
                      inks shall be identified as VCBLK##.
                     mifet be unique for each blank within an
                       ist achieve this by replacing the
                   terminator of the identifier with one or
                  two characters ior numbers, or a combination  of  both.   For
                  example, posaiblte identifiers for volatiles-canister  blanks
                  would be VCBLK1,) VCBLK2,  etc.

      3 .1.1. o\S e ver-a_l other pieoes of  information are  common  to  many of the
      Data Repor-ting Fo^ms. /Che-se include  Lab Sample ID,  Lab  File ID,  SOW
      No., Date Receded, o^te/Extracted, etc.  Following  is a brief
 July,  1991
                                                  Page  B-4/VC
-------
Exhibit B
                      SOW No. XXX - Ambient Air
      description of each of these entries.

            3.1.1.8.1  "Lab Sample ID" is an optional /laboratory-generated
            internal identifier.  Up to 12 alpha-numeric  characters may be
            reported here.  If the contractor does jtot/have^a Lals^Sample ID,
            this field may be left blank.
            3.1.1.8.2  "Lab File ID" is the labc
            GC/MS data system file containing
            particular analysis.  Up to 14 alt
            used here.
                     ry-generated nante^of
                [formation pertaining to"
                .-.numeric characters may be
            3.1.1.8.3  "Date Received" is ifhe /date  of/san
            laboratory, as noted on the Trafftc^Report
            should be entered as MM/DD/YY.
                          >le receipt at the
                          .e.,  the VTSR).   It
            3.1.1.8.4  "Date Extracted" and  "Date^Analy:
            in a similar fashion.  For pesticide/PCB
            analysis should be the date of the first
            The date of sample receipt
            and analysis dates to <-ensi*ce^j:hat contr
            exceeded.
                             should be entered
                               the date of
                                s performed.
                ompared witn^he extraction
                           ding times were not
            3.1.1.8.5  "Instrument ID"
            particularly those containirifi ca^ib
            used by the laboratory must includ
            manufacturer and/tnr-*pde 1 of th
            additional characters that diffei
            the same ty
               on/to many of the forms,
                 ation data.   The identifier
                 some indication of the
                 £rument,  and contain
                   te between all instrument of
in,
     jratory.
            3.1.1.8.6/"GC Column-/ and_J!ID  (?
            forms .  These two f leads/are
                               ZC Column 10)7"
            GC colurlm^in iJti.li^eters  (mm).
                  are common to various other
                 jed to identify the GC column
               ind the internal diameter of the
forms
tain
                                                   "page
                             of
                        in the
            f flo
            2 /of 2
                  field labeled
    Corner.  l  tnvmimber of entries required on any of
exceeds"-£he available s pace, continue entries on another
                       all header information. If a second
                 pages consecutively, as "page 1 of 2" and
    If a s^ponX page is not required, number the page "page
                squired,
the
            . 10\£or  rounding o/ff lumbers  to  the  appropriate  level of
                    lerve  the .following  common  rules.   If  the figure following
      those to^b< reta^iijed  v»  less  than 5, drop  it  (round down).   If the
July, 1991
                                    Page B-5/VC
-------
Exhibit B
                                                      SOW
                                   - Ambient Air
      figure is greater  than  5,  drop  it  and increase  th
      retained by 1  (round up).   If the  figure  followi
      retained equals 5, round up if  the digit  to be
      round down if  that digit is even.
      3.1.1.11  All results must be  transcribed  t
      with the specified number of decimal  place
      Exhibit B.  The raw data result  is  to be
      figures in the raw data result exceeds
      specified for that result entry  for
      figures in the raw data result to ent
      result, then zeros must be used  for
      number of reporting decimals for th
      following examples are provided:
                             ;t digit to be
                              Jast digit to be
                                   odd,  and
            th
   Raw Data Result
Specified Format
   t are described
  .ed only when the num
kximum number of figures
          re are not enough
          ed space for that
          the specified
       'specific form.  The
                                                           ct Entry  on  Form
                                              of
        5.9
        5.99653
      95.99653
     995.99653
     9995.996
    99995.9
   999995.9

NOTE:  6.3 stands for a ma:
decimal places.

3.1.2  Cover Page [CO

     3.1.2.1  This fo*m
     an  SDG,  and  to
     comments.  It is
     Manager  to authorize
     with  the SDG.
                                   5.900
                                   5.997
                                 95.997
                                996.00
                               9996.00
                              99996.
                                invalid

                     figures and up  to three
                 able samples analyzed within
               "information and general
    cent which is signed by the Laboratory
  zase all data and deliverables associated
     3.1.2.2   TKe  "SOW No.lf^is  the 'ERA-designated number  that  indicates  the
     Statement/of/Work~TSQW)  uhder which/analyses in the  data  package  have
     been  performed.   The  SOW No\ appears  on the  cover  of the  contract
     Statement/of  Work.  For  s^mpl^s  analyzed using this  SOW,  enter 291  for
     "SOW .No.
     3.1.2>3lJnaBr'lEPA  Sample/ No/",  enter up to 7  characters  for the  EPA
     Sample No\(inc
-------
Exhibit B
                        SOW  No.  XXX -  Ambient Air
    alphanumeric order using  the  Extended Binary Coded Qecipal Interchange
    Code convention.  Thus, if MAB123A is the  lowest (considering both alpha
    and numeric characters) EPA Sample No.  within the/SDG^it would be
    entered  in the  first EPA  Sample  No.  field.   Samples listed below it would
    be in ascending sequence  - MAB124A,  MAB124B, MA£125£>MACmA^ MA1111A,
    MAllllAD, etc.
                                             list
3.1.2.4  All EPA Sample Numbers must be
order, continuing to the following Cover P

3.1.2.5  Under "Lab Sample ID", a Lab
be entered for each associated EPA Samp^
entered, it must be entered identically
associated data.

3.1.2.6  Under "Comments", enter any
and administrative, the corrective action
for all of the .samples in the SDG.

3.1.2.7  Each Cover Page must
Manager or the Manager's desi
verify the contents of all data"
                       Ln ascending alp!
                      [f applicable.
3.1.3  Analysis Data Sheet [Form I -

     3.1.3.1  This  form  is used  for
     analysis of  canister  sa
     Volatiles  as given  Ex
     1 by  the occurrence
     marked  "Canister
     If  all  compounds
     specifically req
     3.1.3.2   Comple
     according to  the
                                                            10 characters) may
                                                             Sample ID is
                                                           Sample No.) on all
                                                        .ntered,  both technical
                                                           esolution performed
                                                               :he Laboratory
                                                          rize the release and
                                                      associated with an SDG.
                  .nd reporting results for
                     the Target Compound List for
                      .bset is indicated in Table
                       sh (-) in the column
                      'in Exhibit D,  Section 1.
                  .alyzed,  only the  pages
      aformation on each page of Form I-AAVC
      in  3.1.1  and as  follows:
     3.1.3.3   For  each__j>ositive"'iy identified target compound,  the Contractor
     shall  multiply the  det€icted concentration in ppbv by the  dilution factor
     calculated in^-Exhifeit  D/x§ection'-iKJand,  if this value is  greater than or
     equal  t
-------
Exhibit B
       sow
                                                         KX - Ambient Air
is encouraged to use additional flags or footnotes/ Ttfe definition  of
such flags must be explicit and must be included i/h tms^SDG Narrative.

3.1.3.5  For reporting results to the USEPA, th
specific qualifiers are to be used.  The seve
are not subject to modification by the labor
may be reported on Form I for each compound

3.1.3.6  The seven EPA-defined qualifiers/to/be used are as follows
                                                                           ers
      U -
      J -
      N -
      B -
         Indicates compound was analyze^ for but
         sample quantitation limit mus;t by correct
         Indicates an estimated value.
         estimating a concentration for
         where a 1:1 response is assumed, or wl
         indicate the presence of a compound t
         identification criteria-bjotthe result
         quantitation limit b
         sample quantitation l\mi
         is calculated, report
         must be adjusted for dil
             tected.  The
               dilution.
                                                     s
                                                  er  .
         Indicates presumptive evide
         used for tentatively
         identification^ls~~b^&ed on a
         is applied t^6 alJ^JTIC
         This flag/is /used whejn
         blank as/we 1/L as in Jth
         blank
         actio
                                                          Lor
         's used either when
          identified compounds
        the\mass spectral data
          ets^tfae
                 .n the sample
          For Sample, if the
              ntration of 1 ppb
           qu&ntitation limit
              the U flag.
                            as  in
                     ^ntamination/and/warns"
                      Tftis  flag/must be used
   compound.   This flag is only
  pounds,  where the
   ectral  library search.   It
     found in the associated
   indicates possible/probable
  ata user to take appropriate
or a TIC as well as for a
             positive
                               target compound.
      E -    This  flag  identifies
                          range
                                or
                                 as
                 t  be  dilut
                 Exhibit ]
              full  scale shoul
                 Form I-AAVC
                                   the
                                inpounds whose concentrations exceed the
                                   .C/MS instrument for that specific
                                   compounds have a response greater than
                             _ notBd in Exhibit D, the sample or extract
                             re-analyzed according to the specifications
                              .ch compounds with a response greater than
                              e the concentration flagged with an "E" on
                              he original analysis.  If the dilution of
                              iy compounds identified in the first
                              the calibration range in the second
                            results of both analyses shall be reported on
                            Form I-AAVC.  The Form I-AAVC for the diluted
July,  1991
                                                               Page B-8/VC
-------
Exhibit B
                                                SOW No.  XXX - Ambient Air
      D -
       sample shall have  the  "DL"  suffix appended

       This flag identifies all  compounds identi
       a secondary dilution factor.   If a samp
       analyzed at a higher dilution factor,
       the "DL" suffix  is  appended to the sa
       AAVC for the diluted sample,  and all
       reported on that Form  I-AAVC are f
       This flag alerts data  users that any
       concentrations reported may be du« t
       extract.
       e sample number.

     J.n an analysis at
            is re-
            :lag above,
'numbetxpn tfre^Form I-
                                                    iscrepancies
                                                    dilution of the sample or
      X -
       Other specific  flags may  be  re'qu
       results.  If used,  they must
       description attached to the
       SDG Narrative.   Begin  by  using
       required, use "Y" and  "Z" as needed^
       qualifiers are  required for  a sample  re
       combine several flags, as needed.   For
       might combine  the  "A";
       laboratory-defined f]
       and "Z".

The combination of flags  "BU1
contaminants are flagged  "B"
                                                     ins
        define the
cr/bed, and such
    ry Package and the
    than one flag is
     than five
        the "X" flag to
         he "X" flag
                                                  flags for sojaie sample.  The
                                       ire limtea~~CD—the letters "X", "Y",
                                        !IUB\ is/expressly prohibited.   Blank
                                              they are detected in the sample.
3.1.4  Tentatively Identifier

     3.1.4.1   Fill in all/he.

     3.1.4.2   Report  T
     number,  compound
     concentration (ofcit^ria
     Section  1).   Recejitio
                            iounds  [Fo"fcm fl  -  AAVC]

                           Information as\aboVe.

                           Identified Compounds (TICs) including CAS
                                           and the estimated
                       for/re»6rcing Tr&s/are given in Exhibit D,
                           must be reported in minutes and decimal
     minutes,  not seconos^or minuses:seconds.

     3.1.4.3   If, in_the opinibn^of ^he mass spectral interpretation
     specialistXno valid~^entativ^vvideivt^.fication can be made, the compound
     shall be  /repoj?^eTi~-as unknown.

     3.1.4.4'  Lhclude a Form \I-A\VC for every sample and method blank
     analyzed/even if no TICs \are\ found.  Total the number of TICs found,  and
     ente.r th^s number in the "No.)of TICs found." If none were found,  enter
      0" >^ero)>\Form II-AAVC i&usp be provided for every analysis, including
                        and re,anal:yses, even if no TICs are found.
 July,  1991
                                                              Page B-9/VC
-------
Exhibit B
                                                      SOW No/KXXX - Ambient Air
                                                                                    f.
     3.1.4.5   If the  name of a compound exceeds the 28 space's in the TIC
     column,  truncate the name to 28 characters.   If thfe ccnapound is an
     unknown,  restrict description to no more than 28/eha^acter-s^ (i.e.,
     unknown  hydrocarbon,  etc.).

     3.1.4.6   Number  all  pages as described in sub

3.1.5  Method Blank  [Form III  - AAVC]
     3.1.5.1   This  form summarizes  the samples' associatec
     blank  analysis.   A copy of the appropriate/Form II!
     for  each  blank.
                                       th each method
                                       \VC is required
     3.1.5.2   Complete  the  header informati^on
     3.1.1.   The  "EPA Sample  No." entered in
     AAVC  shall be  the  same number entered on the
     results  for  the blank  itself.
                                 Ill-AAVC as described in
                                at^the  top of Form III-
                                  I-^&yc when reporting
    3.1.5.3  On the numbered  lines/  enter
    with the method blank, along with
    EPA Samples.

    3.1.5.4  Number all pages as descrit

3.1.6 GC/MS Instrument Performance Check
                                          »r informati
                              5>ample Numbers associated
                                      ich identifies the
                                              'section 3.1.1.
                                                  Calibration  [Form IV - AAVC]
     3.1.6.1   This  form is/used to
                         /    f^" ''""
     performance  check (previous
     date  and time  of anfalysis of
     with  each analysis/ of/the insgrum
               port  the xesu\ts  of  GC/MS  instrument
             knWn as  "tuning?)  and to  summarize the
                 .es /^-s^andar^s and  blanks,  associated
                     performance  check solution.
     3.1.6.2   Complete theheadeif information ~as in section 3.1.1.  Enter the
     "Lab  File ID"  for\the rnjeycticm containing the instrument performance
     check mixture  of BFB^^^^ Enter/the date and time of injection of the
     instrument performance check mixture.   Enter time as military time.

     3.1.6.3   EOT each ionti^sted on\the jform,  enter the percent relative
     abundances inx^KF^rTrgbthand columnX/Report relative abundances to the
     number of. significant fr^gurXs given for each ion in the ion abundance
     criter/a Column.
     3.1.6.5
     enter "0
                  ion abundances a^e to be normalized to the nominal base
                     Form IV-AAVC /(see Exhibits D and E) .
                not
      abundances  must  be  reported as a number.  If zero,
^dashTVr  o/ther  non-numeric  character.   Where parentheses
July,  1991
                                              Page B-10/VC
-------
Exhibit B
                                                      SOW No.  XXX -  Ambient Air
    appear,  compute  the percentage  of the  ion abundance/of ,che mass given in
    the appropriate  footnote,  and enter that value in Xhe/parentheses.

    3.1.6.6   In  the  lower half of the form,  list all/samples>and standards
    analyzed under  that instrument  performance check in chgonoloTBsLcal order.
    by time  of analysis (in military time).   Refer/to/Subsection 1 ^(Xfjor
    specific instructions for  identifying  standaro^and blanks.
    Sample No.",  "Lab  Sample ID", "Lab File  IDy^ate Analyzed"
    Analyzed" for all  standards,  samples,  and plants.
    3.1.6.7  The GC/MS  instrument  performan
    twelve hours from the  time  of  injectio
    check solution  of BFB  listed at  the  t
    these requirements,  a  sample,  standa
    twelve hours of the injection  of the i
    solution.
    3.1.6.8  Number  all  pages  as  described  in  sectio

                                                 libration Ch4ck [Form V -
3.1.7  Initial Calibration Data and ContiS
AAVC]
                                                             analyzed again
                                                           fent performance
                                                           In order to meet
                                                         t be injected within
                                                        formance check
    3.1.7.1   Each  time  the  GC/MS  system tmdergoes/a  five~=p'oint calibration  to
    initialize  subsequent quantitationXof yOOs  in sample and blank analysis,
    the laboratory must complete  and  su0mit^a Form V.  The RRFs derived  from
    the calibration  and listed  on Form V are used for  quantitation of VOCs
    until  superceded by anptfier^£ive*Poi-nt\al-iXration (along with a new Form
    V).  Each sample and/blank^analysis perfarjroedyfor  any SDG must have  an
    associated  Form  V.
    3.1.7.2   Complete
    "Case No."  and  "/SDG/
    original  Case
    "Instrument ID
    changes during  the
    given on  Form V.
     3.1.7.3
     standar
  header
  ," for/th
  i the/initial calil
tfe
ilibfati
                                                 in subsection 1.0.   Enter the
                                                 a package,  regardless  of the
                                               ation was performed.   Enter
                                     of the  calibration.   If the  calendar date
                                  n procedure,  the inclusive dates  should be
                             tion
                              ICalibra
            es
 id times of the first and last of the
an Dates" and "Calibration Times".
                                  ID"  for  each of the  five calibration
                                  pive response factor calculation  for  the
                                  hen calculate and report  the average
                                    for each target compound in the space
                                  ted  using the following equation:
July, 1991
                                                                  Page B-ll/VC
-------
Exhibit B
                                         SOW. No-^XXX -  Ambient Air
    whe re:
                                 RRF =
                                          * ls
RRF
Ax

Ais
             Cis
                                                     sn for  the  compoi.

                                                   'ion for  the  internal
relative response factor,
area of the characteristi
measured,
area of the characteristic
standard,
concentration of the/intzfernal  standard  nearest in
retention time to the Compound/in/question,  and
concentration of One coHipound/to/be measured.
     3.1.7.5   The  value  of the average RRF is c^culate& by summing the five
     individual values of the RRF and dividing by tiye.   x*i order to be used
     for  the  analysis of samples,  the initial calibration musx^meet the
     acceptance criteria for relativejresponse factors.   Tkis criteria is  that
     the  %RSD of the 5 RRFs for all/targe~r-e»fflpo_unds must be^Wss than 30%.
     3.1.7.6  The  relative  standard oevration
                               %RSD =
                                    3DLis calculated as:
     where:
SD
         leviation o^f initial 5 relative  response
             compoundX calculated as:
                             SD  =
                                            - r
                                in/tial 5 relative response  factors  (per
                         impound )/.

     3.1.7.7  A cojucinuing cal£b«tioh\check is required for each twelve  (12)
     hour time period.   Ava^ue or">ercenit difference (%D) is calculated  as
     part of ^cojarl^iuTrn§^alrfekrationchj6ck in which only the calibration
     concentration of 10 ppbv is\ analyzed.  A RRF is calculated for  this
     concencratzion and compared to> the average RRF value obtained in the
     initial Calibration checkA  T^ie %D is calculated using  the following
     equatior
                                       - RRF
                                     RRF.
                                               x 100
 July,  1991
                                                      Page B-12/VC
-------
Exhibit B
                                                 SOW No. XXX - Ambient Air
    where:   RRFi -
             RRFC =
                    average  relative  response  factor  /Cro
                    calibration,  and
                                                          initial
                    calibration,  and                /   /
                    relative  response  factor from contiwiuing calibration
                    standard.                     /     ^\
    3.1.7.8   For  the  laboratory to continue to report ifhe resets of^sample
    analysis,  the XD  for  all  target compounds mustxbe/less than
    value as  specified in the Exhibit D,  Section/tXGC/MS ANALYSIS
    VOLATILES  FROM CANISTERS.   This yalue has been/feet at 25 percent. >«£m V
    is also used  for  the  Continuing Calibration Ch4ck.  Complete all header
    information.   Enter instrument ID,  date and zit&e of continuing
    calibration,  the  Lab  File ID of the continuing calipratfion standard, and
    dates and times of initial calibration/Xgi^e inclusive/dates if initial
    calibration is performed  over more  than onedate)/  Using the appropriate
    Initial Calibration fill  in the averagexrelabile/re/ponse factor (RRF)
    for each  target compound  and each internalxstandar^.   Report the relative
    response  factor from  the  continuing calibrationstandard (10 ppbv)
    analysis  and  the  % D  calculated using the equatio^ abovfe
3.1.8  Internal Standard Area and Retentic
                                             Summary [Fors/VI - AAVC]
    3.1.8.1  This  form is  used to
    times  'f the internal  standards
    data     used  to  determine when  ch
    will .   ersely affect  quantification
    be completed each time a  continuing
    samples are analyzed unda*—the same GC
    an initial calibratio
                                  langek ir/ internal
                                  .on\of Barge
                                             eak areas ^nd retention
                                                       d blanks.  The
                                                    standard responses
                                             t compounds.  This form must
                                           tion is performed, or when
                                             trument performance check  as
3.1.8.2  Complete
continuing calibre
of the continuing
immediately fol!
performance che<
completed on the ba*
initial calibration se<
of this standacri,  .and its
continuing xfalibratiofr-vstandai
              Frcta the
                                       aatfi«n.   Eh^er  the  Lab File ID of the
                                         weli^aa the date  and time of analysis
                                              If/samples are  analyzed
                                                >n,  before  another instrument
                       .nd^a-v£on/tinx!ting calibration, Form  VI  shall be
                                   internal  standard areas of the CAL 3
                                   ;andard.   Use the date  and time of analysis
                                          and areas in place of those of a
                  inj* an invtia/ calibratl
                  and
3.1.8.3
s tanda
retentzion/time (in
each/internal standard
of tnsL par
the areaxm
area of the
                        s oi the analysis of the continuing calibration
           nter the areaNpeasyred for each internal standard and  its
                           minutes) under the appropriate column.   For
                           iculjate the upper limit of the area  as  the  area
             ular standard/plus 40 percent of its area  (i.e.,  1.4 times
                   HOUR S7D box), and the lower limit of the area as  the
                         .daija minus 40% of its area (i.e., 0.6  times  the
                 thl
                  iterra
July, 1991
                                                              Page B-13/VC
-------
Exhibit B
                                                     SOW No.^JXX  - Ambient  Air
                                                   in
area in the 12 HOUR STD box).  Report these values
"UPPER LIMIT" and "LOWER LIMIT" respectively.  Ca
of the retention time as the retention of the
minutes (30 seconds), and the lower limit of th
retention time in the standard minus 0.50 minu

3.1.8.4  For each sample and blank under a
enter the EPA Sample Number and the area
standard and its retention time.  If the
outside the upper or lower limits calcul
an asterisk (*).   The asterisk must be
of the box for each internal standard
symbol.  Similarly,  flag the retentio
is outside the limits with an asterisk.
3.1.9  Canister Certification [Form VII-AAVC]

    3.1.9.1  This form is used to document the certificat]
    prior to first use.

    3.1.9.2  Complete the header in
    according to the instructions in
    3.1.9.3  Enter in Column 1, Concentra"1
    the initial analysis of a composite s
    directly from the sampLe^soutoe,  (e.g
    After pressurizing the canister
    the standards source/ aijralyzeXa
    results in Column

    3.1.9.4  For eac
    where:



    3.1
    age t
    canister

    3.1.9.6  After  c
                                  ne boxes labeled
                                   the upper limit
                                          plus 0.50
                                          as the
                                                       for  each  internal
                                                       standard  area is
                                                              that  area with
                                                              right hand  space
                                                          Cnder  the "#"
                                                                 standard that
                                      new canisters
                                   Form VII-AAVC
                                 bllows.
                       Standards, the results of
                      f the 59 standards taken
                           ic dilution manifold).
                          with the standards from
                          canister and enter the
                      erence (%D) in Column 3.

                     x 100




     ation  fthe standard in the standard source,

       ion of the standard in the canister, ppbv.
within ±30 percent for all standards,  proceed to
     ek/  (If %D is outside of ±30 percent, the
       d recertified.)

     f 1 week's ageing at room temperature, analyze
July, 1991
                                        Page B-14/VC
-------
Exhibit B
                                                 SOW No. XXX  - Ambient  Air
    a  sample  from the  canister and enter the results foi
    Column 4,  Final  Canister Concentration.
                                                        th standard in
3.1.9.7  For each standard, calculate the %D between the^tandards
concentration (column 1) and the analysis resul/ for^feach standard from
the aged canister, (Column A).  If this value Ls  within x§iO perbent,  the
canister is certified.  (If ZD in Column 5  is^pugside of ±3(NR.erceh^,  the
canister must be recleaned and recertified.
                                                )
3.1.10  Sample Log-In Sheet - Canisters  (FORM
     3 .1.10 .1   This  form is  used to document,
     sample  containers  and samples.   One or,
     for  each  sample shipping container.
     shipping  container must be assigned to"
     Group,  the original Form AADC-1 shall be
     the  Sample Delivery Group of the lowest
     AADC-1  must be  placed with the deliverables for
    Group(s).   The  copies  should be identified as "copy^
    location  of the original  shouLrl be~~n"&te4^_Qnthe copies .^
                                        Arabi
                                                        inspection  of
                                                        C-l  is  required
                                                     ,n a single sample
                                                   fe Sample  Delivery
                                                     the deliverables for
                                                      and a  copy of  Form
                                                          Sample Delivery
                                                         , "7 and the
     3.1.10.2   Sign and date  the  airbil\ (iF~"p~r««ent) .   Exartine the shipping
     container and record the presences/absence of 
tags in items_7 and 8 on
                               om the shipping container(s),  examine  the
                             'if present) , and record  the condition  of the
                                  ing) and presence of absence  of sample
                            rm AADC-1.
     3 .1.10 . 5 / Review~~the sarn^e shipp^in^ documents and complete the header
     informa/rion/aescribeavin subsection 1.0.   Compare the information
     recorded cm all the document^ and samples and circle the appropriate
     answe/r i/ item 9 on Form «ADCyl.

                  there are no/problems observed during receipt, sign and date
     (inclu(i&\tirae)XForm AADC-A, the chain-of-custody record, and Traffic
     Report,  anoN^ri textile sarciplp numbers on Form AADC-1.  Record the
July,  1991
                                                              Page  B-15/VC
-------
Exhibit  B
                                                      SOW No. XXX - Ambient  Air
     appropriate sample tags, and assigned laboratory numi
     The log-in date should be recorded at the top of
     and time of sample receipt at the laboratory sho
     10 and 11.   Record the fraction designation (if
     specific area designation (e.g., refrigerator
     Transfer block located in the bottom left corner/f Form
     and date the Sample Transfer block.  Cross oy^Nnused columns
                           if applicable.
                             -1 and the date
                              rded in items
                                    the
     3.1.10.7   If there are problems observed d
     marked with an asterisk (i.e.,  "absent*")/wa
     document  the contact as well as resolution
     Communication Log.   Following resoluti
     specified in the  preceding paragraph
     resolution of the problem.
              ripig  receipt or an answer
                 circlecfjxcontact SMO and
                 the  p/obLtem on a CLP
              ign and/daCe the forms as
                 where /appropriate, the
3.1.11  Complete SDG File (CSF) Document  InventoryX$hee^HFORM AADC-2]
     3.1.11.1   This  form is  used to record the inventory
     documents  and count of  documen^itT~ehe--
-------
     U.S  ENVIRONMENTAL PROTECTION AGENCY
                 CONTRACT LABORATORY PROGRAM
                 Volatile Organics in Ambient Air - Canister

                            COVER PAGE
Lab Name:
Lab Code:
Case No.:
Contract: / ^
SAS No. : / f^ ^\
SDGNo.: / / "\ "\
SOW No.: / / "\ \
           EPA Sample No.
Comments:
                             /
                      data package isSncompliance with the terms and
                         tract, bbthtechnically and for completeness,
                         ^s detailed above.  Release of the data contained
           hardcopy data paiskage\nd in the computer-readable data submitted
                diskette has B$en athorized by the Laboratory Manager's
                               by the following signature.
                                      Name:

                                       Title:
                        'COVER PAGE - AAVC
-------
U.S. ENVIRONMENTAL PROTECTION AGENCY
        CONTRACT LABORATORY PROGRAM       EPA Sample No.
Volatile Organics in Ambient Air - Canister
ANALYSIS DATA SHEET
Lab Name: " Contract:
SOW^Io.:/
Lab Code: Case No.: SAS No.: SDC/No/
Lab Sample I. D.: Date Received: Da^e Analyzed:
Canister Pressure(umts): As Received: ( ) /(fter Dilution^ ( )
GC Column and I.D.: Dilution Factor:/ / ^\ ^\^
/ / \ \
CASRN
75-01-4
79-01-6
67-66-3
71-43-2
56-23-5
127-18-4
75-35-4
107-13-1
107-06-2
108-90-7
71-55-6
79-06-5
79-43-5
100-41-4
75-09-2
120-82-1 X^
100-42-5/ /^
75-34/3 /
1087*8-3 \.
1330-20^^^
95-47-6 ^
COMPOUND / /
Vinyl chloride / /
Trichloroethylene / /
Chloroform ^. ^\^
Benzene ^^\^
Carbon tetrachloride
Tetrachloroethylene / ~^ — ~^^^^
1,1-Dichloroethene \ ^ -— ^^.^
\ \ / j-.^
Acrylonitrile \ \ / /
1,2-Dichloroethane \. /
Chlorobenz^nfi ^^ \ \
l,l,l-T/chl0foeth»ne \ \ \
/ it •*" 	 "^
1,1,/Trkinloroethan^ " ^X. V
/ / / **"* "^-. ^S^"""T
l-/,2,2^Tetrachlor/fethane ^X^/
Ethylbenz^V /
MethyleneclilorideX^
1,2, 4-Trtshk>robeniftqe ^X
Styrene^x. N>
1 , 1 -DichloroethaneX
•Toluene j I
~Xj(lenes, m- 8t p- /
\^ / /
'Xvlene , CKy /
f CONCENTRATION ^\
(ppbv) ^xV
/N

/ /
L^
\"\
\/
^^7
— -~-/













Q





















\y
Pase of FORMF-AAVC-I
-------
Lab Name:
           U.S. ENVIRONMENTAL PROTECTION AGENCY
                     CONTRACT LABORATORY PROGRAM          EPA Sample No.
                     Volatile Organics in Ambient Air - Canister
ANALYSIS DATA SHEET

    Contract:
Lab Code:
Lab Sample I.D.:
Canister Pressure( units-
GC Column and I.D.:
Case No.:

As Received:

SAS No.:
Date Received:

Dilution
SDj^No4
Date 4nalyz£d^
( ) Aft^Dibti$n: \^
Factor/ / \^ ^


( )
X.
CAS RN
78-87-5
95-50-1
106-93-4
106-99-0
67-64-1
75-00-3
78-93-3
107-02-8
100-44-7
108-10-1
10061-01-5
156-60-5
106-46-7
87-68-3 S'
74-83-9 / /
10061-02/6 /
75-7/8 C
X \^
74-87-3\, ^
156-59-2
167-56-1
COMPOUND / /
1 ,2-Dichloropropane / ^^
1,2-Dichlorobenzene ^N.
1 ,2-Dibromoethane
1,3-Butadiene / " — • — -^^_^_^^
Acetone \ ^X^^^—^ __
Chloroethane \ \ / /
2-Butanone \ /
Acrolein -^ 	 ^^^ \ \
Benzyl chj^nda^ — \. \ \ \
4-Met^l-2/pentanone) " ^^^^.^
cis-/,3-0ichloropropene / ^^^/
— / _S^_... / /
transxL2-Dic1»lQr^fethene
1 ,4-Dichlorobenzene ^^
Hexachlor&bntadiene^x^^ ^\
Bromomethane \,
trans- 1 ,3-DichloK>propene
Dichlorodifluoromctharje
Chloromethane / /
bs^U2-b^l^roetHene
GO>^;ENTRATION
/ / (ppbv)
//
1 ^
\>\
\/
^7
^^^













MethanoYx^^ /
^s/ }
Q











i

!






Page.
  FORM 1 - AAVC-2
-------
              U.S. ENVIRONMENTAL PROTECTION AGENCY
                          CONTRACT LABORATORY PROGRAM        • EPA sample NO.
Lab Name:
Lab Code:
Lab Sample


I.D.:
Canister Pressure(units):
GC Column
and I.D.:
Volatile Organics in Ambient Air - Canister
ANALYSIS DATA SHEET ,.
Contract: SOW^o.:/
Case No.: SAS No.: SDG/No./
Date Received: Da/e An4jyzed:
As Received: ( ) ^fter^ilutionx
Dilution Factor:/ / ^\




( )
^\
       CASRN
            COMPOUND
                                                            CONCENTRATION
       75-27-4
            Bromodichloromethane
                            /
       75-05-8
            Acetonitrile
      541-73-1
            1,3-Dichlorobenzene
       107-05-1
            3-Chloro- 1 -propene
       124-48-1
            DibromochloromethaM
                            V
       80-62-6
            Methyl methacrylate
       108-05-4
            Vinyl acetate
       115-07-1
            Propylene
       76- 13- I
       75-69-4
             richlo/ofluor
Trichloofluorometha
       142-82-5
            „
            HeRcme
       111-65-9
       75-45-6
            Chlorbdi|luorome thane
       98-83-9
            ^al pha^M ethy 1 sty^ene
       109-66-0
       UO-54-3
            Hexane
      1320.
.-3/-2
 1 ,2-Dichloro- 1  ,2,2rtetrafluoroe thane
       108
-4^8
 1 ,3,5-TrimethylBenzne
       95-63-6
Page.
                          FORM I - AAVC-3
-------
   U.S. ENVIRONMENTAL PROTECTION AGENCY

             CONTRACT LABORATORY PROGRAM   ^
Lab Name:
Lab Code:
Lab Sample I.D.:
Date Received:
Dilution Factor:
No. of TICs Found:
Volatile Organics in Ambient Air - Canister / / EPA Sample No.
TENTATIVELY IDENTIFIED COMPOUND/ /
Contract: / ^ "SQ^ No.:
Case No.: SAS No.:/ / "\ SDO^Jp.
Lab File/1. D./ \ \
Date A^jc/ed: \^ "\^
GC 0olunlnandI.D.: \^ /
/ / ^^
/ / /X.
 01
 02
 03
 04
 05
 06
 07
 08
 09
 10
    CAS NUMBER
\
  \  \
7
     \  V
      \
                   RT
               Est. Cone.
                 ppbv
Page	of
FORM II-AAVC
-------
              U.S. ENVIRONMENTAL PROTECTION AGENCY
                         CONTRACT LABORATORY PROGRAM
                           Volatiles in Ambient Air - Canister             EPA Sample No.
   Lab Name:
                            METHOD BLANK SUMMARY
                             Contract:
    Lab Code:
              Case No.:
   SASNo.:
Lab Sample ID:
                                    Date Analyzed: /
  Lab File ID:
                                   Time Analyze^
 Instrument ID:
 COMMENTS:
           THIS METHOD BLANK APPLIES TO THE FOLLOWING/SAMPLES:
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
FS:
EPA
SAMPLE NO.
















/
/
>x


/^
/ s- 	
/ /
/ /
/ /
£ "\
\^ "x^
\^ ^
\^
LABORATORY IDENTIF^ATION
SAMPLE












/^~ "^
/
/ /
/ /
/ /
X, /
x ^xy
x^ 
-------
             U.S. ENVIRONMENTAL PROTECTION AGENCY
                       CONTRACT LABORATORY PROGRAM
                       Volatile Organics in Ambient Air - Canister

                   GC/MS INSTRUMENT PERFORMANCE CHECK AND  ^
. MASS CALIBRATION WITH BROMOFLUOROBENZENE (BFB)>
Lab Name: Contract: ^OW/No.:
Lab Code:
BFB Injection Date:
Instrument I.D.:
Case No.: SAS No.: / SD&^Io.:
BFB Injection/Tim^: ^\
GC Column and 1/6.: X^ \^
m/z
50
75
95
96
173
174
175
176
177
ION ABUNDANCE CRITERIA / /
8.0-40.0% of mass 95 / / /v
30.0-66.0% of mass 95 / / /
Base peak, 100% relative abundance / / / /
5.0-9.0% of mass 174 / X. / /
Less than 2.0% of mass 174 X^ X/ /
50.0- 120.0% of mass 95 \^ X
4.0 - 9.0% of mass 174 \^ ^
93.0 - 101.0% of mass 174 X^
5.0 - 9.0% of mass 176 / ' 	 ^__
% RELAN-
ABUNDANCEs^

y


( )i

s^ ( )1
X ( >i
"X/ ( )2
7
              1-Value is % mass 174
This instrument performance check applies to the following^am]
-Value is %Tmal

01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
Page
EPA
SAMPLE NO.


/
/

^s



/ /" 	
/ /
/ /
'/ /
^ \
\ \
\^ \
\^




of
LAB
SAMPLE ID
/^C
/ / }
y / 1
/ /
\ / /
^ \y /
"\ ^
\^
"^-\ \
-\ X
X \
\ \
\
}
/ 1
^ / /
L ^^ /
-\^ /
\y


Form
Y*V
FH,EID .
v \
U- ^v^
s — \ ^"^
/ "x^ /



\^
. X
\/











IV-AAVC
/ DATE
/ANALYZED
N
V
-7



















TIME
ANALYZED






















-------
U.S. ENVIRONMENTAL PROTECTION AGENCY
          CONTRACT LABORATORY PROGRAM
          Volatile Organics in Ambient Air - Canister
           INITIAL CALIBRATION DATA AND
          CONTINUING CALIBRATION CHEC
Lab Name: Contract: /SOy Ntov^ \^
Lab Code: Case No.: SAS No/ / "~SQG No>\
Calibration Date(s): Calibration Time^^^/ ^\^ ^\
Instrument I. D.: GC Column antf 1. 1^.: ^Ism: 7
/ / ^
Lab File ID: RRF2 = / / RRF$s=
RRF10= RRF20= / / RR000/=
Compound
Vinyl chloride
Trichloroethylene
Chloroform
Benzene
Carbon tetrachloride
Tetrachloroethylene
1 , 1 -Dichloroethene
Acrylonitrile
1 ,2-Dichloroe thane
Chlorobenzene
1,1,1 -Trichloroethane /
1 , 1 ,2-Trichloroe thane
1 , 1 ,2,2-Tetrachloroethane
Ethyl benzene /
/ . 	 .
Methylene chloride ./
1 ,2,4-TrichJorohenzene
Styrene / \,
1 , 1 -Dichloroetftane ^\
Toluene ^\^
Xylenes, m- and p-
Xylene, o-
CALCULATE/) RJfrs / /
2







^
/ /
/ /
^
\^
^v-
^\
^\



\/
\v

5


r—
(
\


^
"~^\ 1
/
/ /
>/ /
s^\
\
\
\ \
) )
^ /
/


10/
^

•^-^
~
A '
\\
\

x--\
^-^



^">







^20
\^
\

^— 	
^7 r
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\^"
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-_/
















AVG.
RRF


>
'

















RSD





















D





















Paae of FORMV-AAVC-1
-------
          U.S. ENVIRONMENTAL PROTECTION AGENCY
                    CONTRACT LABORATORY PROGRAM
                    Volatile Organics in Ambient Air - Canister

                     INITIAL CALIBRATION DATA AND
                    CONTINUING CALIBRATION CHE
Lab Name:
Lab Code:
Calibration Date(s):
Instrument I.D.:
Contract: /SO
Case No.: SAS Nc^K^/
Calibration Tim/(s)f7
GC Column l.f>.: /
*No.:\ \
SDG Ntov^ \^
\^ J
mm:^
Lab File ID: RRF2 = / / RR/S =/
RRF10 = RRF20= / V RRF100 =
Compound
Bromodichloromethane
Acetonitrile
1 ,3-Dichlorobenzene
3-Chloro- 1 -propene
Dibromochloromethane
Methyl methacrylate
Vinyl acetate
Propylene
1,1,2-Trichloro- 1,2,2-
trifluoroethane /
Trichlorofluoromethane \
Heptane
Octane ^- 	
Chlorodifluorom^thanp^
alpha-Methyl/styrene
n-Pentane / /
Hexane ^\^^ ^X^
1 ,2-Dichloro- 1 , 1 ,2^^
tetrafluoroethane \\
1 ,3,5-Trimethylbenzene
1 ,2,4-Tnmethylbenzene
CALCULATED-RRFs \/ /
2






