QATS SPECIAL-REQUEST & SITE-SPECIFIC PESs

QUALITY ASSURANCE TOOLS FOR RPMs
Special-Request and Site-Specific PESs
Keith Strout
Shaw Environmental, Inc.
Quality Assurance Technical Support (QATS) Program
John Nebelsick
USEPA Analytical Services Branch (ASB)

PES PRESENTATION OVERVIEW
QATS Program Overview
PES Program Summary
Special-Request and Site-Specific PES Program
PES Ordering
PES Results Evaluation and Reporting
PES Contact Information
19th Annual NARPM Training Conference • June 2-5, 2009 Atlanta, Georgia 1

QATS PROGRAM SUMMARY
Quality Assurance Technical Support (QATS) Contract Number EP-W-
06-005 operated by Shaw Environmental, Inc.
QATS Program customers include USEPA ASB, USEPA Regions, &
other USEPA Programs.
QATS products include:
Provide Performance Evaluation Samples (PESs) and Reference Materials
(RMs) for the Superfund Program.
Provide electronic and hardcopy data audits.
Conduct on-site laboratory audits.
Perform methods and guidelines development and evaluation.
Provide logistical and administrative support.
Shaw QATS Program has 20 years experience providing PES & audit
support.
Shaw QATS Program Quality Management System (QMS) is ISO
9001:2000 certified.
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QATS PES PROGRAM
PES use in the Contract Laboratory Program (CLP)
PESs are typically analyzed along with environmental
samples as requested by the EPA Regions.
PESs are used to monitor and document the
performance of laboratories and analytical methods.
PESs are used to evaluate the performance of all CLP
labs on a quarterly basis (QB Program).
PES analysis is used in the contract solicitation process.
PES results are used to assist in the validation of
environmental sample analysis results.
PES usage enhances the confidence in the quality of
data and the decision-making process.
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QATS PES PROGRAM
QATS Standard PES Inventory
Single-blind quality control samples.
• Sample is recognizable as a PES.
Analytes and concentrations in PES are unknown to the
laboratories.
Analytes and concentrations are typically in accordance
with the CLP Statements of Work (SOWs).
Aqueous samples are concentrates for dilution.
Soils are full-volume samples.
All standard PESs are shipped with chain-of-custody
records and PES preparation and analytical instructions.
PES results are usually scored using the QATS webbased
PES scoring application (SPSWeb).
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QATS PES PROGRAM
QATS Standard PES Analytical Fractions
Organics include waters and soils for volatiles,
semivolatiles, 1,4-dioxane, pesticides, Aroclors,
dioxins/furans, and PCB Congeners.
Inorganics include waters and soils for metals, cyanide,
and mercury.
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QATS PES PROGRAM
Current QATS standard PES inventory contains
approximately 100,000 aliquots.
All QATS PESs & RMs are listed in the USEPA
Superfund PES catalog which is updated annually
and available in hardcopy and online to authorized
PES requestors.
Previous 12 months:
QATS Program distributed over 2,400 PESs.
QATS Program distributed over 700 RMs.
All QATS PESs & RMs subjected to scheduled
stability testing.
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NUMBER OF PESs
1000
900
800
700
600
500
400
300
200
100
0
ASB
OEM
QATS PES PROGRAM
REGION
I
USEPA QATS SUPERFUND PES USERS
2006, 2007, & 2008
REGION
II
REGION
III
REGION
IV
REGION
V
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REGION
VI
REGION
VII
REGION
VIII
2006 Total 2007 Total 2008 Total
REGION
IX
REGION
X
Other

QATS PES PROGRAM
QATS Special-Request & Site-Specific PESs
PESs not in the standard QATS PES Superfund
inventory or in the Superfund PES Catalog.
PESs that can be made at the QATS Laboratory on
special-request through the Regional CLP PO or
authorized PES requestor.
PESs that can be purchased from commercial PES
vendors through the QATS Program.
