s>EPA
             United States
             Environmental Protection
             Agency
             Region 5
             Central Regional Lab
             536 South Clark Street
             Chicago. Illinois
January 1984

905R84112
State Agency Access
To The National
Contractor Laboratory
Program
  QUALITY ASSURANCE
  -. ' • . AMI*
   DATA REVIEW

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     STATE AGENCY ACCESS TO THE NATIONAL CONTRACTOR LABORATORY  PROGRAM

                    Narrative Audio/Slide Presentation

                                (SLIDE 1)

     Hello and welcome to  the  Region  V training program whlcn  1s  Intended
to familiarize  State  Agency  personnel  with  the  requirements  of  the  EPA
Contractor Laboratory Program  herein  referred  to as the CLP or  NCLP.   "N"
stands for National.

     I am  Chuck  Elly,  Sample  Analysis  Coordinator for  the  EPA Region  V,
Central  Regional Laboratory (CRL), Chicago.

     I have prepared slides which, if followed,  samplers would  have  all  of
the information necessary to successfully sample, maintain custody,  complete
forms and send samples  to National Contractor Laboratories.

     Additional slides  were prepared  by  Ms.  Marcia  Kuehl,  Region  V,  CRL
Quality Control  Coordinator  and  will   acquaint  you  with   the  elements
necessary to successfully  review  data  generated  by the National  Contractor
Laboratories.

                                (SLIDE 2, 3)

     These slides are intended  to  Illustrate the  mass of paperwork generated
by the program, that doesn't mean that 1t 1s bad however.  That's a picture
of me in my office.

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                                 (SLIDE 4)

ELIGIBILITY REQUIREMENTS:   1)  Samples  collected must  be  from a  Superfund
Site or  potential   Superfund  site;  2)   States  must  have  a  cooperative
agreement with EPA, Remedial Response  Branch  or permission  from a Remedial
Response official.  (This is also known as the 3012 Program.)

                                 (SLIDE 5)

REQUESTING PROTOCOL
1.  The first  step is to  submit a  study plan to  the  U.S. EPA,  On-Scene
Coordinator (OSC) the Remedial  Response Branch.
2.  Case set-up is with the EPA,  Sample  Management  Office (called  the  SMO)
which I am responsible for.   State personnel will  eventually  be  delegated
this task.
3.  Shipping requirements are the  responsibilities  of  State personnel, and
are explained in later slides.
4.  Quality  assurance  and  data  review  are  the  responsibility  of  State
samplers and reviewers, and  will be  explained  in detail  by Marcia  Kuehl.

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                                 (SLIDE  6)


STUDY PLAN REQUIREMENTS


1.  The  Information  shown  here are  the items  which  absolutely  must  be
Included in the plan  submitted to the EPA, OSC.


     A.  Number of samples (add to this  blanks and  duplicates).

     8.  Parameters (such as Priority Pollutant  organics, Task 1&2 Metals,
     etc.).  I will explain the term Task 1  and 2 Metals on later slides.

     C.  Matrix types (water,  soil/sediment,  oil,  fish, tissue).

     0.  Concentration level  (low,  medium,  high  -  these  are  contractor
     terms and I will  explain  these later also).

     E.  Survey  type  (Routine  or  SAS  - routine  means  standard  priority
     pollutant organics,  Task  1, 2,  or  3 inorganics with a  turnaround time
     of 30 days).  SAS stands  for Special Analytical Services  - and will be
     explained on later slides.

     F.  Shipment date (this must  be firm,  since National   Contractor Labs
     are reserved by  date).

     6.  Order for bottles - cleaned bottles  are available through  the CLP.
     It takes 3 to 5 weeks after I  send  the  order  in for routine requests.
     Emergency orders can be telephoned  in and speeds up the time
     substantially.

     H.  SAS Request,  if  applicable (I  have prepared 3  slides  which will
     show you the required information)  if necessary.  SAS's should be very
     infrequent.  They help  to use up the routine lab capacity.

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                                 (SLIDE 7)

1.  OSC sends study plan to Chuck Elly.
2.  Elly reviews study plan.
3.  If Elly  has comments,  OSC negotiates  differences  with State  contact
person.
4.  If  no  comments,   Elly  sends  copy  of  approved  study  plan  to  OSC.
5.  Elly sets up case with SMO.
6.  Elly  telephones  information  to designated  State  contact and  approves
SAS request (if any).
7.  Elly sends SMO  forms  and returns copy of bottle order form to designated
State contact.  Note  that  only one  State person should be  the designated
contact with Elly.
                                 (SLIDE 8)  .

     When are SAS's required?

1.  For atypical matrices such as oils  and tissues.
2.  Faster turnaround times than  30 days.
3.  Parameters other  than  the 114 Priority Pollutant Organics  or  the  Task
1, 2, or 3 Inorganics are requested.
4.  Lower detection limits  or more extensive  quality control   than  in  the
regular IF3s are requested.  (IFBs stand for Invitation  to  Bid.)
5.  Dioxins/Furans  are requested.
6.  EP Toxicity,  Flashpoint,   or  other RCRA  solid  waste parameters  are
requested.
7.  Items not mentioned above  are requested.

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                                 (SLIDE 9)

     Sample Descriptions;

     These are terms, defined  in  the contract which must, repeat must,  be
placed on the traffic forms, since  National  Contractor  Labs  have  contracts
based on concentration levels.  Definitions will be given  on later  slides.

     1.  Low
     2.  Medium
     3.  High

                                 (SLIDE 10)

     Orgam'cs Analysis Data Sheet  II

     This is the top  sheet of  the three page analysis  from  which contains
the priority pollutant acids, base neutral and volatile compounds.   (Consult
Appendix C of the SMO  Users Guide to the EPA Contractor Laboratroy  Program.)
The upper  right  hand corner  will  contain  the  laboratory traffic  number.
Results are generally reported in  micrograms per liter (ppb)  for waters  and
micrograms per gram (ppm)  for soil/sediment.

                                 (SLIDE 11)

     Organics Analysis Data Sheet  12

     This sheet includes- the chlorinated pesticides, PCBs, and non-priority
pollutant compounds.  A third sheet is  almost always included which contains
the tentatively  Identified  compounds; which  Marcia Kuehl explains  later.

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                                 (SLIDE 12)

     Inorganic Analysis Data Sheet

     This is a one-page form  which  Includes  all  of  the  Task  1  and  2  Metals
and Task  3  parameters.   Task   1   parameters  are  generally  analyzed   by
Inductively coupled argon  plasma (ICAP) or  atomic absorption (AA for short).
Task 2 Metals  are those  generally  analyzed  by flame!ess AA.   Ammonia  and
sulfide are SAS parameters.  They used to be Task 3  parameters.

                                 (SLIDE 13)

     Definitions - Low Concentration Samples

A.  0-10 ppm of a single contaminant
B.  Environmental  soils and water  samples,  groundwaters, surface waters,
most off-site  wastes,  soils,  wells,  leachate  springs,  ditches,  rivers
C.  Any diluted samples
D.  Low-hazard samples

                                 (SLIDE 14)

     Medium Concentration  Samples

A.  10 ppm to 15% of a single contaminant
B.  On-site water-soil  samples, samples lying  beside drums,  lagoons,  on-
site impoundments, leachate collection pools, on-site ditches
C.  Areas of direct, but diluted concentrations
0.  Medium-hazard samples

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                                 (SLIDE 15)

     High Concentration Samples

A.  15% to 100% of a single contaminant
8.  Samples collected from drums, surface Impoundments, storage tanks,
spills or direct discharges from Impoundments  l
C.  Little or no evidence of dilution
D.  High, unknown hazard

                                 (SLIDE 16)

     Sample Size and Preservation; Orgam'cs  -  Low  Level:

A.  Waters:

     For Extractables:   You must send two one-half gallon  amber narrow neck
                        glass bottles with teflon-inserted cap and iced to
     For Volatiles:   Two 40-ml  Borosilicate glass vials, each sample, iced
     to 4°C.

B.  Soils:

     You must send one 8-ounce wide-mouth  glass jar, with  a  teflon  insert,
     iced to 4°C for each sample.

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                                 (SLIDE  17)

     Sample Size and Preservation;  Organics  - Medium Level

A.  Waters (Extractables and VOAs)

     You may send four 32-ounce or eight 16-ounce wide-mouth  glass bottles
with teflon-inserted caps  for  each sample.   You  will  see  later that the
bottles must be sent in one-half gallon  paint cans.

8.  Soils

     You may send one 8-ounce wide-mouth glass bottle  with  teflon-inserted
cap for each sample.  No preservative.

     Medium soil samples  also have  to be sent  in one-half gallon paint cans.

                                 (SLIDE  18)

     Orgam'cs and Inorganics -  High Level

     These include concentrated waters,  liquids, soils, sludges,  solids out
of drums.

     You must send one 8-ounce  wide-mouth glass bottle  with  teflon-inserted
cap for each sample.  No preservative.

     If EP Toxicity or Flashpoint  is  requested, you  should send two 8-ounce
glass bottles.

     Each sample must be sent in a  one-half  gallon  paint  can.

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                                 (SLIDE 19)

     Sample Size and Preservation;  Task 1  and 2 Metals  - Low level

A.  Waters

     You must send one, one-liter high density polyethylene bpttle
preserved with 3  ml  of 1:1 HN03  or the  sample must  be preserved to a  pH
of 2.

B.  Cyanide

     You may  send  one, one-liter  or  one  500 ml high  density  polyethylene
bottle for each sample preserved with 5 ml of  six  normal  sodium hydroxide.
The sample must be iced to 4°C.

C.  Soils

     You may  send one  8-ounce  plastic or  glass wide-mouth  bottle  for each
sample.  The sample must be iced to 4°C.

                                 (SLIDE 20)

     Sample Size and Preservation;  Inorganic  - Medium Level

A.  Water and Soils

    1.  Task 1 and 2 Metals
    2.  Cyanide
    3.  Ammonia
    4.  Sulfide
B.  You must  send  one  8-ounce  plastic or  glass wide-mouth  bottle  for each
sample.
     No preservative.
     Each sample must be sent in a one-half gallon paint can.

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                                   (SLIDE 21)


  1.  Routine

      A.  Low and medium soil and water samples;  30 days.

      8.  High concentration samples;  51  days  (this Includes 21 days at  the
  EPA, National  Enforcement  Investigations  Center Laboratory -  Fred  C.   Hart
  Associates Contractor, and 30 days at the National  Contractor Laboratory).


  2.  Special Analytical Services (SAS)


      A.  Low and medium soil and water samples; 2 days to 30 days (a  frequent
  request is for 14 to 21 days.

      3.  High concentration samples; 5 days to 30 days.


                                 (SLIDE 22)


     Field Quality Control; Low and Medium Samples


     You should send for each group of samples:

1.  A Field Reagent blank containing distilled-dionized water for
inorganics (carbon-free  water  for   organics).   The  reagent  blank  should
also contain  a  preservative.   Example  for low  metals,  you  should  send
one-liter of distilled-dionized water plus 3 ml of 1:1 HN03.

2.  A duplicate of one of the samples in a batch.


     High Hazard Samples

1.  A reagent blank is not necessary.

2.  But you should send a duplicate of one of the samples.

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                                 (SLIDE 23)


     For the  Contract  Laboratory  Program,  you  must  do  the  following.


1.  Use  U.S.  EPA  Chain-of-Custody forms  and  sample  tags.   Seals  should
be used on the picnic coolers.

2.  Every  member  of  the sampling team must  be listed  on the  Chain-of-
Custody form. •

3.  Information  on the  sample  tag  and  the  cha1n-of-custody  forms  must
match.

4.  Cha1n-of-Custody  forms  must be  completed properly  (as you  will  see
on the next slide).

5.  The  method of shipment  should  be  listed  in  the  lower  right-hand
corner of the Chain-of-Custody form under "Remarks".

6.  A  separate chain-of-custody of  custody  form  must  be  sent  for  each
site and  for  samples  sent  to each   lab.   (Generally  one  custody  for
will be sent to the Organic Lab and one to the Inorganic  Lab.


                                 (SLIDE 24)


     This 1s a picture of a Chain-of-Custody form.


     The project  number  should  contain  either  the  partial   or  entire
laboratory sample  number.   An  example  of  an  EPA  laboratory  number  is

"83-CY05S01".  The Federal  Fiscal  Year 1984,  started  October 1,  1983,  so
the 83 number  becomes  "84-CY05S01".   Note the  requirements for date, time,
and station location.  Time may be either conventional  or  military.   The
number of containers and the parameters requested per sample must be listed
clearly.

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                                 (SLIDE 26)

     This is a picture of a sample tag.  One tag  must  be  attached to  each
bottle and should contain the laboratory number,  date, time,  names  of
samplers, station location, parameters, and preservative  (if  any).

     Note also that it is a good idea to 11st the traffic numbers from the
SMO traffic form.  In this case it was organics as noted  by the  number E5123.

                                 (SLIDE 27)

     Sample Custody Tag (Address Side)

     This is the reverse side of the tag.  Note that the  U.S.  EPA Region V
Regional  Office is the official address.  The EPA, Region V Laboratory is
actually located at 536 South Clark Street, Chicago.

                                 (SLIDE 28)

     Official  Seal

     This is an  illustration  of the  Region V Offical  Seal which should be
secured.   Transparent red  or  clear tape  should  be used  over the  seal.  A
broken seal indicates that the cooler has been tampered with.  If it  was by
anyone other than the  designated  laboratory custodian,  custody is broken.

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                                 (SLIDE 29)


     Forms required for shipment  of  samples to NCL's.  (Note that Region V

will supply all  forms.)


     Low and Medium Samples


1.  The  SMO  Organic Traffic  report  and the Inorganics Traffic  report are
required for all routine sample requests.  Illustrations of these forms are
shown on the next two slides.

2.  Packing List form  for  SAS's,  when the packing list is  used  on organic
and inorganic traffic forms is not required, unless the SAS also contains a
routine case request (seldom), I will indicate if a  traffic form is required.

3.  EPA Chain-of-Custody Form

4.  EPA Sample Custody Tag.

5.  EPA Custody Seal

6.  Stick-on  label  from  the  Organics  Traffic  Form.   Each traffic  form
contains a stick-on label  containing a laboratory number (such as E5000 for
organics and ME5104 for inorganics).

     This label  should be  removed from the traffic form and placed on the
sample bottle.   In  some cases  there are  enough labels  to put  one  on the
bottle and one on the sample custody tag.

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                                 (SLIDE 30)

ORGANICS TRAFFIC REPORT

     This form must  accompany all  samples  for routine  organics  analysis.
Two very important items are:  the  case  number and the  concentration  type.
If you make  a mistake  and check medium  concentration  when you  meant  low
concentration, the  NCL will  expect  you  to  send  four  32-ounce  bottles
instead of two one-half gallon  bottles.   They will  also note that  you  did
not send  the  samples  in   cans   and  possibly exposed  them  to hazards.

     It is also a good idea to put your laboratory sample  number  somewhere
on the form.  EPA samplers  put it under the case number.

     Other items,  such  as the  National  Contractor  Laboratory address,
matrix type,  number  of sample bottles,  sample description, and method  of
shipment, must be completed.

     The Special  Handling  Instructions column  at  the bottom  of the form
should be used  to  note  any hazards  or  other  information  related  to  the
sample.