/
/ /
' /
*\.
\
~~^\
~~~-x



\^|
\^

5

/•
^



\
^
/,
K/ /
. -------
Lab Name:
           U.S. ENVIRONMENTAL PROTECTION AGENCY
                     CONTRACT LABORATORY PROGRAM
                     Volatile Organics in Ambient Air - Canister
                      INITIAL CALIBRATION DATA AND
                     CONTINUING CALIBRATION CHEC
                  Contract:
Lab Code:
Calibration Date(s):
Instrument I.D.:
Case No.: SAS No.:/ / S
Calibration Time(§)svy/
GC Column and/I.D^
«QNo.>\
\^ \
mau

«v.
?
Lab File ID: RRF2 = / / RRF#=/
RRF10= RRF20= / / RR/100C =
Compound
1 ,2-Dichloropropane
1 ,2-Dichlorobenzene
1 ,2-Dibromoethane
1,3-Butadiene
Acetone
Chloroe thane
2-Butanone
Acrolem
Benzyl chloride
4-Methyl-2-pentanone /
cis-l,3-Dichloropropene \
trans-1 ,2-Dichloroethene
1 ,4-Dichlorobenzene/-''
Hexachlorobutadiene x^"^
Bromomethane /
trans- 1 ,3-Bichlqrppropene
Dichlorodifltiocomethahe
Chloromethane ^v.
cis- 1,2-Dichloroethene
Methanol
CALCULATED RR^s / /
2






S
/ ,
/ /
/
\
\
~~^\
"^X



"^x
^^

5


f
\


— x
^ 	 \
)
/ /
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, V
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\ N
\/
^/










/ >
-------
          U.S. ENVIRONMENTAL PROTECTION AGENCY
                       CONTRACT LABORATORY PROGRAM
                       Volatile Organics in Ambient Air - Canister

                  INTERNAL STANDARD AREA AND RT SUMMARY
Lab Name:
Lab Code:
Date Analyzed:
Instrument ID:
Contract: SOW No.: / ^ \.
Case No.: SAS No.: / /SD&sNjx: "\
Time Analyzed: / / \^ ^\
GC Column and ID: ^X/ ^\
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22

12-HOUR STD
UPPER LIMIT
LOWER LIMIT
EPA SAMPLE NO.
















/
/
/ /
/ £
V
\
Chloro-
benzene-d5
Area #










/
/
/
/ /
/ /

\^
""*
^ 	 ^
s
/^ •s\
/


\
^\
RT
#









^ 	 ^
^
S X
/

/
. /
^ /
^^ "x
^\
\
X
X \
\ N
\
!
/ /
Bromochloro- /
methane /
Area /#
^ '
"x.

7"^— ^.
V \-~-~_
\ \ '
\ \
\ \/
\
\
X \
\
} V \
I 	 ~~
/ \-


\
\^
\ >
"xy


)
/

/
/ #
\ /
^s/
\

~—~
^7 r-
/ /
/
/
\
, \
\ >
V
— 7
7











1 ,4-^Djfluoro-
iienz^ne
/ Area #
' /
L
^ \^
\y
~~ — -,
^ /




















RT
#


























   Area Upper Limit = +40%
   Area Lower Limit = -40% of ui
RT Upper Limit = +0.50 minutes of internal standard RT
RT Lower Limit=-0.50 minutes of internal standard RT
   tf Column used to flag values outside^QC/limits with an asterisk
   * Designates values outside of QC limits.
Page	ot	                  FORM VI - AAVC
-------
                 U.S. ENVIRONMENTAL PROTECTION AGENCY
                           CONTRACT LABORATORY PROGRAM
                              Volatiles in Ambient Air - Canister
                               CANISTER CERTIFICATION
Lab Name:
                         Contract:
                                                        SOW No.
Lab Code: Case No.:
Canister I.D.:
SAS No./ / SDG
Date Pr/ssurized^
No.:

Initial Analysis Date: Final,Analysi^Date>\
Concentrations in ppbv. C / ^^ ^\







Compound
Vinyl chloride
Trichloroethylene
Chloroform
Benzene
Carbon tetrachloride
Tetrachloroethylene
1 , 1 -Dichloroethene
Acrylonitrile
1,2-Dichloroethane
Chlorobenzene .
1,1,1-Trichloroethane /
1 , 1 ,2-Trichloroethane' (
1,1,2,2,-Tetrachloroetharie,
Ethylbenzene
Methylene chloride 	
/ /f
1,2,4-Trienlordbenzene
Styren^ /
1 , 1 -tfc^hloroethane
Toluene ^\^ ^"X.
Xylenes, m- & p- ^\^
Xylene, o-
1 ,2-Dichloropropane
1
Cone, of
Standard




/"
\


/"" "~S
' /~^\ \
/ J .
^ / /
k"^/
^^'\
"^\ \
X\
\ \
) )
//
^ /
\/

2 /
Initial /
Canister/
Cone/ /
//
V"
^

— — —_ _
"\^ 	 ;
\\/
\~ /
\:
\
— \^^-
^-^


,?







/ % D
/ (1 to 2W
//
^ /

\^^
"\
~~-~- — -
r~^~~7
/

\
,}












^^
Final
Canister
Cone.



^
J

















^ %D
(1 to 4)






















       of
FORM VII- AAVC-1
-------
                 U.S. ENVIRONMENTAL PROTECTION AGENCY
                           CONTRACT LABORATORY PROGRAM
                             Volatiles in Ambient Air - Canister
                               CANISTER CERTIFICATION
Lab Name: Contract:
Lab Code: Case No.:
Canister I. D.:
Initial Analysis Date:
/ / SOW No.:
SAS No/: \SDG No.:
Date P ressjfriz^d: ^\
fin^t Analysis Date^ ^~\
    Concentrations in ppbv.
Compound
1 ,2-Dichlorobenzene
1 ,2-Dibromoe thane
1,3-Butadiene
Acetone
Chloroe thane
2-Butanone
Acrolein
Benzyl chloride
4-Methyl-2-pentanone
cis- 1 ,3-Dichloropropene /
trans- 1 ,2-Dichloroethene .
1 ,4-Dichlorobenzene^-^
Hexachlorobutadiene
BromomethaneX^^
trans- 1 ,3-Bichlefropropene
Dichlonzxiifluoromethane
ChlorometBane
cis- 1 ,2-DicbloroetiifeHe
Methanol ^^\^
Bromodichloromethane
Acetomtrile
1
Cone, of
Standard



r
\


^ — ^
/ x^O
/ )
/ / /
\//
\^ ^\
^\ ^\
\\ '
\\
)
//
^ /
\y

2 /
Initial /
Canister /
Cond. /
< ^
\

	 -^_
V——
\\ /
\V/
V
\
" "\_
\^y


^
\y






/ % D,^.
(I to/) ?
X //
^ <
"\^\
\,
^^-7
/^^^
/
\
\
V











^N
4
Final
Canister
Cone.


X.
y

















^ 5
% D
(1 to 4)





















Page.
of
FORM VII - AAVC-2
-------
                  U.S. ENVIRONMENTAL PROTECTION AGENCY
                             CONTRACT LABORATORY PROGRAM
                               Volatiles in Ambient Air - Canister
                                 CANISTER CERTIFICATION
Lab Name:
Contract:
SOW No.:
Lab Code: Case No.:
Canister I.D.:
Initial Analysis Date:
SASNo/ / SDGNo.:
Date ^fessunzed^
Fina/' Ana1ysi§ DateN^
     Concentrations in ppbv.
         OtheTs^ontammajits:
Compound
1 ,3-Dichlorobenzene
3-Chloro- l-propene
Dibromochloromethane
Methyl methacrylate
Vinyl acetate
Propylene
1, 1,2-Trichloro- 1,2,2-
trifluoroethane
Trichlorofluoromethane
Heptane
Octane /
Chlorodifluoromethane/ ,
alpha-Methyl styrenfi x
n-Pentane ^\^^
Hexane
l,2-DichloroXtj,2,2-
1 tetrat'luoro^ttiane--'' \
1 ,3,5-T/imethylbenzene
1 ,2;4/Tnmethylbenzene
i / C
I
Cone, of
Standard




/"
\


S A
/ ^\ I-
< / ,
. / /
^ /
\^ ^^
K^
N
\\
\ \
2 /
Initial /
Canister ,
Con/ /
//
C \
\

^^^^~-
\^^~7
\V/
\ (
V
"-X x
^\ ^7
^^


P


/ % D
(lt°A
//
^/
\ ^\
\^
-_^_^ ^
_^7
/

\
y







4\
Final
Canister
Cone.



>
/












' % D
(1 to 4)

















Page	of
         FORM VII - AAVC-3
-------
            U.S.  ENVIRONMENTAL PROTECTION AGENCY
                         CONTRACT LABORATORY PROGRAM
                           SAMPLE LOG-IN SHEET - Canister
         Lab Name:
  Received By (Print):
Case Number:
Sample Delivery Group No.:

       SAS Number:
                                              EPA
                                            SAMPLE
                                                #
                      ASSIGNED
                        LAB
                         #
                         /x
                         SHIPMENT
                           ETC.
                         REMARKS:
                          )NDH
CIRCLE THE APPROPRIATE RESPONSE
jl. Custody Seal(s):        Present/Absent*
                        Intact/Broken
2. Custody Seal Nos.:
                                                       7  /
                                                                  z
                        Present/Absent*

                        Present/Absent*

                        Airbill/Sticker
                        Present/Absent*
3.  Cham-of-Custody
   Records:
4.  Traffic Reports or
   Packing List:
5.  Airbill:

6.  Airbill No.:           	
7.  Sample Tags:          Present/Absent*
   Sample Tag Numbers:   Listed/Not Listp
                       on Chain-of'7
8.  Sample Condition:      Inract/Brok
 9. Does information on     Yes/N
   custody records, traffic
   reports and sample tags agree?
 10. Date Received at Lab:
 11. Time Received:
z
 \  NT
   \\
     \\
7/
                                                     \
 *If Circled, contacNSMO arld^attach record of resolution
        Received by-
              Date:
                                           Logbook No.
                                      Logbook Page No.
                                z
                                    FORM AADC-1
-------
              U.S. ENVIRONMENTAL PROTECTION AGENCY
                           CONTRACT LABORATORY PROGRAM
                           Volatile Organics in Ambient Air - Canister
                          COMPLETE SDG FILE (CSF) DOCUMENT
                                   INVENTORY SHEET
 Lab Name:
  Case No.:
  SAS No.:
                                                City/State:
                           SDG No.:
                        Contract No.:
All documents delivered in the complete SDG file must be original documents
i.
2.
3.
4.
5.
6.

7.
8.
9.
10.
11
Inventory Sheet (AADC-2) (Do Not Number)
Cover Page
Analysis Data Sheet (FORM I-AAVC)
Tentatively Identified Compounds (FORM II-AAVC)
Method Blank Summary (FORM III-AAVC)
GC/MS Instrument Performance Check and Mass
Calibration (FORM IV-AAVC)
Initial and Continuing Calibration (FORM V-AAVC)
Internal Standard Area and RT Summary (FORM VI-
Canistef Certification (FORM VII-AAVC)
EPA Shipping/Receiving Documents
         Airbill (No. of Shipments	)
         Chain-of-custody Records
         Sample Tags
         Sample Log-In  Sheet (Lab & AADC-1)
Misc. Shipping/Receiving Records (list
         Telephone Logs
 12. Internal Lab Sample Transfer Rec,
           Tracking Sheets (desc.
 13. Internal Original Sample Preparai
           (describe or list)
           Preparation Records
           Analysis Recorj
           Description
 14. Other Records (describe o/list)
           Telephone Communication Log
 Comments:
                                         /
            Completed by (CLP Lab>
                  (Signature)
                                 (Print Name & Title)
(Date)
U
                                     FORM AADC - 2
-------
Exhibit B
                                                      SOW No.  XXX -  Ambient Air
                                                                etion of all
                                                               fie  to a given
3.2  VOLATILES - TENAX®

      This section includes specific instructions  for/the
required forms for VOCs on Tenax®.  Each of  the  foi
function.  These instructions are arranged in  the

      •     General Information and Header Infoi

      •     Cover Page [COVER PAGE - AAVT]

      •     Analysis Data Sheet [FORM I -

      •     Tentatively Identified Compounds /FORM

      •     Method Blank Summary  [FORM I]

      •     GC/MS Instrument Performance Check at
            [FORM IV - AAVT]

      •     Initial Calibration D
            [FORM V -  AAVT]

      •     Internal Standard Area afc

      •     Tenax® Certification  [FORM

      •     Surrogate  RecoyeJry-4-FORM VII -"

      •     Sample Log-Jfo Sh€et>sr  T^
                                                             'on Check
                                                          :ary  [FORM VI  - AAVT]
      •     Complete

3.2.1  General Info,

      3.2.1.1  Values
      individual form ins
      concent rat ioris__of
      two sign
      Values/can
      excee
      submi
      to that
                                                   -1]
                                    Documenb-4nventory Sheet [FORM AADC-2]

                                               Lon

                                Ported on the hardcopy forms according to the
                                   in this Section.  For example, results for
                                      lie target compounds must be reported to
                                  \e vaiue is greater than or equal to 10.
                               the diskette file in any format that does not
                               ition as given in the record specifications and
                                "ure", paragraph 5 of Exhibit H.

                                 :h appear on the data reporting forms
                                     be reproduced by the Contractor when
                               format of the forms submitted must be identical
                           /ontract.  No information may be added, deleted, or
July, 1991
                                                                   Page B-l/VT
-------
Exhibit B
                                                SOW  No^XXX -  Ambient Air
      moved from its specified position without prior writt4n  approval of the
      EPA Administrative Project Officer.  The names o/  th^various  fields and
      compounds (i.e., "Lab Code," "Chloromethane") roast appear  as they do on
      the forms in the contract.  For items appearing on thi uncompleted forms
      (Section IV), the use of uppercase and loweroase/lettersxis

      3.2.1.3  Alphabetic entries made onto the
      be in ALL UPPERCASE letters (i.e., "LOW",/no
      entry does not fill the entire blank sp
      characters shall be used to remove the
      comprise the blank line.  However, do
      vertical bar characters that delinea
      exception would be those underscore^ at
      intended as a data entry line.
                                              s by the Contrac
                                              "Low" or "low").
                                            rovided on the  form,  null
                                                      scores  that
                                          remove /he/underscores  or
                                                    e forms.  The only
                                                      a  "box" that are
                                  emaining \a
                                   oxes
                                    e bot
                                                    jn to
3.2.1.4  Seven pieces of information are co:
of each data reporting form*.  They are Lab NamV>. Con
Case No., SDG No., SAS No., an4_SOW No.  Except as
and Case No., this information must
match on every form.
                                               e header sections
                                                  ct, Lab Code,
                                                    elow for  SAS
                                    ejred on everV^form and must
                                                           ted,
            3.2.1.4.1  The "Lab Name"N
            Contractor to identify the
            characters.                  \   ^   /
                                             name
                                               sen by the
                                        It may not exceed 25
            3.2.1.4.2  The
            which the analyses were'
            laboratories/op»ratrhg u:
            contract numbeir entere\
            regardless/of/the fac
                            ct" is the\m.
                               >erformed>
                               ider a corp\>ra
                                fair
                                 thai
                            Lab,
                       assr?
                    processing
3.2.1.4/3
6 letter-
in data
the time a cont:
Contrae-&e-£-r_except
najjfe or owners
 Tema
    £her lab
                                  jerforfi
                                      is an
er of the EPA contract under
  the case of multiple
   -wide contract, the
  f the corporate contract,
 the analyses (see Lab Code).
                                          labetical abbreviation  of up  to
                          by/ the EPA. to  identify the laboratory and aid
                            his lab code shall be assigned by  the  EPA at
                              .warded, and shall not be modified  by the
                                  rection of the EPA.  If a  change of
                        occurs at yhe laboratory, the lab code will
                      utvtil the^e^ntractor is directed by the  EPA  to use
                       assigned by the EPA.
                                  the
             r. 2.1.4.4  The "Cake Ita." is the EPA-assigned Case  number
              jsociated with thq ssjmple, and reported on  the Traffic  Report.
*Except  Form VI
certification.
                             SDG No. will not be  available  at time of
July,  1991
                                                              Page B-2/VT
-------
Exhibit B
                  SOW No. XXX - Ambient Air
            3.2.1.4.5  The."SDG No." is the Sample Delivery/Group number.  The
            Sample Delivery Group (SDG) number is the EPA Sample Number of the
            first sample received in the SDG.  When several samples are
            received together in the first SDG shipment, the\SDG number shall
            be the lowest sample number (considering; bo/^hXalpha^and numeric
            designations) in the first group of sa^ple^s receded uiM^r the
            SDG.
            3.2.1.4.6  The "SAS No." is the EP
            performed under Special Analytica
            analyzed under SAS only and repo
            SAS No. and leave Case No. blah
            according to the "Routine Anal/ti^al
            have additional "SAS" require,
            on all forms.  If the analysesX(iave
            "SAS No." blank.  NOTE:  Some sam*
            while others do not.
             assigned number for
                ices.  If samples are to be
                        orms,  then enter
                        re analyzed
                   'ces/1 (IFB)  protocols and
                       Case No.  and SAS No.
                     equirements,  leave
                     SDG may have a SAS No.
            3.2.1.4.7  "SOW No." is the number of the SfcW^by which the
            contract laboratory is/analyzitag^the samples.
      3.2.1.5  The "EPA Sample No."\is'
      the forms.-This number appears
      the form, or as the left column \»f
      number of samples.  When the "EPA
      triple-spaced box in the upper
      the middle line of the-^h«ee lines tl

            3.2.1.5.1
            identified
            Sample
            Traffic
                          common to many of
                       Ighthand corner of
        taj^le/summarizing data from a
             b." is entered into the
            corner, it should be entered on
             inprise the box.

                 and standards shall be
                For field samples,  the EPA
             ing number given in the
              sample.
            3.2.1.
            sample su
facilitate data assessment,  the following
 used:
                                        nd reanalyzed sample

                                  analyzed at a secondary dilution

                                  and standards, the following identification
                                   the "EPA Sample No."
July, 1991
                                Page B-3/VT
-------
Exhibit B
                                                     SOW
                                                - Ambient  Air
                                                   iden
Volatiles-Tenax® blanks shall be
"EPA Sample No." must be unique for
SDG.  The laboratory must achieve t,
two-character "##" terminator of
two characters or numbers, or a
example, possible identifiers f<
be VTBLK1, VTBLK2, etc.

VOC standards prepared on ad
identified as VTSTD###, whe '
of VOC standards on adsorb,
050, and 100).
id as  VTBLK##.   The
      within an
           the
        Lth one or
             For
                                                      tubes shall be
                                                             ncentration  in ng
                                                            001, 010, 020,
                  The three-character "###
                  combined with other alpha-nunf
                  identify each standard.

                  For volatiles standards, the following
                  to enter "EPA Sample NuSl

                  Name

                  CAL 1 Point VTSTD1###X
                  CAL 2 Point VTSTD2###
                  CAL 3 Point VTSTD3###
                  CAL 4
                  CAL 5 Point VTSTDf
      3.2.1.6  Several «/th
      Data Reporting F^rm
      Received,  Date Efxt^acted et
      of these entrLes.
                           atio^Vare common to many of the
                         La^Sample ID, Lab File ID, Date
                                a brief description of each
            EPA SaraoleXNumber
                                      ill have to be
                                      acters to uniquely
                                              shall be used
            3.2.1.6.1  "TiabSampl
            internal identifier.
                 ID" is an optional laboratory-generated
                   to 12 alpha-numeric characters may be
                       ctor does not have a Lab Sample ID,
            laboratory
            should oe^ente
                                \ID" is the laboratory- generated name of the
                                   containing information pertaining to a
                                     to 14 alpha-numeric characters may be
               Lved" is the date of sample receipt at the
              'on the Traffic Report (i.e., the VTSR).  It
               MM/DD/YY.
July, 1991
                                                 Page B-4/VT
-------
Exhibit B
                   SOW No. XXX - Ambient Air
            3.2.1.6.4   "Date  Desorbed"  and "Date  Analyze
            in a  similar  fashion.   The  date of sample r
            with  the desorption  and analysis dates  of pac
            that  contract holding  times were not  exc

            3.2.1.6.5   "Air Volume  Sampled" is the
            through the Tenax® adsorbent cartridge'
            temperature and pressure.
                           aould be entered
                          )t will be compared
                             Le to ensure
                                       (m3)
            3.2.1.6.6   "Instrument  ID"  is  common tfb  many of the forms,
            particularly those containing  calabr/tion dat^a^  The identifier
            used by the laboratory  must include/some incica^tion of the
            manufacturer and/or model of the  instrument,  /nd contain
            additional characters that  differentiate/between all instrument of
            the same type in the laboratory^

            3.2.1.6.7   "GC Column"  and  "ID (mm)"  a^e conuJtsn to various  other
            forms.  These two fields are to be used  tb\jxien^tfv the GC  column
            (previously called GC CoJ^umn ID) , and the irv&fecjial/diameter of the
            GC column in millimetei
/s  (t
3.2.1.7  Many forms contain a
bottom lefthand corner.  If theNnumfcjer of/ei
these forms exceeds the available\sp
copy of the same fraction-specific
information. If a second page is reqts^iret
consecutively, as "pagerT~~n>f 2" and
not required, number/the page
                                                            'of
                                   in the
                                                   :ries
      3.2.1.8  For rou:
      observe the fol
      retained is le
      than 5, drop
      up).    If the
      round  up if the
      digit  is even.
                         uired on any of
             continue  entries on another
              iplicating all header
              number  the pages
                of 2".   If a second page is
July, 1991
                 opriate level of precision,
                figure  following those to be
                ).   If  the figure is greater
          dTg'it  to  be retained by 1 (round
  the  last digit to be  retained equals 5,
         is odd,  and round down if that
                                               to the forms  in  the  raw data
                                of decanal places that are described in
                                 suit is to be rounded only  when  the number of
                              result exceeds the maximum number of  figures
                                  try for that form.  If there  are  not enough
                                   t to enter in the specified  space for that
                                  !sed for decimal places to  the specified
                                   for that result  for a specific form.   The
                         are/provided:
                                 Page B-5/VT
-------
Exhibit B
                                                   SOW No/v^XXX - Ambient Air
   Raw Data Result: '
                            Specified Format
Correct Entry on Form
                                                                  5.900
                                                                    997
                                                               9996.OC
                                                              99996.
                                                                invalid
     5.9
     5.99653
    95.99653
   995.99653
  9995.996
 99995.9
999995.9
NOTE:  6.3 stands for a maximum  of  six significant figu/es/and up to three
decimal places.

3.2.2  Cover Page [COVER PAGE  -  AAVT]

      3.2.2.1  This  form  is  used to list all billa%4.e satftfkl.es analyzed within
      an SDG,  and to provide certain analytical inf orftra.tion^and.general
      comments.  It  is also  the  document which is signed^fey thp Laboratory
      Manager  to authorize and rele/asean~~dfrta__and deliverabies associated
      with the SDG.
      3.2.2.2  The  "SOW  No."  is the E'RA- designated/ numb~er~fchat indicates the
                                       X   X    /   /
      Statement  of  Work  (SOW)  under whrch analyses in the data package have
      been performed.  The  SOW No.  appeals on toe cover of the contract
      Statement  of  Work.   For  samples analyzedousing this SOW, enter 291 for
      "SOW No."
       3.2.2.3  Under  "EP,
       Sample No.  ( inclxiaing blanks\
       within the  SDG. /Spfkes must
       suffix.  These/sample numbe
       alphanumeric  or derails ing
       Code  conventio
       alpha and  numeric~>sharacte]
       be  entered in the firs< EPA"
       would be  in
       MA1111A,
                                    Center up\to>7 characters for the EPA
                                          Lcates^/ for each required analysis
                                 conjLaj-n arf"
-------
Exhibit B
                    SOW No.  XXX -  Ambient Air
      3.2.2.6  Under  "Comments", enter  any  problems  encountered,  both
      technical ,and administrative,  the corrective acticm taken,  and
      resolution performed  for all of the samples  in tlie  SyG.

      3.2.2.7  Each Cover Page must  be  signed,  in  orAgi/^ais^by ^the Laboratory
      Manager or the  Manager's designee, and  dated/TO /uthorike  the^release
      and verify the  contents of all data and deli^eryables  associated wi^h an
      SDG.
3.2.3  Analysis Data Sheet  [FORM I - AAVT]

      3.2.3.1  This form  is used for tabula
      results for target  compounds.  If  al
      requested to be analyzed, only the
      submitted.

      3.2.3.2  Complete the header information
      required, according to  the instructions in  sect
      Volume Sampled, standard m3" from  Tenax® tube tag?"
                           g sample analysis
                        'ds are not
                           required must be
                           of Form I
                            1.   Enter "Air
       3.2.3.6  Unde
       with  the spec
       Contractor  is  en"
       definition  of  such
       SDG NarratiV'
       3.2.3.3  For positively  ide
       shall report the  total mass
       contaminants.  Report analyti
       the value  is less  than 10, and t
       above 10.

       3.2.3.4  For each
       total ng detected i

       3.2.3.5  Divide
       enter resulting
                          the Contractor
                           r blank
                          ficant figure if
                .nt  figures if the value is
              rget  compound,  enter the
                 tube".
                  volume  (standard m3)  and
              column.

              qualifier,  flag each result
 -ing Qualifiers  listed below.   The
'use  additional  flags or  footnotes.  The
   be explicit and must be included in the
                                             USEPA,  the  following contract
                                  be  used.   The  seven qualifiers defined below
                                  ,tion by the laboratory.   Up to five
                                   n  Form I  for  each compound.

                                   ed qualifiers to  be used are as follows:

                                 ound was analyzed for but not detected.   The
 July,  1991
                                  Page B-7/VT
-------
Exhibit B
             J  -
             N  -
             B  -
             E -
                                   SOW No^XXX -  Ambient Air
                   sample quantitation limit must be cor/rected for dilution.
                                             sed either
                                                identified
                                     umed, "be wheri-xChe mass
                                         compoi
                                                    less"
                                       greater than
Indicates an estimated value.  Thi
when estimating a concentration  f
compounds where a 1:1 response
spectral data indicate the
meets the identification crit
than the sample quantitation/li
For example, if the  sample  ouan^itation  limit  is  0.5 ng,
but a concentration  of 0.3/ng/ls calcuia^d, report it as
0 . 3J .   The sample quantit,atioTi limit/mus/ be adjusted for
dilution as discussed fo/ t#e U  fla

Indicates presumptive evldence^t/a  compound.   This flag is
only used for tentatively ioteotif ied(compounds, where the
identification is based on  a^mas-s^specTj^al library search.
It is applied to all TIC results.
This flag  is useyd when
associated blanB
possible/probableXbl;
user to take appropriat
for a TIC  as well
compound.
                              ilyte is fouftd/in the
                         as in tKe~~5aaple.  It indicates
                        conCaniina£ion and'warns the data
                         action/  Thi?~-fiag must be used
                           positively identified target
                            greater! than
                        )it/D, the
                      ily^ed accor^in^ to
                     ich
               ifies compoundk whose concentrations exceed
       fbration range of tRe GCXMS instrument for that
     zac xSnal^is A.  I_f one orx more compounds have a
                         .1 sca\£, except as noted in
                               t must be diluted and re-
                              ifications in Exhibit D.  All
                 th a response greater than full scale
   jld n~^e /^he/concentration flagged with an "E" on the
           the/original analysis.  If the dilution of the
           ses any compounds identified in the first
         tovbe belbv.the calibration range in the second
          then the results of both analyses shall be
            separatie-^copies of Form I.  The Form I for  the
diluted'^mpre shall have the "DL" suffix appended to the
sample number.

This flag identifies all compounds identified in an
analysis at/a secondary dilution factor.  If a sample or
  ttract is/re-.analyzed at a higher dilution factor,  as  in
        f)4g/above,  the "DL" suffix  is appended to the
              on the Form I for  the  diluted sample,  and all
 July,  1991
                                                 Page B-8/VT
-------
 Exhibit  B
                                                      SOW No. XXX  - Ambient Air
                   concentration values reported on  that
                   with the "D" flag.  This  flag alerts
                   discrepancies between the concentration
                   due to dilution of the sample or
                                            I are flagged
                                           users  that any
                                          reported may be
             X -
Other specific flags may be require
results.  If used, they must be
description attached to the S
the SDG Narrative.  Begin by /usi
flag is required, use "Y" and "Z" as needed.
five qualifiers are requirsTcl for a
"X" flag to combine several flags, a
instance,  the "X" flag m/ght/combin
flags for some sample. /The\].aboratfb
limited to the letters St?,  "Y'V ^nd
                                                                          than
                                                                          the
         If more
     result, use
 needed.  For
th6 "A", "B", and "D"
 ^-defined flags are
 Z".
             The  combination of flags "BU" or "UB'-xi.s exp^ssly prohibited.
             Blank contaminants are flagged "B" onlyfrhen tn>x_ are detected in
             the  sample.

3.2.4  Tentatively Identified  Comp^un
      3.2.4.1  Fill  in all header  id
                       :ion
      3.2.4.2  Report Tentatively  Identrfiedvtompounds (TICs)  including CAS
      number, compound name, retention  time  (R7),  and the estimated
      concentration  (criter^a-^«creporting\TIcSL are  given in  Exhibit D,
      Section 2).  RT must/be reported  in min\tes\and decimal  minutes,  not
      seconds or minutes/sec*

      3.2.4.3  If, in zfhe/opinion ,bf the masVv^Eectral interpretation
      specialist, no/fral/d tentative/idenbificacion can be made,  the compound
      shall be reporyted^as unknc
      3.2.4.4  Include
      analyzed, even if.
      and enter this_number
      enter "CT/Uero).
      includin  rerriredil
      3.2.4.6
      FormMl-AAVT for every  sample  and  method blank
                 found.  Total  the number  of TICs  found,
                      f TICs  found."  If  none were  found,
                   mvist be provided  for  every analysis.
           ,±ons arickiTfeanalyses,  even if  no TICs are  found.

           a Compound exceeds the 28  spaces in the TIC
             to. 28 characters.   If the compound is an
                 to no more than 28  characters (i.e.,
                                   described in  3.2.1.
July, 1991
                                                                    Page  B-9/VT
-------
Exhibit B
                                                SOW No-^XXX -  Ambient Air
3.2.5  Method Blank Summary.  [FORM III  - AAVT]

      3.2.5.1  This form  summarizes  the samples  associated with each method
      blank analysis.  A  copy of Form  III-AAVT is  re/uiff^cNfpr ea^ih blank.
      3.2.5.2  Complete the header  information as
      the EPA Sample No. entered  in the  box at
      be the same number entered  on the  Form I-
      for the blank itself.

      3.2.5.3  On the numbered  lines,  enter
      with the method blank, along  with  ot'
      the remaining columns which identifies

      3.2.5.4  Number all pages as  described

3.2.6 GC/MS Instrument Performance  Check and Mass
      AAVT]
                                             Cal
                                               scribed  in section >x2 .1.
                                               >p  of  Form III-A&VJ  sha^l
                                               when reporting resul
                                                       umbers  associated
                                                    'as designated in
                                                    es.
FORM IV -
                                                            C/MS instrument
                                                             o summarize the
                                                            lanks,  associated
                                                   .nee check solution.
                                                                      Enter
3.2.6.1  This form is used t
performance check (previously
date and time of analysis of s
with each analysis of the instrumfent^per/for;

3.2.6.2  Complete the header information as  in  section  3.2.1.
the "Lab File ID" for/ehe—ituection coxitarning  the  instrument
performance check solution or\BFB.  Enter  tfte date  and  time  of
injection of the ijastrximents^periformance check) solution.   Enter time as
military time.

3.2.6.3  For each i^on listed ojC the^Sorm, /enter the percent  relative
abundance in Che righthanoy column.  Report relative abundances to the
number of signtC^cantxf^igX.ire^B given for each ion in the ion  abundance
criteria column.
3.2.6.4  An^4r»a— aJDundanc
peaks li€ed on  FORM^-IV  - AA^
                                          be normalized to the nominal base
                                      (se& Exhibits D and E) .
                                  .ances  must be reported as a number.  If
                                   or other non-numeric character.  Where
                                   ;the percentage of the ion abundance of the
                                     footnote,  and enter that value in the
       3.2.6.6   rn^the  r«wer Vialf/of the form, list all samples, standards,
       and Tenax® tubs^ blanks analyzed under that instrument performance check
July,  1991
                                                             Page B-10/VT
-------
Exhibit B
                   SOW No. XXX - Ambient Air
      in chronological  order,  by time of analysis (in mi/Lit^ry time).  Refer
      to subsection  1.0 for specific instructions for iraencifying standards
      and blanks.  Enter "EPA  Sample No.",  "Lab Sample/ID6^al £ive-point
      calibration at the specific .concerrtrratianleveIs described in Exhibits
      D and after all initial  calibrafeiancriterTa~TTav«-_ljeen met, the
      laboratory must complete and^eubmita~To-Ho V-AAVT fop  each volatile
      target-compound initial  calibration perfprm^dTwKittf/is relevant to the
      samples or blanks in the SDG,  regaroies/s of when that  calibration was
      performed.                        \   >/  /

      3.2.7.2  Complete alL-he-ad^r informa^Lon^s in section 3.2.1.   Enter
      the "Case No." and /SDG  No."\for the  current data package,  regardless
      of the original Case f6"r~"wticn the initial calibration was performed.
      Enter "Instrument/ID/ and  the  eate^sJ  of ttye calibration.   If the
      calendar date  changes during the_caliD£A£j,on procedure,  the inclusive
      dates should bss gj/ven on Fprm,

      3.2.7.3  Enter-xthe >ajec/6iori' times of the first and last of the
      standards analyz^d^under "(Zalibration Times".   Indicate the method of
      standard preparatio^x^FlasK^Vaporization",  "Static Dilution Bottle",
      or "Permeatij
                               File II
      caribi
-------
Exhibit B
                SOW
                                                            v
                                                            - Ambient Air
                                 RRF =
                                                     stic ion
                    is
where:       RRF   -      relative response
             Ax    =      area of the cha:
                        to be measured,
                        area of the charXct^ristic  ion  for the internal
                        standard,
                        concentration /bf. /he  inte/nal/standard nearest
                        in retention/timX  to  the/coijrfpound in question,
                        and
                        concentration^} f tnexc/omp^und to  be measured.

3.2.7.6  Report the relative response  factor-Ssfor "btie  system monitoring
compounds in the  calibration standards.  Repor^t^je relative response
factors for all surrogate conraounds  in the calibration  standards.
      3.2.7.7  The laboratory must\cal^
      deviation  (%RSD)  for all  compound

                              %RSD =
                                    ite  and report—die relative standard
                                              following formula:
      where:
             SD
                              respo
  devifftiotKof initial 5 relative
e factor  (p»r compound), calculated  as:
                             SD =
                                             -  1
                                ;an/of  initial 5  relative response factors (per
                              "compound).

       3.2.7.8   In^_M=4Ar^to be used fcvCxthe analysis of samples or sample
       extracts/the  initiaS^calibra^ion yust meet the acceptance criteria for
       relatiy/e  resp~bhs~e---factotss outlrh&jz in Exhibits D and E.  All other
       compounds/must meet a\min!Lmum RRF of 0.010.

       3.2/7.9/  Form V-AAVT is\lsd used for the Continuing Calibration Check.
       A (Continuing Calibration (Check is required for each twelve  (12) hour
       3 .2 . 7 .10^£he Contract/laboratory must analyze calibration standards
       and meet all^c-riterra/outlined in Exhibits D for the minimum RRF  and
 July,  1991
                                                             Page B-12/VT
-------
Exhibit B
                        SOW No.  XXX -  Ambient Air
      maximum percent  difference between initial and cor
      as part of  the continuing calibration check.
                           :ini/ing calibrations
      3.2.7.11  Complete  all  header information.   Entfer instrument ID, date
      and time of continuing  calibration,  the Lab Fifle /TlKpf tfife^continuing
      calibration standard, and dates and times of/initial calibration (give
      inclusive dates  if  initial calibration is pejrfafrmed evermore tfaan one
      date).  Using  the appropriate Initial Calibration file in the\averaf
      RRF for each target compound, each systenr monitoring compound fo}
      volatiles, and each surrogate for volatides/  Report the RRF from the
      continuing calibration  standard (CAL 3/ analysis. /^Calculate the
      Percent Difference  (%D)  for all compoidnds/   The %C for all compounds
      must be within 25 percent.   The %D its caT-culatecr us/ing the following
      equation:
                           %J?j  RRFj-RRl^
                   .00
      where:
                   RRF  -
averige^reiative response fac
calibration, and
relaoive\resp"oT*se7 factor fron
calibration standarc
   from initial
continuing
3.2.8  Internal Standard Area and Retenc^.on\jimy Summary [FORM VI  -  AAVT]

      3.2.8.1  This  form isjus«4t;o summarize the peak areas and retention
      times of the internal  standards added\p a\l samples,  blanks,  and
      duplicates.  The  data/aroused to determine yhen changes in internal
      standard responses will advters|e-ly~~affect quantification of target
      compounds.  Thisr  form  must lie complete^d^each time a continuing
      calibration is/per/formed, dr  wfieneamples/are analyzed under the same
      GC/MS instrument /performance /check as^aw initial calibration.

      3.2.8.2  Complet^the "h^ade'r  information.   Enter the Lab File ID of the
      continuing "calibration standard,  as well as the date and time of
      analysis of__ttig^continuSnE calibration standard.  If samples are
                           following anxinitial calibration, before another
      Lnstrunrent^pe-r^ejqriance\check  and/a continuing calibration, Form VI
      shall/be /completeo^xn  th\basis of the internal standard areas of the
      CAL 2 inatial  calibracion\sequence standard.  Use the date and time of
      anaiys/s of this  standard, \and its Lab File ID and areas in place of
      those Cof a continuing  calibration standard.

                     the resuLfcs «Jf  the analysis of the continuing calibration
                           airea jneasured for each internal standard and its
July, 1991
                                     Page  B-13/VT
-------
Exhibit B
                                                SOW- No,rvXXX - Ambient Air
      retention  time  (in  decimal  minutes)  under the app
      each internal standard,  calculate  the upper limiy
      area of the particular  standard plus 40% of its,
      the area in the  12  HOUR STD box),  and the low.
      the area of the  internal standard  minus 40%
      times the  area  in the 12 HOUR STD  box).   Re
      boxes labeled "UPPER LIMIT" and "LOWER LIM
      the upper  limit  of  the  retention time as the
      standard plus 0.50  minutes  (30 seconds) ,/an5
      retention  time  as the retention time iry th
      (30 seconds).
                                                      Late column.  For
                                                      the area as the
                                                             1.4 times
                                                                   as
                                                                 1.6
                                                               intel
                      •respectively.   Ci
                      etention of the
                     the lower limit of the
                              inus 0.50 minutes
                                             standai
                                           ider^a give
                                                anc
                                                  If
                                                 cal
3.2.8.4  For each sample and blank
calibration, enter the EPA Sample Numt
internal standard and its retention  time'
area is outside the upper or lower limits
area with an asterisk (*).  The  asterisk must bl
right hand space of the box for__e_ach internal stanc
under the "#" symbol.  Similarly,
internal standard that is oucside-~the limits
                          Sntinuing
                         irea measured for each
                          internal standard
                             above,  flag that
                         )lacebWin the far
                                                           :d a
                                                  retention
                                 ?ea,  directly
                                e of any
                              sterisk.
3.2.9  Tenax® Certification  [FORM VII

       3.2.9.1  This form  is  used to  doci.
       prior  to field use.
                                            certification of Tenax®
       3.2.9.2   Complete  the header
       The header  inform
       Case  No., and  SASNomust
       more  than one  fo/rm %s used.
       column and  I.D.
                                formation^onNeach page of Form VII-AAVT.
                                b  Name,  Contract,  SOW No.,  Lab Code,
                                3nte~re—enter instrument I.D.,  GC
                 and date analyzed.
3.2.9.3  Each ^fra^ch of^pj'ep.
contamination prior\to use
the batch  immediately
identificati«fr-rtt=unber as
                                    ed Tenax® tubes must be checked for
                                   y analyzing total VOCs from one tube from
                                     eparation.  Enter Tenax® tube
                                        the batch on the Tenax® certification
       form (Fo;
       column/on
       ng/tube)
           VIH-AA\
           r  rejectio
 3.2.10   S/rrofeate  Recovery [FOf
  irt
          ^sults (ng/tube)  in appropriate
jresentar&iVe tube,  indicating acceptance (<10
  vng/tube).

    [II  - AAVT]
       3.ZH0.1 >^rm VIII -  AAVT is used to report the recoveries of  the
       surrogate comtx^unds addea yo each Tenax® adsorbent tube.

       3.2.10.2  Compete "the' h/ader information and enter EPA  Sample  Numbers
 July,  1991
                                                             Page B-14/VT
                                                       •v-/
-------
Exhibit B
                                                SOW No.  XXX - Ambient Air
      as described  in section  3.2.1.   For each surrogate
      recovery  to the nearest  whole percentage point,
      significant figures given by the QC limits at tl
                                                      zport the percent
                                                        the number of
                                                    Jttom of the form.
                                                          JC lie
                                                              jace
3.2.10.3  Flag each surrogate recovery outside
asterisk (*).  The asterisk must be placed  in/
appropriate column, under the "#" symbol.
total the number of surrogate recoveries
sample (Total Out).  If no surrogates wepe o^ttside  the  limits,
"0".
  last
le far righ^hand"
  the  QC
3.2.11  Sample Log-In Sheet - Tenax®  [FORM
                                          -1]
      3.2.11.1  This form is used  to  document^the retfeip/t and inspection of
      sample containers and samples.   One^-origirtal  broken,  missing) and
      presejzfce/alDsence of^amp^e tags in items  7 and 8 on Form AADC-1.

      3.2/11/D  Review the sample\  shipping documents and complete the header
      inforrtktion described injInstruction A.   Review the data for "Air
      Vo-ljjme Sampled" , information on units,  and correction for standard
      tempe~T^ature>and pressur/6. /Compare the  information recorded on all the
      documents-xand samples /nd/circle the appropriate answer in item 9 on
July, 1991
                                                             Page  B-15/VT
-------
Exhibit B
                                                SOW No^iKX -  Ambient Air
                                                                   sign and
                                                                     and
                                                                        ord
Form AADC-1.

3.2.11.6  If there are no problems observed dur,
date (include time) Form AADC-1,  the  chain-of -
Traffic Report, and write the sample  numbers
the appropriate sample tags and assigned lal
applicable.   The log-in date should be  rec
AADC-1 and the date and time of sample  receipt  at  the laboratory
be recorded in items 10 and 11.   Record the /fraction designation (if
appropriate) and the specific area designation  (e. zCNrefrigerator
number) in the Sample Transfer block  Located in tWe  bottom left corner
of Form AADC-1.  Sign and date the Sa4pl/ Transf/r block.   Cross out
unused columns and spaces.
                                                                            Id
      3.2.11.7  If there are problems  observed'auring Receipt or an answer
      marked with an asterisk  (i.e.,  "absent*"  was^rclebX,  contact SMO and
      document the contact as  well as  resolution of tne\probti&m on a CLP
      Communication Log.  Following /te_s_c>lution,  sign and oa^e tne forms as
      specified in the preceding pacagrapK~~aTtd—nctEe^ where appropriate, the
      resolution of the problem.
3.2.12  Complete SDG File (CSF) Docume
                                                     FORM AADC-2]
      3.2.12.1  This form is used  to  reco\d  6he/inventory of the SDG File
      Purge documents and count of documents in\the  original Sample Data
      Package which is
                      2.  As
      3.2.12.2  Organize /all
      Section 1 and Sec/io
      on Form AADC-2 aiid sction 1.
      consecutive number/   (Do
      CSF by reviewing trte  doci
      in the columnsprovid
               >F ^documents
               ^embie tfre^ doci
                     described in Exhibit B
                      nts in the order specified
                     ip each page with a
  no/t number ^he AADC-2 form).  Inventory the
    nt/numbers ana recording page numbers ranges
      e Form AADC-2.  If there are no documents
       for a specific docuia^nt  type,  enter  an "NA"  in the empty space.
                         Laborat
                ito a clear]
              5C-:
3.2.12.3
not fit
Form
No. 7
appr
described or listed  in  t'
              8,
or 10.
            jrLate previous
      spett-^fic documents related to the CSF may
define^catagory.  The laboratory should review
  if it is-^most appropriate to place them under
    ry 10 should be used if there is no
  gory.  These types of documents should be
    blanks under each appropriate category.
July,  1991
                                                             Page B-16/VT
-------
     U.S ENVIRONMENTAL PROTECTION AGENCY
                  CONTRACT LABORATORY PROGRAM
                  Volatile Organics in Ambient Air - Tenax
                             COVER PAGE
Lab Name:
 Lab Code:
 Case No.:
 SOW No.:
                                Contract:
                                SAS No. :
                                SDGNo.:
Commentbi
                      i data package TsSn compliance with the terms and
         -Conditions of the>sontract. Both technically and for completeness,
      tor othef^hantKe^sonditiohs detailed above. Release of the data contained
      'in this hardcopy data package\and in the computer-readable data submitted
         floppy diskette has been authorized by the Laboratory Manager or the
            Manager's designeel as verified by the following signature.
                                        Name:

                                         Title:
Date
                         COVER PAGE - AAVT
-------
       U.S. ENVIRONMENTAL PROTECTION AGENCY
                CONTRACT LABORATORY PROGRAM      EPA Sample No.
Volatile Organics in Ambient Air - Tenax
ANALYSIS DATA SHEET
Lab Name: " ' Contract: / ,

/SOW No.:
Lab Code: Case No.: SAS No.: / / SDG No.:
Lab Sample ID: Lab File ID.: / £^~^\^ ^\y
1330-20/7 /
95-4/7-6 /
~'^o ^\
Xylenes, m- and p-\
Xylene, o- ^ ^
Jl, 1-Dichloropropaiie /
\. 1 \. / /
95-50- 1 ^\jl ,2-Dfetilprobenzene/
1 ^^ ^^ /
106-93-4 |l,2-D>bromoethanfe
CONCENTRATION
ng/,^
/ /
/
\^
\^
~— ^~_
-^/














ng/m3



^>
•s/









o
Q














1





i




Paae
FORM I - AAVT-I
-------
Lab Name:
          U.S. ENVIRONMENTAL PROTECTION AGENCY
                     CONTRACT LABORATORY PROGRAM       EPA Sample No.
                      Volatile Organics in Ambient Air - Tenax

                           ANALYSIS DATA SHEET

                                 Contract:
Lab Code:
                    Case No.:
                                          SAS No.:    /  
-------
      U.S. ENVIRONMENTAL PROTECTION AGENCY
                   CONTRACT LABORATORY PROGRAM        EPA Sample No.
Lab
Lab
Lab
Date
Name:
Code:
Sample ID
Received:
Instrument ID:

Air
Volatile Organics in Ambient Air - Tenax
ANALYSIS DATA SHEET
Contract: / /
Case No.: SAS No.: / /
Lab File ID.: / ^
Date Analyzed! ^ ^
GC Column and ID/ / \^
Volume Sampled, m3(Corrected to STP): / /

'SOWNo.:
SDGNo.:

\
"\
\^ "\^
CASRN
       COMPOUND
                                                  CONCENTRATION
              na/tub^
ng/m3
 78-86-4
2-Chlorobutane
    /
1 190-22-3
1,3-Dichlorobutane
1 10-56-5
1 ,4-Dichlorobutane
760-23-6
3,4-Dichloro- 1-butene
106-89-8
l-ChIoro-2,3-epoxypnjmane
                                                          .y
 1 10-75-8
2-Chloroethoxyethene
 98-86-2
1-Phenylethanone
 74-95-3
Dibromomethane
\    /
 142-28-9
1,3-Dichlopopropane
630-20-6
 , 1 , 1 ,2-/Tetrathlorethatae
 95-49-8
o-Chlorotf/luene
 108-67-8

 106-43-4
p-Chlorbtohiene    /
 104-51-8
 IOB-41-S
 100-527
Benzaldehyde
             Benzonitnle

             1 ,4-Dichlorobenzene
    of
                FORM I - AAVT-3
-------
 U.S. ENVIRONMENTAL PROTECTION AGENCY
           CONTRACT LABORATORY PROGRAM
           Volatile Organics in Ambient Air - Tenax
                              EPA Sample No.
TENTATIVELY IDENTIFIED COMPOUND/ /
Lab Name: Contract: / ^SQW No.:


Lab Code: Case No.: SAS No.:/ / \^ SDQjNfo.
Lab Sample I.D.: Lab File/l.D./ "\ ^\
Date Received: Date AJ»ty£ed: "^\ ^\
GC Column and I. D.: ' Air Xolujae Sample, Standard m3"\^ 7
No. of TICs Found: / /

// /

01
02
03
04
05
06
07
08
09
10
CAS NUMBER









/•
COMPOUNTD>iAME\y
\ "
"\
,^___
/ ~~ — -^__
\ \~^~--^_
\ \ / /—
\ \ / /
\ v /
\ (
' — \ \ \
"^v
^
AT
\
"\
\^ y
\/
^
^~J




Est. Cone.
ng/tube


?







ng/m3










Q










Pnge	of
FORM 1I-AAVT
-------
                U.S. ENVIRONMENTAL PROTECTION AGENCY
                          CONTRACT LABORATORY PROGRAM
                             Volatiles in Ambient Air - Tenax       -     EPA Sample N'o.
   Lab Name:
                             METHOD BLANK SUMMARY
                                    Contract:
                                                       WNo.
Lab Code:
Lab Sample ID:
Lab File ID:
Case No.: SAS No.: / /SDG No.:
Date Analj^ed: X^
Time Ana^ze$fc\^ X^
Instrument ID: / / "\^ \^
                                            ^vX/
          THIS METHOD BLANK APPLIES TO THE FOLLOMNG?SAMPLES:
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
T)
23
24
25
26
27
28
29
30
EPA
SAMPLE NO.
















/
/
X,



/ 	 1
/ s
/ /
/ /
/ x
LAB /
SAMPLE ID /
/
X
"\


, 	
/ ~^~
\ V~~" — -^
\ \
\ \
\ v
\
^ — ~\ \
/ \
/ / \ 1^-.
/ / J \
/ / /-\
t / / ^
^x / /

\ ^x
^^. ^^ "\
_ ^\ x^ /
^x \
\ \
\ \
)
\ \ / /
\ \ / /
\ \ / /
' /LAB /
/FILE ID/
/ /
^X / /
v " /
\, x^
x^
\
- — 	
	 	 .
/ r— —^__
/ /
/
(
\
v \
\ /
V
~7
~y












x TIME
ANALYZED




\
^ ;
"-v
~~7
J





















COMMENTS:
     of
                                 FORM III - AAVT
-------
U.S. ENVIRONMENTAL PROTECTION AGENCY
          CONTRACT LABORATORY PROGRAM
          Volatile Organics in Ambient Air - Tenax

     GC/MS INSTRUMENT PERFORMANCE CHECK AND
  MASS CALIBRATION WITH BROMOFLUOROBENZENE
Lab Name:
Lab Code:
BFB Injection Date:
Instrument I.D.:
Contract:
Case No.:


SAS No.:
BFB Injection
fiOV)
/ SDiS
f'Tim^:
/No.:
kNo.:
^\
GC Column/nd J/D.: X^ X^
m/z
50
75
95
96
173
174
175
176
177
ION ABUNDANCE CRITERIA / /
8.0-40.0% of mass 95 / / /\
30.0-66.0% of mass 95 / / /
Base peak, 100% relative abundance / / / /
5.0 -9.0% of mass 174 ^ \^ / /
Less than 2.0% of mass 174 X^ ~\/ /
50.0 - 120.0% of mass 95 X^ <\
4.0 - 9.0% of mass 174 \^ \
93.0 - 101.0% of mass 174 \^
5.0 - 9.0% of mass 176 f~~" — — -^_
% RELATE ^

?


( )1

\, ( )l
X ( )1
\y ( )2
 1-Value is % mass 174
us in
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
strumeht performance check applies to the following\ampl£s, blaAks,/and standards:
EPA
SAMPLE NO.


/
/
c
^

	 .._. ^- 	 -—
/
/ /^~^*
/ /
/ /
/ /
^ \^
\^ "\
"\ ^
\^




LAB
SAMPLE ID
/ X
/ / \

/ /
\^ / /
\^^\V /
_ /
^\ X
k. \.
"X^ \
^\ \
X \
\ \

/
/ /
~\ / /
\y /
^\ /
xy


\LA^/
FILE ID /
\ \
^\
s — x ^^
/ \-_/



x^
^ ^
\y








/ DATE
ANALYZED
\
V
7


















TIME
ANALYZED





















of Form IV-A4VT
-------
             U.S. ENVIRONMENTAL PROTECTION AGENCY
                      CONTRACT LABORATORY PROGRAM
                       Volatile Organics in Ambient Air - Tenax

                       INITIAL CALIBRATION DATA AND
                       CONTINUING CALIBRATION CHECKf^y
Lab Name: Contract: / /
Lab Code: Case No.: y^AS^o.:
Calibration Times: Calibr/tion DateSx^
SOW No.: SDGNo<: /\ \
Instrument I. D.: GC Cofumn'and I.D.X^ ^\
j\y x^ x^
Lab File ID: RRF2 = / "> RRF5 = \ /
RRF10= RRF20= / / RRF100= ^

Tnchloroethylene
Chloroform
Benzene
Carbon tetrachloride
Tetrachloroethylene
1, 1-Dichloroethene
1 ,2-Dichloroethane
Chlorobenzene
1,1,1 -Trichloroethane
1,1,2- Tnchloroethane /
1,1,2,2,-Tetrachloroethane / ,
Ethylbenzene / /
Styrene ^-N.
1,1-Dichloroe thane
Toluene .^~ ~^~~^
Xylenes, o-, m/, &-X(-^ ~^.
1,2 Dichloropropane
1 ,2-Dichlorob«(Qzene
1,2-Dibromoetiwne ^^^
"Vx\ ^\
CALCULATED RllFs /\
CAL2








S- 	 	
/^~^
/
/
\y
\ '
^ ^
[^ \
\ N
)
i ,
j /
CAL5




/
\\
\

X
\\-
\ V
' /
/
\
X,^
^^
\
)
1

CAI/10
/ /
^'


~^^^
^^^
\ /
\ V
V
\
\.
"x^


>





/CAL20
/
\/
\
^
— —- ^_

/
/
K
v ">
V
— T
/








(/AL/lOO
/ /
/
\
\ \
^^
~?
*- " — /













AVG.
RRF



>
















RSD




















D




















Pa2e.
of
FORM V-AAVT-1
-------
Lab Name:
               U.S.  ENVIRONMENTAL PROTECTION AGENCY
                           CONTRACT LABORATORY PROGRAM
                            Volatile Organics in Ambient Air - Tenax

                            INITIAL CALIBRATION DATA AND
                            CONTINUING CALIBRATION CHECK

                                              Contract:
Lab Code:
                                      Case No.:
                      ,#AS$o.
Calibration Times:
                                                 Calibration DateSx^
SOW No.:
                                              SDGNo./
Instrument I.D.:
                                              GC Co/umn/and I.D?:
Lab File ID
                         RRF2 =
                      z
                      RRF5
RRF10=
                         RRF20=
              /   /   RRF100 =
CAL 2  CAL 5  CAL )/0  QAL 20
                                   CALCULATED' RR/s
                                                            {DO
                                                                 AVG.
                                                                 RRF
                                      RSD
2-Chlorobutane
1 ,3-Dichlorobutane
1 ,4-Dichlorobutane
3 ,4-Dichloro- 1 -butene
1 -Chloro-2,3-epoxypropane
2-Chloroethoxyethene
1 -Phenylethanone
Dibromomethane
1 ,3-Dichloropropane
1,1,1 ,2-Tetrachloroe thane
o-Chlorotoluene
1,3,5-Trimethylbenzene
p-Chlorotoluene
                   /
                                               y
n-Butylbenzene
m-Chlorotoluene
Benzaldehyde
 Benzonitrile
 Page.
         of
FORM V - AAVT-3
-------
           U.S. ENVIRONMENTAL PROTECTION AGENCY
                        CONTRACT LABORATORY PROGRAM
                         Volatile Organics in Ambient Air - Tenax

                   INTERNAL STANDARD AREA AND RT SUMMARY
    Lab Name:
 Contract:
                                                    SOW No.:
Lab Code: Case No.:
Date Analyzed:
Instrument ID:
SAS No.:
Time Analyzed:
GC Column and ID:
/
/
C
/SQQ No-X
/ \x
/ X. \
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21

12-HOUR STD
UPPER LIMIT
LOWER LIMIT
EPA SAMPLE NO.









Perfluoro-
toluene
Area #










/
/
/
i / /




L. — _ 	 _ _
/ /
/ V
\
\

y^ ^
/
/
/ /
/ /
/-"' 	 -^
/


C "X
\ \
RT
#










S^ "^
/ — ^
/ ^

/
/
X/ /
C
^\
\
X
\ \
\ \
\ \

1 /
1,2-Dichloro- /
benzene-d4 /
Area / #
/ <
\

, 	 _

\ \^^1
\ \
\ \ /
\ V
\
\ \
\
[^ — ~\
\
/ \^
/


\
\ X
^v




'/
/ *
\^ /
\y
\.

	 —
*~-7
/ /~~
/
/
V
\
\ \
\/

/










i
/7r ,
' /
/
\^
\>
«^
^7
1 	 /



















RT
#


























   Area Upper Limit = 4-40
   Area Lower Limit = -40% of i
  TdArea
   # Column used to flag values outsi
   * Designates values outside of QC li
                        RT Upper Limit = +0.50 minutes of internal standard RT
                        RT Lower Limit = -O.SO minutes of internal standard RT
     limits with an asterisk
limit
        of
   FORM VI - AAVT
-------
           U.S ENVIRONMENTAL PROTECTION AGENCY
                     CONTRACT LABORATORY PROGRAM
                     Volatile Organics in Ambient Air - Tenax
      Lab Name:
       Lab Code:
    Instrument ID:
    Date Analyzed:
                  TENAX TUBE ADSORBENT CERTIFICATE,
                         Contract:
                         Case No.:
                           SOW No.
                          GC Column & ID:
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
TENAX
IDENTIFICATION
Tube












•








/""
/ s
/ /
/ /
/ /
Batch


TOTAL ORGANIC^ /
ng/tube / /
/ ^
\ X,
\









/"
/ /
/ /
/ /
/ /
/ ^

\
^x
1 ^"-\
	 	 ^ x
X
\

£ \ i
\ "TV.


\ /
\ xy


/—— ~--^__
( ^~~~—-
\ \ — ' — ->
\ \ / /
\ \ / /
\ V /
\ <,
^X \ \
-^ \ \ \
\ l^-~^ \/

/ / \ /
/ / -
J /
c
\ \.
^\ x
X \/
\
s \

/
/ /
/
/
v/
/ACCEPT/REJECT*
/ /
/ /
c
^ ^\
\ "\
^ /
1 — -^__
^7
—-J












i


i





   •ACCEPT IF <10 ng TOTAC
-------
 Lab Name:
                U.S. ENVIRONMENTAL PROTECTION AGENCY
                           CONTRACT LABORATORY PROGRAM
                            Volatile Organics in Ambient Air - Tenax
                                SURROGATE RECOVERY
                              Contract:
 Lab Code:
                             Case No.:
                                                    S/S No.:
SDG No.
Lab Sample I.D.:
     EPA
 SAMPLE NO.
                               SURROGATE %
               Benzene-d6    #
                                 Chlorobenzene-d5   / # /
       TOTAL
        OUT
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
                                                  '  /
                                                    ^>.
                                 \
                                   \
                                     \  \
                                      \
                                          v
                                        \
                                              \
                       /
                                  \
                                             7
                   /
                              /  /
                           \
                               \
 Surrogate Recov
 #Column used to
 designates values outside

	of	
                              imits.
                                   FORM VIII - AAVT
-------
           U.S. ENVIRONMENTAL PROTECTION AGENCY
                        CONTRACT LABORATORY PROGRAM
                           •SAMPLE LOG-IN SHEET - Tenax
         Lab Name:
 Received By (Print):
 ase Number:
Sample Delivery Group No.

      SAS Number:
                                              EPA
                                            SAMPLE
                                           SIGNED
                                           LAB
                                                                                 SHIPMENT
                                                                                   ETC.
CIRCLE THE APPROPRIATE RESPONSE
1.  Custody Seal(s):

2.  Custody Seal Nos.:

3.  Chain-of-Custody
   Records:
4.  Traffic Reports or
   Packing List:
5.  Airbill:

6.  Airbill No.:
7.  Sample Tags:
                       Present/Absent*
                       Intact/Broken
                        Present/ Absent*

                        Present/Absent*

                        Airbill/Sticker
                        Present/ Absent*
                    \
                                   /
                        \
                                                  \
                               v  /
                        Present/ Absent*
   Sample Tag Numbers:    Listed/Not Liste
                        on Cham-ofCustodi'
8. Sample Condition:
9. Does information on
   custody records, traffic
   reports and sample tags agree?
 10. Date Received at Lab:
 11. Time Received:
Intact/Brok/n*/Lyfeaking[\i

Yes/N
 *If Circled, contac^SMO and attach record of resoluti
        Received by:
              Date:
                   Logbook No.
               Logbook Page No.
                                   FORM AADC-1
-------
              U.S. ENVIRONMENTAL PROTECTION AGENCY
                           CONTRACT LABORATORY PROGRAM
                            Volatile Organics in Ambient Air - Tenax
                          COMPLETE SDG FILE (CSF) DOCUMENT
                                   INVENTORY  SHEET
 Lab Name:
  Case No.:
  SAS No.:
                                                  City/State:
                             SDG No.:
                          Contract No.:
                     Rec
13. Internal Lab Sample Transfer Re/ord
           Tracking Sheets (descn
14. Internal Original Sample Preparation
           (describe or list)
           Preparation
           Analysis Rec
           Descnptio
15. Other Records (desofibe/or list)
           Telephone Communication Lo;
 Comments:
All documents delivered in the complete SDG file must be original documents
1.  Inventory Sheet (AADC-2) (Do Not Number)
2.  Cover Page
3.  Analysis Data Sheet (FORM I-AAVT)
4.  Tentatively Identified Compounds (FORM II-AAVT)
5.  Method Blank Summary (FORM III-AAVT)
6.  Surrogate Recovery (FORM IV-AAVT)
7.  GC/MS Instrument Performance Check and Mass
   Calibration (FORM V-AAVT)
8.  Initial and Continuing Calibration (FORM VI-AAVT)
9.  Internal Standard Area and RT Summary (FORM VI
10.  Tenax Certification (FORM VIII-AAVT)
11. EPA Shipping/Receiving Documents
           Airbill (No. of Shipments	)
           Chain-of-custody Records
           Sample Tags
           Sample Log-In Sheet (Lab & A
12. Misc. Shipping/Receiving Records (list yndivi
           Telephone Logs
            Completed by (CLP Lab):
                  (Signature) .
                                    (Prim Name &. Title)
(Date)
                                     FORM AADC - 2
-------
Exhibit B
                                                      SOW No.  XXX -  Ambient Air
3.3
      SEMIVOLATILES
                                                             ipletion of all
                                                             in  ambient  air.
3.3.1
            Complete SDG Fi,

        General Informat

      3.3.1.1     Val
      the individual
      must be fille
      be submitted i
      be submitted on
      This section contains specific instructions for  the
required Data Reporting Forms for analysis of semivolat;f
This section is organized into the following parts:

      •     General Information and Header Informati^

      •     Cover Page - [COVER PAGE - AASV]

      •     Analysis Data Sheet [FORM I - AASV],

      •     Percent Surrogate Recovery Form

      •     Sample Filter and Adsorbent Cei

      •     Method Blank Summary [FORM IV -

      •     GC/MS Tuning and Mass Calibration Form"-

      •     Initial Calibration Data-iFORM VI - AASV]

            Continuing Calibration^

            Internal Standard Area anoXKT\>ummc

            Sample Receipt/Log-In Form -\FORfr A&DC-1]
                                                           I - AASV]
                                                 .et - [FORM AADC-2;
                                                      copy forms according to
                                               Jfection.  Each form submitted
                                            analytes.  Multiple forms cannot
                               sne/form if the information on those forms can
                                        rs to the appropriate level of
                             followij^g common rules.  If the figure following
                                   thatWS, drop it (round down).  If the
                                 rop it and increase the last digit to be
                                    the figure following the last digit to be
                                   re no digits to the right of the 5 or all
                                   equals zero, then round up if the digit to
                                   down if that digit is even.

                                 which appear on the data reporting forms
                                must be reproduced by the Contractor when
July, 1991
                                                                   Page B-l/SV
-------
Exhibit B
                                                      SOW No.  XXX - Ambient Air
      submitting data, and  the  format  of the  forms  submit
      to that shown  in the  contract.   No information may
      moved from its specified  position  without  prior w
      EPA Project Officer.  The names  of the  various
      (e.g., "Lab Code",  "Naphthalene")  on  the forms
      the forms, except that the use of  uppercase a
      optional.

      3.3.1.4     All alphabetic entries made or
      must be in ALL UPPERCASE  letters.

      3.3.1.5     Six pieces of information are  common tjt
      of each data reporting form.  These affe: /Lab  Nan
      Code,  Case No., SAS No.,  SDG No, and/SOU/No.   This
      entered on every form and must matcHon all forms./
                                             lust be identical
                                            .dded,  deleted, or
                                             approval of the
                                           and analytes
                                                as they do on
                                                  ters is
                                                           or
                                          ie header  sections
                                         Zontrac t  No.,  Lab
                                        Information  must be
                  3.3.1.5.1   The "Lab Name" is^he name chosen by the
                  Contractor to identify the labora^ory/^xlt may not exceed  25
                  characters.
                  3.3.1.5.2   The
                  contrac t,  inc lu>
                  performed.
                                  the numbeV of the  EPA
                                          he analyses were
                  3.3.1.5.3   The "Lab XodeN? i/s afi alphabetic abbreviation of
                  up to 6 characters, assj.gne4 by the EPA, to identify the
                  laboratory and aid in da\a piiocessing.  This lab code shall
                  be assigne«i-"Dy-\jphe /Case No." is the EPA-assigned Case number
                  (up to^sS characters) associated with the sample and recorded
                  on the TR>
                             \  \
                                       Na." is the EPA-assigned number for
                               ormed u>vd4r Special Analytical Services (SAS) .
                             are^to be analyzed under SAS only and reported on
                                  n enter SAS No. and leave Case No. blank.
                                  palyzed according to this SOW (Routine
                                   es protocol) and have additional SAS
                                  !en list both Case No. and SAS No. on all
                                  .nalyses have no SAS requirements, leave "SAS
                                 TE:  Some samples in an SDG may have a SAS
                                ers may not.
                                                 Page B-2/SV
-------
Exhibit B
                                    SOW No.  XXX - Ambient Air
3.3.1.5.6   The "SDG No."  is  the  Sample
number.  The SDG number  is the EPA  sample
first sample received  in the  SDG.   Wheta
received together in the first SDG  sWipi
must be the lowest sample number  (cpnsi
numeric designations)  in the  first
under the SDG.
                                                              ivery Group (SDG)
                                                              lumber of the
                                                            :veral  samples are
                                                           Tit,  the SDG number
                                                            ing both alpha and
                                                               samples received
3.3.1.5.7   The "SOW No." is
indicates the Statement of Woi
data package have been perfWmec;
the cover of the contract SjOW.
                                                     PA-des ignatetfxiumbe>xhat
                                                    ider which  analysfe&in
                                                     The  SOW No.  appears\6n
      3.3.1.6     The EPA sample number is /the/unique fdenfcifying  number given
      in the TR that accompanied that sample./ This nombesr  is  assigned by the
      EPA and it must be used exactly as
            3.3.1.6.1   The "EPA SAMPLE No." mbs± be
            forms.  This number appears either
            of the form, or as the left column of a
            from a number of sampl
                                     ^tered  on  several of the
                                    upp-eq: right hand corner
                                            Qarizing data
            3.3.1.6.2   All field^ampies-^aiidquality^cTrntrpl  samples
            associated with field samples mustTT&e idejitified with  an EPA
            sample number.  In addition,\:he sample suffix and quality  control
            sample abbreviations listed^ in\Taole/B-2, Section  2 of this
            Exhibit must be used as appropriate
3.3.1.7     All resu
with the specified/numb
Exhibit B.  The rdw data f
figures in the r^w data result
specified for that/result
figures in the/ray data r(
result, then ./zerosvmust
number of repo
following examples^ajre pro;
                                   be transcribed to the forms  in  the  raw data
                                of Decimal places\that are described in
                                  ul]t Ji to beNrounded only when the number  of
                                             thexmaximum number of figures
                                                 rm.  If there are not enough
                                     to erffcer i/h the specified space for  that
                                      for decimal places to the specified
                                   for that result for a specific  form.   The
                                 ided:
               us
   Raw Data ResuJ
              siecifb;
                                   Format
Correct Entry on Form
NOTE:  6.3 stan
decimal places
                                                                 5.900
                                                                 5.997
                                                                95.997
                                                               996.00
                                                              9996.00
                                                             99996.
                                                               invalid
              of six significant figures  and  up  to  three
July, 1991
                                                  Page B--3/SV
-------
Exhibit B
                                                      SOW No.  XXX -  Ambient Air
      3.3.1.8     Before evaluating  a  number for being in /onErol  or out of
      control  in.relationship  to  a certain limit,  the number/evaluated must be
      rounded  using  EPA rounding  rules to the significance /eported for that
      limit.   For instance,  the control limit for a suifroga^e  compound is 35
      to  150 percent of the  true  value.   A percent reovery vkiue  of 150.4
      would be  considered  in control while a value
      considered  out of control.   In addition,  a c
      would be  in control  while a calculated valueqf150.55 woul
      control.
3.3.2  Cover Page [COVER PAGE - AAVC]
                                         al
3.3.2.1  This form is used to list
an SDG, and to provide certain analy
comments.  It is also the document
Manager to authorize and release all
with the SDG.
     3.3.2.2  Complete the header  information
     section.
     3.3.2.3  Under "EPA Sample N
     Sample No. (including duplicates )or
     SDG.  These sample numbers mustNae \istec
     alphanumeric order using the Exte
     Code convention.  Thus, if MAB123A
     and numeric characters) EPA Sample Nc\. wi
     entered in the f irst EP2T~SaHiple No.
     would be in ascending sequence^ - MAB124
     MA1111A, MAI 11 IAD, /etc
     3.3.2.4  All EPAs
     order, continui/g
>le  numbers must be^1
 the fo/ilowing Cbver
                                                            s analyzed within
                                                            and  general
                                                         y  the  Laboratory
                                                       Verables associated
                                                         t 1 of  this
                                          to 7~c~ha&ajc_ters for the EPA
                                           reouired analysis within  the
                                          'on/thefoTE in ascending
                                             Coded Decimal Interchange
                                          .owest (considering both alpha
                                          :hin the SDG, it would be
                                            Samples listed below it
                                             •124B,  MAB125A,  MAC111A,
                                          ited in ascending alphanumeric
                                          age if applicable.
     3.3.2.5  Under^^^ab SainpJ^- Itf," a Lab Sample ID  (up to 10 characters)
     may be entered fors-each associated EPA Sample No.  If a Lab Sample ID  is
     entered, it must be erl^red identically  (for each EPA Sample No.) on all
     associated
                       ~-\    \  >
                                          problems encountered, both
                                e, the corrective action taken, and
                              al^, of the samples in the SDG.

                                   be signed, in original, by the Laboratory
                                 ignee, and dated to  authorize the release
                                 11 data and  deliverables associated with an
July, 1991
                                                              Page B-4/SV
-------
Exhibit B
                                                SOW No. XXX  -  Ambient  Air
3.3.3  Analysis Data Sheet [FORK I - AASV]

     3.3.3.1  This form  is- used to tabulate  and report
     results fo-r target  analytes  (Exhibit  C) .
                                                        e  analysis
     3.3.3.2  Complete  the header  information accor
     instructions and as follows.
     3.3.3.3  For "Lab Sample  ID," enter  the  lat
     listed on the Cover Page.
3.3.3.4  For "Date Received," enter  the,
sample was received at the laboratory,
(TR) [i.e., the Validated Time of Sam?

3.3.3.5  For "Date Extracted," ente
sample cartridge was extracted.

3.3.3.6  For "Date Analyzed," enter  the
sample extract was analyzed.

3.3.3.7  Enter "Instrument I
Volume."
     3.3.3.10 Enter t.

     3.3.3.11 Under
     result is gre
     Limit (CRQL),
     report the CRQL va
     an analyte is 5 ng an
     will be
     injected/and
     ambien
                                                                       as
                                                   (formatted MM/DD/YY)  the
                                                            the Traffic  Report
                                                        :atted MM/DD/YY)  the

                                                          ed MM/DD/YY)  the

                                                             ?
                                                             njection
     3.3.3.8  Enter the "Air Volume
     temperature and pressure  (STP)
     not known, enter "NA".
     3.3.3.9  Enter the d
     M 1 II
                                            rected to standard
                                               of ambient air sampled is
                                       no Dilution was performed, enter
     ambie
     in
                                          'RATION," if the analytical
                                to the Contract Required Quantitation
                             It.  If the result is lower than the CRQL,
                           [wed with a "J".  For example, if the CRQL of
                               cted level is 3 ng, the reported value
                                     CRQL is expressed in ng on-column
                          coramns  hould be filled if the volume of
                         own to cne laboratory.  If the volume of
                           known to the laboratory, then only the levels
                  columh is\ reported.
     3.3.3.13 The
                             ;ust be reported to two significant figures
                            than 10, and to three significant figures if
                        tei? than or equal to 10.

                         for reporting results to two or three
July, 1991
                                                              Page B-5/SV
-------
Exhibit B
                                                      SOW No. XXX - Ambient Air
      significant figures applies to Form I-AASV only.
      instructions- for reporting all other results on re
      described in this Exhibit.

      3.3.3.14  Under  the  columns labeled "Q",  enter
      identified in the following paragraphs.   If ad
      used,  their explicit definitions must be incl
      the  Comments section.
                              Llo;/ the specific
                                id forms as
     3.3.3.15 FORM  I-AASV  includes  fields  for
     qualifiers  are defined as follows:

     •  U  -       Indicates compound was  ana
                  numerical value  is the  sa
                  corrected for dilution.
                  if the sample final volume
                  volume.   If a 1  to 10 dilution
                  limit is  100 U.
                       ft qualifiers.  These
                     for but n/t detected.   The
                   quantisation limit and must be
                     npler, LO U for acenaphthene
                   the protocol-specified final
                       necessary, the reported
        N
     •  B
                                   zntration
Indicates an estim
estimating a cone
compounds where a
spectral data indie
the identification cri,
sample quantitation limit
sample quantitation limi
ng is calculated, report
must be
Indicate;
only us^d
identi/tic>
                                         ;alue.   This  flag
                                           is
                            ustec
        [or diluti
      iptrve evidenc
 'or te>ktatji3»lv ideni
Xion is)based onNnass
                 is at
to alV Ti
                                          ults
                                   ed either when
                         itiyely identified
                       assume~anor when the mass
                             	 impound that meets
                       e result is less that the
                     eater than zero.  If the
                     ng, but a concentration of 3
                    3J.  The sample quantitation
                      discussed for the "U" flag.
                       ,a compound.  This flag is
                        d compounds, where the
                       ectral library search.  It
     fl3
                           is
          the
                          tfi*
                 indicate
                 the data us
                   Se~ar~fT>s^,a
                 compound.
        bn the sample Form I when the analyte  is
        :iated blank as well as in the sample.   It
 ossitt^e/probable blank contamination and warns
            appropriate action.  This flag must be
              is for a positively identified  target
                 The combina^ion\of flags  "BU"  or  "UB"  is  expressly
                 prohibited. \Blal»k contaminants are  flagged "B"  on
                 they are detedted\ in  the  sample.
                                          when
                   jis flag  identities compounds whose  concentrations  exceed
                       litial ^calibration range of  the  instrument  for  that
                   ^eciti^aryalyssis.  If one or more  compounds  have  a  response
                  thatvaxceed  tne  initial calibration range,  the sample or
                  extract^snust/be  diluted and reanalyzed  according to  the
                  specifications in Exhibit D. All  such compounds  should have
July, 1991
                                       Page B-6/SV
-------
Exhibit B
                                                      SOW No. XXX - Ambient Air
                  the concentration flagged with an "E" on
                  original analysis.  The dilution of the/s
                  some compounds identified in the firstam
                  the calibration range in the second
                  of both analyses shall be reported on separate
                  Form I for the diluted sample shall/hay^e th
                  appended to the EPA Sample Number
                                                          Form I for the
                                                         le may cause
                                                        ysis to be below
                                                            The results
                                                            Forms I.   The
                                                          "DL" suffix
     NOTE:   For total xylenes ,  where . three isom^rs^are quantified
     peaks,  the calibration range of each peak/should be considered
     separately,  e.g.,  a diluted analysis is /ot /required for total xylenes
     unless  the concentration of either peak/separate ly/e^ceeds 25
                  If  a  sample is diluted and reanalyze/l, As in the "E" flag
                  above,  all concentratioi/ values renc-rteci on that FORM I-AASV
                  are flagged with the "D" TOsag.^lEbfe "J3L" suffix is appended
                  to  the  EPA Sample Number on th^ FORM^J-AASV for the diluted
                  sample.
            Other specific fl
            results.  If use
            description atta
            the SDG Narrative
            flag is required,
            five qualifiers are fHau^red/ f
            "X" flag to combine seVe^raVf]/ags
            the "X" flag might combi
            some samp
                                       may be required to^properly define the
                                     they~~fflu»e-b^fully described and such
                                              Sample~~Dar6a->Suinmary Package and
                                                     "X".   Lf more than one
                                                     asneTeded.   If more than
                                                   a sample result, use the
                                                     as needed.   For instance,
                                                      "B",  and "D" flags for
3.3.4
TIC]
  Tentatively Idenfifi
            ids Analys:
ita Sheet [FORM I -  AASV-
     3.3.4.1   FORM  L^AA/V-TIC is/usefd for^epo/ting the identification and
     estimated concentration for up to 10 ofche non-surrogate and non-target
     organic compouhd§  inthe/Volatile fraction.
      3.3.4.2'   Include  a FO
      evaluat
      for  eve
including
                   ar
     I-AAS^-TIC for every sample, performance
        k analyzed.  FORM I-AASV-TIC must be provided
   ,t requii^s a^FORM I-AASV-TIC for target compounds,
dilutions andxffeanalyses, even if no TICs are  found.
      3 .3. y. 3 /Complete  the WsadeV information according to the header
      instfruc/eions  in parts 3A.l\and 3.2.3 of this section.

                  il  the numbeir o| TICs found, and enter this number in the
      "No.  or^TICs^und."  If/no/TICs were found,  enter "0" (zero).
3.3.4.5  Analy^ej-cal
if the result valtie. is
                            sul:ts must be reported to two significant figures
                              ess than 10,  and to three significant figures if
July, 1991
                                                              Page B-7/SV
-------
Exhibit B
                        SOW No. XXX  - Ambient  Air
     the result value  is greater  than or equal  to  10.

     3.3.4.6  Report tentatively  identified compounds
     number, compound  name, retention time, and the  e;
     (criteria for reporting TICs are given in  Exhi
     must be reported  in minutes  and decimal minut
     and seconds.
     3.3.4.7  If in the opinion of the mass spe/trs
     specialist, no valid tentative identification'can be made,  the  compi
     shall be reported as unknown.
                              ;)  including CAS
                                  concentration
                                   jntion time
                                         minutes
                                          ;ore
                                                 in
3.3.4.8  If the name of a compound exoeed/ the
column, truncate the name to 28 chararte/s.  If
unknown, restrict description to no
unknown hydrocarbon, etc.).

3.3.4.9  The requirement for reporting result
significant figures applies to Form I only.  Fol
instructions for reporting aH/-~&ther_ results on
described in this Exhibit.
                          'spaces  in the  TIC
                            /compound is  an
                           laracters (i.e.,
                                                          the
                                                      requl
     3.3.4.10 Under the columns labe
     identified in part 3.2.3 of  thisN
     used, their explicit definitions
     the Comments section.

3.3.5  Surrogate Percent R

     3.3.5.1  FORM II-
     compounds added t
      3.3.5.2   Compl
      according to
                    each  FORM  II-AASV  required,
   ns/in parts 3.2.1 and  3.2.3 of  this section.
                               or  three
                                   ecific
                                  'forms  as
                              ualifiers as
                            onal  qualifiers  are
                    luded on  the  Cover  Page  in
                      covery  of  the  surrogate
      3.3.5.3   In the
      described in Section
      for  each  s
3.3.6  Sampl
      3.3.6.1  This
      analyses of the
     EPA Sample Numbers  for  each  analysis  as
       ,ch sample, report the percent  recovery
           'hole number.
           7
     reco^fery outside  the QC limits with an
    lust be placed next to the appropriate  value
     r righthand  column, total the number  of
     the QC  limits  for each  sample.   If no
     imits,  enter "0".

rber(t Certification Form [FORM III -  AASV]

;eti to report total  analyte levels from optional
    adsorbents,  if performed, and the  required
 July,  1991
                                       Page B-8/SV
-------
Exhibit B
                                                     SOW No. XXX - Ambient Air
     analysis of at  least  one  pair,  or 10  percent  of each
     greater, of filter  and  adsorbent  cartridge  assembly^

     3.3.6.2  Complete the header  information accordi
     instructions  in parts 3.2.1 and 3.2.3 of this s

     3.3.6.3  Enter  "Extraction I.D.",  "Filter Bat
     I.D.", "PUF Batch I.D.",  and  XAD-2 Batch I.D/"
     information should  be correct for all the
     the table.
                                                              ch, whichever is
     3.3.6.4   In  the  table,  enter  the  EPA S
     batch of  filters/adsorbents/cartridge
     FORM III-AASV  as necessary.

3.3.7  Laboratory Method Blank Summary  [

     3.3.7.1   FORM  IV-AASV  lists the samples
     method blank (1MB).  A copy of the appropriat
     for each  method blank.
     3.3.7.2   Complete  the header/i
     according to  the instruction;
     3.3.7.3  Summarize the samples
     below the header, entering EPA
     the Lab File ID and Time Analyzed
                                  informatio
                                                 Numbers^for a particular
                                                           s many page  of
                                                . 1 and
                                                        with each  laboratory
                                                                 is  required
               FORM IV-AASV required,
                     of this sections.
                                            eac
         '/th a given  LMB  in the" table
        ir and Lab  Sample ID.   Enter
         sample.
      3.3.7.4   Under  "Comm
      technical and administr.
      resolution performed for  all
                                      any problems encountered, both
                                    fhe correc\ive\action taken, and
                                                    the SDG.
3.3.8  GC/MS Tuning ahd riass Calibrat
  sample

  FFOE
                                                  - AASV]
     3.3.8.1  This/form^is use*
     summarize the
     blanks, associatedVVith eaa
                                    report the results  of GC/MS tuning,  and to
                                 /of analysis of samples,  standards,  and
                                   GC/MS tune.
      3.3.8.2
      accordi
                         e heac
                    e  instructions"'
      3.3.8/3 /Enter the "L^b File ID"  for the injection containing the GC/MS
      tuning Compound,  DFTPP.X "rvter the date and time of injection of the
      turyina/compound.   Enter \..jaction time as military time.
nation on  each  FORM V-AASV required,
irts  3.2.1 and  3.2.3 of this  section.
      3.3:i
      % Relatl
      ab undanc e s to the"*
      the ion abunda?
                                   for  each  ion  listed on  the  form,  enter the
                                  righthand  column.  Report  relative
                                  significant  figures given  for each ion in
                               a  column.
 July,  1991
                                                                   Page  B-9/SV
-------
Exhibit B
                                                      SOW No.  XXX - Ambient Air
      3.3.8.5   All  relative  abundances must be reported as
    '  enter  "0",  not  a dash  or other non-numeric charact
      appear,  compute the  percentage of the ion abundan
      the appropriate footnote,  and enter that value i

      3.3.8.6   In the lower  half of the form,  list
      blanks analyzed under  that tune in chronologi
      analysis  (in  military  time).   Enter "EPA S
      "Lab File ID",  "Date Analyzed",  and "Time Mat
      standards,  samples,  and blanks.

3.3.9  Initial Calibration Summary  [FORM VI
                                       iber.  If zero,
                                      ere parentheses
                                    the mass given in
                                    arentheses.

                                                  and
     3.3.9.1  After a GC/MS has  undergone
     all initial calibration  technical  cr
     must complete and  submit  all  Form  Vis
     calibration performed which is  relevant  to"
     SDG, regardless of when  that  calibration was
     3.3.9.2  Complete  the header  iafojrmation on each FO&KVI-XASV required,
     according  to  the instructions/in parts~~Jr3-~Land 3.2.3 tff this section.
                                 Oration, and after
                                  met, the laboratory
                                  each initial
                               )les and blanks in the
     3.3.9.3  Enter the  "Case No." «hid ^SDG No"
     package, regardless  of  the  original\ase
     calibration was performed.  Enter
     Analyzed".  If the  calendar date chatJgei
     procedure, the inclusive dates  should\be
     3.3.9.4  Enter the
     Prepared".

     3.3.9.5  In the
     calibration sta
     the calibratio
     for each target Mqmpou:
     average RRF and  the
     for each target  compoui
             bration
3.3.10  Multicjainponent Analyses In
  fo*__£hecurrent data
ror/vhichtne  initial
le/t ID" and -"Date(s)
 iring the calibration
i,iven on FORM  VI-AASV.

    irds were  prepared on  "Date
                         D"  for each of the
                       :he response factor data for
                   response  factor (RRF)  is reported
         'surrogate.   The laboratory must report the
         relative standard deviation (%RSD) for RRF
            rrogate.
                 libration Summary  [FORM VI-AASV-MC]
     3.3.10.1  After a GC/MS^has ^undergone an  initial calibration,  and after
     all  initial  calibration technical  criteria have been met,  the laboratory
     must/complete  and  submit a\l  Form  Vis  that apply for each initial
     cal-^bratr«n  performed whicn ia  relevant to the samples and blanks in the
     SDG, regardlfe^s of  when that  Calibration was performed.
    3.3.10.2  CoihpJ.ete
    required, accorc
    section.
     ade'r  information on each FORM VI-AASV-MC
to^the/instructions in parts 3.2.1 and 3.2.3 of this
July, 1991
                                          Page B-10/SV
-------
Exhibit B
                                       SOW No. XXX  - Ambient  Air
    3.2.10.3 Enter the  "Case No."  and  "SDG  No."  for the current data package,
    regardless  of  the  original  Case for which the initial/calibration was
    performed.   Enter  "Instrument  ID",  Column I.D., and/"Da/te(s) Analyzed".
    If  the  calendar date  changes during the calibratio^l procedure, the
    inclusive dates should  be given on Form VI-AASV^
    3.3.10.3
    Prepared"
Enter the date the calibration stan
    3.3.10.4  In the table, enter the  "Amount  (rig)"> for each of the"
    multicomponent standards  injected.   Comple.ce che RT and relative response
    factor  (RRF) for each  quantitation peak of the calibration standards.
    The RRF is reported for each multicomponent/analyte/ahd surrogate.
on "Date
3.3.11  Continuing Calibration Summary [FOl
                                CI - AAS
    3.3.11.1  The Continuing Calibration Summary
    verify the calibration  of  the  GC/MS  systen
    calibration standards.  Form VII  is  required'"
    period.
                                         II-AASV is used  to
                                     the^analysis of  specific
                                        each^!2-hour  time
    3.3.11.2  Complete the header/Informal
    according to the instructions\in
                                   each FORM VTl-AASV required,
                            3.2.1 oT~t!Trs-sec.tion.
    3.3.11.3  Enter date and time of\onbinuing" calibration  standard
    analysis, the Lab File ID of  the ckntifcmimg /calibration  standard,  and
    date of  initial calibration.  Give  rnclusiye  dates  if initial calibration
    is performed over more than one date .\Entier  the average relative
    response factor (RRF) &3r~~ea<&h target  c^mpoWid that was  calculated from
    the initial calibration data  (deferred to**.inNrhe initial calibration
    date(s)  analyzed fi/ldX" Reborn the relative ^response factor for  each
    target compound ana surrogate] from  ttiexcontfauing calibration standard
    analysis.  The RRF frVllT^ASV fsused tbxysummarize the peak areas and  retention
    times rm/must be completed each time an initial
    calibration or^a^continuirng/calibration is performed,  or when samples are
    analyzed  und«ir  the\same/GC/MS  tune as  an  initial calibration.
July, 1991
                                                    Page B-ll/SV
-------
Exhibit  B
                                                      SOW No. XXX - Ambient Air
     3.3.12.2  Complete the header information on each FORM VIll-AASV
    •required, according to the instructions in parts 3.2/1 /nd 3.2.3 of  this
     section.               .                            '   '
     3.3.12.3  Enter  the  Lab  File  ID,  Date  Analyzed,  pate/vRece'rve.d,
     Extracted, and Time  Analyzed for the continuing/calibration
     samples are analyzed immediately following an
     another GC/MS tune and a continuing calibrati
     completed for the initial calibration standard
     concentration as the continuing calibratio
     ID,  the date and time of analysis,  the ar
     initial calibration  standard in place  of/tho^e of
     calibration standard.
                                                                    Date
                                                                    .ndard.  If
                                                           calibration-,, before
                                                      Torm VIII sHMLJ. be
                                                     hat is the same
                                                    mdard.   Enter the
                                                   md retention times of this
                                                             inuing
     3.3.12.4  From the results of  the analysis
     standard, enter  the  area measured  for ea<^i  inf
     retention time under the appropriate  columhxm  the
     STD".   For  each  internal standard,  calculate t
     area  of the particular  internal  standard plus 40
     the area lower limit as  the  area—o_fdie  internal
     percent of  its area.  Report these  va]
     LIMIT"  and  "LOWER LIMIT"  respjqtr!
                                                     tinuing calibration
                                                     standard and its
                                                   row  labeled  "12  HOUR
                                                  areaxupper limit as  the
                                                            its  area,  and
                                                  standard ^inus  40
                                                          eled  "UPPER
                                                  the boxes
     3.3.12.5  For each internal standard,\calcyiatzfe the detention  time  (RT)
     upper  limit as  the RT of the  partidulaki/tez4ial  standard plus 0.50
     minutes.  The lower  limit is  the  RT  6f the /internal  standard minus  0.50
     minutes.  Report  these values in  the b\xes(labeled "UPPER LIMIT"  and
     "LOWER LIMIT" respecti;  	
                                        ana ly z e>
                                             and'
              This form is use
              ontainers and  s
            d  foixeach  shippin
3.3.12.6  For each
calibration, enter
internal standard/an
is outside the
with an asteris,

3.3.12.7  If sample
calibration as describe
standard
standards
                                                    •er a given continuing
                                                     area measured  for  each
                                                   the  internal standard area
                                                .ted above, flag that  area
                                  rzed immediately following an initial
                                     enter  the  EPA Sample Number,  internal
                                         for  all  of  the  initial calibration
3.3.13 Samp/e Log-In Sheet 1-fORSvAADC - SV-1]

                                td document the receipt and inspection of
                               plels.  One  (1) original FORM AADC-SV-1  is
                               container.

    3.3.13.2  Ifxthe samples/in/a single shipping container must be assigned
    to more  than oriexSDG, Ther/the original  FORM AADC-SV-1 shall be placed
    with  the deliverable^ for/the SDG of the lowest alphanumeric number and a
    copy  of  FORM AADC-SV-iNsdst be placed  with  the deliverables for the other
July, 1991
                                                                  Page B-12/SV
-------
Exhibit B
                                                 SOW No. XXX  -  Ambient Air
                                                              and the location
                                                           nine the shipping
                                                           jals and their
                                                                •1.  Record the
SDG(s).  The copies should be identified  as  "copy(ies
of the original should be noted on  the copies.

3.3.13.3  Sign and date the airbill (if present)
container and record the presence/absence of cus
condition (i.e., intact, broken)  in item  1 on F<
custody seal numbers in item 2.

3.3.13.4  Open the shipping container, remove^
documentation, and record on FORM AADC-SV-l/tems  3-5,  the
presence/absence of chain-of-custody  records/, SMO forms  (i.e.,
Reports, Packing Lists), and airbills or/airbill  stickers.   Specify if
there is an airbill or an airbill sticker p/resent i^^tem  5  on FORM AADC-
SV-1.  Record the airbill or sticker nvunber  in ite
3.3.13.5  Remove the samples from the' shi?{
samples and the sample tag  (if presenfe%.  and^tgcoi
sample bottles (i.e., intact, broken, leaking)
absence of sample tags in items 7 and 8 on FORtJ AAU
                                                         iner(s),  examine the
                                                         the condition of the
                                                       d the presence or
                                                          5V-1.
    3.3.13.6  Review the sample shipE^ng documents and
    information.  Compare  the  infyrmatioiT~re«aided on all
    samples, and circle the appropria$e-~answer inTi
    3.3.13.7  If there are no probleihs ol^serve
    (include time) FORM AADC-SV-1,  the\ichadn/of;
    write the sample numbers on FORM AABC-sV-1,
    entered, enter the corresponding air yplume
    meters  (std. m©) in the-"ap~|nsQpriate columnN
    sample  tags and assigned laboratory numb\rs
    date should be reco/rdedx"at^fche Vopof  FOI
    time of sample receipt at th&\ laboratory  shi
    and 11.  Cross our unused columns—and
                                                          te the header
                                                           documents and
                                                         FORM AADC-SV-1.
                                              iring feteipt, sign and date
                                            'custody record, the TR, and
                                             For each sample number
                                            sampled in standard cubic
                                             Record the appropriate
                                             ,f applicable.  The log-in
                                               -SV-1, and  the  date and
                                              .d be recorded in items  10
    3.3.13.8  If tb^tere
    air volume samplred is
    marked with an aste^?4sk
    and document the resol
    Following
    precedin
    problem
3.3.14  Complet

    3.3.14.1  This
                       problems observed curing receipt (e.g., data on
                              for one or more samples) or  if  an  answer
                               "absent*") was circled, then contact SMO
                        ion 6sSxthe problem on a CLP Communication  Log.
                            ,nd da
-------
Exhibit B
                                                      SOW No. XXX  - Ambient  Air
                                                           /  ^
     Sample  Delivery Group  Case  file  (CSF)  documents which/art
    •Region.
sent to the
     3.3.14.2  Organize all EPA-CSF documents  as  described ^Exhibit  B.
     Assemble  the documents in  the order specified on/FORM AAfr&^SV-2 and
     Exhibit B, and stamp each  page with the  consecutive/numbersi^Dp not
     number the AADC-SV-2 form).  Inventory the  CSF/by
     numbers and recording page number  ranges  in thS^yolumn  providd on
     AADC-2.   If there are no documents  for a  spacirTlc document  typeS«nter"
     "NA" in the empty space.
July, 1991
   Page B-14/SV
-------
                U.S. ENVIRONMENTAL PROTECTION AGENCY
                     CONTRACT LABORATORY PROGRAM
                     Semivolatile Organics Compounds Analysis In Air
                                    Cover Sheet
Lab Name: '
Lab Code:
SOW No.:
Contract No.: / /
Case No.: / /
SAS No.: /SDGSte.:
      EPA Sample No.
   EPA Analysis No.  AO
                                     \ \     77
Comments:
                                  /
I certify that this data pac_kagejs in cofftpjianceswijh the terms and conditions of the contract, both
technically and for cx5mpletenes~s>fQr otherthan th^Bpnditions detailed above. Release of the data
contained in this Mardcopy-dataDackage and ifYttieyComputer-readable data submitted on floppy
diskette has be^n aphorized bylhe^Laob^atory Manager's Designee, as verified by the following
signature:
Signature:,
              Name:
Date:
              Title:
Page	of
COVER PAGE-AASV - 1
June 17, 1991
-------
               U.S. ENVIRONMENTAL PROTECTION AGENCY
                  CONTRACT LABORATORY PROGRAM      EPA Sample NO
                       Semivolatile Organics Compounds in Air
                              Analysts Data Sheet
 Lab Name:.
 Lab Code:
                  Contract No.:_
                  Case No.:	
 Lab Sample I.D.:_
 SAS No.:
SDG No.:
 Date Extracted:.
 Instrument I.D.:
 Injection Volume:	^
 Air Volume Sampled; (Corrected to STP):
Matrix: Air
Date Received
Date Analyzed:  /
GC Colui
Dilution f acti
CASRN
83-32-9
208-96-8
98-86-2
116-06-3
309-00-2
62-53-3
120-12-7
22781-23-3
92-87-5
56-55-3
50-32-8
205-99^2
19^-97/2
/1 91 -,24-2
^207^8-9^
100^M3
319-84-6
58-89-9
92-67-1
84-74-2
COMPOUND
Acenaphthalene / -~^_
Acenaphthalene \ \ — — -^
Acetophenone \ \ /
Aldicarb \ V /
Aldrin ^ 	 ^ \ \
Aniline / ^ — ^^ \ \
Anthra^en/ ^) ^ ^\ ^
Ben^iocarb / /^~^\ "7
Ben2idin>\ / /
Benzo(a)anthracen^
^Bjen2Q(a)Pyrene\^ ^\^
^B«KQ{b)fluoranthenex\^ /
8enzo(e)pyrene \
Ben2o(g,h,i)per^len^
Benzo(k)fluorartynenjB
Bei^l alcoho/ /
^alpba-BHCV /
gamma^&K^/Lindane)
p-Biphenylamine
Bis(n-butyl)phthalate
^ CO>IQENTRATJON
^ v
^^
" — ^^_j
/
/ ~^


\
/













\ng/m3
V

-

















Q




















Page	of
           FORM I - AASV - 1
                          June 14. 1991
-------
             U.S. ENVIRONMENTAL PROTECTION AGENCY
                 CONTRACT LABORATORY PROGRAM      EPA Sample NO.
                     Semivolatile Organics Compounds in Air
                             Analysis Data Sheet
Lab Name:.
Lab Code:
Lab Sample I.D.:_
SAS No.:	
SDG No.:
Date Extracted:_	
Instrument I.D.:_	
Injection Volume:	  u|
Air Volume Sampled; (Corrected to STP):
Contract No.:
Case No.:	
Matrix:  Air /
Date Received:
       ^^
Date
                               nrr
CAS RN
85-68-7
133-06-2
5103-74-2
5103-71-9
57-74-9
59-50-7
106-47-8
111-91-1
111-44-4
1 897-45-6
2921-88*2"
2lXoi;'9r'
1/61^2(2-1
/ 72^54-8
^-^-55^
50-29^
333-41-5
53-70-3
62-73-7
1 1 5-32-2
COMPOJUND^
Butylbenzylphthalate^ T^___
Captan \ \ ~~J
gamma-Chlordane \ \/ /
alpha-Chlordane \ (
Chlordane^fTechnica^ \ \
4-Chlofch3/fnethylp^enV — \ \
4-C/Horpaniline / ^ — ^ ^^^-7
^(2-4ilc*oetho^)m^tnane ^^-^
Bis(2^hlo7b>tb(yO€?rier
Chlorothalbni^ ^\^
Chiorpyhtos^ ^\^ ^^
^hryseh^ N^ ^
Dacthal (DC^A) \
4,4'-DDD )
^,4'-DDE / /
^4,4^00^ / /
DiazJnon /
\y
Dibenzo(a, h) anthracene
Dichlorvos (DDVP)
Dicofol
^x^ONCElslTRATlON
ng\^

r——-~J



$_














/ng/m3




















Q




















-------
              U.S. ENVIRONMENTAL PROTECTION AGENCY
                  CONTRACT LABORATORY PROGRAM      EPA sample NO.
                      Semivolatile Organics Compounds in Air
                             Analysis Data Sheet
 Lab Name:.
 Lab Code:
                 Contract No.:.
                 Case No.:	
 Lab Sample l.D.:_
 SAS No.:	
SDG No.:
Matrix: Air
Date Receive
 Date Extracted:.
 Instrument I.D.:
 Injection Volume:_j	yj
 Air Volume Sampled; (Corrected to STP):
CASRN
60-57-1
84-66-2
105-67-9
131-11-3
534-52-1
51-28-5
121-14-2
959-98-8
33213-65-9
72-20-8
7421-93-4
533-4^
n^ai-T''
2436-44^0
/ 86^-7
133^7-3
76-44-8"
1024-57-3
118-74-1
77-47-4
COMPOUND
Dieldrin / — — _^__
Diethyl Phthalate \ \^—- ^^_
2,4-Dimethyl phenol \ \ /
Dimethylphthalate \ \/ /
4,6-Dinitro-2-methylphenol \ \
2.4-Dinitrpphenol >\ \
2,4-Dinftrotpiuene ^\ ]^ 	 ^^ \
End^ulfanl / ^ — v^ ^^
Ef(dos4anll / / "^^/
Endrtrv^ "^^ /
Endrin Aldehyde^ ^\^
Endrinketoo^ ^\^ /
Bis(2-eth>tt^exyi)^hthalate
Fluoranthene\ \
Fluorene } }
^RQlpet / /
^eptacWor / /
HeptacWc^r Ep/wide
^»y
Hexachlorobenzene
Hexachlorocyclopentadiene
CONCENTRATION
^xrjg^-
\
	 ^
/~~^~~-~^


\
/













^ ng/m3
J



















Q




















Page	of	
           FORM I - AASV - 3
                          June 14, 1991
-------
                U.S.  ENVIRONMENTAL PROTECTION AGENCY
                     CONTRACT LABORATORY PROGRAM       EPA sample NO.
                         Semivolatile Organics Compounds in Air
                                 Analysis Data Sheet
  Lab Name:.
  Lab Code:
                                 Contract No.:
                                 Case No.:
  Lab Sample I.D.:_
  SAS No.:	
              SDG No.:
  Date Extracted:.
  Instrument I.D.:
 Injection Volume:	    u|
 Air Volume Sampled; (Corrected to STP):
                                    rrr
         CASRN
         193-39-5
                                                  ^CONCENTRATION
           lndeno(1,2,3-c,d)pyren*v
                                                           /
          78-59-1
           Isophorone
 \\    /
          72-W-5
           Methoxychlor
\   (
         106-44-5

          95-48-7
          91-57-6
        2385-85-5
          91-20-3
          91-59-8
           2-Naphthylaaiine
          88-74-T
          98-9S-3
           Nitrobenzerie\
          993-3
          4-Nrtrodiphenyl
                  g-Nrtrophenol/
         117-84-0
           Bis^vQcty 1) prjthalate
       27304-13-8
           Oxychlordan
          56-38-2
           Parathion
         608-93-5
           Pentachlorobenzene
Pane
nf
                                       i  A ACW
                                                                      I. ,**r* -I A •«
-------
               U.S. ENVIRONMENTAL PROTECTION AGENCY
                   CONTRACT LABORATORY PROGRAM      EPA sample NO.
                       Semivolatile Organics Compounds in Air
                              Analysis Data Sheet
Lab Name:
Lab Code:
Lab Sample I.D.:
SAS No.:
Date Extracted:
Instrument I.D.:
                                      Contract No.:
                                      Case No.:
Matrix: Air
Date Rec
Date An
QC Colu
Dilutior/Factor:
 Injection Volume:
 Air Volume Sampled; (Corrected to STP):
                                    Cleadup:None/6l
Page	of	
                             FORM I - AASV - 5
                                                                June 14. 1991
-------
             U.S. ENVIRONMENTAL PROTECTION AGENCY
                CONTRACT LABORATORY PROGRAM      EPA Sample NO.
Lab Name:_
Lab Code:
                     Semivolatile Organics Compounds in Air
                            Analysis Data Sheet
                    	  Contract No.:_
                    	  Case No.:	/
Lab Sample I.D.:_
SAS No.:	
                  SDG No.:
Date Extracted:.
Instrument I.O.:
                            uL
Injection Volume:	
Air Volume Sampled; (Corrected to STP):
                               m
CASRN

COMPpUNQ^^
\QONbSHTRAT10N
ng\^
\Pd$s/AK>clors " 	 7
27323-18-8
25512-42-9
25323-68-6
26914-33-0
25429-29-2
26601-64-9
28655-71-2
31472-83-0
53742-07-7
2051/24^3
59536-65^1
/800/35-2
<{l2674
-------
               U.S. ENVIRONMENTAL PROTECTION AGENCY
                  CONTRACT LABORATORY PROGRAM      EPA Analysis NO.
                       Semivolatile Organics Compounds in Air
                          Tentative Identified Compounds
 Lab Name:.
 Lab Code:
                                    Contract No.:
                                    Case No.:	/  /
 Lab Sample I.D.:_
 SOW No.:	
                                    Lab File I.D.:  /
                     SAS No.:
 Date Received:
 Date Analyz ?d:
                                          me Sampled:/Corrected
GC Column I.D.:
Dilution Factor:_
No., of TICs Found:
      CAS NUMBER
                     COMPOUND
RT--	9»
                                                    ESTIMATED
                                                  CONCENTRATION
ng/m3
  01
                                    V
  02
  03
  04
                                        \7
  05
  06
  07
                           /
  08
  09
  10
Page	of	
                           FORM I - AASV-TIC - 1
                  June 17. 1991
-------
                U.S. ENVIRONMENTAL PROTECTION AGENCY
                    CONTRACT LABORATORY PROGRAM

                     Semivolatile Organics Compounds Analysis In Air
                             Surrogate Percent Recovery
  Lab Name:.
  Lab Code:
Lab Sample I.D.:.
SOW No.:
           Contract No.:
           Case No.
           Lab File I.D.:
                           SAS No.:
  Date Received:_
  Date Analyzed:_
  GC Column I.D.:
                                     Date
                                     Instrume
                                          /"O'-'
                                     Dilutiot* Factor:

       EPA
    Sample No.
                 S1
                 NBZ
 S2
FBP
 S4/
PH
ss
2FP
 S6
TBP
TOTAL
 OUT
01
03
09

10


11
13
14
15
16
17
18

19
                            \
20
                   Jtrpbenz^ne^5     Required
                  2-FlDecobiph6nyl     Required
                    erphenyl-dU     Required
                  Phent
                  2-Fluorophenol
                  2,4,6-Tribromophenol
Pano
-------
               U.S. ENVIRONMENTAL PROTECTION AGENCY
                   CONTRACT LABORATORY PROGRAM

                    Semivolatile Organics Compounds Analysis In Air   '
                            Surrogate Percent Recovery
 Lab Name:.

 Lab Code:
                    Contract No.:.

                    Case No.:
Lab Sample I.D.:_

SOW No.:
                                      Lab Pite I n •
                          SAS No.:
                               /
Date Received:
Date Analyzed:
GC Column I.D.:
Date Extracted: / ^\, ^\
Instrument I/a: / ^\ ^\
Dilution F/ctor': ^\ ^
                 13,
       5DT/
         ilorobiphenyl
        i'-Tetrachlorobiphenyl
C^-az.S.S'.S.S'.e.e'-Octachlorobiphenyl
C, 2-Decachlorobiphenyl
Page	of	
            FORM II - AASV -2
                                                               June 17. 1991
-------
              U.S. ENVIRONMENTAL PROTECTION AGENCY
                  CONTRACT LABORATORY PROGRAM
Lab Name:.
Lab Code:
                      Semivolatile Organics Compounds in Air
                Sample Filter/Adsorbent/Cartridge Assembly Certifn/atic
                                    Contract No.:.
                                    Case No.:
                                                  /  /
Lab Sample I.D.:.
SOW No.:	
                                     Lab Fife I.D.:
                         SAS No.:
                                              /
 Date Received:.
 Extraction I.D.:
 Filter Batch I.D.:
                                    Date Extracted:/
                                    Instrume
                                    PUFBs
 XAD-2 Batch I.D.:
         EPA
      SAMPLE NO.
                      FILTER
                                      PUF
ASSEMBLY
 01
 02
 03
 01
 05
 06
 07
 08
 09
 10
 11
 12
 13
 14
 15
 16
 17
 18
 19
 20
                                          /
                                           v
                    /
       CRfTERIA OF < 10 jig TOTAL ANALYTE LEVEL PER PAIR OF FILTER AND ASSEMBLY
Paae   of                      pnoM HI . AACW .1                     lime 17
-------
                U.S. ENVIRONMENTAL PROTECTION AGENCY
                    CONTRACT LABORATORY PROGRAM
                                                               EPA Analysis No.
                       Semivolatile Organics Compounds in Air
                         Laboratory Method Blank Summary
 Lab Name:_
 Lab Code:
                                     Contract No.:.
                                     Case No.:	
Lab Sample !.D.:_
SAS No.:	
                    SDG No.:
 Date Extracted:.
 Instrument I.D.:
 Injection Volume:	
 Air Volume Sampled; (Corrected to STP):
Matrix: Air
Date Rec
Date An
GC CoIyfnn>.D.:
Dilution Factor
Cle
      EPA SAMPLE NO.
                        LAB SAMPLE ID
       LAS'RLE ID
TIME ANALYZED
 01
 02
 03
 03
 05
 06
                                  \
      /
 07
                                    \
 08
 OS
 1C

 13
 14
 15
 16
 18
 20
COMMENTS:
Paae
       of
                              COPM IV . AARV . •(
                                                                         1QQ1
-------
U.S. ENVIRONMENTAL PROTECTION AGENCY
   CONTRACT LABORATORY PROGRAM
  Semfvolatile Organics Compounds Analysis Data Sheet
    GC/MS Tuning and Mass Calibration With DFTPP>
Lab Name:
Lab Code:
Lab Sample I.D.:
SOW No.:
Date Injected:
Extraction I.D.:
GC Column I.D.:
Contract No.: / /
Case No.: / /
lahRiei.D.: / ^ "\
SAS No.: / / srvHln • "^
/ "/ \ 	 ^T 	
	 Time Injected / ^\ ^\
/ "N 	 "" 'x: — ^ 	
Instrument I.0.: ^\ /
/ / 	 	 	 •^TT' 	
RASN6.: /
m/e
51
68
69
70
127
197
198
199
275
365
441
442
443
ION ABUNDANCE CRITERIA / \
30-80% of mass 198
Less than 2.0% of mass 69
Present
/""- 	
Less than 2% of mass 69 \ \- 	
25-75% of mass
Less than 2% of
Nominal peak, 1
5-9% of mass 1£
10-30% of mass
198 \ \
mass 198 \ \ /
00% relative abundancex ^
)8
\ <
198 / X \
Greater than 0.75% jzff" mass~T98 \ N
Present, but less tj&n pfiass 443 ^ ^ \.
40-1 10% of mas.
1 5-24% of ma^6
/1987 / ^ ^
44^ / / \^.
/ /% ABUNDANCE
\RELA-nVE TO
^M ASS 198
"\ "\
\ N
\y
— ^_^
7 / — ~~^ /
/
/

\
N
V
-7

RELATIVE TO
SPECIFIED MASS













THlS^NE^/PLJES TO THE FOLLOWING SAMPLES:

01
02
03
04
05
06
07
08
09
10
11
EPA
SAMPLE N£__
/ „ —
/ /
/ /
/ ^
\ "\
\ ^x
\,




"^LAB \^
.^SAMPli^.
_ \ ^
\ \
\ \
\ }
1 1
/ /
^v /
\ /



LAB
\^FILE I.D.
\ /










DATE
ANALYZED











TIME
ANALYZED











-------
              U.S. ENVIRONMENTAL PROTECTION AGENCY
                  CONTRACT LABORATORY PROGRAM
 Lab Name:
 Lab Code:
                 Semivolatile Organics Compounds Analysis Data
                   GC/MS Tuning and Mass Calibration With D
                             Contract No.:
                             Case No.:
 Lab Sample I.D.:
 SOW No.:
 Date Injected:
 Extraction I.D.:
 GC Column I.D.:
Paae
of
                             CODK4 \l  A AOW
-------
U.S. ENVIRONMENTAL PROTECTION AGENCY
   CONTRACT LABORATORY PROGRAM
      Semivolatile Organics Compounds in Air
            Initial Calibration Data
Lab Name:
Lab Code:
SAS No.: - SDG No.:
Date Extracted:
Instrument I.D.:
Injection Volume:
Air Volume Sampled; (Corrected to STP):
Contract No.:
Case No.:
Date Prepared:
Date Analyzed:
QC Column I.D.
Dilution Factpr
Cleanup:/Nofoe
/>
/ /
/ /
/ \^
. /^\ "\
/ ^\ "\
(/610/Lobar \x. /

CAL1

COMPOUND

CAL2


Acenaphthene
Acenaphthylene
Acetophenone
Aldicarb
Aldrin
Aniline /
Anthracene /
Bendiocarb ^
Benzidine
Benzo(a) anthraee'ne
Benzo(a)Pyriene/
Benzo(b)fHjoranthene
Benzo(ejpyrene^
Benzo(g,run**ylen>\
Benzo(k)fluorantheriex^
Benzyl alcohol
alpha-BHC
gamma-BHC (Undane)
p-Biphenylamine
LABFIL-EJD
CAI^ \^
\^
/ /
/ CAL4
"\

CAL5

INITIAL CAUBRATJON^
RRF
CAL1



/"
/ /
/
C^
\ "^^
\^
"\
"\ \
\

/
\y /
\ /



(R
\


"\
\ V
/ S~
/ /
/ '
^\
^\
X,
\
\

/
f




"~^RRF—
~~CALJ
\ ,
\ V
\ <
\
~\
\ ^
"v--


"y









-JffiF

/

\
\/
7













-GA^S
~~J


















RRF



















RSD




















-------
                  U.S. ENVIhuNMENTAL PROTECTION AGENCY
                       CONTRACT LABORATORY PROGRAM
                           Semivolatile Organics Compounds in Air
                                  Initial Calibration Data
Lab Name:
Lab Code:
SAS No.:
	 Contract No.: /\
	 Case No.: / /
	 SDG No.: Date Prepared: / /
  Instrument I.D.:
  injection Volume:
  Air Volume Sampled; (Corrected to STP):
Date Analyzed:/
GC Column \.l
Dilution F
Cleanup:
                     e/6l 0/Lobar
  Bis(n-butyl)phthalate
  Butylbenzylphthalate
  •~-«-_-_l_-_^_B
  Captan
  •~^-_-_M_-_-_-
  gamma-Chlordane
  alpha-Chlordane
  Chlordane (Technical)
  4-Chloro-3-methylphenol
  4-Chloroaniline
  Bis(2-
  chloroethoxy) methane
  Bis(2-chloroethyl)eth
  Chlorothalonil
 Dibenzo(a,h)anthracene
 Dichlorvos (DDVP)
Page	of	
FORM VI - AASV - 2
                                                                      June 14. 1991
-------
              U.S. ENVIRONMENTAL PROTECTION AGENCY
                  CONTRACT LABORATORY PROGRAM
                      Semivolatile Organics Compounds in Air
                            Initial Calibration Data
Lab Name:
Lab Code:
SAS No.:
Contract No.:
Case No.:
SDG No.: Date Prepared: /
/N
/ /
/ /
Date Extracted:_
Instrument I.D.:	
Injection Volume:.
Air Volume Sampled; (Corrected to STP):
Date Analyzed: /
GC Column LD.:
Dilution Faoror /
Cleanup:/^
(/610/Lobar
COMPOUND
Dieldrin
Dietnyl Phthalate
2,4-Dimethyl phenol
Dimethylphthaiate
4,6-Dinitro-2-
methylphenol
2.4-Dinitrophenol
2,4-Dinrtrotoluene
Endosutfan I /
Endosulfan II /
Endrin \^
Endrin Aldehyde .
Endrin ketone ^ 	 -
Bis(2-ethylhe)^i)ph#ialatB-
Fluoranthepfe /
Fluorene/ /
Folpet \^ ^\
Heptachlor ^\ ^\
Heptachlor Epoxide ^\
Hexachloro benzene
Hexachlorocyclopentadie
ne
/NIJ(AL CAUp^AjfoN
RRF
CAL1





^~
/ /^~
/
/
^\ /
\
^
~^^ ^\
\
\
)
/
^ /
\V

RRF
CAL2

/ 	
<, V
\
\
^\
x Y
) l
/ /
/
<,
\ \
\
\
\
I
/



SiBF
CAClK

• — ___
	
\
\V,
\ '
\
\^
^-^x



/







CAL4^
\^

^ 	 ^
7 -_^__^^
/
\
\
V
/











/ RRF
CAL5
\^
\ /
— -,
~J
















RRF




















%
RSD




















-------
             U.S. ENVIRONMENTAL PROTECTION AGENCY
                CONTRACT LABORATORY PROGRAM

                   Semivolatile Organics Compounds in Air
                         Initial Calibration Data
Lab Name:
Lab Code: • .
SAS No.: SDG No.:
Date Extracted:
Instrument I.D.:
Injection Volume:
Air Volume Sampled; (Corrected to STP):
Contract No.:
Case No.:
Date Prepared:
Date Analyzed:/
GC Column jo).
Dilution Factory
/^N
Cleanup/ None
/>
/ /
/ /


/ "\ \^
/610/Lobar ^\ /
COMPOUND
Hexachloroethane
lndeno(l ,2,3-c,d)pyrene
Isophorone
Methoxychlor
4-Methyl phenol
2-Methyl phenol
2-Methylnaphthalene
Mirex
Naphthalene /
2-Naphthylamine /
2-Nitroaniline ^
3-Nitroaniline
Nitrobenzene /
4-Nitrodiphe/iyl /
2-Nitropher«ol/
Nitroprjenolsicciixed)
Bis(n-octyl)pttttTalate\^
\~~*s,
Parathion
Pentachlorobenzene
Pentachlorophenol
Phenanthrene
/INIJJJAL CALIBRATION
RRF
CAL1






/ _
/ /
/
c^
\/
"\
"~~\
'v\ x
\

/
^y /
\ /



RRF
CAL2

/ 	 	
\ \
\
'

\
> I-
) s~
/ /
/
\^
^^
\
\

)
/






" 	
^— -_.
\ /
\ v
\ <
\
^\
v^
"^


>









N^F /
\CAL4^
\

— — —
A—
/

\
\/
-j













RRF
CAL5
"\
\/
"~^7
-J


















RRF






















%
RSD






















Paae
of
POPM \i\ .
                                                        .>i<3 1 A 1 QQ1
-------
             U.S. ENVIRONMENTAL PROTECTION AGENCY
                 CONTRACT LABORATORY PROGRAM

                    Semivolatile Organics Compounds in Air
                          Initial Calibration Data
Lab Name:
Lab Code: • •
SAS No.: SDG No.:
Date Extracted:
Instrument I.D.:
Injection Volume:
Air Volume Sampled; (Corrected to STP):
Contract No.: /\
Case No.: / /
Date Prepared: / /
Date Analyzed: / \^
GC Column I.e.: /^\, ^\
Dilution Factor / ^\ ^\
Cleanup:/None/610/Lobar ^x. ;?
COMPOUND
o-Phenylphenol
Propoxur
Pyrene
Resmethrin
Ronnel
Toxaphene
cis/trans-Permethrin
2,4,5-Trichlorophenol
2,4,6-Trichlorophenol /
PCB Calibration /
Congeners C^
ci.
Cfe ^ 	 	
«3 / / 	 	
CL4 / /
cu, . / /
CLs ^ \
CL7 \. \
CL, "\
c^
^0
Polybrominated biphenyls
/N|-p(AL CAUpRAJJON
RRF
CAL1






/^~
/ /-•
/
/
\^ ^
^ ^^
^ ^x
N
\
j
/
^ /
\y


RRF
CAL2

t 	 _
< v^
\
\

^\
^J"
) -
//
<
\^ ^v
\x
\
\
}
/




^RRF
CADS^


"~~*~~^
\
- \/
\ (
\
\
•~-^^^
, X-
X^


/








\RR^ ,
CAl4/
"\

	 	 -^,
7 , 	 ^
/

\
X >
—7












/ RRF
CAL5
\^
\ ?
-~-^^^
-J

















RRF





















%
RSD





















Pane   of
-------
               U.S. ENVIRONMENTAL PROTECTION AGENCY
                   CONTRACT LABORATORY PROGRAM

                      Seimivolatile Organics Compounds in Air
                             Initial Calibration Data
Lab Name:
Lab Code:
SAS No.: SDQ No •
Date Extracted:
Instrument I.D.:
	 Contract No.: //
Case No.: / /
Date Prepared: / /
Date Analyzed/ ^ ^\
GC Column /D.:/ ^\ ^\
 Injection Volume:	

 Air Volume Sampled; (Corrected to STP):
       Dilution Fj

       Cleanuc
                               m
Page	of	
FORM VI - AASV - 6
                                                             June 14, 1991
-------
U.S. ENVIRONMENTAL PROTECTION AGENCY
   CONTRACT LABORATORY PROGRAM

      Semivolatile Organics Compounds in Air
          Continuing Calibration Check
Lab Name:
Lab Code:
SAS No.: SDG No.:
Date Extracted:
Instrument I.D.:
Injection Volume:
Air Volume Sampled; (Corrected to STP):
Contract No.: / /
Case No.: / /
Date Prepared:/ \,
Date Analyzed: /\ ^\
GC Columr/I.D./ ^\ ^\
Dilution Faoor ^\ ^\
Cleanup: Ntone/610/Lobar ^^V
COMPOUND
Acenaphthene
Acenaphthylene
Acetophenone
Aldicarb
Aldrin
Aniline /
Anthracene / /
Bendiocarb / /
Benzidine / <^
Benzo(a)anthracene ^\ ^^
Benzo(a)Pyrene - ^\
Benzo(b)fluoraptf1ene ^~"""Vv\
Benzo(e)py^ene/x^ ^^\
Benzo(g,f/i)peiylene
Benzo(k)fludFa£thene
Benzyl alcbhQl ^\^
alpha-BHC "\^ ^\^ /
gamma-BHC (Lindane) ^\^ /
\y
p-Biphenylamine
Bis(n-buty 1) phthalate









^R^RF^
0.800 ^^
~1L3DD-~----^
'^o&m — /
0.010
0.010
0.010
/0.700
0.010
0.010
0.800
0.700
0.700
0.010
0.500
0.700
0.010
0.010
0.010
0.010
0.010
^ %D
y



















MAX
%D
25.0
25.0




25.0


25.0
25.0
25.0

25.0
25.0





-------
               U.S. ENVIRONMENTAL PROTECTION AGENCY
                   CONTRACT LABORATORY PROGRAM
                      Semivolatite Organics Compounds in Air
                          Continuing Calibration Check
  Lab Name:
  Lab Code:
  SAS No.:
  Date Extracted:
  Instrument I.D.:
Page	of	
FORM VII - AASV - 2
                                                            I lino 14 1QQ1
-------
              U.S. ENVIRONMENTAL PROTECTION AGENCY
                   CONTRACT LABORATORY PROGRAM
                      Semivolatile Organics Compounds in Air
                          Continuing Calibration Check
Lab Name:.
Lab Code:_
SAS No.:
                  Contract No.:_
                  Case No.:
SDG No.:
Date Extracted:.
Instrument I.D.:
Injection Volume:	
Air Volume Sampled; (Corrected to STP):
Date Prepared: /   \
           /
Date Analyze
GC Column/D.:/
Dilution
Cleanuc
                                m
                             (/610/Lobar
COMPOUND
Diethyl Phthalate
2,4-Dimethyl phenol
Dimethylphthalate
4,6-Dinrtro-2-methylphenol
2,4-Dinitrophenol
2,4-Dinitrotoluene /*--
Endosulfan I / /-
Endosutfan II / /
Endrin / /
Endrin Aldehyde x^ ^\
Endrin ketone ^\^
Bis(2-ethylhexyl) pjjtoafatc^^^
Fluoranthene/ ^- 	 — >^ ^
Fluorene / / \^
Folpet- / /
Heptacnk^ ^\
Heptachlor Epoxiq^e ^\^ /
Hexachlorobenzene ^\^ ^^^
Hexachlorocyclopentadiene ^\/
Hexachloroethane
lndeno(1 ,2.3-c,d)pyrene
/ INITIAL P^L^RATION
RRF

/ ~
\^
\

— \
^\
) v
/ f
/ /
" t
^^ \
\ ^\
\
\ \
) I
' /
/



^Hv.
CAL3\

	 	 ^.

\ //
\v
\\
\
"^\ x
\^ /



/








\ W»F\
0.01^\^
-JiOlO
AS!P /
0.010
0.200
0.200
YOIO
^0.010
0.010
0.010
0.010
0.010
0.600
0.900
0.010
0.010
0.010
0.100
0.010
0.300
0.500
%D
^>
vy



















MAX
%D




25,0
25.0






25.0
25.0



25.0

25.0
25.0
-------
              U.S. ENVIRONMENTAL PROTECTION AGENCY
                 CONTRACT LABORATORY PROGRAM

                    Semivolatile Organics Compounds in Air
                        Continuing Calibration Check
Uab Name:
Lab Code:
SAS No.: " SDQ No •
Date Extracted:
Instrument I.D.:
Injection Volume:
Air Volume Sampled; (Corrected to STP):
Contract No.: / /
Case No.: / /
Date Prepared:/ _ ^\
_ Date Analvzeci: / ^\ ^\
_ GC ColumrRD/ ^\ ^\
/\ 	 ^\" — ^xT
Dilution factor ^\ /
Cleanup: None/61 0/Lobar ^
                             fTC

COMPOUND
===sss==s=s==i=
Isophorone
Methoxychlor
4-A/lethyl phenol
2-Methyl phenol
2-Methylnaphthalene
Mirex /^
Naphthalene / f
2-Naphthylamine / /
2-Nrtroaniline / ^
3-Nitroaniline ^\^ ^\
Nitrobenzene ^\
^Nitrodiphenyl/^" "^\
2-Nitropheno^ /^~~ "^\
Nitrophenois (^nixed)
Bis(n-oofyl) pl^halate
Oxychloroane^ ^^
Parathion ^\^ ^\^ /
Pentachlorobenzene ^\
Pentachlorophenol
Phenanthrene
o-Phenylphenol

RRF
/ — — -
\ \-
\


"X

) ^
/ /
J /
^ *\
^\ ^
\ ^
\ \

/ /
/
/



V'Nfrl
CAL3

• — -_^^
\ 7
\\/ /
\ <
\ \
-^ \
^ "v^~7
\-y


^









AL.CAUBRA
IWN
\R^RF\
0.400 ^x
~07DTO— — ^.
/Q!Boo — ~j
0.700
0.010
s 0.010
^.700
0.010
0.010
0.010
0.200
0.010
0.100
0.010
0.010
0.010
0.010
0.010
0.050
0.700
0.010
T10N
v %D
/





















MAX
%D
=s^==
25.0

25.0
25.0


25.0



25.0

25.0





25.0
25.0

Pano
-------
                 U.S. ENVIRONMENTAL PROTECTION AGENCY
                     CONTRACT LABORATORY PROGRAM

                        Semh/olatiie Organics Compounds in Air
                             Continuing Calibration Check
Lab Name:
Lab Code:
SAS No.: SDG No.1
Date Extracted:
Instrument I.D.:
Injection Volume:
Air Volume Sampled; (Corrected to STP):
Contract No.: / /
Case No.: / /
Date Prepared: / \
Date Analyzed: /\ ^\
GC Column/I. D.x ^\ ^\
Dilution Faster ^\ ^\
Cleanup None/6 10/Lobar ^x/
                                   mj
         COMPOUND
                               RRF
                                       /
                                                              %D
                                MAX
                                 %D
 Propoxur
 Pyrene
                              25.0
 Resmethrin
 Ronnel
\
                                                 0.010
 Toxaphene
          0.010
 cis/trans-Permethrin
                                                 0.010
 2,4,5-Trichlorophenol
         ">0.200
25.0
 2,4,6-Trichlorophenol
          0.200
25.0
   PCS Calibration Coflgeyfera
      7
                                                 0.010
                                                 0.010
 ci
                                                 0.010
                                                 0.010
 CL,
          0.010
                                                 0.010
                                                 0.010

                                                 0.010
                                                 0.010
                                                 0.010
 Polybrominated biphenyls
          0.010
Pane
                                                                    it mn -1/1 i am
-------
               U.S. ENVIRONMENTAL PROTECTION AGENCY
                   CONTRACT LABORATORY PROGRAM

                    Semivolatile Organics Compounds Analysis In Air
                        Internal Standard Area and RT Summary
 Lab Name:.
 Lab Code:
                                     Contract No.:.
                                     Case No.:
Lab Sample l.D.:.
SOW No.:
                                       Lab Pile 1 T» •
                          SAS No.:

Date Received:
Extraction I.D.:
GC Column I.D.:
Date Extracte
Instrument l.E
RAS No.: /\
*! r^ \


01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20


12 Hour STD.
Upper Limit
Lower Limit
EPA
Analysis No.












/
A
/ /
/ /
t ^
^\
^

AREA
1 ,4-Dichlorobenzene-
d4








^ — ^
/
/ / "
/ /
/ / /
<. \ /
^X^ ^"^
\. /
^\
•^ — *^\ ^
s" "^\ X
X \
N
j
\. / ,
\ ^\ / /
\. ^ /
RT



r~~
\ \
\
\,


\
\ s-
! ,
/
/

^\
\
\

\




/A^EA /v.
Naptrthajene-dS
^ \ /
^\
\
	 	 ^_
*-^.
\ / r*
( \ / /
\ v /
\ \
\ \
-. \>
-^ \^__7"
\^/



>
y






/RT /
/
{
\
\
-—— -
h — ~J


















AREA
Acenaphthalene-
d10


•
>




















RT
























      Area Upper Limit
      Area Lower Limit
      RT Upper Limit
      RT Lower Limit
                            of 12 Hour Internal Standard Area
                      -50% of 12 Hour Internal Standard Area
                      12 Hour Internal Standard RT +0.50 Minutes
                      12 Hour Internal Standard RT -0.50 Minutes
Page	of	
                             FORM VIII - AASV - 1
June 17, 1991
-------
              U.S. ENVIRONMENTAL PROTECTION AGENCY
                  CONTRACT LABORATORY PROGRAM

                   Semivolatile Organics Compounds Analysis In Air
                      Internal Standard Area and RT Summary /^
Lab Name:
Lab Code: - .
Lab Sample I.D.:
SOW No.:
Date Received:
Contract No •
Case No.:
Lab File ID-
SAS No.: /
Date Extracted-
/ /
/ /
/ ^

/ \v \^
Extraction I.D.: Instrumented-' ^^\ ^^\
GC Column I.D.: RAS No^ / ""^X/
01
02
cr
f
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20


12HourSTD.
Upper Limit
Lower Limit
EPA
Sample No.












/
/ /
/ /
/ L
<\ \
"\


AREA
Phenanthrene-d10








/^ 	 -
/
/ /
/ /
/ L /
\ \/
\
^ 	 ^\^
"\
^ "\ \
\
}
>

\. "\/ /
\. /
RT



r
\
\


\
N^
^ ^
1 s
/
/
~~^^
\
\^

\
\
}
i


/ ^REA / /
C^rys4ne-d12 /
\ ^V
^\
\

^-~- — -_,
\ / / ~
\ V /
\ /
\ \
\ \
"^\ V
""X ^~7
\-y



7







^
/
\
^s
\
^^— —
— —J


















AREA
Perylene-d12


x^
V
,



















RT
























      Area Upper Limit
      Area Lower Limit
      RT Upper Limit
      RT Lower Limit
+ 100% of Internal Standard Area
-50% of Internal Standard Area
+0.50 Minutes of Internal Standard RT
-0.50 Minutes of Internal Standard RT
Pane
-------
                 U.S. ENVIRONMENTAL PROTECTION AGENCY
                     CONTRACT LABORATORY PROGRAM
                            Sample Receipt/Log-ln Form
Lab Name:
Lab Code:
SOW No.:
Date Received:
Contract No.:.
Case No.:
Time Receiv
Log-in Date:
Airbill No., or Sticker:
                                                         Received By
    CHECK LIST
CHAIN-OF-CUSTODY
TRAFFIC REPORT
PACKING LIST
CUSTODY SEALS
SAMPLE TAGS
SAMPLE CONDITION
* = If checked, contact SMO and attach tecordoTtesolutiort /
Does information on custody records, traffic ref^ortsxand s/mofe tagsigTee? (Y/N)
EPA
SAMPLE NOs.







S
/ /^
/ /
/ /
CUSTODY
SEALNQs^^
/ _
7 / ^
/ / )
/ / /
\ \ / /
\^ " ^
\^
^~^\^ \
^\ \
\ \
\ \
\ v/
SAMPLE /
TAG Nqs. \
\ \
v — \ x
^^^
/ \^/


"\
\ >
\/


/
ASSIGNED
LAB NOs.
\
k/
f








REMARKS ON
CONDITION OF SAMPLE
SHIPMENT











*\ ^\ / S/AMPLE TRANSFER:
"S\ \
\

\ / /
. \y /
\^ /









\/
Area No. By: On:
Logbook No.:_
      Logbook Page No.:
-------
                  U.S. ENVIRONMENTAL PROTECTION AGENCY
                      CONTRACT LABORATORY PROGRAM
                             Sample Receipt/Log-ln Form
Lab Name:.
Lab Code:_
SOW No.:
                                      Contract No.:.
                                      Case No.:
                        SAS No.:
 Date Received:	
 Airbill No., or Sticker:
                                    Time Receiv
                                    Log-in Date:
                                                         Received Bv:
 Date:
Page	of
                               FORM AADC-1 - 2
June 17. 1991
-------
           U.S. ENVIRONMENTAL PROTECTION AGENCY
               CONTRACT LABORATORY PROGRAM

                    Semivolatile Organics Compounds
                  COMPLETE SDG FILE (CSF) DOCUMENT
                         INVENTORY SHEET     ,.
Lab Name:
City/State:
SOW No.:
Contract No.: / /
Case No.: / /
SAS No.: / sS<3 Nn •
All documents delivered in the complete SDG file must
                                                     fe possible.
//
1. Semivolatile Organics Compounds in Air, Cover Sheet (JZfover Page^x
2. Sample Receipt/Login Form (FORM AADC-1) / / / /
3. Inventory Sheet (AADC-2)(Do Not Number) / 
-------
                 U.S. ENVIRONMENTAL PRC
                     CONTRACT LABORATC
                           Semivolatile Organics
                        COMPLETE SDG FILE (C^F)
                               INVENTORY SK
 Lab Name:.
 City/State:_
 SOW No.:
Contract
Case No.
Jo.:
                        SAS No.:
Completed by (CLP Lab):


(Signature)
Audited by (EPA):


(Signature)
        TECTION AGENCY
        RY PROGRAM
       Compounds
         DOCUMENT
       EET  .
                               FORM AADC-2 - 2
                              June 17 19Q1
-------
Exhibit B
      SOW No. XXX  -  Ambient Air
3.4 INORGANICS
    This  section  contains  specific instructions for the /^omt/Letion of all
required Data Reporting Forms for  analysis  of  inorganic/constituents in
ambient air.  This section is organized  into the  follo/inj/parts:
    •  General Information and Header  Information
    •  Cover Page - [COVER PAGE  -  AAIN]
    •  Analysis Data Sheet [FORM I - AAIN]
    •  Initial and Continuing Calibration Verif/cat?lon [FORM
    •  CRQL Standards/Linear Range Standards PFORM III -  AAIN]
    •  Blanks [FORM IV - AAIN]
    •  ICP Interference Check Sample  [FORM/V /AAIN]
    •  Spike Sample Recovery  [FORM VI  -
    •  Analytical Spike Sample Recovery  [FORM^MJ
    •  Duplicates [FORM VIII  - AAIN]
    •  Laboratory Control Sample [FQ&M^IX - AAIN]
    •  Method of Standard Addition^ [FORM X -
    •  ICP Serial Dilutio- [FORM XlV
       Instrument Detection Limits  (Qu>art
       ICP Interelement Correction Factors
       ICP Linear Ranges (Quajmejrly)
    •  Preparation Log [F/JRM _XV_  -
    •  Analysis Run Lo
    •  Sample Log-In Sne
       Document Inventory Sheet /[FO#M  AADC
3.4.1 General Informat
    3.4.1.1  Values must be "rB^orte&xon  the hard  copy  forms  according to the
    individual >fo"rm instTsuctions^^n this Section.   Each form submitted must
    be  f illed/outjaefflpj.etelyxfor alK^n&lytes.   Multiple forms cannot be
    submitted  Ln  place or\one i^orm if the  information on those forms can be
    submitted /on  one  form.
    3.4.L.2 /For  rounding off numbers  to the appropriate level of precision,
    observe  the. following  common rules.   If the figure following those  to be
    retained is  ra-ss  than  5,  /drop  it  (round down).  If the figure is greater
    than  5,  dr^o  it and  incr/eas/ the  last  digit to be retained by 1  (round
    up) .   If the  i^i^ure^^CpJ/low^Lng  the last  digit to be retained equals  5 and
   |RM XII - AAIN]
 .al) [FORM XIII  - AAIN]
-------
Exhibit B
                                                      SOW No.  XXX - Ambient Air
                                                                the right of
                                                             Lned is odd, or
there are no digits to the right of  the  5  or  all  digi
.che 5 equals zero, then round up if  the  digit to  be
round down  if that digit is even.

3.4.1.3  All characters which appear on  the data
presented in the contract must be reproduced  by
submitting  data, and the format of the forms  s
to that shown in the contract.  No informationSaa^ be added, dfesLeted>xor
moved from  its specified position without  prgor^written approvalbiNthe/'
EPA APO.  The names of the various fields  aWd analytes (i.e. ,  "Lab  CoW",
"Aluminum") on the forms must appear as  they  dto on the forms,  except  that
the use of uppercase and lowercase letter/ i/option.^"
    3.4.1.4  All alphabetic entries made or
    must be  in ALL UPPERCASE  letters  (i.e.
                                                    by7 the Contractor
                                                     Low" or  "low").
    3.4.1.5  Seven pieces of information are common  to<xContract,  Lab Code,  Case
    No., SAS No., SDG No., and SOW No.  This  information musfrsbe entered on
    every  form and must  match on all^-ferms.
      3.4.1.5.1  The "Lab Name" is She
      identify the laboratory.  It m«

      3.4.1.5.2  The "Contract" is the
      hyphens,  under which the analyses
                                       Chosen by£T!5—Contractor to
                                   no,t exceed 25-~charactfers.
                                    W€
 if  Che EPA  contract,  including
Ser/ormed.
      3.4.1.5.3  The "Lab Code'^TS^an alphabe\ic Abbreviation of up to 6
      characters, assigned/bvthe EPA  to iden\ify\the laboratory and aid in
                              ab code\shjgll be assigned by the EPA at the time
                             and mutet not ofe-^modirifed by the Contractor,
                                            charsee of name or ownership occurs
                                  ode/will t«maln the same until the
