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The table below identifies information about the reviews conducted of this Standard Operating
Procedure (SOP).
REVIEW HISTORY
Date
Reviewer Name
Changes Required (Y/N~)
The table below identifies changes to this controlled document and the respective effective date(s)
over time.
REVISION HISTORY
Revision
Number
Revision Description
Effective Date
0
Original Issue
Note: Replaces SOP HW-36a, Rev.l SOM02.2 (Pesticide Data
Validation), October 2016
NOTICE
The policies and procedures set forth here are intended as guidance to the United States
Environmental Protection Agency (USEPA) and other governmental employees. They do not constitute
rule-making by the USEPA and may not be relied upon to create a substantive or procedural right
enforceable by any other person. The Government may take action that is at a variance with the
policies and procedures in this Standard Operating Procedure (SOP).
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TABLE OF CONTENTS
1.0 PURPOSE AND APPLICABILITY 4
2.0 SUMMARY OF PROCESS OR METHODOLOGY 4
3.0 DEFINITIONS 4
4.0 RESPONSIBILITIES/QUALIFICATIONS 6
5.0 REFERENCES 7
6.0 PROCEDURAL STEPS 7
7.0 DATA AND RECORDS MANAGEMENT 10
8.0 QUALITY ASSURANCE AND QUALITY CONTROL 10
9.0 APPENDICES 11
Appendix A - Data Validation Criteria and Actions
Appendix B - Data Assessment Report Template
Appendix C - Definitions/Glossary of Terms
Appendix D - SOP Change Request Form
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1.0 PURPOSE AND APPLICABILITY
This document is designed to promote uniformity of data review of analytical data generated
through the US EPA Contract Laboratory Program (CLP) Statement of Work (SOW) for
Superfund Analytical Methods SFAM01.1 and any future editorial revisions of SFAM01.1. It is
applicable to the review of Contract Laboratory Program (CLP) water, soil, sediment, waste,
TCLP, SPLP and closely related matrices using Gas Chromatography/Electron Capture Detection
(ECD) for Pesticide analyses.
The guidelines presented in this document will aid in establishing (a) if data meets the specific
technical and quality control (QC) criteria established in the SOW, and (b) the validity and
extent of bias of any data not meeting the specific technical and QC criteria established in the
SOW. It must be understood by the user that acceptance of data not meeting technical
requirements is based upon many factors, including, but not limited to, site-specific technical
requirements, the need to facilitate the progress of specific projects, and the availability for re-
sampling. The user should note that while this document is to be used as an aid in the formal
data review process, the site-specific quality assurance project plan, as well as professional
judgement, should also be used to determine the ultimate validity of data, especially in those
cases where all data does not meet specific technical criteria. Professional judgment when used
to qualify data including rejection of any data should be explained.
2.0 SUMMARY OF PROCESS OR METHODOLOGY
This document provides the criteria for performing technical quality assurance reviews of
pesticide analytical data generated through the CLP program. Criteria are based on the quality
assurance/quality control and technical requirements specified in Exhibit D of SOW SFAM01.1.
This SOP incorporates much of the content of the National Functional Guidelines (NFG) and
provides additional guidance specific to EPA Region 2.
Upon receipt by EPA Region 2, CLP data in the Sample Delivery Group (SDG) undergoes a
technical quality assurance review based upon the criteria in this document. A report of this
review is prepared by the data validator, reviewed by the EPA Task Order Contracting Officer
Representative (TOCOR), and provided to the data user.
3.0 DEFINITIONS
3.1. See Appendix C - Definitions/Glossary of Terms
3.2. Acronyms and Abbreviations
The following acronyms and abbreviations may be found throughout this document.
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%D
Percent Difference
%R
Percent Recovery
%R\
Percent Relative Intensity
%Resolution
Percent Resolution
%RSD
Percent Relative Standard Deviation
%Solids
Percent Solids, (also %S)
ASB
Analytical Services Branch
CCB
Continuing Calibration Blank
CCS
Contract Compliance Screening
CCV
Continuing Calibration Verification
CF
Calibration Factor
CF
Mean Calibration Factor
CLP
Contract Laboratory Program
CLPSS
Contract Laboratory Program Support System
COC
Chain of Custody
DAR
Data Assessment Report
DF
Dilution Factor
DL
Detection Limit
DQO
Data Quality Objectives
DV
Data Validation
ECD
Electron Capture Detector
EDD
Electronic Data Deliverable
EDM
EXES Data Manager
EDS
Environmental Data Services
EICC
Electronic Internal Chain of Custody
EPA
Environmental Protection Agency (see also USEPA)
ESAT
Environmental Services Assistance Team
EXES
Electronic Data Exchange and Evaluation System
GC/ECD
Gas Chromatograph/Electron Capture Detector
HWSS
Hazardous Waste Support Section
ICAL
Initial Calibration
ICB
Initial Calibration Blank
ICV
Initial Calibration Verification
IUPAC
International Union of Pure and Applied Chemistry
LCS
Laboratory Control Sample
LEB
Leachate Extraction Blank
MDL
Method Detection Limit
MS/MSD
Matrix Spike/Matrix Spike Duplicate
NFG
National Functional Guidelines
OSRTI
Office of Superfund Remediation and Technology Innovation
PDF
Portable Document Format
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OA
Quality Assurance
QAPP
Quality Assurance Project Plan
QC
Quality Control
QL
Quantitation Limit
RPD
Relative Percent Difference
RSCC
Regional Sample Control Center Coordinator
RSD
Relative Standard Deviation
SAP
Sampling and Analysis Plan
SDG
Sample Delivery Group
SEDD
Staged Electronic Data Deliverable
SMO
Sample Management Office
SOP
Standard Operating Procedure
SOW
Statement of Work
SP
SharePoint
SPLP
Synthetic Precipitation Leaching Procedure
TDS
Total Dissolved Solids
TOC
Total Organic Carbon
TSS
Total Suspended Solids
TOCOR
Task Order Contracting Officer Representative
TR/COC
Trip Report/Chain of Custody
TSS
Total Suspended Solids
USEPA
United Stated Environmental Protection Agency
* The above list may contain abbreviations not used in Pesticide analysis.
3.3. Data Qualifier Definitions
Data qualifier definitions are provided in the beginning of Appendix A.
4.0 RESPONSIBILITIES/QUALIFICATIONS
4.1. Qualifications
Data Validator must be familiar with the current CLP SOW and the documents referenced in
Section 5.0 below.
4.2. Responsibilities
4.2.1. EPA TOCOR (when applicable) - will review data assessments reports and other
deliverables prepared by contract data validators. They will update the MS Planner DV
Flowboard indicating the progress of SDGs, post final deliverables to the EDS
SharePoint site and send notification to clients via the established workflow.
4.2.2. Data Validator - will follow the criteria and actions provided in this document and
prepare Data Assessment Reports (DAR) and Summary Reports, as necessary. If the
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validator is an ESAT contractor employee, they will consult the EPA TOCOR when
questions arise. They will update the DV Flowboard indicating progress of SDGs.
5.0 REFERENCES
National Functional Guidelines for Organic Superfund Methods Data Review, EPA 540-R-20-005,
November 2020.
Contract Laboratory Program (CLP) Statement of Work (SOW) Superfund Analytical Method
SFAM01.1.
FA-0010.1, Standard Operating Procedure for Development and Use of Field SOPs, December
2015.