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QATS SPECIAL-REQUEST & SITE-SPECIFIC PESs
Why do Regions order special-request PESs?
CLP target compounds needed at defined concentrations
and/or in specific combinations.
Site-specific target compounds not found on the CLP list.
Site-specific matrices needed.
Full-volume and/or double-blind PESs required.
Validation of method or site-specific detection limits are
required.
Laboratory comparisons or evaluations are needed.
Verification of project-specific analytical precision and
accuracy needs.
Other RPM considerations.
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QATS SPECIAL-REQUEST & SITE-SPECIFIC PESs
Special-request & site specific PESs have included:
Full-volume and double-blind water and soil samples for
volatiles, semivolatiles, pesticides, Aroclors,
dioxins/furans, PCB Congeners, 1,4-dioxane, metals,
mercury, and cyanide.
Perchlorate in water.
Volatiles in air (SUMMA canisters).
NIST fish tissue RMs (PCBs, pesticides, dioxins/furans,
methyl mercury).
Nitroaromatics & nitramines explosives.
Chloral hydrate in water and soil.
Dioxins/furans and PAHs in air XAD-2 resin cartidges.
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QATS SPECIAL-REQUEST & SITE-SPECIFIC PESs
Special-request & site specific PESs have included
(continued):
Aqueous total and hexavalent chromium.
Hydrazine.
Methyl mercury in marine tissue.
Aqueous selenium.
Uranium in soil.
Carbamate pesticides.
Asbestos.
Full-volume classical chemistry parameters.
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QATS SPECIAL-REQUEST & SITE-SPECIFIC PESs
REGION IX PGAN SITE
Region IX long-term PGAN Site Project
Superfund site contaminated with trichloroethene (TCE)
and perchlorate.
Includes 14 quarterly events over 3+ years.
Full-volume double-blind PESs prepared in containers
provided by sampling contractor.
64 TCE PESs ranging from 2 to 300 ppb.
58 perchlorate PESs ranging from 1 to 200 ppb.
Four (4) laboratories have performed analyses.
Regional personnel coordinate with sampling contractor
and QATS Laboratory.
Samples produced at the QATS Laboratory and sent to
the sampling contractor.
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QATS SPECIAL-REQUEST & SITE-SPECIFIC PESs
REGION IX PGAN SITE
Region IX long-term PGAN Site project (Continued)
Sampling crew labels samples and submit them to EPA
Regional Lab and contract lab as double-blinds.
Results are evaluated at QATS and reported to Regional
CLP PO.
Results are trended by QATS and provided to Region on
periodic basis.
Feedback from Regional CLP PO indicates that the RPM
finds the PESs results and trending very useful.
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QATS SPECIAL-REQUEST & SITE-SPECIFIC PESs
REGION IX PGAN SITE
%RECOVERY
200
150
100
50
0
A - 1
A - 1
A - 1
TRICHLOROETHENE - USEPA REGION IX PGAN SITE
USEPA AND CONTRACT LAB RESULTS AND LIMITS FOR
QATS VOA FULL-VOLUME DOUBLE BLIND WATER PESs, 2005 - 2009
C - 1
B - 1
B - 1
B - 2
A - 2
A - 2
B - 3
A - 4
A - 4
B - 4
A - 5
A - 5
B - 6
A - 6
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A - 7
A - 7
B - 8
A - 8
B - 9
B-10
USEPA LAB %REC
CONTRACT LAB %REC
LAB - EVENT
4 Labs; n=64; Ave %Rec=100%; RSD=12%; Spike Range 2-300 ppb
USEPA CLP MATRIX SPIKE LIMITS (71-120%)
PGAN PERFORMANCE LIMITS (68-133%)
B-10
A-10
A-11
D-11
A-12
D-12
A-13
D-13
A-14
D-14

%RECOVERY
QATS SPECIAL-REQUEST & SITE-SPECIFIC PESs
REGION IX PGAN SITE
200
150
100
50
0
A - 1
A - 1
B - 1
C - 1
PERCHLORATE - USEPA REGION IX PGAN SITE
USEPA AND CONTRACT LAB RESULTS AND LIMITS FOR
QATS FULL VOLUME DOUBLE BLIND WATER PESs, 2005 - 2009
C - 1
B - 2
A - 2
A - 2
B - 3
A - 3
A - 4
B - 4
B - 4
B - 5
B - 5
A - 6
B - 6
B - 6
USEPA LAB %REC
LAB - EVENT
4 Labs; n=62; Ave % Rec=102%; RSD=11%; Spike Range 1-200 ppb
CONTRACT LAB %REC
USEPA METHOD 314 LABORATORY FORTIFIED BLANK LIMITS (85-115%)
PGAN PERFORMANCE LIMITS (72-132%)
B - 7
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B - 7
B - 8
A - 8
B - 9
B-10
A-10
A-11
D-11
A-12
D-12
A-13
D-13
A-14
D-14

QATS SPECIAL-REQUEST & SITE-SPECIFIC PESs
REGION IX PGAN SITE
Ave. %
Rec.