                                     PA to use another lab code assigned by
  data  processing.
  a  contract  is  awac&e
  except  at the  diirec
  at the  laboratory,
  Contractor  is
  the EPA.
  3.4.1.5.4 The  "Case
  characters)
                                isbhe EPA-assigned Case number (up to 5
                             wih^the sample and recorded on the TR.
      NOTE:
                             the £P^-assigned number  for  analyses
                             .lytical  Services  (SAS).   If samples are to be
                               eported  on these  forms,  then enter SAS No.
                                samples are analyzed according to this SOW
                               protocol)  and have additional SAS
                               Case No. and SAS  No.  on all forms.  If the
                             ments,  leave "SAS  No." blank.
                           /
                            SDG may have a SAS  No.,  while  others may not.
July, 1991
                                                               Page B-2/IN
-------
Exhibit B
                              SOW No.  XXX -  Ambient Air
      3.4.1.5.6  The "SDG No." is the Sample Delivery  Group^number.   The SDG
      number is .the EPA sample number of  the  first sample/reoteived in the SDG.
      When several samples -are received together in the /irsr SDG shipment,
      the SDG number must be  the  lowest sample  number  (/onafidering both alpha
      and numeric designations) in  the  first  group ofysam&Les received under
      the SDG.
      3.4.1.5.7  The "SOW No." is the EPA-designat^
      Statement of Work  (SOW) under which  analyse!
      been performed.  The SOW No. appears on  tt
      For samples analyzed using  this SOW,  ent«
                                                    the
                                for  "SOW No."
     3.4.1.6  The  EPA  sample  number  is  the un/que/identii
     the TR that  accompanied that sample.   T# is/number j/s
     and it must  be  used exactly as  assigne
                                   ig number given in
                                   ^signed by the EPA
      3.4.1.6.1  The "EPA SAMPLE No." mus'bvbe erfe^ryd on  several  of the forms.
      This number appears either in  the uppeiNright  harid  corner of the form,
      or as the left column of a table summarizrhc data^from a number of
      samples.  When the "EPA SAMPLE No."  is enteredxmto tbe triple -spaced
      box in the upper right hand corner of a form,  it  must be>centered on the
      middle line of the three lin^s~~etra€-~comprise the  box>
      3.4.1.6.2  All field samples Nand\juaT1rey--control  samples  associated with
      field samples must be identified, with  an/EPA/'"~saTlipi«~'number.   In
      addition, the sample suffix and xmaJxlty/control  sample  abbreviations
      listed in Table B/IN-2, Section 2\>f \flis/Exhibit must  be used as
      appropriate.
     3.4.1.7  All  results jrfust be
     with  the specified
     B.  The raw data reTsu
     in  the raw data
     for that result  nt
     the raw data reySult(^to ente/  ipt' the spe
     zeros must be
     reporting  decimal
     examples are provide
:or
  anscribed\to 'KORMs II-XV in the raw data
decimal places tnat are described in Exhibit
            only/when the number of figures
              number of figures specified
         If thire are not enough figures in
              ed space for that result, then
  places to the specified number of
esult for a specific form.  The following
     IS
    exceed^  the  maxi
   for that  66'rnu
   Raw Data Re;
          LJf iec
                                         rormat
                     Correct Entry on Form
                                      673
                                      6.3
                                      6.3
                                      6.3
                                      6.3
                                      6.3
                                      6.3
                                          5.900
                                          5.997
                                         95.997
                                       996.00
                                       9996.00
                                      99996.
                                       invalid
     NOTE:   6.3
     three  decimal plal
        imum of six significant figures and up to
July.  1991
                                            Page B-3/IN
-------
Exhibit B
                                                      SOW No.  XXX - Ambient Air
     3.4.1.8  Before evaluating  a  number for being in control/or out of
     control  in  relationship to  a  certain limit, the number Devaluated must be
     rounded  using EPA rounding  rules to the significance reported for that
     limit.   For. instance,  the control limit for an IC/ is^lO percent of the
     true value.   A percent recovery value of 110.4 w/uld^be considered in
     control  while a value  of 110.6  would be conside/ed/ou^of cortsrol.  In
     addition, a calculated value  of 110.50 would be iii contrcvFxwhile^
     calculated  value  of 110.55  would be out of confcr/1.

3.4.2 Cover Page  [Cover Page  - AAIN]
3.4.2.1  This form is used to list all b/llable  sample^ analyzed within
an SDG, and to provide certain  analytical  information /and general
                                           s  signeei by the Laboratory
comments.
                   is  also  the  document which
Manager to authorize and  release  all
with the SDG.
                                                 d de/Live'rables associated
    3.4.2.2  Under "EPA Sample No.," enter  up  to  sfe^en c
    Sample No.  (including  spikes  and duplicates)  for
                                       st contain
within the SDG.  Samples spikes/
a "D" suffix.  Other spikes  (
must have an A suffix.  These
in ascending alphanumeric order
Interchange Code convention.
both alpha and numeric characters)
would be entered in the first EPA s
below it would be in ascending
MAC111A, MA1111A,

3.4.2.3  All EPA sam£le/numiWs
order, continuing jlo ^ne follqwiiig
                                                        acters  for the  EPA
                                                       required analysis
                                                  S"  stiffix/and duplicates
                                                   stion/distillation)
                                                         ted on the form
                                                        ry Coded Decimal
                                                   the^lowest (considering
                                              number within the SDG,  it
                                            tber  field.   Samples listed
                                              124A, MAB124B,  MAB125A,
                                                    in  ascending alphanumeric
                                                   if applicable.
    3.4.2.4  Under  "tfab /Sample  !/,"/& Lab^S^mpLe  ID  (up  to  ten characters)
    may be entered for  e-ach ass/Sciafted  EPA sample number.   If a Lab Sample ID
    is entered,  it  mttst be"e
    3.4.2.5  Entei>-u¥u-
-------
Exhibit B
                                                 SOW No. XXX  -  Ambient  Air
3.4.3 Analysis Data Sheet  [FORM I  - AAIN]

     3.4.3.1  This  form  is  used to  tabulate  and report sample''analysis results
     for  target  analytes (Exhibit  C).

     3.4.3.2  Complete the  header  information accordi
     instructions  and  as follows.

     3.4.3.3  For  "Lab Sample  ID,"  enter  the labor
     sample,  as  listed on the  Cover Page.
3.4.3.4  For "Date Received" enter the da
sample was received at the  laboratory, a
Validated Time of Sample Receipt  (VTSR)

3.4.3.5  For "CAS No.," enter the cas
applicable.  If a case number doesn't
provided.
3.4.3.6  Under the column labeled "CONCENTRATION>
result is greater than or equal to the IQL, report
result is lower than the IQL, /eportT
                                                  formatted MM/DD/YY)  the
                                                           ;he TR [i.e., the
                                                           analysis if
                                                        'NA" in the space
                                                               analytical
                                                            result.   If the
                                                        significant
                                                        ree  significant
    3.4.3.7      Analytical resultsNnus\. be^re"po>rted to two
    figures  if  the  result  value  is
    figures  if  the  result  value  is  greater\thn  r equal  to ten.

    3.4.3.8      The requirement for reporting (results to two or three
    significant figures  apoi«rs~~^o  FORM I-AAIN\nly.   Follow the  specific
    instructions  for  reporting allNother resus^tsx^n required forms as
    described in  this Exhibi
     3.4.3.9      Under
     qualifiers  as  id
     qualifiers  are
     Cover  Page  in  t
     3.4.3.10     FORM I - AAItt^inc Itfdes fields for three types of result
     qualifiers.  ^Jhase^gualififths  mu^t  be  completed as  follows:
                                             Q," and "M," enter result
                                             ragraphs.   If additional
                                           ions must be  included  on the
      3.4.3.
      value
      greater
      obt
          E  -
                                     ifier:  Enter "B" if the reported
                            reading that was less than the CRQL but
                           the IQL.  Enter "U" if the reported value was
                               was less than the IQL.

                 (Quality /ionjcrol) qualifier:  Specified entries and their


                          /alue is estimated because of the presence of
July, 1991
                                                               Page B-5/IN
-------
Exhibit B
                                                SOW No. XXX - Ambient Air
                 The sum of the values of the interference/co/rection(s) is
                 greater than the result concentration;
          M  -

          N  -

          S  -


          *  -
            Duplicate injection/exposure precisio

            Spiked sample recovery not within

            The reported value was determine<
            Additions (MSA);

            Duplicate analysis not within/coairol limits; and

            Correlation coefficient for/thgMSA is/les4 than 0.995.
      NOTE:  Entering  "S," or  "+"  is mut
      these qualifiers can appear  in the
 3.4.4  Initial and Co:
     3.4.4.1      This  form
     of calibration

     3.4.4.2
     instructfio
                                                     No combination of
                                                   an analyte.
      3.4.3.10.3   M  (Method)  qualifier:   Enter,  aVvajpprcfp^ate,  the
      following:

       •  P for ICP;

          A for Flame Atomic Absorption'

          F for Graphite  Furnace  Atomic

          MR  if the analyte  is not  require
     3.4.3.11    Under  "Comments,
     concerning the analy/ce pesuT^s a;
     occurred during s
     both technical an
     resolution perfo
                                              -specific comments
                                                ificant changes that
                                              'ermination,  interferences),
                                             tive action taken, and
                                            DG.
                           Lib/ation Verification  [FORM  II  - AAIN]

                                 report analyte recoveries from analyses


                          eader  information  according to the header
                          s\

3.4.4/3 /    Enter  the  "Initial Calibration Source"  (twelve characters
                              alibration Source" (twelve characters
maximum.   Enter "A-     r  EPA-CI" to indicate EPA EMSL-Las Vegas or
EMSL-Cmc^nnat^xjrespec timely, as the source of EPA standards.  When
additional ESA suppled /sol/tions are prepared in the future, the
Contractor musCN^se thw cozies supplied with  those solutions for
identification.  I^vother/sources were used, enter sufficient information
 July. 1991
                                                               Page B-6/IN
-------
Exhibit B
   SOW No. XXX  - Ambient  Air
     in  the  available  twelve  spaces  to identify the manufacturer and  the
     solution  used-

     3.4.4.4    ..Use additional copies of FORM II-AAIN  yi"  njo're  calibration
     sources were  used.

     3.4.4.5     Under "WAVE," enter the number of tlie  ySvelengfck  for which
     the results of  each  analyte  are reported on the form.   The wavelength
     number  is a number assigned  to  each wavelengtk{ us4d when mo
     wavelength is used to obtain data for analyte^V the SDG.  A wa"velengt
     number  of "1" is  assigned to the longest wavelength used for the  ahalyte
     in  the  SDG.   A  wavelength number of "2" is/asisigned to the second longest
     wavelength and  so on.  The field must be/le£c blank/if a single
     wavelength is used to obtain data for an analyte in/th/s SDG.
     3.4.4.6      Under "INITIAL CALIBRATION T each  analyte
3.4.4.8     Under  "INITIAL CALl
nearest whole number) of the per*
following equation:

                        a. „   Found (.
                                                 enter the
                                         vrecove
                                   True(1C
                                             x/00
         ?alue (to the
         according to the


              Eq. B/IN-1
       Where True  (ICV)  is/the  trufev concentr&tioi
     Initial Calibration 37eri£rc-SL£ion solution >and
     concentration of th4 analyte Xn
     Solution.
of the analyte in the
 'ound  (ICV)  is  the  found
 ibration Verification
     3.4.4.9     Unde'r IJtpNTINUItfG CALIBRATrON-Arue,"  enter the true
     concentration (^n jig/l>. to/thtree decimal places) of each analyte  in  the
     Continuing Calibration Verification Solution.

     3.4.4.10    Under" CONTlMmTG CALIBRATION  Found,"  enter the found
     concentrati*fn~(iriMg/Lv. to thcee de^sdmal places) of each analyte  measured
     in the Contiipj*Rg—Qalibrae ion Ve'r^f/cation Solution.

     NOTE:  /The7form containsvtwX "CONTINUING CALIBRATION Found" columns.   The
     column t
-------
Exhibit B
                                                      SOW No.  XXX - Ambient Air
     3.4.4.11     If more than one FORM  II-AAIN  is  required,
     Continuing Calibration Verifications, then the colum;
     second  form must contain values for the third Conti
     Verification,  the column to the right must contai
     Continuing Calibration Verification,  and so on.

     3.4.4.12     Under "CONTINUING CALIBRATION  %R,"
     nearest whole  number)  of the percent recovery
     following  equation:
                                              report multiple
                                             'the  left  on the
                                             Calibration
                                              for the  fourth
                                  Found (CCV}
                                   True (CCV)
                             xAOO/
       Where True (CCV) is the true concentration  of  eac
    (CCV) is  the  found concentration  of ther analyte in/th$
    Calibration Verification Solution.
                Eq. B/IN-2

            lalyte, and  Found
            Continuing
    NOTE:  The  form  contains two "CONTINUING C&t>IBRATl6N ZR" columns.
    Entries to  these columns must follow the sequence det^ojed above for
    entries to  the "Continuing Calibration Found" columns.
    3.4.4.13
Under "M," enter the methoc
    3.4.4.14     If more than one
    then submit additional  copies  of
                         ;th  is
   as in partM. 4. 3.10. 3.

rsed-JEg__analyze an analyte,
[N/as  appropriate.
    3.4.4.15     The order of reporting I&Vs and/CCVs for each analyte must
    follow the chronological  order  in which. the{ standards were run starting
    with the first  FORM  II^ASlT^nd moving fXom\he left to the right,
    continuing to the  foLIowingFORh> II-AAIN *s  appropriate.   For instance,
    the first ICV for  ali  analyte*  mAst__be repo\ted> on the first FORM II-
    AAIN.  In a  run where  /hree  CCVs Verea^AlyzeV;  the first CCV must be
    reported in  the la€tyCCV  column op-6be firW^FORM II-AAIN and the second
    CCV must be  reported/in the  tfight columia^of/the same form.   The third CCV
    must be reported inShe lefz CCv column of the second FORM II-AAIN.   On
    the second FORM rS4^AAIN>^t)ie ICV column and  the right CCV column must be
    left empty in this example.  An the previous  example,  if a second run for
    an analyte was  needed, the 1CV^Nif that run must be  reported on a third
    FORM II-AAIN^^tni—ths^^CCVs rb4^.ow rn^the same  fashion as explained before.

    3. 4.4.16 /   .intne^^se  where more^han one wavelength is used for an
    analyte/in /the  SDG,  aUNICVNand CCV  results  of the  longest wavelength
    from a/1 i/uns must be  rep'srte^d  before  proceeding to report the results of
    the s/cojtfd wavelength  used\and,  so on.

    3.4.4>L7   "Bunder "Commentts,"I enter any ICV and CCV specific comments
    concernirTgv^the  analyte reAilCs,  any  significant problems encountered
    during the fE^and^SCV analysis (i.e., percent recovery outside the
    control limits/^interferences),  both  technical and administrative,  the
    corrective action  ta^en, ,4nd resolution performed for the ICV and CCV.
July, 199L
                                                   Page B-8/IN
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Exhibit B
                                                SOW No.  XXX - Ambient Air
3.4.5 Contract Required Quantitation Limit  Standards/Linear^Range Standards
      [FORM III.T AAIN]
     3.4.5.1  Contract Required Quantitation Limit  Stan

      3.4.5.1.1  This form is used to report analyte
      of the CRQL Standards.

      3.4.5.1.2  Complete the header information a(cc
      instructions and as follows.
                                                        s  from  analyses
                                                 zurce of the CRQL Standard
                                                            (twelve characters
                                                         r as explained in
3.4.5.1.3  Under "SOURCE USED," enter
for ICP and GFAA analyses in their res
maximum each),  as explained in part 3/4

3.4.5.1.4  Under "WAVE," enter the
part 3.4.4.5.
      3.4.5.1.5  Under "INITIAL True." enter the^rue concentration (in
      to three decimal places) of each analyte in theiCRQlNStandard Source
      Solution that was analyzed for analytical s amp lesNa^s so elated with  the
      SDG.

      3.4.5.1.6  Under "INITIAL Found.X ent&r^the found concentration (in
      jug/L, to three decimal p 1 aces)\of^each aOaly€e~TneasArred  in  the CRQL
      Standard Solution analyzed at tree beginnin  of each run.
                                      \ V /
      3.4.5.1.7  Under "INITIAL %R," entefcthe/value (to the nearest whole
      number) of the percent^x&covery computedNaccording to the following
      equation:
      3.4.5.1.8  Und«
      to three dec IE
      Solution anar<
          CRQl

    flNAL  Foufcd,
   >laces)
                                            Tr ue\/
                                               X 100
                                                                Eq. B/IN-3
     ch
:ed
end/ of
                                      the /found concentration (in fig/L,
                                         measured in the CRQL Standard
                                each run.
      3.4.5.1.9  Under
      number) of the__percent^
      equation>
                          <^ enter the value (to the nearest whole
                                computed according to the following
                                Standard Final Found
                                SQL Standard True
                                              X 100
                                 Eq. B/IN-4
      NOTE: /For every initial] solution reported there must be a  final one.
      H6weyer>v^he opposite is/ not true.  If a CRQL Standard was  required  to
      be an^yzea^n the middle of a run (to avoid exceeding the  8-hour
      limit) ,  >t mus^fexbe rep>6rt/d in the "FINAL Found" section of this form.
July, 1991
                                                              Page  B-9/IN
-------
Exhibit B
                                                      SOW No.  XXX - Ambient Air
      3.4.5.1.10  If more CRQL standards analyses were  re/uir4d or analyses
      were performe.d using more than one wavelength per >ana*yte,  submit
      additional copies of FORM III-AAIN in  the appropr/Lat/ order .
                                    eaKanalyte must
                                      re rtm starting
      3.4.5.1.11  The order of reporting CRQL s tandarr&s
      follow the chronological order in which the st4ndards
      with the first FORM III-AAIN and continuing to  ohe  followl*^  FORtt^III-
      AAIN as appropriate.  When multiple wave len§^htf are used  for^sne
      analyte, all the results of one wavelength/rau^t be  reported befoo
      proceeding to the next wavelength.

      3.4.5.1.12  Under "Comments," enter anV" CRQL-specLtic7comments
      concerning the analyte results , any significant ptob/ems  encountered
      during the CRQL standard analysis (e/g. /percent/ recovery outside  the
      control limits), both technical andsadmintsxratave/; the corrective
      action taken, and resolution performeo^Cor tne  standard.
    3.4.5.2  Linear Range Standards

      3.4.5.2.1  FORM III-AAIN is a
      analyses of the Linear Range/Standards'
                5ed  to  report  analyse Xecoveries from
3.4.5.2.2  Complete the header\.i
instructions and as follows.
                irmatio
                                                            o the header
      3.4.5.2.3  Under "SOURCE USED,"
      analyses in their respective fields 03,2
      explained in part 3.
                    the/source  of  the  LRSs  for ICP
                       ^aracters maximum each),  as
      3.4.5.2.4  Under "J
      part 3.4.4.5.
?AVE
      ent
                                   javelength/number as explained in
      3.4.5.2.5  Under "INITIAL
      to three decimal pi
      was analyzed for-v£he
                         true  concentration (in
           ich  analyte  in the  LRS Source Solution that
        :ycal samples associated with the SDG.
      3.4.5.2.6  Under "INITlCAL Fouhd " enter the found concentration (in
      Mg/L, to t}*ree~~3e-eiDial plates) orxeach analyte measured in the LRS
      Solution/analyzed at the begirtn^g/of each run.

                                  ," enter the value (to the nearest whole
                                  ery computed according to the following
                                   Initial Found
                                   LRS True
                        X 100
                                                          Eq. B/IN-5
      3.4.5.2.8
      to three decims
      analyzed at the en£
      Fyund,"  enter  the  found concentration (in
     )/of each analyte measured in the LRS Solution
      ach run.
July, 1991
                                          Page B-10/IN
-------
Exhibit B
                                 SOW No. XXX - Ambient Air
      3.4.5.2.9  Under "FINAL %R," enter the value  (to  the
      number) of_ the percent recovery  computed according
      equation:
                                LRS Final Found
                                   LRS True
                           X 100
                      nearest whole
                           following


                           Eq. B/IN-6
      NOTE:  For every initial solution  reported the.
      However, the opposite is not true.   If  an LR:
      analyzed in the middle of a run  (to  avoid e
      it must be reported in the "FINAL  Found"  s
      3.4.5.2.10  If more LRS analyses were  re
      performed using more than one wavelengty
      copies of FORM III-AAIN in the appropr,
                               d or analyses were
                                        submit additional
      3.4.5.2.11  The order of reporting
      the chronological order in which  th'
      the first FORM III-AAIN and continuing
      appropriate.  If multiple wavelengths are
      results of one wavelength must be reported
      wavelength.
                                      analyte must follow
                                      run starting with
                                   lowing FORM III-AAIN as
                                     one analyte, all the
                                        Ceding to the next
      3.4.5.2.12  Under "Comments,/1 enter  anyTRS^specific  comments  concerning
      the analytes results, any signif\caiTt~-p«Qblems  encountered during the
      LRS analysis (e.g., percent recovery outs/de/"Etre—control  limits),  both
      technical and administrative, tntecorrec/civX action taken,  and
      resolution performed for the stanoard\
3.4.6 Blanks  [FORM IV - AAINJ

     3.4.6.1     This focm is^osed
     the  Initial Calibra/ciopr Blank\(ll
                  report ahalyi
                      :he Cont:
                concentrations found in
              iuing  Calibration Blanks
     (CCB),  and the Preypar/tion Blink (PB).
     3.4.6.2     Con
     instructions ar
-------
Exhibit B
                                                      SOW No. XXX - Ambient Air
     3-4.6.5      For all blanks, enter the concentration
    '(positive  or.negative)  measured above the IQL or be
     of the  IQL.
                                                        e/ch analyte
                                                         ie negative value
     3.4.6.6      Under the "C" qualifier field, for any analytfexenter "B" if
     the  absolute  value  of the analyte concentration/is XlesV^hantke CRQL but
     greater  than  or  equal to  the  IQL.   Enter "U"  i/ tj*e absolu^val^e^of the
     analyte  in the blank is less  than the  IQL.
     3.4.6.7
             Under "CONTINUING CALIBRATION
    concentration  (in  Mg/L,  to  three  decimal places) of
    in  the  first required  CCB analyzed after/the/ICB.
    qualifier, as  explained  for the  "Initial Calibratic
    qualifier column immediately following/thg "CONTI&fUIt
    1"  column.
                                                      ich analyte detected
                                                     itejr any appropriate
                                                       .ank," in the "C"
                                                       CALIBRATION BLANK
    3.4.6.8      If only one CCB was analyzed, Shen leaVethe columns  labeled
    "2" and  "3" blank.   If  up  to  three  CCBs  were an^vzedXcomplete the
    columns  labeled  "2"  and "3,"  in accordance with thV^ns tractions for the
    "CONTINUING CALIBRATION BLANK 17^cOumn_ If more thkrixtWe CCBs were
    analyzed,  then complete additional  copT^e^-Df-JQRtllV-AAItras appropriate.

    3.4.6.9      Under "PREPARATION BLANK, "ente? ^h«-cance/tration  (in
    to three decimal  places) of each atnal^te ij/i tWe PB.   Enter any
    appropriate qualifier,  as  explained\for\tXe  Z'CB,  in the "C" qualifier
    column immediately  following  the "PRE^ARATI/N BLANK"  column.
    3.4.6.10
    3.4.3.10.3.
            Under  "M, 'Venterx6he method
                  as explained in part
    3.4.6.11     If mon
    submit additional/coi
                     tfafan one ^avelengtt
                     i.es of FC
           J.s us«d to analyze an analyte,
                appropriate.
                     order^of
3.4.6.12    Th
follow the chrono
the first FORM IV-
the following FORM IV-
wave lengths _^arS~~u§eri^for ttv
                      -AATtl and
   ing ICBs and CCBs for each analyte must
   in which the blanks were  run starting with
Eving from  left to  right  and continuing to
    lained previously.   When multiple
         of one  analyte,  all the results of
                               as e~
                                  in,
.aly*
    one wavel^gthjou^t be >€^ortedN^foXe  proceeding to the next wavelength.

                 Under "ConmYantsV  enter any ICB and CCB specific comments
           ling'  the analyte results, any significant  problems encountered
            tjie  ICB, CCB and  PB\anAlysis (i.e.,  blanks outside the control
               jth technical  and administrative,  the  corrective action taken,
    and re^Qlutib«^performed for /he  sample.

3.4.7 ICP Interf^tH-snce^'Ch^cl/Samile [FORM V - AAIN]

    3.4.7.1  This form i^used to report ICP Interference  Check Sample (ICS)
    results  for each  ICP  instrument used in SDG analyses.
JuLv, L991
                                                                   Page  B-12/IN
-------
Exhibit B
                                                      SOW No.  XXX -  Ambient Air
3.4.7.2  Complete the header information according to
instructions and as follows.
                                                               header
     3.4.7.3   Fo.r  "ICP  ID  No.,"  enter an identifier thatf uniquely identifies
     the  specific  instrument within the Contractor lab/rat^ry .   No two ICP
     instruments within a  laboratory may have the sam£ ICP

     3.4.7.4   For  "ICS  Source,"  enter the ICS sour
     maximum  each),  as  previously explained in paZ£ 3/4.4.3.
     solutions, include the name and number iden/Mjang it ( e . g . ,
     The  laboratory  must use the identification/supplied by the EPA.

     3.4.7.5   Under  "WAVE,"  enter the wave length /number f*»r which  the  results
     of each  analyte are reported on the for4.  /The wav/lerigth  number  is a
     number assigned to each wavelength usett when more/ th^n one wavelength are
     used to  obtain  data for an  analyte iri th^SDG.  A w/velength number of
     "1"  is assigned so the longest wavelength uS^d/ror/the analyte in the
     SDG.  A  wavelength number of "2" is assigned to me second longest
     wavelength and  so  on.   The  field must be lerXblanfexif a single
     wavelength is used to  obtain data for an analyt^in tfre^SDG.
    3.4.7.6  Under "TRUE Sol. A,"
    three decimal places)  of eaci:

    3.4.7.7  Under "TRUE Sol. AB,"
    three decimal places)  of each  anal

    3.4.7.8  Under "INITIAL  FOUND  Sol.
    Mg/L to three decimal  t^Laees)  of  each
    analysis of Solution/A as reqt

    3.4.7.9  Under "IN^TI
    Mg/L to three
    analysis of Sol
                                        true concentra^tipfa (in Mg/L,  to
                                                   lution A.
                                                      7
                                                      ration  (in Mg/L,  to
                                              in Solution AB.

                                          er the found concentration  (in
                                              measured in the  initial
                                              E.

                                              the found  concentration (in
                                           te measured in the  initial
                                            it E.
    3.4.7.10     U
    whole number) of
    equation:
                              d "%R," enter the value (to the nearest
                             recovery computed according to  the  following
                                        Solution AB
                                         ion AB
                                                    X 100
                                                           Eq. B/IN-7
    3.4.7
    negative,
    by ICP.
                                 ND," enter the found concentration (in
                                  ach analyte  measured  in  the  final  analysis
                          values, enter the concentration (positive,
             zerb-iof e^ch/analyte at each wavelength used for analysis
July, 1991
                                                              Page  B-13/IN
-------
Exhibit  B
                                                      SOW No. XXX - Ambient Air
    ^3.4.7.13    Under FINAL FOUND  "%R,"  enter  the  value /to/the nearest whole
     number)  of the.percent recovery computed according /o ehe following
     equation:
   Found Solution AB
 True Solution AB
                                                      LOO/
                                                Eq. B/IN-8
     NOTE:   For every initial solution reported
     However,  the opposite is not true.   If an
     in the middle of a run (to avoid exceeding
     reported  in the "FINAL FOUND" section of
                                    r             ~^
                                     must be a final one>
                                  fas required to be analysed
                                   8-hour limit), it musrbe
                                  form.
     3.4.7.14    If more ICS analyses were
     of  FORM V-AAIN as  appropriate.
                           required,  si
                              additional copies
     3.4.7.15     The order of reporting ICS>xall the results of
     one wavelength  must  be reported~±K^ar^_proceeding to Che^^ext wavelength
     in the  same  manner.
    3.4.7.16     Under "Comments," ehte
    the  analyte  results, any  signific
    analysis  (e.g., percent recovery ouXrsi
    technical  and  administrative,  the
    performed  for  the  sample.
                        any ICS" stfe-ei£ic^bmments  concerning
                          robl/ems*'encountered during the ICS
                            /th? control limits), both
                                 action taken, and resolution
3.4.8 Spike Sample Recovi

     3.4.8.1      This
     recovery which  i
     the  pre-digest
                     - AAIN]
     3.4.8.2      Comp
     instructions  and as
                            ^results for the spike sample
                                 known quantity of analyte to
                 er information according to the header
     3.4.8.3    x^Tn the~-^PA SAtfN^E NOX^box,  enter the EPA sample number (7
     characters maximum) of^the  sample  from which the  spike results on this
     form  wez%  afertainedT^xrhe number  must  be centered  in the box.   Note that
     the EP/. sample  number ntust  include the spike sample suffix for which the
     spike/analyses  are reported.
     3 .448 .4
Under "WAVE,"
enner the wavelength number for which the
     result&of  e^Stch  analyte  are  i/eported on the  form.   The wavelength number
     is  a  number assigned  to^acti wavelength used when more than one
     wavelength  isxused  Txiobta^n data  for an analyte  in the SDG.   A
     wavelength  numbels^of  "1"  /s  assigned to the  longest wavelength used for
     the analyte in the5fi£. /A wavelength number of "2" is assigned to the
July, 1991
                                                  Page  B-14/IN
-------
Exhibit B
                                                 SOW No. XXX - Ambient Air
    second  longest  wavelength  and  so  on.   The field must beleft blank if a
    single  wavelength  is  used  to obtain data for an analyse yn the SDG.
    3.4.8.5     .Under "CONTROL LIMIT %R," enter "75-12:
    value was  greater  than  or  equal  to  one-fourth  of the
    If not,  leave  the  field empty.
                                                         the spike added
                                                      Cample result value.
     3.4.8.6      Under "SPIKED SAMPLE RESULT (SSR) J erfter th^condftntration
     (in Mg/L,  to  three  decimal  places)  of  each an^lyoe in the spike saisgle.
     Enter any  appropriate  qualifier  in  the "C" cnS&J^trier column
     following  the Spiked Sample Result  (SSR)  co/lump
                                                           entration (in A*g/L,
                                                           ,e sample (reported
                                                             was performed.
                                                          column immediately
3.4.8.7     Under  "SAMPLE RESULT  (SR),"
to three decimal places) of each analyt
in the EPA sample number box) on which
Enter any appropriate qualifier in th
following the Sample Result (SR) col
                                        \^  "   C
3.4.8.8     Under  "SPIKE ADDED  (SA),"  enter^he  concentration (in
to three decimal places) of each analyte added ts^the sample.  If the
"Spike Added" concentration is specified in the cont^act/The value added
and reported must be that speci?Tc~-c«ncgivtration  in
     3.4.8.9      Under "%R," enter
     the percent  recovery  computed ac
     NOTE:   %R must  be  rep
     value  of zero must
     than  the IQL.

     3.4.8.10    Unde
     control limits
     one-fourth of

     3.4.8.11    Under
     is  not required_in_the

     NOTE:   I
     differe
     for ea
                                                         whole  number)  of
                                                       .g equation:

                                                            Eq. B/IN-9
                                              tive, positive or zero.  A
                                                analyte value is less
                                             e recovery (%R)  is  out of the
                                           .ed is- greater than or equal  to
                              :he  method used or enter "NR"  if the analyte
                          s were"~s4s£d for spike sample analysis  of
                            al copies of FORM VI-AAIN must be  submitted
     3.4.8.13
     concerning the
                               ies  of FORM VI-AAIN for each sample on
                              analysis was performed.

                          ts/"  enter any spike sample specific comments
                           Its, any  significant  problems  encountered
July,  1991
                                                              Page B-15/IN
-------
Exhibit B
                                                      SOW No.  XXX - Ambient Air
    during  the  spike  sample  analysis  (e.g.,  percent recovery/outside the
    .control  limits),  both  technical and administrative,  /the/corrective action
    taken,  and  resolution  performed for the  sample.
3.4.9 Analytical Spike Sample Recovery [FORM VII  -

     3.4.9.1      This form is used to report result
     recovery which  is based  upon the  addition of
     to an aliquot of the  digested sample.

     3.4.9.2      Complete the header information
     instructions and as  follows.
                                                  EN],

                                                     the ahaj-ytic^l  spike
                                                 town quant ity^-af ana'iyte


                                             According to the header
    3.4.9.3      Under "WAVE," enter the wavelength numbe*1 for which  the
    results of each analyte  are  reported 4n  thexjfprm/  The  wavelength number
    is a number  assigned  to  each wavelength^used wh/n nfore  than one
    wavelength are used to obtain data  for an analyte 4^1 the SDG.  A
    wavelength number of  "1"  is  assigned to  the  longest waj^elength used for
    the analyte  in the SDG.   A wavelength number of "^'i^is  assigned to the
    second longest wavelength and so—on_^The field mustibe le/t blank if a
    single wavelength is  used to optainda^a-f^L^an analyte rn the SDG.
3.4.9.4      In  the  "EPA SAMPLE Ko. '\box,
characters maximum) of  the sample\froln whij
form were obtained.  The number mus
the EPA sample number must include tl
spike analyses are reported.

3.4.9.5      Under  "CONTROL LIMfcr %R"  and\Q'
blank until  limits are  erstaD^ished_by the
Contractor will be/infprmed on) he
                                                 er—ttieEPA/sample number  (7
                                                   ie  spilce results on this
                                                 sred  in the box.   Note that
                                                  sample suffix for which the
                                                  the fields must be left
                                                     At  that time,  the
                                                    these  fields.
    3.4.9.6      Under "S'PIKED SAMPLE' RESUtS^SSR) ," enter the concentration
    (in Mg/L, to th/ee ctecimal /laoes),  for  each  analyte in the  analytical
    spike sample.  Ehfeer any\a£prorpriate qualifier  in the "C"  qualifier
    column immediately foj^owing^the  spiked  sample  result column.

    3.4.9.7      Ifedsr^^AMPLE RESULT>SR),"  enter the concentration
    to three decimal  placeS-^.  for &ach analyte  measured in the sample
    (reported^ inx^fie~El>ft^sampx>e numbeiNbox)  on  which the analytical spike was
    performed./Enter any  appropriate qualifier in  the "C" qualifier column
                 following  th\"SMPLE RESULT (SR)"  column.

    3.4.^.8 X^^ Under "SPIKE AbDED (SA),"  enter the concentration  (in pg/L,
    to tfrfree decimal  places)  of eAch analyte added  to the sample.   If the
    spike acKte^ conc-entratior/ is/specif ied in the contract,  the  concentration
    added and reTxjrteo^must/oe ,that  specific concentration in
July, 1991
                                                              Page  B-16/IN
-------
Exhibit B
          SOW No.  XXX - Ambient Air
     3.4.9.9      Under "%R," enter the value (to the nearest whole number)  of
    _ the  percent  recovery for all spiked analytes computed/according to the
     following  equation:
                                   SSR - SR
                                      SA
X 100
               Eq.  B/IN-10
       %R must be reported, whether it is negative,
       A value of zero must be substituted for SS
    concentration  is  less  than the  IQL.

    3.4.9.10     Under "M," enter the method u,
    is not  required  in  the spike.

    3.4.9.11     If different samples were
    different analytes,  additional  copies/of
    for each sample  as  appropriate.
    3.4.9.12     Use additional copies of FORM
    which a required  spike  sample  analysis was  per
    3.4.9.13     Under "Comments,"
    comments concerning  the  analy
    encountered during the analyti
    recovery outside  the  control  liniitsX both/tec
    the corrective action taken,  and  reso
                                       \ V /
3.4.10 Duplicates [FORM VIII - AAIN]
       r enter "NR" if the analyte
              sample analysis of
              N must be submitted
             or each sample on


 analytical spr
              ample specific
             problems
le analysT^ (e.g.,  percent
           ,d administrative,
/erformed for the sample.
    3.4.10.1     This form/is used\to report"
    determining  the  prec/sion—of, the^ method.

    3.4.10.2     Compl/te/the header infoi
    instructions and/as /follows ./
      Its of duplicate analyses for


 ton according to the header
    3.4.10.3     In^he lTB£A SAtfPLE' NO." box,  enter the EPA sample number (7
    characters maximuiit^of  the  sample  from which  the  duplicate  results  on
    this  form were  obtaine<.  THa. number must be  centered  in  the  box.
                                   r tne^wavelength number for which the
                                          on  the  form.  The wavelength  number
                                   avelength  used when  more than  one
                                  data  for an analyte in  the  SDG.  A
                                  Assigned  to  the  longest  wavelength used for
                                   elength number of  "2"  is assigned  to the
                                   so on.   The field  must be  left blank if a
                                  obtain data for an  analyte  in the  SDG.
                       Page  B-17/IN
July, 1991
-------
Exhibit B
                                                      SOW No.  XXX -  Ambient Air
    3.4.10.5     Under "CONTROL LIMIT %R," enter the numerical value of  the
    . CRQL  (in  Mg/D  for  the  analyte if the sample or duplicate values were
    less  than five' times  CRQL.   If the  sample and dupl/cacfe values were less
    than  the  CRQL or  greater  than or equal to five ti;ftes GRQL,  leave the
    field empty.

    3.4.10.6     Under "SAMPLE (S)," enter the con/entzration
    concentration units,  to three decimal placesl^af/each analyte^-in
    original  sample (reported in the EPA sample/nunfoer box) on whicn1
    duplicate analysis  was  performed.   Enter any appropriate qualifier it*/the
    "C" qualifier column  immediately following tbfe "SAMPLE (S)"  column.

    3.4.10.7     Under "DELICATE  (D)," ent/r Ghe concentration (in the
    required  concentrati-   units,  to threer de/imal place/) of each analyte
    measured  in  the Dupli;ate sample (rep^ortecNin thfe  E.PA sample  number box).
    Enter any appropriate qualifier in  the^^' qua^lfi/r column immediately
    following the "DUPLICATE  (D)"  column.

    3.4.10.8     Under "RPD,"  enter the absolute value\(to  tha nearest whole
    number) of the  Relative Percenc-Hifference for all arta^yta^  detected
    above the IQL in  either the  sample^r^Efre-du&Hcate, commuted according
    to the following  equation:
                               ___   \l     Y  /~~^—~^ /
                                                                 Eq. B/IN-11
    3 . 4 .10.10    Unde
    analyte  is  out
    values  are  gre
    less  than or  eq
    duplicate values  ar
    difference  between the
    to  be in control.	if botK
    limit is applicable.
    3.4.10.9     A value of zero must be st
    concentration is  lessfiftarT~the  IQL in el
    concentration is  les?  than_ the
    empty.
                                          ktuted  for S  or  D  if the  analyte
                                             one.  If the analyte
                                              nd D, leave the RPD  field
                                            Licate  analysis  for  the
                                          pioth sample and duplicate
                                    five times CRQL, then the RPD must be
                                 to be in control.   If either sample or
                               five times CRQL, then the absolute
                                  must be less than or equal to the CRQL
                                   nre below the CRQL, then no control
     3.4.10/11 / Under "M,^Nente-r the method used.

                 If different Camples were used for duplicate sample analysis
              |nt analytes,  thejn additional copies of FORM VIII-AAIN must be
                   each sample/as/appropriate.
3.4.10.13
which a requiret
                     aeLtiohal/copies of FORM VIII-AAIN for each sample on
                      dupiircat^ sample analysis was performed.
July, 1991
                                                              Page B-18/IN
-------
Exhibit B
                                                 SOW No. XXX  - Ambient Air
     3. 4. 10. 14    Under "Comments , " enter any duplicate  sample  specific
   '  comments concerning the analyte results,  any signif ioant/ problems
     encountered during the- duplicate sample analysis (i/e. , /per cent recovery
     outside  the control limits), both technical and adrgini/strative , the
     corrective  action taken,  and resolution performed/for^the sample.
3.4.11 Laboratory Control Sample  [FORM  IX-AAIN]

     3.4.11.1     This form is used to report resul
     Control Sample  (LCS).
                                                 for the Labbratoi
     3.4.11.2     Complete the header information According  to  the  header
     instructions  and as follows.
     3.4.11.3     For "LCS USED," enter the/appropriate/source  solution
     identifier (12 characters maximum)  provided by tine EPA for the LCS
     solution  that  was  analyzed by the methods irN£j9nib/t D.

     3.4.11.4     If no analyte was analyzed by assert a ihxmethod or  if the
     analyte was  not required to be analyzed,  then le^ave thexappropriate
     spaces empty.
3.4.11.5    Under "WAVE,"  en
results of each analyte are  re
is a number assigned to each wa
wavelength is used to obtain data
wavelength number of "1" is assigne
                                          javelengt
                                          th
                                            n
                                          to
              for which the
          The/wavelength  number
              than one
        in the SDG.  A
he/longest wavelength used for
     the  analyte in the SDG.   A wave lengthV numtfer of "2" is assigned to the
     second longest wavelength— and so on.   The 5ield must be left blank if- a
     single wavelength is/used to obtain data\for\an analyte in the SDG.
     3.4.11.6
             Under/M,/ enter\tht
     3.4.11.7    Und^r ^LIMITS, "/ente'r tfte^lowe/  limit  (to  the  nearest whole
     number)  in the Aef^column/arya the uppe~r~4imit (to the nearest whole
     number)  in theSs^ghtc-o^lumn f/jr each analyte in the LCS.

     3.4.11.8    Under "TlttJE." ert^r the true concentration (to three  decimal
     places)  of ea^h  analyte itv^the
3. 4.11. ft/   JJrnteTS^FOUNr
decimal/places) of eash aris
                                           found concentration (to  three
                                lyte measured in the LCS.
     3.4.11.10   Under
     found v4lue of the LCS.
                        enten "B" or "U" or leave empty to describe the
     3.4.11>Li    uruter
     the percemxreco
                   •%R," y4nt«tr the value (to the nearest whole number) of
                      coinputfed according to  the  following equation:
                          *R = LCS FOUND x 100
                               LCS TRUE
                                                                  Eq. B/IN-12
July,  L991
                                                               Page  B-19/IN
-------
Exhibit B
                                                      SOW No.  XXX - Ambient Air
    ^3.4.11.12   If the analyte concentration is  less  tha
     zero  must be"substituted for the LCS Found.
                                                           IQL, a value  of
     3.4.11.13   Submit additional copies of  FORM  IX-A/IN asNmpropriate,  if
     more  than one  LCS was required.   In addition,  sujaimit^additiboal copies of
     FORM  IX-AAIN if more than one wavelength was us/d t?b de^fermineNin analyte
     for a sample.                                  '   '       ^    ^

     3.4.11.14   Under "Comments," enter any  LCS/specific comments  concte
-------
Exhibit B
                    SOW  No. XXX  - Ambient  Air
     3.4.12.7     Under "0 ADD ABS," enter the observed value in absorbance
     units  (to three decimal places)  of the  analyte before/addition is
     performed.

     3.4.12.8     Under "1 ADD CON," enter the concentr/tiofo in pg/L  (to  three
     decimal places) of the analyte  (excluding sample/contribution) after
     first  addition to the sample analyzed by MSA.
     3.4.12.9     Under "1 ADD ABS', enter the obs
     decimal places)  of the sample solution spik<

     3.4.12.10   Under "2 ADD CON," enter the
     decimal places)  of the analyte (excludi
     second addition to the sample analyzed
                      value in 7»g/L
                    th the first ac

                 ^rved value in Mg/L (to three
                         y.bution)  after
     3.4.12.11   Under "2 ADD ABS," enter/the
     decimal places)  of the sample solutio

     3.4.12.12   Under "3 ADD CON," enter the ob
     decimal places)  of the parameter (excluding sanf
     third addition to the sample analyzed by MSA.
                        lue in Mg/L (to three
                       the second addition.

                         ue in fig/L (to three
                            ibution)  after
     3.4.12.13   Under "3 ADD ABS ,<" enterdie obseTv«KLj£alue in /ig/L  (to  three
     decimal  places)  of the sample \olu^7cm"~5p-iked with the7third addition.
     NOTE:   The "0 ADD ABS," "I ADD AB*
     have  the same dilution factor.
                             ADD ABS"  must
     3.4.12.14   Under "Fin
     (in Mg/L to two decimal
     computed according
     NOTE:   The fin,
     value  for that
     sample.

     3.4.12.15
     places)  t
     the foll/Jwi
     ABS"),
     corre
     squ-ai/e
     enterVtheVfinal analyte concentration
    in the sSmipDs^ as determined by MSA
 losing formul

                                   Eq.  B/IN-13

             Ter does  not have to equal the
   is reported  on FORM  I-AAIN for that
     correlation coefficient  (to four decimal
        squares regression line representing
            ABS"),  ("1 ADD CON," "1 ADD
ABS"),  and ("3 ADD CON," "3 ADD ABS").   The
 be calculated using the ordinary least
 eighted) according to the following formula:
                                                                   _Eq.  B/IN-14
 July,  1991
                                  Page B-21/IN
-------
Exhibit B
                                                 SOW No. XXX - Ambient Air
     3.4.12.16    Under "Q," enter  "+"  if r  is  less  than  0/99/.   If r is
    'greater  than-or equal to 0.995,  then leave the fiel

     3.A.12.17   - Under "Comments," enter any signific
     during the  method of standard addition analysis
     administrative, the  corrective action taken, a
     the  sample.
                                                              encountered
                                                                 and
                                                                       for
3.4.13 ICP Serial Dilution  [FORM XI  - AAIN,]

     3.4.13.1     This form is usd to report re'su^s for T£P  serial  dilution.

     3.4.13.2     Complete the header inform/tiofo according/to  the header
     instructions  and as  follows.
     3.4.13.3     In the "EPA SAMPLE NO."
     (seven  characters  maximum)  of the sample ft
     analysis  results on this form were obtained.
     in  the  box.
                                                    EPA sample number
                                              whi&h^the serial  dilution
                                                  numbejr must be  centered
     3.4.13.4     Under "Initial Sample ResultT^i-H-^enter  the"concentration
     (in Mg/L,  to  three  decimal pla^esyro~f--«acJianalyte~"T3r--she original sample
     (reported  in  the  EPA sample number BOX) on"^rhich--a^serAal dilution
     analysis was  performed.   Enter anV apRropraat/4 qualifier in the "C"
     qualifier  column  immediately follow^ng\^e ^Initial Sample Result (I)"
     column.
NOTE:  The Initial S
equal the value for ifoat
It is the value of the
that is within th
                               CorteentrationVor
                                      reported\on
                              alyi
                        linear ranie of
itratiot
    istr
 analyte does not have to
 RM I -AAIN for that sample.
 ncorrected for dilution)
ent.
     3.3.13.5     Und
     (in /ig/L,  to three
     (reported in the
     analysis  was perform
     qualifier column  immedia:
     column.
                     erial  D^luclon Resttl^/S),"  enter the concentration
                      imal/places) of each analyte  in  the  diluted  sample
                               toer box) on which a  serial  dilution
                         EnGe.r any appropriate qualifier  in  the  "C"
                                lowing  the "Serial  Dilution  Result (S)"
     NOTE:   The SCrial fftiutions Result TS) is obtained by multiplying by  five
     the instrument measureo\conHentration value ( in Mg/L) of the serial
     dilutee sample and that the \C" qualifier for the serial dilution must  be
               i based on the s\erial dilution result before correcting it for
                  regardles of /the) value reported on the form.

     3 . 4.13 . 6^\_ Uncte-r  "Dif faren/e , "  enter  the  absolute  value (to one decimal
     place) of tn^xpercent difference  in concentration of required analytes,
     between the orig~inal sample and the diluted sample  (adjusted for
     dilution) according^cp the following equation:
 July,  1991
                                                              Page  B-22/IN
-------
Exhibit B
                                                      SOW No.  XXX -  Ambient Air
                      % Difference =
x 100
     NOTE:   The values for I and S used to calculate X
     equation must be exactly those reported on this
     must  be substituted for S if the analyte concen
     IDL.   If the  analyte concentration in (I)  is
     concentration,  leave the "% Difference" field
     3.4.13.7     Under "Q," enter "E" if the pe
     than 10 percent and  the original sample conce
     I-AAIN) is  greater than 50x IDL reported/6n /ORM XII
                                                                  Eq.  B/IN-15
                                                      ference  in the
                                                                of zero
                                                             js  that the
                                                 difference is
                                              tration  (reported on  FOl
                                                        IN.
     3.4.13.8
             Under  "M,"  enter the metho/1 used.
3.4.14 Instrument Detection Limits  [FORM
     3.4.14.1     This form documents the Instrument Det>&£ion Limit (IDL) for
     each  instrument  that  the  laboratory used to  obtkin dat&xfor the SDG.
     Only  the  instrument and wavelengths used to  generat^xdata^or the SDG
     must  be included.
     3.4.14.5     Under
     two  decimal  pla<
     established  and  is"
     is used for  ah analyt
     to report  the IDL.
3.4.14.2     Complete  the  heade"
instructions and as follows.

3.4.14.3     For  "DATE," enter  the  date
IDL values were determined  (or became^

3.4.14.4     Enter  the
Number" and "GFAA ID
Numbers are used to/un
uses for CLP analy.
                                                              the header
                                                 .atted MM/DD/YY) on which the
                                                  pr the fields "ICP ID
                                                    maximum each).  These  ID
                                                    rument that  the  laboratory
                                           Wavelength  in nanometers  (to
                              ialyte for which an IDL has been
                             the IDL column.  If more than one wavelength
                             ;her copies of FORM XII-AAIN as appropriate
                        WAVE>\ enter^&h-e/wavelength number for which the
                                 reported on  the  form.  The wavelength number
                                 wavelength  used when  two or  more wavelengths
                                    analyte in  the  SDG.  A wavelength number
                                   est wavelength used  for the analyte in the
                       number bf '/2" is assigned to  the second longest
                                   Id must be left  blank if a  single
                       to obtain7data for an analyte in the SDG.
Julv, 1991
                                                                  Page B-23/IN
-------
Exhibit B
                                                      SOW No. XXX - Ambient Air
     3.4.14.7     Under  "INTEG. TIME,"  enter the integratic
    •to  two decimal places) used for each measurement taken
     instrument.
     3.4.14.8     The Contract Required Quantitation
     Exhibit C  must appear in the column headed "CRC
                 imit
                         Lme (in seconds,
                        from each
              5/L) in
     3.4.14.9     Under "IDL," enter the  IDL  (in ugH^to  three  dec^al
     as  determined by the laboratory for each analyse analyzed by the
     instrument  for which the ID Number is reported/on this form.
     3.4.14.10    Under "M," enter the method/ise/i to  detj
     each wavelength used.
                      iine the IDL for
    3.4.14.11    Use additional copies oft
    and wavelengths are used.   Note that
    exceed  the  analysis dates  in the SDG data"*
    than  three  months.
                    [f more  instruments
                 tb&s  form must not
            ckage <
-------
Exhibit B
                                                     SOW No. XXX  - Ambient  Air
    3.4.15.6     Under  "WAVELENGTH," list the wavelength inxnanometers  (to  two
    decimal places) used for each ICP analyte.   If more  ^nan/one wavelength
    is used, submit additional copies of  FORM XIII-AAIN_

    3.4.15.7     In the "INTERELEMENT CORRECTION FACTO,
    the correction factor  (negative, positive or zer
    places, 10 characters  maximum)  for each  correct,
    ICP.  If an analyte was not corrected for an
    the header of a column, a zero  must be entered t,
    correction was determined to be zero.
     3.4.15.8     Use additional copies of FO!
     correction  factors  for  more  than six ana,

     3.4.15.9     Columns of correction fac
     interelement correction must be  ente
     XIII-AAIN according to  the alphabetic
     starting on the  first FORM XIII-AAIN and'
     XIII-AAIN as appropriate.
     3.4.15.10    Under "Comments," enter alternative
     conditions  under  which  they a
     encountered during  the  intere
     and  administrative,  the
     for  the  sample.
                                                           JR:" column,  enter
                                                              ;n decimal
                                                                 jlyzed by
                                                                         in
                                                  I-AAIN as appropriate if
3.4.16 ICP Linear Ranges (Quarterly)

    3.4.16.11    This form
    for each ICP  instrumevxej(ter the  instrument  ID  number  (twelve
     characters/maximum)  used tb produce the data for the SDG.   If more than
     one I OP instrument is us^d, \3ubmit additional FORMs XIV-AAIN as
     appropriate.

     3.474,6.15"\Under "Integ./TiAe  (SEc.)," enterthe  integration time (in
                 TOodecimal places) used for each measurement taken from  the
     ICP instrument.
 July,  1991
                                                                   Page B-25/IN
-------
Exhibit B
                                                      SOW No.  XXX -  Ambient Air
                                                  concent
                                                     ran
3.4.16.16    Under "Concentration," enter the
is the upper limit of the  ICP  instrument  linear
Exhibit E.  Any measurement  in the SDG package at
concentration is within the  linear range.  Any
out of the linear range, and thus,  is an  estimat
diluted into the linear range.
    3.4.16.17    Under "M," enter "NR" for analyts
    than  ICP.  No  entries  are  required under "VL"/f.ol
    ICP.   If more  instruments  or analyte wavelengths  are used,  submit
    additional FORMS  XIV-AAIN  as appropriate.
             »n  (in Mg/L)  that
            .s determined in
         bje'low this
             it above it is
                 must be
3.4.17 Preparation Log [FORM XV - AAIN]

    3.4.17.1     This form is used to rep
    analyses  only.   In addition,  the sample
    been prepared  in the  same  manner using no
    concentration  steps.   The  results reported on
    listed on this  form  for  each  analyte must be
    analyte's  concentration (in
    factor  (DF)  listed on the  foi
                                              ampae Analysis log for ICP
                                                   n this  form  must  have
                                                           dilution or
                                                   I-ltA^N  for the samples
                                             obtained by multiplying each
                                     2m the instrument
              le dilution
    3.4.17.2     All field samples and a\l quality xroattol^reparations
    (including duplicates,  spikes,  LCSay be/submitted on this  form.

    3.4.17.3     Submit oneXFORtTx^-AAIN perNnetftod if no more than 32
    preparations including  quality  opntrol  preparations  were performed.
    more  than 32 preparations  perMnethod^were performed,  then submit
    additional copies  pf £ORM  XV-AJAIN as  ap>roprD4te.
                                                                      In
     3.4.17.4     Comp
     instructions  a
                                 informe
according to the header
3.4.17.5     For  "Analyte,"  eiijter the  name  of the  analyte as  identified in
the Target Analyte Liststn,Exhibit C.

                                      enter the  instrument ID number (12
                            s the  identifier  that distinguishes each
                         sis\ in  the SDG.   If more than one instrument  is
                               of FORM XV-AAIN as appropriate.

                               enter the  date (formatted MM/DD/YY)  on
                               rted.
     3 .4-m . 7\For "Start Dat
     whicn^&he  analsis  run was

     3.4.17.8
     the  analysis  run^xas  endec
                             enter the date (formatted MM/DD/YY) on which
July, 1991
                                                              Page B-26/IN
-------
Exhibit B
                                                 SOW No. XXX - Ambient Air
     3.4.17.9     For "Run No.," enter the run number  (two  characters  maximum)
     which  is  the. number that applies to a continuous analytical sequence
     consisting of prepared samples and all associated qyal:Lcy assurance
     measurements as required by the contract.

     3.4.17.10   Under  "EPA SAMPLE NUMBER," enter  the/EPA  salable  number of
     each sample in the SDG and of all other prepara/ioi*s>^suchSsas duplicates,
     spikes,  LCSs,  PBs, and repreparations (all for/nat/ed acbarding^^o Table 1
     of this  exhibit) .   All EPA Sample Numbers mus<£ b6 listed
     alphanumeric order, continuing to the next FDRJ^XIII-AAIN if
     If a sample was reprepared, list the same ^PA/sample number in
     of increasing preparation date.
     3.4.17.11   Under "PREP. DATE," enter jfaeAate  (fc
     which each sample was prepared for anadys^/s by tty;
     the  header section of the form.
                                                   •matted MM/DD/YY) on
                                                   method indicated in
     3.4.17.12   Under "Final Volume," enter^fche  finaVvolume  (in mL,  to the
     nearest whole number)  of the preparation for^each sample prepared for
     analysis by the method indicated in the headers«etiorNo_f the form.  This
     field must have a value for each sample listed.
     3.4.17.13   Under "Time," en^er £he^ time  (TrT
     which each analysis  was perforhted\
                                                       format - HHMM) at
3.4.17.14    Under "DF,"  enter  the\di^ti/n
by which the final product of
to be diluted for each analysis performed/
                                                 Factor  (to  two  decimal places)
                                                 iistillate or digest)  needed
     NOTE:   A DF of "1" mus't be enbered if tfte preparation product was
     analyzed without adjaing/ariy-^further volume. ofNlilutant or any other
     solutions to the s/amp^e or ai\ ati^u&t^pf th\t/sample taken for
     preparation.
     NOTE:   For EPA /supplied solutions such>»/ICVs,  ICSs,  and LCSs, a DF must
     be entered if cbe sup>^e7 solution was used at a dilution different from
     that specified by^the instructions provided with the solution.  The DF
     reported in such a ca&e muscxbe that which would make the reported true
     values on the_app_rppriat^xJprni'gor the solution equal those that were
     supplied w^rththeso^ut ion Byx^theeeA.  For instance,  if the  ICV has a
                               for alrumirium at a 20 fold dilution,  and if the
                                  fold dilution, a DF of "2" must  be entered
               •AAIN and the\uncrrected instrument reading is compared to a
                                  this example, FORM III-AAIN will have a true
              2500.0 regardles^ oij the dilution used.  The found value for the
                                   dilution listed on FORM XV-AAIN using  the
     Found value
                             =  Instrument  readout in Mg/L x DF  Eq.  B/IN-16
 July,  1991
                                                               Page  B-27/IN
-------
Exhibit B
                                                      SOW No. XXX - Ambient Air
     3.4.17.15    Under "%R," enter the percent  recovery  (tzb
    'places)  for  each analytical spike analyzed.  Leave the
     analysis  reported is  not: an analytical spike.

3.4.18 Analysis Run Log [FORM XVI - AAIN]

     3.4.18.1     This form is used to report  the  s
     each instrument  used  for analyses in the SDG
     run where  conditions  for reporting on FORM
    XVI-AAIN  is  analyte and  method  specific.

     3.4.18.2     A run is  defined as the tot
     instrument throughout the  sequence ini
     SOW-required calibration standard and
    continuing calibration verification a
    SOW-required field sample.
                                                                 decimal
                                                                  blank if the
                                                         analysis\run
                                                      is includes a
                                                     AAIN were not
                                                            's  performed by an
                                                            iduding, the first
                                                           .nd including, the
                                                         es following the  last
    3.4.18.3     All field samples and all quality"eontrol^reparations
    (including  calibration standards,  ICVs,  CCVs,  ICBsXeCBs>ICSs,  LRSs,
    LCSs, PBs,  duplicates,  pre-digesrtitument ^D Number," enter the instrument ID number
    (twelve characters maximum)  whb>h is the identifier that distinguishes
    each  instrumerrt~~uIeTi-^or  ana^sis to the SDG.   If more than one
    instrumen^/isjj.sed_^suDlliit  addibiojia/ copies of FORM XIV-AAIN as
    appropri^

                                 '\ enter  the date (formatted MM/DD/YY) on
                                  rted.
                                   ter the date  (formatted MM/DD/YY) on which
                                enter the run number  (two characters maximum)
                               pplies to a continuous analytical sequence
    3 .4.1 £
    the analys^ runN^as

    3.4.18.10    For"
    which is the number^
July, 199L
                                                                   Page  B-28/IN
-------
Exhibit B
                                                 SOW No. XXX  - Ambient  Air
    consisting  of prepared samples and all associated qualij
    measurements  as  required by the contract.
                                                           assurance
     3.4.18.11   ..Under "EPA SAMPLE NO.," enter  the EPA  s4mp*e  number,
     including  the  QC  suffix of .each sample (formatted .acccqrding to Table
     B/IN-1  of  this Exhibit).   All EPA sample numbers .must beXListed in
     increasing temporal  (date and time) order of analysl^xcontlnuing to the
     next  FORM  XVI-AAIN for  the instrument run if applLcable^-xThe analysis
     date  and time  of  other  analyses not associated^ wyth the SD(jbut ana-lyzed
     by  the  instrument in the  reported analytical/rwr must be report
     analyses must  be  identified with the EPA Sample'No. of "ZZZZZ"
     3.4.18.12    Under "PREP. DATE," enter thef da€e  (foi
     which  each  sample was  prepared for analysis/by the
     the header  section of  the form.
                                                       ited MM/DD/YY) on
                                                    ietbiod indicated in
     3.4.18.13    Under "VOLUME," enter
     whole  number)  of the  preparation for eacfN^ample
     the method indicated  in the header section orSsfhe
     have a value  for each field listed.
                                                    /(in mL, to the nearest
                                                   repared for analysis by
                                                          This field must
3.4.18.14   Under  "TIME,"  ente.rt
which each analysis was perforated
analysis time and intervals betvee
the run (the time of analysis of \the
later) needs to be reported.
                                         ana
                         (in military Ifo^at - HH:MM) at
                       an autcysafflplferis  used with equal
                              then only?the start time of
                            CV/~or~t56B>/whichever is
                                           inal
     3.4.18.15    Under "DF," enter the dilution/ factor  (to  three  decimal
     places)  by which the  finai-pLroduct of tfc^e preparation procedure
     (digestate or distillate)  can be analyzeOvwichin the instrument standard
     range.   The DF does dot irortude Vhe dilution inherent in the preparation
     as  specified by thereparation  Jnr6~c>dures it} /Exhibit D.
     NOTE:   A "1"  mus
     without adding
     the "Volume"  or
     that sample.
 be/entered /if
ty further
in al:
                                         aratzion product was analyzed
                                   of  diltreAnt  or any other solutions to
                                   "Volume"  listed on FORM XVI-AAIN for
     NOTE:   For EPA
     be entered
     that
     reporte
     values /on
     supplied
     true/val&e of 2500
     sol
     on FO:
     true value"
     value of 2500?
                   )lied  sc
                       aed
                  sut
        /in/such a cas« mus"
        m .the appropriate,  f
        Lywith the solutions 1
        .4e  of 2500.0 Mg/L  fr
        t isxprepared at a  41
        -XV-AAlm. and the uric
                       as  ICVs,  ICSs,  and LCSs,  a DF must
               tionyas used at  a dilution different from
          rucciohs-provided with the  solution.  The DF
             be  that  which would make the reported true
               for  the  solution  equal those that were
              the EPA.   For instance,  if the ICV has a
              aluminum  at  a 20  fold dilution, and if the
              old dilution, a DF of "2" must be entered
              ected instrument  reading is compared to a
             this example, FORM  II-AAIN will have a true
          'of. the dilution used.  The found value for the
 July,  1991
                                                               Page B-29/IN
-------
Exhibit B
                                                      SOW No.  XXX -  Ambient Air
                                                              ^AAIN using the
                                                              x DF  Eq.  B/IN-17
                                                      eipt and
                                                      RM AADC-IN-1 is
     ICV must be  corrected for  the  dilution listed on FORM
    •following  formula:

     Found value .on  FORM  II-AAIN  -  Instrument readout

3.4.19 Sample Log-In Sheet [FORM AADC - IN  -  1]

     3.4.19.1     This form is used to document th
     shipping containers  and  samples.  One original
     for each shipping container.

     3.4.19.2     If the  samples in a single shipping confc4itter must be
     assigned to  more than one  SDG,  then the/original FORM ^ADC-IN-1 shall be
     placed with  the deliverables for  the  SDG o£  the lowes/ alphanumeric
     number and a copy of FORM  AADC-IN-1 rnu^t be^pjacea w/th the deliverables
     for the other SDG(s) .  The copies shouloNbe  id^tifiied as "copy(ies),"
     and the location of  the  original  should be netted onxthe copies.

     3.4.19.3     Sign and date  the  airbill  (if present^x^Exalfrine the shipping
     container and record the presenoe/absence of custody sfeals/and their
     condition  (i.e., intact, broker*;  in item~1r-eaJ[pRM AADC-TO-l.   Record the
     custody seal numbers  in  item 2\
    3.4.19.4     Open the shipping confcainVr, rgmoye the
    documentation, and  record  on  FORM  AADC-
    presence/absence  of chain-of-custody \ecordi
    Packing Lists), and airbills  or  airbil
    airbill or  an airbill  s£±ck~e~r^present
    Record the  airbill  or/sticker number in   tfem
                                                         enclosed sample
                                                   terns  3 - 5 ,  the
                                                fs) ,  SMO forms (i.e.,  TRs,
                                                        Specify if there is an
                                                   5  on  FORM AADC-IN-1.
.stickers.
    3.4.19.5     Remove/the/samples] ffom tfiex§hippVng container(s) , examine
    the samples  and  the  ss&nple  tag' (if-fH^sentT-rrand record the condition of
    the sample bottles  (.i.e.,  intact/broketv^le4king) ,  and the presence or
    absence of sampjte  tags^ in  iyems/7  and 8 on FORM AADC-IN-1.

    3.4.19.6     Review th«sampl^' shipping documents and complete the header
    information.   Compare  tnexinfo^nsation recorded on all the documents and
    samples,  and^e-rrrte--<£ie appr^priatie-^answer in item 9 on FORM AADC-IN-1.
     3.4.19.7
     date  (irrcl
     and wr
     enter
     meters
     sample
     date  shou
     time  of
     and 11.   Cross
                                 problem^ observed during receipt,  sign  and
                                  -IN-1,  the chain-of-custody record, the TR,
                                   n FORM AADC-IN-1.   For each sample number
                                    g air volume sampled in standard cubic
                                    iate  column.  Record the appropriate
                                   atory  numbers if applicable.  The log-in
                                  re top of FORM AADC-IN-1,  and the date and
                               thfe laboratory should be recorded in items 10
                                olumns and spaces.
July, 1991
                                                                   Page B-30/IN
-------
Exhibit B
    SOW No. XXX  - Ambient  Air
    3.4.19.8     If there are problems observed during receipt  (e.g.,  data on
    'air volume  sampled is missing for one or more samples/oy if an answer
    marked  with an asterisk (i.e.,  "absent*") was circle/,  Chen contact SMO
    and document the  resolution of the problem on a CLP/Communication Log.
    Following resolution, sign and date the forms as specified in the
    preceding paragraph and note,  where appropriate, /the resolution of the
    problem.
     3.4.19.9     For "Sample Transfer," enter the
     appropriate)  and the specific area designati
     number)  in  the  Sample Transfer block locataa id the bottom left co
     FORM AADC-IN-1.   Sign and date the sample /transfer block.
  ra/tion desigrvation^
    e.g.,  refrigera"6or
3.4.20 Document Inventory Sheet  [FORM AADC  /IN/- 2]
     3.4.20.1     This form is used to recc
     Sample  Delivery Group Case  file  (CSFr
     Region.
inve^ito
 :s /which
of  the  Complete
are sent to the
     3.4.20.2     Organize all EPA-CSF documents as otfescribe^in Exhibit B.
     Assemble  the  documents  in the order specified on FORM AADC>IN-2 and
     Exhibit B,  and stamp each page/with—6he__consecutive nujftbe/s (Do not
     number the  DC-IN-2  form).   Inventory the CS"F~"by-~teviewing the document
     numbers and recording page numoer ^ange^-~in the  columrHprovided on FORM
     AADC-IN-2.  If there are no docu^encs^ for / sp€cTf-te-^dx>cument type,  enter
     "NA"  in the empty space.
July,  1991
                  Page  B-31/IN
-------
               U. S. ENVIRONMENTAL PROTECTION AGENCY
                        CONTRACT LABORATORY PROGRAM
                                Inorganics in Ambient Air

                                   COVER PAGE
                   ICP interelement corrections a
                   ICP Background corre/tio
                   If tfes, wehs^raw data generated before
                                                                    N" for No
                   applii
Comments:
                                          z
                     certi
                    conditions of
                    the conditions
                                   by
 ckage is in compliance with the terms and
 t, both technically and for completeness, excluding
 foove.  Release of the data contained in this
 md in the computer-readable data submitted on floppy
nzed by the Laboratory Manager or the Manager's
 the following signature.
            Signature:
            Date:
              Name:

              Title:
-------
        U. S. ENVIRONMENTAL PROTECTION AGENCY
              CONTRACT LABORATORY PROGRAMS   EPA SAMPLE NO.
Lab Name:
Lab Code:
Case No.:
SAS No.:
SDG No.:
Inorganics in Ambient Air / /
ANALYSIS DATA SHEET / /
Contract: / /v^ ^\
Lab Sample ID: / / ^\^ ^\
Date Received: ^\/ ^\^ ^\^
Air Volume Sampled/Std. m 3: ^^\ /
Date Analyzed/ /
Comments:
                                     77

CAS NO.
7429-90-5
7440-36-0
7440-38-2
7440-39-3
7440-41-7
7440-43-9
7440-70-2
7440-47-3
7440-48-4
7440-50-8
7439-89-6
7439-92- 1
7439-95-4
7439-96-5 /
7439-97-6 /
7440-02-0 ^
7440-09-7
7882-49-2

74/0-23^-5 	
/440/18-0
744/5-31-5
7^*40-62-2
744^6-6

ANALYTE
Aluminum •
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium
Chromium
Cobalt
CoppeX^ ^^
Iroa/ ,* — ^^
L^d / N
>lagp(esium
Manganese /
MoSjcb^denum/
•Njckel\y /
Potassium x.
Selenium ^\^
SilveYv^ >Xi
Sodium x^
Thallium^ \
Tin \ \
Vanadium \ '
Zinc I \
COM6E^
Mg/L\


/ 	 __
( ~
\ \^—
\ \
\ \ ,
\ N/
\

X \
\
} ^~^
^f ~.:+^_
/ \^
/


^\
X^ ^
\y




CATION/ /
1%/m/
"X^ \
"\^
^
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                        FORM I - AAIN
7/91
-------
           U. S. ENVIRONMENTAL PROTECTION AGENCY
                    CONTRACT LABORATORY PROGRAM
                         Inorganics in Ambient Air
Lab Name:
Lab Code: _
Case No.:
SAS No.: _
SDG No.:
           INITIAL AND CONTINUING CALIBRATION
Contract:
SOW No.:
                     TION
Initial Calibration-source:
Continuing C/libraiion Source:
Concentration l/nits:  /*g/L
7
ANALYTE
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Molybdenum
Nickel
W
A
V
E














A

Potassium *~
Selenium _] 	
Silver X
Sodium / /
Thalliqm /
Tin/ /

-^


VajiadiuQi
Zrite^ \)
INITIAL CALIBRATION
(ICV)
True









S
/ .
/ /
/ /
/ /
x^
\^
\
	 ^
"\
~~^-\^
\,



Found


/
<
\




X
^ — X
^
/
/
/ /
^ /

^\
\
X
N \
\ \
)
/
%R


— —

s \
\
\



\
\s"-
. — .
/



\^

^V




/ V CON-plNU^G CALIBRATION (CCV)
^•SQVNfrsV /
True\


~- — __
— ^
•"• 	 ,
\ /
\/
\ ^ /
\ \
\
\
\
^-_
^-^_/




?





^ Foun^
"X^
\

•— 	 ^

/ ^
/


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^
V












%R
X^

x^

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CCV No.:
True

X
:/





















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Comments:
                             /
                                   FORM II - AAIN
                                          7-91
-------
           U. S. ENVIRONMENTAL PROTECTION AGENCY
                   CONTRACT LABORATORY PROGRAM/
                       Inorganics in Ambient Air
               CRQL STANDARDS / LINEAR RANGE STANDARDS
Lab Name:
Lab Code:_
Case No.:_
CRQL:
Contract:
SASNo.:  / /
  ICP Source:
  GFAA Source:
                          Concentration U
ANALYTE
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Molybdenum
Nickel
Potassium
Selenium /
Silver /
Sodium / x
Thallium / /
Tin / 
-------
             U. S. ENVIRONMENTAL PROTECTION AGENCY
                    CONTRACT LABORATORY PROGRAM       EPA SAMPLE NO.
                          Inorganics in Ambient Air
                             DUPLICATES
Lab Name:_
Lab Code:
Case No.: _
SOW No.:_
Sample
Percent:
Contract:
SAS No.:
  J_L
SDGNo.:
z
Concentration Units:  /g/L
Duplicate     ^/
Percent:
ANALYTE
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Molybdenum
Nickel
Potassium
Selenium
Silver ^~~~
Sodium / ^.
Thalliun/ /
Tin / /
Vanadiujn
Z«4 ^\
W
A
V
E














/
/
1







CONTROL
LIMIT










^~
/ x 	
/ /
' /

^\ /
x^ \y
\^
--^ "x
"\
"\ \
\

)
SAMPLE /
(S) / /
Cone. /
^



f— — ^^
( ^. 	 	
\ \ '
\ \
\ \
\
-^ \
, \
\ V- — \
I ^
/ / ^
' /
/
'\^
^ \^
\^ /
^"^
\
\

F
\
\




• — — .
/
/
/ /
(
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\
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"^ —
> /









/ DUPLICATE
/D)/
Cclhc./
^ / /
~ /
\^ ^\
"v. \
\
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/^_ /
/ ^
/

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 Comments:
                                FORM VIII - AAIN
                                        7/91
-------
 Lab Name:
 Lab Code:
 Case No.: _
 SOW No.:
U. S. ENVIRONMENTAL PROTECTION AGENCY
       CONTRACT LABORATORY PROGRAM
            Inorganics in Ambient Air
                  BLANKS
                        Contract:
                        SAS No.: /_
                        SDG
ANALYTE
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Molybdenum
Nickel
Potassium
Selenium
Silver /
Sodium /
Thallium / /
Tin / /
Vanadiun/ C^
Zinc ^\^
W
A
V
E


















S"
X



\
INITIAL CALIB.
BLANK
(ICB)
Cone.










/
/ /
/ /
/ /
/ c

""\

"~"\
" ^\
\



c









— — ~^

' ^


/
„/
i.
\

\
i \
N

/
CONTINUING C/UBRATIONBLANK
/ fcCB) / /
Cone. 1



, 	
/
\ V
\
\


X
s

\ -
\
7 s —
/
/

\\
-\ ^
\/

\

I



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^



• —
~~— -
\
\
\
\


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\




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boQC. 2
^ ^^
^\
^N

^~— ^
1 	 .
/ r
/ /
' /
\
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/
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BLANK
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Comments:
                             FORM IV - AAIN
                                                       7/91
-------
          U. S. ENVIRONMENTAL PROTECTION AGENCY
                 CONTRACT LABORATORY PROGRAM
                     Inorganics in Ambient Air
                 ICP INTERFERENCE CHECK
,ab Name:
.ab Code:
!ase No.:
OW No.:
CP ID No.:



Contract:
SAS No.:
SDG No.:/
/ /
/ \
' /X. \^
ICS Sou/ce:/ ^\ ^x^


ANALYTE
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Molybdenum
Nickel
Potassium
Selenium
Silver /^
Sodium / /
Thallium / /
Tin / /
Vanadium' \^
^inc "\ \
W
A
V
E














jj


TRUE
Sol.
A










/
/
/ /
/ /
/ /
^x ^
\^
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-^"~



X
^x
-\
\



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AB




/
\



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)
/
/ ,
•x/ /
^
"\^ ^
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X
\ \
\ \



1 /
Conc/ntrMii
^\ ^x.
Dn Units: iig/L x. /
^xy
INITIAj/FQUND /
Sol. /
A/
x


^__


\ \
\ \
\
\


"x
/ \



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xy




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Comments:
                   X/
                   x/
                          FORM V - AAIN
7/91
-------
Lab Name:
Lab Code:
Case No.:
SOW No.:
               U. S. ENVIRONMENTAL PROTECTION AGENCY
                      CONTRACT LABORATORY PROGRAM    EPA SAMPLE NO.
                            Inorganics in Ambient Air
                          SPIKE SAMPLE RECOVERY
            Contract:
            SAS No.:
            SDG No.: /  /
            Percent: //
Concentration Unite:
                                                                T
ANALYTE
Aluminum
Antimonv
Arsenic
Barium
Beryllium
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Molybdenum
Nickel
Potassium
Selenium
Silver
Sodium
Thallium /
Tin /
Vanadium / '
Zinc ^\
W
A
V
E


















X
/
/
/
\

CONTROL
LIMIT
%R












/
/
/ '
\

-
/f^r
/" ~~



"Xr
SPIKED SAMPLE
RESULT
(SSR)
Cone.



/—<
/
\



^ — .
s ^\
/ /~^\ s
/
/ /
/ /
\/ /
\ <
\. ^x
"^\ "\
\ X
N \
\ \
)
/ /
c





X
\
s




I'
f~



"X^
'
\




SAMPLED
RKUIT
/Corfe>^
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\


— — __
^^-^_
\ 7 J
^ \ / /
\ v /
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\ \
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\ v
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y^DbED
/ (SA)
/6onc.
/
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— -7
-^/

















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Comments:
                                FORM VI - AAIN
                                                                        7/91
-------
Lab Name:
Lab Code:
Case No.:
SOW No.:
               U. S. ENVIRONMENTAL PROTECTION AGENCY
                       CONTRACT LABORATORY PROGRAM    EPA SAMPLE NO.
                             Inorganics in Ambient Air
                     ANALYTICAL SPIKE SAMPLE RECOA
Contract:
SAS No.:
SDG No.:  /
Percent:
                           Concentration Units:
ANALYTE
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Molybdenum
Nickel
Potassium
Selenium
Silver
Sodium
Thallium t
Tin /
Vanadium /
Zinc ^ '
W
A
V
E



















/
/
/
/
fX
CONTROL
LIMIT
%R












/
/
/
/ ^
^\
-
^ 	 ^

/^ ^



SPIKED SAMPLE
RESULT
(SSR)
Cone.




r
(
\



s" — \
/ ^ \
c




—
^_^
\
\
\



' / ~\ L-
/ ;
/ / /
\ / /
"v/ /
\ V
^\^^ "x.
"\ \
\ \
X \
\ \
) )

"



x

\y



SAMPLE/
RESULT
/(Sw
/Coj/c.
^ \
\ ^
^X

•^ B|
— —
^—-7
\ / /
V \/ /
\ /
\ \
\ \
^ \ /
"NS^. ^
^\ /
^^~/



7




c
/
y

^>s

- — .


















SPIKE
AQDED
/ (£A)
/ jdonc.
/
/
\^
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7
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Comments:
                           z
                                 FORM VII - AAIN
                                    7'01
-------
tab Name:
.Lab Code:
Case No.:
Sample
Percent
                      U.S. ENVIRONMENTAL PROTECTION AGENCY
                            CONTRACT LABORATORY PROGRAM
                                  Inorganics in Ambient Air
                                     DUPLICATES
                     EPA Sample No.
                       Concentration Units: ug/L
Contract:
SAS No.:
SOG No.:
SOWN
Dupl
Pen
                                  FORM VIII - AAIN
                                  7/9.
-------
           U. S. ENVIRONMENTAL PROTECTION AGENCY
                   CONTRACT LABORATORY PROGRAM
                         Inorganics in Ambient Air
                  LABORATORY CONTROL SAMPLE
Lab Name:
Lab Code:
Case No.:
SOW No.:
/  /
GFAA Source:
 Units:  pg/L
ANALYTE
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Molybdenum /
Nickel <
Potassium
Selenium
Silver ^ 	
Sodium/^ 	
Thall/um /
TV /
^nadrum
£incx^
LCS
USED









^- —
/
/ S
/ /
/ /
* /
k ^"X
^x^ >v/
X^

_ X^
"^-\ N
X
\

w
A
V
E









— ^

X


/
^
/
"
X,

N
\


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LOWER



/ "" —
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\ \
\ x
\
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\
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s — ^
/
/

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x^ /
^^



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x.


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-— _
7
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V /
\ /
\ \
\ N
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. "7
\^y









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/



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s^
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xy

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 Comments:
                               FORM IX - AAIN
                            7/91
-------
U. S. ENVIRONMENTAL PROTECTION AGENCY
       CONTRACT LABORATORY PROGRAM
          Inorganics in Ambient Air
    STANDARD ADDITION RESULTS     /\








1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
Lab Name:
Lab Code:
Case No.:
SOW No.:


EPA
SAMPLE
NO.






















/
/
/ /
' / /
. V
x^
"••,









An






















^--
f
/


\~

X









M



















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—





\

^








ZERO
Found













*
/
/ /
/ /
/ /
X^
x^
X
— \
^->
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x^
^ ^
x^







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Added








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	 	 \
^ 	 ^
\
j
/
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A D
RST
Found



*



r- — -—
^^__
\ \
\ v
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^

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X /









Contract:
SAS No.:
SDG No.:
Concentra

D I
f
Added
/ ,
/ /
/ /
^ X
X^


•— —
— -,
^^-7
^ /
v /
s /
\ \
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/
tion/UnitsT'
/ /
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i

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^ / /
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,. 	 	
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Added
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                FORM X - AAIN
'•91
-------
U. S. ENVIRONMENTAL PROTECTION AGENCY
      CONTRACT LABORATORY PROGRAM^
           Inorganics in Ambient Air    /  /
Lab Name:
Lab Code:
Case No.:
SOW No.:
Date:
METHOD DETECTION LIMIT / /
Contract: / ^\





SAS No.: / /X^ \\
SDG No.: / / ^\ \^
ICP ID NlTKlbB/
GFAA ID Number:
\ \
\7

Concentration Units: /g/L/ ..
(
Comments
ANALYTE
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium
Chromium
Cobalt ^
Copper /
Iron / /
Lead / /
Magnesium / /
Manganese / £
Molybdenum^ ^\
Nickel . "X^
Potassium ^x.
Selenium— 	 \^
Silv^ 	 "X
Sodium/" ^\
/hal/urn X
TV
V^Qadium
Zinc"\^
WAVE-
LENGTH
(nm)


/
\
\



	 ^^
X
^x \
] '
1
/ /
/ /
^ /
\^
"\^
\
X
. \
\ \

/ /
w
A
V
E


-— —
V—~
\
\ V
\
\




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7
^y




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^\^
^
• 	 ~__

~~7 /~-~—
V / /
\/ /
X /
\ \
\ \
\ )
""X ^
""-7
^\-^y










/ CRQL
'X226
\ 9^>
^X>/
	 ^11
/ 7
~^ 18
381
44
55
37 .
126
118
89
15
33
52
758
577
229
592
562
155
26
444
MDL
























M
























^\\//
-'

\/
— '
                FORM X] - AAIN
7/9!
-------
Lab Name:

Lab Code:

Case No.:

SOW No.:
ICP ID No.:
 U. S. ENVIRONMENTAL PROTECTION AGENCY
        CONTRACT LABORATORY PROGRAM
            Inorganics in Ambient Air        /\
 ICP INTERELEMENT CORRECTION FACTORSXAIWUAL)
	.	   Contract:	/  /	
                      SAS No.:     / ^  ^\
                      SDG No.:_
                      Date:
ANALYTE
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead /
Magnesium /
Manganese / /
Molybdenum / /
Nickel / x^
Potabsium ^\
Selenium - ^\
Silver 	
Sodium// ^^
Thallium /^ ~~^\
T,a/ /
Vanad/um
femc^ •
WAVE-
LENGTH
(nm)




r

\



^, 	 ^
\
S.^\

/
/ /
\/ /
, <,
"^x^^ \
\ ^\
x
\ \
\ \

INTXREj^EMENT GQ^JIECTION FACTORS FOR:
/
/ ,
<



	 __
• — .
v— -
\ \
\ \/
\ "
. \
\
	 ^
\^
f — \^
^~N


\
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s ^ /
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/
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 Comments:
                              FORM XU - AAIN
                                                         7-91
-------
U.S. ENVIRONMENTAL PROTECTION AGENCY
      CONTRACT LABORATORY PROGRAM
            Inorganics in Ambient Air     /\
           ANALYSIS RUN LOG (A)
Lab Name:
Lab Code:
Case No.:
SOW No.:
Start Date:
Contract:
SDG No.:
SAS No.:
Run No.:
Method:
//
/ <\
/ A\ \

/x7 ^x. x^^
EndDate: Instrument/D vLh*r- \/
ate:
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
Instrument/ID Number- ^x/
EPA
SAMPLE
NO.



















-
/
/
/ /
/ /
/ /
x. ^X
x^
x




PREP.
DATE













/
/
/ /
/ ^
^x



^- ^




x^
^ "x^
x^
X


TIME











/^
f s 	
/
/

v^
x^/
\
x^
~x^
X,
X, N
\
\
1
/
/
x^y /
/
^^

D/F




f
/
\




^x
•x^
\
/
/
/ /
/
C_
x
x^


\




/





/ / A^A^YTES
A
L




**— •


\





^

/



X

•x










S
B




--

\

S












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A
S







\

\



-x

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^











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\

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B
E






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t

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/

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c
A
X

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C
R


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C
0
/


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X

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               FORM Xlll - AAIN
                                                  7/91
-------
U. S. ENVIRONMENTAL PROTECTION AGENCY
      CONTRACT LABORATORY PROGRAM
          Inorganics in Ambient Air
          ANALYSIS RUN LOG (B)     /X
Lab Name
Lab Code:
Case No.:
SOW No.:
Run No.:
Start Date
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
: Contract: / /
SASNo.: / /
SDG No.: / X^
Analyte: / / ^v^ ^\^
Instrument ID No^ / ^\^ ^X^
End Date: /X^ ^\ X^
/ / xy
EPA
SAMPLE
NO.
PREP.
DATE
1

|












/
/
c



/"
/ /^ ^
/ /
/ /
/ c
x^ x^
x^ x^.
x^
\,




j
(
FINAL
VOLUME
(mL) /
/
\



f — • — -^
^ 	
\ \ ^



^ 	 _^
r /^ x
/ / x,
/ / )
' / )

^x / /
x.- ^x»/ /
\. /
"x X
^ x^
^x ^
~~x^ X
X \
\ \

I I
/ /
^x / /
^ ^ /
x^ /

\ \
\ \
\
\

\
^^~^X
s — ^
I/ ^



x^
•\ ">
^-/









//,
\^
^ Xy
x^
X.


^~ — — ~
•^^
/ /
/ /
/
\
\ \
\ ^
\/
^-—7
^_/















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/ /
/
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x^
X^ X,
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               FORM XIV - AAIN
                                                   7'91
-------
                                    SAMPLE LOG-IN SHEET
Lab Name:
                                                             Page:
                                                                                of
Received By (Print Name):
Received by (Signature):
Case Number:
Sample Delivery
Group No.:

SAS Number:
 CIRCLE THE APPROPRIATE
 RESPONSE:
 1.  Custody Seal(s)
 2. Custody Seal Nos.:

 3. Chain-of-Custody
   Records
 4. Traffic Reports or
   Packing List
 5. Airbill

 6. Airbill No..
                        Present/Absent*
                        Intact/Broken
                        Present/Absent*

                        Present/Absent*

                        Airbill/Sticker
                        Present/Absent*
 7. Sample Tags
   Sample Tag
   Numbers
 8. Sample Condition:
                        Present/Ab,
                        Listed/N
                        on Ch*m-ofyCustody
                        Inta/rt/B
                        L
9. Does information on custody records
  traffic reports, an sample tags
  agree.
10. Date Received at Lab
11 Time Received.
                                               EPA
                                             SAMPLE
                                                #
L
       \
               ~TT
\TT
                                                        \\
                        ASSIGNED
                           LAB
                              7
                                      REMARKS:
                                    ^CONDITION
                                     OFSAMPLE
                                    ^SHIPMENT
                                          ETC.
    *If Circled, contact SMO and attach recorttsQf/resolution
    Reviewed by
    Date:
                                                       Logbook No.:
                                                       Logbook Page No.
-------
Lab Name:
 U.S. ENVIRONMENTAL PROTECTION AGENCY
        CONTRACT LABORATORY PROGRAM
              Inorganics in Ambient Air
             COMPLETE SDG FILE (CSF)
          DOCUMENT INVENTORY SHEET

	City/State:
Case No.:
                             SDG Nos. to Fol)6w:
SAS No.:
                             SOW No.:
/
SDG No.:
                                                 IFBNo.:
                                        //
Contract No.:
                                      /  /
All documents delivered in the complete SDG file must be original d«
(Reference Exhibit B)
                                        tents where possible.

                                                 ase Check:)

                                               ,ab     Region
 1. Sample Log-In Sheet (DC-1)
 2. Inventory Sheet (DC-2) (Do not number)
 3. Cover Page-AAIN
 4. Analysis Data Sheet (FORM I-AAIN)
 5. Initial & Continuing Calibration
     Verification (FORM II-AAIN)
 6. CRQL Standards/Linear Range Standards
     (FORM III-AAIN)
 7. Blanks (FORM IV-AAIN)
 8. ICP Interference Check Sample (FORM V-AAIN)
 9. Spike Sample Recovery (FORM VI-AAIN)
10. Analytical Spike Sample Recovery
11. Duplicates (FORM VIII-AAIN)
12. Laboratory Control Sample/Metf/od Referenc
     Sample (FORM IX-AAIN)
13. Instrument Detection Limit (F/
14. ICP Interelement Correctio
     (Annual)(FORM XI-AAIN)
15. Method of Standard Additions
16. Analysis Run Log (A) (FORM XIM-AAl
17. Analysis Run Log (B)(£0RTvnov>-AAIN)
18. Inductively CouplepvPlasma-Baw Dat
19. Graphite FurnaceAtopnlc Absorption. Ra
20. EPA Shipping/ReceiX/ing Documents
      Airbill (No/of Shipments	
      Chain-oif^Cus^Qdy Records
      Sample
                   Data
                  J
                                   FORM AADC - 2 (Page 1 of 2)
                                                                       3/91
-------
Lab Name:
                U.S. ENVIRONMENTAL PROTECTION AGENCY
                       CONTRACT LABORATORY PROGRAM
                              Inorganics in Ambient Air
                            COMPLETE SDG FILE (CSF)
                          DOCUMENT INVENTORY SHEET

                   .	City/State:
Case No.:
                                             SDG Nos. to Follow:
SASNo.:
                                             SOW No.:
SDG No.:
                                                 IFB No.:
Contract No.:
All documents delivered in the complete SDG file must be original
(Reference Exhibit B)
21.
Misc. Shipping/Receiving Records
   (list all individual records)
   Telephone Logs
Comments:
22.  Internal Lab Sample Transfer Records &
      Tracking Sheets (describe or list)
23.  Internal Orginial Sample Preparation & Analysis Reo
      (describe or list)
      Preparation Records	
      Analysis Records	
      Description	Z
24.  Other Records (described or list)
      Telephone Communication.Log
                   (Signature)
                                       (Print Name & Title)
Date
                                   FORM AADC - 2 (Page 2 of 2)
                                                                                        3/91
-------
-------
Exhibit C
                     SOW No. XXX - Ambient Air
                                    TABLE 1

                           VOLATILES IN AMBIENT AIR
                        TARGET COMPOUND LIST (TCL) AND
                 CONTRACT REQUIRED QUANTITATION LIMITS
Target Compound

Vinyl chloride
Trichloroethylene
Chloroform
Benzene
Carbon tetrachloride
Tetrachloroethylene
1,1-Dichloroethene
Acrylonitrile
1,2-Dichloroethane
Chlorobenzene
1,1,1-Trichloroethane
1,1,2-Trichloroethane
1,1,2,2-Tetrachloroethane
Ethylbenzene
Methylene chloride
1,2,4-Trichlorobenzene
Styrene
1,1-Dichloroethane
Toluene
Xylenes, m- and p-
Xylene, o-
1,2-Dichloropropane
1,2-Dichlorobenzene,
1, 2-Dibromoethane
1,3-Butadiene
Acetone
Chloroethane
2-Butanone
Acrolein
Benzyl chloi
 CAS RN
  79^
 100-4X-
  75-09-
 120-82-1
 100-42-5
   6-93-4
  06-99-0
   7-64-1
      0-3
 107-
 100-44-7
                                 NA
 correspd
 validation.
 2ppbv reference
  sampling  method  is  not  suitable   for  the
NA - no data on CRQL available, pending methods

 nun Hg.
 June,  1991
                                       Page C-l
-------
Exhibit C
                                                     SOW No. XXX - Ambient Air
                                    TABLE 1

                           VOLATILES IN AMBIENT AIR
                        TARGET COMPOUND LIST (TCL)
                 CONTRACT REQUIRED QUANTITATION
                                  (continued)
                                 CAS RN

                                 108-10-1
                               10061-01-5
                                 156-60-5
                                 106-46-7
                                 123-91-1
                                  87-68-3
                               100
                                                      L for Valida
                                                    Sampling Method1
                                    -96-4
                                   8-05-4
                                  74-97-5
                                    r07-l
                                  75-6
                                  96-18-4
                                  42-82-5
                                  75-29-6
Target Compound

4-Methyl-2-pentanone
cis-1,3-Dichloropropene
trans-l,2-Dichloroethylene
1,4-Dichlorobenzene
1,4-Dioxane
Hexachlorobutadiene
Bromomethane
trans-1,3 -Dichloropropene
Dichlorodifluoromethane
Chloromethane
cis-1,2-Dichloroethylene
Methanol
Bromodichloromethane
Tribromomethane
Acetonitrile
1,3-Dichlorobenzene
3 -Chloro-1-propene
Dibromochloromethane
Methyl methacrylate
Te trahydro furan
Bromoethane
Vinyl acetate
Bromochloromethane
Propylene
l,l,2-Trichloro%
   1,2,2-trifl
Trichlorofluc
1,2,3-Trich;
Heptane
2 - Chloropf opafne
 xDash  (-)  it
 corresponding  tai
 validation.
 2ppbv referenced to 25°^
                                  sampling  method  is  not  suitable  for   the
                                   — no data on CRQL available,  pending methods
                              '60 mm Hg.
 June,  1991
                                                                       Page  C-2
-------
Exhibit C
                                                      SOW No.  XXX -  Ambient Air
                                    TABLE 1

                           . VOLATILES  IN AMBIENT AIR
                        TARGET COMPOUND LIST  (TCL) AND
                 CONTRACT  REQUIRED QUANTITATION LIMIT^
                                  (continued)
Target Compound

Octane
Chlorodifluoromethane
Bromobenzene
alpha-Methyl styrene
n-Pentane
Hexane
1,2-Dichloro-
    1,1,2,2-tetrafluoroethane
1,4-Dichloro-2-butene
l-Bromo-3-chloropropane
1-(methylethyl)benzene
l-Methyl-4-(l-methylethyl)benzene
l-Ethenyl-4-chlorobenzene
Bromotrichloromethane
Pentachloroethane
1-Chloropropane
1,2-Dibromopropane
2,3-Dichlorobutane
2-Chlorobutane
1,3-Dichlorobutane
1,4-Dichlorobutane
3,4-Dichloro-l-bute
l-Chloro-2,3-epoxy
2 -Chloroe thoxye thene
1-Phenylethanone "
Dibromomethane
1,3-Dichloropr
l,l,l,2-Tetra<£hlo
o-Chlorotol
             ndicates  that  th\Ls
                rget compound./  N
corresp
validation^
2ppbv referenc
June, 1991
 sampling  method  is  not  suitable  for   the
  - no data on CRQL available, pending methods

mm Hg.
                                                                      Page C-3
-------
 Exhibit C
                                                      SOW No. XXX  - Ambient Air
                                     TABLE 1

                            •VOLATILES IN AMBIENT AIR
                         TARGET COMPOUND LIST (TCL)
                  CONTRACT REQUIRED QUANTITATION LIMI
                                   (continued)
Target  Compound

1,3,5-Trimethylbenzene
p-Chlorotoluene
1,2,4-Trimethylbenzene
n-Butylbenzene
m-Chlorotoluene
Benzaldehyde
Benzonitrile
           CAS RN

           108-67-8
           106-43-4
           95-63-6
           104-51-8
           108-41-8
           100-52-7
(1)    Table  1  lists  all target VOCs whicn\are( required to be analyzed on  air
samples collected  by canis*t?r~(Se^ion 1, Exhibit D)  and on Tenax® (Section 2
Exhibit  D).    Target VOC£  specifiX  for each\sarapling method  are  tabulated
separately in Section 1 ^nd/Sectr^n ? ji£^Exhibi\  D,
(2)     The values in
not absolute detecti
at  or  slightly  ab
concentration of the
volatiles, CRQLS are
     1  are Eon
limits.
           Requl
    auantits
                            :d Quantitation Limits (CRQL),
                           limits in these tables are set
       concentrations  in the  sample  equivalent to  the
               .on standard analyzed  for each analyte.  For
spe>ifj.c fotl each sampling method.
(3)     Appendix^-A-of—this Exhi
been validated//but which
compounds  of
developed during method vali^ati
lead to v
compounds
        ranki
          17 VOCs for which neither method  has
          ir toxics  of concern or  identified as
  during^ the  development of  this SOW.   Data
   and subsequent analysis under SAS and RAS  may
methods in  this  SOW for some  or  all of  these
corresponding ta
validation.
2ppbv referenced to 25
June, 1991
       is/ sampling  method  is  not  suitable  for  the
         IA = no  data on CRQL available, pending methods
   .nd /60 mm Hg.
                                                                      Page C-4
-------
Exhibit C
                       SOW No. XXX - Ambient Air
                                    TABLE 2

                        VOLATILE ORGANIC COMPOUNDS FOR
            TENTATIVE IDENTIFICATION AND DEVELOPMENT OF/
Target Compound

Carbon disulfide
Pyridine
1,2-Dibromo-3-chloropropane
2 -Chloro-1,3-butadiene
trans-1,4-Dichlorobutene
Propanal
2-Hexanone
Cyclohexanone
1-Bromobutane
2-Methylnaphthalene
1,3,4-Trimethylbenzene
2,2-Dichloropropane
1,1-Dichloropropene
n-Propylbenzene
tert-ButyIbenzene
sec-ButyIbenzene
1,2,3-Trichlorobenzene
*     This /tab,
or adsorb
or ident^
SOW.
and RAS may
these compound
June, 1991
                              126-99-8
                              110-57-6
                              123-38-6
                              591-78-6
                              108-94-1
                              109-65-9
                              91-57-6
                              95-63-6
                               94-20-7
                                 -58-6
                                 -65-1
                              98-06-6
                              135-98-8
                              87-61-6
    compounds  for which neither method (canister
    ut which were ranked as air toxics of concern
    onal  interest during the  development of this
    validation and subsequent analysis under SAS
of/the VOC methods in this SOW for some or all of
                                        Page C-5
-------
Exhibit C
                                                     SOW No. XXX  - Ambient Air
                                    TABLE 3

                         SEMIVOLATILES IN AMBIENT AIR
                        TARGET COMPOUND LIST (TCL) AN
                 CONTRACT REQUIRED QUANTITATION LIMI
I.  PAHs, PESTICIDES, AND OTHER SEMIVOLATILES
Target Compound

Acenaphthene
Acenaphthylene
Ace tophenone
Aldicarb
Aldrin
Aniline
Anthracene
Bendiocarb
Benzidine
Benzo(a)anthracene
Benzo(a)Pyrene
Benzo(b)fluoranthene
Benzo(e)pyrene
Benzo(g,h,i)perylene
Benzo(k)fluoranthene
Benzyl alcohol
alpha-BHC
gamma-BHC (Lindane)
p-Biphenylamine
Bis(n-butyl)phthala
Butylbenzylphthala
Captan
alpha-Chlordane
gamma-Chlordane
Chlordane (Tech:
4-Chloro-3-metnylphenol
4-ChloroaniLtne
Bis(2-chloEoetKoxy)raethane
Bis(2-chlotoe/thyl)ether
Chlorothafl.on/1
Chlorpy^ifos
C^rysene
Daethai (OCR
4,4'-DDD
4,4'-DDE
4,4'-DDT
                                  83-32-9
                                 208-96-8
                                  98-86-2
                                 116-06-3
                                 309-00-2
                                  62-53-3
                                                                ng/m3
 37
 37
 37
146
146
 73
 37
183
 73
 37
 37
 37
 37
 37
 37
 37
146
146
183
 37
 37
183
146
146
146
183
 73
183
 37
183
183
 37
183
146
146
146
June, 1991
                                                                       Page  C-6
-------
Exhibit C
      SOW No. XXX - Ambient Air
                                    TABLE 3

                         SEMIVOLATILES IN AMBIENT AIR
                        TARGET COMPOUND LIST  (TCL) AND,
                 CONTRACT REQUIRED QUANTITATION LIMIT$
                                  (continued)
I.  PAHs, PESTICIDES, AND OTHER SEMIVOLATILES  (co
                                 CAS RN
  /On-column
In i ect ion'Xne
                                 959-
                               33213-
                                  72-20-8
                                 421-93-4
                                   4-57-3
                                  18-74-1
                                   7-47-4
                                      2-1
Target Compound

Diazinon
Dibenzo(a,h)anthracene
Dichlorvos (DDVP)
Dicofol
Dieldrin
Diethyl Phthalate
2,4-Dimethyl phenol
DimethyIphthalate
4,6-Dinitro-2-methylphenol
2,4-Dini trophenol
2,4-Dinitrotoluene
Endosulfan I
Endosulfan II
Endrin
Endrin Aldehyde
Endrin ketone
Bis(2-ethylhexyl)phthal
Fluoranthene
Fluorene
Folpet
Heptachlor
Heptachlor Epoxide
Hexachlorobenzene
Hexachlorocyclopentadiene
Hexachloroe thane
Indeno(l,2,3-c
Isophorone
Methoxychlo
2-Methyl pjfien
4-Methyl fihei/ol
2 -Methyl^naphihalene
Mirex
Naphthalene
2 -Naphthylamin
                       Page  C-7
 June,
-------
Exhibit C
                                                      SOW  No.  XXX -  Ambient Air
                                    TABLE 3

                         SEMIVOLATILES IN AMBIENT AIR
                        TARGET COMPOUND LIST (TCL)
                 CONTRACT REQUIRED QUANTITATION LIMITS
                                  (continued)
I.  PAHs, PESTICIDES, AND OTHER SEMIVOLATILES (/ontoinued)
                                                          CRQL
Target Compound

3-Nitroaniline
2-Nitroaniline
Nitrobenzene
4-Nitrodiphenyl
2-Nitrophenol
Nitrophenols (mixed)
Bis(n-octyl)phthalate
Oxychlordane
Parathion
Pentachlorobenzene
Pentachlorophenol
cis/trans-Permethrin
Phenanthrene
o-PhenyIphenol
Propoxur
Pyrene
Resmethrin
Ronnel
Toxaphene
2,4, 6-Trichlorophei
2,4,5-TrichlorophenoJ
  CAS RN

  100-01-6
   88-74-4
   98-95-3
   92-93-3
   88-75-5
2515
  On-coliumw
Injection, me
ne/m3

 73
 73
 37
 183
 73
 73
 37
 183
 146
 183
 183
 183
 37
 183
 183
 37
 183
 183
 146
 183
 183
June, 1991
                                        Page  C-8
-------
Exhibit C
                                                     SOW No. XXX  - Ambient Air
                                    TABLE 3

                         SEMIVOLATILES IN AMBIENT AIR
                        TARGET COMPOUND LIST (TCL) AND
                 CONTRACT REQUIRED QUANTITATION LIMITS
                                  (continued)
II.  PCBs (Congeners)
Target Compound

Monochlorobiphenyls
Dichlorobiphenyls
Trichlorobiphenyls
Tetrachlorobiphenyls
Pentachlorobiphenyls
Hexachlorob iphenyIs
Heptachlorobiphenyls
OctachlorobiphenyIs
Nonachlorobiphenyls
Decachlorob ipheny1
                                 CAS RN

                               27323-18-8
                               25512-42-9
                               25323-68-6'
                               26914-33-0
                               25429-29-2
                               26601-64-9
                               28655-71-2
                               314
                               53
                                20
  iDn-column
Iniect ion/cxne
                                               \ On-column
                                               Iniection. ne
Polybrominated biphenyls
III.  PCBs (Multicomponent
Target Compound
Toxaphene
Aroclor-1016
Aroclor-1221
Aroclor-1232
Aroclor-1242
Aroclor-1248
Aroclor-125
Aroclor-12
 June,  1991
                                                                      Page C-9
-------
 Exhibit C
                                                          SOW No.  XXX - Ambient Air     /*?\
  Analvte

Cadmium
Arsenic
Chromium
Beryllium
Selenium
Lead
Barium
Manganese
Thallium
Zinc
Copper
Antimony
Cobalt
Nickel
Silver
Vanadium
Tin
Molybdenum
Aluminum
Calcium
Iron
Magnesium
Potassium
Sodium
                                       TABLE 4

                             INORGANICS IN AMBIENT AIR
                           TARGET ANALYTE LIST  (TAL) AN
                   CONTRACT REQUIRED QUANTITATION LIM
                              CASRN
                             7440
                             7440
                             7440-
                             7440-
                             7782-
                             7439-
                             7440-
                             7439-
                             7440-
                             7440-
                             7440-
                             7440-
                             7440-
                             1313-
                             7440-
                             7440-
                             7440-
   Cont
Quant itati"
  ng/mg
                                                                                 .2.3
                18
                92
                44
                 7
               577
               118
                11
                15
               562
               444
                37
                92
                55
                52
               229
                26
               155
                33
               226
               381
               126
                89
               758
               592
(1)    The analytical methodsspeetfied iHvExhibit D must be utilized and the achieved instrument
detection limits must inejah^ontratkRequiredQuantitation Limits (CRQL) requirements. Higher
detection levels matronly. b
-------
Exhibit C
                           SOW  No. XXX -  Ambient Air
Interference
  Component

    Al
    Ca
    Fe
    Mg
    Na
    P
    K
    S
    C
    Cl
    Mo
    Ti
    As
    Cd
    Cr
    Co
    Cu
    Mn
    Ni
    Se
    Ag
    V
    Zn
                                    TABLE 5

                  •INTERFERENCE CHECK SAMPLE COMPONENTS
                            CONCENTRATIONS FOR ICP
     Solution A
Concentration (me/Li
         500.0
         500.0
         500.0
         500.0
         500.0
         500.0
         500.0
         500.0
       1,000.0
       3,600.0
          10.0
June,  1991
                                            Page  C-ll
-------
Exhibit C
                                                      SOW No.  XXX - Ambient Air
                                    TABLE 6

                INITIAL AND CONTINUING CALIBRATION
         CRQL STANDARD CONTROL LIMITS, AND LCS STAND
                            FOR INORGANIC ANALYSES
                    VERI
            INITIAL AND CONTINUING CALIBRATION  UERiriCATION  LIMITS
Analytical Method
Inorganic
 Species
    .e Value (EPA Set")
>v/Limit   High  Limit
ICP
GFAA
 Metals
 Metals
    90
                                                             90
110
110
                         CRQL STAND,
Analytical Method
ICP
GFAA
                        of  True Value  (EPA  Set)
                        Low Limit  High Limit
                             85
                             85
              115
              115
                          LCS\£TANDARB^C0NTROL LIMITS

The LCS Standard Control  Linbits Vre  the same for all inorganics species.  The
limits ar
June, 1991
                                                                      Page  C-12
-------
 ANALYTICAL METHOD  FOfc THE  DETERMINATION OF
  VOLATILE ORGANIC  COMPOUNDS (VOCs)  IN AIR
COLLECTED IN SUMMA® CANISTERS 
-------
                             SECTION 1
            ANALYTICAL METHOD FOR THE DETERMINATION
           ' -VOLATILE ORGANIC COMPOUNDS (VOCs) IN
           COLLECTED IN SUMMA® CANISTERS AND ANALY?
          " GAS CHROMATOGRAPHY/MASS SPECTROMETRY
                         TABLE OF CONTENTS
1.1   INTRODUCTION  ....

1.2   SAMPLE STORAGE AND HOLDING TIM

1.3   CANISTER PREPARATION AND CERTIFJ

1.4   GC/MS ANALYSIS OF VOLATILES FROM CANIST

1.5   REQUIREMENTS FOR DEMONSTRATING  METHOD  ACCEPTAt
      ANALYSIS FROM CANISTER]

1.6   OPTIONAL GC/FID SCREENIN
-------
Exhibit D
                                                      SOW No.  XXX - Ambient Air
                                   SECTION 1
                  ANALYTICAL METHOD FOR THE DETERMINATION
                   VOLATILE  ORGANIC COMPOUNDS (VOCs)  IN A
                 COLLECTED IN SUMMA® CANISTERS AND ANALYZED
                 GAS CHROMATOGRAPHY/MASS SPECTROME'
1.1  INTRODUCTION

1.1.1  Scope and Application

      1.1.1.1     The analytical methods  th/t
      whole air samples collected  in  SUMMA'
      canisters for a subset of the organ
      List (Target Compound List for  Volaci
      to be identified and quantified from
      in Table 1 of Section 1, Exhibit D  with
      Quantitation Limits shown there.  The  methods
                                           How ai
                                         .ished,
                                     signed  to  analyze
                                    nless  steel
                          ounds7 on/a Target  Compounds
                                   it C).  The compounds
                                  les are  those listed
                                     Required
                                        on EPA
                                              ontrc
      Compendium Method TO-14,  "The Determination  of Vol^ile  Organic
      Compounds (VOCs) in Ambient ^irr~trrtrig-~5IJMMA® Passivat&d/Canister
      Sampling and Gas Chromatograchi<^_AnalysisT"~~w±th~-apprppriate
      modifications.  The modificarionsN. incTtide->a  more  generic description of
      the method for preconcentrationvof\target/co^pouRSs-^nd  for generation
      of standards.  One result of the\nodifio4tit>ns is  that many systems
      currently in use for VOC analysis\an\te Adapted  to  these  analytical
      methods.  Any reasonable analytical\syst«n can be  used provided  the
      system produces results—equivalent to\the\results  specified in section
      1.5.  (section 1.5 presents insults whrch £re based  on data obtained
      using the TO-14 meXhod£'~3fesscription or eo^aiv^lent) .

                       od/ are divided into^
                      istei
1.1.1.2  The me
storage, canis
analysis; and/ana.
storage and c
as well as canis
a portion of the sanr
concentration_J_£vel of
dilution
MS
preco
GC/M
                         tical performance
                               inn
                              Jars
                            .e ma\
                                 voD
      1.1.1.3
July, 1991
                          following sections: sample
r /leaning^nd/certl^icat^on; sample screening; sample
                         irements. The section on sample
              and certification discusses holding times
            ion.  As described in the screening section,
             e analyzed by GC/FID to determine the
                iles and the possible need for sample
             ,on contains  a description of the full scan
        ,romatog^?aj^hic separation.  The sample
           is included in the analysis section because
           ^concentration technique are interrelated.
            equirements discusses detection limits,
            |e precision that have been achieved in EPA-
            , and which the laboratory must meet when
            is SOW.

       describes a procedure for analysis of target VOCs
                                                                  Page  D  -  1/VC
-------
Exhibit D
                                                     SOW No.  XXX -  Ambient Air
      in ambient air.  The method is applicable  to  whole ^ir/samples collected
    •  in SUMMA® passivated stainless steel canisters.   The  VDCs  are
      concentrated prior to. analysis, subsequently  sepa/ratflKl by  gas
      chromatography, and then detected by scanning mass spectrometry.

      1.1.1.4  This method is applicable to specif icrVQCs th^t hav«, been
      tested and determined to be stable when stored
      canisters.  The organic compounds that haveJbs^n  collected it
      pressurized canisters and successfully analyzed by this method
      listed in Table 1 along with target compound/ for which storage
      stability in canisters has not been fully  documented.  These  compounds
      have been successfully measured at the/par/ts  per  b/lllon by volume
      (ppbv) level.

1.1.2  Summary of Method

      1.1.2.1  A sample of air is drawn througfi>asamp
-------
Exhibit D
                       SOW No. XXX  - Ambient  Air
      of canisters.

      1.1.3.5  Canisters should be manufactured using hiffh  q/dality welding and
      cleaning techniques, and new canisters should be  filled with humidified
      zero air which is then analyzed to determine cle/nlimess.  The  cleaning
      apparatus, sampling system, and analytical system shottid be assembled of
      clean, high quality components and each system/sh^u"i4 be siipwn  to  be
      free of contamination.
      1.1.3.6  Canisters should be stored in a cc
      should be capped tightly during shipment zmd,
      leakage of ambient air into or out of t
      leak develops in the valve.
                       dnant-free
                      rhen not in use to
                     .ister in the event that a
      1.1.3.7  Impurities in the dilution sas /if applicable) and carrier  gas,
      organic compounds out-gassing from ttne plumbing/ah«sad of the trap, and
      solvent vapors in the laboratory acraunt rose  the inajority of
      contamination problems. The analytical s^tem mu/t be demonstrated'to be
      free from contamination under the conditiorts^of the analysis by  running
      humid zero air blanks. The use of tubing otherNt^ian ckromatographic
      grade stainless steel, non-TFE thread sealants, orxflow^ontrollers  with
      rubber components must be avc

      1.1.3.8  Significant contamin^itionoF^eka^analyticaiySquipment can occur
      whenever analysis of samples containing h/gh/TOC-eoocentrations  are
      analyzed.  This in turn can result; rn carryover contamination in
      subsequent analyses.  Whenever an \inusvjalLy concentrated sample  is
      encountered, it should be followed bjr an^nalysis of humid zero  air  to
      check for cross contamination.
      1.1.3.9  The laborator
      be completely fre/ of/solver

1.1.4  Definitions
      analysis o\vo\atiles is performed should
      NOTE:  Definitions
      operating procedi
      D1356. E260," and E3~!
      defined within this doci
July, 1991
   tYtis document and any user-prepared standard
 s)/should be consistent with ASTM Methods
Allxgertinent abbreviations and symbols are
  nt appoint of use.

   pre>&uj/e = Pg + Pa, where Pg = gauge pressure
   and Pa =° barometric pressure (see 1.1.4.7.5).

     Pressure measured with reference to
    [pposed to atmospheric pressure), usually
    sia.

   erant used to obtain very low temperatures in
  analytical system.  A typical cryogen is
                                   Page D - 3/VC
-------
Exhibit  D
                                                      SOW No.  XXX - Ambient Air
       liquid  nitrogen  (bp  -195.8)  or liquid argon (bp -  If

       1.1.4.4  Dynamic  calibration:   Calibration of an /nautical system using
       calibration gas standard  concentrations  in a for/ ideittical or very
       similar to the samples  to be analyzed and by in/rodvcing^such standards
       into  the  inlet of the sampling or  analytical system irKa numhar very
       similar to the normal sampling or  analytical

       1.1.4.5   Dynamic dilution:  Means  of  prepa/in> calibration  mxxturt
      which standard gas(es)  from pressurized  c/lin&ers  are  continually
      blended with humidified zero air in a ma/if old so  that a flowing stream
      of calibration mixture  is available at /he/inlet o/tfoe  analytical
      system.                                '   '       '  '

      1.1.4,6   Gauge pressure:  Pressure mfeasure^abo/e /mbient atmospheric
      pressure  (as opposed to absolute pressvnse). ^Z4ro/gauge  pressure is
      equal to  ambient atmospheric (barometric)xp
-------
Exhibit D
                                                      SOW No.  XXX - Ambient Air
      NOTE: If gauge pressure is <83 kPa  (<12 psig),  the  us^r may wish to
      pressurize the canisters, as an option, with nitrog
      gauge pressure of 137.kPa (20 psig) to ensure  that
      available for analysis.  However, pressurizing th<
      introduce additional error, increase  the method 2  Vachaum pump:  CTapaple of evacuating sample canister (s)  to an
      absolute'pxessur^. of <(/. 05/mm Hg.
July, 1991
                                                                  Page  D -  5/VC
-------
Exhibit D
                                                     SOW No. XXX  - Ambient  Air
      1.3.2.3  Manifold:  Stainless steel manifold with connections for
      simultaneously cleaning several canisters.

      1.3.2.4  Shut-off valve(s):  On-off toggle valve

      1.3.2.5  Thermocouple vacuum gauge:  Capable
      manifold to an absolute pressure of 0.05 mm
      1.3.2.6  Cryogenic trap (2 required):
      tubular trap cooled with liquid argon or
      contamination from back diffusion of oil,
      clean, zero air to sample canister(s).

      1.3.2.7  Stainless steel pressure gauges
      psig) to monitor zero air pressure.

      1.3.2.8  Stainless steel flow control va
      air into canister(s).
                                             Sta
                                                                       in  the
      1.3.2.9  Humidifier:  Pressur
      capable of providing moistur

      1.3.2.10  Isothermal oven (opt^ona^

1.3.3  Reagents

                                 High perf<
                                          water bubbler
                                                    supply.
      1.3.3.1  Deionized water
      grade for humidified
      1.3.3.2  Cryogen:

1.3.4  Cleaning Proced;

      1.3.4.1  A ca:
      Figure D/VOA-i:
      supply traps.   The
      shut-off valve and the"
      remaining
      the vent
      opened.
      vacu1
                                                      nitrogen to prevent
                                                    vacuum pump and to provide
                  kPa (gauge) (0-50


                       flow of zero


                        system
                                                            isters.
      1.3.4.2
      and the zero a
      with humid zero
       e liquid chromatography (HPLC)


liquids-nitrogen.
                                                 assembled as illustrated in
                                   .dded to both the vacuum pump and zero air
                                  s) are connected to the manifold.  The vent
                                      valve(s) are opened to release any
                                              The vacuum pump is started and
                              is tfiteo closed and the vacuum shut-off valve is
                                re evaluated to <0.05 mm Hg and held at this
                                 r.

                                   re often if necessary, the cryogenic traps
                                   r to remove any trapped water from previous
                          an^a vacuum/pressure gauge shut-off valves are closed
                            off/valve is opened  to pressurize the canister(s)
                               gauge pressure of approximately 206 kPa (30
                                                                                     . _./
July, 1991
                                                                 Page D - 6/VC
-------
Exhibit D
                                                      SOW No.  XXX - Ambient Air
      psig).   If a zero  gas  generator system is  used,  the
      to be  limited  to maintain the  zero  air quality.
                                                      Low rate may need
      1.3.4.3  The zero air  shut-off valve  is  closed and tbfe canister(s) is
      allowed to vent down to atmospheric pressure  througlZthe vent shut-off
      valve.  The vent shut-off valve  is closed.  ThLfe  procedure is repeated
      two additional times for a  total  of three  (3)/feva/u*£ion)>^essurization
      cycles for each set of canisters.
                                           IS 1C
                                          ifsh
                                           ^y
                                           than
                                          £analyz<
                                            Init
                                           pero4n
1.3.4.4  At the end of the evacuation/pres/rftbr>zation  cycle,  Che can
is pressurized to 206 kPa (gauge)  (30 psLg) i/ith humidified  zero
The canister is then analyzed by a GC/MS/or/GC/FID  analytical  system
Any canister with a concentration grea
speciated organic must be recleaned a
criteria for cleanliness, or be set
be checked after cleaning to establ
cleanliness criteria.  A total of
analyzed in ten batches to check for
and for batch contamination by the cleanin
two or less individual canisters are contamin
contamination is evident, the laboratory may
canisters tested for cleanli
check 10 percent of the cani(ste
run,  whichever is greater.
                                                                           ;ter
                                                  vappai
                                                   redu
                                             cleaning, but
ppbv or higher of any compound
flagged by the operator and chec
returned to the field.   Subject t
-------
Exhibit D
                                                      SOW No. XXX - Ambient Air
      manifold.   Canister  valves  are  closed.   The oven is,

      1.3.5.2  Liquid nitrogen is placed in the dewar
      cold trap and  is  replenished as needed during tl
      system valve is opened and  the  system lines ar«
      Hg.  If  the system lines will not  pump down,
      To correct  this,  the cryogen is removed and
      heat gun while air is  pulled through the lis/ into
                                                        ted to 100°C.

                                                       to immerse the
                                                       tnup cycle.  The
                                                           to <0.05 mm
                                                              JD locked.
                                                                  th a
                                                      is
                                                      the pv
      NOTE:  Care should be  taken  to  always  kee,
      unless the cold trap is  immersed  in cry
      through the lines to the pump.  This w
      backstream into the line between  the
                                              e  system valve closed
                                          en/or  air is being pulled
                                           'ensure J^ha^t pump oil does not
                                        ap/and can/ste'rs.
      1.3.5.3  Once the system  line  is ev^cuat&<,  the/nu
      and the manifold tubing is evacuated
      whether or not the canister/manifold  connections*
      canister valves are opened, and the canisters\are
      Hg and are held at this vacuum for a  minimum of
      valves are closed, the manifold^alve is  closed,
      disconnected from the manifolti.  TTh^~Tinmi»£oJLd valve
      so that air is flowing to thet pump-r^and thecryo?
      trap.   The trap is allowed toN^arm^ to roofip te/mceratu
      valve is closed.
                                                   F
                                                   dfold valve is opened
                                                  [g.   This  will indicate
                                                  re  leaktight.  The
                                                     .cuated to <0.05 mm
                                                  .e hoxfc    The canister
                                                          canisters are
                                                            ed slightly
                                                        removed from the
                                                        and  the system
      1.3.5.4  This cleaning method may tje e
      canisters are pressurized with humid\fie<
      re-evacuated.  After ^fttgarring, canisters
      zero air and analyz
                                              by adding a cycle  in which
                                          zero air and then
                                             pressurized with humidified
1.3.6  Leak test Procec
      1.3.6.1
                    lem
         Be for
pressurizing
with zero air.
canister valve is
pressure is measured
not decrease—by—more
each sampling nse
                                             car
                          osec
              isters must be tested by
             approximately 206 kPa (30 psig)
 ressure is measured and recorded and the
.fter 24 hours, the valve is opened, and the
  ded.  If leak- tight, the pressure should
      (0.029 psi) over the 24-hour period.
         jge pressure of
                               rec
                               llso be te'sted by evacuating to <0.05 mm  Hg,
                                 ig, closing the canister valve, and setting
                                  jours.  The canister  is then attached  to  the
                                      down to 0.05 mm  Hg.  Then the canister
                                     is recorded.  This vacuum should be
                               'initial vacuum.  Any significant change  from
                     ;uuni may Indicate that compounds are off-gassing from  the
                  JLs orxchat/th9 valve or weld seam are not leak-tight.
July, 1991                —	Page  D  -  8/VC
-------
Exhibit D
                                   SOW No.  XXX - Ambient Air
1.3.7  Certification of Canisters

            All canisters  for  sampling of VOCs  must be certified initially by
      GC/MS analysis of the calibration mixture of 59 compounds.
      Certification of the canister  consists  of comparimg the canister
      contents with the results of a direct analysis from the\sample source,
      e.g., dynamic dilution manifold,  then ageing ttie o£riister at   its
      contents for one week at normal room temperature
      canister contents, and again  comparing the
      the earlier direct analysis of  the  sample
      percent difference for any target compounj
      concentration in humidified zero air  is
      the target compounds should be  present

1.4   GC/MS ANALYSIS OF VOLATILES FROM CANpST!

1.4.1  Summary
            In this analysis procedure,  a whole  ars. sampl
      preconcentrator where the VOCs  are condensed onN-a_ red"
      surface (cold trap).  Subsequently the  condensed
      desorbed and backflushed fro;
      chromatographic column.  The
      is similar to that discussed iti ERA Compwidium Method
                                       with thexresul
                                       The acceptat
                                  i nominal 10 ppbv
                                   No compounds other than
                                         >f 1.0 ppbv.
                           iith  an  inert
is passed through a
   d temperature
  arfe thermally
    onto a gas
ue discussed here
  0-14 "The
      Determination of Volatile Organic Ciqmpound's  fVOC"s}~-i?( Ambient Air Using
      SUMMA Passivated Canister Sampling, and Gas (Shromatographic  Analysis".
      Other preconcentration techniques (Sfor\example,  those using solid
      sorbents) may be employed if equivalency As  established (see 1.5  for
      equivalency requirements-)— £or  the analvsisX procedure  of which it  is
      part. The gas chromatograph ik temperature -programmed to separate the
      individual VOCs, wMch/aTe^Nihen. detected \rLth) a  mass  spectrometer
      operated in a full/ scAn mode\  lHii~~~s-teps of\£he  analytical  method are
      diagrammed in Figure/D/VOA- 3}

1.4.2  Apparatus and/Mac4rials (,/ee/Figure

      1.4.2.1
            1.4.2.1^,1 -^ElectroitLg mas'Bx£Tow  controllers:   Used to  maintain
                     flow^-for caris^er  g^s and  sample  gas)  and to  provide an
                          to monitor  rigw anomalies.

            '1.4^.2.1.2  Vacuum\pump:   General purpose  laboratory pump,  capable
            of reducing the downsttream  pressure of the flow controller to
              ^ovide the minimum] pressure differential  necessary to maintain
            controlled flow raves./
            1 .
.. 3^Stainl/ess/steel  tubing and stainless steel fittings:
July, 1991
                                               Page D - 9/VC
-------
Exhibit D
                                                      SOW No.  XXX -  Ambient Air
            1.4.2.1.4  Stainless steel cylinder pressure  r/gu/ators:
            Standard, two-stage cylinder regulators wither ensure  gauges
            1.4.2.1.5  Gas purifiers:  Used to remove
            moisture from gas streams.

            1.4.2.1.6  Nafion® dryer (optional):  Cx
            coaxially mounted within larger tubinj
            from the sample stream if the MS in use"
            pumping capacity to handle water vapor./

            1.4.2.1.7  Six-port gas chromatographic valve
            and carrier gas flows.          /   /       /

            1.4.2.1.8  Cryogenic preconcen^ratcJisk:  Coofpl*
            commercially available from sev&u^l sobc/es,
                                                       Organic impurities and
                                                       ifsting  o£\Nafic
                                                         to  remove
                                                                    iter
                                                     ioes  not  have  sufficient
                                                             "or  routing sample
                                                          ~e units  are
                  The cooling unit is comprised o
                  (O.D.) nickel tubing loop packed
                  with glass wool plugsat each end.
                  is wound onto a
                  A cartridge heat
                  aluminum plate at
                  additional heat to eim
                  tubing.
                                                     .0.32Nim  outside  diameter
                                                                    Pyrex beads
                                                      TheNvj.ckeZ  tubing loop
                                                        tube Renter  (250 watt).
                                                              between  pieces of
                                                     id  outlet to  provide
                                                    spots~-rn  the  transfer
                  NOTE:   During operation, \he trap is inside a two-section
                                        which, is\we 11 insulated.  Rapid
                  heating /-150_to ^00°C in ?S s)\is accomplished by direct
                                          the heater and the trap tubing.
                  Cooling i4 achie-Ojed'^y ^?a-p$5riza\£on of the cryoge: .  In  the
                  shell/, efficient/cooking (+&£L-£.o -150°C in 225 s) is
                  facilitated by yonfdning^She vaporized cryogen to  the small
                  op/n vb^ume su/rounding the trap assembly.

                  The tra^L assembly and chromatographic valve are mounted  on a
                                        the injection and auxiliary  zones  of
                         on an tnsulatfed pad directly above the column oven.

                         Alternative tba^ assembly and connection to the GC
                  may be usfe
                  v^omprfe^e t
                      X?°P
                                   ine is connected to the injection end  of
                                   lumn with a zero-dead-volume fitting that
                                   n the heated zone above the GC oven.   An
                                  fitted over the sample handling elements to
                               package.  Vaporized cryogen is vented through
                                 box.
July, 1991
                                                                Page D  -  10/VC
-------
Exhibit D
                                                      SOU No.  XXX -  Ambient Air
1.4.2.2  GC/MS System

      1.4.2.2.1  Gas .chromato graph:  The gas chroma'to
      must be capable of temperature programming
      controller that maintains a constant colura]
      desorption and temperature program operations .
      include or be interfaced to a preconcen
      all required accessories including anaLti/al
      All GC carrier gas lines must be cons
      or copper tubing.  Non-polytetra-
  aphic (GC) system
     a flow
w rate throughout
    system must
       ve) and have
           gases.
             ^teel
 (PTFE)^
                                                          from
            sealants or flow controllers with  rubber components  are
            used. The column oven must be  cooLed Co  -50°C at the start of the
            gas chromatographic run;  therefore,  ? subamb^ttnj: oven temperature
            controller is required.

            1.4.2.2.2  Chromatographic col/umn^:   100%/me«!hyl silicone or 5%
            phenyl, 95% methyl silicone ca>4J.lary\calum/s of 0.25 or 0.32 mm
            ID x 50 m length or equivalent arex^equire^ to provide separation