U.S. EPA, 2007. Guidance for the Preparation of Standard Operating Procedures (SOPs) for
Quality-Related Documents. EPA QA/G-6, EPA/600/B-07/001. April 2007.
QA-HWSS-A-001, Document Control Room, Data Dissemination and Archive Operations.
Revision 0, January 2021.
6.0 PROCEDURAL STEPS
6.1. EXES Processing
At the Sample Management Office (SMO) the data package and electronic data deliverables
(EDD) are checked for compliance with the contract. A Contract Compliance Screening
Report (CCS) is issued and posted on the SMO portal website. The EDD is processed
electronically to evaluate QC performance against the NFG and Region 2 criteria by EXES. An
electronic report of the EXES review is also posted on the SMO portal website.
6.2. Initial Notification
The EICC SharePoint web application is setup to send an e-mail alert notification to EPA and
ESAT data validators when a new data package is received and available for review and
validation. Entry of data into the EICC SharePoint site will automatically trigger an e-proxy
card to populate on the DV Flowboard in MS Planner.
Alternate electronic systems may be applied in the future.
6.3. DV Flowboard Updates
Update to DV Flowboard will be performed as per SOP QA-HWSS-A-001, Document Control
Room, Data Dissemination and Archive Operations (or most current version).
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6.4. Data Package Inspection
The EXES Data Manager (EDM) is a useful tool in the data review process. EDM will identify
any missing and/or incorrect information in the data package. When available, the EDM
should be reviewed as part of the initial data package inspection. The CLP laboratory may
submit a reconciliation package for any missing items or to correct the data. If there are any
concerns regarding the data package, contact the TOCOR.
An initial review of the data package is to be performed, taking into consideration all
information specific to the sample data package, (e.g., modified analysis requests, trip
report/chain-of-custody documentation, SDG narratives, etc.). The reviewer should also
have a copy of the Quality Assurance Project Plan (QAPP) or similar document for the
project for which the samples were analyzed. The criteria for data validation outlined in the
QAPP will supersede that in this SOP. The reviewer should access the HWSS SP Documents
Dashboard to obtain a copy of the relevant documents.
The SDGs or cases routinely have unique samples that require special attention from the
reviewer. These include field blanks, equipment blanks, trip blanks, and field duplicates
which must be identified in the sample records. The sampling records (i.e., trip reports or
COC records) should identify:
1) The Region where the samples were taken,
2) The case number,
3) The complete list of samples with the following information as applicable:
a. Sample matrix,
b. Field blanks (i.e., equipment, rinsate and trip),
c. Field duplicates,
d. Field spikes,
e. Shipping dates,
f. Preservatives, and
g. Laboratories involved
6.5. Data Review/Validation
The EXES electronic validation will apply most of the criteria and actions provided in
Appendix A. The data validator will examine the EXES report to identify any issues that
warrant further investigation. All EXES rejected data will be manually evaluated. The data
validator will use the criteria and actions in Appendix A, as well as their own professional
judgement to manually assess these data.
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To use this SOP effectively, the reviewer should understand the analytical method. The
exact number of samples, their assigned numbers, their matrix, and the number of
laboratories involved in the analysis are essential information for the validator.
The Trip Report/Chain of Custody (TR/COC) documentation includes samples descriptions
and date(s) of sampling. The reviewer must consider lag times between sampling and start
of analysis when assessing technical sample holding times.
The laboratory's SDG narrative is another source of general information. Notable problems
with matrices, insufficient sample volume for analysis or reanalysis, samples received in
broken containers, preservation and unusual events should be documented in the SDG
narrative. The reviewer should also inspect any email, telephone or any communication logs
detailing any discussion of sample or analysis issues between the laboratory, the CLP
Sample Management Office and USEPA Region 2.
All data are initially marked as "Reportable" (YES) in EDM before validation is begun.
Sometimes, due to dilutions and/or re-analyses being performed, there will be multiple
results for a single analyte from a sample. The following criteria and professional judgement
are used to determine which result should be reported:
1) the analysis with the lower QL,
2) the analysis with the better QC results, and/or
3) the analysis with the higher result
Data validator will reconcile results from the multiple runs to provide results in one run and
report. The analyte values and their respective QLs are then transferred into a single sample
run. The runs and results that are not to be used are marked "not reportable" or entered
"NO" in the "Reportable" fields of the EDM.
6.6. Data Assessment Report
The data validator will prepare a Data Assessment Report (DAR) documenting the results of
their data review. This report will be formatted in accordance with the template provided in
Appendix B. Modifications to the template are allowed at the discretion of the user.
6.7. Summary Report
If requested by the client on the Analytical Request Form (ARF), the data validator will
prepare a Summary Report using the HWSS Summary Report application.
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7.0 DATA AND RECORDS MANAGEMENT
7.1. DATA MANAGEMENT
Posting data to the SP EDS site is done in accordance with QA-HWSS-A-001, "Document
Control Room, Data Dissemination and Archive Operations".
7.2. RECORDS MANAGEMENT
The data files uploaded to the EDS SharePoint site include:
1) Data Assessment Report (Adobe PDF),
2) Edited/Validated Sample Summary Report from SMO portal (Adobe PDF),
3) Edited/Validated EQulS EDD report from SMO portal (MS Excel),
4) Generated Summary Report (MS Excel), if applicable, and
5) Generated Summary Report with Hits Only (MS Excel), if applicable.
In addition to the above stated documents, data validator also forwards the following files,
which are not uploaded to EDS SharePoint:
6) The CCS Report from the SMO Portal (Adobe PDF),
7) Edit History Report from the SMO Portal (Adobe PDF)
All files stated above are saved to the Local Area Network (LAN) G: drive at
DESADIV/HWSS/DATA VALIDATION/Site Name/Case #/SDG #. Files are renamed using the
following naming convention, Case#_SDG#_Filetype.*, e.g., 12345_BAB12_S3VEM.xlsx.
Note: "M" in the file type signifies that the data has been manually validated by ESAT
and/or EPA Staff.
Additional records management procedures are discussed in QA-HWSS-A-001, "Document
Control Room, Data Dissemination and Archive Operations".
8.0 QUALITY ASSURANCE AND QUALITY CONTROL
8.1. This SOP will be reviewed annually. Reviews will be documented on the Review History
Table on page 2 of the SOP. The SOP shall be updated every 5 years, or more frequently,
when necessary, due to significant changes.
8.2. The "Request for SOP Change Form", Appendix D is used to document changes and is
appended to the final SOP until such time as the changes are incorporated into the body of
the text of the SOP.