                                 (SLIDE 31)

INORGANICS TRAFFIC REPORT

     This form  must   accompany  all   routine  low  and  medium  samples.   It
contains the same information  as  the organics form except  for the  parameter.
At the bottom left-hand  corner  there  is a  statement  which says "Matches
Organic Traffic Report No.XXXX.

     It's a good idea to complete this column,  because it  helps to  resolve
sample bottle mix-ups.  And mix-ups  do occur—believe  me.

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                                 (SLIDE 32)


FORMS REQUIRED FOR HIGH HAZARD SAMPLES


     Don't forget these are  samples generally  out  of drums and go  to  the
NEIC first for extraction and dilution then to National  Contractor  Labs  for

analysis.


1.  The SMO High Hazard Traffic Form  (a packing list  is  sometimes  required
when additional tests,  such  as HP  Toxicity  or Inorganics  are  requested).

2.  Hazardous Waste Sample Preparation Request Form (a picture os this form
will be shown on the slide after the high hazard traffic form).

3.  EPA Chain-of-Custody Form and Tag

4.  The EPA, Region V Custody Seal

5.  The stick-on label  from the High Hazard Form

6.  A Hazardous Shipping Certificate (a picture of the certificate  is shown
in later slides.


                                 (SLIDE 33)


HIGH HAZARD TRAFFIC REPORT


     This form 1s very  similar to  the  other reports, except that it is  a

combined Organics/Inorganics  form.   It 1s very important  to fill  out  the
known or suspected hazards column.

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                                 (SLIDE 34)

THE HAZARDOUS SAMPLE PREPARATION REQUEST FORM

     This sheet  is  very  similar  to the  chain-of-custody  form  but  must
accompany the Cha1n-of-Custody form and High Hazard sheet for each group of
samples.  You may check  any  or all of the  preparation  fractions  under the
column "Check Preparations  Requested".   The parameters  you  will  get  are:

     Total Metals (similar to Tasks 1 and 2 Metals)
     Total Mercury
     Strong Acid Anions ($04 , Cl , N03 , F )
     Volatile Organics
     Base Neutrals, Acids, TCDD (Dioxins)
     Pesticides, PC8s
     Other

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                                 (SLIDE 35)

PACKING LIST

     This 1s a  picture  of the Packing List  Form which must accompany  all
samples analyzed under an  SAS  request.   My name will always appear  as»the
Regional Contact.

     Note the  SAS number  in  the  top  right-hand  corner  of  the  sheet.

     In the  left-hand  corner  you  will  see the  sample  number.   The  SMO
Coordinator prefers that you  use sample numbers starting  with  355E-1, E-2,
and continuing to the last sample such as 355E-4 in  this case.   You can  put
up to 20 samples on each packing list.  It is better to  put  your laboratroy
sample number  under  the  additional  "sample description"  column  and  any
other pertinent  information  that you can  fit  on  the  sheet.   Somewhere
towards the bottom of the sheet, you should Indicate  your parameter request.
In this case the request was for PCBs only.  (This  means  not  the Pesticides/
PCB fraction, but only the PCS fraction.

     At the bottom of the four-page  form are instructions  as to what  copies
go where.  (Two get shipped with the  samples,  one goes  to SMO, one is kept
by the sampler, and the sampler sends one copy to me.)

                                 (SLIDE 36)

REGIONAL REQUEST - SAS FORM

     This three page  form should be completed for all  SAS's.  This particular
SAS Involved the analysis of fish samples  at Chem Dyne for Priority Pollutant
organics (no volatiles  - volatiles   can't  be done  in  fish).  The request
also was  for the  analysis  of  C-56 (which  1s  hexachlorocyclopentadiene).
Note that  % Lipids  is  a  requirement  for  all  fish.   Item  2  requires
specification of the  number of samples and matrix type or level concentration
for each sample.   Items 3, 4,  5  require  program specification  and dates of
collection and shipment.

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                                 (SLIDE  37)
                               Page 2 slides

     Item 6 of the sheet requires the number  of  days  to  complete the  sample
analyses.  While Items 7, 8, 9 deal with the  analytical  protocols, special
technical Instructions and analytical  results requirements  (deliverables.

     Item 7 for example stated to use the attached  CRL Method  for the
analysis of non-volatile extractable organic  compounds,  sections of the
method are referred to for % lipids, grinding and clean-up.

     Item 8 of the form is for special  instructions,  i.e.,  for spiking with
various compounds, detection limits specification,  etc.).

     Item 9 we usually  specify to report all  raw  QA/QC information inclusive
of re-constructed ion chromatograms, library  searches, and  computer
calculations.  Instrument and method blanks must be specified  and sent with
the data.

     Item 10.   "Other"  column  is  used to  state  that  detection  limit
verification should be done by spiking at levels below the  listed detection
limit of the method.

                                 (SLIDE  38)

     Page 3 of the  form is a supplement  to  instructions  on  page 2.  Data
requirements include the parameters, detection limit, and precision
requirements.  While  QC requirements Include the  audits,  frequency,   and
limit requirements.

     Item III is an invitation for the  requestor to  specify the quality  of
data he can live with.  In some cases, 1f audits are  out-of-control a rerun
may not be necessary.

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                                 (SLIDE 39)


DEPARTMENT OF TRANSPORTATION (DOT) SHIPPING REGULATIONS


     These apply mainly to medium and high hazard samples.   The  bottles  and

preservatives amounts  for  low  samples  are  generally  exempt  from  DOT

regulations.


1.  Each  sample  bottle must be  placed in a one-half  or a one-gallon  can
(generally paint cans are used).

2.  Each  sample  bottle must be  placed inside  a plastic bag  which can  be
sealed.

3.  Vermiculite or other  absorbent material  must  be  placed  inside  the can.

4.  The paint can top must  be  sealed with five (5) clips or  can  be taped.

5.  The NCL address and the hazard label must be put  on each can.

6.  A Hazardous Shipping  certificate  (also  known as  Shippers  Certification
for restricted articles) must be completed for each group of  samples  sent.

7.  The cans  must  be packed in  a metallic  or  rigid plastic  picnic cooler
which is  able to  withstand a  4-foot  drop  without breakage of  samples.

     The picnic cooler must be labeled with the following information.


          1.  EPA label
          2.  "THIS SIDE UP" labels  (2)
          3.  "UP" arrow  (4)
          4.  "DANGER" label
          5.  "FLAMMABLE SOLID" (or  LIQUID)
          6.  "FLAMMABLE SOLID, N.O.S. (or LIQUID N.O.S.)
          7.  Laboratory address label
          8.  Number of samples in shipment
          9.  Number of cans in ice-chest.


                                 (SLIDE 40)


     Here's an illustration of  a  cooler that  is  ready to go, with all of  the

labels.

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                                 (SLIDE  41)


SHIPPERS CERTIFICATION FOR RESTRICTED  ARTICLES


     This is a picture of the Federal  Express Form.


     If you were shipping hazardous wastes  for  example,  you would put the
following information on the form.


     Flammable liquid, Flam Liq, NOS

     Corrosive solid
     Corrosive liquid, etc.


                                 (SLIDE  42)


SMO SHIPPING REQUIREMENTS


     This information is required by the Sample  Management Office within 24

hours after samples are  shipped.   It  is a good idea to do it the same day
of shipment.


     You should telephone me at (312)  353-8370 with  the following.


          1.  Carrier and Air Bill  Number
          2.  The Case Number
          3.  The Laboratory the samples were shipped to
          4.  The date of shipment
          5.  The number of samples
          6.  The number of picnic  coolers

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                                 (SLIDE 43)


INTERNAL RECORDKEEPING
1.  It is a good Idea to keep a log with the  SMO  Case Numbers  after a case
has been set up.  A picture of my log is shown on  the next  slide.

2.  The  Central  Regional  Laboratory data  coordinator  also  maintains  an
internal tracking sheet which tracks  sample collection through  data  review.
I'll show you a picture of our sheet  on  a subsequent slide.

3.  Raw data returned:

     A.  Unfortunately, I was unsuccessful  in my  request to have the data
     send directly to the  State  requestor.   It would mean a change in the
     contract and SMO will  not do it.

     B.  State  Agency  data  will   be sent  to  me and  I  will  forward  it
    (unreviewed) to the State Agency  Contact.

     The additional information listed below  is not  in the slide-audio but
should be followed.

     C.  The State reviews its own data.

     0.  State  Contact  sends copies  of  all   Data  Review summaries  to  the
     Regional NCL Coordinator.

     E.  State Contact refers all  un-resolvable. non-routine  QC problems to
     the new Regional  Deputy Project  Officer (DPO).  State  Contact resolves
     all routine QC problems.

     F.  NCL Coordinator refers the QC problem to the Regional  DPO  for the
     laboratory which has the QC problem.

4.  Return of picnic coolers.

     This same procedure will be followed for the  return of picnic coolers.
However, you  can  solve  this problem by  putting   your  return   address  and
stick-on labels on the  coolers  and they will   be  returned  directly  to you.

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                                  (SLIDE 44)

 VIAR CASE PLANNING LOG


     This is  a  picture of the form which I use for pending and future cases.

 After the data  are received, I file this sheet.  It includes the case

 number,  site  name, originator, parameters, projected number of samples,
 actual number of samples, projected shipmnet date, NCL, etc.


                                  (SLIDE 45)

 INTERNAL TRACKING SHEET


     This is  the most valuable document we have to track the whereabouts of
 samples.


     The sheet  includes the following.


     1.  EPA  Data Set (which is how we log samples in)
     2.  Decision Units/Activity Number (Superfund Projects are
         Decision Units  Y905 and Y306)
     3.  Case Number and/or SAS Number
     4.  Number of samples and parameters
     5.  National Contractor Laboratory
     6.  Date samples were shipped by the collector
     7.  Date the analysis results are done (31 days after shipment)
     8.  1st  arrival  date of data results at  the Central  Regional  Lab
     9.  Last arrival date (for which all data are in)
    ID.  Contractor turnaround time for analysis
    11.  Date of Data Analysis Review by the  Central  Regional  Lab
         chenri st
    12.  Date the data were sent to the Data  User
    13.  Time (in hours)  it took the chemist  to review  the data
    14.  The turnaround time it took from the time the  data arrived  at  the
         Central Regional  Lab to the time it  was sent to  the Data  User


     This concludes  my  presentation.  If  there  are any  questions,  please
refer to the  Region  V  Sample Handling  Protocol  for Hazardous  Waste  and the

SMO Users Guide to  the  EPA  Contractor Laboratory  Program,  both  of which

were sent to your Agency.


     Additional  ...now Marcia Kuehl will present  slides which  will acquaint
you with other areas  of the Contractor Laboratory Program.

-------
      STATE AGENCY ACCESS
            TO THE
             EPA
CONTRACTOR LABORATORY PROGRAM

-------
           Eligibility Requirements

1.  Samples must be from a Superfund site (EPA,
   Hazardous Waste-National Priorities List) or a
   Potential Superfund Site.
2.  States must have co-operative agreements with EPA,
   Remedial Response Branch or Permission of EPA,
   Remedial Response Branch to use National
   Contractor Laboratories.

-------
     REQUESTING PROTOCOL
1.  Submittal of Study Plan
2.  Case Set-Up
3.  Shipping Requirements
4.  Quality Assurance and Data Review

-------
   STUDY PLAN REQUIREMENTS

1.  Submit To EPA OSC
2.  Include:
    A.  Number Of Samples
    B.  Parameters
    C.  Matrix Type
    D.  Concentration Level
    E.  Survey Type
    F.  Shipment Date
    G.  Order For Bottles
    H.  SAS Request If Applicable

-------
                   CASE SET-UP
1.  OSC Sends Study Plan To Chuck Elly
2.  Elly Reviews Study Plan
3.  If Comments, OSC Negotiates Differences
   With State Contact.
4.  If No Comments, Elly Sends Copy Of The Approved
   Study Plan To OSC
5.  Elly Sets Up Case With SMO
6.  Elly Telephones Information To Designated State
   Contact And Approves SAS Request (If Any)
7.  Elly Sends Forms & Returns Copy Of Bottle Order
   Form To Designated State Contact.
  9

NOTE: Only One State Person Should Be A Designated
               Contact With Elly

-------
        WHEN TO REQUEST SAS

1.  For Organic And/Or Inorganic Analysis Of Oils Or
   Other Atypical Matrices Such As Fish, Mammal
   Tissues, Air.
2.  For Parameters Other Than The 114 PP Orgs Or
   Task 1,2,3 Inorganics
3.  For Lower Detection Limits Than In The Regular
   IFB's. For Quality Control Which Is More
   Extensive Than In The Regular IFB's.
4.  For Quicker Turnaround Times Than The Normal
   30 Days Of The Regular IFB's.
5.  Foe EP Toxicity, Flashpoint And Other RCRA
   Solid Waste Parameters.
6.  Dioxins/Furans Are Requested.
7.  Other Requests Not Covered Above.

-------
SAMPLE DESCRIPTIONS
1.  Low Concentrations
2.  Medium Concentration
3.  High Concentration
4.  Analysis Parameters

-------
US. ENVIRONMENTAL PROTECTION AGENCY - CLP Sample Management Offic*
P.O. Box SIS, Alexandria, Virginia 22313 - 703/557-2490
ORGANICS ANALYSIS DATA SHEET
Laboratory Name: • Cue Not
Lab Samole ID. No:
Pff
(21A)
(22A)
(24A)
(31 A)
(34 A)
(37 A)
(3SA)
(39 A)
(60 A)
(64 A)
(63 A)
(IB)
(38)
(SB)
(9B)
(12B)
(18B)
(20B)
(23 B)
(26 B)
(27 B)
(28 B)
(33B)
• (36B)
(37 B)
(39B)
(40B)
(4 IB)
(428)
<43B>
* -~ (52B)
(33B)
(54B)
(33B)
(568)
(628)
(638)
(668)
(67B)
(6SB)
(6*6)
(70S)
(718)
(72B)
CAS*
$8-06-2
39-50-7
95-57 -S
120-83-2
105-67-9
SS-75-5
100-02-7
51-2S-5
534-52-1
87-86-5
108-93-2
Sample Nunbe-
ESV3-3

OC Report Not
Multiply Detection Limits by 1 Q or 10 Q (Check Box for Appropriate Factor)
ACID COMPOUNDS BASE/NEUTRAL COMPOUNDS
«R/> «Vt
oru»/V» oruR/kg
(circle on*) PP« CAS* (circlTone)
2,4,6- trichlorophenol (738) 50-32-8 benzo(a)pyrene «
p-cft loro-m^reso 1
2- ctilorophenol
2,4-dichlorophenol
2, 4-dimethy (phenol
2- nitrophenol
4-flitrophenol
2,4-dinitrophenol
4,6-dinitro-2-fhethylphenol
pentachlorophenol
phenol
BASE/NEUTRAL COMPOUNDS
83-32-9 acenaphthene
92-87-5
120-82-1
1 18-74- 1
67-72-1
111 -44-4
91-3S-7
95-50-1
541-73-1
106-46-7
91-94-1
121-14-2
606-20-2
122-66-7
206-44-0
7005-72-3
101-55-3
39638-32-9
111-91-1
87-68-3
77-47-4
78-59-1
91-20-3
9S-95-3
86-30-6
621-64-7
117-81-7
85-68-7
84.74-2
117-84-0
84-66-2
131-U-J
56-55-3
benzidine
1,2,4-trichlorobenzene
hexachlorobenzene
hexachloroethane
bis(2-ch loroethy Dether
2-chloronaphthalene
1,2-dicnlorobenzene
1,3-didilorobenzene
1,4-dichlorobenzene
3,3'-dichlorobenzidine
2,4-d in itr oto luene
2,6-dinitrotoluene
1 ,2-diphenv Ihydrazine
Uuoranthene
4-chlorophenyl phenyl ether
4-bromophenyl phenyl ether
bU (2-chloroisopropyl) ether
bis (2-chloroethoxy) methane
hexachlorobutadiene
hexachlorocyclooentadiene
isophorone
naphthalene
nitrobenzene
N-n i trosod ipheny lamine
N-oitrosodipropylamine
bis (2-ethylhexyl) phthalate
benzyl butyl phthalate
di-n-butyl phthalate
di-n-octyl phthalate
diethyl phthalate
dimethyl phthalate
benzo(a)anthracene
(74B).
(75B)
(76B)
(77B)
(78B)
(798)
(SOB)
(SIB)
(S2B)
(S3B)
(SUB)