            of the target compounds.
            1.4.2.2.3  Mass  spectrometer:
            amu every 1 second  or
            energy  in the electron; imp
            mass spectrum which mee\s
            acceptance criteria -when
            analyzed.
                                     Capable  of  scBnriing^from 35 to 300
                                       Lzing 70 volts  Q-Rp4inal)  electron
                                     ionizaflon-«ad_e,and producing a
                                           strument performance
                                     of p/brx^inoTtttetjobenzene  (BFB) is
            NOTE:  BFB  criteria must  be  meNt  bef/bre any samples are analyzed.
            Any  samples ana!j««
-------
Exhibit D
                                                      SOW No.  XXX - Ambient Air
             che mass spectrometer must  allow the  continuous  acquisition and
             storage, on machine  readable media, of  all  mass/spectra obtained
             throughout the duration of  the  chromatogranfiic/program.  The
             computer must have software that allows selrchl^g  any GC/MS data
             file for ions of a specified mass and plotting sucli^ion abundances
             versus time or scan  number. This type of p]/t  Cs^def^h^d as a
             Selected Ion Current Profile (SICP).  S«
             available that allows integrating the,
             between specified time or scan  numbe,!
             non-target compounds, software  must
             the comparison of sample spectra
             spectra. The 1990 (or most recent
             shall be used as the reference  Vibi
             capable of flagging all data f/
            by laboratory personnel.
            1.4.2.2.6  Magnetic tape storage de
            and must be suitable for long-term, of
      1.4.2.3  Calibration System amJ-Jlanifold
                   Also,
                   >le  that allows^
               reference  library
                     te NIST  Library
                       system must be
                   >een edited manually
                      of recording data
                    prage.
            NOTE:   The following clib
            Method TO-14 which discus,se^
            calibration methods such
            procedures may be used if,
            procedure is not compromised
            specifications in Section 5.

            1.4.2.3.1  Ca
            manifold, (1/25
            baffles for,
            manifold

            1.4.2.3
            grade
  gaseo
   use
 stern is~~&a»ed on EPA Compendium
   caiib^ation standards.  Other
  edr in purge and trap
 sych use, the analytical
respect to the performance
             or high purity quartz
             npling ports and internal
            proper mixing.  The
    impinger flask containing HPLC
            1.4.2.3.3
            unit^mTTme^or rnor*
            number of cylinders in
flow controllers:  One 0 to 5 L/min
  cm3/min units  for air,  depending on
    calibration.
                              fliter(s):   47 mm Teflon filter for particulate
                                sytinges:   For injecting internal standards
           .mixti

1.4.3  Reagents

      1.4.3.1  Gas cylirMers 4f helium and air:   Ultrahigh purity grade.
July, 1991
                         Page D - 12/VC
-------
Exhibit D
                                                      SOW No.  XXX - Ambient Air
      1.4.3.2  Liquid nitrogen.

      1.4.3.3  Deibnized water:  HPLC grade,  ultrahigh pj/rit
      humidifier).
                                                         (for
1.4.4  Standards
1.4.4.1  The Contractor must provide all  stan&aryds  to"b«  useTl^ith this
contract. The Contractor must be able  to  veiQ.fy/ that  the  sfcandartts are
certified traceable to a NIST Standard Refsfrerrce Material
NIST/EPA approved Certified Reference  Mat/ri
certificates of analysis must be retaine/i b
presented upon request.
                                                      (CRM) .  Manufactur
                                                    the  Contractor and
      1.4.4.2  When compound purity  is  assaye
      the weight may be used without corretti
      of the stock solution.   If  the compound
      than 98 percent, the weight must  be  co
      concentration of the stock  solution.
                                          to be  9,8  percent or greater,
                                           to  cadcu.tate the concentration
                                                is/assayed to be less
                                         jctedT wHen calculating the
      1.4.4.3  Commercially prepared  stock  standards  mayxbe usfed at any
      concentration  if  they are cer-tlTle-d— b4r__the  manufacturferyor by an
      independent  source, or  trace(able_to EPA^supp~tt«d^standards .   Fresh stock
      standards must be prepared once evefy^-evelve  months7~~J5r sooner,  if
      standards have degraded or concentrated. /St
-------
Exhibit D
                      SOW No. XXX  - Ambient Air
            1.4.4.5.3   Internal Standard Spiking Mixture

                        Prepare an internal standard  spiking mixture
                  containing bromochloromethane, chlorpbenrane-d5, and
                  1,4-difluorobenzene at 10 pprav each/in ^humidified  zero air
                  to be added  to the sample or calityrat/oriS^andal

      1.4.4.6  Standard Preparation Procedures
            1.4.4.6.1  Dynamic Dilution

                  1.4.4.6.1.1  Prepare stan<
                  gaseous standards  in the
                  air using mass  flow cont
                  The working standard ma
                  clean, evacuated canister
                  controller.  Alternatively,  t!
                  calibrated by sampling directly
                  rates of the dilution air and cylin<
                             dilution  of  the
                             humidified zero
                             ibration manifold.
                          rom  the manifold to a
                          and  mass  flow
                         ical  system may  be
                             anifold.   Flow
                                 rds (all
                   expressed  in the  samg__units)  are  measur&iusing a
                   bubblemeter  or  caaibrateaT~eieUUlpnraXio and the
                   original concentration of  each  compound^ The 10 ppbv level
                   calibration  standard \s the .continuing calibration standard.
               ^ „,-* T*> r*~  -    Original Coftc. xstd.  Gas Flovzate
               Manifold Cone. =                . W Gas Flowrate
              Manifold Co
.Example of 1 cn^/m£n  flow of  10  ppmv standard
   EXOO jcmi/min of\iumid   air provides a nominal
    \ as^alcviiated aelow:

                           = 10 ppb
 July,
             1.4.4.6.2  Sbafic Dilution Bottles

                                          prepared in canisters by spiking the
                   canisterwith a mi5^tur©? of components prepared in a static
                            bocKle.   A Standard Operating Procedure for the
                   preparation or\ static dilution bottles is available from the
                   AtmosphericNResearch and Exposure Assessment Laboratory,
                   Office of ReAearth and Development, U.S. E.P.A, Research
                   Triangle Park), Nf ,  27711, Document AREAL/RTP-SOP-MRDD-036 .

                ,4.6>3^High P/essure Cylinders

                         Stmdar4s may be prepared in high pressure cylinders,
                   as de>sribe0 in the following document:
                                  Page D - 14/VC
-------
Exhibit D
   SOW No. XXX - Ambient Air
                        Pollack, A.J., M.W. Holdren,  "Mult^Adsorbent
                        Preconcentration and Gas Chromatograiviic Analysis of
                        Air Toxics with an Automated
                        System," in the Proceedings of
                        International Symposium on Me
                        Related Air Pollutants, USEP,
                        90/026, pp. 209-218.
   Col
            1.4.4.6.4  Water Methods
                        Standards may be prepared
                  method, as described  in the /ol^owing document:
     / Analytical
     EPA/A&WMA
sent  of Toxic  and
   lumber  EPA/600/9 -
                        J.H.M. Stephenson,
                        Volatile Organics
                        Proceedings of th
                        Symposium on Meas
                        Pollutants' USEPA
                        194-199.
      1.4.4.7  Storage of Standards
                  Working standar
            canisters may be store
1.4.5  Instrument Operating Conditions

      1.4.5.1  Preconcentrator
            The following
      conditions which m
            1.4.5.1.1
           e, "Analysis of
         Methods," in
        International
        and Related Air
      EPA/600/9-90/026, pp.
      ;ds prepared in
preconcentrator analytical
  tor.
                                 enic  trap  fs^-ax a setpolnt from  -150 to
                                    int of  -150°C will trap all the VOCs on the
                  TO - UK^pmpotmd >list.)  A  500 cm3 sample of whole air is
                  passed through ^Shje trap during the sample collection period.

                                     should optimize the flow rate, duration
                              and abs^lyte  sample volume to be used.  Other
                               ion  systems  may be used provided performance
                             re \ealized (see 1.5).

                               on ^Conditions
                         Temperature:      120°C
                              Ra'te: 4  cm3/min helium
                                    <6Q  sec
July, 1991
              Page D - 15/VC
-------
Exhibit D
                           SOW No. XXX - Ambient Air
            1.4.5.1.3  Trap Reconditioning Conditions

                        Before initial use, condition
                .  120°C by flushing with  10 cm3/min o
                  trap effluent to the room and not
                  Prior to daily use, condition the
                  for 30 minutes while flushing wi
                  be vented to the analytical col
                  conditioning.
   e £rap overnight  at
  inept gas. Vent  the
  the ana-iytical column.
             ^at  120eC
  .ert gas>rm/nce check standard.
 July,  1991
                                       Page D  -  .16/VC
-------
Exhibit D
                                                     SOW No. XXX -  Ambient Air
      1.A.6.2  Frequency
                                             es/ blanks, or
                                               .blish that  the
                                                  : criteria for
            1.4.6.2.1  Prior to the analyses of any sami
            calibration standards, the Contractor must
            GC/MS system meets the mass spectral ion
            the instrument performance check standar
            p-bromofluorobenzene (BFB). The instrum;
            solution must be analyzed initially a
            period of operation.  Also, whenever
            corrective action which may change
            criteria (e.g., ion source cleaning'or/repair, column
            etc.), the instrument performance/check must be verified
            irrespective of the 12-hour labo
                                                       check
                                                         time
                                           ioof for
                                              librat
1.4.6.2.2  The 12 -hour time pe
performance check and standa
and continuing calibration ch
of the BFB which the laboratory
compliance tune.   The time period
elapsed.  In order to meet instrument p
requirements,  samples,  blanks, and standar
within 12 hours of the
                                   mits
                                  erft
                                                   aft
                                            tion.
      1.4.6.3  Procedure
1.4.6.3.1  The analysis o]
standard may be performed
                  By trappi
                  By an.
                  stan
July, 1991
                                                              tent,
    nstrument
  /(initial calibration
  egins at the injection
 documentation of a
   12 hours have
ormahce check
   must^be injected
                                                  ient performance check
                                       ly with a calibration
                                       contains 50 ng of BFB.
            1.4.6.3.
            following
            immedi
            averaged
            accomplished
                                   'must be acquired in the
                                  'peak apex scan and the scans
                  tng/and following the apex)  are acquired and
                    /subtraction is required,  and must be
                     iingle scan prior to the  elution of BFB.

                             ns must be identical to those used in
      1.4.
                                the analysis of any samples,  blanks, or
                              rds/,  the Laboratory must establish that the
                               tlrte  mass spectral ion abundance criteria for
                            jrf/'mance check solution.
                                                    Page D - 17/VC
-------
Exhibit D
                                                     SOW No. XXX  - Ambient  Air
                                                               rd must be
                                                                   during which
                                                                         S  mus t
      1.4.6.4.2  The instrument performance check s
      injected once at the beginning of each 12-ho
      samples or standards are to be analyzed.

1.4.6.5  Corrective Action

      1.4.6.5.1  If the BFB acceptance crite
      be retuned.  It may be necessary to c
      quadrupoles, or take other actions
      criteria.
            1.4.6.5.2  BFB acceptance criteria MOST be met Before any
            standards, performance evaluation GPE) samples/ or required blanks
            are analyzed.  Any samples or /equlred blanks/analyzed when tuning
            criteria have not been met wifclreqxHre ^analysis at no
            additional cost to the Agency.
      1.4.6.6  Documentation

            Reporting requirements

1.4.7  Instrumental Analysis

      1.4.7.1  The mass flow controlled
      correct flow rates for the system>
                                  ~Lsted in Exhibit B>
                                    re checked and adjusted to provide
      1.4.7.2  The sample canister is conne1
      analytical system, as^shownHn Figure
      with sufficient pre/surja—to dr
      the controller is /placed on\:h<
      and the canister
      system.  The flow r,ate out
      sample flow raye
                                      ;tec
                               ve an ele\tro
                                    ster,
to the inlet of the GC/MS
  4.   For pressurized samples
    c mass flow controller,
    canister valve is opened
   let to the analytical
 is higher than the optimized
vented while the desired
sample flow islestablisheca through the six-port chromatographic valve
and the preconcen£rom run to run.

                         cryogfem.c/trap are cooled to their set points
                          ctively.

                         ryagenic trap reaches its lower set point  of
                             graphic valve is cycled to the trap
                             ection.  The sample collection time which
                            .alyst is utilized.  Use a. gastight syringe
                         ot introduction of the internal standard during
                       er,a.od.  Add sufficient  internal standard  to  be
                          the  sample volume of 500 era3, e.g. a 0.5  cm3
                        nternal standard compounds, each at 10 ppmv
      has
             ^^
      or some alterna
      the sample
      equivalent  to
      volume of a mixture
July,  1991
                                                           Page  D  -  18/VC
-------
Exhibit D
                            SOW No.  XXX -  Ambient Air
      concentration.

      1.4.7.5  After the sample and internal standards a
      the cryogenic trap, the GC sampling valve is cycly
      position and the cryogenic trap is heated (-150
      and swept with helium.  The trapped analytes ar/4 thei
      the head of the capillary column and are separaterfNin
      the GC oven temperature program.  The canister valve
      canister is disconnected from the mass flow^controller atv
      trap is maintained at 120°C until the begirfn^ttg of the next
                                    econcentrated on
                                 'o  the  inject
                                 120°C  in 60 sec)
                                     ly  desorbed onto
                                        pluran using
                                            and the
                                                 The
                                           ilysi*
      1.4.7.6  Upon sample injection onto the
      operated so that the MS scans the atomy
      At least five scans per eluting chromaroj
      Scanning allows identification of unknot
      through searching of library spectra
                             the  GC/MS  system is
                       iss  rangexfrom 35  to  300 amu.
                      faphic  p/eak/should  be  acquired.
                       compounds/in  the sample
      1.4.7.7  Each analytical run must be checked "for/saturation. The  level
      at which an individual compound will saturate thexdetection system  is a
      function of the overall system sensitivity anSx^he ma^s spectral
      characteristics of that compound.  Secondary ionqHantifcmtion  is  allowed
      only when there are sample matrix—interferences witn^thX primary  ion. If
      secondary ion quantitation i4 performed^3o"CT3Hten£_^the reasons  in  the SDG
      Narrative.  When a sample is anaiyze3~~chat has saturated ions from a
      compound, this analysis must be, followed ,oy ,£~b~iaBl^zero air analysis.
      If the blank analysis is not free or^intrerferences, the system must be
      decontaminated. Sample analysis^ may nVpr resume until a blank can  be
      analyzed that is free of interferences.
      1.4.7.8  If the on-
      exceeds the initia
      discussed in section
      r ead j us ted,  and -the
      dilutions, and/exc
  umn concentration, ofXany compound  in  any  sample
       tidn range, that \ample must  be  diluted  as
  .4.9.V pke~~iciternal\ standard concentration
'sample r/e ana lyzeoN^Gui dance  in performing
         t*ist€Lguirefflent are given  below.
            Use thexresuJ
            mate dilution
            within the
ptions

   of /the/original analysis to determine the approxi-
 faceor /required to get the largest analyte peak
   al caiabration range.
            Thex3Tlution^£actor CHQsenahould keep the response of the  largest
             Kaly£e—^e^k for\a targeTs^compound in the upper half of  the
            Lnirial califer>atiorK range of the instrument.

               not submit datk foV more than two analyses, i.e., the original
            sample and one dilation, or, if the screening procedure  was
                      the most/concentrated dilution analyzed and one further
            Lilutl
July, 1991
                                       Page D -  19/VC
-------
 Exhibit D
                                                      SOW No. XXX - Ambient Air
                                                                 ired blanks
                                                                         >. have
                                                                  inimum. of
                                                                             to
1.4.8  Calibration

      1.4.8.1  Summary

            1.4.8.1.1  Prior to the analysis of samp
            and after the instrument performance ch
            been met, each GC/MS system must be ca
            five concentrations in an initial call
            the calibration check standard in a
            determine instrument sensitivity and tWe linearity of GC/MS
            response for the target compounds.

            1.4.8.1.2  A check of the calibration curve/mu/t be performed once
            every 12 hours.

      1.4.8.2  Frequency

            1.4.8.2.1  Each GC/MS system must be calibratea^upon award of the
            contract,  whenever the Contractor takes co>*ective\action which
            may change or affect the--iattialjcalibration cH^erla (i.e., ion
            source  cleaning or repair,  cobjrnlrrepiacement,  etc'j ,  or if'the
            daily calibration accep\an5£--e*i£eria have~~not~feeen met.
            1.4.8.2.2  If time remains\in\he
            meeting the acceptance criteria
            samples may be analyzed.  It\s not
            continuing calibration standarovif
            the calibration/ScceptsTice criteria
            blank of humidified_ultripure air
            Quantify allsamle
            standard ttyfx ys the s<
            calibration standard.
                                                   »ur time period after
                                                    initial calibration,
                                                tecessary to analyze a
                                               ;he initial calibration meets
                                                  10ve.   However,  a method
                                                n\trogen is necessary.
                                                ,he/initial calibration
                                   ne  concentration as the continuing
            1.4.8.2.^3  It^ime does/not remain in the 12-hour period after
            meeting the^acce^K^hce/criteria for the initial calibration, a new
            analysis of theinstr^ment performance standard is required.
      1. 4 . 8 ./
                BFB, then
               Procedure
                         .the  neV^anal>s4.s  meets  the  ion abundance criteria
                                       calibration standard may be analyzed.
            1/4.8.3.1  A.ssemble a ireconcentration device that meets  the
               unification in setti^n 1.4.2.1.8.  Condition the trap overnight
                     in the des^orb/mode with an inert gas flow of 4 cm3/min.
                         to ua4, /condition the trap for 30 minutes while
                              wi/th the column at 150°C.
            1.4.8.3.2
                          -lectr the  preconcentrator to  a gas  chromatograph.  The
July, 1991
                                                                Page  D  -  20/VC
-------
Exhibit D
                                         SOW No. XXX - Ambient Air
            gas chromatograph must be operated using temperature and  flow  rate
            parameters equivalent to those in section 1.4 .A. /Calibrate  the
            preconcentration-GC/MS system using the internal/standard
            technique.
            1.4.8.3.3  Prepare calibration standards
            concentration levels for each target co
            section 1.4.4.
                                                 timum of five
                                                     :ified in
            1.4.8.3.4  Prepare a spiking mixture/
            internal standards using the procedures'described in sectiot
            1.4.4.3.3.

            1.4.8.3.5  Verify that the GC/MS/sy/tem meetis tzhe instrument
            performance criteria in sectionr 1 .X.6 by analyzing BFB.  Analyze
            each calibration standard, addingx^he eouiv/lent of 10 ppbv each
            of the internal standard compounds during sample collection.

      1.4.8.4  Calculations
            1.4.8.4.1  Tabulate the area response of the\£rimaby ion  (see
            Table D/VC-3) and the o6~rre5p»adinK concentration/for each
            compound and internal
            1.4.8.4.2  Calculate the'
            compound using the follow^
            where:
                                               ors (RRF) for each
                                                                 Eq. D/VOA-3
Th
1. 4^4. 4\Calcu,
(%RSD)
                                                   tor;
                                                   on for the compound to be

                                                  ion for the internal

                               Dncentration of the internal standard ppbv; and
                                  :entration of the compound to be measured,
                                         calculated using the values of area
                                         ific  internal standard associated
                                   Table 3).

                                  he mean RRF  (RRF) for each compound by
                                  ibtained at the five concentrations listed in
                                  the percent  relative standard deviation
                                  over  the working  range of the curve.
July, 1991
                                                    Page D - 21/VC
-------
Exhibit D
                                                      SOW No.  XXX -  Ambient Air
                                      RRF
                                           x 100
            1.4.8.4.5  A percent difference  (%D)  of
            compared to the average RRF from the  in^
            Calculate the %D for each compound.
                                   Eq. D/VOA-4

                                     (12-hour)
                                      Iculated.
                  where:
                             %£> =
RRF
                                  RRF i - RRFC
                                     RRF,
                                Average/RR/ from i/itial curve; and
      1.4.8.6  Corrective Action

            1.4.8.6.1  If
            by more than
            calibration
            for ma1fun
            ion curre
            monitore
            any int
            chromatog
            inspected
            When corrections
            the
                                        Initial curve must
                        RRFC -  RRF fo/ir c/mpound.,

1.4.8.5  Technical Acceptance Crite^a

      1.4.8.5.1  Internal standard responses and'vretention  times must be
      evaluated during or immediately after oa
-------
Exhibit D
                                         SOW No.  XXX -  Ambient Air
      1.4.7 under conditions in section 1.4.5.

      1.4.9.2  Frequency

            1.4.9.2.1  If time remains in the 12-hour i£erj(od, samples may be.
            analyzed without analysis of a continuing/calibration standard.

            1.4.9.2.2  If time does not remain in che^-houTxperib^Lsince  the
            injection of the instrument performance check standard, both the
            instrument performance check standar«F-a]hu the continuing
            calibration standard must be analyzed before sample analyslrs^m&y
            begin.

      1.4.9.3  Procedure

            1.4.9.3.1  All canister sample's
            before analysis.
            1.4.9.3.2  Prior to the analysis of
            appropriate GC/MS operating conditions/
            1.4.5.
                                             establish the
                                                 .ed in section
       1.4.9.4   Dilut
                                             bient temperature
            1.4.9.3.3  Analyze th
            according to section

            1.4.9.3.4  Calibrate the

            1.4.9.3.5  Analyze the sample"
            1.4.7.

            1.4.9.3.6
            compounds
                                           ,ce check standard
                                           17
                                      according to section 1.4.8.
                                   owing the procedures in section

                                       target and non-target
1.4.9.4'
shown the
dilution of
factor needed to
              jratio
 flut
                                    creening procedure,  if used, will have
                                   concentrations  of  sample  components.   If  a-
                                    was  indicated,  first determine  the  dilution
                                        concentration into the  upper half of
                                         ,se one of the  following procedures to
                   ana
                         in section 1.4.9.4.2, calculate the final
                      canister needed to achieve the dilution.
                      anister with air or nitrogen which has been
                      be free of contaminants.  Heasure the final
                     re and calculate the actual dilution factor.

                tetf sample collection period during the GC/MS
           sis so/that a smaller volume of sample is passed
 July,  1991
                                                    Page D -
-------
Exhibit D
    SOW No. XXX - Ambient Air
                  through the trap.  The dilution factor
                 .dividing the standard sample collectio
                  sample collection time.

                  Using a gastight syringe, transfer
                  the original canister to a clean,
                  Pressurize the dilution canister
                  has been demonstrated to be fre
                  the dilution factor from the
                  injected and the volume of diluti
             Iculated by
              by the actual
         iquot^pf sample from
                  £er.
                       which
                          ate
            1.4.9.4.2  If the canister press
            factor is calculated and record
                                    DF =
            where:
DF =  Dilution factor;
Xa =  Canister pressure
Ya =  Canister pressure
            NOTE: (Xa and Ya  must b

            1.4.9.4.3  After sample
            multiplied by the dilutiof
            the sampled air.

1.4.10  Performance Evaluation Samples

      1.4.10.1  Summary

                  The
            Agency in
            not be i
            samples
                                         ^
                                                absolu
                Eq. D/VOA-6
               dilution; and
              dilution.
           oncentrations are
  termine"concentration in
  amples will assist the
•rmance.   The laboratory will
 are contained in the PE
       1.4.10.2
                                        tract, analyze, and report the results
                                          le delivery group, if available.
                                    ory will  receive humidified PE  samples  in
                                    he Agency.  The samples will come with
                                     the  extraction procedure  required  for  the
             1.4.10.3^2   Eacii  laboratory  must  extract  and  concentrate  the PE.
             sample  usingxthe  procedure described in 1.4 for those target
             compounds  listed/in Table D/VC-1.
 July,  1991
                Page D -  24/VC
-------
Exhibit D
                                               SOW  No. XXX  - Ambient  Air
      1.4.10.4  Calculations

                  Calculation concentrations  according  to/se/tion  1.4.9.

      1.4.10.5  Technical Acceptance Criteria

            1.4.10.5.1  The PE sample must be analyzed  ofiNa  GC/PK^system
            meeting the BFB tuning, initial calibr
            calibration technical acceptance  crit
            described in section 1.4.10.2;
            1.4.10.5.2  The PE sample must be
            according to 1.4.7;

            1.4.10.5.3  The PE sample must
            method blank that met  the blar
                                             icted and concentrated
                                         srepared/and'analyzed with  a
                                         jhnical/acG'eptance criteria;  and
            1.4.10.5.4  The results of  analyslr*  must  indicate  the  target
            compounds provided  in  the perforraancexevaluktion sample  and must
            meet replicate precision and  accuracy  crionenC\aynd standard component  mass
spectra.

1.4.11.2  Fory^stafclishing/co/respondehe^ of  the GC  relative retention
time (RRT),  the.sampS.fi component RRT must compare within ±0.06 RRT units
of the RRT of the\stand^rd ^component.  For reference,  the standard must
be run in the same I^hour ^fej-me period as the sample.  If coelution of
interfering cojSfionentspKohibvfcs accurate assignment of the sample
coraponentxRRT froin^the tota"3xion ehromatogram, the RRT should be
assigne^by Jts-irftg^extra^ted  ioh^urrent  profiles for ions unique  to  the
component/of  intere^
       7            \
1.4vll..3  For comparison^of\standard and sample component mass spectra,
mas4 spectra  obtained on thej Contractor's GC/MS are  required.  Once
ob^aineo>vthese standard/spectra may be  used for  identification  purposes
only^f the^Sontractor'a GGyMS  meets the daily  instrument performance
                        hese standard  spectra may be obtained  from the
run used  to obtain^ueerence RRFs.
 July,  1991
                                                           Page D - 25/VC
-------
Exhibit D
                     SOW No.  XXX -  Ambient Air
      1.4.11.4  The requirements for qualitative verification/by  comparison  of
      mass spectra are as follows:
            1.4.11.4.1  All ions present in the stand
            relative intensity greater than 10 perce
            the spectrum equals 100 percent) must b
            spectrum.
                             ^spectra at a
                                      ion in
                                        Le
            1.4.11.4.2  The relative intensities/of/ions
            1.4.8.1.3 must agree within ±20 perycen^ between  the  standard
            sample spectra. (Example: For an Lon i/ith an abundance  of  50
            percent in the standard spectra,/the/correspyond-^ng sample  abun-
            dance must be between 30 and 70/per/ient) .

            1.4.11.4.3  Ions greater than *10 perfc^nt An /the  sample  spectrum
            but not present in the standard spectrum must  be considered and
            accounted for by the analyst making the comparison.   The
            verification process should favor  falseisqsitiv^s.   All compounds
            meeting the identification criteria must beN^porred with  their
            spectra.  For all compou!fTtfa-~heJjow  the  CRQL red^&c £he actual value
            followed by a "J", e.g. "3J.
                                    \
      1.4.11.5  If a compound cannot
      section 1.4.11.4, but  in the tec!
      interpretation specialist, the idei
      Contractor shall report that identiJ
      quantification in 1.4.9._
          Lcati
           	    criteria  in
     :nt of the mass  spectral
'at^bn is correct, then  the
  in and proceed with
      1.4.11.6  Tentative,

            1.4.11.6.1
            sample co
            For this
            Library >
            generated
            routines that
            when  compared  to
               be^xecuted for non-target
                 tentative identification.
                recent) release of the NIST
    00 spectra, shall be used.  Computer
   h routines must not use normalization
   represent the library or unknown spectra
      r.
        ^v
         greatest apparent concentration not
all be tentatively identified via a forward
 .brary.  Only after visual comparison of
  ,e nearest library searches will the mass
    specialist assign a tentative
                                    for making tentative identification:

                   Chatacterist/c ions in the reference spectrum (ions greater
                   than lO^sOf/the most abundant ion) should be present in the
                   sample spectrum.
 July, 1991
                                 Page  D  -  26/VC
-------
Exhibit D
                                          SOW No. XXX -  Ambient Air
                  The  relative  intensities  of  the  major  IOHSI should agree
                  within  ±20  percent.  (Example:  For  an  Lon  with an abundance
                  of 50 percent of the  standard  spectra,/the: corresponding
                  sample  ion  abundance  must be between/30  /nd 70 percent.)

                  Ions present  in the  sample spectruni but  notxin the reference
                  spectrum  should be reviewed  for  pdssi/olexbackg^ismind
                  contamination or presence of coeiuting compounds.
                  Ions present  in  the  reference
                  spectrum  should  be reviewed
                  the sample  spectrum  because/jf
                  coeluting compounds.   Data
                  can sometimes  create thes/ di/screpan
                                     pfectrum but not  in^fche  sample
                                       ossible subtraction
                                      ackground contamination or
                                                reduction  programs
     :em libi
            1.4.11.6.4   If  in  the  technical jo4gment/of/the mass  spectral
                                                    ati
                                                jrted
interpretation specialist, no
be made, the compound should be r
spectral specialist should give additional
unknown compound if possible (i.e., unkn
hydrocarbon, unknown acidtype, unknown chlo"
probable molecular weights c
                                               iistinguishe
            •e identification can
            unknown.  The mass
              ssification of the
                 tic, unknown
              Lnateja compound) .  If
                  nclude them.
1.4.12  Quantitative Analysis

      1.4.12.1  Target Compounds
                                           ien
1.4.12.1.1  Target compounds
internal standard m«Ihen\:orrections are made,  reanalysis of samples
            analyzed while  tHe  system  was  malfunctioning is  necessary.

               .12.1.3   If  aftter  ireanalysis, the  SICP areas  or  the RTs  for  all
            iiv&rnal standards  ar/e  inside the contract limits of ±40  percent,
              ien  th« problemywidi the  first analysis  is considered to have
            beetKwitntr^the/concrol  of the laboratory.  Therefore, submit only
            data  fttam theN/naWsis with SICPs within  the contract limits.
            This  is cOTv^iderera  the  initial analysis and must be reported as
July,  1991
                                                     Page D -  27/VC
-------
Exhibit D
                                                      SOW No.  XXX - Ambient Air
such on all data deliverables.

1.4.12.1.4  If the reanalysis of the sampl
problem, i.e., the SICP areas or internal
the contract limits for both analyses,  t
and sample data from both analyses.  C
initial analysis and the reanalysis on/al
using the sample suffixes specified
SDG Narrative all inspection and co

1.4.12.1.5  The relative response
standard analysis is used to cal/ul
sample.  Use the RRF as determi
below.  When target compounds
quantitation limits (CRQL),  b
identification criteria, report
example, if the CRQL is 5 ppbv and
calculated, report as "2J."
                                                           is  not solve the
                                                                RTs  are outside
                                                          ibmitT^-the  SICP data
                                                                      the
                                                            from  the  daily
                                                            ntration in the
                                                           .nd  the  equations
                                                           t required
                                                             the
                                                        ation  with a "J."  For
                                                        ration of  2  ppbv is
                                                                  Eq.  D/VOA-7
            where:
                                                            ppbv,
                                th^ characteristic  ion  for the
                                     e measured,
                                the/characteristic  ion  for the
                                    ernal standard,
                                  internal standard present in
                                    a:
                                    compound
                                    area
                                    specifiN
                                    amount
                                    jpbv, '
                                                      factor from  the  analysis
                                    of the calibration standard, and
                                             fa~Cjtor calculated as  described in
                                     .. 4. 7 . SN^Iyt no dilution is performed,  the
                                    DF =  1.

      1.4.12.2  Non- Targeli^ConipoUtids

            1 - 4->2T2Tl~~^An estinia
-------
 Exhibit D
                                                      SOW No. XXX  - Ambient Air
 1-5   REQUIREMENTS FOR DEMONSTRATING METHOD ACCEPTABILITY EQR VOC ANALYSIS
    '   FROM CANISTERS                                      7^
             There are three performance criteria which
       laboratory to demonstrate that its analysis raeth
       successfully perform VOC analysis on air sampl
       established for:  the method detection limit,
       audit accuracy.   These criteria are a detect
       replicate precision within 25%, and audit a
       concentrations normally expected in ambien
       each  compound on  the Target Compound List
       ing laboratories.   These criteria were e^ta
       from  the  Toxics Air Monitoring Syst
       Toxics  Monitoring Program (UATMP) ne
       the acceptability of analysis method/on
                                                             be met for a
                                                             choice can
                                                                ia are
                                                                   .sion,  and
                                                        imit
                                                      .cy within
                                                        Specific  criteria
      currently being used for the analysi
      VOCs in air.  Essentially these analyire of^reoisi/n used for this program is the unsigned
      relative differenfcebetv>4en/replicate measurements of the same sample
      expressed as a percentage ix>  [(Measurement #1 - Measurement #2) x 100
      percent] /_AxerAge. Theffexare>everal factors which may affect the
      precisiorKbf the mea^iremenb^TheSnature of the compound of interest
      itself Edayh*VE-~-sMcatexcalibratic/n simples at the 10 ppbv level.  A more
      conservative measure w/s obtained from replicate analysis of "real
      world" canis>&rsam>i/s firom the TAMS and UATMP networks.  These data
      are given in TabTreD/VC/5.   The information presented in Table D/VC-5
Juli
                                                                Page D  - 29/VC
-------
Exhibit D
                                                      SOW No.  XXX -  Ambient Air
      was used to determine the replicate precision value
      goal to be achieved for each of the target  compoun

1.5.3   Audit Accuracy

      1.5.3.1  A measure of analytical accuracy is
      with audit standards.  Audit accuracy  is defi
      difference between the measurement result
      of the audit compound;

             Audit Accuracy, % = Spiked Value -
                                                               5  percent as a
                                        Spikep
                                                                            on
                                                                     -  D/VOA-8
                                                  lue
      1.5.3.2  Audit standards will be supp/Lie4  to  the,
      laboratories, these audit standards
      obtain audit accuracy values.  Audit
      similar values obtained from network data~>\Audii
      TAMS and UATMP analyses are summarized  in .'
      form the basis for a selection of 30 percent  as
      criterion for audit accuracy.
                                                       pai/ticipating
                                                          e  results used to
                                                        es will be compared  to
                                                        accuracy  results for
                                                               These  values
                                                          perormance
1.6   OPTIONAL GC/FID SCREENING OF

1.6.1  Summary
                                              CANISTERS
      1.6.1.1  The air sample is screenedXby ~GC/fID  to determine  the
      approximate range of concentrations oSf volatile organic compounds  and
      whether the sample shpaTcPBe\diluted priorvto  GC/MS analysis.

      1.6.1.2  Since FID/idantifibatipns_^are based <&n retention time  alone,  an
      FID screening anaXysi/s is usdfulineTs^ablisxhing tentative
      identifications ^nd/concentr&tiar»-vpf tnV-eomponents  in a sample and in
      determining whe/ihejc a dilution/of the^^ample will be  required prior to
      GC/MS analysis

1.6.2  Apparatus and

      1.6.2.1  Gas-trhnjwa^ograpFfxAn "at^lytical  system complete  with gas
      chromatoefaph suitabiexfor on^xolumh injection and all required
      access or ies^lnclua^g analytic a l^Tsolumns , gases, flame ionization
      detecDfer,/and integrator. \A data system  is recommended for measuring
      peak/areas.  SubambientN^verv control and  oven  temperature programming
      are/reouired.
      1.6/2x2  Cft^Dmatographic /coLdmn:   30  m x 0.53  mm  fused silica column
      such as^fi^-1, i*§- 5 ,  or D»B-^24,  or  equivalent.   The column temperature
      should be tt^Jd atxx50°!6  for  2 min  and then programmed from -50°C  to
      150°C at 8°C/ral^andsneld/at 150°C until all target compounds elute.

      NOTE:  The wider MegaWre® column  (i.e.,  0.53  mm I. D.) is less
 July,  1991
                                                                 Page
-------
Exhibit D
                                               SOW No. XXX  - Ambient Air
susceptible to plugging as a. result of trapped water,
the need for a Nafion® dryer in the analytical syst
retention time variability has been observed when
not used to remove water vapor from the sample st
therefore must be careful to consider any retenti
identifications are made.  The Megabore® column
approaching that of a packed column, while ret,
resolution traits of narrower columns (i.e.,
operating parameters are to be optimized by

1.6.2.3  Six-port gas chromatographic valve.

1.6.2.4  Cryogenic trap with temperaturf! control as-s^mbly:
1.4.2.
                                                            ^thus  eliminating
                                                              ?However,  greater
                                                             Nafion®  dryer  is
                                                              and  the  analyst
                                                               shifts when
                                                              tie  capacity
                                                                   the  peak
                                                                  see section
      1.6.2.5  Electronic mass flow controlleiump, "capable of
      reducing the downstream press*ffe~~o£—thigflow controlled/to provide the
      minimum pressure differentia^
      rates
      1.6.2.7  Chromatographic grade st
      steel plumbing fittings.

      1.6.2.8  Vacuum/pr
      measuring vacuum and/pressur

      1.6.2.9  Stainless' s
      two-stage cylind*
      nitrogen, and h
                                                    controlled flow
                                            el tubing and stainless


                                            steel gauges, capable of
                                             gulators:  Standard,
                                         re "gauges for helium, air,
      1.6.2.10  Gas
      from gas streams^
      1.6.2.11

1.6.3  Reagen
                             d to remove organic impurities and moisture


                                 manifold described:  see section 1.4.2

                                 >

                            f helium,  hydrogen,  nitrogen and air,


                             r cooling GC oven and cryogenic trap.

                           HPLC grade, for humidifying gas streams.
July, 1991
                                                          Page D - 31/VC
-------
Exhibit D
                                               SOW No.  XXX -  Ambient Air
1.6.4  Procedure
      1.6.4.1  Prepare working calibration standards as,
      and calibrate the GC at three of the five (2, 5
      concentrations to determine the instrument lirv
      Once the FID linearity range has be;  establi
      calibrated using a single-point (5 ppov) cal
      period.
      1.6.4.2  Analyze the sample with the sam-
      1.4.7.5 and 1.4.7.6.  Use the retention
      the calibration standard to tentativel
      sample.

1.6.5  Analytical Decision Point
1.6.5.1  Based on the concentrations of
compounds in the sample, determine whether
whether the target compounds are within the rangl
calibration.
                                                     Zcribed  in  1.4.4.3,
                                                       j>pbv)
                                                          sensitivity.
                                                                  be
                                                                  12-hour
                                             npling described  in sections
                                                      target compounds  in
                                                      tt compounds  in the
      1.6.5.2  If target compounds
      calibration, proceed to sectior
                                      [ithin therST
                                                          identified target
                                                            must be diluted or
                                                               GC/MS
>f  the  GC/MS
      1.6.5.3  If target compounds are presant? at/ concentrations higher than
      the calibration range of the GC/MS \then tfne sample must be diluted as
      described in section 1.4.9.4 prior to\GC/4lS analysis.
 July,  1991
                                                           Page D - 32/VC
-------
Exhibit D
                                                     SOW No. XXX  - Ambient  Air
                TABLE  D/VC-1.   TARGET  COMPOUND LIST (TCL)
                •CONTRACT REQUIRED QUANTITATION LIMITS (CJ
                     FOR  VOLATILES  COLLECTED  IN CANISTERS
Compound

Vinyl chloride
Trichloroethylene
Chloroform
Benzene
Carbon tetrachloride
Tetrachloroethylene
1,1-Dichloroethene
Acrylonitrile
1,2-Dichloroethane
Chlorobenzene
1,1,1-Trichloroethane
1,1,2-Trichloroethane
1,1,2,2-Tetrachloroethane
Ethyl benzene
Methylene chloride
1,2,4-Trichlorobenzene
Styrene
1,1-Dichloroethane
Toluene
Xylenes, m- and p-
Xylene, o-
1,2-Dichloropropane
1,2 -Dichlorobenzene
1,2-Dibromoethane
1,3-Butadiene
Acetone
Chloroethane
2-Butanone
Acrolein
Benzyl chloride
4-Methyl-2-pen
cis-1.3-Dich
trans-1,2-D
1,4-Dichlo/ob
Hexachlorpbut&diene
                                  75-01-4
                                  79-01-6
                                  67-66-3
                                  71-43-2
                                  56-23-5
                                 127-18-4
                                  75-35-4
                                 107-13-1
                                 107-06-2
                                 108-90-7
                                  71-55-6
                                  79_-06-5
                                  7/
                                 r
                                 120-
                                 100-4
                                  75-34-
                                 108-88-3
                                  30-20-7
                                   5-00-3
                                  78-93-3
                                    -02-8
                                       -7
                               10061-
                                 156-60-5
                                  06-46-7
                                  87-68-3
July, 1991
                                                                Page D  -  33/VC
-------
Exhibit D
                                                     SOW No. XXX - Ambient Air
                TABLE D/VC-1.  TARGET COMPOUND LIST (TCL)7
                .CONTRACT REQUIRED QUANTITATION LIMITS
                    FOR VOLATILES COLLECTED IN CANISTER
                                  (continued)
                                   CAS RN
                                   75-6
                                  142-82-
                                  111-65-9
                                   75-45-6
Compound

Broraomethane
trans-1,3-Dichloropropene
Dichlorodifluoromethane
Chloromethane
cis-1,2-Dichloroethene
Methanol
Bromodichloromethane
Acetonitrile
1,3 -Dichlorobenzene
3-Chloro-l-propene
Dibromochloromethane
Methyl methacrylate
Vinyl acetate
Propylene
l,l,2-Trichloro-1.2,2-
   trifluoroethane
Trichlorofluoromethane
Heptane
Octane
Chlorodifluoromethane
alpha-Methyl styrene
n-Pentane
Hexane
1,2-Dichloro-l,1,2,2-
   tetrafluoroethane
1,3,5-Trimethylbenz
1,2,4-Trimethvlbenze
July, 1991
                                                                Page D  -  34/VC
-------
Exhibit D
                                                      SOW No.  XXX -  Ambient Air
        TABLE D/VC-2.  REQUIRED BFB KEY IONS AND ION ABUNDANCE CRITERIA
                         8.0
                         30.0
                         base
                         5.0
                         less
                         50.0
                         4.0
                         93.0
                         5.0
                 Ion Abundance Criteria
                • 40.0  percent  of mass  95
                 -  66.0 percent of mass
                 peak,  100 percent relaj
                • 9.0 percent of mass
                 than 2.0 percent of
                 -  120.0 percent of
                • 9.0 percent of me
                 -  101.0 percent
                • 9.0 percent of
Note :
even though"
   iundances must /be ^normalized to m/z 95,  the nominal base peak,
je  iottvabundance £f rji/z 174 may be  up to 120 percent that  of m/z 95.
July, 1991
                                                   Page D - 35/VC
-------
Exhibit D
                                                      SOW No. XXX  - Ambient Air
            TABLE D/VC-3.  CHARACTERISTIC  IONS  FOR TARGET /OM/OUNDS
                                    Primary  Ion*
                                                                   Secondary
Parameter
lonfs")

Vinyl chloride*-0
Trichloroe thene*'0
Chloroform*-0
Benzene"1"-0
Carbon tetrachloride*'0
Te trachloroe thene* • °
1,l-dichloroethene*'°
Acrylonitrile*'0
1,2-dichloroethane*'0
Chlorobenzene*'0
1,1,1-trichloroethane*'0
1,1,2-trichloroethane0
1,1,2,2-tetrachloroethane°
Ethyl benzene*'0
Methylene chloride*'0
1,2,4-trichlorobenzene0
Styrene0
1,1-dichloroethane0
Toluene*'0
Xylenes, o-, m-,  and p-°
1,2-dichloropropane*'°
1,2-dichlorobenzene0
1,2-dibromoethane*'°
1,3-butadiene*
Acetone*'0
Chloroethane0
2 -butanone*'0
Acrolein
Benzyl chloride0
4-methyl-2-pentanone
c is -1,3 -dichloropropene0
*The primary io/i should be u^ed cmless interferences are present, in which case
a secondar/ iott may be used.
*NIST certified gaseous standads Wre available  for  these  compounds.
°Gaseous/staMards prepared grjiviijietrically  using NIST traceable  weights  are
available^fpr tne^e compounds
Note:   Standards^tpr
either static diluti
apparatus
                           compounds can be  prepared from neat materials  using
                       bottles /or by purging neat materials  from  purge  and trap
           into  canisters-\(see/Section 6).
July, 1991
                                                                 Page  D  -  36/VC
-------
Exhibit D
                                                      SOW No.  XXX -  Ambient Air
            TABLE D/VC-3.   CHARACTERISTIC IONS FOR TARGET GROUNDS
                 •  .               (continued)
Parameter
lon(s)

trans -1,2-dichloroethene
1,4-dichlorobenzene°
Hexachlorobutadiene0
Bromomethane* • °
trans-1,3-dichloropropene
Dichlorodifluoromethane* •"
Chloromethane0
cis-1,2-dichloroethene0
Methanol0
Bromodichloromethane
Acetonitrile*'0
1,3-dichlorobenzene0
3-chloro-l-propene°
Dibromochloromethane
Methyl methacrylate0
Vinyl acetate
Propylene
l,l,2-trichloro-l,2,2-
   tr if luoroe thane*'0
Trichlorofluoromethane*'0
Heptane
Octane
Chiorodifluoromethane
Alpha-Methyl styrene
n-pentane
Hexane
l,2-dichloro-l,l,2,2
   tetraf luoroethan-
1,3, 5-trimethylbenz
1,2 ,4-trimethylbenzene
Primary Ion**
Secondary
July,1991
                                      . 3
                                       29
                           41, 29, 57,-85
                                       31
                        117, 103, 78, 115
                           42, 41, 27, 29
                           43, 41, 29, 27

                                  135, 87
                                      120
                                      120
                            Page D - 3
-------
Exhibit D
                                                     SOW No. XXX  - Ambient Air
    TABLE D/VC-4.   METHOD DETECTION LIMITS (MDL),  PPB FOR
TO-14 List
Lab.//l
Lab.#2
                                     COMPOUNDS *
                                                                    MDL, ppbv
Freon 12
Methyl Chloride
Freon 114
Vinyl Chloride
Methyl Bromide
Ethyl Chloride
Freon 11
1,1-Dichloroethene
Dichloromethane
Freon 113
1,1-Dichloroethane
Cis-1,2-Dichloroethene
Chloroform
1,2-Dichloroethane
1,1,1-Trichloroethane
Benzene
Carbon Tetrachloride
1,2-Dichloropropane
Trichloroethene
Cis-1,3-Dichloropropene
Trans-1,3-Dichloropropene
1,1,2-Trichloroethane
Toluene
1,2-Dibromoethane
Tetrachloroethylene
Chlorobenzene
Ethylbenzene
m,p-Xylene
  0.40
 July,  1991
                                      Page D -  38/VC
-------
Exhibit D
                           SOW No.  XXX -  Ambient Air
   T.--LE  D/VC-4.   METHOD  DETECTION LIMITS (MDL) ,  PPB FOR 1,0-14 COMPOUNDS *
                                  (continued)
TO-14 List
Lab.tfl
Lab.#2
MDL, ppbv
Styrene                   1.64
1,1,2, 2-Tetrachloroethane 0.28
o-Xylene                  0.57
4-Ethyltoluene
1,3,5-TrimethyIbenzene
1,2,4-Trimethylbenzene
m-Dichlorobenzene         0.36
Benzyl Chloride
p-Dichlorobenzene         0.70
o-Dichlorobenzene         0.44
1,2,4-Trichlorobenzene
Hexachlorobutadiene
*Method  Detection Limits  (MDLs)
deviation of seven replicate analy
confidence.  For Lab #2 the MDLs repr
for MS/SCAN for Lab #1 and for MS/SIM
by SIM but not by SCAN, the SIM MDL has
value has been used as  a substitute SC.
given in the  last column. Tep_of^ the compo
                             roduct of  the  standard
                                  test value for 99%
                                ur studies. MDLs are
                        For  those  compounds measured
                   It/plied by a factor  of 5 and this
                     The resultant  list of MDLs are
                      ave no listed MDLs.
 July,  1991
                                      Page D  -  39/VC
-------
 Exhibit D
                                                      SOW No. XXX - Ambient Air
         TABLE D/VC-5.
 Monitoring
    Compound
 Identification
   SUMMARY  OF  EPA DATA  ON REPLICATE
    FROM EPA NETWORK OPERATIONS*
                             Urban Air Toxics
    Monitoring Program
%RP ,      #    ppbv
                                                               ION (RP)
 Dichloromethane       16.3
 1,2  Dichloroethane    36.2
 1,1,1 Trichloroethanel4.1
 Benzene
 Trichloroethene
 Toluene
 Tetrachloroethene
 Chlorobenzene
 Ethylbenzene
 m,p-Xylene
 Styrene
 o-Xylene
 m-Dichlorobenzene
 p-Dichlorobenzene
"' ?/ denotes n
statistic.
difference
*  Styrene
entries.
not inclu<
                                           ~ZT7"
                                            47

                                            47
                                            47

                                            47
                                            47
                                            47
                                            47
                                            47
 0.6

 2.0
 1.5

 3.1
 0.5
 1.5
0.2*
0.5
           ate orMuplicate analysis  used to generate the
           von is defined  as  the  mean ratio of  absolute
             :  the  GC column used in UATMP.   For the TAMS
             ction limits for 18 of  47 replicates and were
JuLv
                                                                Page D - 40/VC
-------
 Exhibit D
                                                      SOW No. XXX  - Ambient  Air
        TABLE D/VC-6.  AUDIT ACCURACY  (AA)  VALUES* FOR TO-L4 COMPOUNDS
Selected  Compounds
From TO-14  List
  FY-88
  TAMS
AA(%), N-30
Vinyl chloride
Methyl bromide
Freon 11
Dichloromethane
Chloroform
1,2-Dichloroethane
1,1,1-Trichloroethane
Benzene
Carbon tetrachloride
I,2-Dichloropropane
Trichloroethene
Toluene
Tetrachloroethylene
Chlorobenzene
Ethylbenzene
o-Xylene
  4.6
*A.udit accuracy is
lute  differenc,
divided by t
the audic ac
because chsrv
 denot
July, i<5<51
          of multiple determinations of the abso-
           .rement  result  and  its  nominal value
           ie number of audits averaged  to obtain
 lation is not available for other TO-14  compounds
in\the audit materials.
                                                                 Page  D  -  41/VC
-------
  Exhibit  D
                                                           SOW No.  XXX - Ambient Air
                                                                                Pressure
                                                                               Regulator

                                                                                if
                          vacuum
                 ..        Pump
                 Vacuum  shutoff
                   Pump    Valve
                                                                Cryogenic
                                                               Trap Cooler
                                                              (Liquid Argon)
                                                   V
                                                  Shuto
                                                   Valve
                             Cryogenic
                            Trap Cooler
                           (Liquid Arg
                 Vacuum
                  Shutoff
                  Valve
                             Vacuum
                                uge
                                 Zero
                                Shutoff
                                 Valve
                                                               Flow
                                                              Control
                                                               Valve
Vacuu
 Gauge
Shutoff
 Valve
                           SampleYv/Simple
                          Canister! \( Canister
               Sample
               Canister

 Optional
Isothermal
  Oven
                                    Canister Cleaning System
July,1991
-------
Exhibit D
SOW No.  XXX - Ambient Air
       Thermocouple
       Vacuum Gauge
      Vent 4
                               ernate Canister Cleaning System
July, 1991
           Page D -  43/VC
-------
Exhibit D
                                                        SOW  No.  XXX - Ambient  Air
                                             Sample
                                           Conditioner
                                           ssure Adjus
                                          rrna^Pore-Oryer
                                            Intern
                                              rds
                Mass
            Spectroscopy
Chromatography
            Ion Trap MS
            Quadrupole WIS
            Other MS Types
                                   • /Two-D Chromatography
^ ^S
Preconcentrator
" ';£: '
?
                           • Auto Cryogen Trap
                           • LAr in Flask
                           • Solid Sorbent Tube
  Sample
Conditioner
                             Cryo focusing
                             - Separate Assembly
                             - Head of Column
                             He Purge of Solid
                             Sorbent
                                       Analysis  Description For
                                   Samples From  Canisters
July,  1991
                             Page D - 44/VC
-------
Exhibit  D
                   SOW No. XXX -  Ambient Air
    LEGEND
      F   = Zero dead volume fitting
      T   = Thermocouple
      FC  = Flow controller
IN  = Liquid nitrogen
V   = Valve
               Calibration Gas
                  Cylinder
   Zero-Air
   Cylinder
                                                      Calibration Manifold
                                                                    =3 Septum
                                                                       Dry Purge
                                                                       •   Gas
                                                            Perma-
                                                             Pure
                                                             Dryer
          Heated Enclosure
         To
     Auto. Temp.
       Control
             Froph LN Tank
                                              GeneratfiC a
                                 Analysis SchematicOven
                   id Canister
—From
He Tank
July,
                               Page D  -  45/VC
-------
 ANALYTICAL METHOD
  VOLATILE ORGANIC CO
    COLLECTED ON  TENAX®"
GAS CHROMATQfiRAPHY/MASS
  INATION OF
 Cs) IN AIR
 .YZED BY
IMETRY  (GC/MS)
-------
                             SECTION 2
2.1

2.2

2.3

2.4

2.5
            ANALYTICAL METHOD FOR THE DETERMINATION OF
             VOLATILE ORGANIC COMPOUNDS (VOCs) IN
                COLLECTED ON TENAX® AND  ANALYZED
           GAS CHROMATOGRAPHY/MASS SPECTROMETRY (0C/MS)
                   TABLE OF CONTENTS


INTRODUCTION

SAMPLE STORAGE AND HOLDING TIMES  .... ^	6

CARTRIDGE PREPARATION AND CERTIFICATION .  / ./	6

GC/MS ANALYSIS OF VOLATILES FfcQM TENAX®yCAR^RIDGES  	 15

PERFORMANCE REQUIREMEMTS FOR DEMONSTBATINGSMETHOD ACCEPTABILITY
FOR THE ANALYSIS OF AMBIENT AIR .  .  .  >\ . /N^	53
-------
                                   SECTION 2
                                                      IN
            ANALYTICAL METHOD FOR THE DETERMINATION,
            •VOLATILE ORGANIC COMPOUNDS  (VOCs)
                COLLECTED ON TENAX® AND ANALYZED
           GAS CHROMATOGRAPHY/MASS SPECTROMETRY
2.1   INTRODUCTION
2.1.1  Scope and Application
      2.1.1.1  This document describes a methou for determining the  presence
      and concentration of specific volatile/organic compounds  (VOCs)  in
      ambient air.  VOCs for which this metbiod/is appropriate are  identified
      in the Target Compound List (Exhibit/C) /and in T4bL6  D/VOAT-  1 of this
      Part.  The method is based on the c/lla^tion of'vO/Cs  on Tenax® solid
      adsorbent [poly (2,6-diphenyl phenylene oxi.de/]./The collected VOCs are
      thermally desorbed and analyzed by gas^-vQhromatography (GC)/mass
      spectrometry (MS).

      2.1.1.2  While this method outlines the use of Tfe«4x® a"5k  the  adsorbent,
      alternative adsorbents (e. g./~~rrraitib_ed) will be allcJwed/   The  Laboratory
      must demonstrate audit accuracy and rep!i^ar6«-4irec:Lsion limits of the
      alternative adsorbent as well aSTa^Sw^hent: characteristic data for
      selected analytes in order for\it\to be e^}uiVa4e*!£_j;4ee part  2.5).   In
      addition, the analysis of Performance Evaluation  (PE)  samples  must meet
      required audit accuracy and replr^ate\precision limits as outlined in
      part 2.5.  They are:
                  Audit
                             30 perceVt;

                                within SL 30
                                                   ercent.
2.1.1.3  These acui
acquired over
System (TAMS) .   Tjrfe TAMs
distributive /air Volume
proximity,
help address breakthrough,
methodology.
                       Volume meth
                  were based upon data
                USEPA's Toxic Air Monitoring
               ,dsorbent tubes as part of the
  'dology.  Tslir tubes are arranged in close
 fferent air volume through the resin bed to
artifact formation and biases in the sampling
                 (GC/MS) i
             rs  as the coecno
             r which precision ani
                 on 2) method
                      knowin
      2.1.1.5
                              r to? Exhibit D, Section 1
                        >n of Vcfiatile Organic Compounds  (VOCs)  in
                          s Steel  Canisters" in that the same analytical
                            Exhibit D, Section 1 uses-Summa® polished
                            mechanism and has been validated for forty
                             accuracy have been fully defined.  While
                            been validated for a larger number  of  VOCs,
                            understanding its many limitations.

                     is/designed to allow some flexibility  in order to
July, 1991
                                                            Page  D  -  1/VT
-------
Exhibit D
                                                      SOW No.  XXX -  Ambient Air
      accommodate procedures currently in use.  However,/sucft  flexibility also
      places considerable responsibility with the user to  document  that such
      procedures give acceptable results (i.e., documentation  of method
      performance within each laboratory situation  is/requiriad) .  Each
      contractor must generate standard operating pr/ce^ses  (^©•£s)  describing
      specific stepwise instructions for the Tenax^pr/para^tl^m  amKhandling
      as well as the analytical procedures.  SOPs ^sho/uld be reaclily available
      to and understood by all involved personnel
                                         procei
      2.1.1.6  This method is based upon
      Environmental Protection Agency, Atmosp,
      Assessment Laboratory, Research Trian
      "Standard Operating Procedure for the/GC>
      Organic Compounds Collected on Tena:
      determined by this method are nonpotur^ org
      the range of approximately 80 - 200°C.
     developed by the U.S.
             and Exposure
             outlined in
           fation of Volatile
Compounds/which can be
         .ving boiling points in
        not all compounds
      falling into this category can be determine"^.  Exhibit C  and Table
      D/VOAT- 1 of this Part list the target compourftisto^B^analyzed by  this
      method.  Other compounds (e.g., semi-polar) may ytedd satisfactory
      results but validation by the/~lnthtvidiial user is requited.
2.1.2  Summary of Method

      2.1.2.1  Ambient air is drawn thXpugk
      approximately 1-2 grams of Tenax®\
      compounds and most inorganic atmospheric
      cartridge,  certain organic, compounds
      2.1.2.2  After the
      cartridge is tagg
      2.1.2.3  Upon
      the lab book
      are stored un
                                           are\trat
                                           ack
                                                  orbent cartridge containing
                                                 ighly volatile organic
                                                onstituents pass through  the
                                                rapped on the resin bed.
    3ed on the resin bed, the
       lab for analysis.
                                                 ,e cartridge  is  logged  into
                                                 completed.   The cartridges
                                   'n until analysis.
      2.1.2.4  Prior to analysis^fey GC/MS,  an internal standard  is added  to
      permit quantitative analysis/"XThe organics trapped on the Tenax® are
      thermally/
-------
Exhibit D
                                                SOW No. XXX - Ambient Air
      2.1.2.6  The scan of  the mass  spectrometer is initi^tecj and the
      analytical procedure, is begun.   Under a flow of heiiup,  the GC column is
      programmed to a temperature  to  allow the elution yof /ll of the organic
      compounds while the mass spectrometer is scanning.  A)ata are recorded by
      the computer for subsequent  processing.   Quant^tation^is performed by
      the method of relative response  factors,  where; th^proporSs^onate system
      responses for analyte and standard  are deterniinsti prioXto tha analysis
      of the sample and this relative  system response/ is  used tbxdetertiwjie the
      quantity of compound present on  the  sample

      2.1.2.7  Components are identified  in a /computerized library search
      routine, on the basis of the GC  retention /time and/mass  spectral
      characteristics .

      2.1.2.8  The quantitative analysis  £s  performed' by/ a combination of
      manual and computerized procedures: \the ctMjjpj/ter/ is instructed to seek
      characteristic ions in a previously  deb&rmined retention window.   At
      this point the operator intervenes  to  determine rf\the  compound of
      interest has been located correctly.   If the  campounoVxidentif ication is
      correct, the computer then performs  the  quantitative calculation using
      the method of relative resporise~~f3e-fcor_s_.^ Data are  re"pyartifacts can arise from
                             dants in the sample, degradation of the
                        rations of certain volatile organic compounds.
                      solve< by running blank and control samples prior
                                ampling volumes.
2.1.3.2/ Ex£»»&iJieconbentratibus/of water vapor on high humidity days
may cause/some changes in\ retention properties of Tenax®.  In general,
this/can/be minimized >V multiple sampling volumes, smaller sampling
volumes/ and the use ofYes\ccants in the culture tubes used for
st0raj
  x.
2.1.
interest
be extreme!
               Cof
                  a c
               ination c/f the Tenax® adsorbent with the corapound(s)  of
                  ionly/eno6untered problem in the method.  The user  must
                      .n tme preparation, storage, and handling of  the
                    :are
July, 1991
                                                           Page D  -  3/VT
-------
Exhibit D
                                                      SOW No.  XXX - Ambient Air
                                                                                   /""'N
      cartridges throughout the entire sampling  and  anaLysig  process to
      minimize this problem.  Otherwise,  false positive/detection of
      chloroform, toluene, benzene, and other common Volatile organics may
      occur.  Precautions should be taken for sampling caus^c atmospheres
      which contain levels of NOX and molecular halc/gen^greate^than  2-5  ppm
      and 25 ppb, respectively.
                                                                           jown
2.1.3.4  Breakthrough volumes  of  the  compoCMa^s'  of interest
or determined prior to use.  Breakthrough: vo/lumes for  some c
(i.e., vinyl chloride, chloroform etc. )/mav/be  so small that
quantitative collection is  impractical/  Other  characteristics of Tenax®
which may adversely affect  its preparation and  usfe in  this method are:

            Poor desorption of highly p^olar compounds;

      •     Possible retention of oxygfe*u  leading to sample oxidation;
            and
                  High benzene background due to manufate^urin|

      2.1.3.5  Tenax breakthrough/volume also Tnrvba»ocesthe linear range of
      the method,  detection limits\ an^"~repre
-------
Exhibit D
                                                      SOW No.  XXX -  Ambient Air
                                                                      eratures
2.1.4  Definitions.

NOTE:  Definitions used in this test method and any usat-prepared SOPs should
be consistent with ASTM Test Methods D1356, B260, and/E35lC   All  abbreviations
and symbols are defined within this document at the point

      2.1.4.1  Cryogen:  A liquified gas used to
      (-150°C) in the cryogenic trap of the analy
      cryogen is liquid nitrogen.

      2.1.4.2  Dynamic calibration:  Calibration j6f an analytical system with
      calibration gas concentrations that are; generated/£tw a  dynamic,  flowing
      system, by metering known volumetric flow/rates of concentrated  gas
      standards and zero gas into a common/in]/et line/to ,che  system.
      2.1.4.3  MS-SCAN:  The gas chromatog^saDh
      selective detector where the instrument"
      mass data for the target compounds and to
                                                    'is/coupled  to  a mass
                                                 progi^ammed  to  acquire all
                                                   ;regar<.all others.
      2.1.4.4  Deuterated compounds:
      (hydrogen isotope that is
      for system quality assuranc
                                      Those chemicals wn~ich contain  deuterium
                                                  hydrogenjNised as  tracers
of
      2.1.4.7  Relat
      chemicals for/th
      where the den
      chemical.

      2.1.4.8  Bre_ak£hrough vi
      particul^Tcomponen~6\will
      Tenax®
      2.1.4.5  Static calibration:  &alf
      known concentrations of calibrate
      gas cylinders or prepared from

      2.1.4.6  Retention ti
      from a chromatograp^c colunf
      measured from the
      until its maxim-
                                                           tical system with
                                                  tained from a source such as
                                                'ock solutions.

                                                 elute a specific chemical
                                                   carrier gas flow rate,
                                                   ed into the gas stream
                                                   e detector.
                                                 itio of RTs of two different
                                               4lumn and carrier gas flow rate;
                                 ?4nts the retention time for a reference
                                          Sample volume at which point a
                                   .initially detected in the eluate from the


                                   (SR):   The quantity of a component measured
                                  . known quantity of an isotopically labeled
                                  into the same Tenax® cartridge.
July, 1991
                                                                 Page  D  -  5/VT
-------
Exhibit D
                                               SOW No. XXX  - Ambient Air
2.2,  SAMPLE STORAGE AND HOLDING TIMES

2.2.1  Receipt of Exposed Cartridges

      2.2.1.1  Receive all exposed Tenax® cartridge
      the appropriate Chain-of-Custody sheet.  Mat
      Sheet with the corresponding sample to ensure

      2.2.1.2  Check each Chain-of-Custody Sheet  carefully  for  the
      items:  1) a signature of a person relinquishing custody,   2)  the
      amounts of surrogate loaded on the cartridge,  3) the  sampling
      temperature and volume collected, and/U) /the Tenax® $atch number.   Do
      not analyze any sample for which Cha/n-or-Custody  s^eet or  any of  the
      above information is missing.

2.2.2  Procedures for Sample Storage

            Put all cans of samples in the cartridgexfreeze-rwhen received,
      and log each sample in the appropriate notebook as^recelved.   Place each
      Chain-of-Custody sheet in th^~prt>j-ac£^notebook (witn^a^Z  other
      information regarding that /articular samp±e-)-^af_tersigning and dating
      it, and store any used cartridge^iir~s«Aied cans so~^hey  can be
      recycled, cleaned, and used againN

2.2.3  Contract Required Holding Times

            Analysis of airsamples must be\completed within 14 days  of  the
      validated time of sample receipt (VTSR\.
2.3
CARTRIDGE PREP/
AND CERTQ
[ION
2.3.1  Apparatus and/Materials

      2.3.1.1  Tena4® Cleaning/

            2.3.1.1.1  Exbractiok^thimbles:   Cellulose  (60 mm x  180 mm).

            2. 3^71.2 """Stschlet e^cractlen  apparatus:  Extraction flask and
              V18£L-ffiauextraction  thrrabl^s,  Fisher  Scientific, 711 Forbes
            /Ave/fue,  Pitts%urgh\ PA,  15Z19,  or equivlaent.

             /3.1.1.3  CondenkerA

                       Tweezeri.

                  . l^Reake/ -A 00 mL.

            2. 3 .1.1-V-x.Variab/e  transformer.
 July,  1991
                                                            Page  D -  6/VT
-------
Exhibit D
  SOW No. XXX  - Ambient  Air
            2.3.-1..1.7  Heating mantle for 1000 mL flask.

            2.3.1.1.8  Mettler balance:  Type H15 for
            Scientific, 711 Forbes Avenue, Pittsburgh,
            equivalent.

            NOTE:  All glassware must be cleaned
            hour in Amway SA-8 laundry compound,
            several rinses with deionized water
            four hours at 500-550°C.

      2.3.1.2  Tenax® Drying

            2. 3'. 1.2.1  Desiccator with gas,
            (Drierite).

            2.3.1.2.2  Jar,  wide mouth amber.

            2.3.1.2.3  Crystallizing dish, Kimax®.
        ing Tenax®, Fisher
        15219, or
            2.3.1.2.4  Vacuum oven/equipp
            to water apparatus va
            Avenue,  Pittsburgh, PA,
dry ice ^s^p and connected
     Lentific, 711 Forbes
            2.3.1.2.5  Aluminum foil.

            2.3.1.2.6  Funnel.

            2.3.1.2.7  Py/ex disks^N

      2.3.1.3  Tenax® Sieving (OpQio*
                     /  /        ;
            2.3.1.3.:

            2.3.1.3>2^ Sieves:/ 40'and 60 mesh.

            2.3.1.3.3  Gla>s^funn>
                ^-	--^
      2.3.1.4
              '   ^———    "\
                              g\oves.

                                 iglass wool:  Unsilanized.
                                 dipping cylinder:  17.8 cm x 1.6 cm O.D.,
                                /371856, Cincinnati, OH 45222.

                                  liners:  24 mm.
July, 1991
              Page D - 7/VT
-------
Exhibit D
                                                      SOW No.  XXX -  Ambient Air
            2.3.'l.-4.5  Stainless steel tweezers.

            2.3.1.4.6  Screw caps:  24 mm.

            2.3.1.4.7  Silicone septa:  Teflon®-ba9

            2.3.1.4.8  One gallon clean metal pa^bi
            Tenax® cartridges.

            2.3.1.4.9  Stainless steel tubes
            Co., P.O. Box 371856, Cincinnati

            2.3.1.4.10  Glass jar:  Cappe
            storage of purified Tenax®.

            2.3.1.4.11  Glass wool, silanized.

2.3.2  Reagents
                             cm 0.D., TEKMAR


                         -/fined screw cap.  For
      2.3.2.1  Tenax®, 60/80 mesh/(2 , 6_-dipheny
      TA - Alltech Associates, Inc
                           oxide polymer), GC or
                              rfield, IL 60015.
      2.3.2.2  Granular activated charcoa\:  For/preventing contamination  of
      Tenax® cartridges during storage .\   \/  /

      2.3.2.3  Acetone:

      2.3.2.4  Methanol:

      2.3.2.5  n-Pent

2.3.3  Procedures f>
                   {
      2.3.3.1  Cartr£
                 tion and Preparation
            2 . 3 . 3.. 1.1  Several car^s^dge designs have been reported in the
            1 i tjeiTaturTXThe mo^^commbn is shown in Figure D/VOAT- l(a) .
                        minimizes cb^aat of the sample with metal surfaces,
                              Decomposition in certain cases.  However,  a
                                 design is the need to rigorously avoid
                                 jutside portion of the cartridge since  the
                                 iected to the purge gas stream during the
                                 Clean cotton gloves must be worn at all times
                                 rtridges and exposure of the open cartridge
                       air mnstyoe minimized.
            2.3.3.1.
nd common type of design is shown in Figure
July, 1991
                                   Page D - 8/VT
-------
Exhibit D
                                                     SOW No. XXX -  Ambient Air
       D/VQAT- l(b).   This design eliminates the ne
       contact with the exterior surface,  since on^Jy
       cartridge is purged.

       2.3.3.1.3   Finally,  a third design has
       as  illustrated in Figure  D/VOAT-  l(c)
       adsorbent beds to capture the more  vo
       cannot  retain.

       2.3.3.1.4   Regardless  of the cart/id
       desorption module and sampling sy/te/ must  be selected to be
       compatible with  that  particular
                                                              avoid  direct
                                                            ie interior  of the
                                                              oped by Supelco,
                                                                 ains three
                                                                       Tenax®
                                                                          rmal
                                            -abridge
      2.3.3.2   Tenax® Purification
                                              .before/
                                                 ting  rt
      All Tenax®, whether new or re
solvent extraction and thermal treatmert
collection of organic compounds.  The f., _
followed (as illustrated in Figure D/VOAT-  5)
packed into cartridges:  1) selection of the Tena
solvent extraction using a  ^
sieving the Tenax®, 5) pac
thermally desorbing the Tena
the cleaning and desorbing procedure by &C
and storing the cartridges.  Al
as well as cartridge materials sh~
rinsing followed by an acetone rins
                                 (.ng
                                      irtric
                                          an<
             >e purified through
            it is used for sample
               tine shall be
                   .x® is cleaned and
                      used, 2)
   .action,  3) dryWg the Tenax®, 4)
                 cartridges,  6)
                 ig the integrity of
                is,  and 8)  packing
       used in Tenax® purification
   >e /thoroughly cleaned by water
     dried  in an oven at 250°C.
                                                      en
                                                   ensurij
     2.3.3.3  Tenax® Selection
           2.3.3.3.1 / T.
           record on/th
           D/VOAT-
           batch that
                     the
iax®,
                    Tenax®
                         sign a unique number and
                 Wo^sljsheet, as illustrated in Figure
f possi^le/new^enax®7should be taken from a single
       ce/tified cT&an by the manufacturer.
                  .as beer
      2.3.3.3.2
      Worksheet.
                       If tM T^nax® is new,  also record batch number on the
                       Ifhe Te^ax® is used,  record previous Tenax® blank
                                        ax® was used (i.e., fixed-site
                              orxersotvil air) .
     2.3.:
         Cenax® Cl«
                              Procedure
            The following adWAent purification procedure is based on U S
     Environmental Protections Agfency,  Atmospheric Research and Exposure
     As^essmint Laboratory (AREAL),  Research Triangle Park,  NC  Standard
     Opera^mg Procedure (SOP) .manual  entitled "SOP for Preparation of Clean
     Tenax® Ca^trid|B«".   I/eviAtions from this procedure should be carefully
     evaluated b>€p.re ihtp/em^ntation into the user prepared SOP.   Shorter
     1991
                                                                Page D -  9/VT
-------
Exhibit D
                                          SOW No.  XXX -  Ambient Air
      cleaning procedures of  the Tenax® have  been docume/ted'.   It is  the
      laboratory responsibility to provide  documentation tc/the variation from
      this cleaning procedure  to the Agency prior to  implementation into the
      laboratory SOP.

            2.3.3.4.1  In a hood, set up a  sufficient /numberxof
            extraction units,  each with a 1000  mL/rouhd flask  atxi a
            cooled condenser.  Load approximatelyx^Ty  g  of Tenax® i
            thimble and cover  the Tenax® with approximately  two centinffe4;ep£ of
            unsilanized glass  wool.

            2.3.3.4.2  Place the thimble in/the/Soxhlet<  aid 600 mL of
            methanol to the 1000 mL flask ^nd/carefully pur an additional  300
            mL of methanol onto the Tena*

            NOTE:  The 300 mL  of extra  methahol are added directly onto  the
            Tenax® to ensure sufficient solvent^Eqr tnex^xtraction process
            after the initial  adsorption of solvent>
                                           jr water  and
                                                irted
2.3.3.4.3  Turn on the
controlled heating ma^tle_and recor
date and time the extr
extraction cycle, adjustvthex tempeyatyfe'
transformer to obtain five, cyixles
extraction for 16-24 hours ,\che
daily and entering the info
             iperature
       Tenax® Worksheet the
            the first
          he variable
 hour.      Continue the
the extraction units twice
 the Worksheet.
            NOTE:  To avojt
            flowing to

            2.3.3.4.4
            methanol
            and let/it
            th imb 1 eC^w i th
            then retu:
                                          ition/on
                        losses, Vnsuke that sufficient water  is
                                   the system and discard the
                                    arefully pull out the thimble
                                    for 10 minutes.  Rinse the
                       lean n-pentane.  Repeat the rinse twice  and
                      e to the Soxhlet.  Discard the n-pentane.

                         tion do not handle the thimble with your
 July,  1991
                                      ^/*
                                 700 mL  of  clean pentane  to  the  flask.
                                  t and  heat  to reflux.   Record  in  the
                                 id time that the  pentane extraction began.
                                   adjust  the temperature to  obtain five
           Complete/the  information  on  the Worksheet  for  this
Tenax^xpatcnV^aTid idontinue  the  extraction for  16-24 hours.   After
extraction^ cool /che  system to  room  temperature,  remove the


                                                    Page  D  - 10/VT
-------
Exhibit D
                     SOW No.  XXX - Ambient Air
            thimble from the Soxhlet with a pair  of twee
            pentane.

      2.3.3.5  Tenax® Drying

      NOTE:  Obtain and fill out a Tenax® cleanup wjzfrk
      and time of each operation.
                          rs/and discard the
            2.3.3.5.1  Place the beak'ers contain
            desiccator at room temperature unde
            25 mL/min) through a cryogenic
            After at least 24 hours, transfe  tl
                   the  thimbles
                  slow  nitrogen  flow
                  remove  residual organics.
                 conten'Ssx.of  the two thimbles
            to a large crystallizing dish. /Coyer  the  dish/loosely with
            aluminum foil, set the dish in/the vacuum/oven and recharge the
            cryogenic trap with dry ice/^sopropanol  And/dry the Tenax®
            overnight at 100°C and slightVa^uum%e_/g./ -15 inches of water) .

            2.3.3.5.2  The following day turn off^^he  he^er and allow the
            oven to reach room temperature (about  3  rtaurs)  r>evfore opening the
            oven.  To open the vacuum oven, first  close  z>-ff the valve leading
            to the pump.  Connect /ChervTCrogen^line  to the  o-fcner valve
            connector on the vacuum o-wau^and slowIy~~tTHftB^j2£, the nitrogen flow
            with one hand while opening. tneva~bve  with the/other hand.  Ensure
            that the nitrogen is venbe^d 
-------
Exhibit D
                                                      SOW  No.  XXX -  Ambient Air
      2.3.3.7  Cartridge Preparation

            2.3,3.7.1  Place the Teflon® liners in a
            in methanol for 10 minutes, and rinse th
            methanol.

            2.3.3.7.2  Repeat the above with n-pe
2.3.3.7.3  Dry the Teflon® liners  i,
hours at 100°C and slight vacuum.
mouth jar, protected from light.

NOTE:  To avoid contamination
tweezers to handle the liners

2.3.3.7.4  Clean the silicone sept
                                                 and  sonicate  them
                                                  sith  fresh
                                                   le vacuum oven
                                                     the liners in a wide
                                                          lways use a pair  of
                                                        ibove procedures.
            2.3.3.7.5  Soak the 24-mm screw caps in m&thanolNfor 30 minutes,
            then remove the paper -linedfoil from the capTs^witj^ a spatula.
            Rinse the caps in cleaja methan»±--an4_dry them inN:he vacuum oven
            overnight at 100°C.
            2.3.3.7.6  Wrap the KimaxS
            secure it with clear tape
            bottom of the culture tube.

            2.3.3.7.7  Plac#--a~silicone  sept
            septum with a/cleaned TXfIon-
            tube with t
                                               uminum foil and
                                  e a' 4-cm glass wool plug at the
                                      the screw cap.  Cover the
                                        loosely close the culture
      2.3.3.8  Cartri
            2.3.3.8
            glass tul
                                   bes before packing.  Discard
                       ends or cracks.
            NOTE:
            is referre
                                     in a rack and insert a 4-cm glass wool
                                          and press the glass wool plug
                                         •el.

                               ^lass funnel,  transfer a known amount (-2
                                 le tube, using a glass funnel.

                                 tjher 4-cm glass wool plug into the other end
                              Lguife D/VOAT- 1) and lightly compress it with a
                    (stainless steel or glass) packed with Tenax®
                 'a Tenax® cartridge.
July, 1991
                                                    Page D  - 12/VT
-------
Exhibit D
                                                      SOW No.  XXX - Ambient Air
            2.3.-3..8.S  Store  the  Tenax® cartridges in th
            tubes until desorption.

      2.3.3.9  Tenax® Cartridge Pretreatment

            2.3.3.9.1  Place  the  Tenax® cartridge
            turn on the helium tank.   This  allows
            cartridge before  heating.
                                                  ipared culture
            2.3.3.9.2  Turn on  the  desorption
            nitrogen in the cryogenic  trap  ar
            desorption chambers.
                                                         unit and
                                                           from the
                                    open
                  liqui
   the helium line to the
                                                  place
            NOTE:  Insure that a cryogeni
            line to remove residual orga^ics>
                                trap has been/placed in the helium
                                   ander
            2.3.3.9.3  Adjust the helium  flo
            approximately 15 mL/min.,  then desor
            five hours at 250°C.  Make sure that he
            each cartridge throughout  desorption.
        chamber, to
  :he T>nax® cartridges for
           ^is maintained to
            2.3.3.9.4  Refill the^ryagenictrap wTch—liquid nitrogen every
            hour, or when the leve\or\liqul
-------
Exhibit D
                                         SOW No. XXX - Ambient Air
            choose to use GC/FID due to logistical and
            Analysis by GC/FID is accomplished as desci
            for the detector.
                                             jst/considerations.
                                            Lbe4 for GC/MS  except
            2.3.3.9.9  While acceptance criteria car( vary^depen4jng on  the
            components of interest and anticipated/coircentra^ionrevel, at a
            minimum, the clean cartridge should b£ demonstrate&xto contain
            less than one fourth of the minimum ytajjel of interestror eac
            component.  For most compounds, the/blank level should be^iess
            than 10 nanograms per cartridge irr omer to be acceptable.  More
            rigid criteria may be adopted, if necessary/^within a specific
            laboratory.  If a cartridge doe/ nor meet pnes/e acceptance
            criteria, the entire lot shoul/1 be/ rejected.
      2.3.3.10  Cartridge Internal Markei
                              ind
            2.3.3.10.1  Each sample cartridge mu"s£ be
            with 300 ng of perfluorotoluene (PFT).and
            prepared from a static dilution bottle tea
            3.6.3).   PFT serves as
            1,2-dichlorobenzene-d
            MS.
2.3.3.10.2  As a quality
cartridges must also be spiked"
standards (-300 ng) as indie.
and analysis.  TJie-^deuterated
markers can bemadded
vaporization/^ sae—Sectifc
or by the perme'ation
                        chlorob5mzefie-d5,  a
 Standards Spiking

 Antitatively spiked
           obenzene
           Section
       for the MS and
internal marker for the
                                                 dicator, all Tenax®
                                             th/three deuterated surrogate
                                               £ performance during sampling
                                                ate standards and internal
                                             ben  cartridge by either flash
                                                   dilution (see part 2.4.2)
                                                     part 2.4.3). They are:
      2.3.3.11  Supplying^vQartribes for Collection of Samples

                         l^epare "fet^e CHMji-of-Custody and Field Data Sheet  for
                              collected/  Remove and label the requested
                              irtridges from the Tenax® storage area.  Store
                             id Xanax® cartridges in the Tenax® storage area
                                one Tenax® batch number has been assigned per
                               from same batch for all the field and duplicate
 July,  1991
                                                     Page  D  -  14/VT
-------
Exhibit D
                                                SOW No.  XXX - Ambient Air
2.4*   GC/MS ANALYSES OF VOLATILES FROM  TENAX® CARTRIDGES

2.4.1  Summary of Method

      2.4.1.1  This section includes  a  description o
      associated procedures for GC/MS tuning,  chara
      of the GC/MS calibration procedures,  and an
      cartridges.
2.4.1.2  The analytical system  is compris4d
spectrometer set in the full scan mode
automatic, repetitive analysis.  The s
data for the target compounds.  The Cpnt
Limits (CRQL) range from 1 ng to 50 iig
analytical precision of about 5 percent
Concentration of compounds based upo1
table is reported by an.automated data
quantitation is provided by this analysis.
                                                           system and
                                                             erformance
                                                                d Tenax®
                                                           equipped
                                                  mass
                          GC/MS is set up  for
                         is prog^uammed to  acquire
                         : Required Quantitation
                      . the fjill/scan mode  with an
                      elatii/e standard deviation.
                          xisly installed  calibration
                      ^iuctioQ program.  Primary
      NOTE:  Considerable variation from one laboratory^fco  another  is  expected
      in terms of instrument config^u7a^ToTh~~-_Xherefore,  each^laboratory  must
      be responsible for verifying' thit__their partltttiar__svstern yields
      satisfactory results.  Part 2\5 o^scusSfe^specific performance
      requirements which must be met\
      2.4.1.3  GC/MS analysis is based
      relative abundances of target ions.
                                          Jination  of retention  times  and
                                         Se qualifiers are stored on the
                        scan m
hard disk of the GC/MJ
each chromatographi,
searching any GC/
such ion abundani
defined as an S
be available t
specified tim<
compounds,  so
sample spectra
recent) release of tf
(NIST) MassSnectral
The data/system mus
been e
quali
rete
ab
ai
wf
dete
reported
analysis,
an experienced
             and are applied for identification of
  peak.   The computer must have software that allows
           for ions o!£ a ^pecified mass and plotting
  tersus fiimfe^or>sund.  The acceptance level for relative
          to be within ± 20 percent of the expected
         ils any of the qualifying tests is flagged
          ta are manually examined by the analyst to
          flag and whether the compound should be
          this adds some subjective judgment to the
       ed identification problems can be clarified by
       Manual inspection of the quantitative results
July, 1991
                                                          Page  D  -  15/VT
-------
Exhibit D
         SOW No. XXX  - Ambient  Air
      is also performed  to verify  concentrations outside/the'expected range.

      2.4.1.4  A block diagram  of  the  typical  GC/MS sy^tenCrequired for
      analysis of Tenax® cartridges  is  depicted in Figure IvVQAT- 2.  The
      thermal desorption module must be designed to/acc/imJttQdate^ehe specific
      cartridge configuration used in  the  samplingyprotocol/X^teelNoj: nickel
      metal surfaces should be  employed.   The  voli^e/of tubing
      leading from the cartridge to  the GC coli
      areas must be well-swept  by  helium carrie/: gis.

      2.4.1.5  The GC column inlet should  beycapble  of Ke-«ig cooled to 10°C
      and subsequently increased rapidly to/appytoximately /0°C.   This can be
      most readily accomplished using  a GC/equ/ipped wyth -/n automated
      subambient cooling capability  (liquid ni-trogenVs  aithough other
      approaches such as manually  cooling  che
      cotton swab containing liquid  nitrogen ma  be a
           the column with a
          :eptable.
      2.4.1.6  The specific GC  column  and temperaturexgrogr^m employed will be
      dependent on the specific compounds of interest.   jfeppropMate conditions
      are described in Table D/VOA7^27~Tn-~geaeral a nonpola^/stationary phase
      (e.g., SE-30, OV-1) tempera t^re ^a^^ammed~T?oTn--3X^tp_ 245° C at 4°/min
      will be suitable.
      2.4.1.7  The relative  response  factol
      calibration standard analysis is used
      the sample.  Secondary ion  quantitatxion
      sample interferences uith~<^ie primary^
      quantitation is performed,  document
      The area of a  secondaryTbTi cannot be su
      primary ion unles/s  a/relative respo~T^e facN
      secondary  ion.
      from the daily continuous
    'alculate the concentration in
   s allowed ONLY when there are
ion\  If secondary ion
      ons in the SDG Narrative.
    tibuted for the area of a
        is calculated using the
      2.4.1.8  The riroc&dure  attfemp/fcs  to quartt^fy peaks which have been
      qualitatively^identrf^ed/  Quantitation is based on integration of the
      SICP  of  a  quantiTfea4y.on  massr or primary ion for the compound.  This mass
      has been previously fralectedsfor each compound based on its spectral
      uniqueness/Jjitejasity,  and lacks^pf potential interferences from known
      coeluting^compounds^^Currehtly  u^wd masses are listed in Table D/VOAT-
        5  for /Dotb-TJrlmaEy and\secondaTSY/ions .
 2.4.2
                              'cartridge:   Sampling cartridges consist of 13.5
             x rtJU mm Oorosil/acaife glass with polished-flat end surfaces.  One
             end is^&tchea^Vith/an I (inlet) and the other with an E (exit).
             Stainlesss^eel cartridges (12.7 mm OD x 100 mm long) may also be
             used.  (see Ftgu^e D/VOAT- 1).   Cartridges must fit into the
 July,  1991
                    Page D  -  16/VT
-------
Exhibit D
                                          SOW  No.  XXX  -  Ambient Air
            thermal desorption unit.

            2.4,2.1.2  Glass fiber filters, 25 nun (opti,
            Sciences, 600 S. Wagner Rd, Ann Arbor, MI
            2.4.2.1.3  Forceps.

            2.4.2.1.4  Lint-free tissues:  (e.g.,
                                                   Gelman
            2.4.2.1.5  Filter holder:  Stainles/
            accommodate 1 inch diameter filtei

            2.4.2.1.6  Cotton gloves:  For h4nc

      2.4.2.2  Sample Analysis
                                       eel or aluminum  (to
                                    .ing Tenax®/cartridges.
            2.4.2.2.1  Sample Desorption/Inje^&on Un
            thermally heating a Tenax® sample
            steel) for sample transfer into a suitaot&iGC/
            analysis.  The configuration of the thermal
            permit the enclosure ai?ara^l?cl-4^a_ting of the
            from room temperature <£o approximately
inert gas (helium) into\a
trap.  The cryogenically
to a preselected temperature (
allowed to sweep the sample
chromatographic column.  A sc
desorption/GC/MS^ee«£iguration
                                              Designed for
                                              lass or stainless
                                                 system for
                                              sorp^ion unit should
                                                  x® cartridge
                                             ijhile purging with an
            2.4.2.2.2  G
            capable of
            resolutio
            region e
            control
            spectra
            and storage^
            silica, 0.30
                                                 ly cooled /liquid nitrogen)
                                          d sarople/must~~th4n be rapidly heated
                                                  C) and a helium gas supply
                                                 trap onto the gas
                                           mat^c diagram of a typical thermal
                                                 wn in Figure D/VOAT- 2.
                     £og\aph/Mass Specrometer (GC/MS) should be
                                         ming, exhibit unit mass
                                    able of scanning a 35-300 amu
                               ,v?ith/tiata system for instrument
                                     data processing using
                       gorithms,  and historical library screening
                      olumn required for this method is fused
                        m, SE-30 or OV-1 coating.
      2.4.2.3
                                :n chambers:   TEKMAR Co., P.O. Box 371856,
                                  r NuTech Co., 2806 Cheek Rd.,  Durham, NC
July, 1991
                                                    Page D - 17/VT
-------
Exhibit D
                                               SOW No. XXX  - Ambient Air
                                                            25,  50,  100,  500,
                                                        x> contain at  least  two
                                                        maintaining 60 ±  5°C;
                                                               connected  to  a
2.4.2.4  Standards Preparation

      2.4.2.4.1  Static Dilution Bottle

            •     Two-liter round-bottom flas)
                  diameter glass beads and
                  magnetic stirring bar -
                  accept a screw-on Mining
                  P.O. Box 371856, Cincij

            •     Gas-tight glass micr/
                  1000, and 2500

            •     Laboratory oven -
                  dilution bottles a

                  Drying oven capable of 3


            •     Helium cy
                  length of

            •     Vacuum syrin

                  Magnetic stirre
            2.4.2.4.2
                                                 saptum cap.
                                                 (see Figure D/VOAT-  3);

                                 ^crosyringes  - 5 , 10 , 50 , and 100 /iL for
                                        liquid standards  into flash
                                         s  -  25,  50,  100, 250 mL;

                         Helitun  cylinder  and  pressure regulator and needle
                         valves  for  controlling  flow  rate;
                         Flow meter  (i.e.,  soap bubble,  rotameter) ;

                         Thermal/conductivity  detector;  and

                        ^Vacuum syringe  cleaner.
 July,  1991
                                                           Page  D -  18/VT
-------
Exhibit D
                     SOW No. XXX - Ambient Air
            2.4..2.4.3  Permeation Tube System

                        Permeation system  (see Figure ^/V^AT- 4);

                        Nylon gloves;

                        Long glass hook  (for retrj/evi^g permition^ubes);

                  •     Permeation tubes;
                        Lint-free tissues (e

                        Stopwatch.
2.4.3  Reagents
      2.4.3.1  Nitrogen gas:  99.995 percent

      2.4.3.2  Helium:  Certified 99.995 percent,  ^w

      2.4.3.3  Neat standards:  C

      2.4.3.4  Spectrograde methan

      2.4.3.5  Spectrograde acetone:
      NOTE:   Individual
      manufacturer's deter
      standards should h
      NMR or direct prol^e
      checked by injec£io
      glass  capillary
      chromatogram
      observed and
      standard is
      GC/MS  to confirm"
      mass spectra.
2.4.4  Standard
             (or  standards must have  a
              percent or better, and  isotopic
                ^Purity should be checked by
                  fed by the  laboratory  is
                    using a 50-m SE-30 WCOT
             ilumn and FID.   The resulting
              Teaks.  If such peaks are
                 of the standard peak, the
  le  following chemicals are  also screened by
Lty of  the  compound by the examination of the
                                resents three procedures for generating known
                                 VOCs for direct injection into the GC/MS for
                                 ion on Tenax® for calibration of the entire
                                  icy are:  1) use of flash vaporization
                                 fted VOC standards upon Tenax® tubes, 2)
                                 trations utilizing static dilution bottles,
                                ube system for generating known concentrations
July, 1991
                               Page D  - 19/VT
-------
Exhibit D
                                                      SOW  No.  XXX -  Ambient Air
      2.4.4.2     The Contractor must provide all standa/ds/fco be used  with
      this contract.   The Contractor must be able to ve;rLf\/that the  standards
      are certified.   Manufacturer's certificates of a/al^sis must be retained
      by the Contractor and presented upon request.

      2.4.4.3     No  correction for impurities in
      manufacturer's  determined purity is 98 perc
                                            EP>
                                             needed if
                           standards may be usec
                          idit procedure.  Standards  on
2.4.4.4     Alternate methods of generati
equivalency is established through an
Tenax® may be stored for no more than

2.4.4.5  Flash Vaporization

      2.4.4.5.1  Summary
                  2.4.4.5.1.1  A dilute solution^af oneNjr more organic
                  compounds in methanol is injected i^nto a^feeated zone in a
                  helium stream.  The methanol and the ssdutepompounds are
                  rapidly vaporized/~anct--tkei^_s_wept onto a £o
instri
false ios
                        Contamination of a compound used as a standard will
                        resu/t in a decreased response.  Contamination of one
                              id with another one to be used in the same
                        solution will result in incorrect responses for both
July, 1991
                                        Page D - 20/VT
-------
Exhibit D
                                    SOW No.  XXX -  Ambient Air
                        compounds; and

                        Chemical reaction between two
                        mixture will result in low re
                        Absorption of a compound int;
                        particles will probably res
                        retained in the cartridge
                        consequent decreased res
                                         iunds  in a standard
                                            for both.
                                            rix of sorbent
                                                 it being
                                                    with
                  2.4.4.5.2.2  Chemical reactions /between compounds  cat
                  deplete them from the mixtu/e and might also result  in
                  unexpected reaction produces. /Use of/a\syringe for
                  consecutive injections fr/om  the same/botrcle without  cleaning
                  after each injection may/result in Erratic responses due  to
                  buildup of sample residues ^-in the ysyrifnge.  Rinse  individual
                  syringes with methanol and ace^ne arid dry in a vacuum
                  syringe cleaner for -30 sec^jds.  (/ heat gun is used to
                  heat the barrel of the syringe^during^-vacuum drying.)
NOTE:  Syringes mus
injection to remove
injection is ne^dec
syringe must be usec
may result in erra\
                                       be rigorously clamed ^fter each
                                             .of sample.  Evea if more than one
                                       rom any given—source a freshly cleaned
                                                injection?? Failure to do so
                                         esponges/
            2.4.4.5.3
                                vaporization unit, as
                  2.4.4.5.3^4 — Assemble
                  illustrated in Figure D/VCT-
                                                  low to 30 mL/min and the
                                                to flow for approximately 30
                                  'ibrate the system.

                                  ^volume of helium required to elute methanol
                                      ^idge is determined by using a thermal
                               directors  Several different flow rates are
                             nd one wh^ch results in as sharp a methanol peak
                               without sweeping volatile solutes out of the
                            ^efo^e it can be removed from the system.

                               Seh the helium flow to 30 mL/min and the heater
                               'C.j  Place a clean (see Subsection 2.3.2) Tenax®
                               Line, and pass helium through the cartridge for
                              5/minutes.
July, 1991
                                              Page D  -  21/VT
-------
Exhibit D
  SOW No. XXX - Ambient Air
                  2.4.4.5.3.6  Using a heated syringe,
                  individual standard flask an aliquot;
                  flushing technique.
      jtrfeve from the
     is Ing the solvent
2.4.4.5.3.7  With the aliquot of jftie /^b&ndaro>L;  and

                                       aliquot of this  solution would contain
                                 !.3 ng.

                    .4.4.^&.2 /Each compound is measured into  a 100  mL
                   volumetric /flask using a microsyringe.   The  flasks are
 July, 1991
              Page D -  22/VT
-------
Exhibit D
                                                      SOW No.  XXX - Ambient Air
                  .filled  to  the  mark with spectrographic
                  the contents mixed thoroughly.   Three/mi
                  solutions, when  injected into  the  fl/sh,
                  the manner specified  above, will de
                  ng of each compound on a sorbent cartridge
                  table above.   The  solution must
            gra&e methanol and
               •oliters of those
              •aporization unit in
              approximately 300
                .as shown in the
                       f a day.
      2.4.4.6  Static Dilution Bottle

            2.4.4.6.1  Summary
                  2.4.4.6.1.1  A quantity of/liquid orgi
                  injected into a two-liter/ro/nd bottom
                  through a septum cap.  Atte/ injections
                  flask is agitated and #eate< to acXie/e
                  vaporization.
            Lc compound is
            Xelium-filled flask
             are completed,  the
             complete
                  2.4.4.6.1.2  Aliquots of the rfesultirfg^vapor are  then
                  delivered to sorbent cartridges orxanalybical instruments.
                  The weight of each compound deliverer-is calculated  from  1)
                  the density of CnTTfrjttid^,2)the volume>a£^ liquid injected
                  into the known Voluiae__of theb~o£tie-T~_arid 3) the volume  of
                  the vapor aliquol
                  NOTE:  The quantity""
                  dilution flask must
                  would result in a partiv
                  pressure a€—ambient
                  aliquofcs inject*
                  positive zrtres-sure'l
                  flaslc must notVef
                  pre/
                    Chloro
                    3-Dichlor
                    4-Dichlor
ompound  injected  into  the
  .tially less  than  that  which
       equal to its vapor
  e.  Vaporization  of  li-quid
   ,le must not result  in a  large
      vapor aliquots from the
    :antial vacuum.  If these
Tatic responses may occur.
                                               ion bottle technique for
                                  rds has been validated for the following 22
                                        ane
                                  ene
                                  -2-butene
                                 butene
                              izene
  1-Ethenyl-4-chlorobenzene
  3 -Chloro-1-propene
  1,4-Dichlorobutane
  1,2,3-Trichloropropane
  1,1-Dichloroethane
  2 -Chlorobutane
  2-Chloroethoxyethene
  1-Methylethylbenzene
  1,3,5-Trimethylbenzene
  Butylbenzene
  l-Methyl-4-(l-Methylethyl)
  benzene
July, 1991
                  Page D  - 23/VT
-------
Exhibit D
                                   SOW No. XXX  -  Ambient Air
                .  2.4.4.6.1.4  Amounts  used have ranged
                  of liquid  samples.  Repeatability of
                  mixture of the  22 compounds into th
                  percent relative standard deviatio^
                  the substance introduced,  the
                  producing  the flask standard, a;
                  of the instrument used to analy
                  Accuracy has not been establi

            2.4.4.6.2  Interferences
                                          teen. 0.3  and 4 fiL
                                           injections of a
                                           is about  ±10
                                            >jLon  depends on
                                              tiyidual
                                                   operator
                  2.4.4.6.2.1   Contaminatio^ of' a compc/und/used as a standard
                  will result  in decreased/ re/ponse.  /Contamination of one
                  compound with another one us^d in the /same vapor mixture
                  will result  in an incorr«£t re^pcjnse/for both compounds.

                  2.4.4.6.2.2   Adsorption of vapois^inoleb^tles on the walls of
                  the bottle or on the septum will result rn^loss of material,
                  with a  consequent decrease in responses.  Thrfe is especially
                  likely  when  new,/ fresfriy— annealed bottles^are used.
                  Contamination o£ apparatus may~~r3^«*liLj.n_ adsorption loss or
                  provide unexpected s&urc~es~-r>£? compounds^n a mixture .

                  2.4.4.6.2.3   ChemicaSL react/onX between compounds can
                  deplete them from the Nmixteure/and might also result in
                  unexpected reaction products/  Use of a syringe for
                  consecutive— inflections from Che same bottle without cleaning
                  after each injection may re^ulc. in erratic responses due to
                  buildup of^s^3Bple\residues rn tw? syringe.  Rinse individual
                  syririges/with mfethlafioT>and acetpne and dry in a vacuum
                  syringe/ cleaner/ for -30 se^sojids.  (A heat gun is used to
                  heat $he barre/ of/the^syringe during vacuum drying.)
inj efc
                   rinse severs
                   at 300°C foi
             Wash the 2-L flask with detergent  and water,
              times with deionized water,  and dry in an oven
             4 ytiours.
                        .6.3y2  ,£lace 30 3-mm glass beads inside the  flask  and
                            an/analytical balance to an accuracy of 0.01  g.

                                Fill the flask with deionized water to  the
 July,  1991
                                               Page D - 24/VT
-------
Exhibit D
                                                      SOW No. XXX  - Ambient Air
                  level  of the  septum cap.

                  2.4.4.6.3.4  Weigh the flask contain!
                  water  on an analytical balance to at;

                  2.4.4.6.3.5  The  weight of the wa;
                  bottle  is the difference  between/
                  calculated below:
           e glass beads  and
         uracy of 0.01  g.
                  where:
                        Vf    -     volume/of/flask,  \fL, /
                                                           with beads and

                                                             with beads,  g.

                                                 \^
                  2.4.4.6.3.6  Two methods  have  been  use^to l)&ad the dilution
                  flask with organ^c~~coKp»Beiitsfor standard/  1)  direct
                  injection of eadh coanp_ound  separaTre4y_J.ntp the flask and 2)
                  a single direct rnjeXtiorT~of~^ previously' prepared mixture
                  of compounds.
                  NOTE:  These methods
                  indistinguishable resul
shown to produce
                                    jthod  involves\ injecting  each  compound (one
                                     ito the  flaskA The  flask  is  inverted
                                    itorfe~cTHLon wicfa/the  syringe  in  place  through
                                             £or  the beads to  remove  any
                                             the/syringe  needle.   The  second
                                               tng a master solution by
                                    mL of each component into  a culture  vial
                                 fch a septum cap.  After all the  compounds
                                   added,  the vial is agitated  to  produce a
                        homogeneous T^quid mixture.  The vial  is  then recapped
                          Ch a nefc^septum.   Aliquots of  this master solution
                             Amoved andyinjected  into  the dilution flask as
                                   the same manner as indicated above; and

                                   method involves retrieving  a clean, dry  2-L
                                 training  70  3-mm  glass beads and  flushing the
                                   helium for  a period of five minutes.   At
                                /f the flushing process,  immediately  cap with
                            
-------
Exhibit D
     SOW No. XXX - Ambient Air
                        volume of each  compound (one at ya t£me) or from the
                        mixture solution into the flask'while the glass beads
                        are agitated by the stirring War at the maximum
                        setting of  the  magnetic stir/er^ Invert the flask
                        after each  injection with the syringe in^place through
                        the septum, in  order for tKe jjeads
                        liquid remaining on the syj^/ge needle .
                        substances  have been inproJiuced,  place the fi^sk it
                        the oven at 60°C for 3y minutes to equilibrate/\»tore
                        the flask in the oven/at/€0°C until needed.  Bottles
                        are stable  for  one  wek^fter

                  NOTE:  The technique  of /injecting a/solution of targeted
                  compounds rather  than i^ndivrdual irijecrion of specific
                  compounds is preferred ifxmany syostamces are involved,
                  because  it is more rapid,  anti\the master solution can be
                  used over a long  period if it i^^refrigerated at 0°C.
                  Before use, the refrigerated solution is allowed to sit at
                  room temperature  fojrabout an hour.   rtxis recommended that
                  a total  less than 90  /UTTrf—liquid be injecTsed and a total
                  less than 20,00(\/iL\ei-^£as be remo"v
                  2.4.4.6.3.7  Remove\the\flas>
                  magnetic stirrer  for\app\p
     tEe~~"~o/ven and place on the
Cely 15 seconds.
                  2.4.4.6.3.8  Place  the  sVrin&e to be used in the extraction
                  procedure^-ln~^thfi oven at  cvO°C\to prevent condensation in the
                  syringe/during delivery.   Ufcing\the heated syringe, insert
                  its n#edlXthrfxugn\ the^ septuihyanji pump three times slowly.

                          .3.9  Af/er  ttie  thir>i-aump,  fill the syringe to
                        Amately 2.5 percenbxgrea/cer volume than needed.  After
                         jond pause / withdrawtne needle from the Mininert
                  se'p-tAim vkiye/  Flush the  excess sample from the syringe,
                  then  ocaw a  small quantity of air into the syringe to retard
                  diffusion^-of sample through the syringe tip.  The aliquot
                          must  tx useoxmmediately.

                                If  the-^sample is to be injected into a clean
                  sorbent cartridge,  the  tip of the needle is inserted to the
                  center of che s;orbent bed.  Then the plunger is depressed
                  over  a 10 second, period while the needle tip is being
                  withdrawn abput half the  distance to the end of the bed.

                      .4.6.3. ill. if.  the sample is injected directly into the
                              instrument,  injection is made in the normal
                     cmer vmless column-head freeze-trapping  (cryofocusing)  is
                  being\employed,  in which  case the plunger  is depressed over
                   about a :tW second  period.
 July,  1991
                Page D  -  26/VT
-------
Exhibit D
                                    SOW No.  XXX - Ambient Air
                .  2.4.4.6.3.12   If a sample is too large/to fie injected in one
                  step,  two  or  more injections may be mz.de J  This causes no
                  complication  for injection into a so/bem: cartridge, but
                  cryofocusing-must be employed when .multiple injections are
                  made directly into a gas chromatog/raph.

            2.4.4.6.4  Calculations

                  2.4.4.6.4.1   Volumes to be iryfr'&^uced into the
                  flask  are  calculated by working/backwards from the quantity
                  of material to be delivered/  JOT example,  if a 500 ng
                  delivery is needed,  it could iSonvenierfbiy be accomplished by
                  using  a 50 p.L syringe conraiping 10 /ig/j/L of compound.
                  Therefore:
50 /*L syringe x 10 ng/}il
                                                       500 ng
                  2.4.4.6.4.2   If  the  typical volum<
                  then to  get  that concentration (10
                  would have to adoZTTTfrS—mg_^of^ liquid com
                  The calculation(wo
                  = quantity of liaui
                  of 10 ng/>L.
                                       thexflask is 2.065 L,
                                              :he flask,  one
                                            id to the flask.
                                           10  ng/juL x 2.065 L
                                          flask concentration
                         10
                                  x
                              . 65 mg
                  2.4.4.6.4^3—-if the  density "bJ the solution was 0.9726 g/mL
                  (or 0.3726 mg//IhO,  then tKfe voi^ume of solution needed to add
                  to ther fLasTT-to maintain a oonceptration of 10 ng/AiL or a
                  deli/era*le  of\OQxfls~>wo.uld bV/21.23 /iL, as calculated:
                      2/.6S mg/0.9;
                               21.23
             It/is not practical  to  deliver  and measure
               microliter,  so,  in practice,  21 pL would  be
                  the deliverable would be calculated:   (21
                        mL  =  0.00989 mg/mL = 0.00989
                  fractions
                  used.
                     x 0.972^
                                This^s^/equivalent to 9.89 ng//iL,  so a 50-/J.L
                  injection  of\the  vapor compound from the static dilution
                  flask woulbd contain:   9.89 ng//iL x 50 ^L = 494.5 ng of
                  compound delivered
                enneation  Calibration Generator
                  2.4V4.7.1.]/  A permeation calibration generator is designed
July, 1991
                                               Page  D  -  27/VT
-------
Exhibit D
    SOW No. XXX - Ambient Air
                  to allow  the permeation  of  gas  through/Teflon® or other
                  plastic material  at  a  constant  rate im a/water bath at
                  constant  temperature to  generate  tear atmospheres.

                  2.4.4.7.1.2  The  permeation tube  fs ma~bXby scaling a liquid
                  chemical  in a tube made  of  some /ernreablemateria"^  It is
                  essential  that  the chemical be  in j£he liquid s-satero< the
                  permeation tube to operate  prc
                  chemical  is a gas at atmospheric
                  in the liquid state  under ics
                  in the permeation tube.  Ttfe
                  with a non-permeable plug
  Ly.   In many cas*
 'pressure,  but is
   saturation vapor pressure
je  is  sealed at both ends
                  2.4.4.7.1.3  Permeation/of ^ehe  pollutant vapor within the
                  tube occurs through the^axposea^s/dewalls because  of the
                  concentration gradient  thab-exists  Between the inner and
                  outer tube walls.  By passing oifferetvt flows  of diluent gas
                  over the tube, gases of varying concentrated on  can  De
                  generated.  If the tube is held at  a Constant  temperature,
                  the permeation r^te~~w±ii-~cgmain constantNv^By  measuring the
                  weight loss at mis^jjonstantteffipe^atiire over  a given period
                  of time, the per^athkorT~ra-Ce--may be determined.  The output
                  rate of the tube will\emain/4ss€nt±aiiy constant  until
                  nearly all of the lixmi\in/th.e/ tube has permeated through
                  the walls.  In generalx. pexme/tion  tubes can be used to
                  generate known pollutan\  con/entrations between 0.7 to 200
                  ppbv.
            2.4.4.7.2
                                              ^tion device  can be  used in the
                                               FES  permeation rate must be
                                    iermeatidtr-iate,  R,  is  determined
                                    In  essence,  the tube  is  weighed,  then
                                  jerature bath (±1°C)  for  a  period of time.
                                  ayed and reweighed.   This process is repeated
                                        calculate a permeation rate at that
                                              difference between initial and
                              Lght  (ng^yciivided by time (min)  determines the
                                :e  at that specific temperature.

                                                                   Eq. D/VOA-2
                               Permeation rate,  ng/min;
                               Weight  change,  ng;  and
                               Time, minutes.
 July,  1991
               Page D - 28/VT
-------
Exhibit D
                                     SOW No.  XXX -  Ambient Air
                  2.4.4.7.2.2  The  permeation rate can be ,£al£ulated either
                  manually, as shown  in  the  above equati/on./or recorded
                  automatically.   At  different  temperaure/,  different
                  permeation rates can be  calculated.

                  2.4.4.7.2.3  Permeation tubes  shouZd bekept
                  temperature  specified  by the  manufa
                  Changes  in temperature as  smal^>as  0.1°C can sigrtificantsLy
                  affect the permeation  rate.  /Tubes  should initially
                  allowed  to equilibrate for 2U hours.   After small changes in
                  temperature  (1 to 5°C) ,  th/tube shoul^Kbe  allowed to
                  equilibrate  for  at  least )(aly an houj

                  2.4.4.7.2.4   A permeation  tfube  system/has been developed for
                  application  of loading Rtxown  s-fc^n/lards onto Tenax®
                  cartridges for use  in  deteruuming tWe  relative response
                  factor and the column  performahce^ evki^tion (CPMX)  of the
                  GC/MS-COMP system in conjunction wi^h  thexfJLash vaporization
                  system.

                  2.4.4.7.2.5   In
-------
Exhibit D
                                   SOW No. XXX  - Ambient Air
                  2.4.4.7.2.8  The following routine shoi/ld/fce  followed when
                  Tenax® cartridges are loaded with deu/tera/ted  standards via a
                  permeation system:   1) determine th
                  be loaded, 2) select the permeatio
                  loading conditions  to be used, 4)
                  load the cartridges, 6) calculat
                  loaded, 7) ensure the integrity^of
                  and 8) pack and store the
                                         er of cartridges  to
                                    tubes>\3) determine  the
                                                  system,  5)
                                                  pmpounds
                                                     iire,
                          cart;
                        Obtain a copy of the
                        Monitoring Coordinat

                        Determine the numb
                        external standard:
                        objectives;
                                                   from  the
                                         standards and
                                       tisfy the sampling
                        Check the permeation noteb<
                        laboratory) to see which
                        available £6T~t&e^£ieeded standards
                               perme
                              ted in the
                                 es are
                                'A
                        Select onlV ttifc
                        rates are stable
                            ;ion tubeswhose permeation
                  NOTE:   A permeation rkte Xs7 considered stable when the mean
                  permeation rate has a coefficient of variation (CV) of less
                  than 10 percent.  The mean permeation rate is calculated
                  using theiast riye indiviHualNpermeation rates.  Do not use
                  penneatfionx-trities with permeation\rates below 100 ng/min or
                  above/1 ?/105

                        (n a bound ncr€eBo<}k assigned for the specific project,
                       ^prepare/a t/ble includjing:  1) the numbers of the
                                 be used,  2) the names of the compounds, and
                                  rresponding mean permeation rates.
            2.4.4.7.3  Calcul
   ^.7,
to be
formula:
:ions

 For
\onto  a
                                       Compound, calculate the amounts needed
                                      fenax® cartridge using the following
                                     P x t x
                                                                  Eq.  D/VOA-3
                             /Amount loaded of compound onto Tenax®  tube,  ng;
                              Permeation rate of specific compound,  ng/min;
July, 1991
                                              Page D  -  30/VT
-------
Exhibit D
                                    SOW No.  XXX - Ambient Air
                              Total  time of  loading  of coppoytnd onto Tenax®
                              tube,  minutes;
                              Flow rate through  the  Ten^x®/cartridge,  mL/min;
                              and
                              Exhaust flow rate,
                  NOTE:  The four variables G, t,
                  loading conditions.  Any three
                  one calculated from the equat
                  2.4.4.7.3.2  The following Restrictions must be  followed to
                  minimize error:  1) do not /load for leysXthan  two minutes,
                  2) do not load with a cartridge flow /beLow  50  mL/min  or
                  above 150 mL/min, 3) do yot/operate/the/system with a total
                  flow below 250 mL/min.
                  2.4.4.7.3.3  If the GC/MS syst&aneedsxto operate  in the
                  range of 200-500 ng per analyte, then thV>analyst  must
                  generate standards concurrent with thax^rangjs.  Fixing three
                  of the four vari^bTe3~-o£-ttieabove equation/will enable
                  calculation of l(he needed loadiiTe-&ato the Tenax®  tube.
2.4.4.7.3.4  As
provided to assist tl
parameters of the pei
standards on QA/QC

OBJECT!
cartr

GIV
                                                          !g calculations are
                                                 'determining operating
                                                fube system in generating
                                                    and chloroform onto a
                                                    per analyte.
                                                te
                                  0 ng/min for chlorobenzene
                                  .0 ng/min for chloroform
                                  0 ng/min)(4 min)j x [(80 mL/min)/(80
                                  in+F2) ]

                                f270 ng/min)(4 min)(80 mL/min)]/200 ng}
                              mli/min

                              352 mL/min
                                                       - 80
July, 1991
                                              Page D  -  31/VT
-------
Exhibit D
                                                      SOW No. XXX - Ambient Air
                  Now, since all tubes are  in the permeation7device together,
                  the flow.(F2) for chloroform will be  T52 /mL/min.   Therefore,
                  the loading on the Tenax<8> tube  for  chloroform must be
                  calculated to verify that it  falls/withinta^e 200-500 ng per
                  tube loading.

                                  Chloroform
      G -    (P)(C)[F1/(F1+F2)
      G =    (520 ng/min)(4
            mL/min)]
      G -   385 ng

All values obtained are/wit
                                                   (80  mL/min)/(80 mL/min + 352
                  NOTE:  Permeation tubes may
                  materials.  The following
                  in a properly ventilated glove
                                                       cc^eptable range.
                          proc
                      oxic or carcinogenic
                        puld be carried out
                              Wear nylon
                  gloves when handling permeation  tubes:
                  2.4.4.7.3.5  Locate J^iechambe?s~~-i»--3diich  the selected
                  permeation tubes\re\sto1ceTh—7With a  long?glass hook,  remove
                  the selected permeatioh tubes/ fr/6nrthe--&torage chamber and
                  transfer immediately\to\he /loading chamber  of the
                  permeation system.   \  \/  /

                  NOTE:  Wheji-a>-~cartridge iS not: being  loaded,  a dummy
                  cartridge is plafeed in theNLoading position.

                                                    to  the side where the
                         ^artridgej will be "fovadedvand allow  the system to
                        Srate for/90/miniites before loading  cartridges with
                       inerated /tes£ atmospheres.

                               DiX/ert the nitrogen flow to the  side  that will
                              forxj-pading cartridges and insert the  Tenax®
                                 theXihamber.
                  test at
                       stopwatch  and  immediately direct the
         nsphe^res gas flow through the cartridge.
                  2.4.4.7.3.
             Ca
                  desired as folL
tculate  the time needed to load the amounts
 rs :
                  pern
                        ition
                                 >P)
              ie calculation only  on  the  compound whose
            zfube has the highest or lowest  permeation rate.
July, 1991
                                               Page D - 32/VT
-------
Exhibit D
                                                      SOW No.  XXX -  Ambient Air
                  2.4. A. 7.3.10   At the calculated  time , k. otite  the  two
                  stopcocks to direct gas flow away fron/th/e cartridge being
                  loaded.
                  2.4.4.7.3.11  Handling the cartridge with^a^Kimwipe®,  remove
                  the cartridge and return it to its cuTbire tube^.  Seal  the
                  tube, then label with the follomng/informa>and 3) the date.
                  2.4.4.7.3.12  Prepare a Chafr-
                  information concerning

      2.4.4.8  Storage of Standards in Car/

            2.4.4.8.1  Secure the cartridg
            glass wool plug to avoid breakage^
            deuterated standards, label the top
            following symbol: D*.

            NOTE:  * The star indi.
            loaded onto the cartr
            participant's code.

            2.4.4.8.2  Store the carti
            freezer until they are ready\to'

            2.4.4.8.3  For
            cartridge usirig the ge
                                                  :-Custody sheet with  the
                                                          Che tube.
                                                        Imax® tube with a
                                                      xansport.  For
                                                         jew cap with the
                                                              .rds have been
                                                         also be added to the
                                                 sealed paint can in the
                                                ent to the field.

                                                late the amount loaded onto a
            2.4.4.8.
            use in

2.4.5  Instrument

      The instrume
Tenax® sampli
desorption c
analysis.
approximat
should be/10 /mL/min
be coole/i wi£h liquid nitrogen
                                                tion tubes to the GC/MS for
                                      ie analysis of volatile organics on
                                          Table D/VOAT- 2.  The thermal