RSD
n
Analyte & Laboratory Comparison
Regional Lab
TCE
103.6
14.9
30
ClO 4 -
106.2
9.4
29
Contract Labs
TCE
97.6
7.6
34
ClO 4 -
97.9
10.9
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33
Combined
TCE
100.4
12.1
64
ClO 4 -
101.8
10.9
62

QATS SPECIAL-REQUEST & SITE-SPECIFIC PESs
REGION IX PGAN SITE
Spike
Concentration
1 ppb (n=3)
2 ppb (n=3)
Perchlorate Detection Limit Challenge
Regional Lab
All detected
Ave. = 1.3 ppb
All detected
Ave. = 1.9 ppb
Contract Labs
All reported as nondetected
All detected
Ave. = 2.4 ppb
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QATS SPECIAL-REQUEST & SITE-SPECIFIC PESs
REGION IX PGAS SITE
Region IX PGAS Site project
Superfund site contaminated with trichloroethene (TCE) and
chromium.
Samples coordinated, prepared, shipped, and evaluated similar to the
PGAN samples – First QATS Lab PES event in February, 2009.
Spike Conc.
5.0 ppb
Spike Conc.
100 ppb
Regional Lab
TCE
4.8 ppb
Total Chromium
98 ppb
Contract Lab
TCE
4.9 ppb
Total Chromium
98 ppb
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QATS SPECIAL-REQUEST & SITE-SPECIFIC PESs
REGION IX SAN GABRIEL SITE
Region IX San Gabriel site – low concentration full-volume PESs
prepared to validate non-standard methods.
Laboratory reported results consistent with nominal concentrations of
PESs prepared at QATS Lab – 5 different PESs and 4 different labs.
PES Analyte
1,2,3-Trichloropropane
1,4-Dioxane
Hexavalent Chromium
NDMA
Perchlorate
Spike Conc.
0.05 ppb
1.5 ppb
0.30 ppb
0.20 ppb
3.0 ppb
Laboratory Result
0.06 ppb
1.7 ppb
0.34 ppb
0.22 ppb
3.4 ppb
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QATS SPECIAL-REQUEST & SITE-SPECIFIC PESs
REGION IX MONTROSE SITE
Region IX Montrose site – 5 different PESs
prepared at custom concentrations
2 Pesticide soil PESs at specific concentrations including
non-CLP targets 2,4’-DDT, 2,4’-DDD, and 2,4’-DDE.
P-Chlorobenzene sulfonic acid (p-CBSA) a 4,4’-DDT
derivative.
Chloral hydrate in soil
Hexavalent chromium
12 Different PES and sampling events using 43 PE
samples
3 Labs participated (Region IX, CLP, & non-CLP)
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QATS SPECIAL-REQUEST & SITE-SPECIFIC PESs
REGION IX MONTROSE SITE
Special-request chloral hydrate soil PESs confirmed
the presence of chloral hydrate at the site.