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APPENDICES
Appendix A - Data Validation Criteria and Actions
Appendix B - Data Assessment Report Template
Appendix C - Definitions/Glossary of Terms
Appendix D - SOP Change Request Form (CRF)
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Appendix A
Data Validation Criteria and Actions
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TABLE OF CONTENTS
I. DATA VALIDATION QUALIFIER 15
Pesticide Table 1. Data Validation Qualifier Definitions 15
II. PRESERVATION AND HOLDING TIMES 16
Pesticide Table 2. Preservation and Holding Time Actions 16
III. GAS CHROMATOGRAPH/ELECTRON CAPTURE DETECTOR INSTRUMENT PERFORMANCE CHECK
19
Pesticide Table 3. GC/ECD Instrument Performance Check Actions 19
IV. INITIAL CALIBRATION 20
Pesticide Table 4. Initial Calibration Actions 22
V. CONTINUING CALIBRATION VERIFICATION 22
Pesticide Table 5. CCV Actions 24
VI. BLANKS 25
Pesticide Table 6. Blank Actions 26
VII. SURROGATE 27
Pesticide Table 7. Surrogate Actions 28
VIII. MATRIX SPIKE / MATRIX SPIKE DUPLICATE 28
Pesticide Table 8. MS/MSD Actions 29
IX. LABORATORY CONTROL STANDARD 29
Pesticide Table 9. LCS Actions 30
X. FLORISIL CARTRIDGE PERFORMANCE CHECK 30
Pesticide Table 10. Florisil Cartridge Performance Check Actions 31
XI. GEL PERMEATION CHROMATOGRAPHY PERFORMANCE CHECK 31
Pesticide Table 11. Gel Permeation Chromatography Performance Check Actions 32
XII. TARGET ANALYTE IDENTIFICATION 33
Pesticide Table 12. Target Analyte Identification Actions 33
XIII. GAS CHROMATOGRAPH/MASS SPECTROMETER CONFIRMATION 34
Pesticide Table 13. GC/MS Confirmation Actions 35
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XIV. TARGET ANALYTE QUANTITATION 35
Pesticide Table 14. Target Analyte Quantitation - Percent Solids of Sediment Actions 35
XV. FIELD DUPLICATES 36
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I. Data Validation Qualifier
The following are the definitions for the qualifiers assigned to results in the data review process.
The reviewer should use these qualifiers as applicable.
Pesticide Table 1. Data Validation Qualifier Definitions
Data
Qualifier
Definition
U
The analyte was analyzed for but was not detected above the level of the adjusted
detection limit or quantitation limit, as appropriate.
J
The result is an estimated quantity. The associated numerical value is the
approximate concentration of the analyte in the sample.
J+
The result is an estimated quantity, but the result may be biased high.
J-
The result is an estimated quantity, but the result may be biased low.
NJ
The analysis indicates the presence of an analyte that has been "tentatively
identified" and the associated numerical value represents its approximate
concentration.
UJ
The analyte was analyzed for but was not detected. The reported quantitation limit
is approximate and may be inaccurate or imprecise.
R
The data are unusable. The sample results are rejected due to serious deficiencies in
meeting QC criteria. The analyte may or may not be present in the sample.
C
The target analyte identification has been confirmed by Gas Chromatography/Mass
Spectrometry (GC/MS).
X
The target analyte identification was not confirmed when GC/MS analysis was
performed.
NOTES:
1. Comments for sample results with data qualifiers other than "U" or no qualification based
on professional judgement must be included in the DAR.
2. With familiarity of project data objectives and/or consultation with project staff, the
reviewer should be able to refine the use of data qualifiers to avoid ambiguity. For example,
if critical site decisions are to be made based on the data, the reviewer may decide to apply
an "R" qualifier rather than a "UJ".
3. Although a "J+" or a "J-" may appear as less ambiguous than a "J", the reviewer should
reserve the application of directional bias indicators to those situations when there is an
overwhelming influence in one direction. The exercise of professional judgment is critical,
especially in situations where ambiguity exists due to opposing factors, to objectively
interpret the effects of all factors.
4. Criteria, evaluation, quantitation limits (QLs), calculations, acceptable ranges and related
parameters and definitions are detailed in the applicable Statement of Work (SOW) and/or
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National Functional Guidelines (NFG) documents referenced above and should be used as
necessary for data validation. Such criteria when available in the project specific quality
assurance plan (QAPP) document supersede SOW and/or NFG criteria. Such occurrences
should be discussed with TOCORs.
II. Preservation and Holding Times
A. Review Items
Laboratory Results Reports, sampling documentation [e.g., Chain of Custody (COC) Records],
sample receipt forms, preparation logs, analysis logs, raw data, and the data package narrative
checking for: pH, shipping container temperature, holding time, and other sample conditions.
B. Objective
The objective is to determine the validity of the analytical results based on the sample shipping
and storage conditions and the holding time of the sample.
C. Action
Refer to Pesticide Table 2 below for the evaluation criteria and corresponding actions for
detected and non-detected analyte results in the deficient samples. Apply the actions to the
field samples, matrix spike/matrix spike duplicate (if requested) and field blanks or as specified
in the project- specific data validation Standard Operation Procedures (SOPs).
1. If samples are delivered to the laboratory the same day they are collected, sample
temperatures may not have equilibrated to the specified temperature and should be
considered to have been received in acceptable condition.
2. If a discrepancy is noted between the sample analysis date on the Laboratory Results
Reports and in the raw data, perform a more comprehensive review to determine the
correct date to be used to establish the holding time.
Pesticide Table 2. Preservation and Holding Time Actions
Matrix
Preservation
Criteria
Action
Detect
Non-detect
Aqueous/Non-
aqueous
Samples received at
temperature > 6°C
Outside maximum
allowed temperature
J
UJ
Aqueous/Non-
aqueous
Cooled at
temperature < 6°C
TCLP/SPLPleachate
samples prepared
within the 14-day
technical holding time
No
qualification
No
qualification
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Not cooled at
temperature < 6°C
TCLP/SPLPleachate
samples prepared
within the 14-day
technical holding time
J
UJ
Aqueous/Non-
aqueous
Cooled/Not cooled
at temperature
< 6°C
TCLP/SPLPleachate
samples prepared
outside the 14-day
technical holding time
J
R
Aqueous
Cooled at
temperature < 6°C
Samples and
TCLP/SPLP leachates
extracted within the 7-
day and analyzed
within the 40-day
technical holding time
No
qualification
No
qualification
Samples and
TCLP/SPLP leachates
extracted outside the
7-day and analyzed
outside or within the
40-day technical
holding time
J
UJ*
Samples and
TCLP/SPLP leachates
extracted within or
outside the 7-day and
analyzed outside the
40-day technical
holding time
J
UJ*
Aqueous
Not cooled at
temperature < 6°C
Samples and
TCLP/SPLP leachates
extracted within the 7-
day and analyzed
within the 40-day
technical holding time
J
UJ
Samples and
TCLP/SPLP leachates
extracted outside the
7-day and analyzed
outside or within the
40-day technical
holding time
J
UJ*
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Aqueous
Not cooled at
temperature < 6°C
Samples and
TCLP/SPLP leachates
extracted within or
outside the 7-day and
analyzed outside the
40-day technical
holding time
J
UJ*
Non-aqueous
Cooled at
temperature < 6°C
Samples extracted
within the 14-day and
analyzed within the 40-
day technical holding
time
No
qualification
No
qualification
Samples extracted
outside the 14-day and
analyzed outside or
within the 40-day
technical holding time
J-
UJ*
Samples extracted
outside or within the
14-day and analyzed
outside the 40-day
technical holding time
J-
UJ*
Non-aqueous
Not cooled at
temperature < 6°C
Samples extracted
within the 14-day and
analyzed within the 40-
day technical holding
time
J
UJ
Samples extracted
outside the 14-day and
analyzed outside or
within the 40-day
technical holding time
J
UJ*
Samples extracted
outside or within the
14-day and analyzed
outside the 40-day
technical holding time
J
UJ*
* If there is gross exceedance and considering all other QC factors, use professional judgment to
qualify non-detects as unusable (R). If exceedance is minor, qualify non-detects as estimated (UJ).