                               port Va^fo valve are maintained at 250°C during
                                 is set to scan the mass range from
                                 ;lium purge gas through the desorption chamber
                                  capillary trap on the inlet manifold should
July, 1991
                                                                Page D  - 33/VT
-------
Exhibit D
                  SOW No. XXX  - Ambient  Air
2.4r6  Instrumental Analysis

      2.4.6.1  Initial Start-Up
            2.4.6.1.1  Prior to instrument calibrate
            helium purge flows (through the desorp
            flow to the GC/MS are set at approxi
            mL/min, respectively.  If applicable
            set at 2-4 mL/min.

            2.4.6.1.2  After the column and
            assembled, condition the column
                              analysis,
                                  ier gas
            2.4.6.1.3  The MS and data sy
            manufacturer's instructions.
            300 amu, the scan time should be
            not to exceed one second per scan.
            general operating conditions for the

            2.4.6.1.4  Once the en
            should prepare a detai
            the operation of the s

            2.4.6.1.5  Turn on the powl
            line pressures for the foil

                  •     Helium:
                        mponents are
                         the manufaturer.
            2.4.6.1.6
            should

            2.4.6.1."
            set manifol
            temperature to
             60 psig
                psig
             30/psig
                   according to the
                      should be from 35 to
                    ive scans per peak and
                      PAT- 2 outlines
                           et up, the user
                      procedure describing
                         sed.

               ss-flow controllers and set
               desorption and GC system
             nstrument requirements.

master power switch to the chromatograph,
  to 105 ± 5°C, and set source ionization
July,  1991
                             in the^power^to the thermal desorption unit and
                          atur^s for the valve, trap, and transfer line on the
                                 control box of the thermal desorption unit
                         manufacturer' s specification.  Typical values are:
                                    275°C

                                    250°C
                                    210°C
                             Page D  - 34/VT
-------
Exhibit D
                                                SOW No.  XXX -  Ambient Air
                                                            .t is  cold and the
                                                           Lng helium through
                                                                   reducing
                                                                  irmal
2.4.6.2   Thermal Desorption of Tenax® Adsorbent Tu

      2.4..6.2.1  Initially, the thermal desorptio
      Tenax® cartridges are placed inside while
      them.  This allows oxygen to be purged fr/m
      oxidative degradation of Tenax®.  Then,
      desorption cycle, helium gas continues
      cartridge to purge the organic vapors anaXyte~~aRd/standard are
            determined prior to the analys\s o/f the sample and this relative
            system response is used to oatermlne/the quantity  of compound
            present on the sample cartridg

            2.4.6.2.4  The/followihg outlines\typ\cal steps associated with
            thermal desozptLatTTislngV the NuTecPk device.   They  are presented as
            a guideline/to/follow yherTTIs-inE thi^/or similar equipment.

                        Remove the ser^led^^paint /can containing the  desired
                       (Tenax® gart/idge from~-«ne freezer.

                                   the freezer in the laboratory designated
                        for-vpartr^4ge storage ONLY for this purpose.
                        Inadvertent storage of containers of solvent in this
                                   1 resnlt in contamination of  all cartridges
                               in the\£yfeezer and will compromise  the
                                  since organic solvents  are frequently target
                                  for quantitative analysis.   Verify that the
                                   personnel are not involved  in any process
                                  jses open containers of  organic solvents,  as
                                  Ivent vapor will contaminate a Tenax®
                                  exposed to this atmosphere in  only a few
                                 thus compromising the quantitative and/or
                               tive assay.
July, 1991
                                                          Page D  -  35/VT
-------
Exhibit D
                                                      SOW No.  XXX -  Ambient Air
                        Open the  sealed  lid  of  the paintca/(  using a flat-
                        bladed screwdriver,  beverage can  opener,  or other
                        convenient  tool  for  this purpc/se.<
                        NOTE:  The cartridge will b
                        with a Teflon-lined screw /ap,
                                           ss  steel tube
                        Remove a single Tenax®  oGb^from  the  paint
                        the paint can and replace /In the  freezer, and
                        the Teflon cap of the/deaorption  chamber.
                        Remove the cartridf
                        forceps.
                            the  shipping tube  using
                        NOTE:  DO NOT TOUCikTHE "GARXRIpfcE WITH YOUR HANDS!
                        Organic compounds present on tjhe fingertips can  be
                        sufficient to compromise^the analysis.  If the
                        cartridge is inadvertently tbvched\make careful note
                        of the circumstances in both theM^nsti^iment log  and
                        the projec,J
                        Insert the\arbridge"~"±nmediately into the desorption
                        chamber.  Close\he Tefloi!^cap~Trf-^the desorption
                        chamber, and iViiti^te/th/ timing of the eight-minute
                        desorption cycle\  DdrLng this time period, helium  is
                        flowing through th^ desorption chamber.
            2.4.6.2.5
            the desorpti,
            are automa
At
the
                  eign^-m
                  the
  .ute desorption cycle,  turn
ECT mode.  The following steps
  liable instruments.
                                                e program;

                                  feating of the nickel trap;

                                   :a acquisition system; and

                             off~"th.e trkp after it has heated to 250°C.
            2.4.6.2.8
            system in an
                                thermal desorption unit valve back to desorb
                                  cartridge.  At the end of the run, the GC
                                  to 30°C, and the data acquisition will stop
                                  1 compounds have eluted.

                              thi:s procedure for each Tenax® cartridge to be
       om GC/MS runs are normally processed by  the  data
      mated program which locates the  compounds of
July, 1991
                                          Page  D -  36/VT
-------
 Exhibit D
                                                      SOW No. XXX  - Ambient Air
interest in  the data  set,  quantifies  those c
calibration  data are  available,  and prints
repprt will  present the quantification  par
those compounds identified and quantifiab
typically list those  compounds which  wer/  searc
sample, indicate which ones were not  foAnd
characteristics and quantification  result/ for
found, and present comments for  the operator's bene
the criteria which caused  a peak to/Se\rejected
for any search which  failed.  The fnfotmation in  the  repof  ^
also be saved in a DS file for ar/hiyal storage and DS  transfer
purposes.
                                                              mds for which
                                                             ort.  A typical
                                                            rs and result for
                                                               report will
                                                                for in the
                                                                   identifying
                                                                      h were
                                                                          as
                                                             or the^benter^scan
                                                  ise
                                                         sue
                                           .d contain 4. fide composed one entry
                                                 each/enKry, the library
2.4.6.2.9  The DS library  sho
for each compound of  interes
contains the compound name, i^mas^-s^ct/urn  from  the Mass
Spectral Data Base, its absolute^setentio/ time,  and  its  retention
time relative to perfluorotoluene or^2-dictilorobenzene  -d4, the
retention time marker, as  determined  fr^a^auttieT^ic standards.
Response lists (RL) are compound specific D5\files>containing the
quantitative calibrata^n^SCa-fcu^each of the  Ca^et  compounds.
2.4.6.2.10  The automated ftrocec
chromatographic peaks coXresTjondii
reverse library search
window:
                                                 attempts  t^ locate
                                                 tp  target/compounds  by a
                                              oi/owing  criteria  for  scan
                  For intei
                    candards: ±>100\seconds from library scan
                              nuraber\
                  For /ingle comp\>urldsT^x+20 s\c/nds from the calculated
                        Corner gr/Sups
                  Peak ic
                  Peak selectic:
                                   Lon:
                                  and +20 seconds from the
                              calculated seconds for the earliest
                              and latest eluting members of the
                              group, respectively.

                              As determined by the laboratory.

                              The scan list is partitioned in
                              order of increasing distance from
                              the center of the scan window,
                              except for isomer groups.
                        The
                       renti
            dichld
            located a
        benz
                  tojfaated procedure begins  by attempting to locate
                  ^ .me  markers  (perfluorotoluene  and 1,2-
                     If  the early  eluting  standard,  PFT,  is not
           .rnina' message is printed and the  procedure  is
<-dL
July, 1991
                                                                Page D - 37/VT
-------
Exhibit D
                                          SOW No.  XXX - Ambient Air
            terminated.  If only the late eluting  internal  standard is not
            found, 'the procedure uses the scan number  catlcuiated from the
            library retention time for this standard a.p  a ^default value.

            NOTE:  Alternatively, the operator may s^ecifjr,scan^numbers for
            the internal standards and then initiate t>le rema^nder^eif the
            automated procedure.  The procedure cjrcles through  tke compounds
            in the library list attempting to lojjTa^^each compound"!^ turi
                                                  i/dentified  in the  search for
                                                           partitioned to order
                                                              of the search
                                                               are sequentially
                                                         /compound in order to
2.4.6.2.12  If one or more peaks
a target compound, the resulting
the scans in increasing distanc
window.  The mass spectra in t
compared to the library entry
the mass weighted purity, fit
            2.4.6.2.13  If the mass spectrum at^fckg peakxmaximum passes either
            of the above tests, the procedure attempts  to  quantify  the peak.
            If the target is a single compound, only tnexfirst^peak to pass
            the qualitative criterLi~T^~-p4^i£essed further/^X£j the  target is
            an isomer group, all peaks detected~~&y-~€tie^search  are processed
            through the qualitativeXfilterSr-aacLall that~pa£s  these filters
            are quantified. If no peaks sore foupd tfy~~th«-^sjsarch or  pass
            through the qualitative filters, a/"not detected"  entry is placed
            in the report.              \  \/  /
                            jst va
                                to,
NOTE:  The failu£e_fif
necessarily prove the
Interfering tfomp
may cause ttie
It is also/po
rfit/purLty,/but have,
absence/of af partic
DS procedure rails /to
the data oy^a person
is necessary rsj: con
 a peak to\sarisfy these criteria does not
             :he^corapound in the sample.
 or\ low level\ of^the compound of interest
                  de of the acceptance range.
                 le values for fit/purity and
                identification.  If the
ar/compoundM-s7 of crucial importance and the
  ocate the compound, manual inspection of
 killed in the interpretation of GC/MS data
 rmation.
-------
 Exhibit D
                                                      SOW No. XXX  - Ambient Air
       2.4.7.2   Frequency

             2.4,7.2.1   Prior to the analyses of any s
             calibration standards,  the Contractor mus
             GC/MS  meets the  standard mass spectral
             is  accomplished  through the analysis of
             (BFB).  The instrument  conditions requ
             the BFB mass  spectrum are given in Ex
                                                        blanks,  or
                                                     ablish that a given
                                                        Criteria.   This
                                                            >enzene
                                                               ;ition of
            NOTE:  BFB criteria must  be  met bef/ore
            Any samples  analyzed when BFB critzteriA have not been met will
            require reanalysis at no  cost to/the/Agency.
                                           'analysis
                                               lye  hour
                                         to"~sneet
                                                 e  D/VQAT-
      2.4.7.2.2  Each GC/MS used for
      checked daily or once per ea
      whichever is most frequent,
      criteria for BFB as outlined in
      corrective action which could change
      performance check for BFB (e.g., ion
      column replacement,  etc.), the instrument
      be verified immediatel
      performance check req
*st
  inical
                                                     aff
                                                  soul
                                                  of  the  twe
2.4.7.3  Procedure

      2.4.7.3.1  Prepare a 25
      Prepare fresh BEB-*eJ,ution evei
      solution has jiegraded
                                               ion of BFB  in methanol.
                                             six months or sooner  if  the
 >e performance
riod of operation,
     acceptance
 3.   Also, whenever
  the instrument
    Ing or repair,
 :prma^ice check must
     -hour/daily
            NOTE:  The ,25
            volume.
            a 1 //L i

            2.4.7.3'

            2.4.7.3.3  Se£
            and injjti^te data
            operator's manual.
                m
            procee
            obtaining
                                           _!Sed with a 2 fiL injection
                                          a 50 ng//xL solution of BFB if
                              BFB into the GC/MS.

                              parameters for the acquisition of the data
                                ".on by following instructions in the


                           lent parameters (e.g., lens voltages,
                            adjusted to give the relative ion abundances
                             3 as well as acceptable resolution and peak
                           iximate relative abundances cannot be
                           •ce or quadrapoles may require cleaning
                           .rer's instructions.   The Contractor must
                         "relative ion abundances for BFB before
                        (pie  anslysis.   Samples  analyzed before
                         ion  abundances specified in Table D/VOAT- 3
July, 1991
                                                                Page D - 39/VT
-------
Exhibit D
                                                     SOW  No.  XXX -  Ambient Air
            must be reanalyzed at no expense to the Agency

      2.4.7.4  Technical Acceptance Criteria

            2.4.7.4.1  Prior to the analysis of any
            calibration standards, the Laboratory
            GC/MS system meets the mass spectral ion
            the instrument performance check sol
            2.4.7.4.2  The instrument performs
            injected once at the beginning
            samples or standards are to be

      2.4.7.5  Corrective Action
                                              ice/check standard must be
                                                   12-hojac^period during which
                                               feed.
            2.4.7.5.1  If the BFB acceptance
            be retuned.  It may be necessary to
            quadrupoles,  or take other actions to
            criteria.

            2.4.7.5.2  BFB accept.
            standards,  performance^va
            are analyzed.   Any sampl
            criteria have  not been me
            additional  cost to the Agen

      2.4.7.6  Documentat ion

            Reporting re

2.4.8  Calibration of

      2.4.8.1  S
                                               iteria Are not met, the MS must
                                                          ion source,  or
                                                      Leve^Ci^e acceptance
                                                       met before any
                                                            or required blanks
                                                           .nalyzed when tuning
                                                    reanalysis at no
                                                  ihibit B.
            2.4.8.1.1
            s tandards tha
            of interest.   The1
            me
             i'trix.iaterfere-
                                   approach,  the analyst must utilize internal
                                       in analytical behavior to the compounds
                                      must further demonstrate that the
                                         tandard is not affected by method or
                              es.   rru^rnal standards specified for this
                                al and tinal  markers for the MS (see part
                                 standards.  The internal markers are:

                                           (m/z)
                                   (PFT)
                       ichlorobenzene - d<,
                                                217
                                                146
            2.4.8.1.
                               ounds specified as internal markers have been
July, 1991
                                                                Page D - 40/VT
-------
Exhibit D
                                SOW  No. XXX  -  Ambient Air
            also used successfully as surrogate spikes,
            generally unique retention times.
                                     ;c=mse  of  their
            2.4.8.1.3  Prior to the analysis of samplers a^d required blanks
            and after the instrument performance che^k standard criteria  have
            been met, each GC/MS system must be cal/bra^fed at axminimum of
            five concentrations in an initial calibration se^uenc^xor with
            the calibration check standard in a d4ll/ calibration sequence,  to
            determine instrument sensitivity and^^t^ie linearity of OG/MS
            response for the target compounds.
            2.4.8.1.4  A check of the calibr/z
            every 12 hours.

      2.4.8.2  Frequency
                        .ticm curve/teust be performed once
                                                    coi
2.4.8.2.1  Each GC/MS system mus
contract, whenever the Contractor
may change or affect the initial calibr
source cleaning or repair, column replaceme'
daily calibration acce£t£
Calibration is accfomplisted by mean"
                                                      on ci
                            calibrated upon award of the
                                    ctive action which
                                       teria (i.e., ion
                                         .),  or if the
                                         n met.
                                   internal standard
                                            Lteria have not*
            calibration procedure
                   rej
                                     response factors (RRFs).
            2.4.8.2.2  If time remains^in\the/12/hour time period after
            meeting the acceptance critHriaXEor/the initial calibration,
            samples may be analyzed.  ItVs no/c necessary to analyze a
            continuing calibration standarcl if\the initial calibration
            standard that/is the same concentration as the continuing
            calibration/stajKterd meets the concinujLng calibration acceptance
            criteria. /Quantify ail I#an5p4e result/ against the initial
            calibration standard £hat is thexgame concentration as the
            continuir
g calibrati
                                 n
            2.4.8.2x3  Ifxt.ime/do$
            with the rnjecti*
            new analysis &f^ the
            performed
             :S not remain in the 12-hour period beginning
             the instrument performance check solution, a
             .strument performance check standard must be
                               of tRe^i^itial calibration curve must be
                                 12 hours.
                                  •e calibration standards containing all the
                              piked on clean Tenax® tubes as outlined in part
                            ^Generations outlined in Table D/VOAT- 4.
July, 1991
                                           Page D - 41/VT
-------
Exhibit D
                                                      SOW No.  XXX -  Ambient Air
            2.4.8.3.2  To each  of  these  tubes,  add  knowr/concentrations of
            internal markers  (300  ng  level),  as outlined inpart  2.3.6,
            and. analyze each  tube  according  to  part 2/3.4SxEach  tube  must
            also contain the  three surrogate  standar/s  Csee p^rt  2.3 6) at the
            300 ng level.

            2.4.8.3.3  Analyze  according to part

      2.4.8.4  Calculations

            2.4.8.4.1  Tabulate peak height /5r  area resooiiaes against
            concentration for each corapound/anci internal  standard.  Table
            D/VOAT- 5 contains primary quanti/ation i/ms/to be used for each
            target compound and internal 4tanoa
            target compound and the internal static
            equation:
            where:
                          factors (RRF) for each
                          Cd using the following
                                                                  Eq. D/VOA-4
            The RRF
            and concent
            the compound.
cea^respoftse for the\com)aound to be measured,
    res^onste ion for Che "internal standard,
                    neaWst internal standard, ng,

                      ipound to be measured,  ng.

        ound is calculated using the values of area
       'specific internal standard associated with
July, 1991
               . 8.4.3  Ini^biate quimtitation of the RRFs for the target
            comn«rtindF~3nd crektion of^-she library in the data system.  The
           'aWrage RRF muVt beXcalculated for each compound by averaging the
            values obtained ^t the five concentrations as specified in part
            L3.4.2.2 and outl\ine\l in Table D/VOAT- 4.

                 ^.4  Internal standard responses and retention times in all
              indardsmust bet evaluated during or immediately after data
            acquisition

            2.4.8.4.5^Sheck /the relative response factor of the calibration
                                       Page D - 42/VT
-------
 Exhibit D
                                                       SOW No.  XXX - Ambient Air
             compounds in the initial calibration  to  see  tKat^the percent
             relative standard deviation (%RSD)  is within/±3(/percent.
                                        SD
                                           X 100
                                           Eq. D/VOA-5
             where:
                   SD  - standard deviation, an<
                   RRF = mean RRF from the initial/calibration.

             2.4.8.4.6  A percent difference/XD/ of the/da^ly relative
             response factor (12-hour) comp/red/to the/average relative
             response factor from the initial 4mrve is'calculated for each
             compound,  utilizing the following eqttat^onv
                                       - RRF
                   - x 100
                                                                   Eq. D/VOA-6
      where:
            %D
            RRFC  -
Percent dif
Average RRF rrom
Continuing (12-hour)
      2.4.8.5  Technical Accj
        ace Criteri
2.4.8.5.1
within ±30 >£ec<
standard.
                                     /curve;  and
                                      check.
                           nds
                                      time  for\ny
                                          ifest
                          internal standard must be
                           y (12 -hour) calibration
            2.4.8.5
            RRFs ii

            2.4.8;5.3
            within__±_30_ percen
\e percent /elative
                                   mdard deviation  (XRSD) of  the
                        •e must be within ±30 percent.

                 continuing calibration sequence, %D must be
                              .ected^^sin/current profile  (SICP)  of  the  internal
                                •nitored and evaluated  for each  standard.   The
                                 .ernal standard must not change by more  than
                                 :ention time for any internal standard changes
                               ronds from the latest daily  (12-hour)
July, 1991
                                                                Page D  - 43/VT
-------
Exhibit D
                                         SOW No. XXX  -  Ambient Air
            calibration standard, the chromatographic 535,
            for malfunctions, and corrections made as
            corrections are made, reanalyze samples wl
            system was malfunctioning.

            2.4.8.6.2  If the %RSD of the RRFs in
            within ±30 percent,  the relative resp
            are calculated and reported.
                                                 must be  inspected
                                               fored.  When
                                               (ere analyzed while
                                                          s  not
                                                              ounds
            2.4.8.6.3  If the retention time
            by more than 30 seconds from the
            calibration standard,  the chrom
            for malfunctions,  and correct!
            2.4.8.6.4  If the SICP area fo
            more than a factor of 40 percent,
            must be inspected for malfunction an
            appropriate.   If the analysis of a subse
            indicates that the systemis functioning
                                             nee
corrections may not be/requi]
outside the limits must be--cg_^analyze
then the laboratory mus\ demonsti
system is functioning pr
analysis of a standard
corrections are made and the\SIC
are inside the contract limit
the first analysis—tt considere
of the laboratory.  Th
with SICPs w/thifPtfte, co
Narrative
                                         internal standard  changes
                                               ,12-hour) continuous
                                               m must be  inspected
                                              ired.
                                         pro
                                             standard changes by
                                           spectrometric system
                                              ons made as
                                                  le or standard
                                                   then
                                                      the
                                              iis /must
                                           (40<
                                    efore,
ami
                                           lim:
                                           rrect
      2.4.8.7  Documi
            Reporti

2.4.9  Sample Analysis
                .-	
      2.4.9.1 /Summary
lie standards>*£th SICP  areas
           rrections are made,
             ss spectrometric
           'accomplished by  the
   the SICP criteria.   After
 reas for all internal standards
percent), then the problem  with
  .ave been within the control
        data from the analysis
     Document in the SDG
   'e actions taken.
                       are listed on Exhibit B.
July, 1991
                            lysi^s of samples, establish the appropriate GC/MS
                                 ,ze the instrument performance check standard
                        GC/MS ^ys^em.  If time remains in the 12-hour period,
                                  out analysis of a continuous calibration
                               ot/remain in the 12-hour period since the
                                  performance check standard, both the
                             ch^ck solution and the continuous calibration
                            zeja before sample analysis may begin.
                                                    Page  D  -  44/VT
-------
Exhibit D
                                                      SOW No.  XXX -  Ambient Air
      2.4.9.2  P-ro.cedure

            Analyze samples according to the GC/MS proo4du/e  outlined in item
      2.4.6.

      2.4.9.3  Calculations
            2.4.9.3.1  Percent Area Response Change /%ARC):
            percent area response change (%ARC) /fb^the sample/blan
            compared to the most recent daily oral
            for each of the internal standard/co
            equation:
                           anal}
        ration  standard analyses
       ounds using  the  following
                                                                  Eq. D/VOA-7
            where:
                              Area response d
                              surrogate standar
                              analysis, and
                              Area response of the
                              surrpgatie
        int
   :ernal  marker or
,n  tne\sample/blank
        intei
  ards in the
            rker  or
            recent
                                         calibratt?
             andard.
            2.4.9.3.2  Retention Timk Sh
            time shift (RTS) between t
            recent continuing calibratic
            internal markers and surrogat
            equation:
            where:
 (R/S)/  T^tttii'ate the retention
       ank analysis and the most
     rd analysis, for each of the
standards, using the following


                       Eq. D/VOA-8
                                'tension
                                   tion time of the internal marker or
                              surrogate standards in a sample/blank, and
                              recetion time of the internal marker or
                                        standards in the most recent
                              conTsojuiin£>calibration standard.

                                  percent recovery (%R):   Calculate the
                                 overy using the following equation:
                                                                  Eq. D/VOA-9
                               y determined by analysis,  ng,  and
July, 1991
                     Page D - 45/VT
-------
Exhibit D
                                                      SOW No.  XXX - Ambient Air
                  Qa =  quantity added  to  sample/blank,

      2.4.9.4  Technical Acceptance Criteria

            2.4.9.4.1  The sample must  be  analyzed
            the BFB performance check,  initial  cal,
            calibration technical acceptance cri
            2.4.9.4.2  The sample must be deso
            contract holding times.

            2.4.9.4.3  The sample must have,
            technical acceptance criteria
            batch.
                                                      tern meeting
                                                         inuing
                                        and analyzed withiri
                                                meeting the blank
                                               tal VOCs per Tenax®
            2.4.9.4.4  The percent recovery
            sample must be within the recovery

                           Surrogate  Recovery Limits
Compound

Benzene-ds
Chlorobenzene-ds
1,4-D ichlorobenzene-

2.4.9.4.5
s tandards f
internal stfan
analysis,/or
                                             the  surrogates in the
                                              follows:
            2.
                                                  -150%
                                                50-150%
                                                50-150%
            2.4.9.4/6
            standards mus"
            sample ancN4;he nt
            analysis.
                  ^or each of the internal
                      40 percent compared to the
                   /continuing calibration
     from initial calibration.
                 7

 Itioh time sftiit for each of the internal
Lessr than or equal to 30 seconds between the
  recent continuing calibration standard
     1.4.7
July, 1991
                           targetxconipOTand concentrations must not exceed the
                        of eke initraj-^ycalibration range and no compound ion
            (excluding tfe&^comfcound peaks in the solvent front) may saturate
            th4 detector.

               Corrective Actibn

                       If the/ sample technical acceptance criteria for the
            sur~rogat'e>ssand i/nte/nal markers are not met, check calculations,
            surrogs.te antikj^nternal standard solutions, and instrument
            performance^.  It^ay be necessary to recalibrate the instrument or
                                                    Page  D  -  46/VT
-------
Exhibit D
                                               SOW No. XXX  -  Ambient Air
            take- other corrective action procedures  to raaet
            internal standard  technical acceptance criteria/
                                                           surrogate  and
            2.4.9.5.2  If the Contractor needs  to  anaWze^more  than one  (1)
            sample to have all the  target compounds yithin the  initial
            calibration range and to have all compovind /Co^as  not^-saturating the
            detector (excluding the peaks in the syolvent  froftO ,  contact
            Sample Management Office (SMO) .  SMO 
-------
Exhibit D
                                                      SOW No. XXX - Ambient Air
                                                        san
for -io.ns unique to the component of  interest

2.4., 10.1.4  For comparison of standard an
spectra, mass spectra obtained on the Co^tra,ctor'
required.  Once obtained, these standar
identification purposes only if the  Contractor's
daily instrument performance requiremeS^r for BFB
spectra may be obtained from the run/us>d to obtain  reference
RRTs.
                                                               component mass
                                                                GC/MS are
                                                                     used for
                                                                       ts the
                                                                   ise standard
                                          may
            2.4.10.1.5  The requirements  for^qualitative
            comparison of mass spectra are as  fallows:  '
                                                rification by
                  All ions present in theAtandard ma'ssy^pectra at a relative
                  intensity greater than UNRerceht/(mo%t  abundant ion in the
                  spectrum equals 100 percent^Nnjost beC^resent  in the sample
                  spectrum;

                  The relative intensities of such ions nJt*st  a^ree within ±20
                  percent between /he stan3ai?4^ands ample  spfectra.   (Example:
                  For an ion with Wi afewndance ofMTTreT?6^nt  in the standard
                  spectra, the corr^po\ding~sa^rple_^bundanfce must be between
                  30 and 70 percent) ;"

                  For each internal stan&ardY determine that  thearea measured
                  in the sample extract ha^s no/ changed by >40  percent from
                  the area^ate'Ssttted during ohe aost recent continuing
                  calibration checkXor by >50\perfcfint from the  mean area
                  measured dCSin^inYtial calib\ati>on.  If either  criterion is
                  not rp4t,/remedia^L actiort^ust b$r taken to improve
                  sens
                       greater /har/25 percenS^in the sample spectrum but not
                                  Candard spectrum must be considered and
                            for b^y the analyst making the comparison.  All
                            neetirtgxthe identification criteria must be
                                their^pectra.  For all compounds below  the
                  CRQL report the^tuay value followed by a "J", e.g.,  "3J."
                  .1.6
                             COB
            criteria in item
                     lound  cannot be verified by all of the
                      .0.1.5,  but in the technical judgment of the
 (ass spectral interpretation specialist the identification is
                      :ractor shall report that identification and
                      :ation.
              ?rrect
            pro
 then
with quant
font
Lfid
July, 1991
                                                    Page D - 48/VT
-------
 Exhibit  D
                                                      SOW No. XXX  - Ambient Air
       2.4.10.2   Non-Target Compounds

             2.4.10.2.1   A library search shall be exec
             sample  components for the purpose of tent
             For  this  purpose, the 1990 (or more rece/t)
             Library,  containing 50,000 spectra, sh
             generated library search routines mus
             routines  that would misrepresent the
             when compared to  each other.   Up to
             greatest  apparent concentration no
   use
 •ary or
•rganic
             tentatively  identified via a forw
             Only after visual  comparison of
             library  searches will  the  mass
             assign a tentative identifica
             search routines must not use
             misrepresent  the library or urtkoown
             other.
                                                        in
            2.4.10.2.2  Guidelines  For Making  Tentat
                                                for non- target
                                                identification .
                                                     of the NISI
                                                       raputer
                                                          ion
                                                 unkrft
                                                compounds
                                               Exhibit
                                      ;earch of the NIST Library.
                                                with the nearest
                                               retation specialist
                                     Computer Generated library
                                            routines that would
                                             when compared to each
                                                  ification:
                  Relative intensities
                  (ions greater
                  should be present
                            lmajor ionSr~ia__che  reference  spectrum
                                        the mosp  abundant ion)
                            th,e  samlespec!
                  The relative intensities
                  within ±20 percent.
                  of 50 peirpetrt-of the
                  sample .fon abundance must
                            ions ftrei
                     ^ent/in sample
                                    ie major  ions should agree
                                      For  an ion with an abundance
                                    ^spectra,  the corresponding
                                   between 30 and  70 percent);

                                refeNr^nce  spectrum should be
                           ictrunfr
                    actrx
            present fn the sample^spectrum but not in the reference
                   lid/be reviewed for possible background
                       presence of coeluting compounds; and
                                  tn
                          ^reference spectrum but not in the sample
      spectruliKshouldNae reviewed for possible subtraction from
            nple^^pectrunKbjScause of background contamination or
      coelutinx compounds.  Data system library reduction programs
      can sometimes Create these discrepancies.

 .4.10.2.3  If in the!technical judgment of the mass spectral
interpretation specialist, no valid tentative identification can
ae madesthe conmounci should be reported as unknown.  The mass
spetet^al Specialist/should give additional classification of the
unknowh^ompotioti i/ possible (i.e., unknown aromatic, unknown
July, 1991
                                                                Page D - 49/VT
-------
Exhibit D
                                                SOW  No.  XXX -  Ambient Air
            hydrocarbon, unknown chlorinated compound). /If/probable molecular
            weights can be distinguished, include  them,

2.4.11  Quantitative Analysis

      The quantitative analysis is performed by a
computerized procedures:  the computer identifies'
characteristic ions in a full scan mode.  At thLspoint  the  operatoi
intervenes to determine if the compound of interest has  been located
correctly.  If the compound identification is/correct, the computer then
performs the quantitative calculation using Wie-method o/f^-relative  response
factors.  Data are reported as ng/cartridge/ ana can be/subsequently converted
to /;g/m3 ,  as outlined in part 2.3.8.1.
                                                             the  data
                                                              et compounds.
                                                               llowing
2.4.11.1  Target Compound Quantitati

      2.4.11.1.1  Sample quantitation is pel
      processing system for all desired ions ol
      Target compounds are quantified according
      equation:        Eq. P/VOA~]
            where:
                                        jour
                                           >f a:
                                      standai
                                            concentration,
                                         ialyte,
                                          standard applied  to  tube,  fig,
                              vol\.
                                jcesponse. f a$
                                      sampl
tor (RRF), and
. (m3), STP.
                        the compv/ter/must^ke ab/e to print out peak  number,
                                relative retention time, area and  amount.

            2 .4.11.1.3 "^Stano^ard/responses and retention times in all
            standards must^be evaluated during or immediately after  data
                          If the reteration time for any standard  changes  by
                 than 30 ^s£onds rs^m trte latest daily (12 hour)  calibration,
                                system-vjnust be inspected for malfunctions, and
                                vrequired.  The SICP of the internal  standards
                                  evaluated for each sample and blank.   If the
                                  srnal standard changes by more than 40
                                  itrometric system must be inspected for
                                  itions made as appropriate.  When corrections
                              5is/of duplicate samples analyzed while the
                             ictjconing is necessary.
 July,  1991
                                                           Page D -  50/VT
-------
  Exhibit D
                                                        SOW No. XXX  -  Ambient Air
        2.4.11.2  Non-Target Compound Quantltation

              2.4.11.2.1  An estimated concentration fo,
              tentatively identified shall be quantif
              The nearest internal standard free of
                                               1-target  components
                                               the standard  method.
                                             ferences shall be used.
 2.4.11.2.2  The formula for calculatj
 as in part 2.3.8.1.1.  Total area c
 the total ion chromatograms are to
 to be measured and the standard
 of one (1) is to be assumed.
 shall be qualified as estimate
 estimated concentration shoul
 identified compounds as well/as ythose
                                              (
                                             becalcul
                                   is the same
                                   Lts) from
                                       ipound
                                         (RRF)
                                   	,_on
                   flagged "J").   This
                         for all  tentatively
                    -nt/fied as unknowns.
                                          ce
 2.4.11.2.3  An estimated c^
 all  tentatively identified
 as unknowns.   This estimated Cw^
 all  tentatively identified compoun
 as unknowns.
                                              entrat
                                                  as
                     3uld be calculated for
                   f *ell  as  those identified
                   Lon must  be  calculated for
                      \1  as  those identified
 2.4.12  Performance Evaluation

       2.4.12.1  Summary
2.4.12.1.1  The perfoi
Agency  in monitoring ContXact
not be  informed as  to whicKcoz
samples or the—concentration^
                                               :ion samples will assist the
                                             performance.   The laboratory will
                                            founds are contained in the PE
                                        icy.
2.4.12.I./ Thg-labor\tory will
adsorben? tube from\ t
ins true,
PE sa
PE s
             2.4.12.
             acceptance
             cor_
                 PE si
                     ^•J   T—^, JJ/+..
                   PE samples on Tenax®
                samples will come with
             ition procedure required for the
             and surrogate compounds to the
procedureS^in part 2.3.6.
                                   lal
                   tion to complying with the PE sample technical
                   xtfie laboratory will be responsible for
          identMyingN-b.e^quantifying the compounds included in
                           will notify the laboratory of
                            rforman
             .2  Frequency

            The Laboratory
             Le once per sample
                    desorb, analyze, and report the results of the
                    delivery group, if available.
July, 1991
                                                                Page D  -  51/VT
-------
 Exhibit D
                                                      SOW No. XXX - Ambient Air
 2.4.12.3   Procedure

       Desorb  and concentrate the PE sample using tHe procedure described
 in part-2.3.5.   See part 2.3.8.1 for equation/necessary for
 calculations.           '

 2.4.12.4   Technical Acceptance  Criteria

       2.4.12.4.1  The  PE  sample must be
       meeting the BFB  performance  chec
       continuing calibration technica
       required frequency.
  tyzed on a GC/MS
        calibration,
ieptance/^riteria at
                        The PE sample mu
                                                                     and
                                                                     the
                                              tec
         ccording  to  part
            analyzed with a
            eptance  criteria.
      2.4.12.4.2
      2.3.5.
      2.4.12.4.3  The PE sample must be"
      method blank that meets  the blank

      2.4.12.4.4  The percerrtr^Eecovery for each of^e/surrogates must
      be within the acceptance windows~~tt»«e4__in part 2.3.8.3.

      2.4.12.4.5  The area response changeytprtween^the PE sample and the
      most recent calibration\taridard /analysis for each of the
      surrogate standards must Be within/^O percent.

      2.4.12.4.6  The^etention timeshlft between the PE sample and the
      most recent continuing calibrafr^on\tandard analysis for each of
      the internal standardsXmust be wi>thi\30 seconds.
                          ,   I .,—^     \  >
2.4.12.5  Corre/tiye Actior

      2.4.12.^.I/ If theyPE Sample ~b6ch/ical acceptance  criteria for the
      internal sta**dard/and/surrogates are not met,  check calculations,
      standar^soluttsns and instrument performance.  It may be
      necessary tbxrecalio^rate the instrument or take other corrective
      action procedure^to daet the technical acceptance criteria
                        \^
                      PE sam>le technical acceptance criteria MUST be
                     ile\data arV reported.  Also,  the Contractor must
                          le performance for compound identification and
                       If \the Contractor fails to meet the PE sample
                           criteria, the Agency may take, but is not
                          ring actions:  reduction of the number of
                             sample shipment, a site visit, a full data
                          e the laboratory to analyze a  remedial PE
                     a contract sanction,  such as a Cure Notice.
July, 1991
                Page D  - 52/VT
-------
 Exhibit D
                                                       SOW No. XXX -  Ambient Air
 2.5    PERFORMANCE REQUIREMENTS FOR DEMONSTRATING METHOD
       ANALYSIS O.F AMBIENT AIR
 2.5.1   Summary

       2.5.1.1  Although this method describes the
       compounds collected on Tenax®,  collection
       acceptable if the performance criteria de
       met.   Specifically,  the analyst must dem<
       alternate solid adsorbent and subsequen
       part  2.3 produce results meeting these/ge
                                                      lEPTABILITY FOR THE
                                                        ;sis of target
                                                            ,ts is
                                                               .pn are
                                                                     an
                                           !/MS  analysis as de^scrib^d in
                                           sral  criteria:
            Minimum contract  require^
            in Table D/VOAT-  1;

            Replicate precision
                                                ntitat*nNlimits (CRQL) listed
                pe;
                                                      it RSD;
                   Audit  accuracy of 30 percent* for^pollutant concentrations
                   normally  expected in ambient
2.5.1.2  These criteria were__es_tablished using
application of TO-10 methodology
Monitoring System (TAMs)
(UATMP).   The primary reaso\to\base
method on performance is to a
analysis of VOCs in water to oe\us
than compressed gas standards ma^
audit standards must be humidifie
resemble the air majet±xT\De tails
criteria follow.
                            :al data from the
                  from the^foxics  Air
                         •nitoring Program
                   _tabi^tty of analysis
                         being used for the
               'DCs in air.  Solutions  rather
       bevus/d for calibration.   However,
               .ndards, to most closely
               determination  of each of the
                                        ^syst
                      /   /
2.5.2  Minimum Contract Requirec
                                           its (CRQL)
      The minimum
measurements of a/con
detection limit, t
concentrations, and t
99 percent confidence for
              .QI/is defined
                  tratic
               star
                   value
                      valuj
         4-abcjratory by making seven  replicate
  the compound of interest near  the  expected
lation computed for the seven replicate
iltiplied by 2.3.14 (the Student's  t  value  for
2.5.3  Replic
           PrecisJ
      The/measure of preHsiok used for this program is the unsigned  relative
difference between replicaos measurements of the same sample.  There  are
several/factors which may affecO the quoted precision of the measurement.   The
nature/of fcive compound of interest itself may have some effect on  the
precisitonsuc:h\as the obserWtidn that styrene generally shows slightly poorer
precision than thfexbulk of rlonp4lar VOCs.  The primary influence on precision
is the coneentr^tion^ieveI/of/the compound of interest in the sample,  i.e.,
the percent relativestahdard:  deviation for a set of replicate values degrades
July, 1991
                                                          Page D - 53/VT
-------
Exhibit D
                                                      SOW No.  XXX - Ambient Air
as the concentration approaches the detection  limit:.
of precision was -obtained from replicate analysis  of  Tei
TAMs network.  This is the source for  the  30 percent/til
overall replicate precision given above.
                conservative measure
                    samples from  the
                 re of merit for
2.5.4  Audit Accuracy

      Audit Bias is defined as the relative
result and the nominal concentration of the
[(True - Found) x 100]/True.  Audit standard
participating laboratories, these audit __
judged against criteria based on historica
                                          i

*     Exceptions are carbon tetrachlori<
      higher audit accuracies are report
    diJ
star
  Snce between the\measur-eoent
 'spiked compound,  i.
Ll  be  supplied to  the
            and the results
            tri/fchloroethane, for which
                TAMs study.
July, 1991
                        Page D - 54/VT
-------
  Exhibit D
                                                       SOW No.  XXX - Ambient Air
   Table D/VT-1.  Target Compound List for Volatiles Col]
                and  Contract  Required Quantitation  Limit
 Compound

 Pencachloroethane
 Trichloroethylene
 Chloroform
 Benzene
 Carbon Tetrachloride
 Tetrachloroethylene
 1,1-Dichloroethene
 1,2 -Dichloroethane
 Chlorobenzene
 1,1,1-Trichloroethane
 1,1,2-Trichloroethane
 1,1,2,2-Tetrachloroethane
 Ethylbenzene
 Styrene
 1,1-Dichloroethane
 Toluene
 Xylenes,  m-  and p-
 Xylene,  o-
 1,2-Dichloropropane
 1,2-Dichlorobenzene
 1,2-Dibromoe thane
 1,4-Dichlorobenzene
 1,4-Dioxane
 Tribromomethane
 1, 3 -Dichlorobenzene
 3 -Chloro-1-propene
 Tetrahydrofuran
 Bromoethane
 Bromochloromethan
 1,2,3-Trichlorop
 2 -Chloropropane
 Bromobenzene
 l,4-Dichloro-2-b
 l-Bromo-3-ch
 (1-Methyle
 1-Methyl
 1-Etheny
 Bromotrich
on Tenaz* Tubes
      CRQL. (ng1)
July, 1991
                                                                Page D - 55/VT
-------
Exhibit D
                                                     SOW No. XXX  - Ambient Air
                                                    Col]
                                                              on Tenax& Tubes
                                                104-51-8
                                                108-41-8
                                                100-52-7
                                                100-47-0
Table D/VT-1.  Target Compound List for Volatiles
             and  Contract Required  Quantitation  Lim
                                (Continued)
Compound

Pentachloroethane
1-Chloropropane
1,2-Dibromopropane
2,3-Dichlorobucane
2-Chlorobutane
1, 3-Dichlorobutane
1,4-Dichlorobutane
3,4-Dichloro-l-butene
l-Chloro-2,3-epoxypropane
2-Chloroethoxyethene
1-Phenylethanone
D ib romomethane
1,3-Dichloropropane
1,1,1,2-Tetrachloroethane
o-Chlorotoluene
1,3,5-Trimethylbenzene
p-Chlorotoluene
n-Butylbenzene
m-Chlorotoluene
Benzaldehyde
Benzonitrile
July, 1991
                                                                Page D - 56/VT
-------
 Exhibit D
                                                       SOW No-. XXX - Ambient Air
             Table D/VT-2.  Typical Operating Conditions for * GC/VS
 Thermal Desorption Unit: • NuTech Model 320, Tekraan
                                                          5000 or equivalent
 Purge Gas (Prior to Desorption)
 Desorption Cycle
 Initial Desorption Temperature
 Final Desorption Temperature
 Thermal Desorption Unit Purge

 Gas Chromato^raphv

 Injection/Detector Temperature
 Initial Column Temperature
 Initial Hold Time
 Program
 Final Hold Temperature
 Final Hold Time
 Maximum Over Temperature
 Carrier Gas
 GC/MS Interface
 Sample Injection to MS
 Column
                                      Helium @ L.2,
                                      8  minutes
                                      25'C
                                      150°C
                                      10 mL/mi
Mass Spectrometer  -

Mass Range
Scan Time
El Condition
Mass Scan and Detecto
Routine Tuni
Preamp Sens
Emission C
Electron
Mass Fil
Filter
Total
Resolution
Display
Response
                                                            4c at 250"C
                                                        .lass jet

                                                         glass capillary
                                                methyl silicone (50 m x 0.3
                                                film thickness) Scientific
                                              .neering SE-30 glass capillary
                                              >d methyl silicone (50 m x 0.5
                                             jum\film thickness)
                                                 )
                                                 tron Impact (El)
                                             nin over entire range
                                    70  eV
                                    Follow manufacturer  instruction for select
                                    mass  selective  detector (MS)  and scan mode

                                       •omofluorobenzene

                                    -0.45
                                    1000  to 1500
                                    10  amu/sec
                                    x 100
                                    1
                                    Normal
                                    TIC
                                    Fast
'ul-i
      1991
                                                                Page D - 57/VT
-------
Exhibit  D
                                                       SOW No. XXX - Ambient Air
        Table D/VT-3.  Required BFB Key Ions and Ion
                                   .nee  Criteria
             Mass

              50
              75
              95
              96
             173
             174
             175
             176
             177
       Ion Abundance  Crlter/a
8.0
30.0
      40.0  percent of maps
      • 66.0 percent of
base peak,  100  percer
5.0 - 9.0 percent of
less than 2.0 percent o£ mass
50.0-120.0  percent
4.0 - 9.0 percent
93.0 - 101.0 pero4nt/of mass/174
5.0 - 9.0 percent
                                         tha nominal basa peak. avan though tha ion abundance
July, 1991
                                        Page D  -  58/VT
-------
 Exhibit  D
                             SOW No> XXX - Ambient Air
     Table  D/VT-4.
Composition and Approximate Com
Calibration Standards  Concentre
in t rat ion of
    (ng)
Compound

benzene*
coluene
1,2-dimethylbenzene*
1,3,5-crimethyIbenzene
ethylbenzene*
styrene
(1-methylechyl) benzene
butylbenzene
l-methyl-4-(1-methylethyl) benzene
chlorobenzene*
broraobenzene
1,2-dichlorobenzene*
1-ethenyl-4-chlorobenzene
chloroform
te trachlorome thane*
bromochloromethane*
bromotrichloromethane*
dibromome thane*
tribromomethane*
1,1-dichloroethane*
1,2-dichloroethane
1,1,1-trichloroethane*
1,1,2-trichloroethane*
1,1,1,2-tetrachloroetha;
1,1,2,2-tetrachloroet
pentachloroethane*
1,1-dichloroethene*
trichloroethene*
tetrachloroethene
bromoethane*
1,2-dibromoethane*
1-chloropropane*
2 -ch.oropropane*
1,2-dichloro
1,3-dichlor^pro
1,2,3-tri
1-bromo-y-
3-chlor
                                               Cal 5
July, 1991
                                       Page D - 59/VT
-------
 Exhibit D
                                                        SOW No. XXX - Ambient Air
      Table D/VT-4
Composition and Approximate Concen^
Standards Concentration (ng)
     (continued)
Compound
1,2-dibromopropane*
2-chlorobutane
1,3-dichlorobucane
1,4-dichlorobucane
2,- 3 -dichlorobutane*
l,4-dichloro-2-butane (cis)
3,4-dichloro-1-butane
ce trahydro furan
1,4-dioxane
l-chloro-2,3-epoxypropane
2-chloroethoxyethene
benzaldehyde*
acetophenone
benzonitrile
                                     Cal  1
of Calibration
                                                                          Cal  5
•Compounds used Co
tubes.
       a de,ily basis either by direct injection or on spiked Tenax* adsorbent
July,  1991
                                             Page  D -  60/VT
-------
 Exhibit D
                                                       SOW No. XXX - Ambient Air
      Table D/VT-5. Target Compound  List  for Volatiles
                '  •    Cartridges with  Characteristic
                                   Secondary)
                                      ted  on  TenaxA
                                      imary and
 Compound

 Trichloroechylene
 Chloroform
 Benzene*
 Carbon Tetrachloride
 Tetrachloroethylene
 1,1-Dichloroethene*
 1,2-Dichloroethane*
 Chlorobenzene*
 1,1,1-Trichloroethane*
 1,1,2-Trichloroethane*
 1,1,2,2-Te trachloroe chane
 Ethylbenzene*
 Scyrene
 1,1-Dichloroethane*
 Toluene
 Xylenes,  o-,  m-,  and p-
 1,2-Dichloropropane
 1,2-Dichlorobenzene*
 1,2-Dibromoethane*
 1,4 -Dichlorobenzene
 1,4-Dioxane
 Tribromomethane*
 1,3-Dichlorobenzene
 3-Chloro-l-propene
 Te trahydro furan
 Bromoethane
 Bromochloromethane*/
 1,2,3-Trichloroprctfane'
 2-Chloropropane
 Bromobenzene
 l,4-Dichloro-2-butene
 1 - Bromo- 3-chloi
 (1-Methyleth;
 l-Methyl-4-l.
 1-Ethenyl-
              Primary Ion**
       ene
*Compounds
or on spiked a
**Ion used for
     GG/MS on a daily basis either by direct injection

tCequ^red Quantitation Limits (CRQL) Determination.
July, 1991
                                                                Page D  - 61/VT
-------
 Exhibit  D
                                                      SOW No.  XXX -  Ambient Air
    Table D/VT-5.
Target Compound List for Volatiles
 Cartridges, with Characteristic I*
              Secondary)
              (continued)
                                                             cted  on  Tenax®
                                                           '(Primary and
Compound
                                     Primary Ion*y
Bromotrichloromethane*
Pentachloroethane*
1-Chloropropane*
1,2 -Dibromopropane*
2,3-Dichlorobutane
2 -Chlorobutane
1,3 -Dichlorobutane
1,4-Dichlorobutane
3,4-Dichloro-l-butene
l-Chloro-2,3-epoxypropane
2-Chloroethoxyethene
1-Phenylethanone
D ib romome thane*
1,3-Dichloroporpane
1,1,1,2-Tetrachloroethane
o-Chlorotoluene
1,3,5-Trimethylbenzene
p-Chlorotoluene
n-Butylbenzene
m-Chlorotoluene
July, 1991
                                            Page D  - 62/VT
-------
 Exhibit 0
                                                       SOW No.  XXX -  Ambient Air
                Table D/VT-6.   Typical Compounds Used in
                -  .   Factor (RF)  Determination vith Spec
                       Mass Loading onto Spiked Cartridge
 Compound
 Benzene
 Chloroform
 1,1,1-Trichloroethane
 Carbon Tetrachloride
 1,2-Dichloroethane
 Trichloroethylene
 1,1,2,2-Tetrachloroethane
 Chlorobenzene
 Tetrachloroechylene
 Ethylbenzene
 Xylenes,  o-,  m-,  and p-
 Styrene
 o-Dichlorobenzene
 p-Dichlorobenzene
July, 1991
                                                                Page D - 63/VT
-------
 Exhibit D
                                                         SOW No, XXX - Ambient Air
             Figure  D/VT- 1.   Common Designs  of Adsor
                                           (c) Multibed Adsorbent Tube
July, 1991
                                                                  Page D  -  64/VT
-------
 Exhibit 0
                                                     SOW No. XXX  - Aabient Air
            Figure D/VT- 2.  Typical Desorption GC/MS Configuration
July, 1991
                                                                Page  D  - 65/VT
-------
Exhibit D
                                                       SOW No.  XXX -  Ambient Air
                    Figure D/VT- 3.  Flash Evaporation
                                                                  5/8 IN. UNION
                                                                 16.5m)
July, 1991
Page D - 66/VT
-------
Exhibit D
SOV  No. XXX - Anbient Air
              Figure  D/7T- 4.   Permeation Tube System for
                •  •            Standard Gas Atmospheres
         at ing
                     Math tson
                     8-S3D
                     Regulator
                                                                                         Nttdlt Vai'
                                                                                    Ptrtntitton Chjmfc
                                                                                    Jacket
                                                                         Th«fmo«at, Heawr, and
                                                                         Circulating Pump
                                                                              Carrier Gai Linei

                                                                              Thtrmoitat Fluid L;nes
July,  1991
            Page D -  67/VT
-------
 Exhibit  D
                                                                  SOW No.  XXX - Ambient Air
                         Figure D/VT-  5.   Ten«j* Clean-Up
                                                              Placed In lab«i«d
                                                              tub*
                                                           •  Store In ei**n room
                                                              In DIM g*jim cam
                                                           •  fWfrigoruo
                                                              untn IMO
                                                           •  Cental**  logbook and
                                                              Chaln-ot-Cuatody Form
                                                                                         Oaalccata
                                                                                         Vacuum OVMI
                                                                                         9 100° C
                                                                                         ovarnlght with
                                                                                         Nltrogw  Flow
                                •  Holhinfilow
                                o  0«*ore\for ¥T|
July, 1991
                                                                              Page D - 68/VT
-------
 Exhibit D
                                                      SOW No. XXX  - Ambient  Air
                             TENAX CLEANUP  WORKSHEET
 Tenax Batch No.
 Virgin/Recycled. Recycled Source
 Extraction
 Number of Soxhlet Units (circle one)

 Methanol Extraction:   Date (Hours)
 Pentane Extraction:
 Nitrogen Chamber:
Vacuum  Oven:
  iphon Rate

 Date  (Hours)

 Siphon Rate
S ieving/Packing
Sieve  (40/60) Date:

Packing Date(s):

Cleanup
Teflon Septum; Date:

Teflon Liner
      (Hours)

Approx. Flowrate

 ate  (Hours)

Pump Trap

Cooldown (Hours)

N2 Vent Thru Act.  C
July, 1991
                                                                Page  D -  69/VT
-------
     ANALYTICAL METHOD FOR
SEMIVOLATILES COLLECTED BY P
  GAS CHROMATi
   INATION OF
^2 AND ANALYZED BY
  .OMETRY (GC/MS)
-------
3.1

3.2

3.3

3.4

3.5

3.6
                             SECTION  3

            ANALYTICAL METHOD FOR THE DETERMINATION/OF
       SEMIVOLATILES COLLECTED BY PUF/XAD-2 AND ANyaYZ^D BY
         GAS CHROMATOGRAPHY AND MASS SPECTROMETRY/(G0/MS)
                   TABLE  OF  CONTENTS

INTRODUCTION  	

SAMPLE STORAGE AND HOLDING TIMES

CARTRIDGE PREPARATION AND CERTIF]

SAMPLE PREPARATION FOR GC/MS

GC/MS ANALYSIS  	
GC/FID/ECD OPTIONAL SCREENING METHODOI
PESTICIDES, AND PCBs/AROCLORS
3.7   BIBLIOGRAPHY
-------
 Exhibit D
                                                      SOW No. XXX  - Ambient Air
                                    SECTION 3

                   ANALYTICAL METHOD FOR THE DETERMINATION 01
              SEMIVOLATILES COLLECTED BY PUF/XAD-2 AND ANALYZED BY
                GAS CHROMATOGRAPHY AND MASS SPECTROMETR* ((*C/MS)
 3.1    INTRODUCTION

 3.1.1  Scope  and Application

   3.1.1.1    Polynuclear  aromatic hydrocarbons' ( PAHs),  pesticides,
   polychlorinated biphenyls  (PCBs)/Aroclors /an/  other ^emivolatile  compounds
   (SVGAs) have  received  increased attention^ in/recent /ea*s  in air pollution
   studies because some of  these  compounds/are/highly /ar/inogenic or
   mutagenic.   In particular, benzo[a]pyr^ne  CB-U] P) /b,lC' -ODD, 4,4'-DDT,  and
   PCBs have all been identified  as being
   3.1.1.2   The analytical method that  follows ^sxdesighed  to  analyze  samples
   containing the compounds listed  on  the Target Compound Li^t  in Exhibit C.
   The samples analyzed under this  method are expected tcNc_ont^in
   concentrations in the following.
             PAHs
             PCBs
             Pesticides
             SVGAs

   3.1.1.3   The analys
   Methods 610 and 625,/Me
   Industrial Wastewa
   Evaluation of Sol
   Statement of Wor
   EPA Method 680,
   Soil/Sediment by Gas
   3.1.1.4   Sur
   sample prep
   extract b
   concentr
   charact
   compou
   each 
-------
Exhibit D
                                                      SOW No. XXX - Ambient Air
   NOTE:  Alpha-chlordane and heptachlor, other major  components  of technical
   chlordane, may. also be present and will be detected ayld  measured with this
   method.
   3.1.1.5   An interfaced data  system  (DS)  to  contr
   store, retrieve, and manipulate mass spectral da
   full-range monitoring data are acquired, all me
   identified and measured with one GC/MS analysi

   3.1.1.6   Applicability of the Method to PCas/Ai4clors
                                                      ition and to
                                                        When
      3.1.1.6.1   This method  is applicable  fib  samples
      single congeners or as complex mixture's, /such as
      PCBs are identified and  measured as i:som4r grout
      chlorination) by GC/MS using specia]>vs_oftw>se.
                                            Snt^ining PCBs  as
                                           :oimnercial Aroclors.
                                             .. e., by leve1 of
      3.1.1.6.2   Total PCB-concentration  in eachxsamptexextract  is  obtained
      by summing isomer group concentrations.  The e^stenc^of 209  possible
      PCB congeners makes the listing of the Chemical Abs^racfesN Service
      Registry Number (CASRN) for ea^r~p«4^ntial method analjct/ impractical.
      3.1.1.6.3   Because PCBs are \dei
      the non-specific CASRN for eachX
      describe method analytes.
                                     measuredTas  isomer  groups,
                               of c^lofTTKbtior/ is used to
      3.1.1.6.4   During optional screening utilizing GC/ECD analysis,  the
      individual Aroclors canjis^qualitative^y and quantitatively determined.
                                i.fied, and meas
                                   ncbrtrration
3.1.1.6.5   PCBs
level of chlorinat/lon;
group, and total
by summing isom
used as calibratio^i standards ,and one
is used to cal4brate\MS re4pc
require the use oi^ the
                           'concentration
                          toup concent
                               icor
                                       s isomer groups  (i.e.,  by
                                       asured for each  PCB  isomer
                                     sample extract is  obtained
                                    rne selected PCB congeners  are
                                   'rnal standard, chrysene-d12,
                       se to PCBs, unless sample conditions
                       internal standard, phenanthrene-d10.
   3.1.1.7
Detection Limits
                              mits va^yainong method analytes and with  sample
                                 procedures, condition of the GC/MS system,
                                  id individual samples.  The procedures  for
                                   thod detection limit  (MDL) for each  atxalyte
                                   ion is presented in Section  5, GC/MS
      3.1.1.7.:
      one instrumet
      comments are pro>
                       analyses of calibration  solutions  using
                      of approximately six months, .the  following
                to/assist the analyst:
July, 1991
                                                     Page  D  -  2/SV
-------
 Exhibit D
                                                       SOW No.  XXX -  Ambient Air
          3.1.1.7.2.1  Pesticide analytes other  than endosuifans  I  and II  can
          be identified and accurately measured  when the  injected aliquot
          contains 2 ng of each analyte.  The endosuifans/retire about 4  ne
          each.                                         /   /               &

          3.1.1.7.2.2  Detection limits for individual PCB conveners increase
          with increasing number of chlorine atoms, /itt/the detection limit
          for decachloribiphenyl being about 5-10 t/me/higheK±hantkat of a
          monochlorobiphenyl.   A monochlorobiphenyk^can be identified ai
          accurately measured when the injected e£hfact aliquot contHns 1
          and full SCAN data are acquired.
          3.1.1.7.2.3  The detection limit fo
          number of individual PCB congeners/pr
          from 1 ng to 10 pg.
                                 to/tal  PCB<
                                  sent.
                                                        >ill depend on the
                                                        PAHs, the MDL is
    3.1.1.8
Safety
       3.1.1.8.1    The toxicity or carcinogenicity^pf ea~bfa reagent used in
       this  method has  not been precisely defined;  however/^ach chemical
       compound should  be  treated as  apotential  health  Ra^ard^  From this
       viewpoint,  exposure to  theseVchernlcaii^must  be  reduceWo the  lowest
       possible level by whatever
       responsible  for  maintaining a\cur^ent~
       Safety and Health Administrati
       of the chemicals specified in  th\s  mXth?
       data handling sheets  (MSDs) shoul
       personnel involved  in the  chemical
       laboratory safety are^avaiiable and h\ve
       analyst.
                                8ust be reducec
                                            oratory is
                                              if Occupational
                                             ig the safe handling
                                    A reference file of material
                                   made available to all
                                 is.  Additional references to
                                  «en identified for the
      31.1.8.2    CareAus^ be  ex^rcfcSed^when wooing with these substances
      This method does/not^ purport/ to address^all of  the safety problems
      associated with/it/ use.  1/6 i/theN^spo/sibility of whoever uses  this
      method to consult4ica;bil/ty of regulatory limitations prior to  use
      The user should Bfexthorbughiy familiar with the chemical and physical
      properties of targete^substances.

      3 .1.1.8 JJx^TreataSl^nalytes  as^carcinogens.   Neat compounds  should
      be weirifed i*-!r^ve &*x.  Spe^/samples and unused standards are  toxic
      waste ^id/should be^spo^ed according to regulations.  Regularly check
      countert^ops and equipifcentWh "black light" for fluorescence as an
      indycat/r of semivolatil^ contamination.
3.1.2 Si
                .Method
           P>iRr  tSseld
       are cleaned in
is then spiked with^three
               ise
                                  the  filter  and  adsorbent  cartridge  (PUF/XAD-
                                  and  vacuum  dried.   The  adsorbent cartridge
                               rrogate compounds.   The  filter and spiked
                                                                 Page D - 3/SV
-------
Exhibit D
                               SOW No.  XXX -  Ambient Air
   adsorbent cartridge are stored in screw-capped jars wrapped  in  aluminum
   foil prior to installation on the sampler.
   3.1.2.2    Approximately 273 m3 of ambient air is
   and adsorbent cartridge at a rate of approximately,
   analytes of interest are retained.  At the end o
   period, the amount of air sampled is recorded,
   are placed in an appropriately labeled contain
   blank filter and adsorbent cartridges to the a'na
   analysis.
                                            the filter
                                            the
                                                  tridge
   3.1.2.3    The filters  and PUF/XAD-2 adsor^entt' cartridge^are extracted
   together by Soxhlet extraction with diethyl /ther/hejtaner solvent  (9:1 v/v) .
   The extract is concentrated using a Kuderna/Danish /K-PO evaporator,
   followed by silica gel  cleanup (optionaflj using calum/ chromatography to
   remove potential interferences.  The eluenx.is fhrther concentrated by K-D
   evaporation,  followed by nitrogen blowdown to^^l mL. \Prior to analysis by
   GC/MS,  internal standards are added to the concentrated
   3.1.2.4    If applicable,  the coi
   of PAHs,  pesticides,  PCBs/Aroclors,
   flame ionization detector (FID) ar
   final identification and quantifie
   capillary column,  temperature-progr^
   are then detected with a mass spectro1!
   acquisition mode.
                       extract is screened for levels
                and o~tKer--S3ZQCsutilizing a GC with a
                       ;ron capture~-de-£ector (ECD) .  For
                          ixt^ract^is/njected onto a GC
                            irate the compounds, which
                  tete
                         in the full SCAN data
   NOTE:   The method is baagqupon'xfull scanxiatax acquisition.
   3.1.2.5    Target comp'ou;
   standards under the /ami
   comparing resultant/ma,
   is established fo
   calibrations by
   the compound to
   standard.  Each identi
   comparing .the responses
   while taking into ac"
   calibration^ the_in_itial

   3.1.2.6
   mass
   Nation,
   Libra
   for the
   nearest  int"

 3.1.3  Interferences
 compou
 mpound
ndard./ A
        .idejxtJLfied iri\th/^ samples by analyzing
  analytical cond^tlpnsNased as the samples  and
s spectra and~SCretention times.  A response  factor
 targey compound eurjjig the initial and continuing
          response for the primary ion produced  by
         for the primary ion produced by an  internal
        et compound in a sample is quantified  by
            get compound and the internal standard,
 t theN^sports^ factor from the most recent
    id fin^k,sample volume, and any sample dilutions.

         are identified by comparing the resultant
         : compounds to mass spectra contained  in the
         and Technology (NIST) Mass Spectral
         re quantified by comparing the MS response
         s to the MS  response produced by the
        esponse factor of 1 is assumed.
                                ions
   3.1.3.1    Contaminants in solvents, reagents, glassware and other  sample
July,  1991
                                           Page D - 4/SV
-------
Exhibit D
            SOW No. XXX -  Ambient Air
   processing hardware may cause method interferences  such/as^discrete
   artifacts and/or.elevated baselines  in the  total ion current  profiles
   (TICPs).  All of these materials must be  routinely  demonstrated to be free
   from interferences under the conditions of  the  analysis Joy  running
   laboratory method blanks.  Hatrix  interferences may/be caused by
   contaminants that are coextracted  from the  sample./ The  extent  of  matrix
   interferences will vary considerably from source /to  zoui

   3.1.3.2    Interferences may be caused by conta&in^nts in solvents,
   reagents, glassware, and other sample processing^equipment.   Labor*
   method blanks are analyzed each analysis  to (demonstrate  that  these
   materials are free of interferences  under the analytical conditions used
   for samples.                                          ""

   3.1.3.3    To minimize interferences,  gl4ssv»are  should/be meticulously
   cleaned.  As soon as possible after  use^  rinseglassware with the  last
   solvent used.  Then wash with detergent I^hotSiater/and rinse  with tap
   water followed by distilled water.   Drain dryland h&at in a muffle  furnace
   at 450°C for a few hours (volumetric  glassware&femildS^t be  heated in a
   muffle furnace).   After cooling, store glassware irrvertedx«r  covered  with
   aluminum foil.   Before using, rin&e^each  piece  with  an^appropriate solvent.
   NOTE:   Some thermally stable materis
   by this treatment.   Solvent rinsed wi
   hexane may be substituted for the
such
 acetZ
  fur
as FCBs~Ti»y-_not be eliminated
        pesticide-quality
   3.1.3.4    For both pesticides and PCBV interference can be caused by the
   presence of much greater quantities of b£herNadditionar\sam^le extract preparation
   procedures must then be/used to Eliminate interferences.  Capillary column
   GC retention times anci the^c^m>^urtd^specif icXchairacteristics of mass
   spectra eliminate majply itoterfer&ncestfiaeure detection.  The approach
   and identification/criteria usied itt thi^methtod for PCBs eliminate
   interference by nj6st ^h^rina^ed/compoundsother than other PCBs .   With the
   isomer group approa<^ co^yting PCBs that contain the same number of
   chlorines are identified and measured together.  Therefore, coeluting PCBs
   are a problem only if they^cont^ina different number of chlorine atoms.
   This interferejie«— piKxb^lem isNabviabsd by rigorous application of the
   identification criteria""describe^L in phis method
                ,— \   x     \y
3.1.4 Definitions
      Definitions used in this \doovument and  in any user-prepared standard
   operaing >rocedures (SOPs) jshoiild be consistent with ASTM Methods D1356,
                       E255.  All /abbreviations and symbols are defined within
   this  document a t^sije point/of yuse .   A detailed glossary of terms can be
   found in Exhife-i^: G .

                   CAL: \Calib4at ion standards are defined in Table D/SV-1  in
Julv.
                                                                 Page  D  -  D/SV
-------
Exhibit D
                                   SOW No. XXX - Ambient  Air
      which 5 levels of calibration are defined: CAL 1,
      and CAL 5. • CAL 1 is the lowest concentration and
      concentration.  CAL 3- is designated as the solut
      continuing calibrations.

      3.1.4.2     Continuing  calibration check  (CCC,
      method analytes used to evaluate the mass sp
      period of time.  A continuing calibration c;
      12-hour period.  The CCC solution is the
      calibration curve.
      3.1.4.3
                                             CAL 3, CAL 4,
                                            is the highest
                                           be used for
                                                 olution  of
                                               onsexpver a
GC response (A^:  The peai
      3.1.4.5     Laboratory method blank (LMB):  An
      solution that is treated as a^sample.   It
      and apparatus,  and all raetho
      and surrogate compounds are
      final volume used for samples
      extract.   The purpose of the
      contamination.
      3.1.4.4     Internal standard (IS) : /A rfure comp'ounft added  to  a  sample
      extract in known amounts and used t«{calikrate /concentration
      measurements of other compounds  that arse sample components.   The
      internal standard must be a compound thatNj^s notAa^ sample component.
      3.1.4.6     Mass spectral interference: Defined as the inability  to
      detect the internal arSn^Srti. quantification ion due to presence of high
      levels of mass spec/ral "pois
      3.1.4.7     Meth/d
      value indicating: t
      identified and/me
      that the analyte
                 limit CMftL):  N( statistically determined
        minimum' conetM^tratibrrrof an analyte that can be
              /a sample fflai^i^ with 99  percent confidence
             iti(yn  is  greater  than zero.   This value varies
                                              extraction
                                          o it'll  glassware
                                      internal standards,
                                          entrated to the
                                           as  a  sample
                                       possible  laboratory
      with the precis
      calculation.

      3.1.4.8

      3.1.4.
      3.1.4.11
July,L991
                 licate measurements  used for the
                      atic hydrocarbon.

                      biphenyl.

               Luation (PE) sample:  A sample containing
                   analytes that has been analyzed by
                jrmine  statistically the  accuracy and
            pecked when a method is performed by a competent
              zation and concentrations are unknown to the
             Supplied by the Agency.

           rethane foam is used as  an adsorbent  and  support
                                               Page D - 6/SV
-------
Exhibit D
                                                SOW No.  XXX -  Ambient Air
      for XAD-3.
      3.1.4.12     Retention time  window:   Retention tim<
      each analyte of interest as the time from injecti
      specific chemical from a chromatographic column
      determined by three injections of a single compon
      hour period as plus or minus three times the
      absolute retention time for that analyte.
                                                       determined for
                                                 fen to  elution of a
                                                  THe^window is
                                                      standard over a 24
                                                       ieviatdon of the
      3.1.4.13     Selected  Ion Current  Profile /SlbP) :   A plot of ior
      abundances of the ions of an analyte projiuce4 by the mass spectrometer.
      3.1.4.14    Stock  Standard  Solution:
      calibration standards.  Normally,
      concentration which is easily dilute
      into the GC.
                                         splution rised to prepare
                                       solution will/be  at a
                                      t0 a  leve/ which can be  injected
      3.1.4.15    Surrogate compound:  A compound not^expected to be found in
      the sample that is added to each sample prior\to fi^Ul deployment and
      before extraction, and is measured with the same\mroceb;ures used to
      measure sample components.   Tke^Eurpose of a surroga
-------
Exhibit D
                   SOW No. XXX - Ambient Air
3.2   SAMPLE STORAGE AND HOLDING TIMES
    »

3.2.1 Sample Identification

   3.2.1.1    In the field,  the  samples are packed in
   glass sample container containing the filter and
   chilled,  and shipped to the designated laborato
                               insure  the
                                    e  are
   3.2.1.2    The  samples  are  logged in the Iaboc4to^y logbook  or  approp^ia;
   data tracking system according to sample location,  filter and adsorbent^
   cartridge number identification,  and total ^ir/volume sampled,  corrected to
   standard temperature and pressure (STP).  The/time  the/samples  are logged-
   in on the Chain of Custody  Log-In Sheet  a/t t#e laboraxor/y is the Validated
   Time of Sample  Receipt  (VTSR).

   3.2.1.3    If the  time  between  sample recent ancKanalysis is greater than
   24 hours, then  the samples  must be kept  refrigiaratedrxjMinimize exposure of
   samples to fluorescent  light.   All samples must De-vextra-Q^ed within five
   (5) days of VTSR.
3.2.2 Sample Storage

   3.2.2.1    The  samples  must be  con
   protected from light,  and refrigera
   receipt until 60 days  after  delivery
   Agency.   After 60 days, the  samples
   complies with all applicable  ^regulations^

   3.2.2.2    Samples musp^be
   of all potential contam

   3.2.2.3    Samples,
   separately.

3.2.3 Sample Extract
   3.2.3.1   .Sample  extracts
   (±2°C) until
   Agency.

   3.2.3.2
   be free
                         ss containers,
                 2°C)  from  the  time  of
                etc  data package  to  the
                    of in  a manner  that
                 e demonstrated  to be  free
               rds must be stored
   3.2.4.2    Extract:
   the extraction.
     rotected  from  light and stored  at  4°C
        a complete  data package  to the
 be  stored in an  atmosphere  demonstrated to
 nants.

 es

 be  started within 5  days  of the  VTSR.

./zed within 25 days  following  the  start of
July,  iyyi
                               Page D ^
-------
Exhibit D
                                                   SOW No.  XXX - Ambient Air
3.3   CARTRIDGE PREPARATION AND  CERTIFICATION

3.3.1 Summary of Method

      This part of the SOW discusses pertinent  inform^
   preparation and cleaning of the filter, adsorbent^
   cartridge assembly.  The separate batches of fil;
   extracted with the appropriate solvent.  At leajS
   cartridge assembly and one glass filter from
   the batch, whichever is greater, must be test
   batch is considered for field use.  The glas  c/rtridge is then assera%yed,
   extracted, and certified.    Prior to sampl^ng/the cartridges are spiked
   with surrogate compounds.
3.3.2 Apparatus and Materials
                                              incf
3.3.2.1    Acid-washed Pallflex filter:
Metal Works, Inc., Cat. No. GMW QMA-4, 145"xSxNo.  1-62, Supelco
   3.3.2.2     Polyurethane foam (P
   and 6.5-cm by 4.5-cm.   These c
   stock, polyether type  (density
   General  Metal Works,  Inc.,  Cat.
   of Cleves,  OH,  45002,  800-543-7412,
   Park,  Bellefonte, PA,  16823-0048,  or
   are also commercially  available from
   3.3.2.3     XAD-2  resin
   Bellefonte, PA,  16823/00.

   3.3.2.4     Aluminu
   rinsing  with hexai
                         SupelcoXlnc
                               eq

                           baked
 rates plugs/^e.5-cm by 2.5-cm
            3 inch thick  sheet
            iture upholstering,
            iami Ave., Village
   Inc., Cat. No. 1-63, Supelco
      The two separate plugs
 Metal Works.

No\ 2-02-79, Supelco Park,
 /ernight at 500"C after
   3.3.2.5     Sampling heacKcov(fi
   filter holder compartsient roL
   PUF and  XAD-2 adsorbentsV^as
                                .ration:  The sampling head consists of a
                              fowed by a glass cartridge for retaining the
                                 .strated in Figure D/SV-1.
   3.3.2.6     S'oxhlet extractors:
   and adsorb4nt/cTa~Ftr~t
               inivials:   2-
              lined with Teflo
                                     te of extracting GMW Model PS-1 filter
                                     tength),  500 mL flask, and condenser.
   3.3.2.
   3.3.2.9
                               rosilicate glass, with conical reservoir and
                             -raced silicone disks, and a vial holder.
                              50-mL.
July,L991
                                                               Page  D  -  9/SV
-------
Exhibit D
                      SOW No. XXX - Ambient Air
   3,3.2.10   Spatulas  ans  spoons:   Teflon®-coated stainless/steel.

   3.3.2.11   Kuderna-Danish  (KD)  apparatus:   500-mL evaporation flask (Kontes
   K-570001-500," or equivalent),  10 mL graduated concetttrato^vtubes  (Kontes K-
   570050-1025,  or equivalent)  with ground-glass stoDper^V^and J^ball macro
   Snyder Column (Kontes K-5700010500,  K-50300-0121  and K-SBSOOl-'HS, or
   equivalent).

   3.3.2.12   Absorption columns  for column chro^at^graphy:   1 cm x
   s tands.
   3.3.2.13   White  cotton gloves:   For hand

   3.3.2.14   Glove  box:   For  working with/ext<
   reagents with explosion-proof hood for
   reagents,  etc.

   3.3.2.15   Vacuum oven:   Vacuum  drying oven syste
   vacuum at 240 torr (flushed with nitrogen) overnight^
   3 . 3 .2 .16   Concentrator  tubes
   variable flow rate.
   3.3.2.17   Laboratory refrigerator.
                            'and  filters.

                            standards and
                              solvents,
   3.3.2.18   Boiling chips:   Solvent extr\cted/10/40 mesh silicon carbide,  or
   equivalent.
   3.3.2.19   Water bath:
   temperature control.
   3.3.2.20   Vortex
                               of maintaining a
                               ;
                        tion  apparatus:  with
                     ing  cover,  capable of ±5°C
   3.3.3
   with
   shallow tra

   3.3.3.6
   .hie  grade,  glass  distilled.

           hie  grade,  glass distilled.

  atographic grade,  glass distilled.

    Chromatographic  grade,  glass-distilled.

    drous (ACS),  granular (purified by  washing
   d by heating at 400°C for 4 hours in a


urity grade.
 July,  1991
                                 Page D  -  LO/SV
-------
Exhibit D
                     SOW No. XXX - Ambient Air
3.3.4 Procedures  for  Preparation  of  Filter,  Adsorbent,  and/Cartridge

   3.3.4.1    Glass Fiber Filter Preparation
      3.3.4.1.1    The quartz fiber filters are baked
      before use.  To  ensure  acceptable  filters,  the
      methylene chloride  in a Soxhlet  apparatus,
      the XAD-2 resin.  The extract may  be  analyze
      determining  cleanliness prior to certificat
                              for five hours
                                    with
                                         of
      3.3.4.1.2    The extracted filters are set: as
      prior to combined extraction with the  PUF/X/D-2/PUF  glass  cartridge
      assembly.                                          "

   3.3.4.2    XAD-2 Adsorbent Preparation

      3.3.4.2.1    For initial cleanup of theOCAD-^^wresfn,  a batch of XAD-2
      (approximately  50-60 grams) is  placed  iri^a^Soxhl^ apparatus  and
      extracted with  methylene chloride  for  16 houts at  approximately 4 cycles
      per hour.
      3.3.4.2.2    At  the  end of the initial
      methylene chloride  is discarded'
      XAD-2 resin  is once again ext
      cycles per hour.

      3.3.4.2.3    The  XAD-2  resin is  remWec
      placed in a vacuum oven connected to\
      and dried at room tempefatttr^ for appi
      solvent odor is detected).
                    extracti
                      at
                  the spent
              h reagent.   The
              proximately 4
               >m the Soxhlet apparatus,
                   -pure nitrogen gas  stream
                 tely 2-4 hours  (until no
iltra
      NOTE:  Alternati
                      /  " J •       I
      with methylene chloride for /
      transferred to /a. <^lean dry^tij
      high-purity n/tro
      with a charcoa
      the XAD-2 resin is
      sufficient space for fiuidiz"
      maintained^*—49^0^ durir?
                   resin  is Soxhlet-extracted
                r extraction,  the  resin is
    o lumn'N^TWn the resin is  dried with
   Ion® tubing from the nitrogen cylinder
  ine. In an alternative  method of drying,
TI a Pyrex® column (10 cm  x 60  cm), allowing
       The column is wrapped with  heat  tape,
the ""Shaving process.  High purity air,
      scrubbed/through a charcoal>^ap, >s forced through the resin bed,
      fluidizang>cKe~BeTKwhilev genera^Wg a minimum load at the exit of  the
      colum-7  /        ^    ^

      3.3/4.2/.4    The  extract Y^oin  the Soxhlet  extraction procedure  from each
      ba/ch bay be .analyzed  ugjind GC/FID or GC/ECD (see part 3.6) or by GC/MS
      (see^part^^S) ,  for the ^ur^ose  of determining initial cleanliness prior
      to cerbificatlsm.
July.
                                Page  D  -  11/SV
-------
 Exhibit  D
                                                      SOW No.  XXX - Ambient Air
3.3.4.3    PUF Adsorbent Preparation

   3.3.4.3.1    The  PUF adsorbent is a polyether-type/po
   (density 0.0225 g/cm3).

   3.3.4.3.2    The  PUF adsorbent is composed of
   illustrated in Figure D/SV-2.  The bottom PUF,
   the top plug is 6.5-cm by 5.0-cm.  The PUF
   stock and should fit with slight compressi
   supported by the wire screen.  The two PUP p
   inch deep) are also commercially available
   from General Metal Works.
                                                              .rethane foam
                                                                          while
      3.3.4.3.3    For initial cleanup,  the
      apparatus and extracted with ace tonefpr
      cycles per hour.  When cartridges are ri
      v/v) can be used as the cleanup solvent.
                                                    gs  (i.e.,  1-inch  and
                                                    pre-cu-t separate  pieces
                                                    ire /laced  in  a  Soxhlet
                                                  ts at approximately 4
                                                      iyl ether/hexane (1:19
   NOTE:   A modified PUF cleanup procedure can be usea^to remove unknown
   interference components of the/TtfF-bJ^nk^  This methocKcoftsists of
   compressed rinsing 50 times w/th toluene7~^rB*^or scainiess steel  screen  (mesh size 200/200)  is
      fitted to the bo ctx*mof>a/heptane-rinsed glass sampling cartridge to
      retain the PUF/XAD-2>a4sorbe-qts,  as illustrated in Figure D/SV-1.  A
      Soxhlet-extracted, vacuutoKdrie^xPUF (2.5-cm thick by 6.5-cm diameter) is
      placed on iKJpof "^Rfrv^creenXn the^glass sampling cartridge using
      polyestf^ ""           ^      \    7
             '  Y      ^\  \
                                   g of 35/60  mesh Soxhlet-extracted,  vacuum
                                   nto  the sampling cartridge (using clean
                                   if the PUF.  A second Soxhlet-extracted,
                                   .5-cm x 5.0-cra) is placed on top of the
                                   ,e top nickel or stainless steel screen is
                                  idge.
                  \  \V  /
      3.3.4.4.3   The>4^ss module containing  the PUF/XAD-2 adsorbent  is
      wrapped with hexane^n^ed aluminum foil, placed in a labeled container
      and tightly sealed with Teflon® tape.
Jul
                                                                Page D - 12/SV
-------
Exhibit D
                                                      SOW  No.  XXX -  Ambient Air
      NOTE:  The aluminum foil should be baked in an oven
      after rinsing with hexane to insure that no residu

3.3.5 Procedure-for Certification of PUF/XAD-2 Cartrid
   3.3.5.1    The  filters  and PUF/XAD-2  adsorbent are
   extraction and concentrated using a Kuderna-Danis
   does  not have to be cleaned by the optional sili
                                                            •night at 500eC
                                                           emain.

                                                        jsemblies
                                                              by Soxhlet
                                                                 The extract
   3.3.5.2   Assemble  the Soxhlet apparatus.   C
   with 300 mL  of the extraction solvent and re
   apparatus cool,  disassemble it, and discard
   Transfer the filter  and PUF/XAD-2 glass ca/tr
   (the use of  an extraction thimble is opti

   NOTE:   The filter  and adsorbent assemb
   reach detection limits and to minimize
   3. 3. 5.. 3    Add  300 mL of diethyl ether/hexan*
   apparatus.   Reflux the  sample  for  18  hours  at
   per  hour.  Allow to  cool,  then disassemble  the  appal
  3.3.5.4    Assemble a K-D concentrator
  tube  to a  500-mL  evaporative  flask:
  techniques may be used  in place tff t
  for all the  target analyte  compounds  £
                                                 used extraction solver
                                                   to the  Soxhlet apparatus
                                                        ether  in order to
                                                         to  the Soxhlet
                                                         at  least  3  cycles
                                                ing a 10-mL concentrator
                                           concentratrreH^devices  or
                                                  ivalenfcy is demonstrated
                                       kstedinExhibit C.
  3.3.5.5    Transfer the extract by pouYing tKe extract through a drying
  column containing  about 10  cm  of  anhydrous granular sodium  sulfate,  and
  collect the extract in th€nrTXconcentraCor7\Rinse the  Erlenmeyer  flask
  and column with 20 to 2(0 mL_of 1& percent dietftylether/hexane to complete
  the quantitative trarysfe)
  3.3.5.6    Add one far. ifwo clea:
  Snyder column to tme /evaporat;
  adding about 1 m^ of Sstje extj
  Place the K-D apparatus
  tube is partially immetsed  in
  surface of the flask is Bached
  position of the—apparatus an
                                        chip^and attach a three-ball
                                  :lask.^\gre/wet the Snyder column by
                                 on solvent to the top of the column.
                                 water bath (50°C) so that the concentrator
                              .the hot water, and the entire lower rounded
                                    hot vapor.  Adjust the vertical
                              ,£he water temperature as required to complete
  the concentration_in on>xhour. ^At th£ proper rate of distillation,  the
  balls of trfie Gt5lurniT>MA actively dhdtter but the chambers will not  flood
  with condensed solvent . N^herK the apparent volume of liquid reaches  5 mL,
  remove Ae /K-D apparatus fXomVhe water bath and allow it to drain and cool
  for a-t/lea'st 5 minutes.  Reiovd the Snyder column and rinse the flask and
  its l^wer^^int into the concentrator tube with 5 mL of cyclohexane.  A  5-
  mL syrime is^ecommended fbr this operation.
3.3.5.7
obtain a final volume
techniques.  These pi
                            ypes of concentration techniques are permitted to
                        o  1 .10 mL:  micro-Snyder column and nitrogen blowdown
                         edu/es are outlined in parts 3.4.4.2.4 and
uly,
                                                                Page  D  -  13/SV
-------
Exhibit D
                                                   SOW No. XXX  - Ambient Air
3.4.4.2.5, respectively.

3.3.5.8    Technical Acceptance Criteria

      The  level  of  target compounds must be less
   each pair of  filter  and adsorbent assembly at
equal to 10
                                                                            for
   3.3.5.9
           Documentat ion
         Reporting requirements are  listed  in Exhibit B.
3.3.6    Deployment of Cartridges for Field
                                              Ling
3.3.6.1    Prior to field deployment, a/min4mum  of /thr;
compounds are added to the center bed
microsyringe.  The surrogate  compounds  (iT^^.  chemic
not expected to occur in an environmental  samp^iej mx;
cartridge assembly.
                                                          e surrogate
                                                         artridge,  using a
                                                         ly inert compounds
                                                          be added  to  each
   3.3.6.2    The recovery of the sufrcrga-ce^standard is use^xt^ monitor  for
   unusual matrix effects and gross' sampling proc~s*sin£errors.  Surrogate
   recovery is evaluated for accept^ce\Ey~~'*le-tej3iiining whet^fer the measured
   concentration falls within the acceptance limits
3.3.6.3    The following surrogate
determining matrix effects, breakthrouf
GC/MS.  Refer to part 3 . 5-S^JJ^ f or prepai
mixture.

       Surrogate Comp
13C6-Gamma-BHC
13C12-4,4'-DDT
13C6-4-monochloroh
13C,2-3,3' ,4,4'-tee
13ci2-2,2' ,3,3' ,5,5' ,
13C12-Decachlorobiphenyl
Nitrobenzene-d
2-Fluorobip
p-Terpheny
2,4,6-Tripromophenol
2-Fluor
Phenol-,
                                                 ave been successfully used  in
                                                 analytical problems, by
                                                  of surrogate spiking
                                            SpikVd Amount  (qg/cartridee)
                                                         50
                                                          5
                                                        100
                                                        250
                                                        400
                                                        500
                                                        100
                                                        100
                                                        100
                                                        100
                                                        100
                                                        100
   3 . 3 . 6 ^\  At^a minimum, the/following three surrogate  compounds  must be
   added to e^tQh adsorbent car/tri/ages at  the  concentrations  indicated:
July,  1991
                                                              Page  D  -  14/SV
-------
Exhibit D
                                                      SOW No.  XXX -  Ambient Air
   Surrogate Compound

   Nitrobenzene-d5
   2-Fluorobiphenyl
   p-Terphenyl-du
                               Spiked Amount (qg/cartridge
                                          100
                                          100
                                          100
3.4   SAMPLE PREPARATION FOR GC/MS ANALYSIS

3.4.1 Summary of Method

      The filters and adsorbent cartridge are
   with appropriate solvent.   The extract is c/e
   (K-D)  evaporator,  followed by optional
   chromatography to  remove potential interf/eref
   cloudy),  optional  GC/ECD/FID screening,
   illustrated in Figure D/SV-3.

3.4.2 Apparatus and Materials
   3.4.2.3

   3.4.2.4

   3.4.2.5
             Glass vials

             Erlenmeyer

             Spatulas
   3.4.2.6    Kuderna.
   (Kontes K-570001-
   (Kontes K-570050^
   ball macro  Snyder  Co
   219,  or equivalent).
   3.4.2.7
   stands.

   3.4.2.8
                           umns
                                                                            on
                                                   itrated by Kuderna-Danish
                                                           Lica gel column
                                                            extract is
                                                          US analysis, as
   3.4.2.1     Soxhlet  extractors:   Capable  of  extract
   and adsorbent  cartridges  (2.3  in.  x 5  in.  length),  si
   condenser.

   3.4.2.2     Pyrex glass  tube  furn
   180°C  under purified  nitrogen  gas
   raising  temperature gradually, best
                                                              odel PS-1 filter
                                                               •ask,  and
                                                            ng silica gel at
                                                           :h the capability of
                 tainless  steel.

              JO-mL evaporation  flask
            •/graduated concentrator tubes
(lent) with  ground-glass  stoppers,  and 3-
 K-5700010500,  K-50300-0121,  and K-569001-
       m chromatography:   1  cm  x  10  cm with
                                   For handling cartridges  and  filters.

                                  osilicate glass, with  conical reservoir  and
                                  ced  silicone  disks,  and a  vial holder.

   3.4.2.10   (Jbove bo>^:   Fo/working with extremely toxic standards  and
   reagents  with  e^p^osiohxproo'f hood  for venting  fumes  from solvents,
   reagencs,  etc.
July,
                                                                Page D - 15/SV
-------
Exhibit D
     SOW  No. XXX -  Ambient Air
   3.4.2.11   Vacuum oven:   Vacuum drying oven system capa#le/of maintaining a
   vacuum at 240 torr (flushed with nitrogen) overnight.
   3.4.2.12   Concentrator tubes and a nitrogen evaporation
   variable flow rate.

   3.4.2.13   Laboratory refrigerator.
                       With a
   3.4.2.14   Boiling chips:   Solvent extracted
   equivalent.

   3.4.2.15   Water  bath:   Heated,  with conce/tr
   temperature control.

   3.4.2.16   Vortex evaporator (optional)
   NOTE:   Reuse of glassware should be minimize
   contamination.   All glassware that is used, espec"
   reused, must be scrupulously cleaned as soon as
   glassware with the last solvent u^i&d—in__ it and then wit
     mesh silicon car
               .e, /or
            ,  capable of ±5°C
  poss]
the risk of cross-
   ssware that is
      r use.   Rinse
      -purity
   acetone and hexane.   Wash with hot water containingdetergent.  Rinse with
   copious amounts of tap water and\sev^?a-t—pxirtions of~dT5~frjLlled water.
   Drain dry and heat in a muffle furnace^ at 400?C £o¥-Jt^hop'rs.   Volumetric
   glassware must not be heated in a muffr& furnace; rather, it should be
   rinsed with high-purity acetone and n^xane/  After the glassware is dry and
   cool, rinse it with hexane, and store £t inverted or capped with solvent-
   rinsed aluminum foil in a clean environmfe

3.4.3 Reagents

   3.4.3.1    Soxhlet E*tr
raphic grade,  glass-
      3.4.3.1.1
      distilled.
       3.4.3.1.2    Sodium'^Sulfate £  Anhydrous (ACS),  granular (purified by
       washing with methylenecbAorib^followed by heating at 400°C  for  4  hrs.
       in a  shal]

                   —    \     "   >W
                                   Chromatographic grade,  glass-discilled.

                               xomatographic grade,  glass-distilled.

                                gh purity grade.

                                  hromatographic grade, glass-distilled.
 July.  1991
                Page D - 16/SV
-------
 Exhibit  D
                                                   SOW No.  XXX -  Ambient Air
   3.4.3.2    Extract Cleanup:  Federal Reference Method 6
                                                            70-230 mesh; pre-
                                                           ride  for  6  hours
                                                              in  a  foil-
   3.4.3.2.1    Silica gel:   High purity grade,  type
   extracted,in a Soxhlet apparatus with  methylene
   (minimum of 3 cycles per hour)  and  activated by
   covered glass container for  24  hours at  180"C.

   3.4.3.2.2    Sodium sulfate:   Anhydrous gram
   450°C for 8 hours prior to use  to activate

   3.4.3.2.3    Pentane:   Chromatographic  gr&de/ glass-distilled.

3.4.3.3    Extract  Cleanup:   Lobar Prepacked /Column

                                           :olumn: /E./Merck,  Darmstadt,
      3.4.3.3.1    Silica gel Lobar prepac
      Germany  [size A(240-10) Lichroprpe
      3.4.3.3.2    Precolumn containing sodium^
      (purified by washing with methylene chloric
      400°C for 4 hours in a shallow tray).

      3.4.3.3.3    Hexane:   Chromatfograp

      3.4.3.3.4    Methylene  chlori
      distilled.
                                                      Granular,  anhydrous
                                                         by heating at
      3.4.4.1.2   Assernl
      apparatus with 300 mi
      Lee the
      adsorbe
      chimb1
      3.4.3.3.5   Methanol:   Chromatogr

3.4.4 Procedure

   3.4.4.1    Soxhlet  Ex^rac^ion

      3.4.4.1.1   The,
      Soxhlet extrac
      in Figure D/sV-
                                           g/ade, glass-distilled.
                                             rbent are extracted by
                                             -D evaporator,  as illustrated
July, 1591
      3.4.4;-
      Figure
      same concentration
                              xhlet apparatus.  Charge the Soxhlet
                                 xtraction solvent and reflux for 2 hours.
                              as salable it, and transfer the PUF/XAD-2
                                       apparatus (the use of an extraction
                               ent are analyzed together in order to reach
                               on Limits (CRQLs),  to avoid questionable
                               and to minimize cost.

                          traction, additional surrogate standards  (see
                               to the Soxhlet extraction solvent at the
                            lined in part 3.4.4.6.   The recovery of the
                                                             Page D - 17/SV
-------
Exhibit D
                                        SOW No.  XXX -  Ambient Air
      surrogate standards are used to monitor for unusual/matrix effects,
      gross sample .processing errors, problems with they&na^ytical method,
      etc.  Surrogate recovery is evaluated for acceptance/by determining
      whether the measured concentration falls within/the Sa^ceptance  limits.
                                                    /  /^
      3.4.4.1.4    Add 300 mL of  diethyl  ether/hexa:
      apparatus.  Reflux the sample for 18 hours
      cycles per hour.  Allow to cool then disas
   3.4.4.2
Concentration and Solvent Exchan;
                                                     .phe Soxhlet
                                                          3
      3.4.4.2.1    Assemble  a Kuderna-Danish
      10-mL concentrator tube to a 500-mL
      concentration devices or techniques /may(
      equivalency  is demonstrated for al
      in Exhibit C.
      3.4.4.2.2    Transfer  the  extract  by pouring
      drying column containing about 10 cm of anhydrdl
      sulfate, and collect the extract^inthe K-D
      Erlenmeyer flask and column/with 20~Eo~-3Q~jaLof 5 to
      ether/hexane to complete the\ quantitative trans!
                                              tor by attaching a
                                                 Other
                                             lace of the  K-D,  if
                                           .yte  compounds listed
                                     concentl
                          ict through a
                                sodium
                                Rinse  the
                              diethyl
      3.4.4.2.3    Add one  or  two  cle
      Snyder column to the evaporative
      adding about 1 mL of the extractio'
      Place the K-D apparatus on a hot wa
      concentrator tube is
      lower rounded surfafce
      vertical position/of /€he appar
      to complete the siona4ntrati
      distillation, ttfe balls of
      chambers will/not/flood wi
      volume of  liquid reaches
      bath and allow
      Snyder column and
      concentrator  tube wit
                           ope
      concent^ktion_to l.O^L by

      3.4.
                        immers«
                  the^flask  is
               clylps and^attach a three-ball
                  -wet the Snyder  column by
         solve/nt  to  the top of  the  column.
               th  (50°C) so that the
                the  hot water,  and  the  entire
                  with hot vapor.   Adjust the
        and tfte witer temperature as  required
                  At  the proper  rate of
                actively chatter  but  the
               vent.  When the  apparent
mfc,  remove tfie K-D  apparatus  from the water
 ,nd  cool for  at least 5 minutes.  Remove the
 flask  and its lower joint into the
     cyclohexane.  A 5-mL syringe  is
ion.\The extract is now ready  for  further
e'i-cherjof the two following techniques.

olumn Technique
                                   one  or  two  clean boiling  chips  to  the
                                   ach  a two-ball  micro-Snyder  column.

                                4  Snyder  column by adding about 1 mL of
                          he/top^ of the column.
 July,  1991~~~Page D -  LS/SV
-------
Exhibit D
               SOW No.  XXX -  Ambient Air
         3.4.4.2.4.3  Place the K-D apparatus on a hot wae€r\bath  (50°)  so
         that the concentrator tube is partially immersejz in/hot water.

         3.4.4.2.4.4  Adjust the vertical position of ,dhe/apparatus and  the
         water temperature is required to complete the concentration  in  15 to
         20 minutes.   At the proper rate of distillationxthe nulls of the
         column will actively chatter but the chamber s/wiHxnot rioted with
         condensed solvent.

         3.4.4.2.4.5  When the apparent volume <6f liquid reaches aboutx^. 5/mL,
         remove the K-D apparatus from the wat^r Vath and allow it to drMn
         for a least 10 minutes while cooline
         3.4.4.2.4.6  Remove the Snyder co
         lower joint into the concentrator' t
                                        (
         3.4.4.2.4.7  Adjust the final vol
         NOTE:   It is not necessary to bring the volume
         the extract will be cleaned up by either of
         cleanup methods.

         3.4.4.2.4.8  Transfer the\ex
         vial,  label the vial and score
        'and rins'e ifts flask and  its
       je with/0.2/mL of cyclohexane.
      3.4.4.2.5   Nitrogen Slowdown Te
        (from ASTM Method D3086)
3.4.4.2.5.2
rinsed down severa

3.4.4<2.5.3
below chewatei
tc/be/ome dry.
                 w i th eye1ohexane.

                    exactly 1.0 mL  if
                  optional silica gel
                     d screw-cap amber
      CAUTION:   Gas  lines from the gas source T:O the blowdown apparatus must
      be  stainless  steel, je-6pper>sor Teflon\tubr*ig.
                        /   ^—\
         3.4.4.2.5.1
         attachment  i
         solvent vol
         clean,  dry
         above  the
      tiibe ywith an open micro- Snyder
       to\35°C) and evaporate the
         •owing a gentle stream of
        'a column of activated carbon)
                                   wall of the concentrator tube must be
                                    tith cyclohexane during the operation
                               of the
   the tube solvent level must be kept
"ath.  The extract must never be allowed
        /3.4/4.2.5.4  Bring thW final volume brought to 1.0 mL with
         cycrsjexane.   Transfei: tie extract to a Teflon-sealed screw-cap amber
                                  store at 4°C (±2°C) .
July, 1991
                          Page  D  -  19/SV
-------
Exhibit D
                                                      SOW No.  XXX -  Ambient Air
         NOTE:  It is not necessary to bring  the volume  toi exactly 1.0 mL if
         the extract will be cleaned up by either of the/Optional  silica gel
         cleanup methods.  Final volume is brought to 1/0  ml, after cleanup.
   3.4.4.3    Extract Cleanup (Optional):   Federal Reference Method 610
                                                         particr
NOTE:  Other extraction procedures can be used
laboratory demonstrates equivalency.

   3.4.4.3.1    Pack a 6-inch disposable Paspeur/pipette (10 mm ID x 7
   length) with a piece of glass wool.   Push  tbfe wool  to  the  neck of the
   disposable pipette.  Add  10 grams of  aotiv/ted sil£ca>gel  in methylene
   chloride slurry  to  the disposable pipe'tte/ Gently  t^p  the column to
   settle the silica gel and elute the m4th^lene chloride.  Add 1 gram of
   anhydrous sodium sulfate  to the top 4*f the^sj-lvca £^ column.

   3.4.4.3.2    Prior  to  initial  use,  rinse  th^columri with methylene
   chloride at 1 mL/min for  1 hr. to remove any o&ace  of\contaminants.
   Pre-elute the column with 40 mL of pentane.  Disc^a*^ the\eluate.  Just
   prior to exposure of the  sodiunr-suJ^gate layer to the^a^r/ transfer  the
   cyclohexane sample extract orito the coTunlTir--uaing an additional 2 mL of
   cyclohexane to complete the tXans^r^-^Aj.lpw toeTute-Tthrough  the
   column.  DO NOT ALLOW THE COLOTTO T\ DRY.

   3.4.4.3.3    Just prior to exposure^ of\^fe  /odium sulfate layer to the
   air, add 25 mL of pentane and continue eluxion of the column.

                        let ion
      NOTE:   The pentane f
      collected on the fi/ter.
      normally discarde
      specific aliph
      chloride/pentane/ (4/6 v/v)
      equipped with a/10/mL conc^
      mtains tfte aMphatic hydrocarbons
   :orb^snt combinavtioX,   This fraction is
interes|t>dT^this Crac/ticn may be analyzed for
                column with 25 mL of methylene
                   'eluate in a 500 mL K-D flask
                      oirganics.  ) Elute
                                       tct the
                                  itor
      3.4.4.3.4   Cone
      apparatus,  using
      extract is  now ready
      by GC/MS
                            the
                    per
   3.4.4.4
    collected fraction to 1.0 mL by  the  K-D
    rinse the walls of the glassware.  The
          GC/FID or GC/ECD screening, followed
                                 tional;
                                        Lobar Prepacked Column Procedure
                                   the  Lobar  prepacked  column consists of an
                                    pre-column containing sodium sulfate,
                                   Ivent reservoir.

      3.4.4.4?2v.  ThVvColumn As /leaned  and  activated  according to the
      following cbsanup
July, 1991                                                 —	Page  D  -  20/SV
-------
Exhibit  D
                                                      SOW No.  XXX - Ambient Air
   Fraction

      1
      2
      3
      4
      5
      6
                 Solvent  Composition
Volume (ml
             100% Hexane .
              80% Hexane/20%  Methylene Chloride
              50% Hexane/50%  Methylene Chloride
             100% Methylene Chloride
              95% Methylene Chloride/5% Methanol
              80% Methylene Chloride/20% Methano
      3.4.4.4.3    Reverse the sequence at the e
      the 100 percent hexane  fraction  in  order
      Discard all  fractions.   Pre-elute the colum
      is also discharged.
                                                    the run, and
                                                Activate the column.
                                                 with 40 mL of hexane, which
      3.4.4.4.4    Inject 1 mL of the cyclofiexane sample extract from
      3.4.4.2.4 or 3.4.4.2.5, followed by/a l^mL  injettLon of blank
      cyclohexane.  Continue elution of tW^columia^yith/20 mL of hexane, which
      is also discharged.  Now elute the colutoqwith lAo mL of  a mixture of
      methylene chloride/hexane  (4:6 v/v) respectively/XCollect approximately
      180 mL of the methylene chloride/hexane mixturexin aSc^D  concentrator
      assembly.  Concentrate to  1.0 mL with the K-D assembly/'}'The extract is
      now ready for optional GC/FIlTor~-S6/EC]^_screening andX#/MS analysis.

3.5   GC/MS ANALYSIS

3.5.1 Summary of Method

      This method outlines a GC/MS procedure fc
   pesticides,  PCBs/Aroclors^-aad other serniyol
   preparation  (Section 4V/or optional scree
                                              ng
                                               the  analysis  of PAHs,
                                               Lies  following  sample
                                               ^Section 6).
3.5.2 Interferences
   3.5.2.1    Method /ntatference^  may" bes-c^used/by contaminants  in solvents,
   reagents,  glassware,
-------
Exhibit D
                                        SOW No.  XXX -  Ambient Air
   placing in a muffle furnace at 450°C for 8 hours to re

   3.5.2.3    The use of high purity water,  reagents,
   minimize interference problems.  Purification of s
   in all-glass systems may be required.

   3.5.2.4    Matrix interferences may be caused b
   coextracted from the sample.   Additional clean)
   may be required (see parts 3.4.4.3 and 3.4.4./).
                                                 trace  organics.

                                              ilvents helps  to
                                                   distillation
   3.5.2.5    The  extent of interferences that/ma/ be enc
   fully assessed.  Although GC conditions
   resolution of compounds covered by this method,  othe
   interfere.   The use of column chroma to gifaphyf or sampl
   analysis will eliminate most of these i
   must,  however,  be routinely demonstrated tb\be free
   contaminants such as contaminated solvents,  g
   which may lead to method interferences.  A labora
   for  each batch of reagents used to determine if reaget
   free.
                                              tered has not been
                                                 unique
                                             impounds may
                                             cleanup prior to  GC
                                           The analytical system
                                          f internal
                                            or other reagents
                                               pd blank is run
                                                  ; contaminant-
   3.5.2.6
There are concerns
      3.5.3.1.1   Gas
      temperature-pr
      injection and
      columns,  and
      column flow rate thr
      carrier- gas -lj.nes_ must
      tubing.
      controllers wi-th-jrubbe
   heat,  ozone,  N02, and ultraviolet
   These  problems should be addressed
   Where  possible,  incandescent or UV-j
   laboratory should be used during analyses.

3.5.3 Apparatus and Materi
   3.5.3.1
                               and analysis,
                               le degradation.
                    .e user-prepared  SOP manual,
                   .orescent  lighting in the
Gas Chromatfog
                     C/MS) System

                   al system complete with a
                   suitable for splitless
     'cessories,  including syringes,  analytical
     a flow controller  that maintains a constant
     ^emperature  program operations.   All GC
         .cted from stainless steel  or copper
             (PTFE) thread sealants or flow
components/are not to be used.
      must allow a
      elutes  fro-
      demonsc:
                .ome'ter:  Capable of scanning from 35 to 500 amu
                  tiiizing 70 volts (nominal)  electron energy in
                   tipn mode and producing a mass  spectrum which
       instrumentyperlformance criteria when 50 ng  of
       henylphosp^inei (DFTPP) is injected through  the GC inlet.
                 ci/ion of mass spectral data,  the MS scan rate
                   at least five scans while a sample compound
              The/GC/MS system must be in a room with atmosphere
              .ee/of all potential contaminants which will
July,  1991
                                                   Page D - 22/SV
-------
Exhibit  D
                                                      SOW No.  XXX - Ambient Air
       interfere with  the  analysis.   The  instrument must be
       facility or  to  a  trapping  system which prevents the
       contaminants  into the' instrument room.

       NOTE:  DFTPP  criteria  must be  met  before  any s
       analyzed.  Any  samples analyzed when DFTPP cri
       will require  reanalysis at no  cost to the
                                                             inted outside the
                                                             l/ease of
                                                                    are
                                                               not  been met
      3.5.3.1.3    GC/MS interface:   Any gas chron
      spectrometer interface  that gives  acceptable
      ng or less per injection,  for  each of the/pa/ameters  of interest,
      achieves all acceptable performance cri&erLa  (Exhibit E),  may be used.
      Gas chromatograph to mass  spectrometer/interfaces/^obstructed of all-
      glass or glass-lined materials are recommended.  /Glass can be
      deactivated by silanizing  with dichlprodamethylsdla^ie.

      3.5.3.1.4    Data  system:   A computer"••s^rstemNnust/be interfaced to the
      mass spectrometer that allows  the  continuous  acquisition and storage on
      machine readable media of  all mass spectra  ob^ainecKsAroughout the
      duration of the chromatographic program.  The cbHmuter^must have
      software that allows searchina-j£he_GC/MS data file^&^r i^ns of a
      specific mass and plotting such iorPlbrHwiaoces versus tame or scan
      number.   This type of plot is: de^fiaedas anSe*teTrte
-------
Exhibit D
                                                      SOW No.  XXX -  Ambient Air
   3.5.4.3    Zero air:  May be obtained from a cylinder or zero-grade
   compressed air-scrubbed with Drierite or silica gel a/d 5A molecular sieve
   or activated charcoal, or by catalytic cleanup of ambient air.  All zero
   air must pass through a liquid argon cold trap for /£inalxcleanup.
                                                    /  ^
   3.5.4.4    Native and isotopically labeled analytre
   calibration and spiking standards, Cambridge Iseto
   Woburn, MA, 01801, 617-547-1818.

3.5.5 Standards
   3.5.5.1    The Contractor must provide all/ standards /o^e used with this
   contract.   These standards may be used oidy/after they Kave been certified
   according to the procedure in Exhibit E/  "me Contractor must be able to
   verify that the standards are certified.  Mahufaccurst's certificates of
   analysis must be retained by the Contracb>r and^-pjresented upon request.

   3.5.5.2    In order to facilitate the confirmation of  "p^asticides,  PAHs,
   PCBs,  and other SVOCs from the library search dataSthe  calibration
   standards  must include the single—cojggonent target compv»und/ in one
   standard solution in each conce/trationT?eVe-l-r^_and the noucicomponent
   analytes in separate standard s^ut^rns-jj^one concerttretion level.  Each
   calibration standard solution mus\cantainaJl cfe*-_aporopriate surrogates
   and internal standards.

   3.5.5.3    When compound purity is assayed7 tc/be 98  percent or greater,  the
   weight may be used without correction tk calculate the concentration of the
   stock solution.  If they
-------
Exhibit D
                                                SOW No.  XXX -  Ambient Air
   3.5.5.6
        PAHs  Stock Standard Solutions
                                                             luminum weighing
3.5.5.6.1   Place  0.1  gram  of native PAHs on a ta^ed
disk and weigh on a balance.

3.5.5.6.2   Quantitatively,  transfer each to
Rinse the weighing disk with several small po
chloride.  Ensure all material has been tra
with methylene chloride.  The concentratio
solution of PAHs in the flask is 10 UK/I
      3.5.5.6.3   Transfer  the stock  standard/solutions into Teflon-sealed
      screw-cap bottles.  Store at 4°C and protect from/ligiit.  Stock standard
      solutions should be checked frequently for signs /of /degradation or
      evaporation,  especially just prior t.p preparing/caibration standards
      from them.

      3.5.5.6.4   Secondary standards may be pr^&gared'•by diluting  the  stock
      standard solutions.  Working standards are tbar^ prepared from  the
      secondary standard solutions.
   3.5.5.7
       Pesticides  Stock Standard Solul
      3.5.5.7.1   Prepare from pure
      25.0 mg (with accuracy of 0.1 m
      Endosulfan I and Endosulfan II.
      stock solution twice as concentrated as
      pesticide analytes.   Dissolve each c
      volume in a 10-mL
      (Concentration of
      which should be S/rag/^fL.)  >ma).lex^or lari
      may be used if d<
                                          ier/tali.   Weigh approximately
                                                    cide analyte, except
                                           two pesticides, prepare a
                                           t prepared for other
                                            in hexane and dilute to
                                           fans) volumetric flask.
                                              except the Endosulfans,
                                             Volumes of stock solution
      3.5.5.7.2   Transfer the
      screw-cap bottles ?\Storey
      solutions shouldxbe cnecjced
      evaporation,  especra^ly jus
      from them.
                               stanc
             zx>lutions into Teflon-sealed
   'C  and  protect from light.   Stock standard
/frequently  for  signs  of degradation or
 prior  to preparing calibration standards
                             tandai
                           Working stai
   3.5.5.
                                    be  prepared by diluting the stock
                                  irds are then prepared from  the
                             olutions
      3. 5r-5^8.1 \prepare  a  stfock/solution  of  each of the nine PCB
      concenrbatioriisalibration (congeners at a concentration of  1  Mg/ML  in
      hexane.  Place eafcb.solution in a clean glass vial with  a  Teflon-lined
      screw cap.  FiH^to  cne/cop so no headspace  is evident.  Store at  4°C if
July, 1991
                                                          Page D  -  25/SV
-------
Exhibit D
                                                     SOW No. XXX  - Ambient  Air
      solutions are not to be used right away.  Solution
      indefinitely .if solvent evaporation is prevented.
      3.5.5.8.2-  The  9  individual  PCB  congeners  lis
      used as the calibration compounds for PCB dete
      each level of chlorination is used as the co'
      standard for all other isomers at that leve
      decachlorobiphenyl (C110)  which  is used  for
      groups.  The basis for selection of these/ca
      reported and referenced in part 3.7 (Cita'ti
                                                              stable
                                                             ble  D/SV-4  are
                                                                 One isomer at
                                                                    ation
                                                                        PC
                                                                           een
                                                    9) and Table D/SV-4.
      3.5.5.8.3   Take  aliquots  of  the  stock/ solutions Af.  fine  nine  PCB
      concentration calibration congeners and mix together/in the proportions
      that will provide a primary dilution/standard s/luoion of the
      composition illustrated in Table D/Sj/-l/x^lacy/eateh solution in a clean
      glass vial with a Teflon-lined screw caoand^stoye at 4°C.  Mark the
      meniscus on the vial wall to monitor solution voi>vme during storage;
      solutions are stable indefinitely if solvent e^apora^pn is prevented.
      3.5.5.8.4   For  full-range
      are required for CALs contai
      standards, surrogates, and singf
      illustrated in Table D/SV-4.
      increasing level of chlorinatio
      increase with level of chlorinati'
      concentration solution (CAL 5) are
      injections of 1 pL aliquots without
      overloading.

   3.5.5.9     Multicomponen
      3.5.5.9.1   Tox4ph;
      except for Aro/ilo
      mixture.
                                     ecause MS yes
                                         xaphe
      3.5.5.9.2
                   Place  0.1  gr
                   uminura weiahi
  uisition, five calibration  solutions
concentratiojisof the internal
           target"cTji^pounds as
                     CBs decreases with
              concentrations in CALs
          inents of the highest
  present at a concentration that allow
         uration or GC column
            id Aroclors)

          prepared individually,
          be combined in one standard
                                  solution of each of the multicomponent
      standard in_ hexane.   Fbaee eatb, solution in a clean glass vial with a
      Teflon-linetr"Scr^w-~cap.  F-yj to^the top so no headspace is evident.
      Store atr 4 ° Cif^sp lutl^ms are^npt ,to be used right away.  Solutioas are
      stable/inde'rinitetVxif solvent evaporation is prevented.
   3.5.5.1,
                                       of  Other  Semivolatiles
                                   f each native semivolatile target  analyte
                                   disk and weigh on a balance.

      3 . 5 . 5 .10 . 2^vQuantt
-------
Exhibit D
                                                   SOW No.  XXX -  Ambient Air
      with methylene chloride.  The concentration of the  s
      solution of semivolatiles in the  flask  is  10
      3.5.5.10.3-  Transfer the stock standard solution
      screw-cap bottles.   Store at 4°C  and protect  fr
      solutions should be  checked frequently  for  si
      evaporation, especially  just prior  to prepari
      from them.
                                                           k standard
                                                        to Teflon-sealed
                                                         j.t.   Stock standard
                                                                    or
                                                                standards
      3.5 . 5 .10.4   Secondary standards may be
      standard solutions.  Working standards  ai
      secondary standard solutions.

   3.5.5.11   Surrogate Compounds Spiking S

      3.5.5.11.1   Prepare  separate  soluti<
      contain approximately  1000 Mg/ni
      the spiking solution  to obtain  the  follov
      extract when 1 pL is  spiked into  the cartric
      Surrogate Compound

   13C6-Gamma-BHC
   13C12-4,4'-DDT
   13C6 - 4 - monochlorob ipheny 1
   13C12-3,3',4,4'-tetrachlorobiphenyl
   13C12-2,2',3,3',5,5',6,6'-Octachlorobip
   13C12-Decachlorobiphenyl
   "Nitrobenzene-d5
   *2-Fluorobiphenyl
   *p-Terphenyl-d14
   2,4,6-Tribromopheno
   2 -Fluorophenol
   Phenol-d5
*  These surrogate ^Qjnpouffr

3.5.5.12   Working_Standar

   3.5.5.1
                                                  d by diluting
                                                    prepared from the
                                                      ogate compounds to
                                                       solutions,  prepare
                                                     entrations  in the
                                               00
                                              100
                                     required;   the  others  are  optional.
         pe
         ultrasonic nfi^ing
         r e sul t irsgx§  lu tl
         1000
                               .ndard
                               lutions of 1,4-dichlorobenzene-d4 ,
                               ,ne-d10,  phenanthrene - d10 , chrysene-d12, and
                                ed by dissolving 100 mg of each compound  in
                                ide.   It  may be necessary to use 5 to 10
                                e  in this solution and a few minutes of
                               er  to dissolve all the constituents.   The
                               contain each  standard at a concentration of
                             ortion of this  solution should be added to each
July,  1991
                                                              Page D - 27/SV
-------
Exhibit D
                                                     SOW No. XXX - Ambient Air
         1 mL of sample extract.  This will result  in  20
         standard in the 1-jtL volume of extract injected
      3 . 5 . 5 . L2 . 2   Instrument  performance  check soluti
              Prepare a solution of decafluorotriph
         that a 1-^L injection will contain 50 ng
         also be included in the calibration stan
      3.5.5.12.3   Single-component  Calibration/Standards
                                                               each internal
                                                              the GC/MS.
              Prepare calibration standards
         concentration levels as outlined  i.\
         standard should contain each comp<
         internal standards, and surrogatal.compi
         D/SV-1.  Great care must be taken
         standard solutions.  Store all standarclxsolut!
         screw-cap amber bottles with Teflon liners>
         be prepared every twelve months at a minimum.
         calibration standard (see
         weekly and stored at 4°C /±2°C).
      3.5.5.12.4   Multicomponent  Calibration Stands
                                         D/SV-4,  CAL 3) sh
                                                             nimum of five
                                                            Each calibration
                                                       es^C.-the appropriate
                                                         utlined in Table
                                                        he integrity of all
                                                         s at 4°C (±2°C) in
                                                            standards should
                                                               tinuing
                            e prepared
              The calibration standards
         prepared at concentrations of 10Q ng/ml
         which must be prepared at 500 ng/
         must contain the v*fl:ernal\standardsand
                                                   te and Aroclors  must be
                                                  execpt for Aroclor 1221
                                                   multicomponent standards
                                                 surrogates at 20 ng//iL.
   3.5.5.13   Storage of/StaAdard^Soli:
      3.5.5.13.1   Sto/e pne stock/an'
      Teflon-lined screw/cap amber b/ttles
      solutions at
                       (±a
             tandard solutions  at  4'
            re  the working standard
Ion-lined screw-cap amber bottles.
                                                                         C  in
      3.5.5.13.2   Protec
      extracts, and standard
                           11 standards from light.   Samples,  sample
                              pustb< stored separately.
                                          ,s must be replaced every twelve
                                        'ith quality  control  check samples
      3.5.5.13/3  Stock standard so^iutio,
             /   ^"~	^^^     ^\
      months / or/Sooner,^vf comparison
      indic/tes/a problem.

3.5.6 Ins^ruijtent Operating Con^itibns

   3 . 5 . 6 . fX.  Gas^x^romatograptf:  /The following are the recommended gas
   chromatographic atta^ytical/contlitions,  as outlined also in Table D/SV-2, to
   optimize conditions to~t compound separation and sensitivity.
 Jul",  L991
                                                                 Page  D  -  Z8/SV
-------
Exhibit D
                                                   SOW No.  XXX - Ambient Air
         Carrier Gas:
         Linear Velocity:
         Injector Temperature:
         Injector:
         Temperature Program:
         Initial Hold Time :
         Ramp Rate:

         Final Temperature:
         Final Hold Time:

         Analytical time:
                                  Helium
                                  28-29 cm3/sec
                                  250-300°C