(2V)
(3V)
(4V)
(6V)
(7V)
UOV)
(11V)
(13V)
(14V)
(15V)
(16V)
(19V)
(23V)
(29V)
(30V)
(32V)
(33V)

(3SV)
(44V)
(45V)
(46V)
(47V)
(48 V)
(49V)
(30V)
(31 V)
(S3V)
(86 V)
(S7V)
(SSV)

203-99-2
207-08-9
218-01-9
208-96-8
120-12-7
191-24-2
86-73-7
83-01-8
33-70-3
193-39-5
129-00-0
107-02-8
107-13-1
71-43-2
56-23-5
10S-90-7
107-06-2
71-55-6
75-34-3
79-00-3
79-34-3
73-00-3
110-73-8
67-66-3
73-33-4
136-60-5
78-87-5
10061-02-6
10061-01-05
100-41-4
75-09-2
74-87-3
74-83-9
75-23-2
75-27-4
75-69-4
75-71-8
(24-48-1
127-18-4
LOS-SS-3
79-01-6
75-01-*

oenzo
-------
bora wry
Name:
b Sample I.D. No:
PP*
(S9P)
(90P)
(9 IP)
(92P)
(93P)
(94p)
(95P)
(%P)
(97P)
(9SP)
(99P)
(100P)
(101P)
(102P)
•











...... . .^* j^^-^-g—-
Case No:
, QC Report Not
Multiply Detection Limits by I Q or '° D (Check Box for Appropriate Factor)
PESTICIDES PESTICIDES
"8/1 . v«/l
orug/kg orus/Vg
CAS* • (circle one) PP*- CAS* , (circTone)
309-00-2 aldrin (103P) 319-83-7 y^-BHC
60-57-1 dieldrin
57-74-9 ehlordane
30-29-3 4,4'-DDT
72-J5-9 4,4'-DDE
72-54-8 4,4'-ODD
UJ-29-7 cC-endosulfan
1 1 3-29-7 A -endosulf an
1031-07-2 endosulfan sullate
72-20-8 endrin
7421-93-4 endrin aldehyde
76-44.3 heptachlor
1024-57-3 heptachlor epoxide
319-84-6 CC-BHC

ACID COMPOUNDS
^i.
w««/lq{
CAS » (circle one)
63-85-0 ben zoic acid
95-4S-7 2-methylphenol
108-39-a 4-methy!phenot
95-95-4 2,4,5-trichlorophenol
BASE/NEUTRAL COMPOUNDS
62-53.3 aniline
100-31-6 benzyl alcohol
106-47.* 4-chloroaniline.
132-64-9 dibenzofuran
91-57-6 2-methylnaphthalene
gJ-74-4 2-nitroaniline
99-09-2 3-oitroaniline
100-01-6 4-nitroaniiine
(104P) 319-J6-8 «P-BHC
(105P) 58-49-9 y.BHC (lindane)
(106P) 53469-21-9 PCB-1242
(107P) 11097-69-1 PCB-1234
(10SP) 11104-28-2 PCB-1221
(109P) 11141-16-5 PCB-1232
(HOP) 12672-29-6 PCB-1248
(HIP) 11096-82-5 PCB-1260
(112P) 12674-11-2 PCB.1016
(113P) 8001-35-2 toxaphene
DKDXINS
(129B) 1746-01-6 2,3,7,8-tetrachlorodibenzo-p-djoxin

VOLATDLES
"^L
orug/kg
CAS * (circle one)
67-64-1 acetone
78-93-3 2-butanone
73-15-0 carbondisulfide
519-78-6 2-hexanone
108-10-1 4-methyl-2-o«ntanone
100-42-5 styrene
108-03-4 vinyl acetate
93-47-6 o-xylene
4/S

-------
  US ENVIRONMENTAL PROTECTION AGENCY
  HWI Sample Management Office
  P.O. Box SIS - Alexandria, Virginia 22313
  703/557-2*90 FTS S-557-2*90
                                                                        Sample No.
                            INORGANICS ANALYSIS DATA SHEET
LAB NAME
LAB SAMPLE ID. NO.
                                         CASE NO.
                                         QC REPORT NO.
1.   Aluminum

2.   Chromium
3.   Barium
    Beryllium
5.  Cobalt

6.
Copper
7.  Iron
8.  Nickel
9.  Manganese
                        TASK I (Elements to be Identified and Measured)
                             ug/1 or mg/kg
                              (circle one)
                                          10.  Zinc
                                                                        ug/1 or mg/kg
                                                                         (circle one)
                                          11.  Boron
                                          12.  Vanadium
                                          13.  Silver
 1.  Arsenic
 2.  Antimony

 3.  Selenium
    Thallium
                        TASK 2 (Elements to be Identified and Measured)
                             ug/1 or mg/kg
                               (circle one)
                                           5.   Mercury
                                                                         ug/1 or mg/kg
                                                                          (circle one)
                                           6.   Tin
                                           7.   Cadmium
                                           8.   Lead
                        TASK 3 (Elements to be Identified and Measured)
                                                      ug/1 or mg/kg
                                                       (circle one)
                         1.  Ammonia	

                         2.  Cyanide	
                         3.  Sulfide
   COMMENTS:

-------
LOW CONCENTRATION SAMPLES
A. 0-10 PPM of Single Contaminant
B. Environmental Soils & Water Samples,
   Groundwaters, Surface Waters, Most Off-Site
   Waters, Soils, Wells, Leachate Springs, Ditches,
   Rivers
C. Any Diluted Samples
D. Low Hazard

-------
      MEDIUM CONCENTRATION SAMPLES
A.  10 PPM to 15% of Single Contaminant
B.  On Site Water-Soil Samples, Samples Lying Besides
    Drums, Lagoons, On-Site Impoundments, Leachate
    Collection Pools, On-Site Ditches.
C.  Areas of Direct, But Diluted Concentrations.
D.  Medium Hazard

-------
       HIGH CONCENTRATION SAMPLES
A. 15% to 100% of Single Contaminant
B. Drums, Surface Impoundments, Storage Tanks, Spills or
   Direct Discharges From Impoundments
C. Little or No Evidence of Dilution
D. High, Unknown Hazard  -

-------
       Sample Size & Preservation
          Organics - Low Level
A. Waters
    EXTRACTABLES (Acids, B/N's, Pests/PCB )
    Send 2-1 /2 Gal. Amber, Narrow Neck Glass
    Bottles With Teflon - Inserted Cap, Iced to 4 C.
    VOLATILES
    Send 2 - 4O ml Borosilicate Glass Vials With
    Teflon Septums, Iced To 4°C.
B. Soils
    1 - 8 oz. Wide Mouth Glass Bottles With A Teflon
    Insert, Iced To 4°C.

-------
       Sample Size & Preservation
        Organics - Medium Level

A. Waters (Extractables & VOA's)
    4-32 oz. or 8-16 oz. Wide Mouth Bottles With
    Teflon - Inserted Cap. Ship In Paint Cans.
    NO PRESERVATIVE
B. Soils
    1 -8 oz. Wide Mouth Glass Bottle With
    Teflon-Inserted Cap. Ship In 1 72 Gal. Paint Cans.
    NO PRESERVATIVE

-------
SAMPLE SIZE & PRESERVATION
Organics-High Level Inorganics

Waters, Liquids, Soils, Sludges, Solids
     1 -8 oz. Wide Mouth Glass Jar, Teflon
     NO PRESERVATIVE

-------
SAMPLE SIZE & PRESERVATION
Task 1&2 Metals - Low Level
    Waters
    1-1 Liter HD Plastic
         3 ml 1:1 HNO3
         or to pH 2.
Cyanide
    1-1 Liter HD Plastic
         5 ml 6N NaOH
         Iced to 4  C.
    Soils
    1-8 oz. Plastic or Glass Bottle
    Iced to 4 C.

-------
         SAMPLE SIZE & PRESERVATION
Inorganic * Medium Level
    A.  Water & Soils
         1.  Task 1&2 Metals
         2.  Cyanide
         3.  NH3
         4.  Sulfide
    B.  1 -8 oz. Plastic or Glass, Wide Mouth Jar
        NO PRESERVATIVE

-------
               TURN AROUND TIMES
1.  Routine
    A.  Low and Medium Soil and Water Samples
        30 DAYS
    B.  High Concentration Samples
        51 DAYS
2.  SAS
    A.  Low and Medium Soils and Water Samples
        2 to 30 DAYS
    B.  High Concentration Samples
        5 to 30 DAYS

-------
FIELD QUALITY CONTROL
Low & Medium Samples
    1. Field Reagent Blank
    2. Duplicate of Sample
High Hazard Sample
    1. Duplicate of Sample

-------
       CHAIN OF CUSTODY
Requirements
    1. USEPA Forms & Tags, Seals (Optional)
    2. Sampling Team Listed
    3. Info on Tags & Forms Match
    4. Custody Forms Completed Properly
    5. Method of Shipment Listed
    6. SEPARATE FORM FOR EACH SITE & LAB,

-------
                       CUSTODY
A Sample Is In Your Custody If The Following Criteria Are Met:

   1.  It is in your possession, or
   2.  It is in your view, after being in your possession, or
   3.  It was in your possession and then locked up
   to prevent tampering, or
   4.  It was in your possession and then transferred
       to a designated secure area.

-------
      TRANSFER OF CUSTODY & SHIPMENT
1.  Relinquishing & Receiving Samplers Sign, Date, Time
2.  Ship To Laboratory
3.  Separate Custody Record For Split Samples And To Each Lab
4.  Retain Bill Of Lading From Carrier
5.  Lab. Custodian Signs Upon Receipt
6.  Original Stays With Samples

-------
u §

-------

-------
EPA S/tnfLE TA

-------
        si ii?e~  a?
                s i D &
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
           REGION 5
       230 South Dearborn Street
        Chicago, Illinois 60604
         &EPA

-------



;v/;;r-*'>::>cV-'- '••-'.'-'.'-" -••"•'. yr'^"-*-'.'*- Xr^-^fe^/'-^^'j^^''--^'::"

                   m

                   I
                o  1
              "14
                     1

-------
                 FORMS REQUIRED
              Low & Medium Samples

1.  SMO Org. Traffic Report
   SMO Inorg. Traffic Report
2.  (Packing List For Sas's)
3.  EPA Custody Form
4.  EPA Custody Tag
5.  EPA or State Custody Seal
6.  Stick-On Label Traffic Report

-------
  Case Number:
 Sample Site Name/Code
 Fo*
(2)  SAMPLE CONCENTRATION
            (Check One)
                               *
                                  Low Concentration
                                  Medium Concentration
                             SAMPLE MATRIX
                                 J^heckOne)
                               S Water
                             	 Soil/Sediment
                                                               Ship To:
                                                            Transfer
                                                            Ship To:
© Regional Office:
Sampling Personnel:
                        (D For each sample collected specify numbe
                           of containers used and mark volume level
                           on each bottle.
                                           Number of
                                           Containers
        (Phone)

 Sampling Date:
                        Water
                        (Extractable)
(Begin)
                 (End)
Water
(VOA)
(?) Shipping Information
                        SoiVSediment
     Name of Carrier
                         Water
                         (Ext/VOA)
                         Other
      Date Shipped:
     Airbill Number:
(§) Sample Description

  	Surface Water

  J*L_ Ground Water

  	Leachate
                         Mixed Media

                         Solids

                         Other (specify).
                                                     Approxima1
                                                     Total Volun
                                                       Sample
 E 3451

 E 3451

Y3451

 E~3451

 E 3451

 E 3451

 E 3451

 E 3451

 E 3451
                                       E  3451
 Water
 (Extractable)


 Water
 (Extractable)


 Water
 (Extractable)


 Water
 (Extractable)


• Water
 (VOA)


 Water
 (VOA)


- Soil/Sediment
 (Ext & VOA)


- Soil/Sediment
 (Ext & VOA)


• Water
 (Ext & VOA)


-Water
 (Ext & VOA)
QO) Special Handling Instructions:
   (e.g., safety precautions, hazardous nature)
                                       SMOCOPY

-------
Sample Site Name/Code
            r
) Sampling Office: _

 Sampling Personnel:


 (Name)'.

 (Phone)
 Sampling Date;

 (Begin)
         g Date:
         iA
   Sample Description:
      (Check One)
    Surface Water
    Ground Water
    Leachate
    Mixed Media
    Solids
    Other 	
                  (specify)
MATCHES ORGANIC SAMPLE NO.
                                        SAMPLE CONCENTRATION
                                                  (Check One)
                                           Low Concentration
                                        — Medium Concentration
                                     0 SAMPLE MATRIX
                                         .X       (Check One)
                                        !—- Water
                                           Soil/Sediment
                                                                            Transfer
                                                                            Ship To:
                                     0 Shipping Information:

                                     Name Of Carrier
Date Shipped:

Airbill Number:
                                    (m\ Mark Volume Level
                                       On Sample Bottle
                                       JKieck Analysis required
                                    ^L Task 1 & 2
                                    __ Task 3 Ammonia
                                            Sultide
                                            Cyanide
                                                SMOCOPY
                                                                 ^ME0176
                                                                                    -T«ikl&2
                                                                  ME 017 6  -Tasltl&2


                                                                  ME 017 6  -TaakS


                                                                  ME 6 176  -T«k3


                                                                  ME 0176  -Ta»k3


                                                                  ME 0176  -TaskS
                                                                      • ME 0176  -TaskS

-------
   FORMS REQUIRED HIGH HAZARD SAMPLE
1.  SMO High Hazard Traffic Form (Packing List For SAS's)
2.  Hazardous Waste Samp. Prep Request
3.  EPA Custody Form & Tag
4.  EPA or State Custody Seal
5.  Label From Traffic Report
6.  Hazardous Shipping Certificate

-------
  c    c    c     c    c    c
o    o    o    o    o    o
                                                                                 o
                                FIELD SAMPLE RECORD
3) Case N
  Sample Site Name/Code:
  1 ~   •    »         -*—
                           Field Sample Description:
                            	Aqueous Liquid
                            _2udge
                            _Sobd

                            Z Other	
                   ,3) SUpTb:
                                                                Attn:
  	Jf^
  Sampling Personnel:
        (ptone)

    Sampling Date:
(begin)
                 (end)
   Shipping Information:
      (airbi number)
                           Known or Suspected Hazards:
                              ftt
Preparations Requested:
(check below)

Sample Volume:   O  #">

i^Organics
        Organics
                               Total Metals
                             .j^jjptal Mercury
                                strong Aod Anicns
                                                                Sample Location:
                     E 5102