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III. Gas Chromatoeraph/Electron Capture Detector Instrument Performance Check
A. Review Items
Laboratory instrument performance check reports (if available), chromatograms, and data
system printouts in the data package.
B. Objective
The objective of performing Gas Chromatograph/Electron Capture Detector (GC/ECD)
instrument performance checks is to ensure adequate resolution and instrument sensitivity.
C. Action
Refer to Pesticide Table 3 for the evaluation criteria and corresponding actions for detected and
non-detected analyte results. Apply the actions to the samples and blanks associated to the
deficient RESC, ICAL PEM and/or mid-point ICAL standards in the same analytical sequence.
Apply the actions to the samples and blanks associated to the deficient CCV PEM and mid-
point pesticide calibration standards.
Pesticide Table 3. GC/ECD Instrument Performance Check Actions
Criteria
Action
Detects
Non-detects
RESC not performed at specified frequency and sequence
Use
professional
judgment
Use
professional
judgment
RESC
% Resolution < 60%
(INDA/INDB)
RESC
%Resolution < 80.0% (INDC,
primary column)
%Resolution < 50.0% (INDC,
secondary column)
NJ
R
PEM not performed at the specified frequency and sequence
R
R
PEM %Resolution < 90%
NJ
R
PEM: 4,4'-DDT%Breakdown > 20% and
4,4'-DDT is detected
J for 4,4'-DDT,
4,4'-DDD, and
4,4'-DDE
No
qualification
PEM: 4,4'-DDT%Breakdown > 20% and
4,4'-DDT is not detected
NJ for 4,4'-
DDD and 4,4'-
DDE
R for 4,4'-
DDT
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PEM: Endrin %Breakdown > 20% and Endrin is detected
J for Endrin,
Endrin
aldehyde, and
Endrin ketone
No
qualification
PEM: Endrin %Breakdown > 20% and Endrin is not detected
NJ for Endrin
aldehyde and
Endrin ketone
R for Endrin
PEM: Combined %Breakdown > 30%
Apply
qualifiers as
described
above
considering
degree of
individual
breakdown
Apply
qualifiers as
described
above
considering
degree of
individual
breakdown
Midpoint ICAL standard not performed at specified frequency
R
R
% Resolution < 90%
(Midpoint INDA/INDB)
%Resolution < 80.0%
(Midpoint INDC, primary
column)
%Resolution < 50.0%
(Midpoint INDC, secondary
column)
NJ
R
IV. Initial Calibration
A. Review Items
Laboratory initial calibration reports (if available), initial calibration standard quantitation
reports and chromatograms in the data package.
B. Objective
The objective of initial calibration (ICAL) is to ensure that the instrument is capable of producing
acceptable qualitative and quantitative data.
C. Action
Refer to Pesticide Table 4 for the evaluation criteria and corresponding actions for detected and
non-detected analyte results in the samples associated to a deficient ICAL. Apply the actions to
the samples and blanks in the same analytical sequence as the deficient ICAL.
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1. If the ICAL is not performed at the specified frequency or sequence, use professional
judgment to qualify detects and non-detects. Notify the designated project management
personnel, who may arrange for the laboratory to repeat the analyses as specified. If a
reanalysis cannot be performed, qualify detects and non-detects as unusable (R).
2. If the ICAL is not performed at the specified concentrations, qualify detects as estimated
(J) and non-detects as estimated (UJ). This is especially critical for the low-level standards
and non-detects.
3. If errors are detected in the calculations of RT windows, CFs, mean CFs, or %RSDs, perform a
more comprehensive recalculation. If the chromatogram display criteria are not met, use
professional judgment to qualify detects and non-detects. Notify the designated project
management personnelto arrange for a revised report.
4. If the %RSD for any target analyte is outside the acceptance limits, qualify detects as
estimated (J). No qualification for non-detects.
5. Based on the project-specific Data Quality Objectives (DQO), a more in-depth review may
be necessary when %RSD criteria are not met. The following guidelines are recommended:
a. If the %RSD criteria of any target analytes are not met, and the %RSD criteria are still not
satisfied after eliminating either the high- or the low-point of the ICAL:
i. Qualify detects in the associated samples as estimated (J).
ii. Use professional judgment to qualify non-detects in the associated samples as
estimated (UJ).
b. If the high-point of the ICAL curve causes the ICAL %RSD to exceed the criterion (e.g.,
due to saturation):
i. Qualify detects in the associated samples with analyte concentrations in the upper
ICAL range as estimated (J).
ii. Non-detects in the associated samples should not be qualified.
c. If the low-point of the ICAL curve causes the ICAL %RSD to exceed the criterion:
i. Qualify detects in the associated samples with analyte concentrations in the non-
linear range as estimated (J).
ii. For non-detects in the associated samples, use the lowest point of the linear portion
of the ICAL curve to determine the new quantitation limit, or qualify non-detects as
estimated (UJ).
6. Qualification of the target analyte data is not necessary based on the surrogate %RSD data
alone. Use professional judgment to evaluate the surrogate %RSD data in conjunction with
the surrogate recoveries to determine the need for data qualification.
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Pesticide Table 4. Initial Calibration Actions
Criteria
Action
Detects
Non-detects
Initial Calibration not performed at specified frequency and
sequence
R
R
Initial Calibration not performed at specified concentrations
J
UJ
RT windows incorrect or Chromatogram criteria not met
J
R
%RSD for target analyte outside specified acceptance limits*
J
No
qualification
%RSD for target analyte within specified acceptance limits*
No
qualification
No
qualification
* %RSD < 20.0% for single component target analytes except alpha-BHC and delta-BHC.
% RSD < 25.0% for alpha-BHC and delta-BHC.
% RSD < 30.0% for Toxaphene peaks.
% RSD < 20.0% for surrogates (TCX and DCB).
V. Continuing Calibration Verification
A. Review Items
Laboratory continuing calibration verification reports (if available), quantitation reports and
chromatograms in the data package.
B. Objective
The objective is to ensure that the instrument continues to meet the sensitivity and linearity
criteria to produce acceptable qualitative and quantitative data throughout each analytical
sequence.
C. Action
Refer to Pesticide Table 5 for the evaluation criteria and corresponding actions for detected and
non- detected analyte results in samples associated with a deficient CCV. Apply the actions to
the samples and blanks in the same analytical sequence as the deficient CCV PEMs or CCVs.
1. If the CCV PEM or CCV standard is not performed at the specified frequency and sequence,
notify the designated project management personnel, who may arrange for the laboratory
to repeat the analyses as specified, if holding times have not expired and there is extract
remaining. If a reanalysis cannot be performed, carefully evaluate all other available
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information, including the quality of analyte peak shapes and RT match of surrogates on
both columns, and compare to the most recent calibration performed on the same
instrument under the same conditions. Using this information and professional judgment,
the reviewer may be able to justify unqualified acceptance of qualitative results and
qualification of all quantitative results as estimated (J). Otherwise, qualify all detects and
non-detects as unusable (R).
If the CCV PEM is not performed at the specified concentration, qualify detects as estimated
(J) and non-detects as estimated (UJ).
If the CCV standard is not performed at the specified concentration, qualify detects as
estimated (J) and non-detects as estimated (UJ). Special consideration should be given to
sample results at the opposite extreme of the calibration range if CCV concentration is not
at the mid-point calibration range. Evaluate the ICAL performance in the concentration
range of the detected analyte results.