                                  Grob-type,  splitle
                                  Initial Temperatu
                                  4.0 ±0.1 min.
                                  10°C/min to 160,
                                  increase to 30,
                                  300°C
                                  10 min (or
                                  interest h,
                                  approx.
   3.5.6.2    Mass  spectrometer:   The folloylng/are the/required mass
   spectrometer conditions for full range jiata/acquis^tio/
                                         i
         Transfer Line Temperature:  250-30
         Source Temperature:

         Electron Energy:
         lonization Mode:
         Mass Range:

         Scan Time:
3.5.7 Instrument Performance Check
                                 According
                                 Specifications
                                 70  volts  (nominal"
             Summary
                                                 full  range"'data

                                                       pe4k,  not to exceed
                                                    C/MS meet tuning and
                                                   ior to initiating any on-
                                                igure D/SV-6.  This is
                                                luorotriphenylphosphine
3.5.7.1
      It is necessary,
   standard ma_  sp
   going data collefctijbn
   accomplished thro
   (DFTPP).

3.5.7.2   Frequency

   3 . 5 . 7 . 2 .1 ^^-^hB—instrumerttvDerfb^mance check solution of DFTPP must be
   analyzed/initially aiM^once p»r  12/hour  time  period  of  operation.   Also,
   whenever th^TaBcTtar^oryN^kes  corrective action  which may  change  or
   affect?  th6 mass spectsal criteria  (e.g.,  ion  source  cleaning  or repair,
   column  replacement, etc\), Vhe instrument performance check must  be
   verified irrespective of\tha 12-hour  laboratory  requirement.

   3 . S^^.2 . 2^xThe  12-hour/tim/fe  period for GC/MS instrument performance
   check atvl standards calibration  (initial calibration and continuing
   calibratio>^xchecl^-crit6ria/) begins  at the injection  of  the DFTPP  which
   the laboratory\$ubmibs  ap  documentation  of a  compliance tune.  The  time
July, L991
                                                              Page D -  29/SV
-------
Exhibit D
                                                     SOW No. XXX  - Ambient Air
      period ends after 12 hours have elapsed.  In order
      performance check requirements, samples, blanks,
      injected within 12 hours of the DFTPP injection.

   3.5.7.3   Procedure

      3.5.7.3.1   Inject 50 ng of DFTPP into  the
      instrument conditions must be  identical to
      except that a different temperature  'progr
                                                             ;eet instrument
                                                            tandards must be
      3.5.7.3.2   DFTPP may be analyzed sepa
      calibration standard.
   3.5.7.4   Technical  Acceptance  Criteri

      3.5.7.4.1   Prior to the analysis  of any^^amplesV^blanks,  or
      calibration standards,  the Laboratory must establisnvxt.hat the GC/MS
      system meets the  mass spectral ion abundance criba^ia fbs; the instrument
      performance check solution containing DFTPP.

      3.5.7.4.2   The GC/MS systemXmusNTTre-^Jisjrrument peTfcwrmance checked  at
      the frequency described in park 3:^. 7 .1 /2~7  The-CC^l^system must be
      tuned to meet the manufacturer's\specifi/atZons,  using a suitable
      calibrant.   The mass  calibration And t^/obdtion of the GC/MS system are
      verified by the analysis of the instrument performance check solution.
      3.5.7.4.3
                  The abu
      for a 50 ng injection o£-QFTP
      acquired by averagang/threeNyc
      immediately precefdin| following the
      required, and mi/st/be accomii
      elution of DFT/P.
-------
Exhibit D
                                                   SOW No.  XXX -  Ambient Air
                                                             >r auto tuning,
                                                             facturer's
                                                            Surce parameters
                                                                 Mass peaks at
                                                            tuning is
                                                                    502 and
                                                                    match  the
   3.5.7.4.5    If the  mass spectrometer has the abili
   then the user  may utilize  this  function  following
   specifications.  Autotune  automatically  adjusts  i
   within the detector using  perfluorotributylamine
   m/z 69, 219, and 502 are used for  tuning.  Afte
   completed, the  PFTBA abundances  at m/z 50, 69
   614 are further adjusted such that their rel
   selected masses of DFTPP.

3.5.7.5   Corrective Action
      3.5.7.5.1    If  the  DFTPP  acceptance  cryterfa are not met,  the MS must
      be retuned.  It may be necessary to cLean/the ion /sobrce, or
      quadrupoles, or take other actions to/acbiieve the; acceptance  criteria.
      3.5.7.5.2    DFTPP  acceptance  criteria^MUSToar me/c before any standards,
      performance evaluation (PE) samples, or rsquireoXblanks  are  analyzed.
      Any samples or required blanks analyzed when^-tuning^criteria have not
      been met will require reanalysis at no additionaix^cost^tp the Agency.

   3.5.7.6   Documentation

         Reporting requirements are

3.5.8 Initial Calibration
   3.5.8.1   Summary

         Prior to the an
      criteria (instrum<
      must be initially c
      determine instr
      the analyte co:

   3.5.8.2   Frequenc
                                                ^.red  blanks  and  after  tuning
                                                 ieen met, each  GC/MS  system
                                                 five concentrations to
                                              inearity of GC/MS  response  for
      3.5.8.2.1    Each GC/MSxsystetevmust be initially calibrated upon award
      of the con>ratTT--«heneverx-the  la"feqratory  takes  corrective  action which
      may change or affect^fetie  initial calibration criteria  (e.g.,  ion source
      cleaning oz^repaTrv^colUHm replacement, etc.),  or  if the continuing
      calib/atyon  acceptance^ criteria  (see  part 3.5.7.3.4) have  not been met.
    3.5/8.
                                 remains in the 12 -hour time period after
   me£tin
   sampS^s
   calibra
   calibratio
   continuing  ca
July, 1991
                                epnance  criteria  for  the  initial calibration,
                                 It  is not  necessary  to analyze a  continuing
                                  the 12 -hour  time period,  if the initial
                                 3)  that is the same  concentration as  the
                                andard meets the  continuing  calibration
                                                              Page D -  31/SV
-------
Exhibit D
                                                      SOW No.  XXX -  Ambient Air
      technical acceptance criteria.  Quantify all sample/results  using  the
    '  the RRFs fr-om. CAL 3 in the initial calibration or /the/RJRFs from  the  most
      recent valid continuing calibration standard within £he same  12-hour
      period.

   3.5.8.3    Procedure

      3.5.8.3.1   Set up  the GC/MS  system per
      and illustrated in Figure D/SV-6.

      3.5.8.3.2   All standard/spiking solutions/ sample .^xtracts,  and blanks
     • must  be allowed to warm to ambient temperature (ap/proXimately 1 hour)
      before preparation or analysis.
      3.5.8.3.3   Tune the GC/MS system   ^
      criteria in part 3.5.7.1.4 for DFTPP.
                ecVtnical acceptance
      3.5.8.3.4   Prepare five calibration  standaroXcon£a
-------
Exhibit D
                                                   SOW No.  XXX - Ambient Air
   ratio in the ranges  found  in  Table  D/SV-7.

3.5.8.4   Calculations

   NOTE:  In the following calculations,  the  area
   primary quantitation ion unless otherwise  stated

   3.5.8.4.1    Relative Response Factors (RRF)
   analyte target compound and surrogate  usin
   the appropriate internal standard.  Table
   ions for internal standards and surrogat
   outlines primary quantitation ions  to  b,
   pesticides.
         where:
                                                             e is that of the
                      Area of  the primary  quan
                      be measured;
                      Area of  the primary  quantitatio
                      standard;
                      Concentration of  the^ttrte-cnaj.standardy and
                      Concentration o5r~the^c_ompoundto^tre—measured.
                                                                   D/SV-
                                                          ach PAH,  PCB,  and
                                                                 Eq.  D/SV-1


                                                    .ion  for  the  compound to

                                                             the  internal
         where:
      3.5.8.4.2    Percent Relative S
      relative response factors  (RRF)
      the %RSD for all target compounds
      equations:
         and
                                                ion (ZRSD):   Using the
                                                    calibration,  calculate
                                             ogates using the following
                                                                   Eq.  D/SV-2
                                                                    Eq.  D/SV-3
                                       ^iation  of  initial response  factors  (per
                                   j^k.  ami
                           Mean of inrfial relative  response  factors  (per
      3y-8'/-3    Relative  Rettentkon Times (RRT) :   Calculate the RRTs for
      e^ch tas^et compound andj surrogate over  the  initial  calibration range
      us ihgthe'^gpl lowing equsttic
July, L991
                                                             Page D  -  33/SV
-------
Exhibit D
                                        SOW No. XXX  - Ambient Air
                                  RRT =
                                                      Eq. D/SV-4
      where: RTC
              RT,
       Retention time of the target compjouncH^and
        Retention time of the internal jstantiarc
      3.5.8.4.4   Mean of  the Relative Retention Tijfra^ (RRT):   Calctt^ate
      mean of the relative retention times (RRT) /for/each analyte  target
      compound and surrogate over the initial cadib/ation range using  the
      following equation:
                                                                    Eq.  D/SV-5
      where:   RRT

               RRT
         Mean relative retentiorNtime frir che target compound or
         surrogate for each initial^i&alibration standard; and
         Relative retention time for thextargVs^compounds or
         surrogate for each initial calibration standard.
         3.5.8.4.5    Mean Area Resj
         the means of the area respt
         each internal standard compot
         using the following equation:
   3.5.8.5
                  Mean ar
                  Area rasp
                  inter
Technical Acceptance
                                         ;nal Standard:  Calculate
                                                quantisation  ion
                                                ibration range
                                                                    Eq.  D/SV-6
      3.5.8.4.6   Me
      Calculate the mean
      standard over th
      equation:
                                        titation  ion for  the
                                       1 calibration standard.

                                     )  For  Internal  Standard:
                        tion times (RT)  for each internal
                               range using the following
                                                                    Eq.  D/SV-7
Mean retention time;  and
Retention^time for the internal standard  for  each
initial calibration standard.

             'riteria
       3.5.8.5.1   ^AJJ. inlr^ial' calibration standards must be analyzed at the
       concentration  le^v^ls  descried  in part 3.5.7.2.1 and at the frequency
       described  in part  TXT  ~ /     n  a  GC/MS system meeting the DFTPP
 July,  1991
                                                    Page D -  34/SV
-------
Exhibit D
                                                SOW No.  XXX - Ambient Air
      instrument performance  check  criteria.

      3.5.8.5.2    The performance criteria for initial ^alj^ration of the CAL
      3 mus t show:
              Baseline separation of beta-BHC and g

              Baseline separation of endrin ketone/an'
        Signal/noise ratio of >5 for m/z
        illustrate MS sensitivity;

        Abundance of >40 percent and >(
        m/z 498 for PCS congener C110 /
        Lack of degradation of endr^ri
        profile (EICP) for m/z 67 in
        4,4'-DDE and endosulfan sulfate;
        m/z 67 at the retention time of
        of the abundance of m/z 67 produced by
                                                                       cPCB/to
                                                            z 502 relative  to
                                                         extracted ion current
                                                         time window between
                                                        hat the abundance of
                                                           de is >10 percent
                                                               d
              Lack of degradation 4f 13C12-^T7trl--aDIiexamine"xf;iCPs for m/z 258
              and m/z 247 in the rVterftr»a^time window^tfrrat., includes 4,4'-ODD,
              4,4'-DDE and 4, 4' -DDT\m/k 258~wo]Zld/b«_grodufced by 13C12-4,4'-
              DDE,  and m/z 247 by 13cX4,V -DDI/. /Confirm~~that the total
              abundance of both ions is\>5 \}e/ce^it of m/z 247 produced by
              »C12-4,4' -DDT.
      3.5.8.5.3    The  rel
      concentration for each
      minimum response fac
      compound's minimum  acceptable
                             ponse fac\pr \RRF) at each calibration
                         rget\compound\nd  surrogate  that  has  a required
                            .e \ny.sJL be greateir  than  or equal  to the
                                        response  factor see Table D/SV-6.
                        jrcent
                    ratiorj^range/ fop  each
                        cimt
3.5.8.5.4
initial cali
has a required"
When an RSD. exceed^25 per-
appropriate CALs to o
concentra£ionTanae, or  t"
                                    Lve
                               in
               deviation  (%RSD)  over  the
        target compound and surrogate that
 must be less than or equal to 25 percent.
ent, analyze additional aliquots of
              %RSD of RRFs over the entire
         to improve GC/MS performance.
                                   ac
                                       pn
      3 . 5 . 8 .6. 5
      target compounds and
                          retention time for each of the semivolatile
                      urris^gates  at  each calibration level  must be within
      relative retention  t\me units of  the  mean relative  retention time
    each compound.
      3 . 5>&
-------
Exhibit D
                                                      SOW No. XXX  -  Ambient Air
      3.5.8.5.7   The retention  time  (RT)  shift for each d£ trhe internal
      standards at each calibration level must be within/±20/0  seconds
      compared to the mean retention time (RT) over the/inirial calibration
      range for each internal standard.
                                                               the minimum RRF
      3.5.8.5.8   The compounds listed in Exhibit  C/mus  me
      and maximum XRSD criteria for the initial cajAbration,
      made for up to four target and surrogate compounds.  However\^he
      for those four compounds must be greater tJlan/0.010, and the %R£tlXof
      those four compounds must be less than or/equ4l to 40.0 percent for^he
      initial calibration to be acceptable.

   3.5.8.6    Corrective  Action
      3.5.8.6.1   If the technical acceptAoce c
      calibration are  not met,  inspect the s^sr^em
      necessary to clean the ion source,  change
      corrective actions to achieve the acceptance
                                                   er£a fcbr initial
                                                      problems.   It may be
                                                    coream, or take other
      3.5.8.6.2   Initial calibration—eecijnical  acceptance^^riLiferia MUST be
      met before any samples or required blanEs~-ai=«^snalyzed.  Any  samples  or
      required blanks analyzed whenXin^ra-t^a^^ratio^TcrTteria have not been
      met will require reanalysis at\p additional cost^ojthe Agency.

   3.5.8.7   Documentation

         Reporting requirements_are listed \n Exhibit B.

3.5.9 Continuing Calibrate
                          on
   3.5.9.1
             Summary
         Prior to th
      criteria,  ini
      GC/MS system
      calibration standar
      meet the instrument sen
      method,  as/£TTus~E?ated in
      standar d
                      analysis  of/saniples
                               fivi
                                all
                                    re
      intern
   3 . 5 . 9 .
                  Each GC/MS ued
                    eriod of
                       DFTPP .
             quired blanks and after tuning
  and LMB criteria have been met, each
  checked by analyzing a continuing
to ensure that the instrument continues to
   and linearity requirements of the
     (SV-8.   The continuing calibration
      4rget compounds, surrogates, and
                                   or  analysis  must  be  calibrated once every
                                         The 12-hour time period begins with
      3.5.9.2.2   If^6
-------
 Exhibit D
                                                   SOW No. XXX - Ambient Air
       samples  may be analyzed.   It is not necessary to anaiyze a continuing
    -   calibration standard within this 12-hour time perio/d, £f the initial
       calibration standard .that is the same concentration a.fl the continuing
       calibration standard meets the continuing calibra-tio.n technical
       acceptance  criteria.

   3.5.9.3   Procedure

       3.5.9.3.1    Set up the GC/MS system per the
       and as specified  by the manufacturer.

       3.5.9.3.2    Tune the GC/MS system to me/t
       criteria in part  3.5.7.4  for DFTPP.
                                               ne technical acceptance
      3.5.9.3.3    Analyze the CAL 3 standard /olution/coritaining all the
      target analytes,  surrogate  compound/,  arrd^inteifnal/standards  using the
      procedure  listed  in part  3.5.8.3  of  fck§  initial  Calibration.

      3.5.9.3.4    All standard/spiking solutions""^! blinks must be allowed
      to warm to ambient  temperature  (approximately  INkiourJ^feefore  preparation
      or analysis.
   3.5.9.3.5    Start the analy
   injecting 1.0 nL  of the CAL

3.5.9.4   Calculations

   3.5.9.4.1    Relative  Response Factoi
   response factor (RRF)x-foT~se4ch
   equation in part  3.3^8.4.
         where
                                                           ibration by
                                                    Calculate a relative
                                                 >und and  surrogate  using  the
      3.5.9.4.2    Percent
      between the raea
      calibration an
      each analyte e?arge-t corapo
                                          Calculate the percent difference
                                              rom  the  most  recent  initial
                                              relative response  factor  for
                                              using the following  equation:
                                           x 100
                                                                   Eq.  D/SV-8
   3.5.9.5
                                  ffe^ence between relative response
                        facxors;
                         verage relative response factor from  the most
                        recentv  initial calibration; and
                        Re Dative response factor from continuing
                        calibration standard.
            chnibal Acceptance7 Criteria
      3.5.9.5.1
      the compounds
                    conbinuyhg  calibration standard must be analyzed for
                           Exhibit C concentration  levels  at the  frequency
July, 199L
                                                             Page D  -  37/SV
-------
Exhibit D
                                                   SOW No.  XXX -  Ambient Air
      described in part 3.5.9.2 on a GC/MS system meeting
      performance, check and the initial calibration tech,
      criteria.

      3.5.9.5.2   The  relative  response  factor for  e
      surrogate that has a required minimum respons
      greater than or equal to the compound's mini
      response factor.
                                                            DFTPP instrument
                                                            acceptance
                                                                    betweet
   3.5.9.5.3    For  an acceptable  continuing/cald.brat ion,  the XD
   the measured RRF for each analyte/surrogate/compound of  the  CAL  3
   standard and the mean value calculated/\sefi part  3/57]?)  during initial
   calibration must be within ±25 percenjr.  fl.1 not, /tem/dial  action must be
   taken; recalibration may be necessary

3.5.9.6   Corrective Action

   3.5.9.6.1    If the continuing  calibration technicals-acceptance  criteria
   are not met, recalibrate the GC/MS  instrument  accJtu^ing'-fcp part  3.5.8.
   It may be necessary to clean &he—icnsource, change che Column or  take
   other corrective actions to Achieve  the~~ace«fttance criteria.
   3.5.9.6.2    Continuing calibrations,technical
   be met before any samples or req\ir
   or required blanks analyzed when cent
   not been met will require reanalysiV at ng
   Agency.
      3.5.9.6.3   Remedi
      Possible remedies
                                      be
                                                            fee criteria MUST
                                                   are analyzed.  Any  samples
                                                  calibration criteria have
                                                 additional cost to the
criteria are not met.
              Flush column
              instructions
                              t porfl
                                               ing conditions;
                                           J
                                 tor liner;

                                     according to manufacturers


                                       pproximately 0.33 m) of the column:
              Prepare
                                  erformance of all initial calibration
                                   equired) ;

                                    or lesser resolution;
                               new continuing calibration; and
 July,  L991
                                                              Page D -  38/SV
-------
Exhibit D
                             SOW No. XXX  -  Ambient Air
              Prepare a new concentration calibration curved

      3.5.9.7   Documentation

         Reporting requirements are listed in Exhibit

3.5.10   Laboratory Method Blank (LMB)

   3.5.10.1   Summary

      3.5.10.1.1  The  purpose  of the  LMB is  to/monitor for possible
      laboratory contamination.  Perform all srep/s in  the  analytical  procedure
      using all reagents, standards, surrogate compounds/isfluipment,
      apparatus, glassware, and solvents th^t would be/use/a  for a  sample
      analysis.

      3.5.10.1.2  An LMB  is an unused,  cerbified'^&a/lte.r'/cartridge  assembly
      which is carried through the same extraction procedure as a  field
      sample.  The LMB extract must contain the saae amount  of surrogate
      compounds and internal standards that is added coeacnxs^ample.   All
      field samples must be extractad^and analyzed with SH^associated LMB.

   3.5.10.2   Frequency

      3.5.10.2.1  Analyze  an LMB aloitewlth  ea£h l$atcl-f~oY/<20  samples through
      the entire extraction, concentrat-ionV a^rid Analysis.

      3.5.10.2.2  The  laboratory may  also\anal
-------
Exhibit D
                                                  SOW No. XXX  - Ambient Air
      3.5.10.4.3   The  area response  change for  each of the internal  standards
      for the blank must be within -50 percent and +100 .percent compared to
      the internal standards in the most recent continuing/calibration
      analysis.  -
      3.5.10.4.4   The  retention time  shift for  eac
      must be within ±30.0 seconds between the bla;
      continuing calibration analysis.

      3.5.10.4.5   The  LMB  must  not  contain any,
      concentration greater than one half of
      additional compounds with elution char^
      features that would  interfere with
      method analyte at its CRQL.  If the
      batch of samples is  contaminated, tfc
      reextracted and reanalyzed.
                                      ids
   3.5.11.
                                                           terna-L standards
                                                               recent
jet  analyte  at  a
       ^must not contain
         'mass spectral
         measurement of a
       'racted along with a
      'of samples must be
3.5.10.5   Corrective Action

   3.5.10.5.1   If a Contractor's/
   acceptance criteria, the Cont
   to be out of control.  It is
   that method interferences causV
   glassware, and other sample stoi
   discrete artifacts and/or elevatei
   eliminated.  If  contamination is a
   contamination must be investigated
   MUST be taken and doc*tfnentettxbefore

   3.5.10.5.2   All s
   control (i.e., c
   no additional c
                                                               .nical
                                                               lytical system
                                                             ility to ensure
                                                            Ivents,  reagents,
                                                         Hardware that lead  to
                                              ine's in gas chromatograms be
                                                  the source of the
                                                ropriate corrective measures
                                                  sample analysis proceeds.

                                                   !od blank that  is out  of
                                             re rVextraction and reanalysis  at
   3 . 5 .10 . 6   Documi

         Reporting requi

 3 . 5.11   Sample

   3.5.11.1  /S
                               e  listed  in Exhibit B.
                                m  3.4  is  analyzed by  GC/MS and quantitated by
       3 .5 .11.2 . l\§efo?fe\samplas or required blanks can be analyzed, the
       instrument mustxjneetrhe/GC/MS  tuning,  initial  calibration,  and
       continuing calibration/technical  acceptance  criteria.
 July,  1991
                                                              Page D -  y-
-------
Exhibit D
                                                SOW No. XXX - Ambient Air
      3.5.11.2.2   If there is time remaining in the 12-hoy
      a valid initial calibration  or  continuing calibrat
      analyzed in  the GC/MS system that  meets  the
      criteria. •
                                             instr
                                   t,ime period with
                                    samples may be
                                    performance check
   3.5.11.3   Procedure

      3.5.11.3.1   Set up the GC/MS system per the/re
                                                                  3.5.6.
      3.5.11.3.2   All samples extracts,  required Blanks and standard/spiking
      solutions must be allowed to warm  to  amoieWt  temperature (approximately
      1 hour) before preparation/analysis.  Xll/sample  (^bracts  and required
      blanks must be analyzed under  the  sanjfe  i/istrumervcal/conditions as the
      calibration standards.

      3.5.11.3.4   Add the  internal  standarokspikiTn^ solution to the 1.0 mL
      extract to contain 20 ng//iL.   For  sample-xjlluti&ns,  add an appropriate
      amount of the internal standard spiking  soitttion  tb^maintain the
      concentrations of the internal standards at 20xtvg//iLin^the diluted
      extract.
      3.5.11.3.5   Inject  1.0
      data acquisition.
                                                     .GC/MS, and start
3.5.11.3.6  When  all  semivolatilfe  ta^ge't Compounds have eluted from the
GC, terminate the MS data acquisition and: store data  files  on the data
system storage device.  Use appropriate 
-------
Exhibic D
                 SOW No.  XXX - Ambient Air
      3.5.11.4.3   The dilution factor chosen should keep/the/response  of the
      largest peak for a target compound  in  the  upper  ha4f pf the initial
      calibration range of -the instrument.

      3.5.11.4.4   If the  on-column concentration of ,any>miantrcation is performed, document
      the reasons  in/the' SDG Narrative.   Tnfe^r/ea of a secondary ion cannot be
      substituted  fqr  thexarea 6f afprimary ion unless a relative response
      factor  is calcula^ted  using fa& secondary ion.

      3.5.11.. 5.3  . A retentio^vtime^vj-ndow  is  calculated for  each single
      component .attaTyCe^and surriagate and for the major peaks (3 to 5)  of each
      multicomponent analyte^ Winotbws are centered abound the average
      absolute  re'tention^ti.me  zpr the analyte establ    ed during the initial
      califa/ratjxin.

      3.5/. 11/5.4   For AroclorsV  a\ set of  three  to five  major peaks is
      sedectetkfor each multicompqnent analyte determination.  Retention time
               foi\each peak ace distermined from the calibration  standards.
                         a mul/ticpmponent analyte  in the  sample is based on
      pattern recwgnitiri LT/ conjunction with the  elution of  three to  f: -e
       sample  peaks ofxChe standard.   The number of poten-.ial  quantita
       peaks are listed tfe4ow /tor selected  aroclors :
 July, 1991
                             Page  D -  42/SV
-------
Exhibit D
                                                SOW No.  XXX - Ambient Air
         Multi-component Analyte

              Aroclor 1016
              Aroclor 1221
              Aroclor 1232
              Aroclor 1242
              Aroclor 1248
              Aroclor 1254
              Aroclor 1260
              Toxaphene
                                Number  of Potential
                                Quantitation Peaks
                                       5
                                       3
                                       4
                                       5
                                       5
                                       5
                                       5
                                       4
      3.5.11.5.5   The  choice  of  the  peaks  used for mult/component analyte
      identification and the recognition of/thp4e  peaks'may be  complicated by
      the environmental alteration of the ytoxaphene oj  Ar/oclors,  and by the
      presence of coeluting analytes, or ^natrifcx.inte/feffences,  or both.
      Because of the alteration of these materialsxvin tfhe environment and
      aging of the Aroclor, multicomponent analyses irKsamples  may  give
      patterns similar to, but not identical withT^^hose^Qif the standards.
      Identification requires visual inspection of an^otj-scale  pattern.
   3.5.11.6   Calculations
3.5.11.6.1  Calculate  target
following equation:
July, 1991
                           or thecompou
                                       targ
                  Area  esp/se
                  quanjeitation
                  st
                  Volume
                  Volume
                  Dilution
                                                      tions/using the
                                                                   Eq. D/SV-9
                tj6 be measured.  The primary
                  compounds, internal
                      in Table D/SV-8 and

                standard.  The target
 sted with their associated internal
 e D/SV-3;
    standard injected in nanograms (ng);
e mo"9-c recent continuing calibration as
                                       ,  STP;
                          act  injected in  microliters
                            extract  in microliters  (^L);  and
                            for  the  extract.   If  there was  no dilution,
                             the sample was diluted, the  Df is greater
      NOTE:  Toral PCB">spnce6trXtion in each sample extract is obtained by
      summing isomeixgroup^-conxfentrations .
                                                          Page D  - 43/SV
-------
Exhibit D
                                                   SOW No. XXX - Ambient Air
      3.5.11.6.2  The  equation in part 3.5.11.6.1 is also/us/d for
      calculating the concentrations of the non-target  compounds.   Total area
      counts (or peak heights) from the total  ion chrom&tograms  are to be used
      for both the non-target compound to be measured /(A^Sand the  internal
      standard (A;s) .   Associate  the nearest  internal/staiKlard"x£ree of
      interferences with the non-target compound to/be/measured.^"^A relative
      response factor  (RRF) of one (1) is to be as/umsti.  The""value fT?om this
      quantitation shall be qualified as estimate/d^S^I")  (estimate
      lack of a compound-specific response factor)^nd  "N"  (presumpti^
      evidence of presence),  indicating the quantitative  and qualitative^
      unce.  ainties associated with this non-Garget component.  An  estimated
      concentration should be calculated for/4.11/tentatively identified
      compounds as well as those identified/as/unknowns/  Jfhis estimated
      concentration must be calculated for/all/ tentative\fl  identified
      compounds as well as those identified
      3.5.11.6.3  Surrogate  Percent Recovery
      percent recovery using the following equatiot
                              %£/=
x 100
                                                  Calculate the surrogate
                                                                   Eq.  D/SV-10
      where:
           Qd - Quantity  determinedN
           Qa = Quantity  added to sample/

   Determine if the surrogate percent
   follows:
      Surrogate
13 C6-gamma-BHC
13C12-4,4'-DDT
13C6-4- monochloro
13C12-3,3' ,4,4'-t
13C12-2,2',3,3',5,
13C12-dechlorobiphenyl
Nitrobenzene-dj
2-Fluorobiphe
p-Terpnenyl
2,4,6-Trib, '
2-Fluoro
Pheno1 -
                                                  meets the specifications  as
                                                    coverv Limits
                                                       35-150%
                                                       35-150%
                                                       35-150Z
                                                       35-150%
                                                       35-150%
                                                       35-150%
                                                       35-150X
                                                       35-150%
                                                       35-150%
                                                       35-150%
                                                       35-150%
                                                       35-150%
                                   ponse Change (%ARC) :   Calculate the percent
                                   for the sample/blank  analysis  compared to
                              ng /calibration  check  standard (CAL 3)  analysis
                                tandard compounds using the following
July, 1991
                                                              Page D - 44/SV
-------
Exhibit D
                                                SOW No.  XXX -  Ambient Air
                                    -£ x 100
                                                                  Eq.  D/SV-11
         where:
           %ARC
           A, =
                                                       ft/(RTS):   Calculate
                                                         lank analysis and the
                                                        analysis for each of
                                                       on:

                                                                  Eq. D/SV-12
      3.5.11.7.2  Int
      samples must b/
      If the retent
      0.50 minutes
      if samples are an2
      calibration, the chrSt
      malfunction
      internal
      sample/
                                                  hould not exceed ±40
             Percent  area response  change;
             Area  response of  the internal
             analysis;  and
             Area  response of  the internal
             continuing calibration stand
This area change for the internal stan<
percent.

3.5.11.6.5   Internal Standard Reten
the retention time shift (RTS)  bet
most recent continuing calibration c
the internal standards using the followi'
      where:
         RTS   =
         RTC   -
            Retention  time
            Retention  time o
   3.5.11.7   Technical Acceptance  Cri

      3.5.11.7.1  All target compound con
      upper  limit of the
      (excluding the compound peak,
      detector.
calibration.
                                         itions must  not  exceed the
                                             and no compound ion
                                       t,vem; front) may saturate the
July, 1991
                                          ;Ci  retention  times  in all
                                          ately after data acquisition.
                                         andard changes by more than
                             continuing calibration standard or CAL 3,
                           the same 12-hour sequence as the initial
                              ic system must be inspected for
                                   as required.  The SICP of the
                      t be f&onitored and evaluated for each field and QC
                      axe described in detail in the instructions for
                          tandard Area Summary.  If the SICP area for
                           es by more than a factor of ± 40 percent of
                            m must be inspected for malfunction and
                            ate.  If the analysis of a subsequent sample
                            he system is functioning properly, then
                           ired.
      3.5.11.7.3  wken target/compounds are below CRQLs but  the  spectrum
                                                          Page D  - 45/SV
-------
Exhibit D
                                                SOW No.  XXX -  Ambient Air
      meets the identification criteria, report  the  concentration with a "J."
      For example,- if CRQL is 3 ng and concentration of / nj/is  calculated,
      report as "3J ."

   3.5.11.8   Corrective Action
3.5.11.8.1   If  the  sample  technical  accepta:
surrogates and internal standards are not
surrogate and internal standard solutions,/ani
It may be necessary to recalibrate the i
corrective action procedures to meet th<
technical acceptance criteria.

3.5.11.8.2   If  the  Contractor  needs
dilution to have all the target com:
range and to have all compound ions no
(excluding the peaks in the solvent
contact the Region for instructions.
                                                    tent or  take other
                                                             internal  standard
                                                           than one (1)  sample
                                                         e  initial calibration
                                                         the detector
                                                          SMO.  SMO will
      3.5.11.8.3  Sample analysis  t^chaicaiacceptance crft«rjLd MUST be met
      before data are reported.  Samples contaffilnate4__from  laboratory  sources,
      or associated with a contaminated\lBe~ehotLj>lank craSy-gamples  analyzed
      not meeting the technical acceptance crita?ia/T«rLL_re/quire reanalysis
      and/or reextraction at no additional\cost/to/the Agency.

      3.5.11.8.4  Sample reruns performed\as  a re suit  of suspected matrix
      interferences beyond thescope of the\metrvod will be  reviewed  on a  case-
      by-case basis for payment put^oses by tt^e Project Officer.
      3.5.11.8.5  The  s
      must be reanalyze/
      demonstrate tha
      This must be a
      meets the SIC
      samples analyze

      3.5.11.8.6
      standards
      problem
      control/ of
      ana ly stis
      initfal
                                      with^SIOP areas outside the limits
                                        made^,  then the laboratory must
                                            em  is functioning properly.
                                             a  standard or sample that
                              r corrections are made, the reanalysis  of
                             stem was malfunctioning is required.

                                  the SICP areas for  all  internal
                                   imits  (± 40  percent), then the
                                is/considered  to have been within the
                                       submit  only data from the
                            he contract limits.  This is considered the
                             reported as  such  on all data deliverables.
                                     of the sample does not solve the problem,
                                     de  the contract  limits  for  both analyses,
      then submit thexSICP  c         sample data  from both  analyses.
      Distinguisn~betweeh\r /   /  -ai.  analysis and the re-analysis  on all data
      deliverables, us-ing  c^c  /ample suffixes specified in Exhibit  B.
      Document  in the  SDG^tJarifative  all inspection and corrective actions
July,  1991
                                                           Page D -  46/SV
-------
 Exhibit D
                                                      SOW No.  XXX - Ambient Air
       taken.

   3.5.11.9   Documentation

       Reporting  requirements  are  listed  in  Exhibit  B.

3.5.12   Performance Evaluation  (PE)  Samples

   3.5.12.1   Summary

       3.5.12.1.1   The  performance evaluation s4mp/es will assist the Agfericy
       in monitoring laboratory performance.  ^The/laboratory will  not be
       informed as  to which compounds  are contained  in  t)tfe^E  samples or  the
      concentrations.

      3.5.12.1.2   The  PE sample  containing  kn~own concentrations of analytes
       is analyzed  by the  laboratory to demonstrafettv/that  it can  obtain
      acceptable identifications  and  measureme~n^s witknrocedures  used to
      analyze environmental samples containing tnVvsamex'&r similar analytes.
      Analyte and  their concentrations are unknown b^xthe ahalyst.
      3.5.12.3.2
      described in
      Che PE sample
   3 . 5 .12.2   Frequency

         The Laboratory must extrac
      PE sample once per sample deli

   3.5.12.3   Procedure

      3.5.12.3.1  The
      PUF/XAD-2 samples from the
      instructions cone
      samples.
                         :he  results of the
                         le.
                samples on filter and
                   5 will  come  with
                  ure  required  for the  PE
             ?E sample using the procedure
              internal  standards  solution to
ilyze  the  PE  sample  as  described  in 3.5.
                                          for calculations.

                                ce Criteria
                                 lust be analyzed on a GC/MS  system meeting
                                  libration, and continuing calibration
                                 ia at the required frequency.
                                must be extracted and concentrated  according
July, 1951
                                                                Page D - 47/SV
-------
Exhibit D
                                        SOW No.  XXX -  Ambient Air
      3.5.12.5.3  The PE  sample must be  prepared  and ana
      blank that met the blank technical acceptance cri

      3.5.12.5.4  The percent recovery for  each of
      within the acceptance windows listed in part 3

      3.5.12.5.5  The area response change  betwee
      recent continuing calibration check standa
      internal standards must be less than or eo/ual
      percent.

      3.5.12.5.6  The retention time shift
      recent continuing calibration check
      internal standards must be within ±3,
                                                 with a method
                                                     must be
      3.5.12.5.7  In addition to complying
      acceptance criteria,  the laboratory will
      identifying and quantifying the compounds inc
      The Agency will notify the laboratory of unaccep
   3.5.12.6    Corrective  Action
                                                            most
                                                 le and the most
                                               for  each of the
                                       PE/sample technical
                                           ;ible  for correctly
                                               the  PE sample.
                                                   ormance.
      3.5.12.6.1  If the PE sample tVchftical acydepraRce__cr/teria  for the
      internal standard and surrogates\arev not/met: ,  check calculations,
      standard solutions and instrument \perEormaiice.  It may be necessary to
      recalibrate the instrument or take \ther (Corrective action procedures to
      meet the technical acceptance criteria
      3.5.12.6.2  Specif i
      criteria associat

              Meet mi

              Repli
                         .borators
                             le:
                       meet the following
                                   rd in Exhibit C;
                    accur
Audit
identified ana
           ysampule dataware re^
           iabVe performancexfo:
           s Contractor failsNti
           r/a or achieves a sai
            tn*t is not limited)
    within ±30 percent RSD; and

    .ss than or equal to 30 percent for
        E sample.

le technical acceptance criteria MUST be met
  orted.  Also,  the  Contractor  must  demonstrate
    compound identification and  quantification.
    leet  the PE  sample  technical acceptance
      of  less than  75 percent, the  Agency may
    'the  following  actions: reduction of the
    n of sample shipment,  a  site visit, a full
      data auoiJ^, ano/pr require/the laboratory to analyze a remedial  PE
      sample, and^or a cTNnt^act/sanction,  such as a Cure Notice.
July,  199L
                                                   Page D -
-------
Exhibit D
                                                   SOW No. XXX - Ambient Air
   3.5.12.7   Documentation
         Reporting requirements are listed  in Exhibit  B.
3.5.13   Identification of Target Compounds
                                                    Jounfcl "fcist (fC*^, Exhibit
                                                     tile interp^tatban of
                                                    ic/trum to the mass spectrum
3.5.13.1   The compounds listed in the Target Co
C, shall be identified by an analyst competent
mass spectra by comparison of the sample mass
of a standard of the suspected compound.
verify the identifications:

   •  Elution of the sample compound at  t
      as the standard compound, and

   •  Correspondence of  the sample comjKmn
      spectra.

3.5.13.2   PCBs are identified and measured withxsj>ecia4 software, using
information found in Table D/SV-7 and the  criteria>resent&d in Table D/SV-
4.  The intensity ratio of the two_jmajor ions in  the mb^eculAr cluster (see
Table D/SV-10) for each homolog/is the~^raje*L_identificatio>ri criteria used.
A ±20 percent range in this ratio aTOundthe theoreTrteaJL or expected value
is considered acceptable.  The labeled surrogTates^are examined for correct
retention time and the absence of rntecference /s showtrby  the ratio of
selected ion abundances from the molecular /on/cluster.
                                             Two/croteria must be sat
                                                             ive  retention time
          jspect
          used to
repo/ted7 PCB coi
   3.5.13.3   The  identification
   calibration utilizing th<
   homolog group with respect to
   (phenanthrene-d10 may
   a response factor wi
   This  response facto
   group.   Thus,
   different inst
   method of quantit
   sensitivities that ma
   the 42 tetrachloro PCB i
   during initial
   calibration

   NOTE: . Fo,
   algorit
                              and quantrficacion extends from the
                                .ve response factors  (RRFs)  for  each  PCB
                                  chryseneNi12 internal standard
                                ed).   The primary ion is used to calculate
                                          ary \pn of  the internal  standard.
                                               ;ember  of a specific homolog
                                               ions are  corrected for the
                                             C1T (homolog)  group.  This
                                 however, take into account  the range of
                                thin a single homolog  series, e.g., among
                                 Therefore, use  the mean RRF calculated
                              the KRF. calculated in  the continuing
         sensitAvicies of eacr
             iers.
   3.5.1'
   (for
   (for
   be examined aftd. comps
   calibration.  Report
                              Automated data  interpretation,  a linear fit
                               s concentration  data.

                                ned on the special PCB qualitative  report
                                 ified as  PCBs)  and the quantitation report
                               B isomer groups.   Individual  spectra should
                              propriate spectra acquired  during
                                values to three significant  figures.
July, 1991
                                                              Page D - 49/SV
-------
Exhibit D
                         SOW No.  XXX - Ambient Air
   3.5.13.5   For establishing correspondence of the GC relative retention
   time,  the same.compound RRT must be within ±0.06 RRT uftiitfe of the RRT of
   the standard compound.  For reference, the standard niust/be run on the same
   shift  as the sample.   If coelution of interfering compounds prohibits
   accurate assignment of the sample compound RRT from the extracted ion
   current profile for the primary ion, the RRT rausy be/assigned cy^using the
   total  ion chromatogram.
   3.5.13.6   For comparison of standard and sam
   mass spectra obtained on the Contractor's
   standard spectra may be used for identific
   Contractor's GC/MS meets the DFTPP daily
   criteria.   These standard spectra may be
   obtain reference relative retention time's

   3.5.13:7   The guidelines for qualitative
   mass spectra are as follows:
                     Le/tompound mass spectra,
                      /are required.  These
                                only if  the
                                acceptance
                                  analysis used to
      3.5.13.7.1   All  ions  present in the  standard mas
      intensity greater than 10 perjaeut^must be present
      spectrum.
                           n by comparison of
      3.5.13.7.2   The  relative inte
      Table D/SV-10 must agree within
      sample spectra.  (Example:  for a:
      in the standard spectra, the  corre
      between 30 and 70 percent.)
                           ~^_

      3 .5.13 . 7 . 3   Ions  gpeatej^thari
      present in the standard  spetet
      the analyst making tfte comparison.
      FAVOR FALSE POSITIVE.  All o/omp,
      must be reported yith thei/ spectra.
                                    at a relative
                                   sample
                   ve
                                 specified in
                              'the standard and
                      an abundance of 50 percent
                     sample ion abundance must be
 £he sample spectrum but not
  idered and accounted for by
 ification process should
g the identification criteria
       3.5.13.7.4   If"^axcompvbvpid cannot be verified by all of the criteria in
       part  3.5.8.2, but  rtvthe  technical  judgement  of  the mass  spectral
       interpretation  specialist:,  the^identif ication is correct,  then  the
       Contractorx-sttaTt~Tf«^prt tha^ iden10 percent of
or/in this method shall be tentatively identified
   NIST Mass Spectral Library.   (Compounds with a
 July,  1991
                                    Page D  -  50/SV
-------
Exhibit D
                                                      SOW No.  XXX - Ambient Air
   peak area response less than 10 percent of  the  area  res
   nearest internal, standard and compounds which elute  be
   compound elutes are not required to be searched in th/s
   after visual comparison of sample spectra with  the
   will the mass spectral interpretation specialist  a
   identification.  Computer generated library searc
   normalization routines if those routines would  mj
   unknown spectra when compared to each other.
                                                                 for the
                                                               the  first target
                                                            fashion.)   Only
                                                               library  searches
                                                              tentative
   3.5.14.3   Guidelines for Making Tentative Id/n
3.6
                                                                    library or
      3.5.14.3.1  Relative  intensities of majrir
      spectrum (ions greater than 25 percent/of
      be present in the sample spectrum.
                                                 /ons in the reference
                                                 ;he  most/^bjundant ion)  should
      3.5.14.3.2  The  relative  intensitis o
      within ±20 percent.  (Example:  For
      percent in the standard spectra,  the  cor
      should be between 30 and 70 percent.)
      3.5.14.3.3  Molecular  ions
      present in sample spectrum.
                                                >e ma/jor/ions should agree
                                                    th an abundance  of 50
                                                jspondiiig sample  ion abundance
             sent  in reference sp
                                                                should be
      3.5.14.3.4  Ions present  in £l^e  s>ample~~s~
      reference spectrum should be re\iewed fo
      contamination or presence of co-eX}.uting>
                                                 ctrumbut dot in the
                                                ptfss ible~~tiackground
                                              compounds.
      3.5.14.3.5  Ions present  in  the  ref^renc4 spectrum but not in the
      sample spectrum should--l5e~-i?eviewed forypossible  subtraction  from the
      sample spectrum because of background contamination  or  coeluting
      compounds.  Data syste^fTTib^ary ^reductionypr^grams can  sometimes create
      these discrepancies.,

      3.5.14.3.6  If/ ii/the  tecKnio-al juctg^ment of the mass interpretation
      spectral spec^alis-t. no vaQid/tentativeldentif ication  can be made,  the
      compound shouRKbe r^p^rVed/as unknown.   The  mass spectral specialist
      should give additiianal classification of  the  unknown compound,  if
      possible (e.g., unknown phtfea^ate, unknown hydrocarbon, unknown acid
      type, unkno>nt--«fe4j2ri.natedvxcompobnd) .   If  a probable  molecular weight can
      be distinguished,  intrude it>

      GC/FIE/OR/GC/ECD OPT^CQNAL^CREENING METHODOLOGY  FOR  PAHs,  PESTICIDES,
      AND fCBs/AROCLORS
3.6.1 Susfmary^of Method

      As an
   approximate fhe app
   dilution prior tb~\Quan€
air s^mpj/e is screened prior to GC/MS  analysis  to
 ria£e c4nge of concentration of analyte compound  for
                           Screening is accomplished
                            at^n with the GC/MS.
July,
                                                                 Page  D -  51/SV
-------
Exhibit D
                                                  SOW No. XXX  - Ambient Air
   utilizing a gas chromatography coupled to specific detectors.  For PAHs,
   flame ionization.detector (FID) is employed, while for pesticides and
   Aroclors an electron capture detector (ECD) is used,/as/Illustrated in
   Figure D/SV-5.   To achieve maximum sensitivity, the/extra«t from part 3.4
   must be concentrated to 1 mL.   Extracts may be concen^M^tedrasJLng a two-
   ball micro-snyder column attached to a K-D appar<
3.6.2 Apparatus

   3.6.2.1    Gas chromatograph:   The gas chro:
   adequately regulate temperature in order
   program and have a flow controller that m,
   rate throughout temperature program oper
   suitable for splitless injection and ha
   including syringes, nalytical columns,

   3.6.2.2    GC column:   30 m x 0.25 mm ID fuse
   thickness (DB-5, J&W Scientific, Folsom, CA, or
   3.6.2.3    Electron capture detec
   (argon/methane) or nitrogen acci;
   GC/ECD system must be in a room
   demonstrated to be free of all cof
   analysis.  The instrument must be ve
   trapping system which prevents the
   instrument room.
                                                 aph (GC)  system must
                                                   reproducible temperature
                                                         ant column flow
                                                     system must be
                                                       accessories
                                                      column,  1.0 /*m filter-
                                                         £>•
                                       The makeup gas mu^thfe P-5, P-10
                                                    ;ent specification.  The
                                                          s been
                                                         erfere with the
                                         to ,fcuGfeide the facility or to a
                                           bf/contaminants into the
3.6.2.4
              Flame ionization det
   3.6.2.5    Data syste
   GC/ECD.  The data sy,
   throughout the dur
   the minimum, the
   data.  Also, the
   in order to report
   this method.

 3.6.3 Reagents

      The
   choose
   in the
   data  i,
   hydro
   leak
   gas .   All
   copper
   controllers  with r
                                                 terfaced to the GC/FID or
                                                us acquisition of data
                                               program and must permit, at
                                              (peak height or peak area)
                                  be able to rescale chromatographic data
                                 meeting the requirements listed within
                             je  applications  is  helium.   Laboratories may
                               :rier gas, but must clearly  identify  its use
                                divider pages preceding  raw chromatographic
                                *y.  Laboratories that choose  to use
                                 caution in  its use.  Use  of  a hydrogen
                                    when hydrogen is used  as  the  carrier
                           Lnes1  must be constructed  from  stainless steel  or
                             ttiluoroethylene  (PTFE)  thread  sealants  or flow
                            ^onents are not to be used.
 Julv, 1991
                                                              Page D - DZ/SV
-------
Exhibit D
                                                      SOW No.  XXX -  Ambient Air
3.6.4 Standard Preparation

      3.6.4.1      Single-component Standards
         3.6.4.1.1
         3.5.5.
                      Prepare stock standard solution
                                       to  section
         3.6.4.1.2    Prepare the screening standa/d
         the stock solution in an appropriate solj
         outlined in Table D/SV-1.
      3.6.4.2
                  Multicomponent  Standards
         3.6.4.2.1    Prepare a stock solution
         Toxaphene/Aroclors as in part 3.5

         3.6.4.2.2    Take an aliquot of th^xstocf
         standard and mix with hexane to give
         ng//jL.
                                                        ion of the Aroclor
                                                        ncentration of  10
3.6.5 Instrument Operating Conditio
      GC Column:

      Carrier Gas:
      Flow Rate:
      Column Program:
      Initial Time:
      Rampe Rate:
      Final Temperature:
3.6.6 Retention Time (

   3.6.6.1    Before
   must be establis
   system is within
   the standard containr
   determination over a 72-
   ±0.5 minutes o^£—the—cetentio
   3.6.6.2
   times fo
   standar
   substicut
   devel/p a
   retent
   new GC co
   notebook
   assurance
DB-5 fu\ed
bonded,
Helium,  28
1 cm/minute.
Initial Tempe
1 min
                                                               methyl siloxane
                                                       to 3"C/min
July, 1591
                                                 he  retention time  windows
                                                2-hour period.   Make sure the
                                   ng conditions.  Make three injections of  -
                                  ipounds for retention time window
                                    .od.   The retention window is defined as
                                 firoesxfor each standard.
            by th«:Lab0s]
             check ol
    idard desolation of the three absolute retention
        standard.   In those cases where the
       ,ular standard is zero,  the laboratory must
        >n of a close eluting,  similar compound to
        indow.   The laboratory must calculate
        standard on each GC column and whenever a
       ie data must be noted and retained in a
   as/part of the user SOP and as a quality
     ical system.
                                                                Page D - 53/SV
-------
Exhibit D
                                                     SOW No. XXX  -  Ambient Air
                                                            s must be allowed
3.6.7 Sample Analysis

   3.6.7.1    All  standards,- field and QC samples,  and b,
   to warm to ambient temperature before preparation o

   3.6.7.2    Inject 1 /iL of the  extract using the
   technique when using capillary column.
   NOTE:   Smaller volumes (less than or equal to
   automatic devices are employed.
   3.6.7.3    Record the volume  injected and
   units or peak height.
   3.6.   4    For each single component and^surrogate / a RT is measured in
   each  of the calibration standards analysesxf  ana
  analyte;
Lyte;  and
   3.6.7.5    A retention
   analyte and surrogate/and/for te
   multicomponent analytfe.  /Windows) are cent
   retention time for jzfae/analyte
                                      is calcurated\for each single component
                                           peaks \{ 3/to 5) of each
                                                   ound the average absolute
                                                  ng the initial calibration.
   3.6.7.6    Identify the\singl^ component analyte peaks based on the
   retention time windows estasistted during the initial calibration sequence.
   Single component analyce* are Identified when peaks are observed in the RT
   window for the analyte on the GC columns.
   3.6.7.7
   each multi
   peak are 4et
   multico
          /"   /
   conjunctions with
   The number
   aroclors>
                               et of^^ehre^ to five major peaks is selected for
                                 termir^ion.  Retention time windows  for each
                                calibration standards.  Identification of a
                                    iple is based on pattern recognition  in
                                   three  to five sample peaks of  the standard.
                           quanttitaltion peaks are listed below for selected
 July,  1991
                                                                 Page D - 34/SV
-------
Exhibit D
                                                SOW No. XXX - Ambient Air
      Multicomponent Analvte

         Aroclor  1016
         Aroclor  1221
         Aroclor  1232
         Aroclor  1242
         Aroclor  1248
         Aroclor  1254
         Aroclor  1260
         Toxaphene
                               Number of Potential
                                Quantitation Peaks
   3.6.7.8    The choice of the peaks used £a/t
   identification and the recognition of those
   environmental alteration of the toxapher
   of coeluting analytes, or matrix interi
   alteration of these materials in the em
   raulticomponent analytes in samples may ,
   identical with, those of the standards.  Identl
   inspection of an on-scale pattern.

   3.6.7.9    Calculate the concen
   using the following equation:
where:

   CF  =

   Vi  -

   Df  =
   3.6.7.10   The calibrati
   initial calibration	If tb7
   calibration s^ere baseo^xi peak
   the sample/musj^-be~~i>as^ed oh^peak
                                                      t analyte
                                                      complicated  by  the
                                                    and by  the presence
                                                   h.  Because of  the
                                                  aging of  the Aroclor,
                                                  similar to, but  not
                                                     requires visual
                                                        ent analyte by
                                                                  Eq.  D/SV-14
   then use .peair height to"
                                                    ;al standard (per ng) ;
                                                 ) ;  and
                                                 If  the extract is not
                                                 extract  is  diluted,  Df is
                                used are those from the most recent
                                      factors used in the initial
                                   len the response of the analyte in
                                     Similarly, if peak height was used,
                          nine the concentration in the sample.
              Jsing the external calibration procedure,  determine the identity
         3i-<$^antity of each component peak in the sample chromatogram through
   retention time window and concentration level of standards.

   3-6.7.12   I&x^s rebtimmendfed xfhat extracts be diluted so that all peaks are
   on scale.   OverI^Rping>/aks/are not always evident when peaks are off
July, 199L
                                                           Page D  -  55/SV
-------
Exhibit D
                                                     SOW No. XXX  - Ambient  Air
   scale.   Computer reproduction of chromatograms,  manipulated7 to ensure all
   peaks are on scale over a 100-fold range, are acceptable ift linearity is
   demonstrated.   Peak height measurements are recommended ofver peak area
   integration when overlapping peaks cause errors  in area integration.

   3.6.7.13   Establish daily retention time windowsxior/eacn^-analyte^  Use
   the absolute retention time for each analyte as  «ie /midpointc-f theVindow
   for that day.   The daily retention time window yeqjials the midpoin^t
   times the standard deviation.
   3.6.7.14   Tentative  identification of an
   sample extract falls  within the daily rete

   3.6.7.15   If no  sample  peaks  are  detect
   deflection, the undiluted extract  is ac
   sample peaks are  greater than the  80 perce
   the dilution necessary to reduce the major
   scale deflection.   Use this dilution factor to df
   GC/MS analysis.
3.7
      BIBLIOGRAPHY
                                              pea
                                                           when a peak from a
                                                             w.

                                                           ess than full scale
                                                             analysis.   If any
                                                         lection,  calculate
                                                         ween half and full
                                                             extract prior to
3.7.1    Glaser, J.A.,  D.L.  Forest, G>
"Trace Analyses for Wastewaters",  Envi
3.7.2
1980.
         Ballschmiter,  K.  and M.  Zell,  FreVenius/Z. Anal.
                                                            'and W.L. Budde,
                                                    mol. 15, 1426, 1981.
                                                              . ,  302, 20,
3.7.3    "Carcinogens - W<
Service, Center for Dise
Safety and Health, Publyca

3.7.4    "OSHA Safety/and^ Health
Occupational Safety
1976.

3.7.5    "Safety in Academic
^oc  —• Publicat

3.7.6    Mul
L.M. Safe,
Properties
                                      arcinogenV1,  Department of Health
                                           al Ins^iKute for Occupational
                                                   977.
3.7.7    
-------
Exhibit D
                                                      SOW No.  XXX -  Ambient Air
PolychLorinated Biphenyls as Isomer Groups", Anal. Chem.
                                                                    1985.
3.7.9 Rote, J.W. and W.J. Morris, "Use of  Isotopic Abundance/Ratios  in
Identification of Polychlorinated Biphenyls by Mass Spe/trdmetry"  J  Assoc
"Tie. Anal. Chem. 16(1), 188, 1973.                                        '
3.7.10   Methods For Organic Chemical Analysis of MunicXp^Kand
Wastewater, U.S. Environmental Protection Agency,
Support Laboratory, Cincinnati, OH, EPA-600/4-82-(H7July, 1983>

3.7.11   Method 680:  Deterioriation of Pesticides/and PCBs in Water an-.
Soil/Sediment by Gas Chromatography/Mass Spect/rom/try,  U.S. Environmental
Protection Agency,  Environmental Monitoring and .Support laboratory
Cincinnati, OH, Draft April, 1987.

3.7.12   Method 8270A:  Test Methods for ^yalvia^ing Solid Waste,  U.S.
Environmental Protection Aency, Office of S*kUd Wa^e and Emergency Response
Washington, D.C.,  SW-846,  Third Edition, November, 19
                                                                fage D  -  57/SV
-------
Exhibit D
                                                      SOW No.  XXX - Ambient Air
                                 TABLE D/SV-1

                 COMPOSITION AND APPROXIMATE CONCENTRA1]
                             CALIBRATION SOLUTIONS
                                     CAL 1
Target Compound
PAHS
Acenaphthene
Acenaphthylene
Anthracene
Benzo(a)anthracene
Benzo(a)Pyrene
Benzo(b)fluoranthene
Benzo(e)pyrene
Benzo(g,h,i)perylene
Benzo(k)fluoranthene
Chrysene
Dibenzo(a,h)anthracene
Fluoranthene
Fluorene
Indeno(l,2,3-c,d)pyrene
2-MethylnaphthaLene
Naphthalene
2-Naphthylamine
Phenanthrene
Pyrene

OTHER SVOCs
Acetophenone
Aniline
Benzyl alcohol
p-Biphenylamine
Bis(n-butyl)phthala
Butylbenzylphthalate
4-Chloro-3-methylphenol
4-Chloroani1ine
Bis(2-chloroeth
Diethyl Phtha
2,4-Dimethyl
DimethyIpht
4,6 - initr/D-2/methylphenol
2,4-Dini
2 ,4-Dini/^ro
Bis(2-ethy
Hexachlorobenz"
Hexachlorocyclope
Hexachloroethane
Isophorone
 July,  1991
                                                                 Page D  -  D8/SV
-------
Exhibit D
SOW No. XXX - Ambient Air
4-Methyl phenol
2-Methyl phenol .
3-Nitroaniline
2-Nitroaniline •
Nitrobenzene
4-Nitrodiphenyl
2-Nitrophenol
Nitrophenols (mixed)
Bis(n-octyl)phthalate
Pentachlorobenzene
Pentachlorophenol
o-PhenyIpheno1
2,4,5-Trichlorophenol
2,4,6-Trichlorophenol

PESTICIDES
Aldicarb
Aldrin
Bendiocarb
Benzidine
alpha-BHC
ganuna-BHC (Lindane)
Captan
alpha-Chlordane
gamma-Chlordane
Chlordane (Technical)
Bis(2-chloroethoxy)methane
Chlorothalonil
Chlorpyrifos
Daethai (DCPA)
4,4'-ODD
4,4'-DDE
4,4'-DDT
Diazinon
Dichlorvos (DDVP)
Dicofol
Dieldrin
Endosulfan
Endosulfan
Endrin
Endrin Aldeh/de
Endrin keto,
Folpet
Heptachl
HeptachVor
Mirex
Oxychlordane
Parathion
400
400
500
200
400
400
500
400
400
400
100
500
500
500
400
400
400
500
500
500
400
100
100
100
100
500
500
400
400
400
400
500
400
800
800
1,000
400
• 800
800
1,000
800
800
800
200
1,000
1,000
1,000
800
800
800
1,000
1,000
1,000
800
200
200
200
200
1,000
1,000
800
800
800
800
1,000
800
July, 1991
           Page D - 39/SV
-------
Exhibit D
                                                        SOW No. XXX  - Ambient Air
cis/trans-Permethrin
Prop'oxur
Resmethrin
Ronne1
Toxaphene

PCB Calibration Congeners

  C12

  Cl!
  Cls

  C17
  C18
  Cl,
  Clio

Polybrominated biphenyls

Internal  Standards
1,4-Dichlorobenzene-d4
Naphthalene-d8
Acenaphthene - d10
Phenanthrene-d
Chrysene-d12
Perylene-d12
Surrogate Compounds
13C6- Gamma -BHC
13C12-4,4'-DDT
13C6-4-Monochl'
               10
 JC.,-3,3',4,4'-Teti
                 .orobi
13,
 C12-2,2',3.3',5,5'.6,6'-O.
13C12 - Decachlorob ipheny
2,4,6-Tribromophenol
2 -Fluorophenal
Phenol-d5
                                                                          1,000
                                                                          1,000
                                                                          1,000
                                                                          1,000
                                                                            800
                                                                            200
                                                                            200
                                                                            400
                                                                          L.OOO
                                                                          1,000
                                                                          L,000
                                                                            400
                                                                            400
                                                                            400
July,  L99L
                                                                   Page D  - '60/SV
-------
Exhibit D
                 SOW No. XXX  - Ambient Air
                                 TABLE D/SV-2

                          GC/MS OPERATING CONDITIONS
   Activity
   Gas Chromatographv
   Column
   Carrier Gas

   Injection Volume
   Injector Temperature

   Temperature Program
   Initial Column Temp.
   Initial Hold Time
   Program

   Final Temperature:
   Final Hold Time
   Mass Spectrometer
   Transfer Line Temperatur,
   Source Temperature:
   Electron Energy:
   lonization Mode:
   Mass Range:

   Scan Time:
Conditions
J&W   Scient
phenylmethj
   film tt
      DB-5   cross
 Llicone  (30  m x 0.
less)  or  equivalent
                       en
July, 199L
                                                                    32
 5%
1.0
            28-29  cm3/sec  at

        litless
                           1 min.  Increase
                      ompounds of interest
250-300\C
Accordingxto Manufacturer's Specifications.
 0 volts (nominal)

             ,  full range data acquisition

           scans per peak, not to exceed 1
second per scan.
                            Page D  - 61/SV
-------
Exhibit D
                          SOW No. XXX - Ambient Air
                                 TABLE D/SV-3
              INTERNAL STANDARDS FOR SEMIVOLATILE GC/MS
1. 4-Dichlorobenzene-di
Aniline
Benzyl alcohol
Bis(2-chloroethyl)ether
2 -Fluoropheno1
Hexachloroethane
2-Methyl phenol
4-Methyl phenol
Phenol-d;
Naphthalene-da
Acetophenone
p-Biphenylamine
B    i    s    (    2
chloroethoxy)methane
4-Chloro- 3-methylpl;
4-Chloroaniline
2,4-Dimethyl phei
Isophorone
2-Methylnaphth=
Naphthalene
Nitrobenzene
Nitrobenzene-i
4-Nitrodiphenyl
2-Nitropl;
Nitrophe
 .cenaphth>
Acenaphthyler
Diethyl Phthala£e\^  /
Dimethylphthalate ^^
  4/s,Dinitrophenol
      nitrotoluene
     !orobiphenyl
     ene
   .achlorocyclopentadie

   aphthylamine
      oaniline
                                                       2,4 T
                                                       2,4,6-Tribromophenol
                                                             rTrichlorophenol
 July, 1991
                                      Page D -  62/SV
-------
 Exhibit D
                                                       SOW No. XXX - Ambient  Air
                            TABLE D/SV-3  (Continued)
               Internal Standards for Semivolatile  GC/MS
                                                             |/ysis
Phenanthrene - dtn	
Aldicarb
Aldrin
alpha-BHC
gamma-BHC  (Lindane)
13CS-Gamma-BHC
Anthracene
Bendiocarb
Bis(n-butyl)phthalate
Butylbenzylphthalate
Captan
Chlorothalonil
Chlorpyrifos
Dacthal (DCPA)
Diazinon
Dichlorvos  (DDVP)
4,6-Dinitro-2-
methylphenol
Endosulfan  I
Fluoranthene
Folpet
Heptachlor
Heptachlor  Epoxide
Hexachlorobenzene
Oxychlordane
Parathion
Pentachlorobenzene
Pentachloropheno1
Phenanthrene
o-Phenylphenol
Polybrominate'd biphenyls
Propoxur
Ronnel
                            Chrvsene-d1?	
                            Benzidine
                            Benzo(a)anthracene
                            B    i    s    (   2
                            ethylhexyl)phthalap
                            alpha-Chlordane
                            gamma-Chlordane
                            Chlordane (Technical)
                            Chrysene
                            4,4'-ODD
                            4,4'-DDE
                            4,4'-DDT
                            13C12-4,4'
                            Dicofol
                            Dieldrij
                            Endosul
                            Endrin
                            Endrin All
                            Methoxychlo^
                            cis/trans-Pei
                            Pyrene
                                 jhrin
                           'Toxaphet
-DDT
 2hy\e
                                     rl-d
July, L991
                                         14
                            Monochl/orobiphenji
                            13C6 -4 yMonochlc^Bobiphf
                            D ichLx>r oliS ipheny Is""
                            rriahlo/tobiphenyls
                            Tetrachlorobiphenyls
                            V C iSsT 3 .  3  ' .  4  , 4
                            TsXachlorolHphenyl
                            Penta^hlorols^phenyls
                              xachlo^isob ipl^eny Is
                                achlorob-iphenyls
                   Benzo(a)P>
                   Benzo (b) fluora*vtheri€
                   Benzo(e)pyrene
                   Benzo(g,h,i)perylene
                   Beftstp (k) f luoranthene
                   lis (A- oc tyl) phthalate
                   )ib4nzo(a,h)anthracene
                   Endrin ketone
                   mdeno (1, 2 , 3 - c, d) pyrene
                   lirex
    ,2-2.>>' , 3 , 3 ' , 5, 5' , 6 . 6 ' •
 Oc t acntoropiph eny1
 NonachTorobiphenyls
      ilorobiphenyl
^Ci2/Decachlorobiphenyl
                                                                 Page  D  -  63/SV
-------
Exhibit  D
    SOW No.  XXX - Ambienc Air
                                  TABLE D/SV-4

                  PCB CONGENERS  USED AS CALIBRATION ST,


PCS Isomer Group              Congener Number*

Concentration  Calibration Standard
  Honochlorob iphenyl
  D ichlorob iphenyl
  Trichlorobiphenyl
  Tetrachlorobiphenyl
  Pentachlorobiphenyl
  Hexachlorobiphenyl
  Heptachlorobipehnyl
  Octachlorobiphenyl
  Nonachlorobiphenylb
  Decachlorobiphenyl
2,2-3,3',4,4',5,5',6,6'

Retention Time Calibration Standar

  Tetrachlorobiphenyl
  Pentachlorob iphenyl
  Nonachlorobiphenyl
          2
          2,3
           ,4,5
          2,2',4,6
          2,2',3,4,5'
          2,2'4,4',5,6'
          2,2'3,4',5,6,6'
          2,2'3,3',4,5',6,6'
          3,3',4,4'
          2,2',4,6,6'
          2,2',3,3',4,5,5',6,7'
A Numbered according to the s;
b Decachlorobiphenyl is used
  ion 3.7, Citation 2).
-and decachlorobiphenyl isomer groups.
 July,  1991
               Page D - 64/SV
-------
Exhibit D
                                  SOW No. XXX - Ambient Air
               Mass

                51

                68
                69
                70

               127

               197
               198
               199

               275

               365

               441
               442
               443
              TABLE  D/SV-5

DFTPP KEY IONS & ION ABUNDANCE CRITi


                 Ion Abundance  Or

                 30-80%  of mass/19

                 Less than 2%/ot>mass  69
                 Present
                 Less than/2% of  mass  69
                 25-752

                 Le s s
                 Base  peS
                 5-9%  of ma!
  198
itive  abundance
July, 1991
                 10-30%  of mass  19
                                             Page D -  65/SV
-------
Exhibit D
                                                     SOW No. XXX - Ambient Air
                                 TABLE D/SV-6
         RELATIVE- RESPONSE FACTOR CRITERIA FOR INITIAL
                 CALIBRATION OF SEMIVOLATILE TARGET CO;
                                                             NTINUING
                                      Minimum
                                        RRF
Semivolatile
Compounds
2-Methylnaphthalene
2-Methylphenol
2-Nitropheno'l
2,4-Dimethylphenol
2,4-Dinitrotoluene
2,4,5-Trichlorophenol
2,4,6-Trichlorophenol
4-Chloro-3-methylphenol
4-Methylphenol
Acenaphthylene
Acenaphthene
Anthracene
Benzo(a)anthracene
Benzo(a)pyrene
Benzo(b)fluoranthene
Benzo(g,h,i)perylene
Benzo(k)fluoranthene
bis(-2-Chloroethoxy)methane
bis(-2-Chloroethyl)ether
Chrysene
Dibenzo(a,h)anthracene
Fluoranthene
Fluorene
Hexachlorobenzene
Hexachloroethane
Indeno(l, 2, 3-cd)pyrene"
Isophorone
Naphthalene
Nitrobenzene
Pentachlorophe^l
Phenanthrene
Phenol-d5
Pyrene
Terphenyl/d14
 July,  199L
                                                                 Page  D  -  66/SV
-------
Exhibit D
                SOW No.  XXX -  Ambient Air
                                 TABLE D/SV-6
         RELATIVE RESPONSE FACTOR CRITERIA FOR  INITIAL
                 CALIBRATION OF SEMIVOLATILE TARGET COMP,
                                  (continued)
                          INUING
SemLvolatile
Compounds

Naphthalene
Acenaphthylene
Acenaphthene
Fluorene
Phenanthrene
Anthracene
Fluoranthene
Pyrene
Benzo(a)anthracene
Chrysene
Benzo(b)fluoranthene
Benzo(k)fluoranthene
Benzo(a)pyrene
Indeno(l,2,3-cd)pyrene
Dibenzo(a,h)anthracene
Benzo(g,h,i)perylene
Minimum
  RRF
Maximum
  2
imum
:iaium     trajcimu
RSD/X.  XDifrf
July,
                           Page  D  -  67/SV
-------
Exhibit D
                        SOW  No.  XXX -  Ambient Air
                                  TABLE D/SV-7
       QUANTITATION. CONFIRMATION, AND  INTERFERENCE CHEC
                  INTERNAL STANDARDS, AND  SURROGATE CO*
                                  FOR PCBs,
Analyte/
IS/Surr. Comp.

PCB Isomer Group

    C12
    C13
    C14
    C15
    C16
    C17
    C18
    Cl,
    Clio
                  Quant.
                     Ion
                  188
                  222
                  256
                  292
                  326
                  360
                  394
                  430
                  464
                  498
Confirm
   Ion
190
224
258
290
324
362
396
428
466
500
Internal Standard  (IS)
  Chrysene-d12     240
  Phenanthrene-d10
Surrogate Compound
  13C6-gamma-BHC   187
  «c12-4,4' -DDT   247
1 Ratio of quantitacion ion
Expected
 Ratio3
3.0
 July,  1991
                                    Page D - 68/SV
-------
Exhibit D
                  SOW No.  XXX - Ambient Air
                                 TABLE D/SV-8

           CHARACTERISTIC IONS FOR SURROGATE AND INTERN/
Classification

 Surrogates
 Phenol-ds
 2 -Fluorophenol
 2,4,6-TribromophenoL
 Nitrobenzene-d5
 2-Fluorobiphenyl
 p-Terphenyl-du

 Internal Standards
 1,4- Dichlorobenzene -d<,
 Naphthalene-da
 Acenaphthene-d10
 Phenanthrene-d10
 Chrysene-d12
 Perylene-d12
Primary Ion
Secondary
                                                                Page D - 69/SV
-------
Exhibit D
                                                      SOW No.  XXX -  Ambient Air
                                 TABLE D/SV-9

                   CHARACTERISTIC  IONS FOR TARGET  COMPOJE
                         OF PAHs,  PCBs,  and PESTICIDES,
                                          Pr imarv I*
                                              152
                                              153
                                              159
                                              166
                                              170
                                              173
                                              178
                                              178
                                              181
                                                                       225
                                                                       257
                                                                       296,  291
                                                                       330
                                                                       364,  361
                                                                       392,  400
                                                                       434,  431
                                                                       494,  504
Compound

PCS congeners8
  2-Cl1-PCB(l)
  2,3-Cl2-PCB (5)
  2,4,5-Cl3-PCB (29)
  2,2',4,6-Cl4-PCB (50)
  2,2'3,4,5'-Cls-PCB  (87)
  2,2',4,4',5,6'-Cl6-PCB (154)
  2,2',3,4',5,6,6'-CL7-PCB (188)
  2,2',3,3'4,5',6,6'-CLg-PCB (200)
  2,2'3,3',4,4',5,5',6,6' -C110-PCB (209)
Pesticide Analvtes
  2.4-D
  aldrin
  endrin aldehyde
  Captan
  heptachlor
  DDVP
  trans-nonachlor
  Propoxur
  Oxychlordane
121
  Resmethrin
81
  Ronne1
  Naphthalene
  Diazinon
  Dicofol
140
  Carbaryl
  Bendiocarb
51
  Acenaphth
  Acenaph
  Toxaph
  Fluor
  1-Pheny
  Malathion
  Anthracene
  Phenanthrene
  beta-BHC
  , 45, 85, 175,  220
263,  220
345,  250
119,  117, 77, 149
272,  274
79,  185, 187, 202
98,  85, 73,  65
111,  41, 43, 81
57,  87, 117, 149,

128,  143, 141, 171,

119,  93, 79,  57, 62
129,  127
179,  199, 93, 97
111,  141,  250,  75,

115,  116, 146
126,  166,  223,  58,

151,.153
152,  154
231,  233
165,  167
169,  168, 141,  115
125,  127, 158,  172
179. 176
179, 176
183, 109
 July,  T991
                                                                 Page D - /U/SV
-------
Exhibit D
                                                      SOW No.  XXX -  Ambient Air
                                 TABLE D/SV-9

                   CHARACTERISTIC IONS FOR TARGET COMPO
                         OF  PAHs,  PCBs,  and  PESTICIDES
  alpha-BHC
  alpha-BHC
  gamma-BHC (Lindane)
  cis-Permethrin
  trans-Permethrin
  endosulfan I
  Chlorpyrifos
  Atrazine

  Fluoranthene
  Pyrene
  methoxychlor
  Benzo(a)anthracene
  Chrysene
  4,4'-ODD
  4,4'-DDT
  4,4'-DDE
  Benzo(a)pyrene
  Benzo(b)fluoranthene
  Benzo(k)fluoranthene
  Folpet
76
  dieldrin
  endrin
  Chlorothalonil
133
  Pentachlorophenol
  endosulfan sulfate
  Benzo(g,h.i)peryle
  Indeno(l,2,3-cd)p
  D-ibenzo (a . h) anthra
  Hexachlorobenzene
  Dacthal
  endrin ketone
  endosulfan I
  hepcachlor /epo
  chlordane/(aLp'ha and/or
   Congener/
                                                             339, 341
                                                             97, 199, 125, 258
                                                             58, 202, 215,  173,

                                                             101, 100
                                                             101, 100
                                                             228
                                                             229, 226
                                                             226, 229
                                                              37, 165
                                                             2>7, 165
                                                              48, 176
                                                             253, 125
                                                             253, 125
                                                             253, 125
                                                             262, 130, 117,  104,

                                                             82, 81
                                                             82, 81
                                                             264, 268, 109,  124,

                                                             264, 268
                                                             387, 422
                                                             138, 277
                                                             138, 227
                                                             139, 279
                                                             142, 249
                                                             45, 44, 142, 221
                                                             67, 319
                                                             339, 341
                                                             355, 351
                                                             375, 377
July,
                                                                 Page  D  -  7I/SV
-------
Exhibit D
                                                      SOW No.  XXX -  Ambient Air
                                 TABLE D/SV-10

        KNOWN RELATIVE ABUNDANCES OF IONS IN PCB MOLEC
m/z
Relative
Intensity
Monochlorobiphenyls
  188   100
  189    13.5
  190    33.4
  192     4.41

Dichlorobiphenyls
  222   100
  223    13.5
  224    66.0
  225   .  8.82
  226    11.2
  227     1.44

Trichlorobiphenyls
  256  100
  257   13.5
  258   98.6
  259   13.2
  260   32.7
  261    4.31
  262    3.73
  263    0.47

Tetrachlorobiphenyls
  290   76.2
  291   10.3  •
  292  100
  293   13.4
  294   49.4
  295    6.57
  296   11.0
  297    1.43
  298    0.9X
m/z
Relative
Intensity
                              8.78
 Relative
Intensity
  324
  325
  326
  327
  328
                 Hepta-chlorofedphenyls
392\
393
^394
3V
W6
397
3)58
399
400
401
402
. A3
^ 5
100
13
98
13
53
-•
17
2
3
.7
.91

.5
.3
.2
.8
.16
.7
.34
.52
                                             Octachlorobiphenyls
                                                           33.4
                                                            4.51
                                                           87.3
                                                           11.8
                                                          100
                                                           13.4
                                                           65.6
                                                            8.76
                                                           26.9
                                                            3.57
                                                            7.10
                                                            0.93
                                                            1.18
                                                            0.15
                                                            0.11
                                             Nonachlorobiphenyls
460
461
462
463
464
465
466
467
468
469
470
471
472
473
474
26.0
3.51
76.4
76.4
100
13.4
76.4
10.2
37.6
5.00
12.4
1.63
2.72
0.35
0.39
July,  L991
                                                     Page D - 72,/SV
-------
Exhibit D
                                            SOW No. XXX - Ambient Air
m/z
Relative
Intensity
Decachlorobiphenyl
494
495
496
497
498
499
500
501
502
503
504
505
506
507
508
509
   20.8
   2.81
   68.0
   9.17
   100
   13.4
 87.3
   11.7
 50.0
   6.67
   19.7
   2.61
   5.40
   0.71
   1.02
  0.13
July,
                                                       Page D  - 73/SV
-------
       Exhibit D
         Figure D/SV-1..  Sampling  Hea
       Protective Cap
    SOW No.  XX3T- Ambient Air
PAHs,PCB/'s and Pesticides
Protective
  Cap
                         105mm
                         Quartz Fiber
                         Filter and
                         Support
         Air Flow
         Exhaust
                     'articulate
                    Filter
                    Support
                      Absorbant
                      Cartridge and
                      Support
           Glass Cartridge
     Adsorbent
     (PUF/XAD-2/PUF)


       Retaining Screen
                                                                      Silicone
                                                                      Gasket
                                                                      Adsorbent
                                                                      Support
       July,  1991
                  Page D  -  /4/SV
-------
Exhibit  D
                             SOW No. XXX -  Ambient Air
  Figure D/SV-2.  Dual Adsorbent Trap for Sampling PAHs,
                                    , and Pesticides
65mm x 125mm
   GLASS
  CYLINDER
'e"o°o o o oo o o oWo
    "
                                                             50mm PUF
                                                                Plug

                                                            Sorbent Bed
       Support
       Screens
                                                           • 25mm PUF
                                                               Plug
July, iyyi
                                       Page D -  75/SV
-------
Exhibit D
Air Flow

   *
                                               105 mm
                                 . XXX - Ambient Air
 Fifeure D/SV-3.   Analytical Sch<
                  riner riuer
                     of PAHs/ PGfes  and Pesticides.
              Surrogate
              Std's Added
                                                      culate
                                                  Pilfer
                                                    pport
                                                  Adso/be
                                                  Cartridog and
                                                      po
                                                  (PUF AXAD -2 / PUF)
                                   Air Flow
                                   Exhaust
                                hyl Ether/Hexane
                                                      Silica Gel Column
     Clean-op
                                 Screening by
                                  c AECD / FID
            Internal
            Standard
                         Nitrogen Slowdown
                              Hydr«carbo>is (PAH *s)
                                                             HRGC/HRMS
      • Detection Limits:
         ng Qn-Column
•\Detection Limits:
  Ona On-Column
      •DB-;
                        • Detection Limits:
                          SOng On-Column

                        • DB-5 Column
 July, 1991
                                       Page D - /o/av
-------
Exhibit D
                                                        SOW No. XXX  - Ambient Air
                                                       KudeiW-I
                         Filter
      Surrogate Standard
           Addition
        Hexane Rinse
      Figure D/SV-4.  Soxhiet Extraction Followed Bv Kuderna7-Danish (K-D)
Evaporator.
    Adsorben^
PUF/XAD-3/PUF
                                 Soxhiet Extraction wi
                                Diethyl Ether/ Hexana(1:9
                                v/v) (18 Hours/3 Cycjes/tjfj
                                  Vblume Adjusted \
                                     U^OmL  \/
                                Concentrated to 1 ml_
                               with^Nitrogen Slowdown
                 Internal   \
             Standard AdoWony
                 (optional)	
                                vaporatoKAttacrje  wi
                                            r
                                                              Hexane Rinse
              raterBathat50°C
                                                                 Internal
                                                             Standard Addition
 July, 1991
                                                                    Page D - ///SV
-------
Exhibit D
                                                     SOW No.  XXX - Ambient Air
                                                     	XV.	
   .  Figure D/SV-5
                    Optional GC/ECD/FID  Screening of
                        PUF/XAD-2 Adsorbent Cartridge.
ted Filter and
                                                   Can
                                                  Recorder
                                                    And
                                                  Integrator
July.
                                                                   page D -
-------
 Exhibit  D
                                                     SOW No. XXX -  Ambient Air
                        =nteY PIU5 PUF/XAD-2
               Figure
                              nf. an /XfO CtrtofH
                              Soxhlet
                             Extraction
                              Kuderna-   /
                      Danish (K-D) Concentrator
                                    InitiahCalipration
                                    Using WiltPPoint
                                    Calibration Standards
                                    -Relative Response
                                   \Factors (RRF)
                                    -Systems Performance
                                    Check Compounds
        Routine
      Calibration


-Continuous Calibration
 Check (CCC)
July, 1991
                                                                Page D - 79/SV
-------
Exhibit
D Ion Abundance
Criteria to Maat PFTP-g
                                        GCJMS
                                      Performance
                                    Tuning and Mass
                                  Calibration to DFTPP
                                     Specifications
  Figu
          Mass Assignment
         and ion Abundance
        Criteria Demonstrated
           Each 12-Hours
         Initial Calibration At
         Five Concentration
        Levels of Each Analyte
        and Internal Standard
         Calculated Relative
        Retention Time (RRT)
       and Mean RRT for Each
        Analyte and Internal
             Standard
                           Initial CaliBrationFor
                           Each Analyte ah€l_a!l
                           Internal/Surrogate
                           Standards
                                                      Calculate Relative
                                                    Response Factor (RRF)
                                                    For each Compound At
                                                    Each Concentration Level
                                                           System Performance
                                                           Check Compounds (CCC)
   Sample Component Relative
   Time (RT) Must Compai
   Within 0.06 RRT of Statfda
   Compound
Standard
  Compare RF For Eac
   Fron/l2-«our Stan<
   InitiarGaJib
   Accepta
                                                  .j^Verify Acceptability For
                                                     nimum, Maximum % RSD
                                                    and Max. % Diff. For Each
                                                           Analyte	
                                                    Comparison of Sample
                                                   Mass Spectra to Standard
                                                   • Ion Mass
                                                   • Ion Intensity
                                                   • IS area  	
   Calculation of
   Concentration   ^
   Utilizing RRFs
 For TCLs and TICs
                                                           Calculation of:
                                                             Surrogate Recovery
                                                             Internal Std ARC and
                                                             RTS
                  Continuing Calibration
                                                   Continuing Calibration Check
                                                   (CCC) must be analyzed Each
                                                        12-Hour Period
 July,  1991
                                                          Page D - 80/SV
-------
Exhibit D
                                                        SOW  No.  XXX  -  Ambient Air
                   Figure  D/£ 7
                                         Prepare Calibration Standards
                                                             7
            Internal Standards
          Having Simflar Behavior
            to Compounds of
            Interest Normally
            Deuterated PAHs
                                 TuneGC/MStoDFTPFy
                                      Specifications   /
Internal Standard
                                          ±
                                  Calibration Tecrdo^
Standard
(OpUona/)
           Prepare Calibration
               Standards
        Add Internal Standards to
        Calibration Standards and
            Sample Extract
       Inject Clatoratran Standards:
           Calculate Response
       	Factor (RRF)
       Verify Working Calbration
         Curve or RF Each Day
         Calibration
^StandarBsforEach
          ofmterest
                                                                                       f
                                                                   Inject Calibration Standard:
                                                                  Prepare Calibration Curve or
                                                                     Response Factor (RF)
                                                                   Verify Working Calbration
                                                                 ~>  Curve or RF Each Day
Concentrate Extract
  and Reanalyze^
                                             Introduce ExtractJttto
                                               /MSDirechniecOon
                                                          v
                                           Does^esponse^xceed
                                          /Linear Rdnge ats vstem?
                                          Does Response Fall Below
                                           Method Detection Limits?
                                                          Yes,
                                                                        Dilute Extract
                                                                        and Reanalyze
                                           Calculate Concentration o<
                                                 Anaryte, Using
                                             Cafe ration Curves
                                        ation(
                                        T
                                          GC / MS Performance Test
                                                                      12-Hr Continuing
                                                                      Calibration Check
                                            System Performance
                                                  Check
July,  L991
                                                                     Page D  -
-------
ANALYTICAL METHODS FOR
   OF IKt5RGANiC\COMPOUND£
                 SRS AND
               3UPJ
EMI '
  'ETERMINATION
COLLECTED ON
  .YZEJD  BY
      ) ATOMIC
        FURNACE
    CTROMETRY
-------
                                   SECTION 4
4.1


4.2


4.3

4.4


4.5

4.6
                    ANALYTICAL METHODS FOR THE DETERMINATION
                      OF INORGANIC COMPOUNDS  COLLECTED ON
                         HI-VOL FILTERS AND ANALYZED BY
                    INDUCTIVELY COUPLED PLASMA (ICP) ATOMIC
                       EMISSION SPECTROMETRY  OR GRAPHITE
                 FURNACE ATOMIC ABSORPTION (GFAA) SPE^TROMETi
                               TABLE OF CONTENTS
INTRODUCTION	/../...  ./^	D - I/IN

SAMPLE PREPARATION BY MICROWAVE EXT
AND RELATED HANDLING PROCEDURES    -^X^  • ^\/  /	D - 2/IN

SAMPLE ANALYSIS BY ICP	-^X  -^\	D   8/IN

ALTERNATE SAMPLE PREPARATION/FOR GFAA-At}ALYSIS   .  .  .>*/.  .  .  .  D -36/IN

SAMPLE ANALYSIS BY GFAA    .  \ \^^77. ^_  .  /	D -38/IN

BIBLIOGRAPHY	\  .V  ./.	D -60/IN
-------
Exhibit D
                                                 SOW No. XXX  - Ambient Air
                                   SECTION 4

                   ANALYTICAL METHODS  FOR THE  DETERMI
                      OF INORGANIC COMPOUNDS COLLECTED,
                        HI-VOL FILTERS AND ANALYZED
                    INDUCTIVELY COUPLED PLASMA (ICP
                       EMISSION SPECTROMETRY OR G
                 FURNACE ATOMIC ABSORPTION (GFAA) <§PECTROMETRY

4.1  INTRODUCTION

4.1.1 Scope and Application

     4.1.1.1  The methods  specified in  ExhL&it/D must #e
     documented  instrument or method deteoriof
     Required Quantitation Limits (Exhibit
     detection limits  may  be  used only  if the
     five  times  the  documented detection limit
                                           .imits/
                            ed and the
                          t meet the Contract
                         al methods with higher
                 jpple concentration exceeds
                           rument or method.
                                                ftie
                                                   ie ins
    4.1.1.2  All samples must  initially be  run undilutecl\(i.e
    of  the sample  preparation  procedure^":—Whejian analyte
    exceeds  the  calibrated or  linear -tajige  (as app?Op-eia£eJ
    that  analyte(s)  is required afoer smpropYiraite dilution,
                                                            final product
                                                          icentration
                                                         reanalysis  for
                                                         The Contractor
    must use  the  least dilution nece!
    valid  analytical range (but not
    valid  value for each analyte as measured
    analyses.  Unless the Contractor can
    required  to obtain valixi—results,  bothx
    measurements  must be/containeoxin
    shall  be  made with dieio/fize~ik waiser appropi
    constant  acid strejagtt
                      raptor  is  remi
                                                      ilyte(s) within  the
                                                and report the highest
                                            bm the undiluted and diluted
                                            proof that dilution was
                                               and undiluted sample
                                                 All sample dilutions
                                              Ly acidified to maintain
                     quired and
4.1.1.3  The Con,
compendium of
performance of
assurance/quality
association with these"
                               or
                  ioned that Exhibit D is a
     ifitted analytical methods to be used in the
 er/this contract.  The quality
procedures or measurements to be performed in
     or analyses are specified in Exhibit E.
                             is  relttinded
                                     nd cautioned that the collection and
                                     be referred to within the  individual
                            Quality Assurance Protocol of Exhibit E.  The
                             ments are specified in Exhibit B.  Raw  data
                              ciation with the performance of analyses
                              brm to the appropriate provisions of
July, 1991
                                                               Page D-l/IN
-------
Exhibit D
                                                      SOW
                                                                    Ambii
     4.1.1.5  Lab "gl-assware  to be  used in metals analyst
     according to  EPA's manual "Methods for Chemical A:
     Wastes" or an equivalent procedure (see part 4.6)
     opened and digested in  a hood.   Stock solutions
     instrument or method calibration standards may
     as  described  in part 4.6.  All  other solutions/to
     Assurance/Quality  Control measurements shall
     requirements  of Exhibit E.
                                                        ft  be  acid  cleaned
                                                          of Water  and
                                                         Les must be
                                                              r  preparing
                                                                 repared
                                              red /for all
4.1.1.6  Background corrections are requi
Each GFAA analysis requires a minimum of/two' inject
during full Method of Standard Addition/ (MSAs)
shall require a minimum of two replicate  Exposure/
Appropriate hard copy raw data for eabh  expbsure/in
included in the data package in accordanc^witn^Ex}
of each set of exposures/injections shall be"'
sample analysis, and reporting as specified  in
must be reported in the raw data in concentration
                                                           'AA measurements.
                                                             (burns) except
                                                           !CP measurements
                                                        except for full MSA.
                                                         ection shall be
                                                        'ibit  B.  The average
                                                           standardization,
                                                                All exposures
4.2 SAMPLE PREPARATION  BY MICROWA'
PROCEDURES

4.2.1 Introdtict ion

    4.2.1.1  This Section describes a mic^
    extract the  inorganics  from  the
    Following microwave ex/cractior
    GFAA.
                                                        TED
                                                           DLING
                                                extraction procedure  to
                                                 loaded glass-fiber  filter.
                                              ly\es  are analyzed by ICP  or
4.2.2 Sample Preservat}

     4.2.2.1  Ambient/ai
     half lengthwise<(witli
     protective envelo
     to  30°C until analyst

     4.2.2.2  Th
     days.  To/b'e
     samples
     data s

4.2.3 S

     4.2.37
     the Feder>
     11.)  The ino
     hydrochloric aci
                                            uld be received folded in
                                     material inward and enclosed in
                              rotective envelopes shall be stored at 15
                                          under this contract is 180
                            thi^xconcract, the Contractor must analyze
                             if these times are less than the maximum
                              in this contract.
                             it from the 8" x 10" filter as described in
                             for lead (see Figure D/IN-1 and Reference
                           :racted from the filter strip by a
                              solution using a laboratory microwave
July, 1991
                                                               Page D-2/IN
-------
 Exhibit D
                                                     _SOW No. XXX - Ambient Ai;
    ' digestion system.  After cooling, the digestate is centr^fuged  to remove
     any insoluble material-.

     4.2.3.2  Microwave extraction is used to prepare ^amp^es for ICP.  This
     method (using nitric acid only) or an alternate *iot^extrke±ion  technique
     (see part 4.4) may be used to prepare samples

 4.2.4  Apparatus  and Materials
     4.2.4.1  Microwave digestive system and caj
     programmable power settings up to 600 wat
                                 station:  With
                             fsee Figure D/IN-2).
     NOTE:  Commercial kitchen or home-use micr/wave sh
     digestion of samples under this contract./ The
     corrosion resistant and well ventilated.
     protected against corrosion for safe op-ejatiot
                            be used for  the
                       favity must be
                   ct/onics must be
                                   in
     4.2.4.2  PFA Teflon digestion vessels:   Capable of
     of up to 100 psi.   Pressure venting vessels capat
     pressure relief at pressures Breeding 100 psi.  (6(K
     4.2.4.7  Centri
     polypropylene,
     4.2.4.3  Teflon PFA overflow
     capacity).

     4.2.4.4  Rotating table:   For unif
     oven.

     4.2.4.5  Volumetric gl
     borosilicate).

     4.2.4.6  Bottles
     caps,  for storin
     standards (500-
                                      ^standing pressures
                                          atrolled
                                            -mL capacity).

                                         -  to  120-mL
                             t
                              e  of samples within the



                              capacity (Class  A
                              /propylene  with  leakproof
                             r storing multielement
50
Lypropylene  tube  with  screw tops  of
3119-0050 or equivalent).
                        .utomat
                                equiva
                        with  an  accuracy  of  setting  of
                       20  p.L (Grumman Automatic Dispensing
                                 14-793-1) or polypropylene (Fisher 14-8090),
                                  luring shaking.

                                    No.  8500):   To be worn while cutting and
July, 1991
                                                                   Page D-3/IN
-------
Exhibit D
                                                      SOU No/^XXX -  Ambient Air
    .4.2.4.11    Centrifuge:  Capable of maintaining spe
     (International'Equipment company Model UV or equiv,

     4.2.4.12    Template:  To aid in sectioning the
     Federal  Register 1978 43 (Oct.  5),  46258-46261.
                                                              f  2000  rpm
                 Pizza cutter:  Thin wheel  (< 1

                 Mechanical shaker:  Eberbach C
     4.2.4.13

     4.2.4.14
     equivalent.

4.2.5 Reagents
     4.2.5.1  Hydrochloric acid:  American^hem
     grade, concentrated (12.3  M)  (or equiva

     4.2.5.2  Nitric acid:  Redistilled  spectrograp'
     eqivalent),  for preparing  samples.

     4.2.5.3  ASTM Type  II water (

4.2.6 Microwave Extraction Procedurex

     4.2.6.1  Microwave  Calibration ProcN
                                                            (ACS)  reagent
                                                        reparing samples.
      4.2.6.1.1   Calibration of the micro
      to its use.   In orderxcfiat^absolute
      from one microwave unit^tp^ another, the
      determined.
                                                tnit is a critical step prior
                                                 .ettings may be interchanged
                                               ctu$l delivered power must be
      4.2.6.1.2   Calitfratdon of a/lab»3fa^ory"Jirir&rowave unit (see Figure D/IN-
      2) depends on the type of eAectfronic^s^stem used by the manufacturer.
      If the unit has a precise/and/accurate linear relationship between the
      output power amkthe s«^4 used in controlling the microwave unit, then
      the calibration cahxbe a single-point calibration at maximum power.  If
      the unit is not accurate or precise for some portion of the controlling
      scale, ther^-a—nrottiple-point calibration is necessary.  If the unit
      power calibration neetis multiple-point calibration, then the point where
      the linearLty^be~gTms muss be identified.  For example:  a calibration at
      100, W, 9^, 97, 95,^0, SO, 70, 60, and 50 percent power settings can
      be applied and the dataNolo\ted.  The nonlinear portion of the
                                   uded or restricted in use.  Each percent is
                                   .5 - 6.5 W and becomes the smallest unit of
                                     If 20 - 40 W are contained from 99  -  100
                                   microwave calibration is not controllable
                                   of the linear portion of the control  scale
                               'ion of precise power conditions specified in
                                scale.
July, 1991
                                                                    Page  D-4/IN
-------
Exhibit D
             SOW No.  XXX - Ambient Air
      4.2.6.1.3 .  The equations in the following paragraph7 evaluate  the  power
      available for heating in a microwave cavity.  This/isAccomplished by
      measuring .the temperature rise in 1 kg of water eKpoped  to
      electromagnetic radiation for a fixed period of/cimeC  Measurements are
      made on weighed replicates (five replicates) of/1 kg samples  of room
      temperature distilled water in thick-walled mi^
      (Teflon) vessels.  The containers must be circulated conxMea;gure  the  final
      temperature of the water, af^rs£iTriBg^__(Tf) , to withi!n 0.1°C, while
      stirring the water (an electtronie^atirrer using-^a—Large  stir  bar  works
      best) within 30 seconds of the. end ofT~TrTadiation.  IJse  the maximum
      reading.  Repeat for a new sample ,^for a/topalof~~f-tve replicates per
      microwave setting, of distilled roomXterapetfature water using  a new,
      clean container.  Calculate the miarowave/power according to  the
      formula:
                           ^	~~^   -   -  \.  ^
                                                                  Eq. D/IN-1
                                                                  Eq. D/IN-2
                                                                  Eq. D/IN-3
,87  xT
       whe/e
                                  ,t power absorbed by the sample in watts  (W =

                                  ion factor for thermochemical calories-sec"1
                                   to 4.184);
                                 apacity, thermal capacity, or specific heat
                                    = 1.0 for  water) ;
July, 1991
                           Page D-5/IN
-------
Exhibit D
                                                      SOW Ntfxjtxx -  Ambient Air
          M
          T
          t
                   The mass of the sample in grams;
                   Tf  --T!  in  °C; and
                   Time in seconds.
      4.2.6.2.2   Derive an equation for the linear/port ion~xif the\calibration
      range and determine the equivalent value  inX/at^s of  the^arbitrJ
      setting scale.  Use the actual power in waw^vM determined
      appropriate setting of the particular microwave unit  being  used>\Eac
      microwave unit will have its own setting/that corresponds to  the  actual
      power delivered to the samples.
4.2.6.3  Cleaning Procedure for PFA Veaseli

  4.2.6.3.1   Prior  to first use,  new^yesse1
  are  used.   A pre treatment/cleaning
  procedure calls for heating the vessels to*: 96
  vessels must be disassembled during annealin
  (the top of the vessel or the rim) must not be
  vessel during annealing.
                                                     nd
                                                    annealed before  they
                                                  be  followed.   This
                                                  yrs  to  200"C.   The
                                                       sealing  surfaces
                                                  id to ^support the
4.2.6.3.2   Rinse with disti
1:1 HC1 for a minimum of thre^
reached a temperature just belo'
Immerse in a cleaning bath of l:i\HNi
after the bath temperature has reached"a
The vessels are then rinsed with copious
water prior to use fpr"~any~
digestions, the PFA/vesJ5fiJLs snpuld be
rinsed followed b
                                           Immerse
    4.2.6.4  Digestion Procedure .for
                                     tilled
                                    cpwave
                                                            cleaning bath of
                                                           temperature has
                                                            distilled water.
                                              or/a minimum of three hours
                                                emperature just below boiling.
                                                 ounts of deionized, distilled
                                                   s contract.  Between sample
                                                   nt washed and 1:1 HN03
                                                      rinse.
                                             ctraction
      4.2.6.4.1   P^epafexextra/ting acid (2.06 M HC1, 0.89 M HN03)  for use
      with ICP analysis-  Ihva/l-I: volumetric flask, combine in order and mix
      well 500 mL of deibnlzed, <(istilled water, 55.5 mL of concentrated (16
      M) redistilled spectro^raphicxgrade nitric acid, and 167.5 mL of ACS
      reagent-gr>dB~~corieem:rateoXiwdr
-------
Exhibit D
                                                SOW No.  XXX -  Ambient Air
      4.2.6.4.3  . Cut a 1" x 8" strip from the folded partficuAate bearing
      filter using "a template and a pizza cutter as desc/ibe4  in  the  Federal
      Reference .Method for Lead (see Figure D/IN-1 and/Reference  11).  Using
      vinyl gloves or plastic forceps, accordion-fold^or tightly  roll  the
      filter strip and place it on its edge in a cenj
      NOTE:  A breathing mask and vinyl gloves are/
      personnel handling dry glass-fiber filters.
      the inhalation of minute glass shards and
      gloves protect the skin from the same mab^ri^ls and also prevent
      contamination of the sample by skin secyetipns.
      NOTE: It is suggested that more than
      extracted to ensure adequate sample
      analysis.
                                          strip  from
                                     !olume for  s-amr
                                    filter be
                                  e and QC sample
                                                       [The
4.2.6.4.4   Add 10.0 mL of extracting ac^id for
3 M nitric acid for GFAA analysis, using ap
-------
Exhibit D
                              SOW NOX--OCXX -  Ambient Air
    • bottom of the tube.  The matrix is 0.45 M nitric aotd,/1.03 M
      hydrochloric acid for .ICP analysis or 1.5 M nitric/acid, for GFAA
      analysis and deionized, distilled water.  The sample T^ now ready  for
      analysis.

4.3  SAMPLE  ANALYSIS BY  INDUCTIVELY  COUPLED  PLASMA
SPECTROMETRY
4.3.1 Introduction

     4.3.1.1   Inorganic analytes listed in Tal
     List  in  Exhibit  C  are  determined by  ICP
     microwave digestion.   Appropriate step
     potential interference effects.

     4.3.1.2   Table D/IN-2  lists analytes along
     and typical  estimated  instrumental detection
     pneumatic nebulization.   Actual  working detection
     dependent and as the sample matiriX-varies,  these
     vary.  In time,  other  analytes/may
     available.
                                     he Target Analyte
                                    eparation by
                                   to correct for
     4.3.1.3  Because of the differenc
     satisfactory instruments,  no  detail
     can be provided.   Instead,  the  analy
     provided by the manufacturer  of the
4.3.2 Summary of Method

     4.3.2.1  The analyt^ concentrations
     spectroscopic ana
     nebulizer.  The ^era/sol formed i4 tran
     plasma and  the
     and  ionic line
     are  produced when  tfifexelectrc
     The  spectra are disperse^by  a
     line radiations) -aiLe  monit
     photomultiplTier tube(s>^ The
                                 amended wavelengths
                                       conventional
                                        e sample
                                     rations may also
                                        tion becomes
                                     and models of
                          fental operating instructions
                                to the instructions
                            instrument.
                       als^are excited into
     photomul
     concentzrat
     specific
     system a'
                            ned by ICP atomic emission
                          e pumped into a. pneumatic
                         d into an inductively coupled
                        .er electronic states.  Atomic
           4 characteristic of the particular metals
             decay back to the lower energy levels.
              ectrometer and the  intensity of specific
                 Itaneously or sequentially by a
                  rrent produced  by the
                 n direct proportion to the
           in the sample within the linear range of  a
           hotocurrent is processed by a computer
           tation through a calibration procedure.
                                     >tocv
     4.3.
     series o
     the acid
     calibration sta
     matched  to  the  samp
     pe/foi/med by standardizing  the  instrument with a
       :andards and  a blank that  are  matrix matched to
          Every solution analyzed,  such as a dilution,
ity "Vtandard,  or  reference sample must be matrix
        act.
 July, 1991
                                             Page  D-8/IN
-------
Exhibit D
                                                 SOU No. XXX - Ambient Air
    4.3.2.3  Appropriate  steps  must  be  taken to  ensure  th/t potential
    interferences 'are  corrected.   This  is especially imnort^mt for spectral
    interferences.   Recommendations  for correcting for /Interferences are
    briefly  summarized below under headings  that categori£e^ the type of
    interference  that  is  being  considered.

      4.3.2.3.1  Recommended  Corrections for Phys
                                                  t
       •  The use  of peristaltic pump to introduo^
          nebulizer.

       •  Frequent (20  percent or better) an,
          stability  standard.
       •  Adequate rinsing (one minute
          10 percent HN03  or  10 percent
          argon or a nebulizer tip washer as n

      4.3.2.3.2  Recommended Corrections for Chemica
                                                     ample  analyses using
                                                     use of humidified
          Optionally ,/wa
          wavelengths)
          calibratioTkblar?
          performed.
4.3.2.4  Even
       •  Matrix matching between
          diluting the sample duri

      4.3.2.3.3  Recommended Corrections^or Spei
                                                         id  sample
                                                      •ferences
          Use  of calculated interelement\cor
          first or second order equations
          function (on-peak^oeri?e£tion).

          Optional use o
          both sides  of/th<
                                            ons  in the  form of  factors  or
                                          'describe the  interference
                                               shift on either side  or
                                              correction).
Lution,
                             Scarfs  (fb-j^eacb/of  the analyte element
                            >f /he  samples-^simultaneously plotted with  a
                             and a  calibration standard scan may be
                                       calibration standards, calibration and
    method blanks,  and  reference ^*amples>,  must  be  analyzed using two full
    exposure^ (pe-ak~ST&an) ,  e^ch  of whie/i  is  sufficient  to  meet  the  method
    detection lamit for e^ch  analyte  emission line.   All exposure times must
    be  the/same  for all analysesXand  all  quarterly analyses (i.e.,  method
    detec/tioj?l limit and intere,lera\ent  correction factor.)
    4.3>2X5  B>th the off-peaV
    correcrton  cc^&ficients
    all analyte^ must~^b_e  ca^cuJ
                           (b/kckground) and on-peak (interelement
                           equations)  interference corrections made for
                            ted and reported with the analysis results.
July, 1991
                                                               Page D-9/IN
-------
Exhibit D
                                                      SOW Noc-OCXX -  Ambient Air
    '4.3.2.6   If  the  sum of the  values of the interferenq
     on any analyte is greater than the resulting analy
     reported value is to be flagged with an "I" on FQ
                                                        /rrection(s) made
                                                                    the
                                                        UN.
     4.3.2.7   If  the  analyte  requiring dilution inte
     analyte,  the interference corrections)  must r/fl
     concentration of the interferent in the  undi
     4.3.2.8  The specific  spectral  lines  that

     4.3.2.9  All reported  analyte data  must
     linear range of the respective  analyte
     concentration  results  in the linear
     exceeded,  the  sample must be diluted
     concentration  falls within the  linear rl

4.3.3 Safety

     4.3.3.1  The toxicity  or carcinj;
     method has  not been precisely
     should be  treated as a potential
     responsible for maintaining a ci
     regarding  the  safe handling of
     reference  file of material handlihg\dat
     personnel  involved in  the chemical  afialy*
4.3.4 Interferences

     4.3.4.1  ICP emissi
     which  in practice
     cause  a translati
     overlap or  increase
     recombination  cpnti
     For  a  given matri:
     produced that  is
     interference of the  ana
     in sensitivi
                                   icity of each reag
                                               imployed must be repor
                                                        .ed within the
                                                       If any analyte
                                                      ral line being
                                                    •esulting solution
                                                   t below the CRQL.
                 ed in this
                cal compound
              oratory is
              OSHA regulations
             in this method.  A
:he/ts shall be available to all
                                               /interelement effects,
                                              ''forms.   Interferences that
                                             ire caused by spectral  line
                                            'electron/metal ion
                                         light within the spectrometer.
                                line, a constant additive interference is
                             (of the analyte concentration.  Rotational
                               lurve, experienced essentially as a  change
                              combined effects of variations in nebulizer
performance produced byxthe phys4cal/properties of the sample solution
and changes ifithefexcitacion conditions in the plasma caused by the
matrix inetads.  Both forms of interference can operate simultaneously for
a par^Lcu^ar sample matrij

4.3 A.2 ^S^ectral interference! from poorly resolved metal spectral lines,
such aascaCEered light, o/r byroad continuum spectral background, will
lead to systematic error An ,the analytical results unless proper
corrections a^e made^ hjtolecular band emission will lead to a
deterioration of^v^he de'teccion limit and will increase the difficulty of
off-peak backgroun^correetion.  Methods of correcting translational
July,  1991
                                                              Page D-10/IN
-------
 Exhibit D
                                                      _SOW No. XXX - Ambient Air
     interference (.other than exact matrix matching of
     sample) include the on-peak correction technique.
     applied to both spectral line overlap and backgrou
     requires specific knowledge of the metals causin
     peak correction can only be performed on a quan
     interfering metals are included in the multi-m-
     uncertainties may still exist in whether the
     employed match those required for the particu'
                         th
                              nterference.
  andards to the
 'method can be
:ihancement,  but it
               On-
        if the
       Although
          ents
     4.3.4.3  Rotational calibration curve intezTepence manifests itself^f^r a
     given matrix and spectral line as a. chang/6 ii/the slope of the analyte
     calibration.  This type of interference -Include: sanipie nebulization  and
     transport effects, often called physical i/terfere/ce/Including lateral
     diffusion interferences; and chemical /int/rferenc/s ^uch as solute
     vaporization interference and ioniza^ion ic^terferencfes.  Such
     interferences can be reduced by matrix^-matchin^' of/the standards and
     samples and by the method of standard add£t4.pns, ^although standard
     additions can become quite lengthy and impra^t^cablexfor multi-metal
     analyses) and by the use of internal standards /NCatrixNuatching can
     correct for any of these interferences  but the corre^ion/is dependent on
     the accuracy of the matching. /Vartaetw«_an^the matrix^from sample to
     sample will cause corresponding i^ac£uraciesT!rr~the--analyte results.

     4.3.4.4  Listed in Table D/IN-3 \re\ome  i/tei^ference^effects  for the
     recommended wavelengths given in Table\p/^LN-/.  The data in Table D/IN-3
     are intended for use only as a  rudimentary/guide for the indication of
     potential spectral interferences.   Fo\thite  purpose, linear relations
     between concentration aad~±n
-------
Exhibit D
                                                      SOW No^xXXX - Ambient A:
  regression
:al  interference
       of creating
     ler
            net
          and on-peak (coefficients of  first or  second  o
          equations' describing expected interference) s
          corrections.  In addition, the software mus
          a hard copy output of both types of correc
          concentration units or analyte raw intensi
          calculated concentrations .

     4.3.5.2  Argon gas  supply:   Welding grade  or/be

     4.3.5.3  Assorted laboratory volumetric  glassware,  pipets and
     micropipets .

     4.3.5.4  Operating  conditions:   Becauae"  of the  differences among various
     makes  and  models  of satisfactory insG^umenfcsu  no/detteiled operating
     instructions  can  be provided.   Instead/^the anWys/ should follow the
     instructions  provided by the manufacturer  di^the particular instrument.
     Sensitivity,  instrumental detection limit,  prechvdroch4^ric acid,  ASTM Type  I water,  1:1 nitric
     acid,  and  A§JJf-Typft-^I watei

     NOTE:  CKromic ac fo>sha 1 iNno t be  u~s4d because chromium is one of the
     contrac/t required analyses ,\and its use  may lead to cross contamination.

     NOTE/ A/ids  used in  the pVepkration of  standards and for sample
     pro«^essiftgmust be  below t|xe fRQLs for the analytes of interest for the
                    SOW.
    4.3.6.2  Nitr-ic aci'dxa.nd/ hy/irochloric acid used in the preparation of
    standards  and tb^sample processing must be of high purity.
July, 1991
       Page D-12/IN
-------
 Exhibit  D
                                                      SOW No. XXX - Ambient Air
     4.3.6.3  Water equivalent to ASTM Type II is used thr/ugbfout.

     4.3.6.4  Stock standard solutions:   Standards must/be /rom ultrapure
     materials.   The stock standard solutions may be tb4 same as  the  spiking
     standard solutions,  if desired.
     4.3.6.5  Spiking standard solutions:   Standarc
     ultrapure materials.   Both multi-metal and
     needed.  Because of the limited sample voli
     solutions will be needed to maintain the s«
     original strength after the addition of t}
                                               mi/st be Tfeade frl
                                                 metal
                                               .00 mL) , multi-rffetal
                                               matrix at 95 percei
                                             ike volume.
                                            J.1 be
     4.3.6.6    No  more  than five  multi-metal/stock stan<;
     containing metals  in the following concentrations,
                                                       will be required
      Na, Al, Ca, As, Se
      Ba, Co, Mn, Ni, Pb, Ag, Tl, V, K
      Be, Cd, Cu, Cr, Zn, Sb,/JSn, Mo, Fe, Mg

4.3.6.6.1   Using the appro
following standards have

         Metals Mixes

   Al,  Ba,  Be, Fe,  Ni, Ag, Na, Tl
   Ca,  Cd,  Co, Cu,  Pb
   Cr
   V
                                                    Zoncy.  mg/L
    4.3.6.7  A single/me
    each metal.
                                                        500
                                                           lution matrices,  the
                                                        foryone  year.
                                                     20  percent  cone.  HC1
                                                     10  percent  cone.  HN03
                                                     Water
                                                     2 percent cone. HN03
                                          00 mg/L will be needed for
    4.3.6.8  Calibration >fcand/rds/:  Prepare calibration  standards  by
    dilution of stock os^spiKlng/standard solutions.   All calibration
    standards must be matr^matehed with the  extracting  acid solution
    according to£he__p^pearati^n procedure used in the analysis.
    Concentrate^ hydrochlo
-------
Exhibit D
                      sow
                                                                  - Ambient Air
    patched with  the  extracting acid solution according
    procedure  used in the  analysis  with the  following
    given  concentrations:

                   Metals

               Na, Al, Ca, Fe, Mg
            .   Ba, Co, Mn, Ni, Pb, Ag, V, Tl
               Be, Cd, Cu, Cr, Zn
                              ie preparation
                            Ks present  at  the
                                             ffefent
                     The  yhffaial calibration
                     soutce/than that used  for
                oximate/ly in the middle  of  the
                  ion/standard must be in the
4.3-6.11     Initial calibration verifica,
verification solution shall be  from a di
the calibration standards and shall be/ap
respective calibration curve.   This verifier
same acid matrix as  the calibration standards?

4.3.6.12     ICP  interference  check sample:   Prepare By-^dilution of the
stock standards if  it is not available from  the EP?^  If^she  solution is
prepared by the analyst, it shati-be_jnade using the  cbn^entzrations  in
Table D/IN-4.  It shall be run/at  least~~trv»~_times and tne mean  standard
deviation shall be  reported in\the^
    NOTE:  The  interference  check  solution/s)
    known  concentrations  of  interferingX^lei
    magnitude of  interferences  and provi<
    corrections.   The  ICS is used  to verif^
    corrected by  the data sys"tenT~w4;thi-n  qual\ty

4.3.7.  Quality Control

    4.3.7.1  Instrume

      4.3.7.1.1
          Prior to the an.
       shall be initially ca
      4.3.7.1.
                     is prepared to contain
                  that will demonstrate  the
                 'equate test of any
                  the interference levels are
                  pntrol limits.
    samples and  required QC,  each  ICP  system
      to determine instrument sensitivity.
                                  ibrated daily or once every 24 hours and
                                   set up.
          Cal?
       matrix an
       following
 sKall be prepared using the  same type of
  icentration as the preparation blank
tion.
July, 199L
                                   Page D-14/IN
-------
 Exhibit D
                                                      _SOW No. XXX  -  Ambient:  A
          Calibrate according  to  instrument manufacturer';
        procedures using at least two standards, one being

        Before  beginning the sample run, reanalyze the
        calibration standard as if it were a sample.

       4.3.7.1.4   Calculations
                                   ommended
                                  lank.
                     % Recovery =  Found C°ncentrat
                                   True Concentration
      4.3.7.1.5  Technical Acceptance  Crite
          Recovery for the highest mixed
       ±  five percent  of  the  true  value

      4.3.7.1.6  Corrective Action
                             (dard shall be within
                             rcent)
          The instrument
       raw data.  The fin
          Immediate
       of the initial^Valibr
       analyte by-the ana
       Solution(s) CECV)

      4.3.7.2/2'
          Follow instrument manufacturer's recommendations  to"borrect  the
       problem.  Also, baseline  cofffec-trioiu_isaccep table asX^ng as it is
       performed after every samp](e  orafter^h^~c4mtiouing calibration
       verification and blank check:  rVsTop-rng^is  acceptable as long as it is
       immediately preceded and  immeHjat^ly  fol/Loy£dr-by-~a^CCV and a CCB.
      4.3.7.1.7  Documentation
    iized data \nd\ime shall be included in the
concentration sh6uld\be in
     4.3.7.2  Initial Ca/ibjr4tion yer

      4.3.7.2.1  S
        system has  been calibrated,  the accuracy
      shall be verified and documented for every
      ,EPA Initial Calibration Verification
          .ength used for analysis.
                                 vt is calibrated, the ICV shall be run
                                  :alibration, before any samples  are
July, 1991
                                                                  Page D-15/IN
-------
Exhibit D
                                                     SOW Nox-xXXX  - Ambient  Air
    ,  4.3.7.2.3  Procedure

          If the. ICV solution(s)  are not available fron/EPA^xor where a
       certified solution of an analyte is not availayie-^roma^jy source,
       analyses shall be conducted on an independent/sta4da~l?dat
       concentration other than that used for instrument calib>a£ion>^ut
       within the linear range.  An independent st£H4ard is define*
       standard composed of the analytes from a different source than^-those}
       used in the standards for the instrument/caVlbration.
      4.3.7.2.4  Calculations

                    % Recovery =
Found Concentration
 True Concentration
LOO/
Eq. D/IN-5
      4.3.7.2.5  Technical Acceptance Criteria

          Recovery  for  the ICV shall/4ie^within ± 10 percentSxpf ylfhe true value
       (i.e.,  90-110 percent).
      4.3.7.2.6  Corrective  Action

         When recoveries  of the  ICV  exch;
       the  analysis shall be terminated,
       instrument recalibrated,  and the ca}

      4.3.7.2.7  Documentation

         Report  the  1C
       (Mg/L), and

    4.3.7.3   Contin<

      4.3.7.3.1  Summary
                 chnical  acceptance criteria,
                  i corrected, the
               ion reverified.
                    true  concentration
          To  ensu,
       calibra
       every

      4.3.
        during  an  analysis  run,  a continuing
    ion"XCCV) is analyzed and reported for
the ahalysis of each analyte.
                                  .ency of 10 percent or every two hours
                                   hever is more frequent.

                                    the last analytical sample in the analysis
July, 1991
                                 Page D-16/IN
-------
Exhibit D
                  SOW No.  XXX -  Ambient Air
      4.3.7.3.3  Procedure
          The same CCV shall be used throughout the ana