                     E 5102


                     B 5102

                    •  5102

                    E  5102
   Special Handling Instructions:
                                        SMOCopy

-------
   o
   ^•^
   LU
I/I
01
 e-o
 re  a>
oo  >
   •*-
 0}  
 x
 LU

-------
US. ENVIRONMENTAL PROTECTION AGENCY
HWI Sample Management Office
P.O. Box SIX  . Alexandria, Virginia 22313
Phone 703/557-2*90 -  FTS/557-2490
                                    PACKING LIST
                                                 SAS Number
                                                 3S5 £
 Regional Office:
 Regional Contact:
            E//
       (name)
       (phone)
Sampling Date(s):
                      Date Shipped:
                        //* 3
Ship To:
For Lab Use Only
                 5*330
                                                                   Date Samples Rec'd:
                    S/,
                           '    $000*
                           . rw/r
                                               Received By:
        Sample
       Numbers
              Additional Sample
                 Description
                           Sample Condition
                             On Receipt
 5.
                           cyp5"S^  - Me4.
 6.
 7.
 S.
 9.
10.
11.
12.
13.
         PCfe*      flivlv
1*.
15.
16.
17.
IS.
19.
20J
                                                                     For Lab Use Only
   White - SMO Copy,  Yellow - Region Copy, Pink - Lab Copy for return to SMO,  Gold - Lab Copy

-------
U.S. ENVIRONMENTAL PROTECTION AGENCY
rltfl Sample Management Office
P.O. Sox 813  - Alexandria, Virginia 22313
Phone: 703/557-2*90 -  FTS/557-2*90


                       SPECIAL ANALYTICAL SERVICES
                               Regional Request
        Regional Transmittal  .  .              _   Telephone Request
                                              \ _ |
 A.   EPA Region:
B.   Regional Representative: £,/•> t/C fa Ell
                                               y

 C.   Telephone Number:     3/^* 35*3*^37 O

 D.   Date of Request:       $ 4J?T*H b* A,  Ij
 Please provide below a description of your request for Special Analytical Services
 under the Uncontrolled Hazardous Waste Dumpsite  Program.  In order to most
 efficiently  obtain laboratory  capability for your  request, please address the
 following considerations, if applicable.  Incomplete or erroneous information may
 result in a delay in the processing of your request.   Please continue response on
 additional sheets, or attach supplementary information as needed.
                 X^**1.
      ' Definition and number of workrunits involved (specify whether whole samples
      or fractions; whether organics or inorganics;  whether aqueous or soil and
      sediments: and whetherlow. medium or his
              *A  **   <••>• I _i       «te  ft r
                        of analytical service requested:
 3.    Purpose of^nalysis (specify.whether enforcement, RCRA, NPDES, etc.):
                           '
       Estimated date(s)of collection:
  5.    Estimated date(s) and method of shipment:

-------
   6.   Approximate number of days results required after lab receipt of samples:
            40-tiC.  No  /**<*.   +h*u  NOV.  /?,/<./»>/><      Tg *OA5Ttf ^r?.  /OX c,hAiH*T* 9
    10.  Other (use additional sheets or attach supplementary information, as needed):
         Vti^ti**   J  * -*£	'*- -*--••     -•--*<*•-  Jr.. -
     PcTfVf  A-Tfr  /tVt/4 ~
     fy^Yf-7ft p   «»H!  jw 7^?
11.   Name of samplins/shippmg contact:  JoAv P/€/S5K< ^
                                   «a V
                                              P/€
                                              JL4
    Please return this request to the Sample Management Office as soon as possible to
    expedite processing of your request for special analytical services. Should you
    have any questions or need any assistance, please call us at the Sample Manage-
    ment Office.

-------
                                          -3-
I.
     Data Requirements
     Parameter:
      ff
 II.  QC Requirements
     Audits Required
   /•(
                               Oetection  Limit
                   .ycQM
                                    't- &
III.  *Action Required if Limits are  Exceeded :
    IP
Precision Desired
 (±% or  Cone.)
                                                                    ¥0
                               Frequency of Audits         Limits*  (% or Cone.)
                                           4J*4~to* 4/

-------
                DOT SHIPPING REGs
Medium & High Hazards
     1.  In 1/2 or 1 Gal. Cans
     2.  Inside Plastic Bag
     3.  Vermiculite (Zono-Lite)
     4.  Clips or Tape on Cans
     5.  Address & Hazard
     6.  Haz. Shipping Cert.
     7.  Metallic or Plastic Picnic Cooler Required

-------
                 SHIPPER'S CERTIFICATION FOR RESTR|CTED ARTICLES
                               (excluding radioactive materials)
           Two completed and signed copies of this certification shall be handed to the carrier. (Use block letters)

   WARNING: Failure to comply  in  all respects with the applicable regulations  of the Department of
   Transportation, 49-CFR, CAB 82 and, for international shipments, the IATA Restricted Articles Regulations may
   be a breach of the applicable law, subject to legal penalties. This certification shall in no circumstance be signed
   by an IATA Cargo Agent or a consolidator for  international shipments.

  'This shipment is within the limitations prescribed for: (mark one)

   C£ passenger aircraft                    D  cargo-only aircraft                        v

i Number
1 of
I Packages

PfcS #1




Article
Number
(Int'l only
See Section
IV IATA RAR)





Proper Shipping Name of Articles as
shown in Title 49 CFR. CAB 82 Tariff 6-D,
and (for int'l shipments) the IATA
Restricted Articles Regulations. Specify
each article separately. Technical name
must follow in parenthesis the proper
shipping name for N.O.S. items.
Poison B, Solids, NOS:
Polycyclic Aromatic Hydro-
carbons
Poison Babel

Class

Poisor
B



IATA
Packing
Note No.
Applied
(int'l
only)
L 364
a)(l)



Net
Quantity
of Each
Package

100 tag



m
Flash Point T
(closed cup) 1 A
For Flammable u£
Liquids Kg
•c.




•F. |r
V
S
r

Special Handling Information:
    I hereby certify that the contents of this consignment are fully and accurately described above by Proper
Shipping Name and are classified,  packed, marked, labelled and  in proper condition for carriage by air
according to applicable national governmental regulations, and for International Shipments, the current  IATA
Restricted Articles Regulations.
Name and full address of Shipper

  Analabs	
                                      Name and title of person signing Certification
  80 Republic  Drive
  North Haven,  Conn.  06473
                                                     Eleanor Rome, Export Clerk
Date
                ?Q.1Q30
Air Waybill No.*
                                      Sigrja*ure of the Shipper (see WARNING above)

                                                        O<
    OOX i
dl for,
                        ,ion
                    Airport of Departure*
                                  ,g can-
Airport of Destination*
                                                              JBMt
                                                                                   J626 3'

-------
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-------
          Internal Record Keeping
                      and
           Data Handling ,  Review

1.  VIAR Case Planning Log for future and pending cases.
2.  Internal Tracking Sheet
3.  Raw Data Return
     a)  NCL Data to EPA, CRL.
     b)  CRL forwards it to State
     c)  State reviews own data
     d)  State sends copy of review comments to CRL
     e)  States resolve Q..C. probs.
     f)  Unresolved Q.C. probs. referred to Regional DPO
        For lab which has the Q.C. problem.
4.  Picnic Cooler Return

-------
                      VlAZ
                       NO.
I

-------

-------
            CLP SCRIPT
QUALITY ASSURANCE AND DATA REVIEW
          SEPTEMBER 1983

-------
QA 0

Hello I am Marcla Kuehl.  I am the Quality Control Coordinator for the
Region V Central  Regional Laboratory.  My duties Include auditing not
only the data generated by our In-house laboratory but data generated by
the National Contract Laboratory Program.  I am one of a five person team
responsible for CLP data review.  Two people review organic data, two
review inorganic data, and I do both on an as needed basis.  I have been
with the lab for three years, in the capacity of Chemist, GC/MS Operator
and now paper pusher.  I have retained both my eyesight and my sense of
humor since I began reviewing CLP data in January of 1980.

-------
INTRODUCTION

Now that you have collected, packed, and shipped your samples you will
be buried in a sea of data.  It is essential  that this data he reviewed
by competent technical level personnel before it is released for use.
It would be very naive to think that this slide show alone will  enable
everyone to quickly review Contractory laboratory program data.   Persons
responsible for review should already have working and preferably hands-on
knowledge of AA, ICAP, GC/EC, GC/MS and basic extraction chemistry.

QA 1

This presentation will deal with the technical  review and quality level
assessment of the data.  The contract specifies the general quality
assurance program to be followed and details the specific quality
control audits to be used.  It is your job as the reviewer to determine
the level of quality of the data based on these audit results and
recommend if the data quality is sufficient to meet its intended use.
I will discuss both organic and inorganic data review by examining the
specific pieces of paper we at the Region V Central Regional Laboratory
key in on.  Examples presented are from various Contract laboratories
and several cases.  The names have been deleted to protect the innocent
or the guilty as the case may be.  Actual forms and data printouts in your
data packages may vary from Contractor to Contractor based on instrument
differences.  Guidelines for the preparation of Special Analytical Services
requests relating to QC requirements will also be presented.

QA 2

All data review requires the Elementary School  three R's- reading, writing
and arithmetic.  Keep this in mind and you will not be side-tracked or
put unnecessary time into paper shuffling.

QA 3

Before you even look at any data, read the Statement of Work, the analytical
methods and the QA/QC sections of the contract.  Imagine that you are a
sample and trace your progress through the laboratory and note what kinds
of paper are generated along the way.  You may find deficiencies in the
methods, or lapses in the documentation.  The Contractor is only responsible
for what is written in the contract.  There is no such thing as a free  lunch-
Contractors generally will not provide extras.   Recommendations  for additions,
deletions, or changes to existing contracts should be made in writing to SMO.

-------
                                 - 2 -
Write down the data or sampling objective for the case to be reviewed.   This
is determined by consultation with the Samplers, Engineers and  Project  Leader.
I usually classify the overall level  of the study into one of three  categories:

Category 1 - Screening Surveys: These are intended to serve as  quick looksees.
             Quantisation, precision  and accuracy is not  as vital.   Correct
             qualitative identification is needed.

Category 2 - Remedial or Monitoring Surveys:   These surveys require  more
             quantitative results in  order to determine whether the  clean-up
             level is sufficient or to detect trends in ambient levels.

Category 3 - Criminal or Known Enforcement Investigations:

             These necessitate that the custody paper trail be  reviewed
             carefully as well as flagging all out of control situations.
             Precision and accuracy of both quantitative  and qualitative
             data is crucial.

When the end action or purpose of the study is not known, aim for the
criminal category as it is much better to be safe than sorry.

The calculations involved in the basic statistical expressions  of mean
and standard deviation should be reviewed.  In order to cross-check  Contractor
values, you should known how to calculate percent recovery, relative percent
difference (RPD), response factor (RF), relative response factor (RRF),
relative retention time (RRT), and mean percent change.  Definitions of
these can be found in the text of the contract.  Arithmetic errors do occur,
and may often directly involve the sample values reported.

QA 4

Since organic data generally constitutes a bigger and more awesome pile, I
will tackle its review first.  Listed here are eight target areas that  are
examined during the data review process.  They are not listed in order
of importance, but in an order that personally like to use.  Once you
are familiar with the layout of the data packages you may wish  to revise
the order.  On the following slides each of the eight items will  be
presented along with key forms to look at.

QA 5

Do decafluorotriphenylphosphine and bromofluorobenzene mass spectra  meet
the contract required abundance criteria?  The required abundance criteria
were taken directly from the December 3, 1979 Federal Register.  These
criteria were meant to help laboratories determine if their GC/MS system
is in tune and stable enough to generate reproducible data.  The key piece
of paper to look at is the mass spec  abundance list, either computer
generated or a form similar to the ones seen in the next  slides.

-------
                                     - 3 -
QA 6

This form is for OFTPP, injected on January 26, 1983 relating to all  samples
in run OH830136C15.  This information is at the top of the form and  should
be used to correlate real samples to the appropriate DFTPP injection.  You
should_be able to find at least one injection per 8-hour shift.  The two
masses most often out of specs for DFTPP are 51 and 443.  There are  two
schools of thought on what effect flags like these have on sample data.
One school recommends scrapping the associated sample data as invalid,
since adherence to these criteria are required by law.  The other school
relies on whether the specific masses out of spec affect the identification
of any priority pollutants or tentatively identified compound search matches.
Your professional judgement should be used to choose what criteria you  will
follow- but be consistent.

Note that that chromatography and sensitivity checks are also listed on this
form below the DFTPP specs.  When these do not meet the contract limits,  a
notation of poor chromatography conditions or sensitivity should be  made
and affected samples in the run flagged.  Contract limits for these  audits
are:

     - pentachlorophenol response factor should be greater than 0.05
       relative to dig-anthracene.
     - 50ng of benzidine should be detectable, double check the actual
       RIC for its presence.
     - Area counts for 20ng d]Q anthracene should be between 20,000-
       50,000 to avoid detector saturation at the higher standard
       concentration levels.

The column description should be checked to see that the contract specified
column has been used in the instrument.

QA 7

Recently, the Regional data reviewers have requested that the contract  lab
summarize their tuning results on an easy-to-find one page form such as
this one.  I will then randomly check actual abundance lists in a case  to
verify the presence or absence of listed deviations.

QA 8

Are the instrument and method blanks contaminated?  The key item to  look  at
is the actual RIC of the blank and the reagent blank summary.  Contamination
of lab or instrument blanks negates any quantitative sample results  for those
compounds detected in the blank.  This is especially vital where sample
results are of the same order of magnitude as the blank.  Blank subtraction,
when done, will be noted by the contract lab.  If you are not sure,  contact
the contract lab before you release data.

-------
                                     . 4 -
QA 9

Here are some examples of contractor generated QC notices to alert you to
blank problems and calm your fears that the lab is totally out-of-control.
The top notice refers to the presence of siloxane in the volatile blank
fraction due to the anti-foaming agent added to the purge and trap vessel.
The bottom notice attempts to determine the source of 4-hydroxy-4-methyl,
2-pentanone which is a common artifact seen in ABN fraction blanks and
field blanks.  This compound is formed from residual acetone reacting
with NaOH during the pH'^ adjustment.  Check to make sure that these
compounds are not listed as positive hits in the samples for this case.

QA 10

Highlighted in this reagent blank summary is the presence of acetone and
methylene chloride in the volatile fraction above the contract detection
limit and trace amounts of three phthalates in the semi-volatile fraction.
The K code under "concentration found" stands for a trace value present,
which is below the contract detection limit but not quantifiable.  The
presence of these lab blank contaminants is not an unusual occurence, but
is an annoying one.  What do you do for samples in this case that have
similar levels of these compounds reported?  You flag them as being
indistinguishable from lab induced contamination and therefore not a reliable
indication of the actual sample level.  You may circle the results directly
on the result sheet, or list them on a review form.  At any rate, do not
let these contamination notes be separated from the associated data.

QA 11

Are positively identified or positive "hit" priority pollutants actually
present?  In order to minimize the cost and panic over false positives,
each positive "hit" should be verified by you.  Look at the dual display
Mass Spectrum of the sample peak and associated standard peak.  The sample
and standard retention times should agree to within j* 8 seconds.  The
contract also requires that all ions present in the standard at a relative
intensity of greater than 10% must also be present in the sample spectrum
and that the relative intensities must agree to within _+20%.  Extraneous
ions greater than 10% intensity in the sample and not in" the standard
must also be accounted for.