QATS also developed a method for the extraction and
analysis of chloral hydrate in soil.
Presence of chloral hydrate resulted in the identification
of a new responsible party (PRP).
Large amount of chloroform at the site led to suspicion
that breakdown of chloral hydrate was the cause – PES
usage helped confirm this.
Region was prepared to abandon efforts for chloral
hydrate detection until provided with the PESs and
method.
Pesticide PESs with 2,4’-DDT, -DDD, and -DDE are now
standard QATS PESs due to additional requests.
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QATS SPECIAL-REQUEST & SITE-SPECIFIC PESs
REGION IX CASMALIA SITE
Region IX Casmalia site – 5 different PESs
prepared at custom concentrations.
Nitroaromatics and nitramines (Explosives).
Hydrazine.
Organophosporous pesticides.
Ethylene glycol & ethylene oxide.
7 Laboratories participated.
44 samples provided.
95% of approximately 400 analyte results within limits.
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QATS SPECIAL-REQUEST & SITE-SPECIFIC PESs
REGION IX PALOS VERDE SITE
Region IX Palos Verde and United Heckathorne
sites – NIST SRM 1946 Lake Superior Fish Tissue
QATS purchased and distributed SRM 1946 to four
different labs.
QATS evaluated results for pesticides, PCB Congeners,
dioxins/furans against several sets of acceptance limits.
Results from pre-award samples convinced contractor to
use a specific lab.
QA Plan for Palos Verde specifies use of SRM on longterm
basis to demonstrate recoveries in difficult matrix.
QATS is compiling data from all events to demonstrate
trending from labs and methods.
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QATS SPECIAL-REQUEST & SITE-SPECIFIC PESs
REGION IX TARGET CONSTRUCTION SITE
Region IX Target Store Construction site – volatiles
in air (SUMMA canisters).
QATS Lab coordinated and purchased air samples from
commercial vendor for pre-award and sampling events.
Pre-award sample results disqualified lab based on QA
lab (Region IX) results.
Additional pre-award samples validated additional lab’s
analytical capabilities.
PESs for sampling event demonstrated lab deficiencies.
Regional Lab performed well on all PE samples.
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QATS SPECIAL-REQUEST & SITE-SPECIFIC PESs
REGION IX TARGET CONSTRUCTION SITE
* Outside Limits
EVENT
Pre-award 1
Pre-Award 1
Pre-Award 2
Sampling
Summary of Air PES Results
Region IX Lab
% Recovery
92.3%
90.7%
99.0%
98.0%
Contract Lab #1 %
Recovery
63.9*
59.9*
Contract Lab #2 %
Recovery
72.9%
29.4%*
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NA
NA
NA
NA

QATS SPECIAL-REQUEST & SITE-SPECIFIC PESs
REGION IX McCORMICK & BAXTER SITE
Region IX McCormick & Baxter site – multiple
fractions
QATS Lab provides full-volume double-blind aqueous
PES for semi-annual groundwater sampling events.
PES project is similar to the PGAN site.
PESs provided include volatiles, semivolatiles, low-level
SIM PAHs, dioxins/furans, & metals.
60 PESs have been provided over the last 3 years.
5 different labs analyzed samples for recent event.
Approximately 98 percent of the analyte results are
within acceptance limits.
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QATS SPECIAL-REQUEST & SITE-SPECIFIC PESs
ADDITIONAL PROJECTS
Summary of additional special-request PES projects
Region IX
Sulfur Bank Mine Site - Hg in tissue.
Casmalia Site – metals spiked onto site soil.
Riconada Mine Site – Hg in soil.
Eldorado School District – Asbestos air samples.
Guadalupe River Water Shed – methyl mercury in tissue.
ASARCO Site – TCLP metals in soil.
Rico Argentine Site – Aqueous Hg.