       of samples received.  The analyte concentratio
       calibration standard shall be an EPA solution
       standard solution and should be at or near ±
       range levels of the calibration curve.
                         runs for a Case
                        the continuing
                   r a Contactor prepared
                       ient oC. the mid-
          Each CCV analyzed shall reflect the co
       of the associated analytical samples  (t
       samples or the preceding analytical s
       The duration of analysis, rinses and
       affect the CCV measured result shall Act/be
       greater extent than the extent applied/to the
       samples.  For instance, the differencexin tim<
       and the blank immediately followin,
       time between the CCV and the analyticaixsample
       it shall not exceed the smallest differen<
       consecutive analytical samples associated withxthe

      4.3.7.3.4  Calculations

                    % Recovery
                 ions of analysis^xfor
                eceding 10  analytical
                up  to  the previous  CCV).
               relate^Nqperations  that may
                    ed/to  the  CCV  to  a
                       iated  analytical
                     :ween  a  CCV analysis
                      the difference in
                   mmediately  preceding
                       between any two
          When  recovy
       the analysis^halT
       recalibrated, t
       analytical" samples
       Last complijji£__CCV

      4 . 3 . 7 . 3/
                              Eq. D/IN-6
      4.3.7.3.5  Technical Acceptance Crio^ria<

          Recovery  for  the/CCV sha^ be  withi^ ± \0 percent of the  true value
       (i.e.,  90-110 per/en

      4.3.7.3.6  Corre,
            technical acceptance criteria,
I, the problem corrected, the instrument
 reverified, and the preceding 10
 (or all analytical samples since the
                                  :centration (ng/L),  true  concentration
                                  y on FORM II-AAIN.
July, 1991
                              Page D-17/IN
-------
Exhibit D
                                                  SOW N/>XXX -  Ambient Air
'4.3.7.4  CRQL Standard

  4.3.7.4.1- Summary

      To  verify linearity near the CRQL, the Co/tr«=
   ICP standard at two times  the  IDL or  two  td
   greater.  This standard shall  be run  for
   analysis.

  4.3.7.4.2  Frequency

      The CRQL standard shall be run at/
   sample analysis run, or a  minimum
   is more frequent.

  4.3.7.4.3  Procedure

      The CRQL standard shall not be run before

  4.3.7.4.4  Calculations

                % Recovery =
                                                                        e an
                                                           ,nd end of each
                                                            hours, whichever
                                                                tion.
                                                                  Eq.  D/IN-7
                                  TXUA Coheentialtidn
      4.3.7.4.5  Technical Ac£££tance Criteria

          Recovery of the/CRQIs-s£and^rd shall
       true value for eaten
                                                :hin ± 15 percent of the
                                               ysis.
  4.3.7.4.6  Corre'ct

      If the CRi
   analysis shall
   samples since the

  4.3.7.4.7
                                    not fall within the control limit, the
                                    , the problem corrected and the analytical
                                        CRQL standard  reanalyzed.
                                    found concentration (jig/L) ,  true
                                 ..percent recovery on FORM III-AAIN.
          The conc~Bntratl«n/rang'e over which the ICP calibration curve remains
       linear must be~^determirred and  any values above  this  linear  range  shall
       be diluted and reanalyzed.
July, 1991
                                                               Page D-18/IN
-------
 Exhibit D
                                                     _SOW No.  XXX - Ambient A,
       4.3.7.5.2  Frequency

          For all  ICP analyses,  a  linear  range verific
        shall be analyzed at the beginning and end of
        run,  or  a minimum of twice  per eight hour wor
        more  frequent, but not before the  ICV.   Thi
        all wavelengths  used for each analyte repo
4.3.7.5.3  Procedure

    The standard shall be analyzed as tl
 analytical sample  (i.e., each  measure/
 and/or any other procedure  normally
 separate samples).
                                                      check standard
                                                    Cample  analysis
                                                          whichever  is
                                                           LI  be  run  for
      4.3.7.5.4  Calculations

                     % Recovery =
                            Found Concenti
      4.3.7.5.5  Technical Acceptance

          Recovery for the linear rai
       of the true value  (i.e.,  90-111

      4.3.7.5.6  Corrective Action
                                                   it were a separate
                                                           :ollowed by a rinse
                                                           :n the  analysis of
                                                            Eq. D/IN-8
                                                     ithin ± 10 percent
                                                  dard does not meet the
                                                        shall be terminated
                                                  all be reanalyzed until the
                                              ion of this standard that meets
                                                the instrument linear range
                                               under this contract without
    If the recovery,
 technical accept^nce^c?
 and successive
 control limits
 the control
 beyond whic
 dilution of

4.3.7.5.7  Documenta
          Report the linear rangeXs^tandajds found concentration (in
       true ^once«tra*ion  UX/^g/L) lied/percent recovery for each analyte on
       FORM/I I P^AAIN.   ^    X

    4.3./. 6
                             1C? system is not contaminated,  an initial
                               shall be analyzed after calibration.
July, 1991
                                                                  Page D-19/IN
-------
                                                      SOW Ncr-^XXX -  Ambient Ai:
      4.3.7.6.2  Frequency

          The ICB shall be analyzed each time the systt
       immediately after the ICV.

      4.3.7.6.3  Procedure

          If the absolute value of the ICB is greats
       shall be reported.
      4.3.7.6.4  Calculations

       Not applicable.

      4.3.7.6.5  Technical Acceptance

          The  absolute value  of the ICB must be le>5vvthanxthe CRQL.

      4.3.7.6.6  Corrective Action
                            alibrated and
          When  the  ICB  concentrati
       criteria,  terminate analysis ,\co
       the calibration, and reanalyze\the
                           ical acceptance
                           calibrate, verify
                                           It
      4.3.7.6.7  Documentation

       Report the ICB valu

    4.3.7.7  Continuing

      4.3.7.7.1  Suram

          To  ensure
       run,  continui

      4.3.7.7.2  Frequency

          Anal
       whichever
  'is  not  contaminated during the  analysis
 'blanks (CCB) are analyzed.
         f 10  percent or every two hours,
          A
       absolute
       reported.
  the  last CCV in the analysis run.   If the
is greater than the IDL, the result shall be
July, 1991
                                 Page D-20/IN
-------
Exhibit D
                 SOW  No. XXX  -  Ambient Air
      4.3.7.7.4  Calculations

       Not applicable.

      4.3,7.7.5  Technical Acceptance Criteria

          The absolute value of the CCB must be le

      4.3.7.7.6  Corrective Action

          When the CCB concentration does  not
       criteria, terminate analysis, correct
       the calibration, and reanalyze the
       all analytical samples since the la<

      4.3.7.7.7  Documentation

       Report the CCB values in Mg/L on FORM IV-"}

    4.3.7.8  Preparation Blanks

      4.3.7.8.1  Summary

          To  ensure against contamina\ion\durin|
       preparation blank (PB) is analy^

      4.3.7.8.2  Frequency

          At  least one PB
       each batch of samzfle
      4.3.7.8.3  Proce.

          The PB sh
       sample preparation

          The first batch
       second batch__ofsample
              the technical acceptance
                      ecalibrate, verify
                      ytical samples  (or
                      analyzed).
                      paration, a
                   with every SDG or with
               more frequent.
          •rater processed through each
  procedure step.

in a SDG shall be assigned to FBI,  the
  etc.
                                   ce Criteria

                                  B must be less than the CRQL.
July, 1991
                             Page D-21/IN
-------
Exhibit D
                                                     sow
                                                                   Ambient  Air
      4.3.7.8.6  Corrective Action

          If  the- absolute value of the concentration o;
       equal to the CRQL, sample results are not cor
                                                           is less than or
                                           associ;
      If  any  analyte  concentration in the PB i
   concentration of the analyte in the
   times  the  PB concentration. Otherwise,
   PB and with the analyte's concentration
   concentration and above the CRQL shall
   for that analyte.   The sample concent^at
   the PB value.

      If  an analyte concentration  in
   then all samples reported below 10
   shall  be redigested and reanalyzed.

  4.3.7.8.7  Documentation

      The values  for  the  PB  sh

4.3.7.9  ICP  Interference Check

  4.3.7.9.1  Summary
                                                                        lowest
                                                    than 10 times the PB
                                                            and reanalyzed
                                                             be corrected for
                                                         the negative CRQL,
                                                        ociated with the PB
                                                               RM IV-AAIN.
                                                Correction factors,  an ICP
                                                   of each analysis  run or a
                                                hift, whichever is more
     To verify intereleraent, and
   Interference Check

  4.3.7.9.2   Freque

     Analyze the
   minimum of twi
   frequent,  bu/not

  4.3.7.9.3   Procedur^
          The  ICS--c~5nsT5
-------
Exhibit D
                                              SOW No. XXX  - Ambient Air
       deviation shall be established by initially analysing/the ICS at  least
       five times repetitively for each analyte.
                                                               analyzed by ICP
                                                              ined by
                                                                   '  for  the
   If true  values  for analytes contained in th
are not supplied with the ICS, the mean shal
initially analyzing the ICS at least five t
particular analytes.  This mean determination  hall
analytical run where the results for the
met all contract specifications.  Additi
initial mean determination is to be use
lifetime of that solution (i.e., until/ the' solution is exhausted).
      4.3.7.9.4  Calculations
                    % Recovery =
                                                                          an
      where:
              Standard deviation: and
               x    — mean

      4.3.7.9.5  Techni
                                                           Eq. D/IN-9
                                                                 Eq. D/IN-10
          Recovery fo
       (i.e.,  80-120/

      4.3.7.9.6  Co

          If the ICS
       criteria
       instr
       analy
          The
                                 witnfra ± 20 percent of the true value
                            s not meet the technical acceptance
                              \s, correct the problem, recalibrate the
                                  ,  and reanalyze all of the
                                  the last compliant ICS.
                                  .centration (/tg/L) ,  true concentration
                                  :ean and standard deviation on FORM V-AAIN.
                         deviation shall be reported in the raw data.
July, 1991
                                                           Page D-23/IN
-------
Exhibit D
                                                 SOW NoCxXXX -  Ambient Air
4.3.7.10
                 Spike Sample Analysis
4.3.7.10.1   Summary

    To provide  information about the effect o
 digestion, a known amount of analyte is add

4.3.7.10.2   Frequency

    At least one spike sample analysis
 of samples for each SDG.  EPA may reqt,
 analysis upon special request by the.
 Contractor will be paid.

    If two analytical methods are usec
 the same analyte within a SDG  (i.e., 1C!
 shall be run by each method used.
                                                          ormed
      4.3.7.10.3
               Procedure
     The  spike  is  added befor
   microwave digestion).

     Samples  identified as  field
   analysis.  EPA may require that a
   spike sample analysis.   In the
   spike sample per SDC
   contract criteria,/flag_all
   method in the SDC

  4.3.7.10.4
                                                           on each group
                                                        spike sample
                                                         for  which the
                                                           reported values for
                                                        ),  then spike samples
                                                             . e. ,  prior to the
                                                    be used for spiked sample
                                                  sample be used for the
                                                here  there is more than one
                                                 recovery is not within
                                                   he same matrix, level, and
                                                                 Eq. D/IN-11
                                                 100
        pe
        sample
        of  the du
        percent reco
                            is\ performed on the  same sample  that is chosen
                             rialysis, spike calculations shall be
                           ilt$ of the sample designated as the "original
                               Duplicate Sample Analysis).   The average
                         Its/cannot be used for the purpose of determining
 July,  1991
                                                              Page D-24/IN
-------
Exhibit D
                                                SOW No.  XXX -  Ambienc Air
          When the sample concentration is less than the  instrument detection
       limit, use SR = 0 only  for  purposes of calculating percent recovery.

      4.3.7.10.5  Technical Acceptance Criteria

          Recovery for the spike should be within ±
       amount (i.e., 75-125 percent).

      4.3.7.10.6  Corrective Action

          If the spike recovery is not within/^he/limits  of 75-125 percent,
       the data of all samples received associated with/€hat  spike sample and
       determined by the same  analytical me/hooY shall  bfe  flagged with the
       letter "N" on FORMs I-AAIN  and VI-AAIN,

          An exception to this rule is grarited iri^&ytua^ions where the sample
       concentration exceeds the spike concen£r?ation b^f a factor of  four or
       more.  In such an event, the data shall beN^por^eHi unflagged  even if
       the percent recovery does not meet the 75-125fs.ercentxrecovery
       criteria.

      4.3.7.10.7  Documentation
          Report the spiked sample results, sample/ result^ spike added and
       percent recovery for the spike aamp\e Analysis  on  FORM VI-AAIN.
       The units for reporting spike sample re<

    4.3.7.11     Analytical SpJ.ke Sample Analysis'

      4. 3 . 7 .11.1  Sunm
                                         ults will be  in A«g/L-

                                             !ethod of Standard Additions
    To provide /information
 measurement sys tern and
 interference^^fect^v. tfte
 utilized.

4.3.7.11.2
                                 kbovit the\^ffeoft of the sample matrix on the
                                 ensure against bias resulting  from
                                 ^ethod of Standard Additions (MSA)  is
          At Zeas/fc-"one~-spike "Sample a"hlyte withi/ a/SDG (i.e.,  ICP and  GFAA),  then spike samples
       shall be^cun bjNeach .metbtod used.  The  frequency  of MSA will  depend  of
       the recover^-Qf thexyana/ytical  spike.
July, 1991
                                                             Page D-25/IN
-------
Exhibit D
                                              SOW No/rvXXX - Ambient Air
      4.3.7.11.3  Procedure

          The analytical spike sample analysis shall b
       containing measurable amounts of the analytes.
                                                      rmed on a sample
          The spike is added after the sample prepa,
       analysis.

          Samples identified as field blanks capriotybe used for spiked s<
       analysis.
          EPA may require that a specific sa
       analysis.
          The analyte spike shall be spiked
       percent of the analyte's  linear range.
       The sample and spiked sample shall be at  the  s
   In the  instance  where  the
per SDG and one spike sampl
flag all the samples of the s
and run the MSA series.

   The sample and three spikes  shal
quantitation (the "initial" spike
from use in the MSA

   MSA spikes sha

a) Spike 1 is
b) Spike 2 is
c) Spike 3 i
                                                      the spike sample


                                                  tration equal to 30
                                                        on.
                 = Spiked Sampld Reteult;
                 = Sample Result): and
                   Spike Added.
       4.3.7.11.4  Calcut
                                                   one spike Sample per method
                                                              ntract  criteria,
                                                             'ethod in the  SDG
                                                 alyzed consecutively for MSA
                                                a  is  specifically excluded
                                                  .the  linear  range  in
                                                  the  linear  range  in
                                                  the  linear  range  in
                                                                  Eq.  D/IN-12
                                                x 100
           If  the^soike ^^analys/is  is  performed on the  same  sample that is chosen
        for the duplicate sample'analysis,  spike calculations shall be
        performed usingtfee results of the sample designated as the "original
 July. 1991
                                                            Page D-26/IN
-------
Exhibit D
                                                 SOW No. XXX - Ambient Air
       sample"  (see part 4.3.7.12, Duplicate Sample Analysisy.  The average
       of the duplicate results cannot be used for the pjarpc/se of determining
       percent  recovery.
          When sample concentration is less than the
       purposes of calculating percent recovery.
      4.3.7.11.5  Technical Acceptance Criteria

          Recovery for the analytical spike shcy
       the spiked amount  (i.e., 85-115 percen^

      4.3.7.11.6  Corrective Action
                                                               0  only for
                                         /or
thin
                                            lall
                                                    ierl
                                                the P£
     If  the  spike  recovery  is not  at
   percent,  a second analytical  spike
   analytical spike is out of control,  tlv
   same spiking solution.   If spiking  the PB
   out  of control,  the spiking solution shall be
   previous  spiking procedure repeated.   If not, the"
   received  associated with th,
   analytical method with the
                                                  and dete
                                 ORM VII-AA

                                  analytical
     imits of 85-115
    rmed.   If the  second
    is  spiked with  the
       recovery  that  is
         :ed and the
           all  samples
          .ed by the  same
       IN and VII-AAIN.
                                                          flat
  4.3.7.11.7   Documentation

     Report the spiked sample resu£
   percent recovery (positive,
   spike  sample  analysi
     The units for /ep
   Mg/L.

4.3.7.12     Dup

 4.3.7.12.1   S'

     Duplicate aliquo
   and  analys
   analyti
                                                 e results,  spike  added and
                                                zero) for the analytical
ample results will be in
      4.3.7
                                  iample are  carried through the preparation
                                          nation about the precision of the
                                         ix effects.
July, 1991
                                  ample analysis shall be performed on each
                                  DG.  EPA may require additional duplicate
                       upon spfeclal request by the Project Officer, for which
                      will be/pa/d.
                                                              Page D-27/IN
-------
Exhibit D
                                                      SOW MtfXXXX
    If two analytical methods are used to obtain
 the same  a'nalyte within  a  SDG  (i.e.,  ICP and
 samples shall be run by  each method used.

4.3.7.12.3  Procedure

    Samples identified as field blanks
 sample analysis.

    EPA may require that a specific samp
 sample analysis.

    In the  instance where there  is more.
 SDG and one duplicate result is nc
 the samples of the SDG.

    Duplicate  sample analyses are required
 percent difference.

4.3.7.12.4  Calculations
                                                           reported values for
                                                           'then duplicate
          where:
            RPD
              S
              D

       Duplicates c_
                   i
      4.3.7.12.5  Tec1

          A  control limit  oJ
       and d
       (Exhibj
       valuer le-s's than"
                                                          :or the duplicate
                                                          licate sample per
                                                           criteria, flag all
                                                            tions of relative
                                                                 Eq. D/IN-13
                         limt
                                              and
                                         ing on FORM I-AAIN.
  cent for  RPD shall  be  used for original
greyer than or equal to five times CRQL
     ± CRQL shall be used for sample
                        imes CRQc.
                                  he  five  times  CRQL level  and the other is
                                  ria.

                                afe  less  than the  IDL,  the  RPD is  not
       calcu
July, 1991
                                                             Page D-28/IN
-------
Exhibit D
                                                     _SOW No.  XXX,-  Ambient Air
          Specific control limits for each analyte will be
       AAIN at a'later  date, based  on precision  results.,

      4.3.7.12.6  Corrective Action

          If the duplicate sample results are outsit
       with an asterisk all the  data for  samples  re'ce:
       that duplicate sample.

      4.3.7.12.7  Documentation

          The  results in jig/L of the duplicates
       reported on FORM VIII-AAIN.

          The  absolute value of the contr
       the "CONTROL LIMIT" column on FORM

     4.3.7.13     Laboratory Control Samples

      4.3.7.13.1  Summary

          A laboratory control  sample
       against analyte  loss in the
                             ed to FORM IX-
                                  iraits, flag
                                    with
                        shall be entered in
                           analyzes to ensure
      4.3 .7.13.2  Frequency

         One LCS shall be prepared and an
       a SDG, or for each ba£eh-of samples,

      4.3.7.13.3  Proced/re

         A LCS  shall
       preparations,
       EPA samples
                for every group of samples in
                ,ever is more frequent.
                e  using the  same  sample
                 procedures employed for the
          The LCS solut
       EPA Quality Assuraiv
       be used.)

      4.3.7.12^
se  obtained from EPA.   (If unavailable,  other
 ^samples or other certified materials may
                               _\Found Concentration
                                  True Concentration
                    x 100
Eq. D/IN-14
July, 1991
                                 Page D-29/IN
-------
Exhibit D
                                                      SOW
                                                              Ambient Ai:
      4.3.7.13.5  Technical Acceptance Criteria

          Recovery for the LCS shall be within ± 20 pe^entS^ the true value
       (i.e.,  80-120 percent), with the exception of
                                                       Sb:
      4.3.7.13.6  Corrective Action
          If  the  percent  recovery for the LCS falls ^outside the technic
       acceptance criteria, then the analyses stiall/be  terminated,  the
       problem corrected, and the samples asso/iaKed with,^that LCS  reprepared
       and reanalyzed.

      4.3.7.13.7   Documentation
         Report  the  LCS  found concentration
            ,  and percent recovery on FORM IX-AA^

    4.3.7.14     Instrument Detection Limits

      4.3.7.14.1   Summary

         Prior to sample analysis,  t
      be  determined for  each instrume

      4.3.7.14.2   Frequency
                                                    concentration  (in
                       det
    IDLs  shall  be
 and at least quart
 the contract.

4.3.7.14.3  Proc,

    IDLs  (in
 t 99) by the
 consecutive analys
 shall be performed as
 (i.e. ,  eaph"~meastn?€ment nv
                                                       limit (IDL) shall
                                                  ,pf the start of the contract
                                                    months) until the end of
                                    termined by multiplying 3.707 (Student
                                   .on for each analyte obtained  from  the
                                  ;en different PB extracts.  Each measurement
                                       were a separate analytical sample
                                         llowed by a rinse and/or any other
       procedure normally p^r-formedT'betw^en the analysis of separate
       sampled) ./IDLs shaJJ be\determihed and reported for each wavelength
       used/in /he analysis i*f the samples.
          Che/quarterly  determined \IDL for an instrument shall always be used
          the^-LDL for that insttumint during that quarter.  If the instrument
       is Adjustiettvin anyway tttat Lay affect the IDL, the IDL for that
       instrument shail  be re
-------
Exhibit D
                        SOW No.  XXX -  Ambient Air
      4.3.7.14.4  Calculations

                               IDL = 3.707 x on_ j



      4.3.7.14.5  Technical Acceptance Criteria

          The IDLs shall be < the CRQLs in Exhibi

      4.3.7.14.6  Corrective Action
                                    Eq.  D/IN-15
                                         so;
                              lyte, that
                              lyte concentration
                             IDL.
     If an instrument's  IDL  exceeds  the
   instrument cannot be used in this
   is  greater than or equal to two ti

  4.3.7.14.7   Documentation

     IDLs shall be  submitted with each data
   XI-AAIN for each instrument used.   If multiple
   for  the analysis of an analy/te^within a SDG,  the'
   analyte shall be used for

4.3.7.15     Interelement Corre*

  4. 3 . 7 .15.1   Summary

     To ensure against  spectral  interferences,  interelement  correction
   factors are determined—f-er all waverengtl^s used for each analyte
   reported by ICP.
                                                          ,nd reported on FORM
                                                             ients are used
                                                                IDL for  the
                                                              s for that SDG.
       4.3.7.15.2  Fre

          Before any
       interelement/co
       months prior
       thereafter
                  under this contract, the ICP
                   determined within three
       contract analyses and at  least annually
       the
 sr spectral interference due to Al, Ca, Fe, K,
   nined for all  ICP instruments  at all
ich\analyte reported by  ICP.  Correction factors
    iue to analytes  other  than  Al,  Ca,  Fe,  K,
 irtad if they were  applied.

    ijusted in any way that may affect  the  ICP
  factors,  the factors shall  be redetermined and
 ir use.
July, 1991
                                     Page D-31/IN
-------
Exhibit D
                                                      SOW
                                                                    Ambient Air
          Follow the instrument manufacturer's recommendations for applying
       interelemenf correction factors.

       4.3.7.15.4   Calculations

          Not applicable

       4.3.7.15.5  Technical Acceptance Criteria/

          Not applicable

       4.3.7.15.6  Corrective Action

          Not applicable

       4.3.7.15.7  Documentation
                                                               ition shall be
          Results from interelement correction factors
       reported  on FORM XI-AAIN  for/*U__ICJ> parameters.

4.3.8. Instrument Operation

    4.3.8.1  No  detailed  operating instruction/ a/ to  the~~optimization of the
    plasma power,  argon  flows,  torch an>i co\l/corifiguration,  etc.  will be
    given.   The  analyst  should follow the\ instractions provided by the
    manufacturer of  the  particular instrument.
    4.3.8.2  The sample
    The use of a perist
    A tip washer is a
    sample flow syste
    line just before
    runs to the neb
    third is connect^
    the carrier flow is
    carrier argon  flow
    the salt buL3rdnp~a

    4.3.8.3 /Ch
    characteristics
    concro/ile
                         introductions system is\to ""be  of a pneumatic  type.
                        pltijC pumpXinstf-ad of dv&ecz aspiration is required.
                            useful jaid and ean be Vasily inserted into the
                                                  r" on the carrier argon flow
                                                 .e arm of the "tee connector"
                                    'to the carrier argon flow line and the
                                   rom the peristaltic pump.   When a drop in
                                   a small pulse of water is  pumped into the
                        and Si^wn through the nebulizer orifice,  dissolving
                          resorting the\qriginal carrier argon flow.
 entering ttye nemilizei
lize
      ?erved<
         awn
                             caXrier  argon flow may change the  emission
                              aly\te.   The use of a digital mass flow
                               to Control the carrier argon flow.
    4.343.4  "For direct reading instruments,  every  solution, including
    calibration standards,  cal/ibr/ation and method blanks,  reference  samples,
    and sampie-s shaTi^be  anaWzaa  using two full  exposures (peak  scan) ,  each
    of which  is sufficient  zo  meet the instrument detection limit (at  each
    analyte  emissionXUne):  All exposure  times shall  be  the same for  all
    analyses  and all  quarterly analyses (i.e.,  method  detection limit  and
July, 1991
                                                                   Page  D-32/IN
-------
Exhibit D
                                                      SOW No.  XXX -  Ambient Air
    „interelement correction factor.)  Each background spe/tral region shall
     have an exposure time equivalent to a full exposure jc.im? for direct
     reading instruments.

     4.3.8.5  Selection of the  appropriate backgroundyfepectralxregion for each
     analyte shall account for  the major interferents/wi^fcic thaKregion and
     for the possibility of analyte line broadening/at/nigh concentrations
      4.3.8.5.1   One of the best ways to select
      spectral region is to perform a wavelengt;
      wavelengths in the presence of metals
      levels in the samples.  Alternately, ifth^ instr
      automatic scanning capability, selection of the bXck
      region will have to be determined on/the/basis o,
      experience.
                      appropriate background
                    4n around the analyt^
                    .tly encountered at high
                              does not have
                            ground spectral
                           'nual scans and
      4.3.8.5.2   It is possible, if the backg1
      too close to the analyte line, to observe
      or other erroneous net intensity readings
      error, it is required, at a minimum, that
      concentrations be derived fr
      addition, the equivalent cortcen
      background correction wavelen
      uncorrected intensity data for
      correction wavelengths shall be
      data prior to submission to assureXtha^
      this type of error.

     4.3.8.6  A calibratio
     be  sufficient to pr
                jund coi
                    ler
         rection wavelength is
            .et intensity of zero
               ircumventing this
  uncorrecbcd analyte
tted raw data>^ckage.  In
           .etermined at the
              inally, all
             background
     e analyst shall review this
   orted values do not reflect
                     sample aspiration should
                    iples.
    4.3.8.7  The determination of/the linear^-canee of each analyte line,
    interference effects/ and an/ typeorsxietec~eion  limit or precision
    measurement shal:l b^establfshed under thVsame  conditions used  for  the
    analysis of the^ample^. including the background correction  scheme,

4.3.9 Procedure
    4.3.9.1
      4.3.9.
      instrumen
s^rument with proper  operating parameters.   The
   to become thermally stable before beginning
  \least  30 minutes  of operation with the
  jions.

  iate operating  configuration of the
July, 1991
                                   Page D-33/IN
-------
Exhibit D
                                                      SOU NoyTSQCX  - Ambient Air
      4.3.9.1.3   Perform the appropriate steps recommended Ky the
      manufacturer to align the exit slits with the entrance slit.  These
      steps are commonly called the profile or wavelength calibration
      procedure.
4.3.9.2  Analysis Sequence

  4.3.9.2.1   Before  beginning the sample
  initial calibration blank (ICB), initial
  (ICV),  interference check sample, two t
  the  linear range standard (LRS).  The
  values  shall not deviate from the act
  The  calibration blank values may not
  check sample found  values shall not
  the  true values. If these conditions
  discontinue the analysis and refer to
                                              an
      Initial and Continuing Calibration Blanks) an
      information.
4.3.9.2.2   Upon successful analysis o
analyze all PB extract(s) preoar
blank(s) values are not less tftan ^r equa
and E for the appropriate action
                                            ys/.s run, analyze
                                               ration verifications
                                                     standard  (CRI)  and
                                                        concentration
                                                      e than 10  percent.
                                                        The  interference
                                                     than 20 percent  of
                                          notTNhet/for any analyte,
                                                   uality Control  -
                                          the sample
                                             to/-eha. CR
                                                        dditional
                                                            CRI, LRS, and ICS,
                                                             f. any of the
                                                              see Exhibits D
      4.3.9.2.3   If the PB and LCS values\are wdthin the acceptable ranges,
      analyze the spike sample and the analy^isxspike sample.  If the recovery
      of any analyte deviaterg^Tromxthe acceptable\ranges, see Exhibit E for
      the appropriate actibn.^_£rpcefed to the analysis of samples if the
      recoveries are acceptable or\ af|t£i-_consultinR/Exhibits D and E.
                       oncinuing c,ali
                     calibration Sola
                         of
                           lysej
  4.3.9.2.4   The
  the  continuing
  analytical s
  after the ana
  wash or other clearf
  deviate from the actua
  the  absolupe-^aTCce-s^for
  conditions are .not
  the  anaiysvsands&e^ Exh
                                  (CCF)
                  ication standard  (ICV)  and
                  . be analyzed after every 10
       analyst "shall run CCV and CCB samples
   vious sample,  but prior to use of a tip
  ce.   CCV concentration values shall not
        more than 10 percent.  In addition,
  CCB  Shall be lower than the CRQLs.  If these
          uring samples analysis, discontinue
its D  aWa E for the appropriate action.
    4.3.9.3
      4.3.9.3.1
                                ttte sample analysis run, analyze the ICS, CRI,
                            the\ values for any of these samples deviates  from
                                •xhibits D and E for additional information.
                           tracts shall first be analyzed without any
July, 1991
                                                              Page D-34/IN
-------
Exhibit D
                                                 SOW No. XXX - Ambient Air
      dilution.  Diluting sample extracts  is permissible  iff  necessary,
      provided that the dilution does not  produce  result/ bedow CRQL.

      4.3.9.3.2   All concentrations within the linear/rarige of  the analyte
      shall be reported.  All concentrations reported/shall  DB^obtained within
      the established linear range for  that analysis/ruiV^and  interference
      corrections shall be made based on the actual; concentratjipn  ofx^he
      interferent and not the apparent  concentrat&m /obtained  wheTk. the
      interferent concentration is above the lin^ars range.

    4.3.9.4  Method of Standard Additions
  4.3.9.4.1   To  the  first  aliquot  add ah a£propric
  spiking  standard reagent  blank solution ./mix, ar
                                                           /olume of the
                                                           ilyze.
      4.3.9.4.2   Add appropriate volumes M^the "fep^kin^ standard to the
      remaining three aliquots that result in'&oncentr^tions  at  20  percent,  40
      percent and 60 percent of the instrument's^inearrange.   The spiking
      standard solution volume added to each aliquot*shall rteit exceed  10
      percent of the volume of the aliquot.  Add the appropriate amount of
      blank solution to each aliqupt to~~ffiafce—ttie^total of spike  plus blank
      volumes added equal.

      4.3.9.4.3   Using a calculator^ a\stati£tL6al~paCteage on a  computer,
      determine the slope, the intercepts\f tfhe/ordinate (y-axis)  and the
      abscissa (x-axis), and the correla^ion^cofiffficient using the  found
      concentration as the ordinate and trie st/ndard addition concentration  as
      the abscissa.  The abs^-ttrts^value of she intercept of the  abscissa  is
      the concentration o? the analyte in the\dilVce solution.   If  the
                                 jss\than 0.99!
  correction  coeffic/en
  repeated.   If  the/second ana
  0.995,  then repe4t  ifhe  analysis
  digest.   Be cer/tain to  correct,
  using  a smaller  sample  digest
  is  still less

4.3.9.5  Calculations
              tr^en the analyses shall be
                 coefficient is less than
              Her aliquot of the sample
             ference in volume created by
 aliquot.^^f the correlation coefficient
g the sample data with a "+".
                            the analyte^ir concentration (in Mg/m3), multiply
                                 anaiyt^ values  (in Mg/D by nine  times  the
                                ,ers) used  in the extraction and  divide by  the
                                  3) sampled and the number of l"x 8" strips
                                  .e factor  "9" represents the total  area (63
                                  Ixposed to the  air stream divided by the
                                  l"x 8" strip.
July, 1991
                                                              Page D-35/IN
-------
Exhibit D
                                                      SOW N(/NZXX  - Ambient-
             Analyte Cone.
              air, \ig/m2
                            9 x
                                Interference-Corrected
                                  Analyte Value.
                                  no. of
                              strips digested
                       abs
                       Volume, L Eq. D/IN-16
                                                               to  extract  the
                                                             r,  for subsequent
    4.4.3.3  Hot place

    4.4.3.4  Centrifu_
    (International Equip
    4.4.3.5  Cen.
    polypropy
    4.3.9.6  Documentation

      4.3.9.6.1  .Report the air concentration
      interference-corrected analyte value in

4.4 ALTERNATE  SAMPLE  PREPARATION  FOR GFAA

4.4.1 Introduction

    4.4.1.1  This method describes a hot  extract
    inorganics from the particulate  loaded glass-:__
    analysis by graphite furnace  atomic absorption

4.4.2 Summary of Method
    4.4.2.1  The inorganics are extrXcte
    After cooling to room temperature \th

4.4.3 Apparatus and Materials

    4.4.3.1  Graphite furn

    4.4.3.2  Volumetric ^la^sware^
    Borosilicate).
                                                         	   from  the  filter.
                                                    is  allowed to  settle.
                                                  ectrometer  (GFAA).

                                                   Opacity  (Class A
                          .bes:
f
}f maintaining speeds  of 2000  rpm
   Model UV or equivalent).

       lene tube  with  screw  tops of
    4.4.37
    fiber  fif
                       Automat icXdispens ing with an accuracy of 0.1 mL or
                                    ~,  (Grumman Automatic  Dispensing  Pipet,
                                   worn while cutting and handling  glass-
July, 1991
                                                                  Page D-36/IN
-------
 Exhibit  D
                                                     _SOW No.  XXX - Ambient Air
    .4.4.3.8  Template:    To  aid in sectioning the  glass-flbei? filter.
     Federal Register 1978,  43 (Oct.  5),  46258-46261.   See Figure D/IN-1.

     4.4.3.9  Pizza  cutter:   Thin wheel  (<  1 mm).

4.4.4 Reagents

     4.4.4.1  Nitric Acid  (HN03):  Concentrated, 1
     spectrographic  grade.

     4.4.4.1.1   Nitric Acid, 3M:  Prepare by
     nitric  acid (4.4.4.1)  to distilled,  deiq
     to  1  L.

     NOTE:   Nitric acid  fumes are toxic.
     hood.   Stir slowly.

     4.4.4.2   ASTM Type  II Water  (ASTM D1193):

4.4.5 Sample Preservation and Handling

     4.4.5.1   Exposed Hi-Vol  filters
     material  inward, enclosed in p
     30°C  until  analysis.

4.4.6 Hot Extraction Procedure

     4.4.6.1  Cut a  1" x 8'
     for Lead  (see Figure
                                                 tng 192 mL of concentrated
                                                             slowly diluting
                                                         11-ventilated fume
     4.4.6.2  Fold the /tri
     15  mL of 3 M HN03
     a watch glass,  ylt ps  impor
     corrosion prod
     are not deposi
    NOTE:  Ic  is s'uggested
    ensure  adequate—stolume fo

    4.4.6.3
    hood  f

    NOTE;
                                                           be  monitored.
                                                         ialf with  particulate
                                                        and/stored  at 15 to
                                                 the Federal Reference Method
    to
    distilled,
                                                     in a 150-mL beaker.  Add
                                                 iple.  Cover the beaker with
                                                sample covered so  that
                                               face which may contain lead)


                                    than one strip per filter be extracted to
                                      ,and QC analysis.
                              jample rn^ beaker on a hot plate under a fume
                               ,t let the sample evaporate to dryness.

                                 toxic.

                                  love the beaker from the hot plate, and cool
                                 nse watch glass and sides of beaker with
July, 1991
                                                                  Page D-37/IN
-------
Exhibit D
                SOW. NcvT^XXX -  Ambient Air
    A.4.6.5  Decant extract  and  rinsing  into  a 100-mL vo
    distilled,  deiohized water to the 40-mL mark on bearer
    glass  and set  aside  for  a minimum of 30 minutes.
    and cannot  be  omitted since  it allows the HN03  t
    diffuse  into the  rinse water.
                        ric flask.  Add
                       cover with watch
                         a critical step
                             filter to
    4.4.6.6  Decant the water from  the  filter  int>
    rinse  filter  and beaker twice with  distillec
    rinsing  to volumetric  flask until total vojXime/is 80 to 85 mL.

    4.4.6.7  Stopper flask  and  shake  vigorou
    approximately five minutes  or until foa.
    4.4.6.8  Bring solution  to volume  wit
    mix  thoroughly.  Allow solution to sett
    with analysis.
    NOTE:  Do not  filter  the  extracted sample to removfexpartitulate matter
    because of  loss  of  lead due  to filtration.   The f inal^s^tr/ct can be
    centrifuged at 2000 RPM for  30/minutesto~Teaoxe__any suspended solids.
                   ionized water, and
                  /our before proceeding
    4.4.6.9      If sample is to be
    to a polyethylene bottle, being c
    solids.
                      alysis,  transfer
                      the settled
               acted and analyzed,  and
             evels of metals in the
     4.4.6.10     Samples prepared by hot exXracs.ion procedure are now in 0.45
     M HN04.
     4.4.6.11     Blank
     digestion blanks  s
     reagents  used.
4.5  SAMPLE ANALYSIS
4.5.1 Introduction
.CE ATOMIC ABSORPTION (GFAA)
     4.5.1.1  GFAA-~analysis proceNiiures "asce provided to achieve lower detection
     limits (where reguired)^for the^analysis of inorganic analytes listed in
     Table 1 a^d/^ieTarg>C Ana^yte List/in Exhibit C.

     4.5.1..2  Because of the differences among various makes and models of
     satisfactory instruments, mo detailed instrument operating instructions
     can foe prodded.  Instead, (thai analyst is referred to the instructions
     provided by tke manufactuiyer pf that instrument.
 July,  1991
                             Page D-38/IN
-------
Exhibit D
                                                      SOW No. XXX - Ambient Air
                                                            :h an atomic
                                                            of a sample is
                                                                 .ess, charred,
                                                                   d through
                                                                       nsity
                                                                           the
                                                                        are';
4.5t2 Summary of Method

     4.5.2.1  Using  the furnace  technique  in conjunctio
     absorption  spectrophotometer,  a representative al
     placed in a graphite  tube in the furnace,  evapor,
     and  atomized.   Radiation from a given excited e,
     the  vapor containing  ground state atoms of th
     of the transmitted radiation decreases in projx^r/tion
     ground state  element  in the vapor.  The met.
     placed in the beam of radiation by increasing/che temperature of
     furnace  thereby causing the injected  specimen'to be volatilized.
     monochromator isolates  the  characteristic  rafdiation/ftom the hollow
     cathode  lamp  and a photosensitive devic/ me4sures #he /attenuated
     transmitted radiation.

4.5.3 Interferences

     4.5.3.1  The composition  of  the  sample  matrixNxan haVea major effect on
     the  analysis.   By modifying the  sample matrix,  etfcher tbxremove
     interferences or to stabilize  tfteanalyte,  interferences ^kn be
     minimized.  Examples  are  the aaditiorTTrf-^nimonium nitrate to remove
     alkali chlorides and  the  addic^ont^of^ammoniumpRospbate^ to retain
     cadmium.
     4.5.3.2  Gases generated  in  the  furnac\  dri
     molecular  absorption bands encompassing
     Therefore  the use  of background  corre6iorvis
     analysis.
                                                   atomization  may  have
                                                 analytical wavelength.
                                                   required for  all  furnace
    4.5.3.3  Continuum
    background interference'.  Whei
    compensated for, (Zhoose an alj
    analyte from the/intzerferantx
    correction (e.
                                     rection c^mo^  correct  for all types  of
                                            rourtd/interference cannot be
                                                  th, chemically separate the
                                                 rnate form of background
                                                ion).
    4.5.3.4  Interferenfc^s from ^ smoke producing  sample  matrix can sometimes
    be  reduced by extending^he charring  time  at a higher temperature or
    utilizing anasfeiag^cycle^bn^ the^esence  of air.   Care must be taken to
    prevent  loXs of  analyst

4.5.4 Apparatus

    4.5.4/1  /Atomic  absorptionX spfectrophotometer:   Single or dual channel,
    single d-i^double beam  instrument  having a  grating  monochromator,
    photomultipper  detector, /adjustable  slits,  a  wavelength range of 190- to
    800-nm,xfeackgrbu^d  correc/tio^i,  and provisions  for  interfacing with a
    recording device.
July, 1991
                                                                  Page D-39/IN
-------
Exhibit D
                                                     SOW No/^-XXX - Ambient Air
    .4.5.4.2  Graphite furnace:  Any furnace device capable
    specified  temperatures Is satisfactory.
     4.5.4.3  Operational Requirements.  Because of t.
     various makes  and models  of  satisfactory instr
     operating  instructions  can be  provided.   Inste
     follow the  instructions provided by the  manuf,
     instrument.  Sensitivity,  instrument  detection
     dynamic range  and interference effects mus
     established for  each individual analyte  o
     It  is the  responsibility  of  the analyst
     configuration  and operating  conditions
     requirements set forth  in this SOW and/to
     confirming  instrument performance and^analy
                                                               reaching  the
                                                'be
                                                                   between
investigated and
 particular instrument.
         he instrument
         analytical
       lity control data
      Its.
                                               verify that
                                            /sed/satisfy
                                               aintair/ q
4.5.5 Reagents and Standards
    4.5.5.1  Matrix matching with the samples is mandatt
    standards,  and quality  control  s^m^les^  to  avoid  inacci
    values due  to  possible  standarc
                                                                   blanks,
                                                                concentration
                                    curve
    4.5.5.2  Calibration standards ar« prepared tty diluting/stock metal
    solutions  at  the  time  of  analysis amd^are  discarded after use.   Prepare
    at  least three  calibration  standards^in^ctfaduated amounts in the
    appropriate range by combining an appKoprialze volume of stock solution in
    a volumetric  flask.  The  calibration  st^nda^ds must be prepared  using the
    same  type  of  acid or confbinattiap of acids\at^he same concentration.
    4.5.5.3  Two types o,
    calibration blank
    preparation blank
    from various aci
                    (
4.5.6 Quality Control

    4.5.6.1  Instrument Call
      4.5.6.1
                                              fo\ GJfAA analysis; the
                                              the^analytical  curve while  the
                                                  ible contamination  resulting
                                                 sing.
                   to  the anaiysik of samples and required QC, each GFAA
                 shall be initially calibrated to determine instrument
              itivity.
      4.5.

             \_^\
             Instruments  stoaLi be7 calibrated  daily or once every  24 hours  and
       each  time  the >nstrumenjz  is set up.
July,  1991
                                                                  Page D-40/IN
-------
Exhibit D
                                                     SOW,No. XXX - Ambient Air
4.5.6.1.3  Procedure

      Calibration standards  shall be prepared
 solutions at the time of analysis, and are dis
          Calibration standards shall be prepared
       or combination of acids, and at the same
       in the samples following sample preparati
                                                           iting the stock
                                                          id after use.
          The instrument shall be calibrated
       manufacturer's recommended procedures
       Beginning with the calibration blank
       standard, run at least three standa
       shall be a blank, and another shal

          Baseline  correction is acceptab
       each and every sample, or after the
    Resloping is  acceptable as long as it is
 immediately followed by a CCV and CCB.

4.5.6.1.4  Calculations

    Not  applicable.

4.5.6.1.5  Technical Acceptance

    Not  applicable.

4.5.6.1.6  Correc

    Not  applica

4.5.6.1.7  Do/um
                                                                of acid
                                                              1 result
                                         :or/ling to instrument
                                             at least four standards.
                                                   Awards the highest
                                                     ition standard
                                                    is performed after
                                                  respectively.
                                                               preceded and
          The  instrume
       the raw data.   Con
                          tization date  and time  shall be  included  in
                               shall be in
                                        at ion
                                 'AA system has  been calibrated,  the  accuracy
                                  shall be verified and documented for every
                                  EPA Initial Calibration Verification
                                  wavelength used for analysis.
July, 1991
                                                            Page D-41/IN
-------
Exhibit D
                                                      SOW No^XXX -  Ambient: Air
      4.5.6.2.2  Frequency

          Each time the instrument is calibrated,  the
       immediately following the calibration and befo
       analyzed.

      4.5.6.2.3  Procedure
                                         indei
    If the ICV solution(s) are not availat
 certified solution of an analyte is not/avc
 analyses shall be conducted on an ii
 concentration other than that used
 within the linear range.  An indepei
 standard composed of the analytes
 used in the standards for the instrv.

4.5.6.2.4  Calculations
              % Recovery =
                                                          be run
                                                           les  are
      4.5.6.2.5  Technical Acceptance Criteria

          Recovery for the ICV shall be within i( 10 percent of the true value
       (i.e.,  90-110 percent
EPA,
  from  any source,
    sd  at  a
    Libration,  but
  '/s  defined as a
   source  than those
fion.
                                                                  Eq.  D/IN-17
4.5.6.2.6  Corrective

    When recovery
 the analysis s
 instrument reycali'

4.5.6.2.7  Documenba£ion

    Report
                                                  chnical acceptance criteria,
                                                 lem corrected,  the
                                                ion reverified.
                                             (in Mg/L),  true concentration(  in
                                           II-AAIN.
                             ;pvery

                                 Lon Verification
                    calibration/accuracy during an analysis run, a continuing
       calibration/"Verification solution  (CCV)  is analyzed  and  reported for
       every wavfeiengtn^-^used/for/the analysis of each  analyte.
July, 1991
                                                             Page D-42/IN
-------
Exhibit D
                                                SOW No.  XXX - Ambient Air
      4.5.6.3.2  Frequency

          The CCV is run at a frequency of 10 percent 017 every  two  hours
       during an analysis run, whichever  is  more freqt
          The CCV is also run after the last analytical
       run.
                                                            the  analysis
                                                   oncentration  at  or  near the
                                                          is runs  for  a Case
4.5.6.3.3  Procedure

    The CCV shall contain the analytes a
 mid-range of the calibration curve.

    The same CCV shall be used throu.
 of samples received.
    If the  ICV solution(s) are not available froitf EPA, or where a
 certified solution of an analyte  is not  avat b\  applied to  the CCV to a
                                 ttent applied  co  tne associated analytical
                                               in\£ime  between  a CCV analysis
                                               s  well  as  the difference  in
                                                -ample  immediately preceding
                     the ]/oweiSt difference in time between  any  two
                             Les associated with the CCV.
                                  founc
                                  oncentration
                                  T5*«e Concentration
                                                     x. 100
                                                           Eq.  D/IN-18
      4.5/6.3/5  Technical Accentcince Criteria

                   for the CCV/sha/Ll be within ± 15 percent of the true value
                     percent)
July, 1991
                                                             Page  D-43/IN
-------
Exhibit D
                                                  SOW No/^KXX -  Ambient Air
                                                               tance criteria,
                                                                  instrument
•  4.5.6.3.6 .Corrective Action

      When recoveries of the CCV exceed the techni
   the analysis shall be stopped, the problem co
   recalibrated, the calibration reverified, an
   analytical samples reanalyzed (or all analytic
   last compliant CCV analyzed).

  4.5.6.3.7  Documentation

      Report the CCV found concentration
   Mg/L),  and percent recovery on FORM

4.5.6.4  CRQL Standard

  4.5.6.4.1  Summary

      To verify linearity near the  CRQL, the Contrac-fc
-------
Exhibit D
                                                 SOW No. XXX - Ambient! Air
                                                             Mg/L),  true
                                                             III-AAIN.
  4.5.6.4.7   Documentation

     Report  the CRQL  standard's  found  concentration
   concentration (in Mg/D.  and percent recovery

4.5.6.5  Initial Calibration Blank

  4.5.6.5.1   Summary
          To verify  that the GFAA system is not/cor
       calibration blank (ICB) shall be analy^-fed /fter calibration.

      4.5.6.5.2  Frequency

          The  ICB shall  be  analyzed each
       immediately after the ICV.
                                                           the>IDL,  the result
                                                     is calibrated and
      4.5.6.5.7  Documenta
  4.5.6.5.3  Procedure

     If the absolute value of  the  ICB  is greater
   shall be  reported.
      4.5.6.5.4  Calculations

         Not applicable.

      4.5.6.5.5  Technical Acceptance Cri

         The absolute  value  of th
                       /  /—^
      4.5.6.5.6  Corre

         When  the  I
       criteria,  te
       the  calibrat4
                                             ss than the CRQL.
                                              the technical acceptance
                                           ,e problem,  recalibrate,  verify
                                        pn FORM IV-AAIN.

                               ition Blanks
                                 km is  not contaminated during the  analysis
                                6n blanks (CCB) are analyzed.
July, 1991
                                                              Page  D-45/IN
-------
Exhibit D
                                                     SOW- NcfNJEXX  - Ambient  Air
      4.5.6.6.2  Frequency

          Analyz£ the CCB at a frequency of 10 percent
       whichever is more frequent.

       Analyze the CCB after every CCV.

      4.5.6.6.3  Procedure

          A CCB shall be run after the last CC

          If the absolute value of the CCB #
       shall be reported.

      4.5.6.6.4  Calculations

          Not applicable.

      4.5.6.6.5  Technical Acceptan<

          The absolute value of th

      4.5.6.6.6  Corrective Action
             ry two hours,
          lysis  run.

        an/the  IDL,  the result
              CRQL.
          When the  CCB concentration
       criteria, terminate analysis, correi
       the calibration, and--feana~ivze the prfc
       all analytical samples since

      4.5.6.6.7  Docume;

          Report the
                    <
     4.5.6.7   Prepara

      4.5.6.7.1  Summary
   the  technical  acceptance
 problem, recalibrate, verify
ing 10 analytical samples  (or
  iant CCB analyzed).
V-AAIN.
                                          during sample preparation, a
                                  ;t be prepared and analyzed with every SDG
                                     digested, whichever  is more  frequent.
July,  1991
                  Page D-46/IN
-------
Exhibit D
                                                SOW No.  XXX -  Ambient Air
          The PB shall consist of ASTM Type II water processed through  each
       sample preparation and analysis procedure  step  (se4  Exhibit D) .
                                                           igned to PB one,
    The first batch of samples in an SDG is to b
 the second batch of samples  to PB two, etc.

4.5.6.7.4  Calculations

    Not applicable.

4.5.6.7.5  Technical Acceptance Criteria

    The absolute value of the PB must jae

4.5.6.7.6  Corrective Action
          If the absolute value of the PB concfentratiojt^ is less than or equal
       to the CRQL, sample results are not

          If any analyte concentration in the blank is above tfie CRQL, the
       lowest concentration of thayanatyte--inthe associate's/samples  must  be
       10 times the blank concentration  OtherwTsl7~~aJ-L_samples associated
       with the blank and with the anaryTe^s^^ceRcentration^ess than  10  times
       the blank concentration and ab'oveNthe CRQL /sliaTlr-be/redigested  and
       reanalyzed for that analyte.  The skmplfe concentration  is not  to  be
       corrected for the blank value.  \   \/  /
          If the concent rati.
       all samples
       shall be redigest
    4.5.6.8  Spike Sam
                                           low the negative CRQL, then
                                            sociated with  the blank
                                                d in ftg/L on FORM IV-AAIN.
       of s
       analys is
       Contractor
                              xabout the^/effect of the sample matrix on  the
                            nount of analyte is added (spiked)  into a  sample.
                              analysis shall be performed on each group
                           /(EPA may require additional spike sample
                  icial/recfuest by the Project Officer, for which  the
July, 1991
                                                            Page D-47/IN
-------
Exhibit D
                      SOW
                                                             XXX - Ambient Air
          If two analytical methods  are used to obtain tKe Deported values for
       the same metal within a SDG (i.e., ICP and GFAA)< t/en spike samples
       shall be.run by each method used.

      4.5.6.8.3  Procedure

          The  spike  is  added before  the sample pr
       digestion).

          Samples identified as  field blanks
       analysis.
          EPA may require  that  a  specific
       analysis.
                   t be  used for  spiked sample


               Le  be us4d jfor the spike sample
          In the  instance  where  there  is  more than one<^pike  sample per method
       per SDG and one spike sample recovery is no^tv^witnlTi^contract criteria,
       flag all the samples for the same method in
          If the  spik
       for the dupli^at
       performed us,
       sample" (see
       duplicate result
       percent recovery
      4.5.
      4.5.6.8.4  Calculations

                          % Recover
       where:
          SSR  =  Spiked Sam
           SR  = Sample
           SA  - Spike Ade
                                  Eq.  D/IN-20
                 Ehe  same  sample  that  is  chosen
                'calculations shall be
               Le designated as the "original
  z'ate Sample Analysis).   The average of the
    used for the purpose of determining
          s  less  than the  instrument detection
or purposes of calculating percent recovery.

   nee Criteria
                                   ould be within ± 25 percent of the spiked
                               ceht).
July, 1991
                                   Page D-48/IN
-------
 Exhibit D
                                                      _SOW No. XXX - Ambient A:
       4.5.6.8.6  Corrective Action

           If  the  spike  recovery is not  at or within the/limits of 75-125
        percent, the data of all samples received associate^"with that spike
        sample and determined by the same analytical methodlhall be flagged
        with the letter "N" on FORMs I-AAIN and VII-AAIN.T

           An  exception  to  this  rule  is  granted in 4iRations whefre  the^sample
        concentration exceeds the spike  concentrator/by a factor of^four
        more.   In such an event, the data shall lie  reported unflagged even Jit
        the percent recovery does not meet the /5-125 percent recovery
        criteria.                              '  '

           When  the digestion spike recovery/fa^ls outsicie/the  technical
        acceptance criteria and the sample/test^t does/no/ exceed 4x the  spike
        added,  an  analytical spike must  be>^rform^dyfor/those metals that do
        not meet the  specified  criteria  (exce^Kon:   Ag£.   Spike the unspiked
        aliquot  of the sample at 2x the  indigenouK^eveTx^ 2x CRQL,  whichever
        is  greater.
  4.5.6.8.7   Documentation

     Report  the spiked sample
   percent recovery for  the  dige
   AAIN.

     The units for reporting spike

4.5.6.9  Duplicate

  4.5.6.9.1   Summary
          Duplicate a
       and analysis
       analytical m

      4.5.6.9.2  Frequency

          At
       group
       samp
       the
                                                            'spike added and
                                                           .ysis  on  FORM VI-
                      icate
       samp
                                           :ied through the preparation
                                            about  the precision  of  the
                              as  matrix  effects.
         lalysis shall be performed on each
       ^ !PA may require additional duplicate
;ial request by the Project Officer, for which
"
                               are used to obtain the reported values for
                               (i.e., ICP and GFAA) ,  then duplicate
                            /ach method used.
July, 1991
                                                                  Page D-49/IN
-------
Exhibit D
                                                     SOW No^OCXX  - Ambient Air
4.5.6.9.3  Procedure

    Samples identified as field blanks cannot b«
 s ample analysis.

    EPA may require that a specific sample
 sample analysis.

    In  the instance where there is more t#an/
 method per SDG and one duplicate result
 criteria, then flag all the samples frir tfie methe

    Duplicate  sample analyses are re^uii
 percent difference.

    Duplicates cannot be averaged for rep<

4.5.6.9.4  Calculations

                        RPD
                                                             or duplicate
                                                                        te
                                                                 Eq. D/IN-21
                                                          in contract
                                                             the SDG.
                                                          lation of relative
Percent Difference
             (origi
       where:
         RPD -  Relative
            S    = First
            D    = Second

      4.5.6.9.5  Techni

         A  control
       and duplicat
       (Exhibit  C).
       values less  than

          If one
       below,  >dse
       val
       ca

          Specif
       AAIN at a lat
                                          \Mg/L,  and
                                              g/L.
                                            shall  be  used for original
                             greater than or equal to five times CRQL
                           idt of ± CRQL shall be used for sample
                          
-------
 Exhibit D
                                                     _SOW No. XXX - Ambl.
       4.5.6.9.6  Corrective Action

           If  the  duplicate  sample  results  are  outside  t
        all the data for samples received associated w
        sample with an asterisk "*

       4.5.6.9.7  Documentation

           The  results of  the duplicate sample  an
        FORM VIII-AAIN in
                                                      mtrol  limits,  flag
                                                       t duplicate
          The absolute value of the control 1
        the  "CONTROL LIMIT"  column of  FORM VJ1I

     4.5.6.10    Laboratory Control Sampl

      4.5.6.10.1   Summary

          A laboratory control sample (LCS) is diges._
       against  analyte loss in the sample  preparation.
4.5.6.10.2  Frequency

    One  aqueous  LCS shall be pr>
 samples in a SDG or for each bafcch\i.<
 at the same time) of samples,

4.5.6.10.3  Procedure

    The  LCS  shall b4 a;
 preparations,  a
 EPA samples re

    The  LCS  so,
 solutions ma
                                                        lalyzed to ensure
                                                           r every group of
                                                   group of samples prepared
                                                's more frequent.
                                                     using the same sample
                                                   rocedures employed for the
                                                  EPA (if unavailable, the ICV
          If the EPA LCS
       samples

      4.5.6
                            .able,  other  EPA Quality Assurance  Check
                                rials may be  used.
                                 Found Concentration
                                  True Concentration
                                               x 100
Eq. D/IN-22
                                  ance Criteria
July, 1991
                                                                  Page D-51/IN
-------
Exhibit D
                                                      SOU No/^XXX  - Ambient  Air
          Recovery for the aqueous LCS shall be within ±/20 percent of the
       true value' (I.e., 80-120 percent) with exception/of/Ag and Sb.

          Technical  acceptance criteria for Ag and Sb
       determined at a later date.

      4.5.6.10.6  Corrective Action

          If the percent recovery for the LCS f/llf' outside
       acceptance criteria, the analyses shall/be/terminated, the problem
       corrected, and the samples associated/witn that Lj^Nreprepared and
       reanalyzed.
      4.5.6.10.7  Documentation
          Report the LCS  found concentration
       and percent recovery on FORM IX-AAIN.
    4.5.6.11     Analytical Spike S

      4.5.6.11.1  Summary
      4.5.6.11.2  Frequency
          All GFAA analy
       one analytical sp
          The frequenc^
       spike.
      4.5.6.11.3  Pr
          All GFAA analyses
       range.
                          ncentration (/jg/L) ,


           Analysis/Method of^ Standard Additions

                           •—

                            e  effects in GFAA
          To ensure against bias resu
       analyses, the Method of Standard\Addltions7 (MSA) is utilized.
          An analyti
       sample.
                     iple will require at least


                    recovery of the  analytical




        MSA shall fall within the calibration
    all analyses require duplicate injections.
    required for MSA quantitation.  Average
    ed for reporting purposes.

     two times CRQL) of a sample must be run
    le.  The percent recovery of  the analytical
   fethod of quantitation for the  sample.

j/s not required for the pre-digestion spike
July,  1991
                                    Page D-52/IN
-------
 Exhibit D
                                                      SOW No. XXX - Ambii
          A maxipum of  10  full  sample  analyses  to  a maxim
        may be performed between each consecutive calibr
        and blanks.   Each full MSA counts as two analyt}
        determining  10 percent CCV/CCB frequency (i.e.
        performed between calibration verifications).

          For analytical runs containing only MSAs
        used for  QC samples during that run.   For
        an MSA mode only,  MSA can be Used to det
        run.

          The sample and three  spikes must
        quantitation  (the  "initial"  spike  r
        from use  in the  MSA quantitation).
                                             20 injections
                                            verifications
                                          samples  towards
                                           full MSAs  can be
          MSA spikes shall be prepared sue
                                              \
        a)   Spike  1  is  approximately 50  percent
        b)   Spike  2  is  approximately 100 percent
             and
        c)   Spike  3  is  approximat
             (all concentrations  e

      4.5.6.11.4  Calculations

                          % Recovery =
                                         ecutively for MSA
                                         ically excluded
       where:
             SSR
             SR
             SA
SpikfiJd Sample R'fesi
Sample /Result; ,and
Sp/ke/Added.
                                          e concentration;
                                           e concentration;
                                           'e concentration
                                               Eq. D/IN-23
                                                                 Eq. D/IN-24
       where:
       within ±
                              > tandairiKQeviat ion
                              Aviation; and
                                  :ance Criteria
              -QL, the duplicate  injections must agree
              "  or CV.
July, 1991
                                                                  Page D-53/IN
-------
Exhibit D
                                              SOW N(X>OQCX - Ambient Air
          The  analytical spike recoveries for the LCS ana Pyshall be within
       control limits of ±.15 percent (i.e., MSA is NOT/ pe^Tormed on the LCS
       or PB).  .
      4.5.6.11.6  Corrective Action

          If the RSD (CV)  technical acceptance cri
       sample once.  If the criteria are still not
       reported on FORM I-AAIN with the letter

          NOTE:   The "M"  flag is required fo
       the sample.

          If the PB analytical spike tech;
       met, verify the spiking solution by
       once.  If the criteria are still not
       reanalyze all analytical samples associated^
                                                                    the
          If the LCS analytical spi
       met,  correct the problem an;
       associated with that LCS.

      4.5.6.11.7  Documentation
          The raw data package must ir.cluis
       values for both injections, the
       variation  (or RSD).

          The data for each
       data documentat
       absorbance as
       intercept, an-
       of the data.
                                                   criteria  are  not
                                                  rerunning the PB
                                                  the problem and
                                                     blank.
                                echnical  acceptance
                                           analytical
     4.5.6.

       4.5/
  ria  are  not
amples
                                         •bance  and concentration
                                        lvalue,  and the coefficient of
                                             arly identified in the  raw
                                            n as the x-variable and
                                          :he slope, x-intercept, y-
                                         ) for the least squares fit
   Reported value
on FORM I-AAIN if
correlate
XII-AAlX'with
                                   by MSA must be flagged with the letter "S"
                                    £ion coefficient is > 0.995.  If the
                                        5, flag  the data on FORMs I-AAIN and
        sample
                            limit (IDL) shall be determined before any
                           ery instrument that will be used.
 July,  1991
                                                           Page D-54/IN
-------
Exhibit  D
                                                     .SOW No.  XXX - Ambient Air
      4.5.6.12.2.  Frequency

          IDLs must be determined within 30 days of the
        and  at  least quarterly  (every three  calendar m

      4.5.6.12.3   Procedure
          IDLs (in /ig/L) shall be determined by m
       average of the  standard deviations  (ffn-i
       nonconsecutive  days  from  the  analysis o
       analyte in reagent water)  at  a  concent
       of the instrument manufacturer's  sugg
       measurements per day.  Each measurement
       were a separate analytical sample
       followed by a rinse  and/or any  ot
       between the analysis of separate  s
       and reported for each wavelength  used
        t of the contract
          The quarterly determined IDL for an instrv
       as the IDL for that instrument^ during that
       is adjusted in any way that,
       instrument shall be redetei
       the established IDL for thatN
       quarter.

       IDL must be determined in /ig/L.

      4.5.6.12.4  Calculatic

                                 IDI\
       where :
three times to five times
        seven consecutive
       brmed as though it
      .rement shall be
     •mally performed
    shall be determined
   lysis of the samples.

           always  be  used
           the instrument
           for that
     iubmitted for use as
   remainder of the
             Eq.  D/IN-25
                                                in Exhibit C.
                                  annot meet the CRQL for an analyte,  that
                                  :o quantitate an analyte unless the sample
                                  times the IDL.
July, 1991
              Page  D-55/IN
-------
Exhibit D
                   SOW Nox-OCXX - Ambient Air
          For each instrument used,  IDLs shall be report
       submitted with each data package.  If multiple G
       used for the analysis of a metal within a SDG,
       GFAAs shall be used for reporting concentratio;

4.5.7 Instrument Operation

     4.5.7.1  Set up the  instrument with the proper
     established by  the  instrument manufacturer
     (drying, charring and atomization)  require/ca/eful
     ensure each process  is carried out  effective]
     allowed  to become thermally  stable  before heginnin,
     usually  requires at  least  30 minutes of operation
     Background correction shall be used.
                                                              FORM XV-AAIN and
                                                            Instruments are
                                                                  IDL for the
                                                                >r that SDG.
                   crating
                 !e individual steps
                     consideration to
                          trument shall be
                          analysis.  This
                          to calibration.
                                                      The
    4.5.7.2  Calibrate the  instrument according^^p  the
    recommended procedures  using calibration stan<
                    so
                      lanuf acturer' s
                         ions.
    4.5.7.3  In order to determine l£_the  sample result  LSX^O b4  calculated
    by MSA,  an analytical  spike  at /two  ti5e~5—€RQl
-------
 Exhibit D
                                                      SOW No. XXX  - Ambient
                                                               hall be matrix
                                                              pe of the
                                                                         ICB,
f  4.5.8.1.4  All standards, blanks,  and sample soluti
  matched.  "A  change  in the acid strength changes
  calibration  curve and can cause inaccurate result

4.5.8.2 Analysis  Sequence

  4.5.8.2.1   Before beginning the sample
  ICV and CRA  under the same  operating conditj
  analyses.  The ICV and CRI  found concentrat_.
  from  the true values  by more than  10 percent/  The  calibration
  values may not exceed the CRQL.  If  thes/ conditions  are  not met for any
  element, the analysis shall be  discontinue/and corrective  action
  applied until the conditions are met (^ee/Exhibits^D/and  E  for
  additional information).

  4.5.8.2.2   Upon successful analysis\of  tnXIC^  arid ICB, analyEe  all
  method PB extract(s)  prepared with theNLUes^ed /amples.  If any of  the
  blank(s) are not less  than or equal  to  theXRQL.Sw^e  Exhibits D  and  E
  for the appropriate action.
      4.5.8.2.3   If the method bl
      LCS.  If any LCS values devote
      D and E for the appropriate acti>
                                        uesare acceptat^e/ analyze the
                                  _from theaCce-p£able ranges, see Exhibits
      4.5.8.2.4   If the LCS values art
      the method spike sample.   If the
      the acceptable ranges, see Exhibits\D
      Proceed to the analysis_af_^samples  ii
      after consulting Exhibits
                                        anc
    acceptable  ranges,  analyze
 jf any element deviates from
 E for the  appropriate  action.
.recoveries are acceptable or
      4.5.8.2.5   The CGV a^d the\CCBxmtr»
-------
Exhibit D
                                                      SOW  Nco^XXX -  Ambient Air
      4.5.8.3.2  .All concentrations reported shall be o#taifaed within  the
      established linear range for  that  analysis run.  .All/concentrations
      within the linear range of the analyte are to ber reported.

      4.5.8.3.3   In order to determine  if the sample
      calculated by MSA, an analytical spike at tvp tttnes
      performed and analyzed immediately after eac^K^ample analysts^,  Tfis
      analytical spike recovery is  used  to deteE&injfe the need  for MSA^as
      explained in part 4.5.6.11 and Exhibit E/ "^he spiking solution vol
      shall not exceed 10 percent of the samp]
      3.5.8.3.4   Add appropriate volumes o
      remaining three aliquots that resul
      100 percent, and 150 percent of  theQ.nst'
      spiking standard solution volume adde
      10 percent of the volume of the  aliquot.
      blank solution to each aliquot to make  the t
      volumes added equal.
                      andard  to  the
                         of 50 percent,
                     near range.   The
                   iquot shall not exceed
                    appropriate amount of
                        ike plus  blank
      NOTE:  If more than 10 minutes has eTip^e4~_s_ince tne  flfst  aliquot  was
      analyzed, it is suggested, bW rt&C—ceguired, thlfE—the-,, CCV and  the CCB be
      analyzed to determine whether\recklibratic?n  i*-_rj|quii7ed.  Performing the
      calibration verification prior B« reanalyzing thetirst aliquot  and the
      spiked aliquots may save consider^ble\ti!me/in the long run, as it can
      eliminate the repeat analyses required  if/the CCV or  blank  values are
      not within the acceptable limits pos\
        sample  analysis.
      4.5.8.3.5   Using a/cal
      determine the slo
      abscissa (x-axisY", ajfid the
      concentration asr the ordina
      the abscissa. /The/absolut
      the concentra/ionSaf the
      correction coeticien
      repeated.  If th
      0.995, then  repeat th<
      digest.  B
      using a/*maller
      is sti

     4.5.8
or a  stat
felatit
                   al  package  on a computer,
          of thV oi&iinate (y-axis) and the
                  icient using the found
                  rd addition concentration as
                ntercept of the abscissa is
               ilute solution.  If the
  'ss than 0.995, then the analyses shall be
  lysis correlation coefficient is less than
    s using a smaller aliquot of the sample
         the difference in volume created by
         .ot.  If the correlation coefficient
flag £he' sample data with a " + ".
                                    trument  detection  limit  (IDL)  from  the
                                   thod blank analyte  analyses,  based on the
July,  1991
                              Page D-58/IN
-------
Exhibic D
                                                      SOW No.  XXX -  Ambient Air
      4.5.8.4.2.. Calculate the method blank(s) concentra
      multiplying the value obtained  in part 4.5.8.2  for/th
      dilution factors used in part 4.5.8.1.
                                          value
                                       Found
                  Method Blank
                  Cone.  (\ig/L)

4.5.8.4.3   Calculate sample extract concent^at
multiplying the analyte concentration calc
dilution factors used in Sections 4.5.8.1
concentration for each analyte in Mg/m3
concentration in Mg/L by the extract vo
dividing by the volume of the air samp
the number of filter strips digested.
area (63 in2) of the Hi-Vol filter
the exposed area (7 in2) in one 1"
                                    (Mg/L) by
                                   blank  by  the
                                      Eq.  D/IN-26
                                                   .Itiplying  the
                                                   (liters^  times 9  and
                                                           ,3) per filter  and
                                                            represents  the
                                                          r stream  divided  by
            Analyte Cone.
             In air, \ng/m3
      Determine the
      standard addition
      concentration and
      percent re
      a sample/
      concen
      deter
      than10
           o
              nee-Corrected^
            Valued	/r       '
                                                           )  Eq.  D/IN-27
                 Analyse Ct
                          Dilution
                           Factor
                                                            Eq. D/IN-28
        ion for each sample analysis from the
       ide the standard deviation by the sample
         100 to obtain the percent RSD.   This
               (%RSD) is a measure of the effect of
              cess precision.   If the sample
    than fiv/ times the limit of detection
     ,2 and the %RSD for the sample value is greater
   ag\the results with an asterisk "*" to denote a
the\ result.
July, L991
                                                                  Page D-59/IN
-------
Exhibit D
                                                     SOW No/^XX  - Ambient  Air
                                             100
                                              Eq. D/IN-29
       where;
          %RSD  -  % Relative Standard Deviation
             <7n-i   -  Standard Deviation
                 x   = Mean Sample Concentratioi

     Calculate  all  method spike  levels  relative  t6  the  co/re/ponding unspiked
     sample  concentration in  units  of    "
    Calculate  the  relative  percent  difference  (RP^^/or ,60th  the method  and
    analysis duplicates.  Calculate  the  RPD  byM^iding^the absolute  value  of
    the difference between  the sample value  and  thV^dupli^ate value by their
    mean and multiplying by 100.
                              RPD
       where;
            RPD
Relative
                                                                 Eq. D/IN-30
             S   -  First  S
             D  =  Second
4.6 BIBLIOGRAPHY

4.6.1 Winge, R.K.,  V
Plasma-Atomic Emissio

4.6.2 Winefordner,  J.D.
Elements," Chemical^Analysis

4.6.3 Handbook/for.
Laboracori
4.6.4 Gar
Emission
Spectroscopy

4.6.5 Methods
                              ,  "Inductively Coupled
                 Prominent Lines,"  EPA-600/4-79-017.

                  •sis:   Spectroscopic Methods  for
                      .  41-42.
                      ?
                      :rol in Water and Wastewater
              SEPA Environmental Monitoring and Support
                 1979.

             ,  H.E.,  "An Inductively-Coupled Plasma Atomic
             r Routine Water Quality Testing," Applied
            ysis of Water and Wastes.  EPA-600/4-79-020.
4.6.6 Annual Book of ASTM
           dards.  Part 31.
July, L991
                                               Page D-60/IN
-------
Exhibit  D
                                                     _SOW No.  XXX -  Ambient  Air
4.6;7  "Carcinogens_- Working With  Carcinogens,"  Deparcme
Education, and Welfare,  Public  Health  Service, Center  f
National Institute  for Occupational  Safety  and Health,
Aug. 1977.

4.6.8  "OSHA Safety  and Health Standards, General  I
Occupational Safety and  Health  Administration, OS
1976) .
            Health,
         [sease Control,
        Lication No.  77-206,
4.6.9 "Safety in Academic Chemistry Laboratorie
Publications, Committee on Chemical Safety,  3;

4.6.10 "Inductively Coupled Plasma-Atomic
Trace Elements Analysis of Water and Waste
Inorganic Data/Protocol Review Committee/
Martin,  EMSL/Cincinnati.

4.6.11 Federal Register 1978, 43 (Oct. 5), 46258^
                  1910) ,
                   .anuary
      an Chemical
ition,  1979.
4.6.12 "Standard Operating Procedure^for Microwave Extrate
-------
Exhibit D
                                               SOW  No.  XXX  -  Ambient Air
                           TABLE D/IN-1

        INORGANICS  IN AMBIENT AIR TARGET ANALYTE
                                                       LIST rJT
                                                           ontract
                                                             itation
  Analvte
Cadmium
Arsenic
Chromium
Beryllium
Selenium
Lead
Barium
Manganese
Thallium
Zinc
Copper
Antimony
Cobalt
Nickel
Silver
Vanadium
Tin
Molybdenum
Aluminum
Calcium
Iron
Magnesium
Potassium
Sodium
                      CASRN
                     7440-43-9
                     7440-36-2
                     7440-47-3
                     7440-41-7
                     7782-49-2
                     7439-92-1
                     7440-39-3
                     7439-96-5
                     7440-28-0
                     7440-66-6
                     7440-50-8
                     7440-36-0
                     7440-48-4
                     1313-99-1
                     7440-22-
                     7440-62
                     7440-31>
                     7439-98-7
                     7429-90-5
                     7440-70-2
                     7439-89-6
                     7439-95-4
                                         Required
                                          Limit1-2-3
                                           ue/L
                                             18
                     7440^23-
 (D
The analytical mepno
achieved method det
Quantitation Limit
only be used in t
                     iSt y must be utilized and the
 tion limits shaltxsmeetv<'the Contract Required
(CRQL)  i/eqiLJrreTBents^^ligher detection levels may
f o 1 low/ng /circumsbanc/
      If  the samples*jncerib3^ati/bn
      instrument or method  in  use
      instrument or instrument
      required  quan£-Lta^ion
      documented! as described  in
 (2)
 (3)
                             xceeds two times the detection  limit  of  the
                             the value may be reported even  though the
                             .ction limit may not equal the contract
                                  method detection  limit must  be
                              ibits? D and E.
As
volumes
      d detection limits (for metals) and the
       ank values (for all other parameters)
     od\blank preparations that must be met using
         ,nd E.
          Hi-Vol filter and 40 mL final extract
        ter 3, Section 3.7.1.4 for calculations.
 Julv, 1991
                                                             Page D-62/IN
-------
Exhibit  D
                               SOW No.  XXX - Arch Jen:
                                  TABLE D/IN-2

                     RECOMMENDED WAVELENGTHS2 AND ESTIMATED/^
                         INSTRUMENTAL DETECTION  LIMITS    /  /
Element
       Wavelength,  nm1
                                                                 Detection
Aluminum
Antimony
Arsenic
Barium
Beryllium
Boron
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Molybdenum
Nickel
Potassium
Selenium
Silver
Sodium
Thallium
Tin
Vanadium
Zinc
          308.215
          206.833
          193.696
          455.403
          313.042
          249.773
          226.502
          317.933
          267.716
          228.616
          324.754
          259.940
          220.353
          279^079
          2
(1)
i/sted are/
                           Othe;
reotmunendiadbecause of their sensitivity  and
wavelengthsimay be substituted  if  they  can
      The  wavelength^ 1
      overall  accep/anc'
      provide  the  ne&4ed s>asi/ivfty and are treated with the same corrective
      techniques  for spe-s^ral interference.  The use of alternate wavelengths
      shall  be reported (irfxjra)  w>th the sample data.

      The  escima-€e~d ins~t^jmentaPxietecbipn limits as shown are taken  from
      " Induct^velv__Ccmj>led Plasma-Absmicr Emission Spectroscopy-Prominent
      Lines/  E/A-600/4^7^017\  They are given as a guide for an instrumental
      limit?.  ;ihe  actual meChodNietection limits are sample dependent and may
      vary as/the  sample matrix varies.

(3)    Hyghlyxdependent on operating conditions and plasma position.
(2)
Julv. L991
                                                                   Page D-63/IN
-------
Exhibit: D
                                                     SOW No/^XXX -  Ambient Air
                                 TABLE D/IN-3

          EXAMPLE  OF  ANALYTE CONCENTRATION EQUIVALENTS
                   FROM INTERFERENTS AT  THE 100 MG/L
Interferent
                 Wavelength
Analyte
             nm
                      Al
                  Cr
Cu
Fe  /
Ni
Ti
Antimony   206.833
Arsenic    193.696

Barium     455.403
Beryllium  313.042
Boron

Cadmium
Chromium

Cobalt
Copper
249.773

226.502
267.716

228.615
324.754
                      0.47
                      1.3
                       0.04
                  2.9
                  0.44
Lead       220.353      0.17
Manganese      257.610
Molybdenum     202.030
Nickel     231.604
Selenium   196.026
 Thallium   190.864
 Vanadium
 Zinc
           292.402
           213.856
      .25
                                 0.45
                                 1.1
                                                                   0.04  0.05
                                                                         0.04

                                                             0.03  0.15  --
                                                                   0.05  0.02
                                                  002  0.002 --
                              0.005
                                                                    0.02
                          ,14
0.29
 July, 1991
                                                                   Page  D-64/IN
-------
 Exhibit  D
                                                     _SOW No.  XXX -  Arabian- A
                                  TABLE D/IN-4




                           INTERFERENCE CHECK SAMPLE
July, 1991
                                                                  Page D-65/IN
-------
Exhibit D
                                                     SOW Nfry XXX - AmMgnr A
                                 FIGURE  D/IN-1




                   TEMPLATE FOR CUTTING GLASS-FIBER E
July, 1991
Page D-66/IN
-------
Exhibit D
                                                     SOW No.  XXX -  Ambient Air
                                FIGURE D/IN-2




                          MICROWAVE DIGESTION SYSTEM
July, 1991
Page D-67/IN
-------
                                   EXHIBIT E
                QUALITY ASSURANCE/QUALITY C
July, 1991
-------
                                   EXHIBIT  E
                QUALITY ASSURANCE/QUALITY CONTROL REQU,
                               TABLE OF CONTENTS
SECTION 1   INTRODUCTION	/./... ./X	E_2
SECTION 2   QUALITY ASSURANCE  PLANS  .../../...././	   £.5
SECTION 3   STANDARD OPERATING PROCEDURES^.  /^V . /	   £-8
SECTION 4   CHAIN-OF-CUSTODY	-^^X. • -^X	   E-15
SECTION 5   DOCUMENT CONTROL   .  .  ^_^_	>X^-  V	   E-18
SECTION 6   ANALYTICAL STANDARDS xtyuiiLe^ENTS  .  .  r~:—?—^.	   E-22
SECTION 7   METHOD SPECIFIC QA/QC  REQUIREMENTS    '
      7.1   Volatiles Collected in Canistefcs/  ./	   E-27
      7.2   Volatiles Collected on Tenax®\.  . /.	   E-32
      7.3   Semivolatiles/f^  ^N-  •  •  •  .\  X,	   E-37
      7.4   Inorganics /.  ./7~~>~.  \	\ ' /	   E'42
SECTION 8   REGIONAL .DATA: REVIEW y .  	    •S>>~-7	   E-51
SECTION 9   LABORATORY 4yALUATION CAMPLES  />/	   £.52
SECTION 10  GC/MS
SECTION 11  ON-S]
                	   E-54
JORATORYxEVALUA^IONS	   £.55
SECTION 12  JQUALPTY-SSSIIRANCXDATA
SECTION iy  DyCTA MANAGEMENT
SECTION/14 ^-REFERENCES
                   ANALYSIS
                                                    E-58
                                                    £-60
                                                    E-62
July, 1991
-------
                                   SECTION 1
                                 INTRODUCTION
                                                     are
    Quality  assurance (QA). and quality control (QC)
EPA's Contract Laboratory  Program  (CLP).  The  CLP  QA p
management review and oversight at  the planning, impl
completion stages of environmental  data  generation a
data provided are of the quality required.  The CLP
program includes those activities required as  part,
ensure that the data are of known and documented
     During  the  planning of an environmental da/a
activities focus on defining data quality obj
designing a QC system to measure and documea
generated.  During the  implementation of th;
activities ensure that  the QC system is f-
deficiencies uncovered by the QC system
environmental data are generated, QA actr
of data obtained to determine its suitabilit
remedial decisions.
                             jgral  parts of
                              consists  of
                           Ration, and
                                to ensure  that
                                 rol (QC)
                                        to
                                                   >llection program,
                                                      and  criteria,  and
                                                              data  that will be
                                                  colle'cti^n  effort,  QA
                                                          :ively, and that the
                                                            corrected.   After
                                                          assessing the quality
                                                  support  enforcement or
    The purpose of  this  Exhibit  is  to describe the over^l QA^QC operations
and the processes by which the CLP/mee~ts~--th£j3A/QC objectives/defined above.
This contract requires a variety o'f QA/gC activT&te-s-T-^Ihese  contract
requirements are the minimum QA/QC^opexatioTts—necessary  to~7satisfy  the
analytical requirements associated withN^ie deterralHarteayof  the different
method analytes.   These operations arevdesdgnpd zo facilitate laboratory
comparison by providing the EPA with comparaele/data from  all Contractors.
These requirements do not release the lab\rato^y from maintaining its own QC
checks on method and instrumeat^performance
    Appropriate  use  of
conditions encountered
quality control proce
methods in this cont
received by the labj
validation of thes
for all samples collec
result from causes such a
human error.
indispensable.
              Therefore
       under the giteat range of analytical
                    ires  reliance on the
               orated into the methods.   The
              on/samples  typical of those
                :he CLP.   However,  the
   /ot guarantee that they perform equally well
        field conditions.  Inaccuracies can
     artifacts, equipment malfunctions,  and
       ontrol component of each method is
           ta acquired frbTa qua}
     The da
and evaluate analytical results
effect  of/co/rective actions .\ Tli
results
precisi
indicators^"
         include quantitative and
           accuracy, detection/
ity control procedures are used  to estimate
  .nd to determine the necessity for or the
    means used for evaluating the analytical
   ualitative indicators of quality such as
lijfait,  and other quantitative and qualitative
   give an overview of the activities required
in an integratedorogijam to/generate environmental data of known  and
documented qualityxvrsequit«id' to/meet defined objectives.
July,  1991
                                                                     Page  E -  3
-------
 Exhibit  E
                                                      SOW No. XXX - Ambient Air
     Necessary components of a complete QA/QC program incl/de^internal QC
criteria  that  demonstrate  acceptable  levels of performan/e, As determined bv
QA review.   External  review of data and procedures  is  a/complished by the  '
monitoring  activities  of the National Program Office, Xegi£nal data users
Sample Management  Office,  NEIC,  and EMSL/LV.   Each  ex/erna]>*eview
accomplishes a different purpose.   These reviews  are/de/c^ibedSn. specific
sections  of this Exhibit.   Performance evaluation s4mpXes  p^ide^a^external
QA reference for the program.   A laboratory on-si4 ^aluatiorT>ystemSs  also
part of the external QA  monitoring.   A feedback /bvi/provides  the re^u
the various review functions to the contract la/oratories  through dire     /
communications with the  Administrative Project/Officers and Technical Protect
Officers.                                     '   '

     This  Exhibit  is not  a  guide to constru/tin£ qualicy assurance project
plans, quality control systems,  or a  qual/ty 4§suranc6 o/ganization.  It  is
however,  an explanation  of  the  quality cokt^ol  ahdoualZty assurance
requirements of the CLP.  It outlines  some  minimum  standards for  QA/QC
programs.   It also  includes  specific  items  thatisce required in a QA Plan  and
by the QA/QC documentation  detailed in this  contracth\Delivery of  this
documentation provides the  Agency with a complete datap-ackage^which will
stand alone, and limits  the  need foF^trrt€*c£__with the Cont^acjfor  or with an
analyst, at a later date, if some tespectof  thT~Htaiy&is__i.s questioned.

     To ensure  that the product deliv\redvby th& CaGSrsn&Mj/ meets  the
requirements of the contract and to imfero've'  inter/aboratory data comparison,
the Agency  requires the  following from  Cfce
Development and imple
the key elements
described in Section

Preparation of
(SOPs) as des

Adherence
specified in
                                      of aN^A program, and documentation of
                                    rogram throug^ a written QA Plan, as
                                      Exhibit>

                                               Standard Operating Procedures
                                                 Ixhibit.
                                ^I/methods and associated QC requirements
                       analyt
Verification of
of neat nta^erials^-and the^
from p/ivate—etiemicalHiouses
idards and documentation of the purity
   ;nd accuracy of solutions obtained
                             ^naiVsis of laboratory performance evaluation
                               ence to corrective action procedures.
       Submission
       review.
July, 1991
                         laboratory evaluations,  including adherence
                       ocedures.

                      data and pertinent documentation for Regional
                                                                    Page E - 4
-------
Exhibit E
                                                     SOW No. XXX - Ambient Air
       Submission, upon request, of GC/MS tapes and applicable documentation
       for tape audits.
       Submission for Agency review of all original
       during sample analyses.
tation generated
July, 1991
        Page E  - 5
-------
Exhibit E
                                                      SOW No.  XXX  - Ambient  Air
                                   SECTION 2

                           . QUALITY ASSURANCE PLANS

     The Contractor shall establish a quality assura
objective of providing sound analytical chemical m
shall  incorporate  the quality control procedures,
action, and all documentation required during dat
quality assessment measures performed by manage
production.

     As evidence of such  a program,  the Cont
Quality Assurance Plan (QAP) which describ
implemented to achieve the following:

     •  Maintain data integrity, validity,

     •  Ensure that analytical measurement
       acceptable state of stability and reproducibi

     •  Detect problems through da
       action procedures which ke
                                                                with the
                                                                  is program
                                                                      tive
                                                                         the
                                                                           ta
                                                           :pare  a written
                                                            that are
                                    \
     •  Document all aspects of the m
       data that are technically sound"1
     The  QAP  must present,  in  specific ter
objectives, and specific Q.
quality requirements in tKis contr
each element shall be ipfcl
be available during On
the Administrative Pr
preparation of a QAP

2.1  ELEMENTS OF A

2.1.1  Contractor QA

2.1.2  Organization and

      2.1.2/1 /QA
                                                          tained in an
                                                              orrective
                                                           reliable.
                                                          order to provide
                                                 y defensible."
                                               te policies, organization,
                                                 igned to achieve the data
                                                     ble, SOPs pertaining to •
                                                 f t of the QAP.   The QAP must
                                                  and upon written request by
                                                information relevant to the
                                                M publications12-4'.
                              .nd/QA Responsibilities;  and

                             onships.
      2.1.2.2   Personnel

          •   Resumes;
July, 1991
                                                                    Page E - 6
-------
Exhibit E
                            SOW No.  XXX -  Ambient Air
             Education and Experience Pertinent to this Contract; and

             Training Progress.

2.1.3  Facilities and Equipment

          Instrumentation and Backup Alternatives;

      •   Maintenance Activities and Schedules.

2.1.4  Document Control

      •   Laboratory Notebook Policy;

          Sample Tracking/Custody Procedure^

          Logbook Maintenance and Archivi

          Case File  Organization,  Preparation
          Procedures  for Preparation,  Approval,
          Distribution of SOPs ;  and
       •  Process  for Revision of

2.1.5  Analytical Methodology

      •   Calibration Procedures and F:

          Sample  Preparation/Extraction

          Sample  Analysi

          Standards  P

      •   Decision
          Correct!
                               Procedures;

                                 ision, and

                                 -^y
                           intation Procedures.
                     .esponsibility for Initiation of
Proce
2.1.6  Data Generation

          Data

          Data Keduction^roce^ures;

               Validation Procedures;  and

                                 irization Procedures.

            ».    -   "     7  /
2.1.7  Quality\Conti

          Solvent, Reagent"and' Adsorbent Check Analysis;


July, 1991
                                          Page E  - 7
-------
Exhibit E
                                                     SOW No. XXX - Ambient Air
          Reference  Material  Analysis;




          Internal-QC  Checks;




          Corrective Action and  Determination of QC




      •   Responsibility  Designation.




2.1.8  Quality Assurance  Program Assessment




          Data Audits;




      •   Systems Audits;




          Performance  Audits;




          Corrective Action Procedures;  and




      •   QA  Reporting Procedures.
July,  1991
Page E - 8
-------
 Exhibit  E
                                                      SOW No.  XXX -  Ambient Air
                                   SECTION 3

                         STANDARD OPERATING PROCEDURES
     In  order  to  obtain reliable results,  adherence
methodology is imperative. In any operation that
basis, reproducibility is best accomplished thro
Operating Procedures (SOPs) .  As defined by the
document that provides directions for the step
operation,  analysis, or action which is commo
performing certain routine or repetitive
                                                                   nalytical
                                                                       etitive
                                          ta
    SOPs prepared by  the  Contractor  must
comprehensive, up-to-date, and sufficien
results by qualified analysts.  All SOPs,
reflect activities as they are currently perfo
addition,  all SOPs must:

    •  Be  consistent with current
       contract's requirements3•*•*

    •  Be  consistent with instrumen
       manuals;
       Be available to the EPA during an\0n
       complete set of SOPs shall be boun
       inspection at such
       laboratory personal ma
       the SOPs;
                                                          as  the method  for
                                                          .e.,  clear,
                                                     to/permit duplication of
                                                       to the Agency, must
                                                       he laboratory.  In
                                                               and the CLP
                                                      ecific instruction
Provide for t
complete to rf
protocol;

Describe the mec
by the Contractor
results;

Descr
ana
                                                 Laboratory Evaluation.  A
                                                    and available for
                                                 -Site evaluations,
                                              monstrate the application of
                                         :umentafeion that is sufficiently
                                                 tasks required by the
     •  Be ar
       situatiorT

     •  Be available at
                                  demonstrating the validity of data reported
                                    ing the cause of missing or inconsistent
                               measures/and feedback mechanism used when
                                 meet protocol requirements;

                                  ipdated as necessary when contract,
                                  icedural modifications  are made;

                                 'erence in usability or  evidentiary
                             ic work stations as appropriate;  and
July,  1991
                                                                    Page E -  9
-------
Exhibit E
                                                      SOW No.  XXX -  Ambient Air
     •  Be subject to a document control procedure which  p/ec^udes  the  use  of
       outdated or inappropriate SOPs.
                                                                  tivity  for
                                                                sections  must
                                                               econdary
      laborato
      proced
      be avil
      are
3.1  SOP  FORMAT

3.1.1  The format for SOPs may vary depending upon tfhe /IciBd of~
which they are prepared.  However, at a minimum,  tfle  £6llowii
be included:

     •  Title Page;

     •  Scope and Application;

     •  Definitions;

     •  Procedures;

     •  QC Acceptance Criteria;

     •  Corrective Action Procedures^Including  Procedure
       Review of Information Being/

     •  Documentation Description a

     •  Miscellaneous Notes and Precaut?

     •  References.
3.3  SOPS  REQUIRED

3.3.1  The Contractor
maintenance of custod;
analysis of samples, /an<
                    /  •
3.3.2  Specif icationsfor^
                                                   eceipt of samples,
                                  ntificatioh^sample storage, tracking the
                                  of/comp^i^ted
      li/tiga^ion
      d
      used
      shall ha"
 fenyStandard Operating Procedures

     ^s a written narrative  step-by-step
             procedures including examples of
     je SOPs  must  accurately describe the actual
laboratbxyyand copies  of the written SOPs shall
  ;>riate  laboratory personnel.   These procedures
      analytical data  produced under this
    (use  in EPA enforcement case preparation and
     s SOPs shall  provide mechanisms and
    if the  following specifications and shall be
      laboratory evidence audits.  The Contractor
     operating procedures (SOPs) for:
       •  Sample recerp-c and logging;
July, 1991
                                                                    Page E -  10
-------
Exhibit E
                                                     SOW No. XXX - Ambient Air
        •  Sample storage;

        •  Preventing sample contamination;

        •  Security  for laboratory and samples;

        •  Traceability of standards;

        •  Maintaining instrument records and logb

        •  Sample analysis and data control  syst/sms

        •  Glassware cleaning;

        •  Technical and managerial review
          package preparation;

        •  Internal review of contractually-r
          quality control data for each  individual
                           ility  assurance  and
                             package;
       •  Sample  analysis,  data  handling,  and  reporting^

       •  Chain-of-Custody;

       •  Evidentiary SOP;

       •  Laboratory Data Validation/LabNarab^ry/Self Inspection System; and

             Data flow and chain-of-command, fory data review.

             Procedures ^or/sreasuririg precision artci accuracy.
                      / /     >  ^>\   \7
             Evaluation parameters for identifying systematic  errors9.
             Proced
             requi
             SOW Exhi
                     and diskette  deliverables  (if
         and compliant with the requirements  in
                                       hardcopy deliverables  are  in agreement
                                        tte deliverables,  if  required.

                          ^of internal QA inspection procedure  (demonstrated
                                     on personal notebooks, internal PE
     Evidentiary     ^
Written Standard Opera^

July, 1991
     are discussed  in  Exhibit  F,  "Specification  for
Procedures"

                                        Page  E  -  11
-------
Exhibit E
                                                      SOW No. XXX  - Ambient  Air
             Frequency and type of  internal  audits  (e.g./ random,  quarterly,
             spot_checks, perceived  trouble  areas).
          •   Demonstration of problem  identification
             resumption of analytical  processing.
             internal audit (i.e., QA  feedback).
          •   Documentation of audit reports,  (i
             response, corrective action, etc.
          Data  Management and Handling

          •   Procedures  for controlling a;
                                  actions and
                                 uiting from
             Procedures for reviewing ch4nges
             ensuring traceability of upda

             Lifecycle management p-rocedures for
             implementing changes to existing computii
             hardware, software, ajid—documentation or  ins

             Database security, b
             recovery from system
                            a entry errors.

                          d deliverables  and
          •   System maintenance proce

          •   Individuals(s) responsible fc
             data integrit
          •   Specifica

       •  Document co,

     3.3.2.2  The  Centra
     responsible  for
     his/her  duties and

     3.3.2.3  T
     in of th
     docume
                            modifying and
                               is  including
                               ng new systems.

                            res including
              id Response  time.

                 tern operation,  maintenance,
    lave  a  designated sample  custodian
  imples  and have written SOPs describing
 iilities.
informa
written SOPs for receiving and logging
 hall include but not be limited to
on:
                             vof\EPA chain-of-custody forms;

                                 lirbills or airbill stickers;

          Pre^se_nce ~bx. absence' of/EPA Traffic Reports or SAS packing lists;

        •  Presence c5rs^ absence /of custody seals on shipping and/or sample

          containers and tits'ir condition;
July,  1991
                                     Page E -  12
-------
Exhibit E
                                                 SOW No. XXX  - Ambient Air
      Custody  seal  numbers,  when present;

      Presence  or absence  of sample  tags;

   •   Sample tag ID numbers;

   •   Condition of  the  shipping  container;

   •   Condition of  the  sample container;

   •   Verification  of agreement  or nonagre«
      receiving documents  and sample cont^

   •   Resolution of problems or  discrep^
      Office; and

      The definition of any  terms us«
      receipt.
                                                    of information


                                                  with/the? Sample Management


                                                   Lbe/sample condition upon
                                                   shal]
3.3.2.4  The Contractor shall have written SOrSKfor
security of samples after log-in and shall demons
sample storage and laboratory
descriptions of all storage area£
steps taken to prevent sample
list of authorized personnel
areas.
    3.3.2.5  The Contractor shall have
    performed on any particular^ sample.
    following:
  Lntenance  of  the
     :urity  of  the
    :ifically. include
 the  laboratory,  and
   shall  include  a
/to secure storage
                                           SOPs for tracking the work
                                           acking SOP shall include the
         A  description o
         sample  stor
         analyses;

         A  description
         calibration

         Examples of  the do~
         in th^^s ampTe--£§c. e ip t;
         an
                                    ion usWl/to record sample receipt,
                                        ample preparations, and sample
                            /umentation used to record instrument
                            #A/QC activities;  and

                                jrmats and laboratory documentation used
                                   storage, sample transfer, and sample
July, 1991
                                1 have written SOPs for maintaining
                                 ; throughout the laboratory.

                                 signs unique laboratory identifiers, written
                                tion of the method used to assign the unique
                               'ross-reference to the EPA sample number.
                                                               Page E -  13
-------
Exhibit E
                                                      SOW No.  XXX -  Ambient Air
     3.3.2.8  If  the Contractor  uses  prefixes  or suffixes An .addition to
     sample  identification numbers,  the written SOPs sha/1 i/nclude their
     definitions.' -The  Contractor shall have written SO/s describing the
     method  by  which  the laboratory  maintains  samples ,unde4: custody.

     3.3.2.9  The Contractor  shall have written SOPs/fo.r' <5*ganiz"as&4on and
     assembly of  all  documents relating to each EP^/Case, inctudj-ng^chnical
     and managerial review.   Documents shall be fiSLeo/on a
     basis.  The  procedures must ensure that all/cJbsuments including^
     pages,  sample tracking records,  chromatographiJc charts,  computer
     printouts, raw data summaries,  correspondency,  and any other written
     documents  having reference  to the Case are corn-pi.led/in, one location for
     submission to EPA.   The  system  must include a document!: numbering and
     inventory  procedure.
    3.3.2.10   The  Contractor shall have
                                                       >r  laboratory safety.
     3.3.2.11   The  Contractor shall have written "SOPs for\cleaning of
     glassware  used in preparing and analyzing sample&xunderx^his contract.
    3.3.2.12   The  Contractor shaljf have
    used  in sample analysis  QA/QC

3.4 HANDLING  OF  CONFIDENTIAL
                                              £or  traceability of standards
3.4.1  A Contractor conducting work undeV tMs .contract may receive  EPA-
designated confidential information from ohe Agency.  Confidential information
must be handled separately^frrjnr-Qther documentation developed under  this
contract.  To accomplish/this, theNfollowing^proc^dures for the handling  of
confidential informatiori hatfeTJe^n established\
                         Jocuments/
3.4.2  All confidentis
designated Document ^ongrol Offi
                                                  the supervision of a
                     ccJnfidenti
                            prma
3.4.3  Any samples
shall be handled as
maintained to store this 11
nonconfidential information.
be treated
logs these
then made
out to
file at tzhe Conclusion
be  reptfoduoed except upon
will ent>
information"
Officer.  Tl
information
disposition
                               on/received with a request of confidentiality
                                     A separate locked file shall be
                                   jn and shall be segregated from other
                                      grated from confidential samples shall
                                          of confidential information, the DCO
                              nfidentirial Inventory Log.  The information  is
                                  personnel but only after it has been signed
                                  e documents shall be returned to the locked
                                  king day.  Confidential information may not
                                  1 by the EPA Contracting Officer.  The  DCO
                                  .uraent control system.  In addition, this
                                   except upon approval by the EPA Contracting
                                nd retain the cover page of any confidential
                                year and shall keep a record of the
                                Inventory Log.
July,  1991
                                                                   Page  E  -  14
-------
Exhibit E
                                                     SOW No. XXX  - Ambient Air
3.5  SOPS  DELIVERY REQUIREMENTS
   r
3.5.1  Within forty-five (45) days of contract receipt,/a c/mplete set of SOPs
relevant to this contract shall be sent to the Technics
and EMSL/LV.  Also, during the term of performance of/
SOPs which have been amended or new SOPs which have
to the Technical Project Officer, EMSL/LV (quality
(evidentiary SOPs).
 oject Officer, SMO
contract, copies of
   Jen shall be sent
       ) and NEIC
July, 1991
         Page  E  -  15
-------
Exhibit E
                                                     SOW No. XXX  - Ambienc  Air
                                                                 from  the
                                                                  ffort  is
                                                                     llowing
                                                                         eking
                                   SECTION 4

                "  •             CHAIN-OF-CUSTODY

      A sample is physical evidence collected from
environment.  An essential part of hazardous waste
that the evidence gathered be controlled.  To ace
sample identification, chain-of-custody,  sample
procedures have been established.

4.1 SAMPLE  IDENTIFICATION
4.1.1  To ensure traceability of samples while/in possession of the
Contractor,  the Contractor shall have a specified metinod/for maintaining
identification of samples throughout the ^laboSsa^ory./

4.1.2  Each sample and sample preparation container sl^all be labeled with the
EPA number or a unique laboratory identifier.  Ir^-a unib^ae laboratory
identifier is used,  it shall be cross-referenced to the EPANq.uraber.
4.2 CHAIN-OF-CUSTODY PROCEDURES

4.2.1 Because of the nature of the'
samples must be traceable from the
are introduced as evidence in legal pffc
procedures ensuring that EPA sample cust
sample is under custody if the following
                                                           e custody of EPA
                                                          llected until they
                                                  The Contractor shall have
                                                ;aintained and documented.  A
     •  It is in your pos

       It is in your v,

     •  It was in yo

     •  It is in a
       authorized pers

4.3  SAMPLE  RECE

4.3.1  The
receiving

4.3.2
the evejit

4.3.3  The
inspected upon

4.3.4  The  condition^
inspected upon receipt by
                                                  ession, or

                                                it up, or

                                  e area (secure areas shall be accessible  to
                                        sample custodian responsible for
                                  late a representative to receive samples  in
                              sdikn is not available.

                                     containers and sample bottles  shall be
                            >ie smple custodian or his/her representative.

                             Zustody seals (intact/not intact)  shall be
                              sample custodian or his/her representative.
July,  1991
                                                                   Page  E  -  16
-------
 Exhibit  E
                                                      SOW No.  XXX - Ambient Air
4.3.5   The  sample  custodian or his/her representative shall check for the
presence or  absence  of  the  following documents accompany2ng>the sample
shipment:      "'  •

     •   Airbills  or airbill  stickers;

     •   Custody seals;

     •   EPA custody records;

     •   EPA traffic reports  or  SAS  packing lis

     •   Sample tags.

4.3.6   The sample custodian  or his/her re
forms (e.g., custody records,  traffic  rej^or
accompanying the samples at  the time of

4.3.7   The Contractor shall  contact  SMO to resc
such as absent documents', conflicting  information^
unsatisfactory sample condition (e.g.,  leaking sample^
4.3.8  The Contractor shall record
problems on Telephone Contact Logk.

4.3.9  The following information shal
by the sample custodian or his/her rep:

     •  Condition of the shi

     •  Presence or abserice
       sample containers;
                              11 sign and date all
                              lists,  and airbills)
                            ^epancies and problems
                                ustody seals,  and
                          discrepancies and
                        on appropriate  Form AADC-1
                    fe as samples are received and inspected:
                      y seals  on shipping  and/or
       Sampl
       numbers;
July, 1991
      •ties;

     r^bills  or airbill  stickers;

            :s;

  sEPA custody records;

       traffic reports  or  SAS packing  lists;

     tiple  tags;

ition numbers  cross-referenced  to  the  EPA  sample




                                        Page E  -  17
-------
Exhibit E
                                                     SOW No. XXX - Ambient Air
     •  Verification of agreement or non-agreement of infibrm/tion recorded on
       shipping .documents and sample containers; and

     •  Problems or discrepancies.

4.4  SAMPLE TRACKING PROCEDURES

4.4.1 The Contractor shall maintain records
handling from receipt to final analysis.  The
documentation of the movement of samples and
designated laboratory storage areas.
                                                        all phass, of
                                                   ds shall include
                                                      samples into andbt of
July, 1991
                                                                   Page  E  -  18
-------
Exhibit E
                                                      SOW No.  XXX - Ambient Air
                                   SECTION 5

                               DOCUMENT  CONTROL

     The  goal of the laboratory document control  program ^s to assure that all
documents for a specified Sample Delivery Group  (SDG/ will^be  accounted for
when the project is completed.  Accountable documents u§fedby&*xntract
laboratories shall  include but not be limited to Logbofoks,  Ckain-~oN&*custody
records, sample work sheets, bench sheets, and ot^r/documents^telatijlx to  the
sample or sample analyses.  The following docume^n^eontrol  procedures havfe
been established to assure that all laboratory,
stored for delivery to the EPA or are available upon request from the EPA
prior to the delivery schedule.

5.1  PREPRINTED  LABORATORY FORMS AND LOGBOQ&S
5.1.1 All documents produced by the Contractor
the preparation and analysis of EPA samplessfaall becme
EPA and shall be placed in the complete sample
observations and results recorded by the laboratoryNjut
laboratory forms shall be entered into permanent laborat
all data from a SDG are compiled,
all SDG-related logbook entries s^alljae include*
package.
                                           Lnal laboratory
directly related to
the property of the
roup file (CSF).  All
   on preprinted
      books.  When
       and copies of
documentation
5.1.2 The Contractor shall identify t!
documents which is directly related to
samples.
                                                /recorded on all laboratory
                                               iration and analysis of EPA
5.1.3 Pre-printed laborat
and be dated (month/day/yea
performing the activity at/the tfjpe
                             formsxshalL coriXain\the name of the laboratory
                                  signed by tne person responsible for
                                          ivity\iy performed.
5.1.4 Logbook entries' si
responsible for perforr
                        ill be d^ted^nio>k^h/day7year) and signed by the person
                           the actvvity at ch«/tirae an activity is performed.
5.1.5 Logbook entries-shall"
with the exception of insl
only one SDG per page.

5.1.6 Pages

5.1.7 Inst,
of the r
provide
exercis&^the
numbers in
client names
                                  chronological order.  Entries in logbooks,
                                 run logs and extraction logs, shall include
                              unbourtd^lpgbooks shall be sequentially numbered.

                                 e maintained so as to enable a reconstruction
                                  instruments.  Because the laboratory must
                                  un logs to the EPA, the laboratory may
                               lyj laboratory or EPA sample identification
                                  rather than government agency or commercial
                             confidentiality of commercial clients.
July, 1991
                                                                   Page E - 19
-------
Exhibit E
                                                      SOW  No.  XXX -  Ambient Air
5.1.8 Corrections to supporting documents and raw data  shall/be  made  by
drawing a single line through the error and entering  the/co/rect information.
Corrections and additions to supporting documents and /aw Aata shall  be  dated
and initialed.  No information shall be obliterated o/  rendered  unreadable.
All notations shall be recorded in  ink.  Unused port/ons of ctecuments shall be
"z'd" out.

5.2 CONSISTENCY OF DOCUMENTATION

5.2.1  The Contractor shall assign  a document /onjTrol officer responsibtB/for
the organization and assembly of the CSF.

5.2.2  All copies of laboratory documents ^nal/ be comp/lej?e and  legible.

                                                         control officer
                                                        e tags, custody
                                                         and other relevant
                                                           le or sample
5.2.3  Before releasing analytical result^,
shall assemble and cross-check the informa
records, lab bench sheets, personal and instr
data to ensure that data pertaining to each parti
delivery group is consistent throughout the CSF.
5.3 DOCUMENT  NUMBERING  AND  INVENT
5.3.1  In order to provide document\acc\3untaEiTrity_Qf_the Completed analysis
records, each item in a CSF shall be Vnve^itori/d /nd assTgned a serialized
number as described in Exhibit B, Sectipn
         CSF # -  Region -  Serialized numbe
5.3.2  All documents relevant to e^tch sample ^delivery group, including
logbook pages, bench sheets/mass, spfectra, chromat^grams, screening records,
re-preparation records/ re/analysas recorclSs. records of  failed or attempted
analysis, custody records7, libr  / res^ajch remits, etc., shall be
inventoried.
                                                           75-2-0240).
5.3.3 The Document
that all documents gene
delivered to the EPA.  The
the file.  Figur§>-t—ts—an ex
                                   (DCO) shall be responsible for ensuring
                                 placed in the CSF for inventory and are
                                     place the sample tags in plastic bags in
                                       document inventory.
 July,  1991
                                                                    Page  E  -  20
-------
Exhibit E
                                                      SOW No.  XXX -  Ambient Air
Document Control #*
232-2-0001
232-2-0002
232-2-0003
232-2-0004
232-2-0005
232-2-0006
232-2-0007
232-2-0008
etc.
                             Figure 1

                              Example


                        DOCUMENT INVENTORY

                            Document Type

                  Case File Document Invi
                  Chain-of-Custody Reco
                  Shipping Manifests
                  Sample Tags
                  SMO Inorganics Tra
                  Inorganics Analys
                  Analysts'  Notebo
                  ICP and AA Instr
                  etc.
5.5
SHIPPING DAT.
*This number is to be recorded on eacfo s
5.4   STORAGE OF EPA FI

5.4.1   The Contractor/shall marital
location.
                                               documents in a secure
5.5.1   The Contracto^xshal^dootiment shipment of deliverables packages to
the recipients.  These sfripments\require custody seals on the containers
placed such thatthej_cannotNae opened without damaging or breaking the seal.
The Contractors-shall dotaqient wfraj^was^ent,  to whom, the date, and the method
(carrier) us
5.5.2   TKe
Region 1

5.5.3
and the S
                        ur^ge the CSF deliverable to the appropriate EPA
                           submission.

                            letter for the CSF will be sent to the NEIC
July, 1991
                                                             Page E - 21
-------
Exhibit E
                                                     SOW No.  XXX -  Ambient Air
5.5.4   The Document Control form  is used to document thj
inspection of shipping containers and samples.   The Con*
one (1) original FORM AADCrl for each shipping contaii

5.5.5   The Contractor shall sign and date the airbj
the shipping containers,  record the presence or
their conditions.

5.5.6   The Contractor shall note any problems
the instructions explained in Exhibit B, Samp]

5.5.7   The Contractor shall submit a comple4ec
each SDG package.
                                                             eipt and
                                                            or shall  submit
                                                                     examine
                                                                   seals  and
July, 1991
                                                                   Page E  -  22
-------
Exhibit E
                                                      SOW No.  XXX -  Ambient Air
                                   SECTION 6
                       ANALYTICAL STANDARDS REQUIREMENTS,
      The U.S. Environmental Protection Agency will
reference standards either for direct analytical  me
purpose of traceability.  All contract laboratories/wi
prepare from neat materials, from cylinders  of co
NIST Standard Reference Materials or NIST/EPA ap
material, or purchase from private chemical  sup
necessary to successfully and accurately perform  £he analyses require
protocol.
                                                              y  analytical
                                                              or  for  the
                                                                      to
                                                                    eable  to
                                                                       nee
                                                                           this
6.1   PREPARATION OF CHEMICAL STANDARDS FRC
MATERIAL
                                               iffi NEAT HIGH7 PURITY  BULK
6.1.1   A laboratory may prepare  their  ch«micalN§tahda^ds from neat
materials.  Commercial sources for neat chernioal  standards  pertaining to
analytes listed on the TAL are given  in AppendiitxC  of ci^e "Quality Assurance
Materials Bank: Analytical Reference  Standards,"  Seventh Edition,  January
1988.  Laboratories should obtain the highest  purity pbs^ibleNwhen purchasing
neat chemical standards; s tandards/ptrrcfeaagdat less thanS^j/ purity must be
documented as to why a higher puraty  could not~~Be—obtained.

6.1.2   Neat chemical standards mustxbe\kept r/efrXgeTaeed/when not being used
in the preparation of standard solutions \ Pr/ope^r storage of neat  chemicals is
essential in order to safeguard them  fr$m decomposition.
6.1.3   The purity of a com'
chemical supply house.  S^fnce kna
concentration of solute An
laboratory's responsibility to haVe
the purity of each cocnpouTid is co,
performed, should us/e either
chromatography with/florae ionij
chromatography,
of two or more independent
impurity when weighing nea< mate
is:
                                 can somerunes\be misrepresented  by  a
   edge of p\iri
,uti^n standar
         tical
     detect
                                                  is needed to calculate the
                                                i  is the contract
                                                .cvcumentation ascertaining that
                                                  Purity confirmation, when
                                                ng calorimetry, gas
                                                high performance  liquid
                                  try, or other appropriate techniques.  Use
                                 s is recommended.  The correction factor for
                                 ials in the preparation of solution standards
                             of
                        ire compound
                                         . of pure compound Eq. E-l
                                        / percent purity •,
                                               100
where "ws
of a so]
              of pure compound"  is  that  required to prepare a specific volume
              standard of a snecilfied  concentration.
 6.1.4    Mi^identification of' compounds  occasionally occurs and it is
 possible  that^misi^tieled tfonraound may  be  received from a chemical supply
 house.   It  is the^contrais^/laboratory's  responsibility to have analytical
 documentation confirming  that/ all compounds used in the preparation of
 July,  1991
                                                                    Page  E  -  23
-------
Exhibit E
                                                      SOW No.  XXX -  Ambient Air