QA 12

Here is a dual display of sample 023890 peak (shown above) which was
identified as priority pollutant 445 which is pyrene.  The pyrene
standard mass spectrum is shown below.  This is an obvious good match.
Also check the retention time of the scan (1922) against the retention
time of pyrene for the initial  or continuing calibration standards found
on other forms in the packet.  Remember that a +_ 8 second or scan window
is allowed.                                    "~

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                                   - 5 -
"Hits" not meeting these criteria should he considered  false  positives
and be labelled accordingly on the data sheets.

QA 13

This 1s the associated GC/MS computer generated quantitation  report  foV
sample~023890.  This is an example from a Finnegan  OWA  system.   Hewlett
Packard and other GC/MS system printouts vary in format,  but  the basic
information is still similar.  The first column on  the  left labelled  No  refers
to compound number- usually the contractor lab will  list  these  in order
of f>C column elution.  Compound number 62 represents pyrene.  The next
column labelled m/e is the mass of the base peak of compound  62, mass 202.
The scan column contains the scan number the compound pyrene  eluted  at,
here 1922, at a retention time of 24 minutes, 1 second.  Remember that this
retention time should be within that 8 seconds of the pure pyrene standard
run that day.  Pyrene relative response time (RRT)  is calculated relative
to compound 48 (nearest internal  standard, D-jgchrysene).  A base-to-base
peak integration was done resulting in an area of 41541,  representing
an injection concentration of 22.604ng, or 2.42% of the total RIC peak
area.

The circled amounts with a "Y" scribbled near them  means  that these
priority pollutants were verified by the contractor GC/MS supervisor
or expert to be present at a quantifiable level. You should  also
examine their dual display spectra and RIC and confirm  their  presence.

QA 14

This sheet reflects the contractors worksheet for calculation of positive
final results.  The compound number 445 or pyrene quant report  value  from
the previous slide was rounded up to 23.  The correction  factor includes
dilution, original sample weight and dry weight calculations.  When  multiplied
by the quant report value, the result of 920 ug/Kg  should be  found on the
data report form.  Double check multiplication on all positive  "hits" as
time permits.  The column labelled detection limit  is the low level  solid
determined value in ug/Kg and gives you a comparison of how high above the
matrix detection levels the compound actually is.

QA 15

Are the tentatively identified compounds matches reasonable?  Once the
positive priority pollutants are confirmed by your  review, the  tentatively
identified compound searches should be visually examined  by keying in on
the RIC to determine the approximate size of the unknown  peak,  and the
mass spectra of the unknown and the top three ranked computer library
searches.  Not only is a visual inspection needed,  but  a  mental one  is'
needed also.  Is the compound match too exotic to survive the extraction
or GC/MS conditions?  Is the compound one not expected  in the sample or
site?  For example, long chain sugars are not usually found in  environ-
mental water or sediment samples.

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                                     - 6 -
QA 16

This is the simultaneous display of the sample unknown  peak  I486,  of  sample
023890, of a base peak of 97 and the top three ranked  library  search  matches:
1,1,2-trichloroethane, 2,2-dichloropropanoyl-chloride  and  1,1-dichloro-l-
nitroethane.  The unknown was identified by the contract lab as  1,1,2-tri-
chloroethane, purity 892.  This area of data review is  where GC/MS spectral
interpretation experience will  be needed.  Although several  light  masses
appear in the sample and not in the match, all trichloroethane masses are
accounted for in the sample.  Note that the sample base peak is  97 whereas
the best match base peak is 83.  Generally speaking, purity  or fit figures
of less than 800 or 80% are often questionable matches. Contractors  are also
required to estimate the concentration of these unknowns  (up to  20 A8N, up to
10 VOAs) will be estimated this way on the basis of internal standard response.
You may check the reasonableness of the magnitude of tentative ID  concentrations
by checking the Quant report or RIC for relative area  response.   Since quantitation
of these compounds is only an estimate, I rarely try to recalculate the reported
figure.  Unreasonable matches in your opinion should be deleted  and marked with
your initials and date.  Identification of unknown peaks spectra using hard  bound
library spectra is a colossal task and should not be attempted unless you are
requested to do so by the Project Leader and are well  versed in  MS interpretation.

QA 17

Were the sample extraction and analysis holding times  met?  The  contract requires
that volatiles be extracted within 7 days and ABN's be extracted within 5 days
of sample receipt by the contract lab.  To monitor this, the laboratory analysis
chronicle copy could be checked.  Recently, this can additionally be  monitored
by internal lab GC screen bench records.

The holding time requirements delineated in the contract must  be met  or data
should be flagged.  Remember the end use of the data when  you  do flag holding
times.  Samples sitting in drums for years should not  change if  held  in a lab
over 14 or 30 days.  The lab analysis chronicle is a key item  to check as  it
lists all of the sample extraction and analysis times.

QA 18

This is a contract lab GC screen extraction record for Case 1850.  The sample
extraction procedure is clearly spelled out in the narrative below.  These
samples were extracted on 6/29/83.  Check your sampling and chain-of-custody
record to calculate the days elapsed since collection, shipment  and lab  receipt.
Note that the contract lab is not responsible for your shipping  delays.  Their
holding and data turnaround time clock starts when they actually receive the
samples.  Now that these liquid samples have been extracted for  pesticides,
they are screened by GC/EC.

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                                     - 7 -
QA 19

The sample extracts of 6/29/83 were screened on 7/4/83 by GC/EC according
to the procedure narrated in the top three items on this Screen Evaluation
Form.  Note that all of these extracts were judged to be low based on
Point #3:  No peaks appeared in the screen chromatogram at a response
greater than 25% of p,p'-methoxychlor.  Also note that the contractor  was
working on the fourth of July.

QA 20

Sample E3434's GC/EC pesticide screen chromatogram is shown here.   Note
that no peaks of a response near 25% of p,p'-methoxychlor are seen.  You
should particularly check screen chromatograms of samples designated as
medium level to ensure that the higher detection limits were justified
based on screen peak response.  Also verify that 5ng methoxychlor  does
produce at least a 50% full scale deflection response.
                      •
OA 21

Are the results reported of acceptable precision? Matrix spiked duplicates
should be included in each case or one per 20 samples, whichever is more
frequent.  This duplicate should be an environmental sample, split by  the
laboratory, not^ a method blank.  The key form to look at is the presentation
of duplicate relative percent difference (RPO).  A matrix spike duplicate  is
a random environmental sample that is split into three separate aliquots.   One
is extracted and analyzed as is, the other two are spiked with a variety of
priority pollutants at the same level, then extracted and analyzed.  This
concept was used to give some meaningful precision and recovery data  in  actual
sample matrices, as samples chosen at random, and analyzed without a matrix
spike were more often than not, clean samples.  Not detected compared  to not
detected is great, but not useful precision.

QA 22

This is a summary of the QC sample and original sample results for a matrix
spike duplicate pair pertaining to Case 1439.  The sample chosen for the
matrix spike duplicate is in the upper left hand corner under EPA  Number.   Other
samples in the case containing this duplicate pair are listed under associated
sample numbers.  The first seven compounds listed are the surrogate spike
compounds.  Note that four out of six show poor precision.  The next  11  compounds
are those used in the matrix spike solution.  1,2,4-trichlorobenzene,  hexachloro-
benzene, and 1,4-dichloronenzene are outside the contract precision  allowances.
Contract precision allowances expressed as RPO are: +, 15% for volatiles, ^ 40%
for acids, +_ 50% for base neutrals, ^40% for pesticides and TCOO.  Similar
sheets in the data packet should list" the other fractions' precision  results.
What should you do for a case where the matrix spike

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                                     - 8 -
duplicate floes not meet precision limits?  First flag the actual  sample
chosen as yielding erratic results, therefore quantitative sample results
for the affected sample fractions may only be considered as precise as
the matrix spike fraction precision.  This statement may or may not be
extended to the other samples in the case, depending on their degree of
similarity to the matrix chosen.

QA 23

Are the results reported of acceptable accuracy?  Surrogate spike compounds
are added to every real sample, QC sample, and blank,  the recovery of  these
compounds are your key to the extraction efficiency and therefore accuracy
of each sample fraction.  The contract lab will  summarize the entire case
surrogate recovery on a form to enable you to quickly scan for out-of-control
results.

QA 24

This is a percent recovery summary for a case of low level water samples.
The three volatile surrogates used are Ds-toluene, bromofluorobenzene (8FB),
and 04-!,2-dichloroethane.  Advisory limits only have been set for 8FB  and
04-1,2,-dichloroethane due to lack of enough interlab data points.  No
samples were outside of the QC or advisory limits.  The next seven surrogate
compounds are used to evaluate semi-volatile fraction accuracy.  Ds-nitrobenzene,
2-fluorobiphenyl, Ds-phenol, 2-fluorophenol and 2,4,6-tr'ibromophenol  are the
required surrogates.  Pentafluorophenol and decafluorobiphenyl  are two  additional
chosen by the contract lab as an option.  Since no QC or advisory limits have
been set for these two optional surrogates, no flags can be assigned.  This
data is evaluated by the contract lab to judge the suitability of these optional
surrogates.  2,4,6-tribromophenol recovery was out-of-control low for the
entire case.  This surrogate is one of four compounds used to assess acid
fraction accuracy- the others are pentafluorophenol, 05-phenol, and 2-fluorophenol
Look in the data package for an explanation of consistent low recoveries such  as
these.  None of the three base-neutral surrogates have any flags assigned- look
at the actual Ds-nitrobenzene, 2-fluorobiphenyl  and Decafluorobiphenyl  recoveries.
Although generally biased low, none are outside the lower limit.  Decafluoro-
biphenyl has no limits assigned to it due to inadequate data base.  The current
sole pesticide surrogate 1s dibutylchlorendate.  No recoveries are outside
the 67-114% limit.  The surrogate used for 2,3,7,8-TCDD analysis is 1,2,3,4-TCDD,
chosen because of its lower toxicity and rare occurence in environmental samples.
Two recoveries of 332 and 334% were flagged by the contract lab.  An explanation
as to the possible spiking error or evidence of native 1,2,3,4-TCOO in  these
samples should be included with the data package.  A 0% recovery was also  found
for sample E3431.  If any positive 2,3,7,8-TCDO is reported for this sample,
its quantitatlon may be biased low due to the poor surrogate recovery.

-------
                                     - 9 -
Sample E3432 1,2,3,4-TCOD recovery was 17.1%, below the QC limit  of  26-104%,
but was not asterisked or flagged by the contractor.  In the comments  section,
there should be explanations of out-of-control  situations or notation  of  reruns,
but alas there is nothing there in this example.  The contract  requires that
any out-of-control  surrogate recovery occuring in a blank necessitates reinjection
or repurging.  If the recovery is still outside limits, no data is to  be  generated
or reported until corrective action is taken, such as recalibration.  When  the
recovery of any one surroga'te falls outside the limits for a sample, the  contractor
must verify and document that the deviation is due to the sample  matrix itself
and not his laboratory.  This may be done by checking calculations,  instrument
conditions and time, and surrogate/internal standard solutions.  If  an error
in any of these systems cannot be established, the affected sample fraction
should be re-extracted and reanalyzed if sufficient native sample remains.
If this repeat indicates the same type of surrogate flag, the situation may
then genuinely be termed a matrix problem.  You should be able  to find both
sets of data(the original and repeat) and you should qualify the  affected
sample fraction data as biased due to an intractable matrix or  matrix  interference
problem.  The contractor gets paid for this additional rerun only if it turns
out that poor recovery was not his problem.

Since no clear correlation of extraction behavior of each surrogate  to specific
priority pollutants has been made yet, a whole fraction such as acid,  base-
neutral, pesticide, must be flagged as biased high or low when  out-of-control
surrogate recoveries occur.  Do this directly on the final  sample data sheet  or
on your review form.  You might also note an estimate of the magnitude of the
bias, for example for sample E3430, 2,3,7,8-TCOn results (if positive) may  have
been biased 200% high.  An additional means of verifying the accuracy  of  reported
positive "hit" sample values is by examining the initial and subsequent checks
of the GC/MS calibration.

QA 25

This is the response factor and retention time information of the initial
injections of 3 concentrations of volatile priority pollutants.  At  the top of
the form is the instrument identifier- which becomes extremely  important  if the
contract lab has more than one GC/MS and therefore must calibrate each one  used
to run your samples.  You should be able to trace the instrument  to  the samples
run to check that the appropriate standard response factors and retention
times are used to calculate final  results.  Note the calibration  date  of
August 3-4, 1983 in the upper right hand corner.  Make sure your  samples  and
calibration checks  were run after or on this date.  Highlighted is the statement
minimum mean RF (response factor) for SPCC is 0.30.  This means that for  all

-------
                                    - 10 -


compounds designated as a system performance check (labelled with an asterisk
in the SPCC column) the minimum response factor of the instrument should  be
0.30.  Note that all SPCC compounds meet this criteria.  Response factors are
obtained at the three concentration levels of 20, 100 and 200ng.   You may want
to eyeball the values contributing to the mean to check for any wild deviations.
The effect of are inadequate response factor for a SPCC may be minimal, but
several- indicates poor response and the system should have been recalibrated.
                                    t
The mean RRT column should be used to check against the positive  "hits"
identified in the sample case mentioned previously.  At least once every  8 hour
shift subsequent to the initial calibration, a calibration check  standard
solution should be injected.

QA 26

These are the results for such a check.  The OWA instrument which was initially
calibrated on August 3-4, 1983 was checked on 8/12/83 at 17:47 hours by an
injection of VOAICS812C.  Note the highlighted statements "maximum % 0 for CCC
is 20" and "minimum RF for SPCC is 0.300".  CCC refers to calibration check
compounds which are different than the SPCC's indicated earlier.   These compounds
are used to verify that the original  calibration curve is stable  to within
4^20% measured as daily response factor deviation from the initial calibration
"response factor mean.  All of the % D or % deviations (alias mean percent change)
are in control, as are the SPCC responses.  This gives you confidence that the
GC/MS instrument quantitation of positive sample results are accurate to  within
+ 20%.  Compounds showing much greater deviations (for example methylene  chloride
T-40.6%), acrolein (36.4%) and 4-methyl-2-pentanone indicate that quantitative
sample results for these compounds may he less accurate.

Since all response factors and tentatively identified compounds are quantified
on the basis of internal standard response, the contract requires tracking
internal standard response.  Contract labs do this in a variety of ways,  but
the principle and limits are the same.

QA 27

Here is a form entitled "Internal Standard Response Verification  Control  Chart".
These are plotted as relative response of one internal standard to the next
closest in elution over time (x axis).  The top control chart is  the response
(area) of D3~phenol to Dg-naphthalene, the middle one of Dg-naphthalene to D-jg-
phenanthrene and the bottom of D-|Q-phenanthrene to O^-chrysene.   The limits
are +. one standard deviation.  Notations of corrective action are made in
the Ubttom chart, and correspond to the low out-of-control points indicated
for 03-phenol/Og-naphthalene response seen in the top.  I look at these
charts as an indication of the suitability of the internal standard in the
matrix and as a reflection of spiking technique.  I do not flag any sample
data directly as a result of this audit.  As a point of information, the
corrective action taken reads- recalculated manually- computers sometimes
do make poor judgement calls in area integration.