If the RT of any target analyte in the CCV PEM and CCV standard is outside the RT window,
carefully evaluate the associated sample results. All samples injected after the last in-
control standard are potentially affected.
a. For detected target analytes in the affected samples, check the sample chromatograms
that may contain any peaks that are close to the expected RT window of the target
analytes of interest. If the peaks are close to the expected RT window of the Pesticide of
interest, it may require additional effort to determine if sample peaks represent the
target analytes of interest. For example, the data reviewer may examine the presence of
three or more standards containing the target analytes of interest that were analyzed
within the analytical sequence during which the sample was analyzed. If three or more
such standards are present, the RT windows can be re-evaluated using the mean RTs of
the standards.
If the peaks in the affected sample fall within the revised windows, qualify detects as
estimated (J).
b. For non-detected target analytes in the affected samples, check the sample
chromatograms that may contain any peaks that are close to the expected RT window of
the target analytes of interest.
i. If no peaks used for Pesticide analyte identification are present, non-detects should
not be qualified.
ii. If any peaks present are close to the expected RT window of the analytes of interest,
use professional judgement to qualify the non-detects as estimated (UJ).
If errors are detected in the calculations of either the %D or %Breakdown in the CCV PEM,
%D in any CCV standard or %D for any Toxaphene peak in the applicable CCV standard,
perform a more comprehensive recalculation.
If the time elapsed between the injection of an instrument blank as opening CCV and the
injection of either a PEM or a CCV standard as closing CCV exceeds 14 hours, carefully
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evaluate instrument stability during the entire sequence to decide whether degradation has
occurred, including column bleed, RTs, peak shapes, and surrogate recovery. If system
degradation has been found, qualify positive results as estimated (J). If any possibility exists
for either false positives or false negatives, qualify non-detects as unusable (R).
7. If the time elapsed between the injection of an instrument blank as opening CCV and the
injection of the last sample or blank in the same analytical sequence exceeds 12 hours,
carefully evaluate instrument stability during the entire sequence to decide whether
degradation has occurred, including column bleed, RTs, peak shapes, and surrogate
recovery. If system degradation has been found, qualify positive results as estimated (J). If
any possibility exists for either false positives or false negatives, qualify non-detects as
unusable (R).
8. Qualification of the target analyte data is not necessary based on the surrogate %D in CCV
PEM and CCV standards alone. Use professional judgment to evaluate the surrogate %D
data in conjunction with the surrogate recoveries to determine the need for data
qualification.
9. If more than 72 hours have elapsed from the injection of the sample with a Toxaphene
detection and the Toxaphene calibration verification standard, qualify detects and non-
detects as unusable (R).
Pesticide Table 5. CCV Actions
Criteria
Action
Detects
Non-detects
CCV PEM or not performed at specified frequency and
sequence
J
UJ
CCV PEM not performed at specified concentrations
J
UJ
CCV standard not performed at specified concentrations
J
UJ
RT outside specified RT window
J
UJ
CCV PEM %D for target analyte outside specified limit*
J
UJ
CCV standard %D for target analyte outside specified limit*
J
UJ
RT, CCV PEM %D, CCV %D, and time elapsed within specified
limits
No
qualification
No
qualification
Time elapsed between opening CCV instrument blank and
closing CCV exceeds 14 hours
J
R
Time elapsed between opening CCV instrument blank and last
sample, or blank exceeds 12 hours
J
R
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Time elapsed from the injection of the sample with a
Toxaphene detection and the Toxaphene calibration
verification standard exceeds 72 hours
* %RSD < 25.0% for single component target analytes and surrogates (TCX and DCB).
%RSD < 25.0% for Toxaphene peaks.
VI. Blanks
A. Review Items
Laboratory Results Reports, chromatograms, and quantitation reports in the data package and
sampling trip reports.
B. Objective
The objective of a blank analysis results assessment is to determine the existence and
magnitude of contamination resulting from laboratory (or field) activities.
C. Action
Refer to Pesticide Table 6 for the evaluation criteria and corresponding actions for detected and
non-detected analyte results in the samples associated with deficient blanks. Apply the actions
to all samples associated with the method blank by the same preparation batch; all samples
associated with the TCLP/SPLP LEB by the same leachate extraction batch; all samples
associated with the ICAL instrument blank in the analytical sequence; all samples associated
with the opening or closing CCV instrument blank in the same analytical sequence; and all
samples associated with the sulfur blank by the same cleanup batch.
1. Action regarding unsuitable blank results depends on the circumstances and origin of the
blank. Verify that data qualification decisions based on field quality control (QC) are
supported by the project QAPP or the project-specific Standard Operating Procedures
(SOPs). At a minimum, contamination found in field blanks should be documented in the
Data Review Narrative. In instances where more than one blank is associated with a given
sample, qualification should be based upon a comparison with the associated blank that
has the highest concentration of a contaminant. Do not correct the results by subtracting
any blank value.
2. For any method blank reported with results that are < QLs, no qualification is required for
sample results that are > QLs.
3. For any method blank reported with results > QLs, report sample results that are > QLs but
< Blank Results at sample results and qualify as non-detect (U). No qualification is required
for sample results that are > QLs and > Blank Results.
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4. For TCLP/SPLP LEBs, sulfur cleanup blanks, instrument blanks, and field blanks (including
equipment and rinse blanks), sample result qualifications listed in Pesticide Table 5 should
apply if supported by the QAPP.
5. There may be instances where little or no contamination is present in the associated blanks,
but qualification of the sample is deemed necessary. If it is determined that the
contamination is from a source other than the sample, the data should be qualified, or in
the case of field QC, should at least be documented in the Data Review Narrative.
Contamination introduced through dilution water is one example. Although it is not always
possible to determine, instances of this occurring can be detected when contaminants are
found in the diluted sample result but are absent in the undiluted sample.
6. If an analyte result in a diluted sample analysis is < QL, the final analyte result should be
checked against a less dilute analysis and reported from that analysis. However, if no less-
dilute analysis is reported, use professional judgment to decide whether to report from the
dilution.
7. If gross contamination exists with blank results that are > ICAL high-point standard
concentrations, qualify detects as unusable (R).
Pesticide Table 6. Blank Actions
Blank Type
Blank Result
Sample Result
Action for Samples
Not analyzed at
the specified
frequency
Non-detect
No qualification
Detect
J
Method,
TCLP/SPLP
LEB, Sulfur
cleanup,
Instrument,
Field
(including
Equipment
and Rinse)
Blank
Detect
Non-detect
No qualification
Detect < QL
MDL < Detect < QL
Report at QL and qualify U
>QL
No qualification
>QL
Detect < QL
Report at QL and qualify U
> QL but < Blank Result
Report at sample result and
qualify U
> QL and > Blank Result
No qualification
Gross
contamination
Detect
Report at sample result and
qualify R
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VII. Surrogate
A. Review Items
Laboratory surrogate reports (if available), quantitation reports and chromatograms in the data
package.
B. Objective
The objective is to evaluate surrogate percent recovery (%R) to ensure that the analytical
method is efficient
C. Action
Refer to Pesticide Table 7 below for the evaluation criteria and corresponding actions for
detected and non-detected analyte results associated with the deficient surrogates in samples.
Qualification of the target analyte data is not necessary based on the surrogate %RSD data
alone. Use professional judgment to evaluate the surrogate %RSD data in conjunction with the
surrogate recoveries to determine the need for data qualification.