solution standards are correctly  identified.   Identification /confirmation,
when performed, should use GC/MS  analysis  on  at  least  tw/5  different  analytical
columns, or other appropriate techniques.
                                                                a specified
6.1.5   Calculate  the weight  of material  to be  weighed out
volume taking into account the purity of  the compourfcl  an^the
concentration.  A second person must verify the accuracy ofthe  calTfcvdations .
Check balances for accuracy with a set of s tandardvWights .  All>«eighb
should be performed on an analytical balance to
verified by a second person.  The solvent used /to
be compatible with the protocol in which  the sta
solute should be soluble, stable, and nonreaotiv
case of a multicomponent solution, the compone
other.
                                                    .nearest 0.1 mg  at
                                                   dissolve the solute  si
                                                   ird is to be used; the
                                                  with tKevjsolvent.  In the
                                                s must /notreact with  each
6.1.6   Transfer the solute to a volume trhxflaskxa/d  dilute  to  the  specified
solution volume with solvent after ensuring dr&solution of the solute  in  the
solvent.  Sonication or warming may be performedco pronto^e dissolution of  the
solute.  This solution is to be called the primary sfcandard^and  all  subsequent
dilutions must be traceable back to the primary standarc
                                                  yd anc
6.1.7   Log notebooks are to be k
subsequent dilutions from the primaXy s^andarTJ-^nd J:he
determining their concentrations are
person.  All solution standards are to\pe
solution standards are to be clearly lab
compound or compounds, concentration, dat
the preparer.

6.2   PREPARATION OF GASEOUS
               dilutions.  All
                 lations for
                ified by a second
^f/ig^rated when not in use.  All
     to the identity of the
prepared, solvent, and initials of
6.2.1 As discussed in
gaseous standards in/a
to a National
or to a NIST/EPA ap'proved
may be purchased in one"
gaseous standards preparat
3.2.  For these alternate
Contractor thr
must be able/to yerTfy—t£iat
certificate/ of/analysis
request.

6.3
                          bit D, Section 1.4>4v^_the Contractor may prepare
                            lie didution system from compressed gases traceable
                           Standards (NIST) sWndard Reference Material (SRM)
                                    Reference Material (CRM).   The components
                          linger/or separate cylinders.  Other methods of
                              are^xiescribed in Exhibit D, Sections 3.1 and
                                   equivalence must be established by the
                           iidit pr-acedur'a.   In either method,  the Contractor
                              ^ stanclarjas are certified.  Manufacturer's
                            t tte retained by the Contractor and presented upon
6.3.1
Contractors pro
                                   S IN SOLUTION

                     analytical Reference standards can be purchased by
                 Lded^thev meet the following criteria.
   6.3.1.1 Labor at orie
   the integrity of  the
                              aintain the following documentation to verify
                              rd solutions they purchase:
July,  1991
                                                                   Page E  -  24
-------
•Exhibit  E
                                                      SOW No. XXX - Ambient Air
       •  Mass spectral identification confirmation of the neat material;

       •  Purity confirmation of the neat material; and
•  Chromat'ographic and quantitative documentatio
  standard was QC checked according to the
                                                          at the solution
   6.3.1.2 The  Contractor must purchase standards
   demonstrated statistically and analytically by
   choice.  One way  this  can be demonstrated is
   solutions; a high standard,  a low standard,
   concentration  (see parts  a and b  below).   The  /Supplier must then
   demonstrate  that  the analytical results  feir phe  high /standard and low
   standard are consistent with the  differe/ce Au theoretical  concentrations.
   This is done by the Student's t-test in/pa/t "d" wj/icb/follows .   If this  is
   achieved, the  supplier must then  demonstrate that/the' concentration of the
   target standard lies midway between  theconc^tr/ticms of the low and high
   standards.   This  is done  by the S tudent^sx^- test irt part  E.   Thus the
   standard is  certified  to  be within 10 percent^of tfie^target concentration.
   6.3.1.3 If the procedure above  is used,  the  supplied
   following have been achieved.
                                                  nust (iocument that the
        Two solutions  of  identical
        independently  from  neat
        must be diluted to  the intend
        standard").  One  aliquot  is  taen
        diluted to a concentration ten
        standard.  This is  called the "hij
        is taken from  the/^econd>solution
        percent less th
        standard";
        Six replicat
        be performe
        standard,
                                          (a total of 18 analyses)  must
                                          low standard,  target,  high
                            rget standard,  high standard;  and
                                                   prepared
                                                    the first solution
                                           tion (the "target
                                             second solution and
                                         greater than the target
                                         .ndard".   One further aliquot
                                           uted to a concentration 10
                                             s is called the "low
        The-mean-and var
        calculated.
                           the six results for each solution must be
                                                    Y6)  /6
                                                    - (6 x Mean)2
                                                                 Eq.  E-2
                                                                      E_3
      T
      eac
      designa
      target, an<
      Additionally,
                           represent the results of the six analyses of
                          if.  the  low,  target,  and high standards  are
                         ''respectively.   The variances of the  low,
                     iar^s  are  designated Vlt V2, and V3,  respectively.
                       Variance,  Vp,  is  calculated.
July, 1991
                                                             Page  E  -  25
-------
Exhibit £
                                                      SOW No.  XXX -  Ambient Air
               VP =

If che square root of Vp is  less  than  one  percen
/10.000 is to be used as the value  of  Vp  in all  '

The test statistic must be calculated:

       TEST STATISTIC  -   |(M3 /l.l) -  (Ml

If the test statistic exceeds 2.13  then
demonstrate a twenty percent difference/becween  the high and low
standards.  In such a case, the standa/ds/are  not/afcseptable.

The test statistic must be calculat

     TEST STATISTIC  =  JM2 - (Mt
                                                                        Eq.  E-4
                                                            M2,  then M22
                                                            quent calculations.
                                                                            E-5
If the test statistic exceeds 2.13,  the  sup
demonstrate that the target standard concentra
high and low standards.  In s;uc_h_ a case,  the  stani
acceptable.

The 95 percent confidence int^rv,
must be calculated:

        INTERVAL FOR LOW STANDARD \-

       INTERVAL FOR

        INTERVAL
                                                                        Eq.  E-6
      These intervals
      supplier has
      percent diffe
      not acceptable^
      quality of the sti
6.4   REQUESTING
                                                            failed  to
                                                                    between the
                                                                e not
                                                            It of  each  standard
                                                                  Eq.  E-7

                                                                  Eq.  E-8

                                                                  Eq.  E-9
                                           Lap  is  observed,  then the
                                          Llity to discriminate  the 10
                                           such a  case,  the  standards are
                             ,  the laboratory  is  responsible  for the
                           nployed for analyses under  this contract.

                                  STANDARDS REPOSITORY
                                                  (2.13)(Vp

                                                 ± (2.13)(Vp

                                                    .13)(Vp
6.4.1   Solucions-^or~~atia4.ytical reference materials can be  ordered  from the
U.S. EPA Ch/mic^a! StandaroVRepesitory, depending on availability.  The
Contractor/carl place an order^ fok standards only after demonstrating  that
these standa/ds are not available\ from commercial vendors either  in solution
or as a Aieacxmaterial.

6.5   DOCUMENTATIOtKQF THE VERIFICATION AND PREPARATION OF  CHEMICAL STANDARDS

6.5.1   It  is  the rs^ponsteili/ty  of each  laboratory  to maintain the necessary
documentation  to show tkat the chemical standards they have used  in the
performance of CLP analysrs-yconform to the requirements previously  listed.
July,  1991
                                                              Page E -  26
-------
Exhibit E
                                                     SOW N'o. XXX  - Ambient Air
Weighing logbooks, calculations, chromatograms, mass spec
prpduced by the laboratory or purchased from chemical
maintained by the' laboratory and may be subject to
inspection visits.  Documentation of standards prepara
be sent to EPA for verification of contract complian
the documentation is supportive of the analytical r
sent to EPA,  such documentation is to be kept on fi
a period of one year.
;a, etc, whether
  houses,  must be
iring on-site
may be required to
 those cases where
       packages
               for
                                                                  Page E -
-------
Exhibit E
                                                      SOW No.  XXX -  Ambient Air
                                                                       ions
                                   SECTION 7

                      METHOD  SPECIFIC  QA/QC  REQUII

7.1   VOLATILES COLLECTED  IN  CANISTERS

   This sections is to outline  the minimum quality/control  (QCXpperl
necessary to satisfy the analytical  requirements^ssyciated withtbe
determination of the volatile organic  target coroooi
using the procedures in Exhibit D, Section 1 fc
canisters.  This section is not intended as  a/comprehensive quality control
document, but rather as a  guide to the specificyQC operations  that must be
considered for volatile analyses using this/meohod.  At/a Minimum, the
laboratory is expected to  address these op/ratfions in/preparing  the quality
assurance plan discussed in Section  2  andAtariaard Operating Procedures
discussed in Section 3.

   The specific QC operations that must be considered foV>5jplatiles analysis
include the following:

   •   Canister Cleaning and Certif

   •   GC/MS Mass Calibration and lo

      GC/MS Initial and Continuing Calfc

      Sample Analysis;

   •   Internal Standard R^sponsjes a

   •   Method Blank Ana

      Performance Ev,

7.1.1 Canister Clean
   7.1.1.1  Prior to the in
   the laborato
   use,  the
   clean the
   cleanliness
            la'
        of any canister in an analytical scheme,
           nliness of the canister.   Before each
veriry-s£hat>the canister is leak-free and shall
  ze a san^/le of humidified zero air to verify
                                  ified clean before initial use as outlined
                                  J2.2.8.   Results documenting initial
                                  brm VII-AAVC, Canister Certification.
   7.1.1.3  Befol
   to the procedure!
   1.2.2.5,  or alterna^J


July, 1991
                             th0 laboratory must clean each canister according
                                e criteria described in Exhibit D, subsection
                                                   Canisters cleaned and
 subsection 1.2.2.6.
                                                                   Page E - 28
-------
 Exhibit E
                                                       SOW No.  XXX -  Ambient Air
    stored more than one month before use must be recleanedthrough  one cycle
   tof the standard three-cycle cleaning procedure; however/Sio subsequent
    analytical  confirmation of cleanliness is required beTor,/ use.

    7.1.1.4  As a  blank check of the canister(s) cleanup procedure,  the final
    humid  zero  air fill of 100% of the canisters must/be analyzed until the
    cleanup system and canisters are proven reliable/as/bvtlinlhL in  Exhibit D
    Section 1.2.

    7.1.1.5  Only  canisters determined to be leak^ft^e according
    procedures  and criteria described in Exhibit/D/Section 1.2.2.7
    used by the laboratory in sampling and a.r\a.Yjsi/s under this SOW.

 7.1.2  GC/MS  Mass  Calibration and Ion Abunda/ce/Pattern$

    7.1.2.1   Before analysis  of samples,  b/anl^s,  or s/andards, the laboratory
    must demonstrate  that  a given GC/MS  system nteets/th/ instrument performance
    check  standard specified  in Exhibit  D,  Se^ionT. 4/5 .4.   The purpose of
    this instrument performance check is  to ensure corWct mass  calibration,
    mass resolution,  and mass  transmission.   This  i^vaccomHished through  the
    analysis  of bromofluorobenzene (BFB).

    7.1.2.2   BFB analysis  (once ev/ry 12  hours~~oTr~e^ch_GC/MS system)  is
    described in detail in  Exhibit\, ^ctiofi^L 4. 5 .4.
   7.1.2.3  The key ions produced durli
   respective ion abundance criteria mi
   Section 1.4.5.4.4.
                                    Lg\he /na/ysis  of  BFB  and  their
                                          'me/t.  as outlined in  Exhibit  D
   7.1.2.4  The documentat
   Instrument Performance Ct
                           me
   ides repor>ting\data on Form IV-AAVC, GC/MS
and\Mass Calibration.
7.1.3 GC/MS Initial C«=
      Compounds
                      f       1        ^\     \ /
                   Lib/ation fir Target^Sqmpounds and System Monitoring
7.1.3.1  Prior &D the^an^aly^
instrument performance
initially calibrated
linearity of response uti]
compound staiKlardsT
                             mil
   7.1.3.2
   compounds
   as des/ri
                standards are
                    given in
  /            —
  >f samples and required blanks,  and after
   have been met, the GC/MS system must be
     of five concentrations to determine the
    jxget compound and system monitoring
                       ions\of the initial standards for volatile target
                     monitoring compounds are 2, 5, 10, 20, and 100 ppbv,
                           Section 1.4.4.3.2.
                            o be analyzed according to the procedures and
                           ixhibit D,  Part 1A, Section 4.6.
July, 1991
                                                                   Page E - 29
-------
Exhibit E
                                                      SOW No.  XXX -  Ambient Air
   7.1.3.4  The relative  response factors  (RRFs)  are  dete/miried according to
   the procedures  in Exhibit D, Section 1.4.6.4,  using  the Assignment of
   internal standards to  target compounds  and system  monitoring compounds
   given in Exhibit D, Section 1.4.3.3.3,  and Tables  ]/anoS2^.   The
   documentation includes reporting data on Form  V-A#VC./
   7.1.3.5  The calibration of the GC/MS is evali
   magnitude and stability of the relative respoi
   target compound and system monitoring compour
   compound in the initial calibration and the  '
   deviation (%RSD) across all five points
   Exhibit D,  Section 1.4.6.4.4.
                                                   fed/on  the
                                                     factors
                                                    'The minimum  RRF otxeact
                                                   Sent relative  standard
                                                     the Criteria  given in
   7.1.3.6  The documentation includes repyo'rt^ng data.,
   data system printout for the analysis
   the mass spectrum of each target compounoXand

7.1.4 GC/MS Continuing Calibration for Target Cc
      Compounds
                                                          rorm V-AAVC,  a  GC/MS
                                                         Lbration standard,  and
                                                        monitoring  compound.
                                                                   Monitoring
   7.1.4.1  Once the GC/MS system
   verified each twelve (12) hour
                                   las been
:ed,  the
                                              for each
 .ibration must be
system.
   7.1.4.2  The standard is to be analyze"*! accofrdidg to^tKe procedures  and  at
   the frequency given in Exhibit D, Seb±io\i i. 4A,  using Form V-AAVC to
   report results.

   7.1.4.3  The continuing/c'aliEr^i.on of thX^GC)cause\the quantitative determination of volatile
   compound/ by7these procettures\is based on the use of internal standards
   added immediately prior to\analysis.

   7.1.5/2  Ttve specific compounds! used as internal standards are given  in
              Section 1.4.4.3^3. /The concentration of each internal standard
   in the samp-le ana^zed by-GC/MS must be 10 ppbv.

   7.1.5.3  The retention cime/and the selected ion current profile  (SICP)  of
   each internal standabi.mus/t be monitored for all analyses.
July, 1991
                                                                    Page  E  -  30
-------
Exhibit E
                               SOW No.  XXX - Ambient Air
   7.1.5.4  The area response of each  internal  standard f?£m the SICP and the
  .retention time of the internal standard are  evaluated/foy stability,
   according to the procedures in Exhibit D,  Section l-A.6/4.6.   The area of
   the internal standard in a sample must not vary by .mores  than  a factor ±40
   percent from the area of the same internal standard  iz( the associated
   continuing calibration standard.  Likewise,  the yetenticJTL time of an
   internal standard must be within ±0.50 minutes /X 3Q/s^aconds>vof its
   retention time in the continuing calibration standard. ^"I^ternaS,^standard
   areas and retention times are reported on  Forni Vy-AAVC.
7.1.6 Sample Analysis

   7.1.6.1  The GC/MS must be set up per re
   1.4.5 and meet BFB instrument performan

   7.1.6.2  The internal standard must b
   Exhibit D, Section 1.4.6.4.

   7.1.6.3  Guidelines for qualitative verifica
   in Exhibit D,  Section 1.4.8, and outlined belowT
                                   Ixhibit  D,  Section
                                   bration criteria.
                                 .centration outlined in
                                  be met as  discussed
      7.1.6.3.1    All ions preseEft^Trr-eheL^tandard mass s>e/tra at a.relative
      intensity greater than 10 percent  (mostaDTmdaat_j.on  in the spectrum
      equals 100 percent) must be^presfint~^m--the sample spectrum.

      7.1.6.3.2    The relative intertsltres c/f i/bns must agree within ±20
      percent between the standard-and^sampie sfpectra as specified in Exhibit
      D,  Section 1.4.8.1.  (Example:  For. an ion with an abundance of 50
      percent in the standaj^-s^ectra, the\cor^esponding sample abundance must
      be between 30 and 1/Q percem
      7.1.6.3.3    lo
      present in the
      the analyst makin
      favor false posi
      must be reported
      report the actu
           .atvTCr^p£rcent\ifi the sample spectrum but not
           trum mustNl^econsidered and accounted for by
  the comparirsonNxThe Aerification process should
ive.  Al/t cj&mpounds^^mWting the identification criteria
wtth their/spectra.  For all compounds below the CRQL
 valuVtoAlowed by a "J", e.g., "3J."
   7.1.6.4  Guidelines for
   Exhibit D, xS^ctionTTr4^8 .2 a
      7.1
                   /e identification as presented  in
                 led below:
        ensities of major ions in the reference
      tlian 10 percent of the most abundant ion) should
          ectrum.
                   The relative Intensities of the major  ions should agree
      witnsto+20^>ercent.  (pcample:  For an ion with an  abundance of  50
      percent^af the^standa/d spectra, the corresponding  sample ion abundance
      must be between 30x4Zid 1/Q percent.)
July, 1991
                                             Page  E  -  31
-------
Exhibit E
                                                      SOW No. XXX - Ambient Air
      7.1.6.4.3    Molecular  ions  present in reference s/ec^ura should be
      present in.sample spectrum.

      7.1.6.4.4-    Ions present  in the  sample spectrum butNwt in the
      reference spectrum should  be reviewed for posslblexbackb?Qund
      contamination of presence  of coeluting compounds

      7.1.6.4.5    Ions present  in the  referenca^Wctrum but not^io the"
      sample spectrum should be  reviewed  for possible  subtraction from\th«
      sample spectrum because of background cofcta/ination or  coeluting
      compounds.  Data system library reduction /rograms/vcan  sometimes create
      these discrepancies.

   7.1.6.5    Results are reported on Fond  I-^AVC.  othe/ documentation
   includes Form V-AAVC and VI-AAVC, a  G(&MS dkta  sVste/n  printout for the
   analysis of the volatile calibration standard/"arid /the mass  spectrum of
   each target compound and system monitoring cbnipounc

7.1.7 Method Blank Analysis

   7.1.7.1  A method blank is a Wlume  of humtti—aaro_air  (air with  no
   detectable levels of any analyse o$^£trt»cest) thaT~IS-caarried through the
   entire analytical procedure.   ThX^i^volum^mu^t^-ke^ejjual to the  volume of
   samples associated with the blankX  THe purposfe of a method  blank  is  to
   determine the levels of contamination^ as^yci^ted with  the  processing  and
   analysis of samples.
   7.1.7.2    For volatile
   every 12 hours on eac)
   1.4.6.6.
                       GC
analy^s^s, a metftod Mank must be analyzed once
    system, as required in Exhibit D, Section
7.1.7.3    For the/ p
analysis must result/in no
in Exhibit D, Section
                          oses o:
                                                 an acceptable method blank
                                                 or above the CRQL as outlined
   7.1.7.4    If a methdoSsblank Exceeds the limits for contamination above,
   the Contractor must consrder thV-^nalytical system out of control.  The
   source of the-^ontaSttination flru^t be^jnvestigated and appropriate corrective
   actions taken arid^documen^ed before further sample analysis proceeds.  All
   samples ptocjarssed wiSh^a method blahic that is out of control must be
   reanalyzfed^t no additional &ost to the agency.  The laboratory manager or
   his de/ign4e must address\rob\lems and solutions in the SDG Narrative
   (Exhi)
   7.1.7.
   described
   Form III-AAVC^Methoc
   analysis are reposed
                                must be assigned to each method blank, as
                             'on 3.1.  This EPA sample number is listed on
                            'ummary, and the results of the method blank
                           rm I-AAVC under this unique EPA sample number.
July, 1991
                                                                Page E  -  32
-------
Exhibit E
                     SOW No. XXX  - Ambient Air
7.L.8 Performance Evaluation  (PE) Samples

   7.1.8.1    Performance and method evaluation  samples Are/intended to assist
   the Agency in monitoring Contractor and method performance.   The laboratory
   will not be Informed as to which compounds are conp4ir\ed in the PE samples
   or the concentrations.
   7.1.8.2    The laboratory shall extract, analyz
   (Form I-AAVC) o- the PE sample once per sampl
   available.

   7.1.8.3    The laboratory will receive PE
   the Agency.  The samples will come with
   extraction procedure required for the PE;

   7.1.8.4    Each laboratory shall extr
   using the procedure described in Exhi
   7.1.8.5    The laboratory must meet  the
   acceptance criteria:
           fol
                                    results
                 Les in SUMMA® canisters from
                        Concerning the
 te the PE sample
.4.

sample technical
      7.1.8.5.1    The PE sample mu"3t-be__analyzed on  a  GC^MS/sys tern meeting
      the BFB tuning, initial calibration,  an3~~tro»tiiiuing calibration
      technical acceptance criteria  atvEhe—frequency  described in Exhibit D,
      Sections 1.4.5 to 1.4.6.
      7.1.8.5.2    The PE sample must
      to Exhibit D, Section 1.4.6.
      The PE sample must
      meets the blank te/fhni
  id and analyzed with a method blank that
acceptance cr\teri
   •  The percent recover
      must be within
      5.

7.2   VOLATILES CO
             acped and concentrated according
                  compounds in the PE Sample
             accuracy, as outlined in Section
   This section purpose  is  £bxoutrtiafi  the  minimum quality control  (QC)
operations necas^ary^tS^aatisfy^ehe  ana-lytical  requirements  associated  with
the determinaytfLonaf__£he volatile  otgaim:  compounds  listed in Exhibit C,  using
the procedures in  ExhibiTx^D for  samples  of ambient air  captured on Tenax®.
This secticm Ls not  intended. as\a  comprehensive quality control document, but
rather as/a guide  to  the specific.  QC operations that must be addressed  during
analysis/of //olatiles using this taethod.   The  laboratory is  expected to
address^Fhese^-oDerations in preparing  the  quality assurance  plan and Standard
Operatingl^rocemlKes  discusseid in  Sections 2 and 3.

   These operatior^ inctude/thss  following:
July,  1991
                                   Page E  - 33
-------
Exhibit E
                                                     SOW No.  XXX - Ambient Air
      Testing and Spiking of Tenax® cartridges;

   •  GC/MS Instrument Performance Check and  Ion Abum

      GC/MS Initial and Continuing Calibration;

      Internal Marker and Surrogate Standards and

      Method Blank Analysis;

      System Monitoring Compound Recoveries;

      Performance Evaluation (PE) Samples;

7.2.1  Testing and Spiking of Tenax®  Car
                                         \  >y  ,
   7.2.1.1    As part of the procedure  for  preparing 'JJenax® cartridges for
   sampling and subsequent analysis  (see Section^&^S. 5Kxthe laboratory is
   required to analyze by GC/MS or FID  one  cartridge^romsach batch of
   prepared Tenax® cartridges, and confirm  that total V£)Ss  aryless than 10
   ng.  If the total VOCs exceed Ij2r~ng7^the~-eivtire batch oT^Lenax® cartridges
   shall be rejected.
   7.2.1.2    For acceptable batches\t)^laboJa.tdrf~i3~-a¥so required to spike
   each cartridge with 300 ng  of  PTI,\.2^icAloi!obenze-ne-d^, benzene-d6
   chlorobenzene-d5, and l,4-dichlorobenXeneVd4//as initial and final markers
   and surrogate standards, respectively.
7.2.2 GC/MS Performance
      Patterns

   7.2.2.1    Prior t
   samples, blanks,
   GC/MS system mee
   D, Sections 2.3.*3xand
   check is to ensure
   transmission.  This is
   bromofluo-robenzejne__/BFB)
                                      Mass Spectrometer and Ion Abundance
                                                .ection activities involving
                                                ~"  to establish that a given
                                                  criteria specified in Exhibit
                                    .e purpose of this instrument performance
                                    calibration, mass resolution, and mass
                                        through the analysis of
    7.2.2.2  /Th
    each GC/MS
    2.3.4.
    7.2.2.4    The
    bar graph spectrum


 July, 1991
                                            analysis  (once every  12 hours  on
                                    in detail  in  Exhibit  D, Sections 2.3.3  and
                                   ;d during the analysis of BFB and their
                                   ia are given in Exhibit D, Section 2, Table
                                 includes  Form V-AAVT and a mass listing and
                               analysis.


                                                   ~~~              Page E - 3'
-------
Exhibit E
                                                      SOW No.  XXX - Ambient Air
7.2.3 Initial Calibration of GC/MS for Target  Compounds  and System Monitoring
      Compounds                                           /^
   7.2.3.1    Prior to the analysis of samples and re
   instrument performance criteria have been met, th
   initially calibrated utilizing target compound (
   monitoring compound standards.

   7.2.3.2    Both external and internal calibra/i
   Exhibit D, Sections 2.3.4.1 and 2.3.4.2 resp

7.2.4 Internal Standard Calibration Procedur

   7.2.4.1    The GC/MS may be calibrated
   Tenax® tubes,  and calculating concentr
   factor (RRF) method.
                                                          zd blanks  and after
                                                         /MS system  must be
                                                              4.)  and system
   7.2.4.2    Calibration standards contain"*
   interest are prepared as outlined in Exhibi
   2.4.3.
   7.2.4.3    The Tenax® tubes ar
   internal markers and surrogat
   2.3.6.
   7.2.4.4    The tubes are then ana
   7.2.4.5    Relative response factors
   Exhibit D, Section 2.3.4.2.
                                                                       ibed in
                                                          ndards  spiked onto
                                                          lative response
   7.2.4.6    The docum
   printout for the
   mass spectrum of

7.2.5 GC/MS Contin'
      Compounds

   7.2.5.1    Once the
   be verified each twelve
   7.2.5.2
   in Exhil
              The
                                                      get compounds of
                                                          s 2.4.1, 2.4.2  or
                                               with knowrNco^centrations of
                                                    ibed in Exhibit D, Section
                                                 ribed in Exhibit D, Section 2.3.5

                                               are calculated as described in
                                              VII^AAVT, a GC/MS data system
                                                  .bration standard, and the
                                             system monitoring compound.
andar
                 Sectio
                 Compounds  and  System Monitoring


      has been calibrated,  the calibration must
       j:ime period  for  each GC/MS  system.

 to be^anadyzed according to the procedures given
L and at the  frequency  given in Section 2.3.5.1.
   7.2.5.X3  / The continuing\caiibration of the GC/MS system is evaluated on
   the tiasiA of the magnitude\ of\the response factors and the percent
   diffcerencexbetween the average RRF of each compound from the initial
   calibration and the RRF of that compound in the continuing calibration
   standard !\Ihe mismnum ressponse factors of each compound in the continuing
   calibration alxi the^p-erjcent? difference must meet the criteria given in
July, 1991
                                                                   Page E - 35
-------
Exhibit E
                     SOW No.  XXX - Ambient Air
   Exhibit D, Sections 2.3.4.1.6 and  Section 2.3.4.2.   AlAow4nce is made for
   any two volatile compounds that  fail  to  meet  these  c]rite. and^fche
                    monitoring compound.

                   Retention Times
                       A
                       rdsr  in all calibration
                        ;tsion of reliable
                        ation of volatile
                     of. internal standards
   7.2.6.2    The specific compounds used  as  internal
   standards are given in Exhibit D_Section  2.2.3.6.
   and surrogate standard is spikac on~tn~e—^^oaax® cartridge^
   approximately 300 ng.
                              and surrogate
                               ernal marker
                             't a level of
   7.2.6.3    The retention time and\the\selectee
   of each internal marker and surrogate s-candar,
   analyses.                            \   v  /
                  ion exit-rent  profile  (SICP)
                  must be  monitored for all
   7.2.6.4    The area r
   from the SICP and the /retention
   standard are evaluated
   Exhibit D, Section /. 3y8.  The
   standard in a sample Must not
   the same internal/marker and
   continuing calib/ratofian standard
   internal marker
   retention time in tn~6xcontlm.
   Exhibit D, Section 2.3.
  each internal  marker  and surrogate standard
  .time of  the  internal  marker and surrogate
,bi$iit, accorHin£> to  the  procedures  in
             im^Trnal marker  and surrogate
        more-^-than 40  percent  from the area of
               rd in  the  associated
               the retention time of  an
 tandard must  be within 30 seconds of its
   calibration standard,  as described in
   7.2.6.5    Jtequirements\for anklesis"yDf  samples  when internal marker and
   surrogate/stai«Iar35~Ni^ not\meet  specifications  are given in Exhibit D,
   Section/2.3/10.

   7.2.6/6  / The documentation  includes  Form III-AAVT and the GC/MS data
   system printout for the anajlys^s of  each sample, blank, matrix spike, and
   standard.
 July,  1991
                                   Page E - 36
-------
Exhibit E
                                                      SOW No. XXX - Ambient Air
7.2.7 Method  Blank Analysis
                                                          tube thermally
                                                         entire analytical
   7.2.7.1    A'method blank  is a certified  clean  Tena>
   desorbed with a volume of  helium carried  through  the
   procedure.  The volume of  helium must be  approximateI)/equal  to the  volume
   associated with the blank.  The purpose of  a methcfd blahi is  to determine
   the levels of contamination associated with the /rocfe&sing^and analysis  of
   samples.
   7.2.7.2    A method blank shall be  analyzed
   GC/MS system, as described in detail  in  Exhibit
                                                    'every  12  hours^Qn  eae
                                                   'D, Section 2.3.4.
   7.2.7.3    For the purposes of this protocol/ an
   must contain less than or equal to the Cpnttfact Reqi
   (see Exhibit C) of any single target compound, or
   for total VOCs, whichever is less.
                                                         liable  method blank
                                                            Quantitation Limit
                                                           than  10  ng/cartridge
                                              .mits foj
   7.2.7.4    If a method blank exceeds the
   the Contractor must consider the analytical
   source of the contamination shall be investigat
   corrective actions taken and documented before
   proceeds .   The requirements for,
   in Exhibit D, Section 2.3.8.3.
                                                 Astern
                                                     and
                                                  further s
                                          •sis of associat
contamination above,
 t of control.   The
     ropriate
       le analysis
       mples are given
   7.2.7.5    The documentation inc!l
   and a GC/MS data system printout
                                    £d«X Form IV-ASVT-fat/the blank analysis
                                    f\r t^e a/al/sis of the method blank.

7.2.8 System Monitoring Compound Recoveries
   7.2.8.1    The recover^s of l:he three surrogate compounds (see Exhibit D,
   Section 2.2.3.6) are/alcttla^ed ^f rom the ahalysds of each sample, blank,
   and matrix spike.  The jfurpose\ o4xthev^stem\mo(nitoring compounds is to
   evaluate the performance of thi entire Tenax^Xiesorption GC/MS system.
   Poor purging efficiency, leaks/,  arfoTc^d sp5£s in transfer lines are only a
   few of the potential/causes -blank/
   described in Exhibit D,
                                  compounds are added to each Tenax® tube
                                 and matrix spike,  at the concentration
                                 ^".2.3.6.
               in the quali
              f the recovery
            its,  the
               10'.
                             of theNsystiem monitoring compounds are calculated
                               in Exhibit D,  Section 2.3.8.  The recoveries
                              control limits  given in Exhibit D, Section
                                  iy one system monitoring compound is outside
                                nAist follow the steps outlined in Exhibit D,
   7.2.8.4
   printout for


July, 1991
                             on/includes Form I-AAVT,  and a GC/MS data system
                             of each sample,  blank,  and matrix spike.


                                                           'Page E - 37
-------
Exhibit E
                                               SOW No. XXX  - Ambient  Air
7.2.9 Performance Evaluation (PE) Samples

   7.2.9.1    Performance and method evaluation samples' ar£ intended  to  assist
   the Agency in monitoring Contractor performance.  JZtie laboratory will not
   be informed as to which compounds are contained in the Pt^amples  or  the
   concentrations.
   7.2.9.2    The Laboratory shall extract, anal}
   the PE sample once per sample delivery group.
                                               and report tt
                                              available.
resv
        of
   7.2.9.3    The laboratory will receive PE Camples on Tenax® cartridges  from
   the Agency.   The samples will come with instructions/concerning the
   desorption procedure required for the PE/saaples.  the/Laboratory must  add
   internal markers and surrogate compounds tp the PE/san3^5 rb-t those target
   compounds listed in Exhibit C, Table 1.
   7.2.9.5    The laboratory must
   acceptance criteria as detaile
      7.2.9.5.1    The PE sample must:\be ^analyZed/on a GC/MS system meeting
      the BFB tuning,  initial calibratron,\ana continuing calibration
      technical acceptance criteria at the frequency described in Section
      2.3.5.
7.3
                                               PE sample technical
                                                      .12:
      7.2.9.5.2    The PE/sample mxis
      D, Section 2.3.5.

      7.2.9.5.3    Th
      blank that meel^s
7.2.9.5.4
within acceptable

7.2. 9."5. 5
recent
must b

7.2.
be
5.

SEMIVCJ
                                             .ccording to Section Exhibit
                                            and analyzed with a method
                                          tance criteria.
                                  'overy for each of the surrogates must be
                                   outlined in Exhibit D, Section 2.3.8.3.
                                        .nge between the PE sample and the most
                                         s for each of the surrogate standards
                                  overy for each of the target compounds  must
                                  >n and audit accuracy, as outlined  in  Section
   The purpose of this section/is to outline the minimum quality control  (QC)
operations necessary to^satis/ry the analytical requirements associated with
July,  1991
                                                             Page  E  -  38
-------
Exhibit E
                    SOW No. XXX - Ambient Air
the determination of  the semivolatile  organic  compounds  listed  in  Exhibit  C,
using the procedures  in Exhibit D.  This  section  is not /ntended as a
comprehensive quality control document, but rather as a/gufde to the specific
QC operations that must be addressed during analysis
on PUF/XAD-2.  The laboratory is expected to address
preparing the quality assurance plan and  Standard 0
discussed in Sections 2 and 3.
                                     captured
                        e operations in
                            rocedures
   These operations include the following:

      Testing and Spiking of PUF/XAD-2 cartridges/

      GC/MS Instrument Performance Check anjz

      GC/MS Initial and Continuing Calibr^

   •  Internal Standards, Surrogate Compl

   •  Laboratory Method Blank Analysis;

   •  Surrogate Compound Recoveries; and

      Performance Evaluation (PEj

7.3.1  Testing and Spiking of PUF/
   7.3.1.1    As part of the procedureNfor^
   sampling and subsequent analysis, the\
   GC/MS or GC/ECD one car
   cartridges from each
   that the total level/of
   PUF/XAD-2 sandwich),
   10 /ig, the entire
              aring PUF/XAD-2  cartridges  for
                   is  required to  analyze by
               whichever  is  greater,  of the
                 2  cartridges,  and confirm
                 idge  assembly (filter  and
                 total semivolatiles exceed
            or cleaned until acceptable.
   7.3.1.2    For
   each cartridge
   3.

7.3.2 GC/MS Performance Chec"
      Pattern
July, 1991
            jratory  is  also  required to  spike
:ompounds  as  discussed  in  Exhibit  D,  Section
    Mass  Spectrometer  and  Ion Abundance
                                  any data collection activities involving QC
                               ^sary to establish that a given GC/MS system
                                ice criteria specified in Exhibit D, Section
                                 nent performance check is to ensure correct
                                :ion, and mass transmission.   This is
                               l/ysis of decafluorotriphenylphosphine (DFTPP) .
                                  Page  E -  39
-------
Exhibit E
                                                      SOW No.  XXX -  Ambient Air
   7.3.2.2    The required frequency  of  DFTPP  analysis  Q6nce< every 12  hours on
   each GC/MS system) is described  in detail  in Exhibit^!), /Sections 3.
                                                           ^DFTPP  and  their
                                                              Section  3,
   7.3.2.3    The key ions produced during the analy
   respective ion abundance criteria are given in
   Table D\SV-5.

7.3.3 Initial Calibration of the GC/MS System

   7.3.3.1    Prior to the analysis of samples/and required
   instrument performance criteria have been/met/ the GC/MS system must be
   initially calibrated using calibration s^andfirds con/£a^tning the target
   compounds, surrogates, and internal star
   7.3.3.2  The detailed procedure is gi;

   7.3.3.3    The GC/MS is calibrated by
   PUF/XAD-2 cartridge assemblies, and calculating
   relative response factor (RRF) method.

   7.3.3.4    Calibration standar
   interest are prepared as outli
   the PUF/XAD-2 cartridges.
                                                        ,  Section 3.

                                                      ridards spiked onto the
                                                         trations by the
                                                   target compounds of
                                                           3 and spiked onto
   7.3.3.5    The PUF/XAD-2 cartridges
   internal standards and surrogate
   Section 3.

   7.3.3.6    The cartri
   Section 3.

   7.3.3.7    Relati
   Exhibit D,  Secti
                                                d with known concentrations of
                                               s described in Exhibit D,
                                               ak described in Exhibit D,

                                                v
                                                .re calculated as described in
   7.3.3.8    The
   printout for the ana1
   the mass spectrum of

7.3.4 GC/MS C,

   7.3.4.1
   be veri^fi
   7.3.4.3    The c^antinu
   the basis of the ma


July, 1991
                                  Deludes Form III-AASV,  a GC/MS data system
                                feach semivolatile calibration standard,  and
                                    and surrogate compound.
                               stem has been calibrated,  the calibration must
                              i \iour time period for each GC/MS system.
                                  e analyzed according to the procedures given
                                 t the frequency given in Exhibit D, Section
                             Calibration of the GC/MS system is evaluated on
                              of the response factors and the percent


                                                                   Page E -  40
-------
Exhibit E
                                                     SOW No. XXX  -  Ambient  Air
                                                                data system
                                                                       and the
   difference between the average RRF of each compound from the  initial
  „calibration and the RRF of that compound in the contiriuiife calibration
   standard.  The'minimum response factors of each compcnmd/with minimum RRFs
   in the continuing calibration and the percent diff&/&nikebKon the PUF/XAD-2
   cartridge at the level specified in Exhibit D,  Section 3.
   7.3.5.3    The retention time 
-------
Exhibit E
                                                      SOW No.  XXX - Ambient Air
   7.3.6.3    For  the  purposes  of this protocol,  an acceptable laboratory
   method blank must contain  less than or equal to the Gbnt/act Required
   Quantitation Limit  (see  Exhibit C)  of any single target/compound,  or less
   than 10 Mg/cartridge  for total semivolatiles,  whic#ever\is  less.
                                                    the>
                                                   ier/the  anal
                                                       ;t be
7.3.6.4    If a  laboratory method blank exceeds
contamination above,  the  Contractor  shall
out of control.  The  source  of  the contaminati
appropriate corrective actions  taken and documented before furthei
analysis proceeds.  The requirements for reXna}/ysis of associated san
are given in Exhibit  D, Section 3.

7.3.6.5    The documentation includes Fo/m .ZV-AASV  for /fche blank analysis
and a GC/MS data system printout  for tbfe a/alysis ft tzhe  laboratory method
blank.                                 f   C       r  r
7.3.7 Surrogate Compound Recoveries
7.3.7.1    The recoveries of  the  surrogate  compound* are^salculated from
the analysis of each sample and Man^ The purpose orxrtie^surrogate
                                :forman5e-~e€-£he  entire wF/XAD-2  acrtridge
                                               leaks-;—and cold  spots in
                                                 auses of poor recovery  of
   compounds is to evaluate the p
   and GC/MS system.  Poor extrac
   transfer lines are only a few
   these compounds.
Lorn
 ^th«
                                       \
   7.3.7.2  The surrogate compounds are
   assembly prepared for sampling at the
   D, Section 3.
                                        pncei
               each PUF/XAD-2 cartridge
            itrations  described in Exhibit
   7.3.7.3    The recovafrieX of^she \surrogate kompdunds are calculated
   according to the procedures injExKibit^SL Sec\Zon 3.  The recoveries must
   be within the qua!/ty/control Iimits-^giveri^ia Exhibit D, Section 3.  If the
   recovery of any oj(e ^rrogate/compounoNisou^side these limits, the
   Contractor shall/ follow the /tej/s outlinedin Exhibit D, Section 3.
   7.3.7.4    The documentation /ncludes Form I-AASV, and a GC/MS data system
   printout for the analysi^of eksh sample and blank.

7.3.8 Performarlce Evaluation^ (PE)
   7.3.8.1 /  Performance
   the Agancy/in monitoring
   be informed as to which co
   concentrations .
                           method evaluation samples are intended to assist
                           mtisactor performance.  The laboratory will not
                            lounds are contained in the PE samples or the
   7 . 3 .8 .2
   the PE sampi
                  ^oratoryyshall extract, analyze, and report the results  of
              pnce >er sainpl^fe delivery group, if available.
July, 1991
                                                                Page  E  -  42
-------
Exhibit E
                                                SOU No. XXX - Ambient Air
   7.3.8.3    The laboratory will receive  PE  samples  on PyUF/XAD-2 cartridges
  .from the Agency.   The samples will come with  instruction^ concerning the
   extraction procedure required for the PE samples.   The  ^laboratory shall add
   internal and surrogate compounds to  the PE sample,/following procedures in
   Exhibit D, Section 2.3.6.

   7.3.8.4    Each laboratory shall extract and  co
   using the procedure described in Exhibit D, Seit
   semivolatile target compounds listed in Exhibit
                                               /^^
   7.3.8.5    The laboratory shall meet the fc
   acceptance criteria as detailed in Exhibij

      7.3.8.5.1    The PE sample must be aj
      the DFTPP tuning and initial calibr^
      technical acceptance criteria at
      Section 3.

      7.3.8.5.2    The PE sample must be desorb>
      D, Section 3.
      7.3.8.5.3    The PE sample niust~
      blank that meets the blank(technical accept
                                          losing PE  sample  techm
                                            Section  3:
7.4
7.3.8.5.6    Th.
be within repl^
D, Section 3.

INORGANICS
                                                        system meeting
                                                    ing calibration
                                                 fecribed in Exhibit D,
                                                       to  Section Exhibit
                                                        d with a method
                                                   iteria.
      7.3.8.5.4    The percent reco
      within acceptable windows as
                                        ,ch/oiT~Ehe—Surrogates must  be
                                          Ixhibit D, Section 3.
      7.3.8.5.5    The area response chaWe between the PE sample and the most
      recent calibration standard analysisVforveach of the surrogate standards
      must be within 40
                                            ea^ and the SjOPs/discussed in Section 3.
      These operations
                         the following:
July, 1991
                                                             Page  E  - 43
-------
Exhibit  E
                                                      SOW No.  XXX -  Ambient Air
                                                            Calibration
                                                                           and
       Instrument  Calibration;

    •   Initial Calibration Verification  (ICV) and Conti/fuii
       Verification  (CCV);

    •   CROL Standards;

    •   Linear Range  Standard  (LRS) Analyses;

    •   Initial Calibration Blank (ICB), Continuing/Calibration Blank  (CCl
       Preparation Blank  (PB) Analyses;

    •   Interference  Check Sample (ICS) Analy/

       Spike Sample  Analyses;

    •  Analytical Spike Sample Analyses;

      Duplicate Sample Analyses;

      Laboratory Control Sample (

      Instrument Detection Limit (

      Interelement Corrections for ICP\

7.4.1 Instrument Calibration

   7.4.1.1  Guidelines for instrum
   Inorganics,  Section if. 3
   inscrument shall be
   the instrument is set
   7.4.1.2  The ca
   matrix and at tti
   sample preparation
   and Section 4.5.4 and

7.4.2   Initi

   7.4.2.1
   calibr
   do cum
   resu
   Table
   ins trume
   the ICV sha
   analysis.
July, 1991
                                              ion\are outlined in Exhibit D,
                                                  r 4.5.5.1 for GFAA.   Each
                                                  :ery 24 hours and each time
                                            be prepared using the same type of
                              snt/ation as the preparation blank, following
                                /outlined in Exhibit D,  Section 4.3.6 for ICP
                                ^ vGFAA.
                                         (ICV)
                              each of the ICP and GFAA systems have been
                                   initial calibration shall be verified and
                                  the analysis of EPA ICV solution(s).   When
                                  :he control limits in Exhibit D,  Section 4,
                                  1 be terminated, the problem corrected, the
                                 :he calibration reverified.   For ICP and GFAA,
                            reported at each wavelength and mass used for
                                                                   Page E - 44
-------
Exhibit E
                      SOW No. XXX - Ambient Air
   7.4.2.2  If the ICVs are not available from EPA, or a  certified  solution  of
  .an analyte is not available from any source, analyses/shall be conducted  on
   an independent 'standard, at a concentration other thai*  that used  for regular
   instrument calibration, but within the calibration /ange.  An independent
   standard is defined as a standard composed of the .analqrtes from  a different
   source than those used in the standards for the instrument, calibration.

7.4.3   Continuing Calibration Verification  (CCV)

   7.4.3.1  To insure calibration accuracy durii
   required in Exhibit D, Section 4.3.7.3 for /CP/and Section 4.5.5.3"
   GFAA, the laboratory shall analyze a CCV aolutaon, either prepared by  EPA
   or Contractor-prepared, for every wavelength/used foifvanalysis at the
   beginning of the run and after the last /analytical pampLe.

   7.4.3.2  Each CCV analyzed shall reflect fel].e conditions of analysis of all
   associated analytical samples (the preseding^lO/anaiytical samples or  the
   preceding analytical samples up to the pre-^ious CC#).  The duration of
   analysis, rinses, and other related operatiorfcsvthat^may affect the CCV
   measured result may not apply to the CCV to a greater  extent than the
   extent applied to the associated analytical samples/"
   7.4.3.3  If the deviation of
   specified in Exhibit D, Section"
   terminated, the problem corrected^ a^\d the yCCV,
   the reanalysis yields a CCV value «ith\n pont?
   10 analytical samples or all analyt
   acceptable calibration verification shall
   affected.  Otherwise the^ias^rument shal
   verified, and the affected ana
   ftical sample!
        the control limits
-3, the analysis shall be
          ed only once.  If
 ol limits, then the preceding
es analyzed since the last
analyzed for the analytes
recalibrated, the calibration
 rerun.
7.4.4   CRQL Standards/  /      \
   7.4.4.1  To veri: _
   CRQL standard at/tw«(times ttie
   lower.  The CRQbxstanSard shaLJ
   each sample analysis^run or a/n
   shift, whichever is
   Exhibit D, Section4.3.7.
   standard mu&€be run^or ever1
7.4.5
July,  1991
                 :he Contractor shall analyze a
               'times the IDL, whichever is
    be analyzed at the beginning and end of
  minimum of twice per eight hour working
   nt, but not before ICV, as outlined in
       and Section 4.5.5.4 for GFAA.  This
         ngth used for analysis.
   7.4.4.2 /Re
   percent/of
   the analy,
   samples
lysis of the CRQL standard must be within ±10
  each wavelength used for analysis.  If not,
  ed, the problem corrected, and the analytical
   le CRI reanalyzed.

  lysis
                                    Page E - 45
-------
Exhibit E
                                                      SOW No.  XXX -  Ambient Air
   7.4.5.1  A Linear range verification check standard  n&SV shall  be  analyzed
   .at the beginning and end of each sample analysis run/ OT/a minimum  of twice
   per eight hour'working .shift, whichever is more frequer(t,  but  not before
   ICV, as outlined in Exhibit D, Section 4.3.7.5 for'ICIKand Section  4.5.5.5
   for GFAA.  This standard must be run for every waVel^ejigthSused for
   analysis.
                                                                   percent  of
7.4.5.2  Results for the analysis of the LRS i&isjz'be within ^1
the true value for each wavelength used f or/ana^ys is .   If not,
must be terminated and successive dilutions/of/the standard must be'
reanalyzed until the control limits are met. /The concentration of  this
standard that meets the control limits is/th/ upper /iMt of  the instrument
linear range beyond which results canno/be/reporte/G u^der this contract
without dilution of the analytical sample,
7.4.6   Initial and Continuing Calibration^
                                                    irses
   7.4.6.1  A calibration blank must be analyzed
   analysis immediately after every initial and
verification, at a frequency of.
run, whichever is more frequent
and 4.3.7.7 for ICP and Sectios
must be analyzed at the beginni
sample .
            eacRxwavelength used for
        continuingcalibration
                      rs during the
                      Sections 4.3.7.(
                    GFAA.  The blank
the^ruiy and__af ter /6he last analytical
                                       ercent of every
   7.4.6.2  If the absolute value of thexblYnk/result exceeds the CRQL
   (Exhibit C) ,  analysis must be terminated,  toe problem corrected, and the
   continuing calibration
   CCB with an absolute v-alue beloV the CRQL\al
   since the last accepytablecaMbration blankXm
   the instrument must/be/recalibYatr^d7^h< calr
   affected analytical sample(s) yrer
                                                If the reanalysis yields a
                                               analytical samples analyzed
                                                 be reanalyzed.  Otherwise,
                                               •ation verified, and the
   7.4.6.3  Each analytical sample/must be bracketed by two consecutive CCBs
   that have been afta^yzea^s^itnin/two hours of each other with no more than
   ten analytical samplfesrun between the CCBs.   The absolute value for each
   analyte in these two CC&s^mustNfall below the CRQL or IDL, whichever is
   greater.
7.4.7
                               Analyst

                                 eagent blank) consisting of reagent water
                                  reparation and analysis procedure must be
                                    SDG or with each batch of samples
                                 requent),  as outlined in Exhibit D, Section
                                '.5.5.7 for GFAA.
July, 1991
                                                                Page E - 46
-------
Exhibit E
                                                      SOW No.  XXX - Ambient Air
   7.4.7.2  The first batch of samples  in  an  SDG  shall to
  ,one, the second batch of samples  to  PB  two,  etc.   Eae
   the results of'all the PB analyses associated  with t

   7.4.7.3  The PB is to be reported for each SDG an
   ascertain whether sample concentrations  reflect
   following manner:

      7.4.7.3.1    If the absolute value of the
      less than or equal to the CRQL (Exhibit C)
      results is performed.
                                                           assigned to PB
                                                           kage must contain
                                                           ples in that SDG.

                                                         in all analyses to
                                                          :ion in the
      7.4.7.3.2    If any analyte concentration/in  the
      all associated samples containing le
      must be redigested and reanalyzed
      concentration not to be corrected for &h.e bla:
                                                        is  above  the CRQL,
                                            .an lOx ;fhe /blank concentration
                                                   te/  The  sample
                                                      lue.
                                          that  ana]
      7.4.7.3.3    If an analyte concentratibti  in the
      CRQL, all samples with reported analyte values
      associated with the blank must be redigested
                                                   'PB  is below  the  negative
                                                     ^w lOx  CRQL and
                                                    reanalyzed.
      7.4.7.3.5
                The values for
                                         it be recorded
/Mg/L.
7.4.8   Interference Check Sample\naWs~Is~
   7.4.8.1  To verify interelement
   Contractor must analyze and report
   Sample (ICS).   The ICS must be analyzed at,
   analysis run or a minimum—ef^twice per eiglvl
   is more frequent, but/not befo
   The ICP ICS must be obtaifieUsfrofy EPA (EMSt^
   according to the instructions
                                               correction factors,  the
                                             s for an Interference  Check
                                             e beginning and end of each
                                             hour working shift, whichever
                                              Exhibit D, Section 4.3.7.9).
                                            LV>>, if available, and  analyzed
                                                ICS.
                        pOt€
   7.4.8.2  The ICS donslst of
   Solution A must
   contain both analytes
   analyzing both solvte^ons
   wavelengths used for e
                            ite
                           ns
                          ana
                                 "6luti4ythe true value for the analytes
                              terminate the analysis, correct the problem,
                              .d reanalyze the analytical samples analyzed
                                If true values for analytes contained  in
                                not supplied with the ICS, the mean
                               must be determined by initially analyzing
                              petitively for the particular analytes.  This
                             de during an analytical run where the results
                            EPA ICS met all contract specifications.
include
recali
since
the
cone"
the ICS
mean deternfioatioitxmust 1/e i
for the previo
          ratie the instrument,
         Che/last acceptable\CSl
       EtlS and analyzed by ICE ai
           att^n for each analyte
July, 1991
                                                                Page E  - 47
-------
Exhibit E
                                                      SOW No. XXX  -  Ambient Air
   Additionally, the result of this initial mean determinatin  is  to  be  used
   as the true value for the lifetime of that  solution  #l.e/, until the
   solution is exhausted)..

7.4.9   Spike Sample Analysis

   7.4.9.1   The spike sample analysis is designed' to/provideX^nforlftation
   about the effect of the sample matrix on the digestion and mea^ureme
   methodology.  The spike is added before the «e?r~b^ the same
with the letter "N".
                                                lin the limits of 75-125
                                            received associated with that
                                                rtical method must be flagged
7.4.10  Analytical Splice Sample
   7.4.10.1  The an
   information abo
   system.  The spi
   analysis.  At least
   group of samples of
   Section 4.3.7

   7.4.10.2
   that is/ch
   be per
   sampl
   results Cannot
   Samp
   analysis^
   sample analyses
July, 1991
                    Leal
                         spit
                                imple
                      effect
                                'the sample"
                   is
                        spike
                    sinffciar
                LS is designed to provide
               natrix on the measurement
  fer the sample has been prepared and prior to
 'sample analysis must be performed on each
   ?e for each SDG, according to Exhibit D,
      an 4.5.5.11 for GFAA.

spike Tactalysis is performed on the same sample
 ate sample analysis, spike calculations must
   of the sample designated as the "original
   .nalysis).  The average of the duplicate
   purpose of determining percent recovery.
  anks cannot be used for spike sample
  t a specific sample be used for the spike
                                                                 Page  E -  48
-------
Exhibit E
                    SOU No.  XXX - Ambient Air
   7.4.10.3  For analytical spike sample analysis, each
   with a concentration equal to 30 percent of the ana
   The sample and spiked sample oust be at the can* dilu
                            ce must be spiked
                            Linear range.
   7.4.10.4  If the spike recovery is not within the IfaitA of 852-1152, a
   second analytical spike must be performed.  If the/sacon&Nanalytical spike
   is out of control, the preparation blank must be /pifcfed^witfcvche same
   spiking solution.  If spiking the blank yields
   control, the. spiking solution oust be prepared
   spiking procedure repeated.  If not, all
   sample and determined by the same analytical
   the latter "E".
                    d must be
7.4.11  Duplicate Sample Analysis

   7.4.11.1  One duplicate sample must be
   for each SDG, as outlined in-Exhibit
   Section 4.5.5.9 for GFAA.  Duplicates canrfc
   results,
                                                     -v
   7.4.11.2  Samples identified as field blanks cannot
   sample analysis.  EPA. may requiygTSrut-tL_Specific
   duplicate sample analysis.  If     x
   the reported values for the sane\el
   duplicate samples oust be run by
                            group of samples
                       .12 for ICP and
                      'ag«d in reporting
                    sample^1
                        are
7.4.12  Laboratory  Control Sample Analy

   7.4.12.1  The Laboratory
   analyte using the same
   procedures employed fj
   Section 4.3.7.12 for/IC!
 7.4.13
July. 1991
ol Sample \LC
   paration.
                                                            :or duplicate
                                                            used for
                                                          used to obtain
                                                          ICP  and GFAA),
                                              must be analyzed for each
                                                 leal methods and QA/QC
                                                  as outlined in Exhibit D,
                                                  GFAA.
7.4.12.2  The EPA-y
the procedures a'
unavailable,  oth'
materials may be
group of samples in a
is more frequent

7.4.12.3
establis
and the
contro
limit
                                                 d and analyzed using each of
                                                d.  If the EPA LCS is
                                   'ssuranca check samples or other certified
                                   must be prepared and analyzed for every
                                    each batch of samples prepared, whichever
        e not within the control limits
   must be terminated,  the problem corrected.
  the LCS prepared again and reanalyzed.  A
  the true value must be used if no control
 s solution.

 ) Sample
                                  Page E - 49
-------
 Exhibit E
                                                      SOW Ho. XXX - Anhient Air
    7.4.13.1  The Performance Evaluation (PE) Sample will assist the Agency in
    monitoring contractor performance.  The laboratory wilVW be informed in
    advance of the analytes in the PE sample or their concentration
    7.4.13.2  The Contractor must prepare, analyze and
    one PE sanple per each SDG, if available, as outli
    3,  Inorganics.
                                                    fep/rt the results of
                                                         ^Exhibit D,  Section
    7.4.13.3  Prepare the PE sample using the proce^u
    preparation section of Section 4,  Exhibit D, a^Lnalyzs the
    using the methods described in Exhibit D for/th> analysis of EPA"
    samples.   All contract required QC must als/ be' met.
    7.4.13.4  The Contractor must demonstra
    analyt*  identification and quantificati
    score  of less than 75  percent,  the Age
    the  following actions:   Show Cause and^
    number of samples  shipped to the  labora
    a.  site visit,  a full data audit,  and/or req
    remedial PE  sample.
                                          ac^eptable/paVformance  for
                                             If  the .Contractor  achieves  a
                                            iy take/bu/is not  limited to
                                                        reduction  of  the
                                                    •ion of sample shipment,
                                                    Aboratory to analyze  a
7.4.14   Instrument Detection Limit

   7.4.14.1 The Instrument Detection
   for each instrument used,  within\30
   analysis and at least quarterly  (e\
   Exhibit D. Section 4.3.7.14 for  ICP*
   must be equal to or less  than CRQLs ()
                                      lination
                                          1	
                                          EDL) (in /ZgTt^ust be determined
                                      lys prlySr »—nhg__s^art of any contract
                                            .en/dar months), as outlined in
                                             m 4.5.5.11 for GFAA.  The IDL
                                             •ecified in Exhibit C.
   7.4.14.2 The IDLs must
   the standard deviations o
   in reagent water) at/a co'nceri
   consecutive measure;
   ware a separate
   by a rinse and/a
   analysis of sep
   each wavelength
                            ine
                                nined by
                                \on three
                                          lt
                  ilytfical
                      other
                           Eacfl measur
                rate
                     in
                lying by  chree ch« averag«  of
             nconsecutive days  (each analyce
                  IDL, with seven
             must be performed  AS though it
               measurement must be followed
           ^ .y performed between the
      must be determined and reported for
lysis of the samples.
                                         ea
                                LDLs
   7.4.14.3 The quarterly d>i^rmi£esnay af^act die IDL. the IDL for that instrument
   ™?*e 5fde£f™in«a>«^ the result submitted for use as the established
   IDL forythaX instrumentXor the remainder of the quarter.
7.4.14<4
reportxng
             DLs must be repored^for each instrument and submitted with each
                  If multiple instruments are used for the analysis of an
                    SDG, the highest IDL for the analyte must be used for
                  ation v
                                  for that SDG.
July, 1991
                                                                   Page E - 50
-------
Exhibit E
SOW No.  XXX - Ambient Air
   7.4.14.5 The IDL for each analyte must be  less  than or^qual  to  the  CRQL.
  FAn exception is granted if the analyte concentration yn  t*he samples  is
   greater than"or equal to five times  the reported  IDL,

7.4.15  Interelement Corrections for ICP
   7.4.15.1 The ICP intereleraent correction factor
   3 months prior to beginning sample analyses um
   least annually thereafter, as outlined in Exhj,
   Correction factors for spectral interference
   wavelengths used for each analyte reported J/y ]/CP

   7.4.15.2 The correction factors must be
   instrument conditions used for sample a
   adjusted in any way that may affect th<
   factors, the factors must be redeterm
   use.  The interelement factors determ'
   analytes, for each instrument used to
           rmined within
               .nd at
                  5.
       the  same
      instrument was
     t correction
   ults submitted for
   reported for  all ICP
  in the SDG.
July, 1991
             Page E  - 51
-------
Exhibit E
                                                      SOU No.  XXX -  Ambient Air
                                   SECTION 8

                             REGIONAL DATA REVIEW

      Contract laboratory data are generated to meet
Regions.  In order to verify the usability of data
each Region reviews data from the perspective of e
functional aspects of data quality.  General gui
been developed jointly by the Region and  the Nation;
Region uses these guidelines as the basis for data/evaluation.  Individ
Regions may augment the basic guideline revieypr/cess with additional review
based on Region-specific or site-specific concerns.  Reg/fohal reviews, like
the sites under investigation, vary based o/thfe nature/of/the problems under
investigation and the Regional response ap/ropriate tc/the specific
circumstances.
                                                                  needs of  the
                                                                    purpose,

                                                                          tve
contractual discrepancies, and the
to evaluate Contractor and method
are integrated into a collective
laboratory administration and manag^
action to correct deficiencies in the^
      Regional data reviews relating usability^af the 4iata to a specific site
are part of the collective assessment process.   Tnfev comp^i^ment the review
done at the Sample Management Office, which is designed, to
                                          done at EMSL/L^vWhi«fli is designed
                                                 lese individual evaluations
                                                           jr program and
                                                            take appropriate
                                                          ffance.
 July,  1991
                                                                   Page E  -  52
-------
Exhibit E
                          SOW No.  XXX -  Ambient Air
                                   SECTION 9

                         LABORATORY EVALUATION SAMPLES

      Although intralaboratory-QC  may  demonstrate Contra
performance that can be  tracked  over time,  an extery
program is an essential  feature  of a QA  program.
Contractor and method performance, Contractors p
comparison studies conducted by  the EPA.   Resul
laboratory evaluation samples will be  used by
Contractor's continuing  ability  to produce  ac
-------
Exhibit E
                                                      SOW No.  XXX -  Ambient Air
        Deficiencies  exist  in the  Contractor's performanc

        Within  14 days  of receipt  of notification from/EPA/ the Contractor
        shall describe  the  deficiency(ies)  and the actn.on$$)  taken to correct
        the deficiency(ies)  in a letter  to  the Administrative\Project
        Officer, the  Technical'Project Officer,  andEMS
      Unacceptable Performance, Response Explainir
      (Score less than 75 percent):
Teficiency(ieX)  Reqttijred
      • Deficiencies  exist  in  the  Contractor's' performance to the extent that
        the National  Program Office has  determined that/€he Contractor has
        not demonstrated  the capability  to  ineetr the conftract requirements.

      • Within 14 days of receipt  of notification fr^m BPA,  the Contractor
        shall describe the  deficiency (ies )^and tfts^/ctifon^) taken to correct
        the deficiency (ies) in a letter  to  the\Adminis(trative Project
        Officer, the  Technical Project Officer,  ah< EMSt>tLV.

      The Contractor  shall be  notified by the  Administrative Project Officer
or Technical Project  Officer conce/ning~~Etre—iaaiedy for their\«macceptable
performance.  A Contractor may expect ^--hut!EPA isnot-iimited to,  the
following actions:  Reduction  of th\ number~~o~f—samoles seny under the
contract, suspension  of sample shipment  oo  the/CootractSr/ a site visit,  a
full data audit, analysis of remedial RE samples / and/or  a contract sanction,
such as a Cure Notice.                 \   v   /
NOTE:  A Contractor's promot^re»fionse demonstrating that  corrective  action has
been taken to ensure the Contractor's capabirity\o meet  contract  requirements
will facilitate continuatiopr^of^£u.ll\ sample deisj-vei
July,  1991
               Page E - 54
-------
 Exhibit E
                                                      SOW No. XXX  -  Ambient  Air
                                                              .agnetic tapes
                                                                 its.
                                   SECTION 10

                               GC/MS  TAPE AUDITS
       Periodically,  EPA requests from Contractors th
corresponding  to  a specific Case in order to accompYis
Generally,  tape submissions and audits are request
reasons:

       Program  overview;

    •   Indication  of  data quality problems from EMSL/LV, /SMO,  or Regional data
       reviews;

       Support  for on-site audits;  and

       Specific Regional  requests.

       Depending upon the reason for an audit,  the "fea^es fbom  a recent Case, a
specific Case, or a  laboratory  evaluation sample may t?e\re queued.   Tape
audits provide a  mechanism to assej«-a4he£ence to contractual/requirements and
to ensure the consistency of data/reportedorrThe-4iaEdcopy/floppy diskettes
with that generated  on the GC/MS  ^e^~-Jfbia^unctionpTcByides  external
monitoring of Program QC requirements ahd checks aOhtiejicj/of the Contractor
to internal QA procedures.   In  addition,\ape/audits enable EPA  to  evaluate
the utility, precision,  and accuracy orVthe\Xna^ytical  methods.

      The GC/MS tape shall include  raw data  and quantitation  reports  for
samples, blanks,  laboratop/evaliia±ion samples,\Lnitial calibrations,
continuing calibration,  /ndBF&asstociated wiNsh the  Case requested.  'The
specific requirements f/r ^submiss^orls^-of^GC/MS \ap4s are discussed  in Exhibit
      Upon request:
required tapes and
within seven (7) days
                          Admini'stE4tive Pr»j^t Officer  or  EMSL/LV,  the
                           ssay documentation  shall be submitted  to  EPA
                         no
                              icarion.
July, 1991
                                                                   Page E  -  55
-------
Exhibit  E
                                                     SOW  No.  XXX -  Ambient Air
                                  SECTION 11

                        ON:SITE LABORATORY EVALUATIONS

      At a frequency dictated by a contract laboratojfy
Administrative Project Officer, Technical Project
representative will conduct an on-site laboratory
laboratory evaluations are carried out to monito
meet selected terms and conditions specified in/fcfi
process incorporates two separate categories:
and an Evidentiary Audit.

11.1  QUALITY ASSURANCE ON-SITE EVALUATION
11.1.1  Quality assurance evaluators ins
verify the adequacy and maintenance of ins
personnel meeting experience or education requ
performance of analytical and QC procedures.  The
that items to be monitored will include but not be 1
items:
      Size and appearance of the

      Quantity,  age,  availability,
      instrumentation;
                                                                       the
                                                                   authorized
                                                                            to
                                                                            on
                                                     of SOPs;

                                              rso^mel training programs;

                                                  lities;
11.1.2  Prio
performance/of
discussio
on-site
Regiona
trend re
                                                     :ra£tor's facilities to
                                                        the continuity of
                                                        and the acceptable
                                                             should expect
                                                              the following
                                                          .nd performance of
      Availability,  appropriateness,  and

   •  Staff qualificatio

   •  Reagents,  standa

      Standard prepa

   •  Bench sheets a1
      Review of the
      procedures
                                   ogbook maintenance and review,  and

                                    pie  analysis/data package inspection
                                        various documentation pertaining to
                           NCon\ractor is  integrated in a profile package for
                                   Items that may be included are previous
                                 ition sample scores,  Regional review of data,
                       GC/MS  t^pe audit reports,  results of CCS,  and data
July, 1991
                                                                   Page E - 56
-------
Exhibic E
                                                      SOW No. XXX  - Ambient Air
11.2  EVIDENTIARY AUDIT

11.2.1  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.  The evidence a(udit is comprised of
the following three activities'.

   11.2.1.1  Procedural Audit

      11.2.1.1.1  The procedural audit consists/
      actual standard operating procedures and/acc/ompanying
      the following laboratory operations:

           Sample receiving;

           Sample storage;

           Sample identification;

        •  Sample security;

           Sample tracking (from

        •  Analytical proj ect fil

   11.2.1.2  Written SOPs Audit

      11.2.1.2.1  The written SOPs audit
      the written SOPs to determine if
      following laborato
      sample identifica
      completion of
      assembly.
   11.2.1.3  Analy

      11.2.1.3.1  The
      review and examina
      The auditors review tfi
                                                             lysis); and
                                             fets of review and examination of
                                            ar*^ accurate and complete for the
                                                jceiving, sample storage,
                                              sample tracking (from receipt to
                                                 {ect file organization and
                                              Audit

                                'project file evidence audit consists of
                                    analytical project file documentation.
                                       determine:

                             cumentNi4jyentory;

                                ile;

                                 of the document numbering system;

                                  activity;

                              etivity recorded on the documents; and
July, 1991
                                                                   Page E - 57
-------
Exhibit E
                                                      SOW No.  XXX - Ambient Air
            Error  correction  methods.

11.3  DISCUSSION"  OF THE ON-SITE TEAM'S FINDINGS
11.3.1  The quality assurance  and  evidentiary audi
with the Administrative Project Officer/Technical
debriefing the Contractor.  During the debriefin
findings and recommendations for corrective
Contractor personnel.
11.4
                                                                   ir findings
                                                                         to
        CORRECTIVE ACTION REPORTS  FOR FOLLOV^T
        EVIDENTIARY AUDIT REPORTS
                                                                           .eir
                                                            LITY ASSURANCE AND
                                                     irance and evidentiary
                                                    ag /he  on-site  evaluation
11.4.1  Following an on-site evaluation, A}uartty as:
audit reports which discuss deficiencies  fbund dul
will be forwarded to the Contractor.  The Contractor  i6ust discuss  the
corrective actions taken to resolve  the deficiencies  discussed during the
on-site visit and discussed in the on-site reports  m^a letb&r to  the
Administrative Project Officer, Technical Project OfficebxEM&L/LV (response
to the quality assurance report) and NElC^tresparise to  the evidentiary report)
within 14 days of receipt of the tind«tg^D^_within~^R5r-64=oifi agreed upon
between the Administrative Project Slffrcer/TectmicalProje/t Officer and the
Contractor.  If SOPs are required toNie writtep or  SOPs~~are required to be
amended, the Contractor must provide the  S^s/to/the  Technical Project
Officer, EMSL/LV (quality assurance/tecKnicM  SOPs) and NEIC (evidentiary
SOPs) within 30 days of receipt of the finding&^ Officer/Xecmvical  Project Officer and the
Contractor.
11.4.2  If the Contrac
resolve the deficienc
expect, but the Age
the number of samp
to the Contractor,
remedial PE samples an
                                            .roprri&ce corrective action to
                                                   reports,  a Contractor may
                                                 llowing  actions:   reduction of
                                                suspension of sample  shipment
                               si;Ce visit,  a  full  data audit,   analysis of
                                 ct sanction,  such as a  Cure Notice.
 July,  1991
                                                                    Page E - 58
-------
 Exhibit E
                                                       SOW No.  XXX -  Ambient Air
                                   SECTION  12

                •  •  QUALITY ASSURANCE AND DATA TREND

       Data submitted by laboratories are subject to reVi<*w  from  several
 aspects: compliance with contract-required QC, usability7>tvJ  full  data
 package evaluation.  Problems resulting from any of/the^Lrev^s may
 determine the need for a GC/MS tape audit, an on-stte/labo>avaluation
 and/or a remedial laboratory evaluation sample. An Addition, ^^res^ibed  in
 the methods provides information that is continually used by the
 assess sample data quality, Contractor data qualiey and Program datacuaLIty
 via data trend analysis.   Trend analysis is acWplished by entering data  into
 a computerized data base.   Statistical repots /hat evaluate specific
 anomalies or disclose trends in many areas/including ^he/following  are
 generated from this data  base:

       Surrogate Spike Recovery;

       Laboratory Evaluation Sample;

    •   Blanks;

    •   GC/MS  Instrument  Performano^ Checks;

    •   Initial  and Continuing Calibr£ioV Data;

    •   Other QC and Method  Parameters.
   Program-wide statistical^xesults are usN
observe  the relative perfonnancebsf each Cor
against  its peers.  TheVrepjwrts^areX also used"
laboratories.  The res "
overall  evaluation of/a Gbntractoi:' s perfo^
determine if corrective/action OJK arx^on>s4te l
indicated in order
                                     require
                           rank laboratories in order  to
                           l^or using a given protocol
                             ientify trends within
                              analyses are included in
                             and are reviewed to
                          moratory evaluation is
                         its of the contract.
      Contractor per
techniques to detect
levels of quality_control. a
problems whic
depa"z
          to p
     apparent fro:
time is monitored using these trend analysis
 Contractor output from required or desired
 "--(vide an early warning of Contractor QA/QC
      the results of an individual case.
      As a
informati
analytic
vast em-
ana lyz
performanc
control and p
achievable and
production analysis
                ^vy
          .he Program, the data base provides the
            erformance-based criteria in updated
            .ory criteria have been previously used.  The
             
-------
Exhibit E
SOW No. XXX - Ambient Air
Agency in meeting its objec,  -es of obtaining data of kn^wn/4nd documented
quality.
 July,  1991
              Page E - 60
-------
Exhibit E
                                                  SOW No. XXX - Ambient Air
                                  SECTION 13

               •  .               DATA MANAGEMENT

      Data management procedures are defined as proce/
acquisition or entry, update, correction, deletion,
computer readable data and files.  These procedure
and contain a clear definition for all databases
resubmit deliverables.  Key areas of concern inc
(including personnel and security), documentati
quality control.
      Data manually entered from hard-copy
error rates estimated.  Systems should pre
out-of-range data and alert data entry pe
entry error rates must be estimated and
reentering a statistical sample of the
discrepancy rates by data element.

      The record of changes in the form of correc
originally generated, submitted, and/or resubmitted mt
allow traceability of updates.  DowHaen£ation must inclu?
each change:

      Justification or rationale
                                                      s specifying the
                                                         and security of
                                                            n written form
                                                                generate or
                                                                   tion
                                                                        and
                                                quality controlled and the
                                                       .correct or
                                                      s.   In addition, data
                                                     nthly basis by
                                                     calculating
      Initials of the person making tnte cnange /or. changes.  Data changes must
      be implemented and reviewed by a person/or group independent of the
      source generating the deliverable;
•   Change documentation
   original deliver

•   Resubmitted d
   part of the
   resubmissio
   inspected;

•   The Laboratory Manage
   de1iverabi€^T
                              t beXretained according to the schedule of the
      Docv
                                                        updates to data
                                                           cumented to
                                                            following for
                                               Fes must be reinspected as a
                                              'tion pro  ss prior to
                                           ,  not just cne changes, must be
                                    iprove changes to originally submitted
             ion ofctata changes may be requested by laboratory auditors.
   Life cycle/management procedures must be applied to computer software
systems/developed by the laboVatary to be used to generate and edit contract
delivei£ablesV^Such systems mpstjbe thoroughly tested and documented prior to
utilizati*
 July,  1991
                                                                Page E - 61
-------
Exhibit E
                                                     SOW No. XXX  - Ambient Air
      A software test and acceptance plan including test
      results and acceptance criteria must be developed
      available in'written form.
                                                             lirements, test
                                                            flowed, and
   •  System changes must not be made directly to pr
      generating deliverables.   Changes must be
      system and tested prior to implementation.

      Each version of the production system wil]
      number, date of installation, date of

   •  System and operations documentation
      each system.  Documentation must ii
      operations and maintenance manual.

      Individual(s) responsible for the fo]
identified:

      System operation and maintenance including doc

   •  Database integrity, including data
      control; and

   •  Data and system security,  backu
                                                               stems
                                                                  velopment
                                                       ion and archived.
                                                            and maintained for
                                                           .ual and an
                                                       ions must be


                                                               and training;

                                                              and quality
July,  1991
                                                                   Page E - 62
-------
 Exhibit  E
                                                      SOW No. XXX - Ambient Air
                                   SECTION 14

                '  •                 REFERENCES

14.1   Fisk, J.F'.  and Manzo,  S.M.   "Quality Assurance/Quality Control in
Organics Analysis",  Proceedings from the Water Pollu/ion Control Federation
Meeting, May  1986.
14.2  Office of Monitoring Systems  and Quality A
Protection Agency,  "Interim Guidelines and Spec
Quality Assurance  Project  Plans", QAMS-005/80,
                             U.S.Enviror
                      itions  for Prepa^ng
                     -rnber 1980.
14.3  Office of Solid Waste  and Emergency Re/ports e,  U.S -Environmental
Protection Agency, Test Methods for  Evaluating/Solid Wa4ta^  Third Edition
SW-846, November  1986.

14.4  Laidlaw, R.H., "Document  Control  anUsChaihxp£/Cus'tody  Considerations for
the National Contract Laboratory Program,"  Qttality Control in Remedial Site
Investigations:   Hazardous and  Industrial Solid"W^ste Testing,  Fifth Volume,
ASTM STP 925, C.L. Perket, ed.,  American  Society forxTestihi and Materials
Philadelphia, 1986.
14.5  Health Effects Research
Agency, Manual of Analytical Method >
and Environmental Samples, EPA-600/J
                                           U.S.
                                     ,80>Q36, jv
14.6  Environmental Protection Agency,
Procedures for the Analysis of Pollutant;
Rule and Interim Final Rule aad^Proposed
Register, Vol. 49, No. 209<\ pp 43SJ34-4"
                                           Jnde
                         oental  Protection
                  ilysis  ofPe's tic ides  in Humans
                     Establishing Test
                  the Clean Water Act; Final
                  V40 CFR Part 136, Federal
                  fiber 26, 1984.
14.7  Health Effects Re-sea/ch Labbraleofy^^U.S. Environmental Protection
Agency, Manual of Analytical Quality ControK^or Pesticides and Related
Compounds In Human ami Environmej/tal/Saliip^es-Second Revision,
EPA-600/2-81-059, A/ril/1981.
14.8  Environmental MohxJ-M>and Pearson/ J/G.  "Quality Assurance Support for the
Superfund Contract Laborator^ P/ogram", Quality Control in Remedial Site
Investigation:   Ha^ardousxafid Industrial Solid Waste Testing, Fifth Volume,
ASTM STP 925,  C.L. Pe>ket, ed/, American Society for Testing and Materials,
July, 1991
                                                                   Page E  - 63
-------
Exhibit: E
                                                     SOW Xo. XXX  - Ambient Air
Philadelphia  L?36
July,  1991
Page E - 64
-------
-------
                                   EXHIBIT F
                           EVIDENTIARY REQUIREMENTS
                               TABLE OF CONTENTS
                                                                       Pace No.
SECTION 1  SAMPLE CHAIN OF CUSTODY
     1.1  Sample Identification	/ • ^	^X;  -7 F-1
     1.2  Chain-of-Custody Procedures
     1.3  Sample Receiving Procedures
     1.4  Sample Tracking Procedures  .   ./.  ./.  .  .  •/. /	F-3
SECTION 2  DOCUMENT CONTROL PROCEDURES
     2.1  Preprinted Laboratory Forms and Logbooks   . ">\.	p-4
     2.2  Consistency of Documentation	7X.  .  /"X	f--5
     2.3  Document Numbering and
     2.4  Storage of EPA Files
     2.5  Shipping Data Packages
SECTION 3  STANDARD OPERATING PROCED
     3.1  Specifications fo_r—Written SOPs
     3.2  Handling of Confidential
-------
Exhibit F
                                                      SOW
                                                              XXX  - Ambient Air
                                                             or  from  the
                                                             tion effort is
                                                                 he following
                                                                    le tracking
                                   SECTION 1

                •  .          SAMPLE CHAIN-OF-CUSTODY

    A  sample  is  physical  evidence collected from a
environment.  An essential part of hazardous waste
that the evidence gathered be controlled.  To  acco;
sample identification, chain-of-custody, sample  r
procedures have been established.

1.1 SAMPLE  IDENTIFICATION
1.1.1  To assure traceability of samples while  ifn  possession of the
Contractor, the Contractor shall have a specif/ed  meth/d l?or maintaining
identification of samples throughout the l4bo/atory.

1.1.2  Each sample and sample preparationvconta^iner/shall  be labeled with the
EPA number or a unique laboratory identifier-*.  If  a  unique laboratory
identifier is used, it shall be cross-referencettsj:o  tfes^EPA number.
                                                     ;ted,  the  custody of EPA
                                                           Llected until they
                                                          ;ractor  shall have
                                                 iintained  and  documented.
1.2 CHAIN-OF-CUSTODY PROCEDURES

1.2.1  Because of the nature of rfie data being""
samples must be traceable from the
are introduced as evidence in legal\pro\eeding^.
procedures ensuring that EPA sample c\

1.2.2  A sample is under custody if the following applies:
     •  It is in your posse^ssToTr>^or

     •  It is in your view af-td^beiNng in your\posCession, or
     •  It was in your/pos/ess ion janoyou^iocked^t up, or
     •  It is in a deysigiteted sec/ire/^ire^N^secure areas shall be  accessible to
       authorized p,ersWnnel only) ./
1.3 SAMPLE RECEIVING^PROCEDT:

1.3.1  The Contractor shall'
receiving all
                                      a sample custodian responsible  for
1.3.2  The Loneractor sna^U. designate a representative to receive  samples  in
the event/that the sample custodian is not available.The condition of  the
shipping /containers and sample bottles shall be inspected upon receipt by  the
sample jmstAiian or his/her representative.

1.3.3  Thexcondibion of the custody seals (intact/not intact) shall  be
inspected upahxjrecei>i^by th4 s/ample custodian or his/her representative.
July, 1991
                                                                     Page  F -  1
-------
Exhibit F
                                                      SOW  No.  XXX -  Ambient Air
1.3.4  The sample custodian  or his/her  representative  sh
presence or absence of  the following documents  accompany'
shipment:        '  •
     •  Airbills or airbill stickers;

     •  Custody seals;

     •  EPA custody records;.

     •  EPA traffic reports or SAS packing lis/s.;

     •  Sample tags.
                                                              leek  for  the
                                                            ''the sample
                                                  md
1.3.5  The sample custodian or his/her
forms (e.g., custody records, traffic repo
accompanying the samples at the time of sampl
                                              or"
  ill  sign and date all
*g  lists,  and airbills)
                                                eceipt
1.3.6  The Contractor shall contact SMO to resolve
such as absent documents, conflicting information, broket
unsatisfactory sample condition (e
1.3.7  The Contractor shall record
problems on Telephone Contact Logs.
                                               sample bottD
1.3.8  The following information shall
by the sample custodian or his/her repres
inspected:

     •  Condition of the

       Presence or absen
       sample contai
       Custody sealaumbe
       Condition of the s
                                                                 and problems
                                                               dy seals,  and
                                                            ancies and
                                                   on appropriate Form AADC-1
                                               .ve as samples are received and
                                                ody seals on shipping and/or
       Presence
                           of airbills ^dr airbill stickers;

                                  numbers ;

                              EPA custody records;

                                  traffic reports or SAS packing lists;

                              s-ample tags;
July, 1991
                                                                    Page F - 2
-------
Exhibit F
                                               SOW No. XXX  - Ambient Air
       Sample tag identification numbers cross-referenced to the EPA sample
       numbers.

       Verification of agreement or non-agreement of ipttor/nation recorded on
       shipping documents and sample containers; and
1.4
 Problems or discrepancies.

SAMPLE TRACKING PROCEDURES
1.4.1  The Contractor shall maintain records documenting all phases
handling from receipt to final analysis.  The/reoords shall include
documentation of the movement of samples and/prepared samples into and out of
designated laboratory storage areas.
July, 1991
                                                              Page F -  3
-------
Exhibit  F
                                                      SOW No.  XXX - Ambient Air
                                   SECTION 2
                          DOCUMENT CONTROL PROCEDURES
      The goal of the laboratory document  control
all documents for a specified Sample Delivery Gro
for when the project is completed.  Accountable
laboratories shall include but not be limited t<
records, sample work sheets, bench sheets,'  and/otber  documents  relating""^ the
sample or sample analyses.  The following  docjkerit  control  procedures have
been established to assure that all laboratory Records ^reassembled and
stored for delivery to the EPA or are avail4bl/ upon  r/qu/st  from the EPA
prior to the delivery schedule.

2.1 PREPRINTED LABORATORY FORMS AND LOGBO*

2.1.1  All documents produced by the Contractor^whi^h a^fexdirectly related to
the preparation and analysis of EPA samples shall be^bme  th~exproperty of the
EPA and shall be placed in the comnlgtesample deliveryg^oupytile (CSF).   All
observations and results recorded by thTT^b^tatorybut notSta  preprinted
laboratory forms shall be enter edWt^p«riaanentlaBora€«r5t logbooks.   When
all data from a SDG are compiled,  aU. ^iginTr-^abor^tory^orms and copies of
all SDG-related logbook entries shall\be\4.ncluxled/inthe~~6locumentation
package.
2.1.2  The Contractor shall identify the
documents which is directly-fela-ted to
samples.
2.1.3  Pre-printed
and be dated (month/'
performing the activ,
      labpracory foi
        ay /year )  and/ sit
       .ty/at the time /an aci
                                  ty recorded on all laboratory
                                    •ation and analysis of EPA
          the name of the laboratory
        rperson responsible for
        is performed.
2.1.4  Logbook entrti
person responsible for
performed.

2.1.5  Logbook^entries
with the except Lerfr"o1
only one SDX3 p^r page.
                       shal
               ^    ited (month/day/year) and signed by the
            rformine the activity at the time an activity is
                                irr-
                be
            trumejit run
^logical order.   Entries in logbooks,
  and extraction logs,  shall include
2.1.6
numberec
in both bound ana unpound logbooks shall be sequentially
2.1.7  Instrument tun logs shalybe maintained so as to enable  a
reconstruction o^the run sequence of individual instruments.   Because  the
laboratory must provide cbpies/of the instrument run logs to  the  EPA, the
July, 1991
                                                       Page F  - 4
-------
 Exhibit  F
                                                      SOW No. XXX - Ambient Air
 Laboratory  may  exercise  the option of using only laboratory or EPA sample
 identification  numbers  in the Logs for sample ID rather charfr government agencv
 or'commercial client  names to preserve the confidentiality/of commercial
 clients.

 2.1.8  Corrections  to supporting documents and raw d£ta sfia^l be made by
 drawing a single  line through the error and entering tWexcorr^st information.
 Corrections and additions to supporting documents/and/raw oa^a sha^Ll be dated
 and initialed.  No  information shall be obliterated /r renderebXunre^iable.
 All notations shall be recorded in ink.  Unused/options of documents stia-U be
 "z'd" out.

 2.2 CONSISTENCY OF DOCUMENTATION
2.2.1  The Contractor  shall  assign a doci
the organization and assembly  of  the CSF.
                            pent/control/officer  responsible for
2.2.2  All copies of  laboratory  documents shalL be  coi&pLete and legible.

2.2.3  Before releasing analytical  results,  the docmnent^xmtrol officer
shall assemble and cross-check the  information  on samite  tags^y custody
records, lab bench sheets, persona^T~an«i-4%ns,trument  logs/^a^ytother relevant
data to ensure that data pertaining to  eachpa?tri«ularsample  or sample
delivery group is consistent  throughoSj~~Che—CSF.

2.3  DOCUMENT NUMBERING AND INVENTORY\PROlSEDt
                                      \  V /
2.3.1  In order to provide document accountability  of  the completed analysis
records, each item in  a CSFshall be inventoried  and assigned  a  serialized
number as described in E>^IibitB>\Section 2\
CSF # - Region - Serialized number
                           *xample\ /75-2-0240).
2.3.2  All documents/relevant to/ea
logbook pages, bencft sheets,
re-preparation records ,i?e-an£
analysis, custody recfc
-------
Exhibit F
                                                     SOW No. XXX  - Ambient Air
                                                           es packages to the
                                                           containers placed
                                                                 seal.  The
                                                                  & method
2.5  SHIPPING DATA PACKAGES AND CSF

2.5.1  The Contractor shall document shipment of delive
recipients.  These shipment's require custody seals on
such that they cannot be opened without damaging or
Contractor shall document what was sent, to whom,
(carrier) used.

2.5.2  The Contractor shall purge the CSF delive
Region 180 days after the report submission.   '

2.5.3  A copy of the transmittal letter for
and the SMO.

2.5.4  The Document Control form is used
inspection of shipping containers and sampl
one (1) original FORM AADC-1 for each shipping^

2.5.5  The Contractor shall sign and date the airbill
the shipping containers, record the/_j>resence or absence
their conditions.

2.5.6  The Contractor shall note an;
instructions explained in Exhibit B,
                                                         receipt and
                                                        ractor shall submit
                                                              ent),  examine
                                                               ody seals and
                                                            es and follow the
2.5.7  The Contractor shall submit a co
each SDG package.
                                                ocument Control Form with
July, 1991
                                                                    Page F - 6
-------
 Exhibit F
                                                      SOW No.  XXX -  Ambient Air
                                   SECTION 3

                •  •       STANDARD OPERATING PROCEDURES

       The  Contractor  must  have  written standard operating/procedures (SOPs)
 for  receipt  of  samples,  maintenance  of custody,  sample  iden^f ication,  sample
 storage,  tracking  the analysis  of  samples, and asse^bly^ofcomHeted data.

 3.1  SPECIFICATIONS FOR WRITTEN STANDARD OPERATING/PRtKIEDURES
3.1.1  An SOP is defined as a written narrativ
laboratory operating procedures including ex
documentation.  The SOPs must accurately des
in the laboratory,  and copies of the writte
appropriate laboratory personnel.  These
that analytical data produced under this
EPA enforcement case preparation and
                al
                                                    p -by- step  descriptiTt
                                                    of  laboratory
                                                              procedures  used
                                                            available  to  the
                                                           cessary  to  ensure
                                                          ep table for  use in
3.1.2  The Contractor's SOPs shall provide
meet each of the following specifications and
basis for laboratory evidence audits.  The Contractor
standard oper-.ring procedures (SOPz

     •  Sample receipt and logging;

     •  Sample storage;

     •  Preventing sample contamination;

     •  Security for labor;

     •  Traceability of

     •  Maintaining iristi

     •  Sample anal]

     •  Glassware-cleaning>
                documentation  to
                  by EPA as the
                      written
       Technic
       packa
laboratory operation and data
                                 tually-required quality assurance and
                                  .ch individual data package;

                                  ing,  and reporting;
       Chain-di<
July, 1991
                                                                    Page F - 7
-------
Exhibit F
                                                      SOW No.  XXX -  Ambient Air
     •  Document control, including Case file preparation.
                                                            ian  responsible
                                                             er duties and
                                                                     ing  in  of
3.1.6  The
on any particu
July, 1991
3.1.3  The Contractor shall have a designated sample
for receipt of samples and have written SOPs describir
responsibilities.

3.1.4  The Contractor shall have written SOPs for
the samples.  The procedures shall include but noi
the following information:

     •  Presence or absence of EPA chain-of-cu<

     •  Presence or absence of airbills or aifrbi

     •  Presence or absence of EPA Traffic/Repc
                                           ^*X^      "**   /
     •  Presence or absence of custody seals ohxshippiqfe and/or sample
       containers and their condition;

     •  Custody seal numbers, when present;

     •  Presence or absence of sam-

     •  Sample tag ID numbers;

     •  Condition of the shipping contai
     •  Condition of the s

     •  Verification of
       documents and s

     •  Resolution of
       Office;  and

     •  The definition
       receipt.

3.1.5  The ConJ
of samples af
and laboratory
storage
sample cor
who have/ace
                                jntainer;

                                    rvonagreemeHt o^E information on receiving


                                                frith the Sample Management


                                its used to describe sample condition upon
                                         
-------
 Exhibit F
                                                      SOW No. XXX  - Ambient Air
        A description of the documentation used to record
        sample storage,  sample transfers,  sample preparat
                                           ample receipt,
                                               and sample
        A description of the documentation used to re
        calibration and other QA/QC activities;  and
     •  Examples  of the  document formats and labor
        the  sample  receipt,  sample storage,  sampl
        analyses.

 3.1.7   The  Contractor shall have written SOP<
 of EPA  samples throughout  the  laboratory.
                                                      used in
                                   maintaining identification
 3.1.8   If  the  Contractor  assigns  unique  laboratory ide'nt/f iers,  written SOPs
 shall  include  a description  of  the method7 us^d  to  as£ig/the  unique laboratory
 identifier and cross-reference  to the EPA^sampie. nufabe/

 3.1.9   If  the  Contractor  uses prefixes or suffixes ifNaddition  to  sample-
 identification numbers, .the  written SOPs shall  inc^de  their  definitions
 The Contractor shall have written SOPs describing  the^method^y  which  the
 laboratory maintains samples undei
3.1.10 The Contractor shall have
of all documents relating to each
review.  Documents shall be filed on
must ensure that all documents includr
records, chromatographic charts,  compute^
correspondence, and any other written doc
are compiled in one location
document numbering and
                        se
                          56-
                  ubmission
                    cedure,
3.1.11 The Contractor/sh

3.1.12 The Contrac
in preparing and

3.1.13 The Contractor
sample analysis QA/QC.
3 . 2   HANDLI

3.2.1  A. 06nt.
designate^ c
must be/ha
contra
conf identl
      _for  organisation and assembly
                  inical  and managerial
         fie basis.  The procedures
         pages, sample tracking
  printouts , raw data  summaries,
        having reference to the Case
        iPA.  The system  must  include a
                                  laboratory safety.
                              for cleaning of glassware used
                   under this contract.

                 SOPs for traceability of standards used in
             L INF'
ON
                ork under this contract may receive EPA-
             nation from the Agency.   Confidential information
             i>m other documentation developed under this
:omplish thisl  the following procedures for the handling of
 Cmation have7 been established.
July, 1991
                                                                    Page F -  9
-------
Exhibit F
                                                      SOW No.  XXX -  Ambient Air
3.2.2  All confidential documents shall be under  the  supei
designated Document Control Officer  (DCO).
                                                       rion of a
3.2.3  Any samples or information received with a request^of  confidentiality
shall be handled as  "confidential."  A separate locked filesiiall be
maintained to store this information and shall be
nonconfidential information.  Data generated from
be treated as confidential.  Upon receipt of conf
logs these documents into a Confidential Invent
then made available to authorized personnel bu
out to that person by the DCO.  The documents/s
file at the conclusion of each working day.
be reproduced except upon approval by the E
will enter all copies into the document co;
information may not be disposed of excep
Officer.  The DCO shall remove and retain
information disposed of for one year and shal
disposition in the Confidential Inventory Log
                                   Figure 1
                                                           Bother
                                                                 shall
                                              /tial information/^she DCO
                                              3g.  The informais^on i<
                                            ly after it has been sighed
                                            1 be returned to the locked
                                                      .formation may not
                                                     'fficer.   The DCO
                                                      addition, this
                                          ipproyalfiy the EPA Contracting
                                                   of any confidential
                                                 ecord of the
Document Control #*
232-2-
232-2-
232-2-
232-2-
232-2-
232-2-
232-2-
232-2-
etc.
0001
0002
0003
0004
0005
0006
0007
0008
        Inventory Sheet
      Recorc
             .eports
            :a Summary Sheets
btebook Pages
Instrument Logbook Pages
                            .edxm each set of documents.
# Pages

    1
    2
    2
   50
   10
   10
   14
   12
 etc.
July,  1991
                                                             Page F - 10
-------
EXHIBIT G
-------
Exhibit G
                                                      SOW No.  XXX - Ambient Air
                                                                  through a
                                   EXHIBIT G

                               GLOSSARY OF TERMS


Absorbance - A measure of the decrease  in  incident  light
sample into the detector.  It is defined mathematic.

                         A  =  I(solvent)
                               I(solution)

                        Where, I = radiation  i/nte/isity

Aliquot - A measured portion of a field sample/taken  f$*r  ^halysis.

Analysis Date/Time - The date and military  tifae  (24-tfou]/ clock)  of  the
introduction of the sample, standard, orx^lank^into/the; analysis system.

Analysis Group - An analysis group is a set ofno more^han twenty  analytical
samples (as defined below) for the purpose  of methb<0uail> at a minimum,
prepared and analyzed at a f requen£y-e£_o_nce  per twenty ahalv/tical  samples.
Analysis Replicate - A single anaIytiS5l~-3enip4.e pressed
preparation method and analyzed in^epricate. /
                                                           zough the analytical
Analysis Run - The actual instrumental^anal^is/of the sample preparations
from the time of instrument calibration \hrougji the running of  the  final  CCV.
All sample preparation analyses during theXana^ysis run are subject to  the  QC
protocols set forth in Exhibit t>3k£ this con^rac^ unless  otherwise  specified
in the individual methoc
Analysis Spike Sample /
preparation method ana
Analyte - The element o
interest.

Analytical Preparation - An
preparation me

Analytical
fusion, et
from its ;nat
suitable
                                  cal sampis.  tak¥n  through  the  analytical
                                   prlot\to analysis.
                                    lysis  seeks  to  determine;  the  element of
                                        sample  taken  through  the  analytical
                                         preparation or  sample preparation.

                                A method (digestion,  dilution, extraction,
                                r otherwise  release  the  analyte(s)  of interest
                                  1  solution containing  the  analyte which is
                                   analysis  methods.
July, 1991
                                                                     Page G - 3
-------
Exhibit G
                                                      SOU No.  XXX -  Ambient Air
Analytical Sample  - Any  solution  or  media introduced int
which an analysis  is performed  excluding  instrument  cal
calibration verification,  initial calibration blank,
verification and continuing calibration blank.   Note
defined as analytical samples:  undiluted and dilute
EPA), predigestion spike samples,  duplicate  sampl
analytical spike samples, post-digestion  spike s
samples (ICS), CRQL standard for  AA  (CRA), CRQL s
laboratory control sample  (LCS),  preparation bl
analysis sample (LRS).
                                                             'instrument on
                                                            "ion,  initial
                                                           •iuing calibration
                                                           Allowing are all
                                                               JEPA and non-
                                                                      samples ,
                                                                      :heck
Analytical Spike - A post-digestion spike  to/be/prepare
adding a known quantity of the analyte  to  an aliquot  of  t
The unspiked sample aliquot must compensate f^r  any
samples by addition of ASTM Type II wate
volume of the spiking solution added must
sample volume.
                                                            ior to  analysis  by
                                                             prepared sample.
                                                            change  in the spike
                                               .e unsjiike'd sample aliquot.   The
                                                      101%  of  the  analytical
ASTM Type II Water - Distilled water with a conductivity  ofNLess  than  1.0
^mho/cm at 25°C.  For additional sp/ecj.fications refer  toN^STM^)1193-77,
"Standard Specification for Reager
                                                          o.
                     inten
Calibration - The estao
absorbance, emission
standards.  Calibj^a-&iotxj)roce
this SOW.  Refer to the
method.
Autozero - Zeroing the instrument
to running a standard blank with the

Average Intensity - The average of two di,ff€

Background Correction - A £ettfirriqjie to comp>
contribution to the inst

Batch - A group of s

Breakthrough volume
will be initially
                                                              It  is equivalent
                                                 injections  (exposures).

                                                  for variable background
                                                   ination of trace elements.
                                                  .me.
Calibration B
acidified/ wi,
reagent
preparat
-------
Exhibit G
                                                      SOW No.  XXX -  Ambient Air
Calibration Standards - A series  of  known standard solutions  used by the
analyst for calibration of the  instrument (i.e.,  preparation^of the  analytical
curve).  The solutions are not  subjected  to  the  preparaGlon/method but contain
the same matrix as the sample preparations to  be  analysed./
           Lenient standard
                   of the
   performance  du^ng the
   lire  of theNs^librl
  £nts  being meastnted
  ird and the standar'd^mvtst
ild have  a concentration in
                                                                         on
Calibration Verification (CCV)  - A single element  or/multi^
solution prepared by the analyst to be used  to veri/y
instrument calibration with time and  the instrumei
analysis of samples.  The CCV can either be  one
standards and/or an ICV.  However, all analyte
particular system must be represented in this i'tar
have the same matrix as the samples.  The CCV/shc
the middle of the calibrated range.   Analytical /standaroS~run every  10
analytical samples or every 2 hours,  whichever/is  more/frequent,  to verify the
calibration of the analytical system.

Case - A finite, usually predetermined number of\sample/s  collected  over  a
given time period, from a particular site.  Ca^e numbe/s are assigned by  the
Sample Management Office.  A Case consists of orte^pr nib-re Sample  Delivery
Groups.
Coefficient of Variation (CV) - I
arithmetic mean.

Continuing Calibration - Analytical
verify the calibration of the analyti
                                             deviation as
Contract Required Quantitation Limit  (CR
acceptable under the contracj Statement o
more) times the standard ^eviatioh\of seven
blank.
            jrcent  of the
                                                          every  12 hours  to
                                               Inimum level of quantitation
                                                  Generally defined as 3.3 (or
                                                 cate analyses of the method
Control Limits - A rangeywithin which specified measurement results must  fall
to be compliant.  Control limits/ma^be^tsandata^y, requiring corrective action
if exceeded, or adv/soc4,  requi/ins^that nohsompliant data be flagged.

Correlation Coefficient. -  A tvamber  (r) which  indicates the degree of
dependence between two var
-------
Exhibit G
                                                     SOW No. XXX  - Ambient Air
Day - Unless otherwise specified, day shall mean calendar/day.

DDI'- Deionized Distilled water.

Deuterated Chemicals - Those chemicals which contain
isotope that is twice the mass of hydrogen);  used a
quality assurance.
Digestion Log - An official record of the sample
                                                               (hydrogen
                                                                   stem
                                                 :lcer
Dissolved Metals - Analyte elements which
analysis and which will pass through a 0.45

Dry Weight - The weight of a sample based ^n pfercent
drying in an oven.
                   been  digested prior  to

                          ?
                          .s.  The weight after
Duplicate - A second aliquot of a sample that^is trea'
original sample in order to determine the precisi
                                                      Zed the same as the
                                                           method.
Dynamic Calibration - Calibration of an analytical systebKusing calibration
gas standard concentrations in a f
to be analyzed and by introducing
sampling or analytical system in a
or analytical process.

Dynamic Dilution - Means of preparing ca^3
gas(es) from pressurized cylinders are coi
zero air in a manifold so that-allowing
available at the inlet of/the
                                              l__pr very sim
 External
 to  sample
EBCDIC - Extended Bina:

Exposure - A full me
concentration of the' a;
manner that meets t;
peak scan.
                               r  to  the  samples
                           inlet  of  the
                            ,e  normal  sampling
                                             tipn mixtures in which standard
                                               lly blended with humidified
                                                of calibration mixture is
                                                   Code.
                                                ,e of an analyte from which the
                                               in the exitation system in a
                                   tion limit.  It is also referred to as a
         S tandards
          anal
 Extractable
 the  sampl
 semi-vol

 Field  B

 Field  Sample
 in single  or multi
               at  a  known  concentration prior
           factors.

  be  partitioned  into  an  organic  solvent from
  to  gas  chromatography.   Extractables include
  mpounds.

    from the field identified as a blank.

zrial  received to  be analyzed that is contained
  and  identified by a unique EPA Sample Number.
 July,  1991
                                                                     Page  G -  6
-------
Exhibit G
                                  SOW No. XXX - Ambient Air
Flame Atomic Absorption  (AA)  - Atomic  absorption which -ut^izes flame for
excitation.
Graphite Furnace Atomic Absorption (GFAA)  -  Atomic abs
graphite cell for excitation.
Holding Time - The elapsed  time  expressed in days
the sample by the Contractor  until  the  date of it

Independent Standard  - A contractor-prepared stj
composed of analytes  from a different source
for the initial calibration.
                                        on which utilizes a
                                                                    receipt of
                                                   those used in the
                                                       rds
Inductively Coupled Plasma  (ICP)  -  A technique/for the/simultaneous or
sequential multi-element  determination of/feleinents in/solution.   The basis of
the method is the measurement  of  atomic emission by An optical spectroscopic
technique.  Characteristic  atomic line emissiort^pedtr/ are produced by
excitation of the sample  in a  radio frequencJy^inducti^rely coupled plasma.

In-House  - At the Contractor's facility.
Initial Calibration  - Analysis  ofy
different specified  concentratior
range of the response of  the  anal}
                       il standards for-^/series of
                 used to define—thglinearity and dynamic
               ;icaj~~iftst*ument to the~~j£arget analytes.
Initial Calibration Verification  (ICV\ -^olu^ionCs)  obtained from the EPA or
prepared from stock standard  solutions\metxa4s hr. salts obtained from a source
separate from that (those) utilized to prepare/the calibration standards,  and
that have known concentratioji-jcalues.   The\ICV\is used to verify the
concentration of  the calitfration5±andards  and  the adequacy of the instrument
calibration of the calibrat>on-~-startdards  and \he \dequacy of the instrument
calibration.  The ICV  fs  not  res\ri
-------
Exhibit G
                                                      SOW No.  XXX - Ambient Air
Interferents  - Substances which affect  the  analysis  for phe/lement of
interest.

Internal Standards  - Analytes added to  every  standard/  blfenk,  sample (for
VOAs), and sample extract (for semi-volatiles)  at  a  Ifcnown concentration,  prior
to analysis.  Internal standards are used as  the ba/is/f^auanbitation of the
target analysis.                                   '   '     ^^    ^^
Laboratory - Synonymous with Contractor as used/herein.
Laboratory Control Sample - Aliquot spiked
specific analytes and subjected to the entir,
monitor method and contractor performance.

Laboratory Receipt Date - The date on whi
Contractor's facility, as recorded on the
sample Traffic Report.  Also referred to as
receipt).
                 lown concentration  of
                          'ocedure in order  to
                       received at  the
                      ivery  receipt and
                     dated time of  sample
Linear Range - The concentration range over which the arta^ytiokl curve  remains
linear.  The range of the instrumefttto?—*-sp£cific analyte>As determined
using calibration standards.  The\upp^tjj.mit of~~tRrs-ii4Qear range  (determined
at each analysis) is the highest c^ce\tratiOTi--^alibration7standard that has a
determined value within 10% of the khownXvalue/

Mass Spectral Interference - Defined asXthe^inability to detect the internal
standard quantification ion due to preserve of/high levels of mass  spectral
"noise" at the same mass.
Matrix - The predominan
composed.
Matrix Modifier - S
interf erents,  visco
Matrix Spike - Aliquot
specific analytes and subfec.ted
indicate the appropriateness
recovery

Mega®-bore
narrow bo
    which the\sam>le to be analyzed is


                effects of chemical
Method
method
concentrati
e fortified (spiked) with known quantities of
  the entire analytical procedure in order to
     thod for the matrix by measuring
    of capillary columns,  the other being the
target compounds under this SOW.

  by performing the analytical preparation
 ample.  The solution thus contains the same
 other analytical preparations plus any
July, 1991
                                   Page G - 8
-------
Exhibit G
                                                      SOW No.  XXX -  Ambient Air
impurities derived from the preparation process.   For  preparations containing
reagents of variable concentrations,  the method blank  shoXild^match the  maximum
reagent concentration used in the sample preparation(s)
Method of Standard Additions (MSA)  - The addition of  / increments  of a
standard solution (spikes) to sample aliquots of the/same  rize.  Measurements
are made on the original and after  each addition.  jihe/sS^pe, x^intercept and
y-intercept are determined by least-square analys
concentration is determined by the  absolute valu
Ideally, the spike volume is low relative to th<
10% of the volume).   MSA may counteract matrix/ef
spectral effects.  Also referred to as Standard
                                                         e  atialyte
                                                  of/the x-inte"i£ceptr
                                                    pie  volume  (app\The metVtod detection  limit for
metals is t 99 times  the standard deviation  of  ser^en  meTshod blank  analyses.
Of course, all spectral background techniques mustbe operative and the  same
integration times must be utilized as when  actual sampl-e^ are">analyzed.
MS-SCAN - The gas chromatograph (,
where the instrument is programme
to disregard all others.

Narrative (SDG Narrative) - Portion
laboratory, contract, SDG and sample numt
documentation of any problems encountered
with corrective action ta^en andproblem
specifications are
Narrow-Bore Capillary/Co
the wide-bore (Mega-
under this SOW.

Performance Evaluatia
pesticides/PCBs under

Performance Ev,
EPA for Cont

Preparati
inorgani
reagent
and an.
                                                      .ass selective  detector
                                                            target analytes  and
                                                package which  includes
                                               ntification, and descriptive
                                                        the samples, along
                                                 on.  Complete SDG Narrative
                                             illary columns, the other being
                                                 the analysis of compounds
                               -/The continuing calibration standard  for
                                        ,ample of known composition provided  by
                                        'A to evaluate Contractor performance.
                                 procedure, and method blank)  - For
                                  that contains distilled, deionized water  and
                                   the entire analytical procedure  (digested
July,  1991
                                                                     Page  G -  9
-------
Exhibit G
                           SOW No.  XXX -  Ambient Air
Preparation Log - An official record of the sample preparation  (digestion).
Protocol - A compilation of the procedures to be folio;
sample receipt and handling, analytical methods, data,
deliverables,  and document control.  Used synonymo
(SOW).

Qualitative Accuracy - The ability of an analytic
identify compounds.
                                     respect to
                                      and
                                     tement of Work
Quality Control (QC) Check Sample - A sample
of analytes that is analyzed by a laboratory
acceptable identifications and measurement
analyze environmental samples containing
Analyte concentrations are known by the
sample by a laboratory or standard supplie
performing the analysis is highly desirable.

Quality Control Set - A group of 10 analytical sampl
that bracket those samples.

Quantitative Accuracy - The abili
measure the concentration of an ide*
Reconstructed Ion Chromatogram (RIC) -
representation of the separation achiev
total ion current versus retention time
Recovery  - A determinate
comparing measured valuers
spike values.  Recovery isdetermine1

            %Surrog
Relative Response Facto
response of an analyte co
Factors are 'dete
calculation o
the  following e
                              known concentrations
                                  that it can obtain
                                  to be used to
                                ar analytes.
                           pa/ation of the QC check
                             the laboratory
                                    e CCVs  and CCBs
                                  to correctly
                    spectral graphical
                      as chromatograph;  a plot of
                        analytical procedure made by
                         sample against the known
                        iwing equation:

                        x 100*
       A measure of the relative mass spectral
         its internal standard.   Relative Response
analysis ofxstandards and are used in the
    of analyte)s in samples.   RRF is determined by
 July,  1991
                                         Page G - 10
-------
Exhibit G
                                                      SOW No.  XXX -  Ambient Air
      Where
            A  = area of the characteristic  ion  measured
            C  ?= concentration
            is = internal-standard
            x  - analvte of interest
Resolution - Also termed separation, the separatio
chromatogram, calculated by dividing the height o
peaks by the peak height of the smaller peak bei
100.

Retention Time (RT) - The time to elute a spec^ifLfe  chemical  from a
chromatographic column for a specific carrie/  gas flow  tf*ute, measured from the
time the chemical is injected into the gas ptrpam untij: ips  maximum
concentration appears at the detector.

Retention Time Window - Retention time wndow  i^xde/6erm'ined  for  each analyte
of interest and is the time from injection co^elution/of a specific chemical
from a chromatographic column.  The window is  a&tsrminfed by  three injections
of a single component standard over a 24-hour  pericJd^as plus or  minus three
times the standard deviation of-the absolute retention^time  rr  that analyte.
Rounding Rules - If the figure following
the figure :  . dropped, and the retlaine~
example, 11.-,43 is rounded off to 1J
                                                              is less  than  5,
                                                are keptHSchanged.  As an
If the figure following those to be re
dropped, and the last retained figure is
is rounded off to 11.45.
                                        ine^oy is/greater than 5, the figure  is
                                         raise/a by 1.  As an example, 11.446
If the figure following
other than zeros beyon
figure retained is increased by
unchanged if an even/n
while 11.425 is rou/ded/off to
                            five,
                              As/
i retained \s  5\ and if there are no figures
     jure 5\s/dropped,  and the last-place
             odd number or it is kept
         1T7435 is rounded off to 11.44,
If a series of multipte>oper^ioris is to be performed  (add, subtract,  divide,
multiply), all figures ar>xcarrrad through the calculations.  Then  the final
answer is rounded_to _the prop«r^ nuniber of significant  figures.
See  forms  in.

Run  - A co/iti
associataa qi/ality
Stateme
                                       sxceptions.

                              sequence consisting of prepared samples and  all
                              eaaurements as required by the contract
July, 1991
                                                                   Page G  -  11
-------
Exhibit G
                                                      SOW No.  XXX -  Ambient Air
Sample - A portion of material  to  be  analyzed that is  co
multiple containers and  identified by a  unique sample  n

Sample Delivery Group (SDG)  - A unit  within  a sample
identify a group of samples  for delivery.  An SDG  is
samples within a Case, received over  a period of up
from all samples in an SDG are  due concurrently.
defined by one of the following, whichever occurs

            Case; or
            Each 20 samples within a  Case; or
            Each 14-day calendar period  duri
            received,   beginning with rece/pt
            or SDG.
                                                              .ed in single or
                                                            hat is used to
                                                                 20 or fewer
                                                                    days.   Data
                                                                       oup is
                                                              in a Case are
                                                             sample in the Case
                                                        nple  collection method
                                                       jother).

                                                               iber  designated
                                                               ample  Traffic
Samples may be assigned to Sample  Delivery
(i.e., all Tenax® tubes in one  SDG, all  canis

Sample Number (EPA Sample Number)  - A unique  identifi"
by EPA for each sample.  The  EPA Sample  Number  appears
Report which documents information/ontEa'

                                  \  \
Sample Recovery (SR) - The quantity\of^a compotrant/_measured/ in a sample  as
compared to a known quantity  of an isotoplcall/ lifoeleor~cTHnpound injected
directly onto the same Tenax® cartridge^.

Selected Ion Current Profile  (SICP) - A  pi
number for ions of a speci£iett~Tnass.
                                             of ion abundance vs.  time  or  scan
Semi-volatile Compounds/- Targe~fr\conk>ounds with\normal vapor pressures between
1 x 10'1  and  I x  10'7 mn/ He/ and whicKaTeNamenabl/ to analysis by SOW Method
2.
Serial Dilution - Tfte dfy.ution 6f a7 sample by~~4 known factor.  When  corrected
by the dilution facbar, tnV^dilute^i sample must agree with the original
undiluted sample within^-specifie^ limits.  Serial dilution may reflect the
influence of interferents.
Standard Anal;
target compoj/ndsy

Static Ca
concentr
cylinde
                             ticar^determination made with known quantities  of
                              ,rmine rteejkmse  factors.

                                  of an  analytical  system with known
                                as\ obtained from a source such as  gas
                                  d stock  solutions.
July, 1991
                                                                    Page G - 12
-------
Exhibit G
                                                      SOW No.  XXX -  Ambient Air
Stock Solution  - A standard solution which  can be diluted
standards.

Surrogates (Surrogate Standard)  - Compounds  added to e
matrix spike, matrix spike duplicate, and standard;  u.
analytical efficiency by measuring recovery.   Surro
fluorinated, or isotopically  labelled compounds not,
environmental media.
                                                              derive other
                                                            blank,  sample,
                                                             evaluate
                                                              brominated,
                                                                    detected in
Tentatively Identified Compounds  (TIC)  - Compour
are not target compounds, internal standards  oy  s\.
peaks are subjected to mass spectral  library  /ear^hes  for  tentative
identification.

Time - When required to record time on  any/deliverable7 ipem,  time  shall be
expressed as Military Time, i.e., a 24-hour

Total Metals - Analyte elements which have often  digested prior to  analysis.

Traffic Report (TR) - An EPA sample identificationiqrm fii^eol out by the
sampler, which accompanies the sample during  shipment  DSL the^aboratory and
which is used for documenting sampZe"~Cr>Rdij:ion and  receipt^iiy the  laboratory.

Twelve-Hour Time Period - The twelve  Ol2T~fceuc_.time perio37for GC/MS system
tuning, standards .calibration (initial  or contfnu±ng~~c«li]/ration)  begins at
the moment of injection of the BFB analysis ttlat/the laboratory submits as
documentation of compliant tune.  The ti,me\ieripd ends  after  12 hours has
elapsed according to the system clock.

Validated Time of Sample Receipt "WTSR)  - Tttedate  on which a sample is
received at the Contractor's--£a 0.1 mm Hg,
                        :o analysis .toy SOW Methods 1A and/or IB.

Viewing Area AdjustmefttStandard / A solution containing a standard of a
strong atom line -(i .e. ,  CTai and ^weak ion line (e.g., Ba) used to verify the
proper adjustment of_the obsVsvatiolxheight in the plasma for metals analysis
by ICP (see Meth6d^200^2^B forSe_taiD
 10%  Frequen
 allowing
 verificat
                                cification during an analytical sequence
                                 ytical  samples  between required calibration
                                   ified  by the contract Statement of Work.
July,  1991
                                                                    Page G -  13
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U.S. Environmental Protection Agency
Region 5, Library (PL-12J)
77 West Jackson Boulevard, 12th Floor
Chicago, IL  60604-3590
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