George AFB – Classical chemistry parameters and TCE .
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QATS SPECIAL-REQUEST & SITE-SPECIFIC PESs
ADDITIONAL PROJECTS
Summary of additional special-request PES projects
Region VIII
Gilt Edge Mine Site – Aqueous metals and anions.
Gilt Edge Mine Site – High level aqueous cadmium, copper, zinc.
Rocky Flats Industrial Park – Aqueous selenium.
Rico Argentine Site – Aqueous Hg.
Lathrop Canyon Mine Site – Uranium soils.
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QATS SPECIAL-REQUEST & SITE-SPECIFIC PESs
ADDITIONAL PROJECTS
Summary of additional special-request PES projects
Region II
Aroclor 1221 & Aroclor 1242 soil and aqueous PESs for the
Hudson River Project.
– Continual requests from Region II and other Regions resulted
in these becoming standard inventory PESs.
Region I
1,4-Dioxane aqueous PESs for both purge & trap and extractable
methods.
Medium level volatiles in soil PESs for several projects.
– QATS Lab has been purchasing from a commercial vendor.
Long-term needs indicate a need for QATS Lab to design and
develop this PES type.
Region 4
Aqueous and soil toxaphene PESs
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QATS SPECIAL-REQUEST & SITE-SPECIFIC PESs
PES ORDERING
Special-Request PES Ordering Considerations
RPM coordinates with Regional CLP PO or authorized
PES requestor.
Region determines if PES type is available in standard
Superfund PES inventory.
Cost of special-request PES.
Scheduling needs of special-request PES.
Coordination with sampling crews, if required.
Sample containers
Shipping containers (coolers)
Sample preservation needs.
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QATS SPECIAL-REQUEST & SITE-SPECIFIC PESs
PES RESULTS EVALUATION AND REPORTING
Special-Request PES Results Evaluation
Results are typically submitted to QATS Lab for
evaluation.
Analytical results are evaluated using:
Established acceptance limits from PES scoring database – 95%
and 99% confidence intervals.
Acceptance limits calculated using the HBAL database statistics –
95% and 99% confidence intervals based on nominal values.
Method-defined acceptance criteria for QA samples.
Acceptance limits based on nominal value of analytes (i.e., +/percentage
of the nominal value.
Project-defined acceptance limits.
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QATS SPECIAL-REQUEST & SITE-SPECIFIC PESs
PES RESULTS EVALUATION AND REPORTING
Special-Request PES Results Evaluation
Commercial PES analytical results evaluated using:
Acceptance limits provided by the vendor.
Acceptance limits calculated using the HBAL database statistics
based on nominal values provided by the vendor.
Method-defined acceptance criteria for QA samples.
Acceptance limits based on nominal value of analytes (i.e., +/percentage
of the nominal value provided by the vendor.
Project-defined acceptance limits.
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QATS SPECIAL-REQUEST & SITE-SPECIFIC PESs
PES RESULTS EVALUATION AND REPORTING
Special-Request PES Results Evaluation Reporting
PES results evaluations are delivered to the Regional
CLP PO or authorized PES requestor by QATS contact.
Report can include any, or all, of the following:
– Tables summarizing results and acceptance limits and
additional statistics.
– Spreadsheets including results, past results, and charts
illustrating trending of results.
– Narrative evaluation and interpretation of results.
Reports are forwarded to RPMs.
Feedback from Regional CLP PO or RPM to QATS is
welcome.
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QATS SPECIAL-REQUEST & SITE-SPECIFIC PESs
Contacts for PESs Provided by QATS
Regional CLP Project Officer
Regional Authorized PES Requestor
ASB Contact:
John Nebelsick
Email: nebelsick.john@epa.gov
Phone: (703) 603-8845
QATS Contacts:
Keith Strout Clyde Hedin
Email: keith.strout@shawgrp.com Email: clyde.hedin @shawgrp.com
Phone: (702) 895-8722 Phone: (702) 895-8711
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