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                                     -11  -
QA 28

Did the method efficiently extract and quantitate the priority  pollutants
present?  The recovery of priority pollutants from an actual  sample  matrix
is the key to check.  It, however, only tells you the effectiveness  of  the
method, for the sample chosen.  Period.  It cannot he extrapolated  to every
sample in the case unless every sample matrix is known to be  identical.
The matrix spike duplicate protocol will give you not only the  accuracy
of the extraction in the matrix, but the precision.

QA 29

This is the contractor supplied matrix spike duplicate recovery summary
for Case 1927, low level water samples.  SMO Sample # E3869 was chosen  as
the volatile matrix sample and E3871 as the acid, base-neutral  and pesticide
sample.  Note that columns for both percent recovery and  relative  percent
difference are presented.  The current QC limits for both are also listed
to make flagging or "asterisking" of out-of-limit data easier.   Only two
flags were assigned.  2,4-dinitrotoluene recovery of 4.1.% was  below the
limit of 43% and p,p'-DDT recovery of 60.9% was below the limit of 82%.
Since the other duplicate pair was in control and the precision was
acceptable, sample data for the base-neutral and pesticide fractions
for the E3871 or E3869 was not labelled as biased low. What  number  of
matrix flags constitutes invalidating the entire fraction's precision
and accuracy?  This is a judgement call on your part.  If a matrix spike
compound flagged appears at appreciable levels in the native  sample, valid
recovery information is hard to obtain.  Remember the rules of  statistics when
looking at these large number of data points- most limits were  calculated at  a
90 or 95% confidence level- so try to avoid unnecessarily invalidating  associated
sample results.  Audits may be out simply due to random statistical  error.

You have now finished pawing through the average 3 inches of  paper for
a 5 sample case, you've waved your pen and raised your flags.  Now it
is time to clearly and concisely present your review findings.   The  CRL
prefers a one page data cover with various options for final  acceptability.

QA 30

This is a suggested format for a final review form.  It contains the date
the data package was received- 9/15/83, and the date the  reviewed  data  was
transmitted 9/22/83.  At one time, we were shooting for a 5 day turnaround
per case, no matter how large or complex.  This has not been  reasonable as
of late.  A three quarter to an hour per sample figure is a better estimate
of review time.  This case, 1927, contained 5 samples- SMO Numbers E3S68 to
E3872, CRL Numbers 83MS08S47 to 83MS08R08.  A field blank was sent,  indicated
by the R08 sample designation.  The review took 3.5 hours. The four major
findings of the review are listed.

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                                     - 12 -


Point 1;   Detection limits are not listed on the final  reports.   The  reviewer
felt that the contractor should complete the data forms,  including  the  detection
limits.  Note at the bottom that copies of this  review are sent  to  Or.  Haeberer
who is in charge of technical  support to the contract  labs and  CLP  users,  Ross
Robeson,  who will  take up these complaints on the next on-site  audit  by EMSL-LV
of the contract lab, and Robert Pritchard of SMO, who  is  responsible  for obtaining
missing contract required deliverables.

Point 2:   Pesticide and PCB chromatograms are of poor  quality,  difficult
to read and interpret.  The reviewer was unable  to confirm the  presence of
the positive reported values because the standards did not agree with the
sample, and samples were not confirmed on GC/MS.  The  contract  lab  was  called
and will  send better copies,

Point 3:   Several  compounds were detected in the method blank,  these  were  flagged
on the final reports with the Code "8", this indicated that the  quanti-
tation and presence of these compounds may be due to lab  induced contamination.

Point 4:   Several  of the surrogate spike recoveries did not meet the  CLP
criteria  although they were marginally by a (few percent) out,  no major impact
on sample data was judged necessary by the reviewer.  1,2,3,4-TCDD  surrogate
recovery  for Sample E3871 was 223%, way outside  limits, but no  action was
taken to  invalidate the 2,3,7,8-TCDD result as visual  inspection of the
chromtogram and mass spectra indicated none was  indeed present.

The final call on the data is "Data are preliminary, pending verification,
by the contractor laboratory", which in this case means receipt  of  better  GC/EC
pesticide chromatograms.

This form gets directly attached to the data for the case and sent  to the  user,
in this case FIT.   This ends the organic portion of data  review. Are you  ready
for the easy stuff?  Inorganic data has mistakenly been slighted in the inches
of paper delivered, but they unfortunately are catching up.

QA 31

Inorganic data review, like organic, consists of eight major items.  Again,
these are not listed in order of importance.  These items are:   Checking
Data Sheets for clarity, verifying that a complete package is present,
looking for positive lab blank contents, calibration check results  and
frequency are sufficient, interference check samples are  analyzed properly
for ICAP  analyses, lab duplicates RPD are within acceptable limits, matrix
spike recovery is within acceptable limits, and  positive  field  collected
blank and duplicate sample results are verified.  Each of these items will
be explained in detail on the following slides,  along  with examples of  actual
cases from several contractor laboratories.

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                                     - 13 -
QA 32

Are the data sheets clear and properly coded?  Illegible data sheets  are
particularly frustrating in metals analyses.  Labs often concoct  additional
data qualifier codes which are not mentioned in the contract.  Quality
assurance summaries, provided by the contract lab, are often  hard to  decipher
because of their design.  Since we at the CRL send the report sheets  for
both organic and inorganic data without transcription onto other  forms,
clarity and readability of data sheets is an important part of data quality.

QA 33

This is a fortunately very readable Inorganics Analysis Data  Sheet for
Sample E5356, a soil collected for Case 1787/701E.  Note the code C flag
on aluminum and iron results.  This indicates that the lab method blank
contained these metals at detectable concentrations and that  the  values
of 120 mg/Kg and 904 mg/Kg have been corrected for these concentrations
by subtraction of the blank value.  The code ND/B indicates that  zinc
and lead were found at detectable concentrations in the lab method blank
and that these concentrations were higher than the sample concentration.
For example, in this case the lab preparation blank contained 20  ug/1
lead, the detection limit for lead is 5 ug/1.  Sample extract E5356 could
theoretically contain up to 25 ug/1 lead.

Note the Inorganic branch manager's signature in the lower right  hand corner.
This is an indication that the contractor has reviewed this sheet for clarity
and completeness- and it shows.

QA 34

Is the data package complete enough to allow checking of positive results
reported?  Just recently, raw data such as ICAP burn reports, and Atomic
absorption worksheets have been suggested as deliverables.  Prior to
this point, all the reviewer had to verify data was the result sheet, a
list of detection limits and often unreadable QA Summary forms.  The
deliverables should be adequate enough to allow you to recalculate the
metals values reported.  If the raw data is insufficient, detail  what
you need and send it to SMO for inclusion into the next contracts.

QA 35

This is an actual contractor lab logsheet for the graphite furnace analysis
of cadmium.  The actual conditions are listed, as is the date of  preparation
of the standard used (9/14/83).  Details of the spike preparation and the
Conostan oil and NBS river sediment values are listed.  The sequence  of
cups is also listed.  Note that the five point curve was analyzed first  at
concentrations of 0 to lOppb, and the correlation coefficient was 0.9966.

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                                     - 14 -
The actual  absorbance was listed as well  as the adjusted  and unadjusted
concentrations.  Check that the absorbances of the samples are within
the calibration curve range.  Sample 5846 and 5849 were rerun later,
after dilution, as their absorbance exceeded the lOppb standard of 203.
The unadjusted concentration multiplied by dilution factor should  equal  the
adjusted and actual  reported concentration.  The blank in position 7 is  the
prep blank, check this for contamination  above the reporting detection limit,
here it is less than one.  The EPA 475-S  in position 6 was a check QC sample,
recovered at 99%.

QA 36

Are instrument and method blanks contaminated?  As seen previously, lab
preparation blank contamination directly  affects sample results.  Check
the raw ICAP and AA data, if the QA summary indicates contamination.
Occasionally check raw data even if the contractor has not indicated a problem
to assure yourself that common contaminants such as Al, Zn, 8 are  definitely
not present.  One prep blank should be included for every 20 samples or  case.

QA 37

Here is the QA summary supplied by the contractor for the Task II  flameless
AA metals, Sb, As, Cd, Pb, Se, Tl, and Sn.  The results reported across  the
blank value row are the results of the zero standard, whereas the  results
reported across the preparation blank row are the actual  method blank  results.
Note lead contamination at 20 ug/Kg.  This was the cause  of the previous
NO/8 code.  As
a sidelight, the 129% recovery circled for selenium in spiked sample  results  is
out-of-control high, the contract limits  are 75-125%.

QA 38

Was the instrument properly calibrated and verified?  Initially, before  samples
are sent to a lab, the lab must demonstrate that it can comply with the  contract
detection limits by multiplying the standard deviation for calibration blank
solutions from 3 non-consecutive analysis days- with at least 10 consecutive
runs per day.  Each day after this that samples are analyzed, the  instrument
sensitivity expressed as absorbance for AA and gain for ICAP for the  calibration
solution must be reported.  Fresh calibration solution dilutions must  be prepared
monthly and be traced to the original reference standards by a "t" test  on data
from 5 alternating measurements of old and new standards.  Once each  10  samples
an EPA QC Solution, a NBS solution and a  contractor prepared standard  must be
run.  The % recovery of the measured values from the true cannot exceed  those
in the contract which are generally around 80-120%.  If an element recovery
is out-of-control, the instrument must be recalibrated and the proceeding
10 samples reanalyzed for the out-of-control element.

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                                     - 15 -
QA 39

Here is the ICAP data system printout for a case to look at to verify ICAP
calibration frequency.  Note that the first highlighted sample run  AR 1s  a
blank, then EPA, an EPA QC solution, then ICAP-3, EPA 10, two additional
contractor prepared QC solutions, and two ICP Interference checks.   Eight
samples are run, then a duplicate and spike of sample 5850.  This makes  a
total of 10 real samples.  Next comes the required EPA and contractor QC
solutions, 10 samples, etc...  Raw burn numbers are converted and  reported
as concentrations.  Percent recovery calculations should be included on  the
QA summary to enable you to check adherence to recovery acceptance  limits.

QA 40

Were ICAP interelement corrections made properly?  ICAP Interference check
samples are used to verify that interelement and background correction factors
are done properly.  These samples should be run initially before the days
analysis of real samples and at the end of the day to give at least 2 runs per
8 hour shift.  Results should be reported on the QA Summary and recoveries
should not be biased.  There is no contractual acceptance range.  It has been
discovered that several metals are known contaminants 1n these check samples:
Boron, manganese and barium have biased recoveries.
Here is a prime example of the boron contamination problem.  Continuing and
initial calibration show no high bias, but the highlighted initial  and final
ICP interference checks do- 172% and 146%.  All other interference check agree-
ment is good.  Associated data does not need to be flagged.

QA 42

Are the results reported of acceptable precision?  At least one lab duplicate
per 20 samples or case should be prepared and analyzed.  No contractual relative
percent difference limits have been set, we use 20% as the limit, and flag
sample elements as imprecise which exceed this limit.  The QA summary reports
these RPD's.

QA 43

Here is a no miss situation of precision- less than compared to less than-
comparable to 0 vs. 0- great precision.  As you recall, this was the driving
force to use matrix spike duplicates in organic analyses.  But what if one
duplicate had shown a detected result and the other did not?  Flag the sample
E5364 mercury result as imprecise and request a rerun if possible, or a resampling.
Note the out-of-control spike recovery of 58%.  When this occurs, the sample
may have been rerun, and a notation made, but the contract does not require a
rerun, these must specifically be requested by you after you get the data, at
an additional cost.

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                                     - 16 -
Did the method efficiently extract and quantitate the pollutants  present?
The spiked sample recovery provides the key to the effect  of the  sample
matrix on the method efficiency.  The spike solution, however,  is added
to the extract, not prior to sample extraction.  One  spiked sample per
20 samples or case should be included and the results recorded  on the
QA Summary sheet.  The spike level should be at least twice the native
sample level  if the native sample level is at least 10 times the  detection
limit.

Recovery information for elements where the spike level  swamped the  native
level, or was much too low in comparison, is useless.  The action outlined in
the contract when spike acceptance limits are not met 1s limited  to  reporting
the net response of the sample spike as a single point method of  addition
calibration for the spiked sample.

QA 45

Here is a prime example of several out -of -control spike sample  results.
Copper and maganese recoveries were out of limits- high at 121%,  nickel, silver
and zinc were all low, in fact silver was not recovered at all  at a  spike level
of 1320 ug/1 .  The 72% recovery seen for zinc may be  due to the fact that the
original sample result used in the calculation was ND/B- not detected due to a
blank contamination of 1,070 ug/1.  ND/B was considered as 0 in the  calculation,
giving the low recovery.  You might also look at the  high  silver  recovery for
all calibration and IC^P interference checks.  It would not be  unwise to invalidate
the silver data for this case.

QA 46

Is the field and sampling precision and accuracy acceptable?  If  your field
team has collected a trip or field blank and field duplicates,  these should be
sent with the samples in the case, either blind or labelled as  such. Common
hefty level contaminants seen from using bakelite capliners on  sample bottles
are Ca, Na, Mn, and phenol.  High boron is seen when  inadequate rinsing of
alconox occurs.  When metals are detected in field blanks  at measurable levels,
quantitative sample results should be flagged as possibly  due to  field contamination.

QA 47

In this field blank, 200 ug/1 of boron was detected,  the other  samples in this
case showed boron results of a similar magnitude.  Boron data therefore, was
invalidated.  Field duplicate precision limits have not been addressed in the
contract protocol, but we Regional reviewers generally use 20%  RPO as an allowable
level .

Now that you have completed your inorganic review checklist, a  summarization of
your findings should be made and attached to the data.

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                                     - 17 -
QA 48

Here 1s a completed Region V review form for metals results  for Case  1696,
which consisted of 18 water samples.  Three major problems were cited
which were used as reasons to totally invalidate the data for Task  1  metals.

Spike recoveries were unacceptable for Be, 8, Ag and Hg.   The reviewer  called
the contract lab to find out if they had rerun the samples when they  discovered
this.  A phone memo was made to document the conversation and attached  to
the review.  N£ action was taken by the lab.

Duplicate precision for six metals:  Cr, Co, Ni, Zn, B and Ag were  erratic
and outside 20% RPD.

No ICAP interference corrections were made, which indicates  that ICAP metal
data may be biased due to possible interelement interferences in the  sample
matrix.  Since this case was for a known enforcement action, reruns were done.
after the lab was clearly notified of these problem areas and corrected them.

QC 49

Some general data review hints are listed here to avoid discouraging  you.
I realize that after looking at this slide presentation,  which only represents
a small sample of the paper you must look through to assess  data quality, you
must be overdosed.

FLAG. BIASED. UNACCEPTABLE.  IMPRECISE. INVALID.  These are  not as  common as you
might think.  Good solid data 1s generated, it is not all questionable- but
it is your job to determine the good, the bad and the ugly.

If you have a problem with a piece of paper- For example, a  chromatogram
that is unreadable, or one that's missing, call SMO.  It  is  their responsibility
to ensure that you get a complete data package as defined in the contract.

Do you have a question on a result, a label on a chromatogram, the  level of
the screen, the procedure for the calibration, or the action taken  on an
out-of-control audit?  Call the designated contact person at the laboratory.
Have information such as case number, affected SMO sample number, contractor
lab sample number and your exact question and document numbers written  out
before hand.  Document what you asked and what the answer was on a  telephone
conversation record.  Send a copy to the contract lab, and SMO.

Continual QC problems with a laboratory or a method should also be  documented.
Notify SMO in writing of these problems and they will be  covered during the
next on-s1te audit or contract preparation.  You may get  to  feel like your
complaints are going to the Bermuda Triangle, but results are gotten  by
increasing the volume and force of your concerns.