1. If surrogate standards were not added to the samples and blanks or the concentrations of
surrogates in the samples and blanks are not as specified, use professional judgment to
qualify detects and non-detects. Examine the data package narrative and standards and
sample preparation logs included in the data package or notify the designated project
management personnel who may arrange for the laboratory to repeat the analyses as
specified and/or to provide any missing information. If a reanalysis cannot be performed,
qualify the data as unusable (R).
2. If any surrogate %R in a blank is outside the limits specified in the QAPP or in the SOW,
special consideration should be taken to determine the validity of the associated sample
data. The basic concern is whether the blank problems represent an isolated problem with
the blank alone, or whether there is a fundamental problem with the analytical process.
3. If one or more samples in the same extraction batch have surrogate %R within the
acceptance limits, use professional judgment to determine if the blank problem is an
isolated occurrence. However, even if this judgment allows some use of the affected data,
note analytical problems for project management personnel action
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Pesticide Table 7. Surrogate Actions
Criteria
Action*
Detects
Non-detects
Surrogate not present or not at specified concentration
J
UJ
RT out of specified RT window
Use
professional
judgment**
Use
professional
judgment**
RT within specified RT window
No
qualification
No
qualification
%R < 10% (sample dilution not a factor)
J-
R
%R < 10% (sample dilution is a factor)
No
qualification
No
qualification
10% < %R < 30%
J-
UJ
%R within specified Acceptance Limits (30% -150%)
No
qualification
No
qualification
%R > 150%
J+
No
qualification
* Diluted samples with dilution less than or equal to (<) 5 should be qualified for surrogates
recovery outside criteria. Diluted samples with dilution factor greater than (>) 5, no
qualification is applied.
** Use professional judgment in qualifying data, as surrogate recovery problems may not directly
apply to target analytes.
VIII. Matrix Spike / Matrix Spike Duplicate
A. Review Items
Laboratory Results Reports, quantitation reports and chromatograms in the data package.
B. Objective
The objective of Matrix Spike (MS)/Matrix Spike Duplicate (MSD) analysis is to evaluate the
effect of each sample matrix on the sample preparation procedures and the measurement
methodology.
C. Action
Refer to Pesticide Table 8 for the evaluation criteria and corresponding actions for detected and
non-detected target analytes in the original samples associated with deficient MS/MSDs.
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Apply the actions to the same analytes in the parent samples used for the MS/MSD
analyses or as specified in the project-specific Standard Operating Procedures (SOPs).
Pesticide Table 8. MS/MSD Actions
Criteria
Action
Detects
Non-detects
MS/MSD not analyzed at specified frequency
Use
professional
judgment
Use
professional
judgment
MS/MSD not prepared from field sample
Use
professional
judgment*
Use
professional
judgment*
%R or RPD limits not specified
Use
professional
judgment
Use
professional
judgment
%R < Expanded Lower Acceptance Limit (20%)
J
R
Expanded Lower Acceptance Limit (20%) < %R < specified
Lower Acceptance Limit
J
UJ
%R or RPD within specified Acceptance Limits
No
qualification
No
qualification
%R or RPD > specified Upper Acceptance Limit
J
No
qualification
* Notify CLP PO if a field blank was used for the MS/MSD.
IX. Laboratory Control Standard
A. Review Items
Laboratory Results Reports, chromatograms, and data system printouts in the data package.
B. Objective
The objective is to evaluate accuracy of the analytical method and laboratory performance.
C. Action
Refer to Pesticide Table 9 for the evaluation criteria and corresponding actions for detected
and non-detected analyte results in the samples associated with the deficient LCSs. Apply
the actions to all associated samples prepared together (in the same preparation batch) or
as specified in the project-specific Standard Operating Procedures (SOPs).
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Pesticide Table 9. LCS Actions
Criteria
Action
Detects
Non-detects
LCS not performed at specified frequency or concentration
Use
professional
judgment
Use
professional
judgment
LCS %R limits not specified
Use
professional
judgment
Use
professional
judgment
%R < specified Lower Acceptance Limit
J-
R
%R within specified Acceptance Limits
No
qualification
No
qualification
%R > specified Upper Acceptance Limit
J+
No
qualification
X. Florisil Cartridge Performance Check
A. Review Items
Laboratory Results Reports, chromatograms, and data system printouts in the data package.
B. Objective
The objective is to evaluate the performance of the Florisil cartridge used for the Florisil
cleanup procedure on sample extracts.
C. Action
Refer to Pesticide Table 10 for the evaluation criteria and corresponding actions for detected
and non-detected analyte results in the samples associated with deficient Florisil Cartridge
Performance Checks. Apply the actions to all associated samples, blanks and LCSs that have
undergone Florisil cleanup (in the same cleanup batch) in the analytical sequence or as
specified in the project-specific Standard Operating Procedures (SOPs).
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Pesticide Table 10. Florisil Cartridge Performance Check Actions
Criteria
Action
Detects
Non-detects
Florisil Cartridge Performance Check not performed at
specified frequency or concentration
Use
professional
judgment
Use
professional
judgment
%R < Expanded Lower Acceptance Limit for target analytes
(10%)
J
R
Expanded Lower Acceptance Limit for target analytes (10%)
< %R < Lower Acceptance Limit for target analytes (80%)
J
UJ
Lower Acceptance Limit for target analytes (80%) < %R
< Upper Acceptance Limit for target analytes (120%)
No
qualification
No
qualification
%R > Upper Acceptance Limit for target analytes (120%)
J
No
qualification
%R > 5% (2,4,5-trichlorophenol)
Use
professional
judgment
Use
professional
judgment
XI. Gel Permeation Chromatography Performance Check
A. Review Items
Laboratory Gel Permeation Chromatography (GPC) calibration verification reports (if available),
two ultraviolet (UV) traces, GPC cleanup blank quantitation reports and chromatograms in the
data package.
B. Objective
The objective is to evaluate GPC cleanup efficiency.
C. Action
Refer to Pesticide Table 11 for the evaluation criteria and the corresponding actions for
detected and non-detected analyte results in the samples associated with a deficient GPC
Performance Checks. Apply the actions to all associated samples, blanks and LCSs that have
undergone GPC cleanup (in the same cleanup batch) in the analytical sequence or as
specified in the project-specific Standard Operating Procedures (SOPs).
1. If GPC calibration frequency, UV traces, and GPC blank criteria are not met, examine the
raw data for the presence of high molecular weight contaminants, examine subsequent
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sample data for unusual peaks, and use professional judgment to qualify the data. If the
samples have been analyzed under unacceptable GPC criteria, notify the designated project
management personnel.
If the RT shift of bis(2-ethylhexyl) phthalate and perylene is greater than (>) 5%, the GPC
unit may be in an unstable temperature environment and subject to erratic performance.
The expected result may be an unknown bias in the data. Notify the designated project
management personnel, who may arrange for the laboratory to repeat the analyses as
specified.
2. If GPC calibration verification is not performed at the specified concentrations, use
professional judgment to qualify detects and non-detects.
3. If errors are detected in the calculations of the %R in the GPC calibration verification,
perform a more comprehensive recalculation.