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                                     - 18 -

We have looked at actual  examples of review forms for CLP data.   If you
develop a format similar to these to summarize your comments- do not allow
data to be released without these comments or forms attached.  Cover yourself-
if your name or initials appear on CLP data, the quality of that data better
be clearly Indicated, or it will  be taken carte blanche as perfect data.

I mentioned at the beginning of this presentation that you should always
keep In mind the end use of the data.  Now you know why.  CLP data review
is a labor and eyesight intensive process.  It often requires patience in
waiting for answers from the contract lab or field team.  It always involves
good technical judgement in translating study objectives to data quality
1evel.

Once you have mastered the routine menu of data packages, requests for exotic
matrices, and compounds done on unbelievably quick turnaround times need  to
be addressed.  Special analytical services, to quote a SMO coined phrase
"is not a candy store".  You must provide not only the method but the QA  for
the request.  As a veteran of the school  of hard QC knocks, I have taken  my
lumps on inadequate methods, little to none or inappropriate QC audits and
less paper to use to assess the data.  If you provide none or poor analytical
direction on SAS requests, the labs will  not bid reasonable prices, they  will
estimate time and resources poorly and you will pay the piper.

 A 50  '
Listed here are several items to include in your SAS request.  If you address
all of these, or at least realize how the data quality will  be affected
without them you will be able to provide the user with known quality data.

The method you chose to have the contractor follow should be verified.  If
your laboratory or another has not determined the precision and accuracy of
the method, you will need to rely on the contract lab.  Any deviations that
the contract lab considers should be cleared with you after the possible
effect on the data is discussed.

If unusually low detection limits are requested, the contract lab should
verify that they can meet them.  This may be accomplished by a small initial
spiking study of the blank matrix at levels equal to, twice and five times
the requested detection limit.  Determination of a reasonable detection limit
should be made based on these recoveries.

If deliverables over and above those outlined in the regular contracts are
needed, list these additional paperwork requirements precisely to ensure that
you will have enough data to verify results.

Require that Instrument and method blanks be done at a prescribed frequency
and results reported with the data.  Determine an action level for the lab
blank and require that no sample data be reported unless all blanks fall below
the level.

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                                     - 19 -

Request additional surrogate spike compounds or different ones  to monitor
the recovery of the compounds you are interested in.  Choose those that
mimic the extraction behavior and are easily chromatographed.  Don't  forget
to define acceptable recovery limits for these surrogates and request that
action such as re-extraction be done if they are exceeded.

Matrix spikes should be requested at a suitable frequency, with the compound
or compounds of interest to determine how good the method is in the actual
matrix-.  Define the concentration to be used and an acceptable  recovery
range, if you know the method and matrix well.  If not, you may well  have
to go with the flow and take what the contractor gives you on the first
shot.

Blind QC spikes and duplicates are only as good as their disguise. I
have been known to stomp on sample tags, dip them in water, roll  bottles  in
vermiculite and write left handed to aid in their camouflage.  I  prepare  these
blinds from EPA QC ampules, spikes of lab water or garden dirt.  For  duplicates
I rely on the field people.  Reviewer know thyself in what you  consider acceptable
performance on these samples before you send them out.  Remember  that the spike
results also are only as accurate and precise as the spikee.

A check sample alleviates some of the pressure on your spiking  technique. A
check samplji is a real sample that has been analyzed over the course  of several
runs and a x and sd established for the concentration level and compound(s) of
interest.  The contract lab should be able to fall within your  statistically
determined acceptance limits using the same method.  This may be  a blind, or
designated sample.

Additional field QC samples such as trip blanks, preservative blanks  or equipment
rinsates should be incorporated into the SAS, with action levels  determined
beforehand, so you can notify the sampling team if they are exceeded.  Invalidation
of entire cases of data due to field contamination is a situation to  be avoided
at all costs.

QA 51

In general, data review for SAS's is simple, as 1t follows the  GIGO principle-
Garbage In, Garbage Out.

You can only expect data of the level of quality you wrote into the request
so the method supplied and the QC audits required should yield  the precision
and accuracy needed to fulfill the study objectives.

Remember that there is a definite trade-off in assuring the quality of data-
QC audits mean time and time means money.  There is a notion that quality is
free- unfortunately not in the contract laboratory process.

Our experience has been that contracting out for analytical services  or "outhouse"
as it is coined; has become a necessity due to resource constraints.   However,
with competent contract laboratories and in-house technical review, the quality
of environmental results need not suffer.

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                                     - 20 -

I will  now be stationed by my phone waiting to receive your  questions  or
comments on this presentation.  My phone number is  FTS or (312)353-8370.
Ask for me, Marcia Kuehl .  I hope this short training/talking  slide  show
has been helpful in starting you on your way to data  review.

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        CLP
QUALITY ASSURANCE
        AND
   DATA REVIEW

-------
The Three R's

   Read
   'Rite
   'Rithmetic

-------
             BACKGROUND HOMEWORK

1.  Read Statement of Work, Analytical Methods, QAIQC
   Sections of Contract(s)
2.  Write The Data/Sampling Objective For The Case
   To Be Reviewed
3.  Brush Up On Arithmetic Behind "x,SD, RPD, % Recovery
   RF, RRF, RRT, % Change Calculations

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         ORGANIC 8
1.  Instrument Tune
2.  Blanks
3.  Positive Priority Pollutant Hits
4.  Tentative ID Hits
5.  Holding Times
6.  Duplicates
7.  Surrogates
8.  Matrix Spikes

-------
ORGANIC 1
Do DFTPP and BFB
Spectra Meet Contract
Required Abundance Criteria?
Key: MS Abundance List

-------
           SC/MS PERFORMANCE STANDARD - DecaHuorotriphenylphospMne
           Pit* i-iu-vs    tun Mo. Byiiiei'auciT Analyst
•/t
SI
«.
70
127
197
198
199
27S
365
441
442
443
Ion Abundance Criteria
30-601 of MSS 198
less than 21 of MSS (9
less than 21 of MSS 69
40-601 of MSS 198
less than 11 of MSS 198
base peak, 1001 relative abundance
5-91 of MSS 198
10-301 of MSS 198
>11 Of MSS 198
less than MSS 443
greater than 401 of MSS 198
17-231 of MSS 442
Spec «
G-^T 1
^i Q O
%
•
4^ 1 m A
K*%
^J • 0
100%
>.u%
»*%
*w
•».**
50'.
(»gV)
Spec!
dS
01
^\%
fcO%
07,
\o*'k
11*
11%
J-n
•r/.
5b7,

Spec «
31'/.
'•^
^'r/,
YIC/,
zr/.
1007.
c-f.
A3V.
17,
/of.
^7.
. 2./'/=
Coonents:
                                     20
fentachlorophenol Response Factor » Area  166
Area 266
   50
teniidfne Detectable I SOng level  IT! yes  PI no
Area (counts) 20ng dlO anthracene
CoTuan description

-------
                         INSTRUMENT TUNE AND PERFORMANCE SUMMARY
CASE NO 	
SAMPLE TXPS
CONTRACTOR
LEVEL
                    NO.'
                                                                            82-AQfiQ
DFTPP and BFS Performance Results;

   r^ DFTPP performance results were reviewed and found to be within specified criteria
 X   BFB performance results were reviewed and found to be within specified criteria
                  DFTPP
Mass   Ion Abundance Criteria
       30-60 percent of ness 198
       less than 2 percent of mass 69
       less than 2 percent of mass 69
       40-60 percent of mass 198
       less than 1 percent of mass. 198
       base peak, 100 percent
       5-9 percent of mass 198
       10-30 percent of mass 198
       greater than 1 percent of mass 198
       present but less than mass 443
       greater than 40 percent of mass 198
       17-23 percent of mass 442
177
                                    BFS

                             Ion Abundance Criteria	
                             15-40 percent of mass 95
                             30-60 percent of mass 95
                             base peak,  100 percent
                             5-9 percent of mass 95
                             less than 2 percent of mass 174
                             greater than 50 percent of mass 95
                             5-9 percent of mass 174
                             greater than 95 percent but
                             less than 101 percent of 174
                             5-9 percent of mass 176
DEVIATIONS

Date/TOTe/lnst F5_Le Number Canpound
OWA
/Required
m/z . / Abundance
/

OWA /
                                                                       Observed
                                                                      ^Abundance
           nwa
           CHA
 CCf&ENTS
                                      FORM VTE

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ORGANIC 2

Are Instruments and
Method Blanks Contaminated?
Key: Blank RIC's

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                            QUALITY CONTROL NOTICE
Tht volatile analysis of blankgBeSoT/^shows the presence of the laboratory
irtifact s1lo»at»e it «can  a****-    .  The pre&enc* «f thi* compound Jus
resulted from the addition of an ant1foaming agent and maj- or •§/ not Actually
b« present 1n this samplt.  SlUxane has not been listed as one of the non-
priority pollutant conpounds identified In this saapl*.
                            QUALITY ASSURANCE  NOTICE
                 The compound 4-hydroxy-4-methyl-2-pentanone  has been
       detected in the semi-volatile fraction's  analysis  of this sample.   .
       This compound has been flagged in the data  report  as a suspected
       contaminant or artifact of the analytical procedure.   One
       literature reference indicates that in the  presence of acetone  and
       hyrdroxide this compound can be formed, so  it 1s possible to  have
       been produced during extraction of the semivolatile*.   The  laboratory
       glassware 1s rinsed prior to use with acetone, followed by  methylene
       chloride;  if the second rinse 1s incomplete, it is possible  that
       residual acetone could produce, as above, this compound.  Further
       studies are underway to determine the source of this compound.

-------
(M
00


g
i
     en
     Ot
    W
    9
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8   i
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                                                                                               lo

-------
       ORGANIC 3
 Are Positive "Hit" Priority
Pollutants Actually Present?
Key: MS of Sample/Standard

-------
                          _a  	j	•
o 
-------
NO
57
58
59
*rf 9
60
A,*
Ox
62
%f ^»
63
64
65
66
67
68
69
70
71
72
73
74
75
76
77
78
79
NO
1
2
3
4
5
6
7
8
9
10
11
12
13
14
IS
16
17
18
19
20"
21
22
23
24
25
26
27
28
29
30
31
M/E SCAN TIME REF RRT HETH
NOT FOUND
&*/««r BT/M v^m
NOT rOWU
178 1658 20: 43 48 JL 002 A W
178 1666 20: 49 48 JL 007 A VB
932 .1B80 23: 3O 48 JL 137 A BB
4£ VC* ^"iS^?^^ ^M%» ' Vv^r T^rf Mto* ^»*w f ^^ vrW
202 1722" 24: 01 48 JL 162 A BB
77 1506 18: 49 48 0. 911 A W
149 1776 22: 12 48 JL 074 A BB
266 1634 20: 25 48 0. 988 A BB
240 2182 27: 16 66 JL 000 A BB
228 rgj?77 27:13 66 0.998 A BV
228 GHS9 27:22 66 1.003 A VB
NOT FOUND
149 2056 25: 42 66 0. 942 A BB
149 2209 27: 37 66 JL 012 A W
149 2437 30:28 66 1.117 A VB
NOT FOUND .
NOT FOUND
NOT FOUND
278 3600 45: 00 66 1. 650 A*BV
NOT FOUND
252 2581 32: 16 66 JL 183 A VB
NOT FOUND
RET(L) RATIO RRT2^

RATIO
1. 00

0.02
0. 16
0. 01
0. 00

O. 00

0. 01

0. 00
0. 04
0. OO
2.07
1.59
2. 28
2. 39
JL 89
2.95
1. 00

0.01

0.00


0.01




-------
IDENTIFIER   SEMI-YOLATJLES
LOW LEVEL SOLID
CO^OUND QUAKT. REPORT CORRECTION DETECTION
UUJ-BER CO*OUNDS VALUE * FACTOR • RESULT LIMIT (ug,
478
460
476
479
626
401
605
607
432
417
424
604
443
414
433
>444
403 -
M31
M45
430
426
609
"405
~418
423
415
413
429
404
406
437
419
408
^•407
409
2-NITROAMILINE 	 Vo 4000
3.N1TROANILINE 	 \ 4000
DI BENZU" URAH ••••••••••••••••«••••
4-NlTROANILlNE •••••••••••••••••••
2.4.5-TRICHLOROPHENOL 	

2.4-DINITROPHENOL 	 ; -
4-MITROr HtNOL ••••••••••••••••••••
FLUOR ENt •••••••••••••••••••••••«•
4-CHLOROPHENYL PHEMYL ETHER 	
DIETHYLPHTHALATE 	
4.6-OIN1TRO-0-CRESOL 	
DIPHENYLAWNE (K-NITROSO) 	
4-BROMOPHENYL PHEMYL ETHER 	
HEXACHLOROBCNZENE 	 	
PHtNANTHRtMt •••••••••••••««•••... i.^
ANTHRACENE 	 	
CJ Hftfi lUTHTUT 2.V
r LUwi\Ani ribnb •••»••«•••••••••••••• **7
PYRENE 	 r?
1.2-DIPHENYLHYDRAZINE (AZ08ENZENE)
OI-N-BUTYLPHTHALATE 	
PENTACHLOROPHENOL 	
BEN20{ A) ANTHRACENE 	 2-3
CiWTStNfc ••••••••••«....•.•.•...•• •
3.3'-DICHLOROBENZIOINE 	 	
BUTYLBENZYLPHTHALATE 	
BIS(2-ETHYLHEXYL)PHTHAUTE 	
OI-M-OCTYLPHTHALATE 	
BbnZIUtNC •••••...••••«.•••• ••«••«
BENZO(A)PYRENE 	
INOENO(1.2.3-C.O)PYRENE 	
DIBENZO( A. H) ANTHRACENE 	
BENZOfG.H.nPERYLEME 	
400
4000
4000
400
2000
4000
400
400
400
800
400
400
400
&£ 400
400
Ho 400
?z-o 400
800
400
800
tt-» 400
/r
-------
      ORGANIC 4
Are Tentatively Identified
Compound Matches Reasonable?
Key: MS of Sample/Search

-------
en
  Is-
   (0  P

       CD

   ® §<5
  I mca •
  ! in ji
                              in

                                                    CM
                                                    a
                                                                         T
                                                                                               
                                                                                               CM
                                                                                               CD
                                                                                               O
                                                                            ••     CO

-------
       ORGANIC 5
Were Sample Extraction And
Analysis Holding Times Met?
Key: Analysis Chronicle Traffic Report

-------
                                EXTRACTION - GC  SCREEN
                                       NEIC II
     EPA Case i
                                         Document Control I
    For:  PESTICIDE
 Matrix:  Liquid

3-S~-/^
Dash I
EPA
Sample 1
Tare 4
sx (g)
Tare
(9)
sx Wt.
(9)
Vf
Date/
Time
Analyst

     -07
      /
-------
                SCREEN EVALUATION FORM
                        NE1C »1
                                    For:  Pest1ci<1e/7££>/)
                                 Matrix:
EPA Case I
1g/i
-------
                                                        SAMPLE  NO.
                                                        PESTICIDE  SCREEN
cs
 24. ?
0.B
' 27.51

                f ' f

RUN I  172

HEIGHT*
   RT
 22.38
 24.99
 25.78
 28.82
 29.23
 29.48
 29.69
 38.77
 31.21
 37.76
TOTAL HGHT=
HUL FACTOR=
                                                                     JUL/W/83
HEIGHT TYPE
28534 PV
41787 PB
116528 PB
46689 VB
45618 PB
24645 BB
98952 BV
1451538 SPB
52638 PB
AR/HT
8.879
8.645
8.847
8.839
8.839
8.883
8 839
6 854
8.633
                                                            24858   VB   8.112
               1923788
                                 HEIGHT*
                                   1.483
                                   2.168
                                   6.857
                                   2.427
                                   2.371
                                   1.281
                                   4.72S
                                  75.457
                                   2.736
                                   1.292
 34.48
 34.91
                                                                 000253
 S7

-------
             ORGANIC 6
Are The Results Of Acceptable Precision?
          Key: Duplicate RPD

-------
25&  zwae   CVK>
                                                   US MWC:
                                                      Mat
                                               CASE
                                       0*16. iw«»u
     CWQUOS
                                                           KLATIVC KJCCWT
    J-f lucre* f>Ttt*«
     o-ch!oro-m-cr«soT
     2.4-dlmethvlohenol
_Ifi5&)_
     hsxachlorobenzene
                              1000
                                  91*
                                            1200
                                           22 ««
                                                               t/o
                                                                   0.2.

-------
     ORGANIC 7
Are The Results Reported
Of Acceptable Accuracy?
Key: Surrogate Recovery

-------
FORK III
000003

-------
                Initial Calibration Data - Volatile HSL Corpounds
              Contractor
Case no.
Instnment Identifier
Hininun HF for SPCC IB 0.30
                            Contract Ho. VA 82-A069
         CCM>C(JND
                             RKT
         ^
                                                20
^
                                                       200
RF  I SPCC
  Chlorane thane
                                                    X.??4?
  Be
thane
&gT7
  Dichlarorti f luaranethane
  Vinvl Chloride
  Chloroe thane
  Methvlene Chloride
                                                    L3JL
                                 2S&2L.
  Acrolein
                                            Q./W
                                                              .SZfi.
  Acetone
                                    LISTS
   Acrylonitrile
  Carbon OisnTfirie
   Trichloroflixsrome thane
   1^ 1-Dichlaroethylene
   1,1-Dichloroethane
   trans-1 , Z-Dichloroethylene
                            /./<*>
                 2./3L5"
2.&SC*
   Chlorof arm
   2-Butanone
                            t,Z5*>
                 &LLL.
0.705-   a.usq
   1 , 2-Dichloroethane
   1.1. 1-Trichlorethane
                                    2. 636
   Carbon Tetrachlaride
                            /,*//
         /
   Vinyl Acetate
   EtoroiichlcDramethane
                                    3.0X7
   Carbon Tetrachlaride
   1,2-Dichlc

   Trlchloroethvlene
                            o.'fcn
   Benzene
                                                             I.S3S7
   1,1, 2-Trichloroethane
                                    6S10
   2-Chloroethyl vinyl ether
   4-Methvl-2-pentanone
   2-Hexanone
   1 . 1 . 2 . 2-Ttetrachloroethane
                                                     Q3/&
   TetrachloroethYlene
   Toluene
   Crxluii t <.**i iz
   trans-1,3-DichlQropropen
                            M22.
 Q.9/7
 o"
-------
CASE SO.
INSTRUMENT IDENTIFIER

STANDARD FILE
Maximum ED for CCC is   20
CALIBRATION CHECK - VOLATILE BSL COMPOUNDS

 CONTRACTOR 1SBSSB3SSSBBBSS&    CONTRACT NO. VA 82-A069

  QUA                   CALIBRATION DATE  ^/3 ^

        	    DATE   %-U-*ft       TIME   /7

                       Minimum RF for SPCC  is  _0.300_
CCHPOJND 1
I
1
Chloromethane
BtuociiethdnB
Dichlorodi f luonromethane
Vinvl Chloride
Chloroe thane
Mfethylene Chloride
Acrolein
Acetone
Acrylonitrile
Carbon DisuLf ide
Trichlorofluorometlianc
1. 1-Dichloroethylene
1 . 1-Dichloroethane 1
trans-1 . 2*0ichloroethyljena
Qilorof onn
2-Butanone
1 . 2-Dichloroe thane
1.1, 1-Tr ichlorethane
Carbon Tetrachloride
Vonvl Acetate
Bronodichloranethane
Carbon Tetrachloride
1 f 2— Dichluji i.^>i. ufi&ns
TrichlaroethYlene
Benzene
Chlorodibraicmethane
1 . 1 . 2-TricW oroe thane
2-ChloroethYl vinyl ether
Branoform
4-MeLhvl-2-Dentanone
2-Hexanone
1.1.2. 2-Tfetrachlorcethane
Tetrachloroethvlene
Toluene
Qxlorobenzene
I trans-1, S-Duchloroytopene
Ethylbenzene
cis-1,3- Dichloropr-operie
Styrene
• o-Xylene


RF
2,051
t.SW

mi
ICLL
2.C03 1
A.m
0.1^
Ai73
5.-72JO

2./05"
r?i,M^
/.TT^
?.9Fi
O.CiSV
z.ni
2.3 »
Z.3&
3.2J1
\2.
O.VT3
hlH5
6.U3-
C.3GC.
A^^O
AVT7
A5S7
O.'HV
J5.1KL
rt.vsi;
/.rf*5"
t>,^?C.
/.^/3


»
f?7?
/.7«3

ED 1 CCC 1
vJ
-/Si,

2.C^ -7.T
/.5S? -^.1
3$fe
0.//7
J.33.C
n.^T
27.577

2.y&?
^?.3^6£>
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-/^
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-7.7
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-Mo
-/7,v
-/7^

-317. X^
^. 
-------
                       SEMIYGUTXL&
                                                   CONTROL CHART  ^'"
        BELAT1YE RESPONSE
        r
        ».
          *-*-*-
      .4

      .•
           *~-r
                    SEMIYOLATILE:  DB-NAPHTHALENE/DlO-P^CNANTHRENE

                               KM             IB.
                                            UL




It
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RELATIVE RESPONSE
r
i*
: >T TT
:
f i - A i » « "ANALYSIS" " « •• "
ewxr MOVE currna » z/is/w IK» nu ZSRVCCID

^
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                     SEMIVOLATILL-  D10-PHENANTHRENC/D12-CHRYSENE
                                                IB.
      1.4



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      0.0
         3FLATTVE RESPONSE
t-^t-
                         buirr
   DATE
  ANALYST
CDHHENTS

                                        A
                                            oco rnj

-------
              ORGANIC 8


    Did The Method Efficiently Extract
And Quantitate Priority Pollutants Present?
    Key: Matrix Spike Recovery

-------
     f
           3
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                                                                                                                                    2

-------
                  UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
                                      REGION V
   DATE:
SUBJECT: Review of Region V CLP Data     /  /
        Received for Review on        ?////
  FROM: Curtis Ross, Director
       Central Regional Laboratory
      : Data User:
        We have reviewed- the data  for the following case(s) .
        EPA Data Set No. SF J
 No.  of
-Samples:
                                                        SMO Case No.
D.U./Activity .
  Numbers  Yfaf I c
        CRL No.'s
        SMO Traffic No.'s
        Contract Laboratory:

                              Hours  Required
                             -  for Review:
        Following are our findings.
        ( ) Data are acceptable for use.
        ( ) Data are acceptable for use with qualifications noted above.
        J^) Data are preliminary - pending verification by contractor laboratory.
        ( ) Data are unacceptable.
   » "•
        cc:  Dr."Alfred Haeberer, EPA Support Services
             Ross K. Robeson,  EMSL-Las Vegas
             Robert Pritchard.  CLP-SMO
 B»* FORM 12204 «EM 3-7»          /    .

-------
INORGANIC 8
1.  Data Sheets
2.  Complete Package
3.  Blanks
4.  Calibration Check
5.  Interferences (ICP)
6.  Duplicates
7.  Matrix Spikes
8.  Field QC

-------
     INORGANIC 1

Are The Data Sheets Clear
  And Properly Coded?
Key: Report Sheet, QA Summary

-------
  US ENVIRONMENTAL PROTECTION ACENCY
  rfTT Sample Management Office
  Pa Box SIS - Alexandria. Virginia 22313
  /03/357-2*90  fTS "	
                                              i-i-
                                                   SCP201C33
 7S1.1V
                                                        :
                          INORGANICS ANALYSTS DATA-SHEET
                                                                               No.
                                                                         5336
LAS NAME
                                            CASE NO.
                                                            /
LAB SAMPLE 03. NO.   SS'VV £8 £94.^94  QC REPORT NO.
                                                                   - 3 3
L>  Aluminum
2>  Chromium
3.  Bartum
   Bervllium
   Ccbalt
 6.  Cfiooer
 7.  Iron

 *  NM«*
 9.
                      TASK L (Element! to b« Identified and Measured)
                                           10.  Zinc
                               or
                            (circle ere
                        16.
il.   Boron
                       HO.
12.   Vanadium
                                                 Silver
                         VO.
                        16.
                        60.
                         7.
                                                                          ug/l of ^
                                                                           (circle cne
                                                                  JLO.
                                                                   16.
1.   Araenic
2.  Anfjr.cnv
 3.  Selenium
 *.  Thallium
                       TA2X 2 (Elements » be Identified and Measured}

                      .
                                              3.  Mefgary
                                              4.
                                              7.   Cadmium
                                             «.   Lead
                          01

                          02
                                            ar.aoer

-------
       INORGANIC 2
Is The Data Package Complete
 Enough To Allow Checking
Of Positive Results Reported?
Key: Raw Data Present
     To Allow Recalculation

-------
                                                   Page
                      TRACE BETALS SECTION
                FLAHELESS AAS ANALYSIS LOG SHEET
CLEMENT:
PROJECT/BATCH:
                    Cc/
                                      DATE
             im SLIT:  O, 7
               EOL   t<_ HCL
INSTRUMENT:
WAVELENGTH:
LIGHT SOURCE: 	
CURRENT/POWER: 	
BACKGROUND CORRECTION: .
STANDARD PREP. DATE:    ?•/¥•&*
    TUBE:
    PURGE: 	
    PIPET  VOL:
                                             A/
                                                          REP:
                                                          _»1
CUP
1.
2.

4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
LAB I
Jjff
A/X
                   ': Jtt&L tft
Steo
Tewp *C
ijtamp (s)
Hold (*)
Boc (s)
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1
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                          UNAOJ.
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                   £7
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                               X2
AOO.
CONC.
COWENTS
                                                            9-
                 '3ap
                                                            99%
                                                       (/
                                  INITIALS
                                                                         3S

-------
      INORGANIC 3
Are Instrument And Method
  Blanks Contaminated?
Key: AA, ICP Printout, QA Summary

-------
o
CO
9
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A
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                                                     37

-------
      INORGANIC 4

Was The Instrument Properly
  Calibrated And Verified?
Key: QA Summary

-------
  •
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                                                       . .. ,_*. _ - - .  — - — - - .^ - -. - -  -•  *"^ (^

-------
      INORGANIC 5

  Were ICAP Interelement
Corrections Made Properly?


Key: Standard Solution Recovery
                                      4o

-------
       ! J
                i
                        ;<3:
                    i re O. Q «t
                    I ti  
-------
     INORGANIC 6


Are The Results Reported
Of Acceptable Precision?
Key: Duplicate RPD

-------
CASE
t A«?
                       INORGANICS Q,UAUTY ASSURANCE
OC HEWITT * :.
                  TASK 1I/COLO VAPOR

                  ATOMIC ABSORPTION
INITIAL CAUIAA71QM
VES1WCATHJII
                       STAflOAAQ
                       IUUIX VALUE
                                            KlUMO
                                           mui
                                           « fttcavt RY
'HE5ULTX
                        /GO.
II.
camnuiNO
CAUSRATUM
VtfllFICATtQM
                        IUJIK t  t JTf/S
                                           MSULT3
                        ILAMKZ
                                           HBULTS
                        STAMOARO
                        soumon 1
POUMO
                                            TMUt
                                             ai cavcnY
ntuf
                                            % RCcavtaY
                        STAJIOAAa
                        saLimai 3
                                            mut
                                            X RCC3VUY
                        STAJIOAflO
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                                            nui
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                       /of
                                                                 /ol
 IIL
 OUWJCATI
 SAMTU XESUITS
                        BWUCAT11
                                            tfJffUfttSlLT
                                          3 01VUCATI RESULT
                        OIVUCAT12
                                            SAMPU RESULT
                                            OIVUCATI RESULT
                                            Rn*
                                                                 
-------
           INORGANIC 7
Did The Method Efficiently Extract And
  Quantitate The Pollutants Present?
Key: Recovery Spiked Sample

-------
8
>
I
   3
n 4 
          to S' <*:
       I —
    N  iS
                  O
                  ^
                       o ^l^'^S.^SX^
                       T > i» •>• rC! P"  i lO,
                 C'^ 
-------
       INORGANIC 8
Is The Field/Sampling Precision
  And Accuracy Acceptable?
Key: Field Blank, Duplicate

-------
US ENVIRONMENTAL PROTECTION AGENCY
HVI Sample Management Office
P.O. Box SIS - Alexandria, Virginia 22313
703/557-2*90 FTS S-557-2*90
        NEB
  MAY 2 41283
 535 S. Cl A<
^ $
< f 0
TASK 2 (Elements to be
^—{circle one)
«L/0
^t^>
*- Z-
«^/o
CASE NO. /^^S
QC REPORT NO. &*J
Identified and measured.)
11. Manganese
12. Zinc
13. Boron
1ft. Vanadium
15. Calcium
16. Magnesium ^*
17. Sodium ^^
identified and measured.)
3. Mercury ^»0 • 2
6. Tin
7. Silver

^ ^u(^ji/ir

Icircle one)
*- 10
1«-o
^ z^-o
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COMMENTS!
                                                                            47

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                UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
                                   HEGION V
MOM. Curtis Ross. Director
    'Central Regional Laboratory
  TO-.Data User:

     He have reviewed the data for the following case(s).

     SITE

     EPA DATA SET ftO.

     CRL NOS.

     SMO TRAFFIC MS.

     CONTRACT LAB:
HOURS REQUIRED   u >/
  FOR REV1W:  —-f-f*
     Following are our findings.
                   ,  tio. D.J


         Data are acceptable for use.
         Data are acceptable for use with qualifications noted above.
         Data are preliminary - pending verification by contractor laboratory.
         Data are unacceptable.
          Or. Alfred Kaeberer. EPA Support Services
          Or. Gene Meier, CMSL-las Vegas
          Robert Pritchart, CLP, Sample Management Office

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         DATA REVIEW HINTS
Missing Paper? Call SMO
Questions On results? Call Lab
Document Continual QC Problems
Document Telephone Conversations
DO NOT Allow Data To Be Released
Without Review Comments Or Form Attached
Keep In Mind End Use Of Data During Review

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SAS QC SUGGESTIONS
Verification Of Method Adherence
Detection Limit Verification
Paperwork Requirements
Instrument And Method Blanks
Surrogate Spike(s)
Matrix Spike(s)
Blind QC Spike
Blind Duplicates
Check Sample
Field QC Samples

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        SAS DATA REVIEW
       THE GIGO PRINCIPLE
1.  Can Expect Data Of Level Of Quality
   YOU Wrote Into The Request So ...
2.  Contract Method Supplied Or Chosen
   Should Be Of Known P&A
3.  Remember: QC=Time=$

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