Pesticide Table 11. Gel Permeation Chromatography Performance Check Actions
Criteria
Action
Detects
Non-detects
GPC calibration not analyzed at specified frequency or
concentration
J
UJ
Analyte resolution in the most recent UV traces and/or RT
shift that does not meet specified criteria
Use
professional
judgment
Use
professional
judgment
GPC blank not analyzed at the specified frequency and
sequence
Use
professional
judgment
Use
professional
judgment
Analyte result in GPC blank > QL
Use
professional
judgment
Use
professional
judgment
GPC calibration verification not analyzed at specified
frequency
J
UJ
%R < Expanded Lower Acceptance Limit for target analytes
(10%)
J
R
Expanded Lower Acceptance Limit for target analytes (10%)
< %R < Lower Acceptance Limit for target analytes (80%)
J
UJ
Lower Acceptance Limit for target analytes (80%) < %R
< Upper Acceptance Limit for target analytes (120%)
No
qualification
No
qualification
%R > Upper Acceptance Limit for target analytes (120%)
J
No
qualification
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XII. Target Analvte Identification
A. Review Items
Laboratory Results Reports, quantitation reports, mass spectra, and chromatograms in the data
package.
B. Objective
The objective is to provide acceptable Gas Chromatography/Electron Capture Detector
(GC/ECD) qualitative analysis to minimize the number of erroneous analyte identifications.
C. Action
Refer to Pesticide Table 12 for the evaluation criteria and corresponding actions for detected
and non-detected analyte results in the deficient samples. Apply the actions to the applicable
samples, blanks and LCSs in the data package or as specified in the project-specific Standard
Operating Procedures (SOPs).
Pesticide Table 12. Target Analyte Identification Actions
Criteria
Action
Detects
Non-detects
Detected target analyte RT outside specified RT window (false
positive)
Report at QL
and qualify U
Not
applicable
Detected target analyte peak exhibits an interference with the
potential detection of another target peak (false positive)
R
Not
applicable
Reported non-detect target analyte RT within specified RT
windows on both GC columns (false negative)
Use
professional
judgment to
report results
Not
applicable
Toxaphene peak RT windows overlap with single component
target analytes or chromatographic interferences exist
Use
professional
judgment
Use
professional
judgment
Toxaphene peaks exhibit a marginal pattern-matching quality
Use
professional
judgment or
Report results
and qualify NJ
No
qualification
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Evident chromatographic interference or co-elution for the
detected target analyte
Use
professional
judgment to
Report results
at lower value
and qualify NJ
or
Report at QL
and qualify U
Not
applicable
%D for any target analyte 0% - 25%
No
qualification
Not
applicable
%D for any target analyte 26% - 200%
J
Not
applicable
%D for any target analyte > 200% (Interference detected)
NJ
Not
applicable
%D for any target analyte > 200% (Interference not
detected*)
NJ
Not
applicable
* Visual examination of the chromatograms should be performed to check for interference and
compliance with SOW Technical Criteria for Identification. Note the finding in the report.
XIII. Gas Chromatoeraph/Mass Spectrometer Confirmation
A. Review Items
Laboratory Results Reports, sample preparation sheets, data package narrative, quantitation
reports, and chromatograms in the data package.
B. Objective
The objective is to ensure the accuracy of the positive identification of a target analyte.
C. Action
Refer to Pesticide Table 13 below for the evaluation criteria and corresponding actions for
detected analyte results in the samples.
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Pesticide Table 13. GC/MS Confirmation Actions
Criteria
Action
Detects
Analyte confirmed by GC/MS
C
Analyte indicated but not confirmed by GC/MS
X
XIV. Target Analvte Quantitation
A. Review Items
Laboratory Results Reports, sample preparation sheets, data package narrative, quantitation
reports, and chromatograms in the data package.
B. Objective
The objective is to ensure that the reported results and quantitation limits (QLs) for target
analytes reported by the laboratory are accurate and are sufficient to meet requirements.
C. Action
Refer to Pesticide Table 14 below for the evaluation criteria and corresponding actions for the
percent solids (% Solids) of the samples.
If analyte results are < QLs and > Method Detection Limits (MDLs) or limits in the QAPP,
qualify as estimated (J).
Pesticide Table 14. Target Analyte Quantitation - Percent Solids of Sediment Actions
Criteria
Action
Detects
Non-detects
% Solids < 10.0%
J
R
10.0% < % Solids < 30.0%
J
UJ
% Solids > 30.0%
No
qualification
No
qualification
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XV. Field Duplicates
A. Review Items
Review Chain of Custody and Trip Report (COC/TR) to identify which samples within the data
package are field duplicates.
B. Objective
Field duplicates may be taken and analyzed as an indication of overall precision. These analyses
measure both field and laboratory precision.
C. Action
In the absence of QAPP guidance for validating data from field duplicates, the following action
will be taken.
1. Identify which samples within the data package are field duplicates.
2. Estimate the relative percent difference (RPD) between the values for each compound.
3. If large RPDs (> 50%) is observed, confirm identification of samples, and note difference in
the executive summary.
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Appendix B
Data Assessment Report Template
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UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
REGION 2
LSASD/HWSB/HWSS
2890 Woodbridge Avenue, Edison, NJ 08837
EXECUTIVE NARRATIVE
Case No.:
Site:
Number of Samples:
Analysis:
QAPP:
Contractor:
Reference: DCN Number
SUMMARY OF DEFINITIONS:
Critical: Results have an unacceptable level of uncertainty and should not be used for making decisions.
Data have been qualified "R" rejected.
Major: A level of uncertainty exists that may not meet the data quality objectives for the project. A bias is likely to
be present in the results. Data has been qualified "J" estimated. "J+" and "J-" represent likely direction of the bias.
Minor: The level of uncertainty is acceptable. No significant bias in the data was observed.
Critical Findings:
Major Findings:
Minor Findings:
SDG No.:
Laboratory:
Sampling dates:
Validation SOP:
COMMENTS:
Reviewer Name(s):
Approver's Signature:
Name: Date:
Affiliation: USEPA/R2/LSASD/HWSB/HWSS
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Appendix C
Definitions/Glossary of Terms
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DEFINITIONS* & GLOSSARY OF TERMS
Analyte - The element of interest, ion, or parameter an analysis seeks to determine.
Analytical Services Branch (ASB) - Directs the Contract Laboratory Program (CLP) from within the
Office of Superfund Remediation and Technical Innovation (OSRTI) in the Office of Solid Waste and
Emergency Response (OSWER).
Analytical Sample - Any solution or media introduced into an instrument on which an analysis is
performed excluding instrument calibration, Initial Calibration Verification (ICV), Initial Calibration
Blank (ICB), Continuing Calibration Verification (CCV), and Continuing Calibration Blank (CCB). Note that
the following are all defined as analytical samples: undiluted and diluted samples (USEPA and non-
USEPA); Matrix Spike samples; duplicate samples; serial dilution samples, analytical (post-
digestion/post-distillation) spike samples; Interference Check Samples (ICSs); Laboratory Control
Samples (LCSs); and Preparation Blanks.
Associated Samples - Any sample related to a particular Quality Control (QC) analysis. For example,
for Initial Calibration Verification (ICV), all samples run under the same calibration curve. For
duplicates, all Sample Delivery Group (SDG) samples digested/distilled of the same matrix.
Blank - A sample designed to assess specific sources of contamination. See individual definitions for
types of blanks.
Calibration ~ The establishment of an analytical curve based on the absorbance, emission intensity, or
other measured characteristic of known standards. The calibration standards are to be prepared using
the same type of reagents or concentration of acids as used in the sample preparation.
Calibration Blank ~ A blank solution containing all of the reagents in the same concentration as those
used in the analytical sample preparation. This blank is not subject to the preparation method.
Calibration Curve ~ A plot of instrument response versus concentration of standards.
Calibration Standards - A series of known standard solutions used by the analyst for calibration of the
instrument (i.e., preparation of the analytical curve). The solutions may or may not be subjected to the
preparation method, but contain the same matrix (i.e., the same amount of reagents and/or
preservatives) as the sample preparations to be analyzed.
Case - A finite, usually predetermined number of samples collected over a given time period from a
particular site. Case numbers are assigned by the Sample Management Office (SMO). A Case consists of
one or more Sample Delivery Groups (SDGs).
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Contract Compliance Screening (CCS) - A screening of electronic and hardcopy data deliverables for
completeness and compliance with the contract. This screening is performed under USEPA direction by
the Contract Laboratory Program (CLP) Sample Management Office (SMO) contractor.
Continuing Calibration Verification (CCV) - A single parameter or multi-parameter standard solution
prepared by the analyst and used to verify the stability of the instrument calibration with time, and the
instrument performance during the analysis of samples. The CCV can be one of the calibration
standards. However, all parameters being measured by the particular system must be represented in
this standard and the standard must have the same matrix (i.e., the same amount of reagents and/or
preservatives) as the samples.
Contract Laboratory Program (CLP) - Supports the USEPA's Superfund effort by providing a range of
state-of-the-art chemical analytical services of known quality. This program is directed by the Analytical
Services Branch (ASB) of the Office of Superfund Remediation and Technical Innovation (OSRTI) of
USEPA.
Contract Laboratory Program Project Officer (CLP PO) - The Regional USEPA official responsible for
monitoring laboratory performance and/or requesting analytical data or services from a CLP
laboratory.
Contract Required Quantitation Limit (CRQL) - Minimum level of quantitation acceptable under the
contract Statement of Work (SOW).
Duplicate - A second aliquot of a sample that is treated the same as the original sample in order to
determine the precision of the method.
Field Blank - Any sample that is submitted from the field and identified as a blank. A field blank is used
to check for cross-contamination during sample collection, sample shipment, and in the laboratory. A
field blank includes trip blanks, rinsate blanks, bottle blanks, equipment blanks, preservative blanks,
decontamination blanks, etc.
Field Duplicate - A duplicate sample generated in the field, not in the laboratory.
Holding Time ~ The maximum amount of time samples may be held before they are processed.
a. Contractual - The maximum amount of time that the Contract Laboratory Program (CLP)
laboratory may hold the samples from the sample receipt date until analysis and still be in
compliance with the terms of the contract, as specified in the CLP Analytical Services Statement
of Work (SOW). These times are the same or less than technical holding times to allow for
sample packaging and shipping.
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b. Technical - The maximum amount of time that samples may be held from the collection date
until analysis.
Initial Calibration - Analysis of analytical standards for a series of different specified concentrations to
define the quantitative response, linearity, and dynamic range of the instrument to target analytes.
Initial Calibration Verification (ICV) - Solution(s) prepared from stock standard solutions, metals, or
salts obtained from a source separate from that utilized to prepare the calibration standards. The ICV is
used to verify the concentration of the calibration standards and the adequacy of the instrument
calibration. The ICV should be traceable to National Institute of Standards and Technology (NIST) or
other certified standard sources when USEPA ICV solutions are not available.
Internal Standard - A non-target element added to a sample at a known concentration after
preparation but prior to analysis. Instrument responses to internal standards are monitored as a means
of assessing overall instrument performance.
Matrix - The predominant material of which the sample to be analyzed is composed. For the purposes
of this document, the matrices are aqueous/water, soil/sediment, wipe, and filter.
Matrix Spike - Introduction of a known concentration of analyte into a sample to provide information
about the effect of the sample matrix on the digestion and measurement methodology (also identified
as a pre-distillation/digestion spike).
Method Detection Limit (MDL) ~ The concentration of a target parameter that, when a sample is
processed through the complete method, produces a signal with 99 percent probability that it is
different from the blank. For 7 replicates of the sample, the mean value must be 3.14s above the blank,
where "s" is the standard deviation of the 7 replicates.
Narrative (SDG Narrative) - Portion of the data package which includes laboratory, contract, Case,
Sample Number identification, and descriptive documentation of any problems encountered in
processing the samples, along with corrective action taken and problem resolution.
Office of Solid Waste and Emergency Response (OSWER) - The USEPA office that provides policy,
guidance, and direction for the USEPA's solid waste and emergency response programs, including
Superfund.
Percent Difference (%D) - As used in this document and the Statement of Work (SOW), is used to
compare two values. The difference between the two values divided by one of the values.
Preparation Blank - An analytical control that contains reagent water and reagents, which is carried
through the entire preparation and analytical procedure.
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Relative Percent Difference (RPD) - As used in this document and the Statement of Work (SOW) to
compare two values, the RPD is based on the mean of the two values, and is reported as an absolute
value (i.e., always expressed as a positive number or zero).
Regional Sample Control Center Coordinator (RSCC) - In USEPA Regions, coordinates sampling efforts
and serves as the central point-of-contact for sampling questions and problems. Also assists in
coordinating the level of Regional sampling activities to correspond with the monthly projected
demand for analytical services.
Relative Standard Deviation (RSD) ~ As used in this document and the Statement of Work (SOW), the
mean divided by the standard deviation, expressed as a percentage.
Sample - A single, discrete portion of material to be analyzed, which is contained in single or multiple
containers and identified by a unique Sample Number.
Sample Delivery Group (SDG) - A unit within a sample Case that is used to identify a group of samples
for delivery. An SDG is defined by the following, whichever is most frequent:
a. Each 20 field samples [excluding Performance Evaluation (PE) samples] within a Case; or
b. Each 7-calendar day period (3-calendar day period for 7-day turnaround) during which field
samples in a Case are received (said period beginning with the receipt of the first sample in the
SDG).
c. Scheduled at the same level of deliverable.
d. In addition, all samples and/or sample fractions assigned to an SDG must be scheduled under
the same contractual turnaround time. Preliminary Results have no impact on defining the SDG.
Samples may be assigned to SDGs by matrix (i.e., all soil/sediment samples in one SDG, all
aqueous/water samples in another) at the discretion of the laboratory.
Sample Management Office (SMO) - A contractor-operated facility operated under the SMO contract,
awarded and administered by the USEPA. Provides necessary management, operations, and
administrative support to the Contract Laboratory Program (CLP).
Statement of Work (SOW) - A document which specifies how laboratories analyze samples under a
particular Contract Laboratory Program (CLP) analytical program.
* The above list is all inclusive and may contain terms not applicable to Pesticide Analysis.
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Appendix D
SOP Change Request Form (CRF)
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REQUEST FOR SOP CHANGE
Requestor
Name:
Date of
Initiation:
Dept.:
SOP#:
Revision #:
Date:
SOP Title:
Please Check One
MINOR REVISION
MAJOR REVISION
CHANGE(S) (Use attachment if necessary):
CHANGE FROM:
CHANGE TO:
REASON(S) FOR CHANGE(S):
APPROVAL
NAME:
Signature/Date
EPA Branch Chief /
Section Chief/Team
Leader
EPA TOCOR
REQUESTOR
Effective Date
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