NATIONALFUNCTIONALGUIDELINES
for Superfund Organic Methods Data Review
v>EPA
Office of Superfund Remediation and Technology Innovation (OSRTI)
United States Environmental Protection Agency (EPA)
Washington, DC 20460
OSWER 9200-2.134
EPA-540-R-014-002
OCTOBER 2013
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NOTICE
The policies and procedures set forth here are intended as guidance to the United States Environmental
Protection Agency (EPA) and other governmental employees. They do not constitute rule-making by the
EPA, and may not be relied on 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 manual.
This document can be obtained from the EPA's Contract Laboratory Program (CLP) Web site at:
http://www.epa.gov/superfund/programs/clp/guidance.htm
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TABLE OF CONTENTS
LIST OF TABLES vii
ACRONYMS AND ABBREVIATIONS ix
I. Terminology ix
INTRODUCTION 1
I. Purpose of Document 1
II. Limitations of Use 1
III. Document Organization 1
IV. For Additional Information 1
PART A: GENERAL DATA REVIEW 3
I. Preliminary Review 5
II. Data Qualifier Definitions 6
III. Data Review Narrative 7
PART B: METHOD-SPECIFIC DATA REVIEW 9
TRACE VOLATILE DATA REVIEW 11
I. Preservation and Holding Times 13
II. Gas Chromatograph/Mass Spectrometer Instrument Performance Check 15
III. Initial Calibration 23
IV. Continuing Calibration Verification 28
V. Blanks 31
VI. Deuterated Monitoring Compound 34
VII. Matrix Spike/Matrix Spike Duplicate 37
VIII. Internal Standard 39
IX. Target Analyte Identification 41
X. Target Analyte Quantitation and Reported Contract Required Quantitation Limit 43
XI. Tentatively Identified Compounds 44
XII. System Performance 47
XIII. Regional Quality Assurance and Quality Control 48
XIV. Overall Assessment of Data 49
LOW/MEDIUM VOLATILE DATA REVIEW 51
I. Preservation and Holding Times 53
II. Gas Chromatograph/Mass Spectrometer Instrument Performance Check 57
III. Initial Calibration 65
IV. Continuing Calibration Verification 70
V. Blanks 73
VI. Deuterated Monitoring Compound 76
VII. Matrix Spike/Matrix Spike Duplicate 80
VIII. Internal Standard 82
IX. Target Analyte Identification 84
X. Target Analyte Quantitation and Reported Contract Required Quantitation Limit 86
XI. Tentatively Identified Compounds 88
XII. System Performance 91
XIII. Regional Quality Assurance and Quality Control 92
XIV. Overall Assessment of Data 93
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SEMIVOLATILE DATA REVIEW 95
I. Preservation and Holding Times 97
II. Gas Chromatograph/Mass Spectrometer Instrument Performance Check 101
III. Initial Calibration 109
IV. Continuing Calibration Verification 116
V. Blanks 119
VI. Deuterated Monitoring Compound 122
VII. Matrix Spike/Matrix Spike Duplicate 126
VIII. Gel Permeation Chromatography Performance Check 128
IX. Internal Standard 130
X. Target Analyte Identification 132
XI. Target Analyte Quantitation and Reported Contract Required Quantitation Limit 134
XII. Tentatively Identified Compounds 136
XIII. System Performance 139
XIV. Regional Quality Assurance and Quality Control 140
XV. Overall Assessment of Data 141
PESTICIDE DATA REVIEW 143
I. Preservation and Holding Times 145
II. Gas Chromatograph with Electron Capture Detector Instrument Performance Check 150
III. Initial Calibration 155
IV. Continuing Calibration Verification 161
V. Blanks 166
VI. Surrogate 169
VII. Matrix Spike/Matrix Spike Duplicate 171
VIII. Laboratory Control Sample 173
IX. Florisil Cartridge Performance Check 175
X. Gel Permeation Chromatography Performance Check 177
XI. Target Analyte Identification 179
XII. Gas Chromatograph/Mass Spectrometer Confirmation 181
XIII. Target Analyte Quantitation and Reported Contract Required Quantitation Limit 182
XIV. Regional Quality Assurance and Quality Control 184
XV. Overall Assessment of Data 185
AROCLOR DATA REVIEW 187
I. Preservation and Holding Times 189
II. Initial Calibration 192
III. Continuing Calibration Verification 196
IV. Blanks 200
V. Surrogate 203
VI. Matrix Spike/Matrix Spike Duplicate 206
VII. Laboratory Control Sample 208
VIII. Gel Permeation Chromatography Performance Check 210
IX. Target Analyte Identification 212
X. Gas Chromatograph/Mass Spectrometer Confirmation 214
XI. Target Analyte Quantitation and Reported Contract Required Quantitation Limit 215
XII. Regional Quality Assurance and Quality Control 217
XIII. Overall Assessment of Data 218
APPENDIX A: GLOSSARY A-l
APPENDIX B: ORGANIC DATA REVIEW SUMMARY B-l
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LIST OF TABLES
Table 1. Data Qualifiers and Definitions 6
Table 2. Preservation and Holding Time Actions for Trace Volatile Analysis 14
Table 3. Ion Abundance Criteria for BFB 21
Table 4. RRF, %RSD and %D Acceptance Criteria in Initial Calibration and CCV for Trace Volatile
Analysis 25
Table 5. Initial Calibration Actions for Trace Volatile Analysis 27
Table 6. CCV Actions for Trace Volatile Analysis 30
Table 7. Blank Actions for Trace Volatile Analysis 33
Table 8. Trace Volatile DMCs and Recovery Limits 34
Table 9. DMC Recovery Actions for Trace Volatile Analysis 35
Table 10. Trace Volatile DMCs and the Associated Target Analytes 36
Table 11. MS/MSD %R and RPD Limits for Trace Volatile Analysis 38
Table 12. MS/MSD Actions for Trace Volatile Analysis 38
Table 13. Internal Standard Actions for Trace Volatile Analysis 40
Table 14. Preservation and Holding Time Actions for Low/Medium Volatile Analysis 56
Table 15. Ion Abundance Criteria for BFB 63
Table 16. RRF, %RSD, and %D Acceptance Criteria in Initial Calibration and CCV for Low/Medium
Volatile Analysis 67
Table 17. Initial Calibration Actions for Low/Medium Volatile Analysis 69
Table 18. CCV Actions for Low/Medium Volatile Analysis 72
Table 19. Blank and TCLP/SPLP LEB Actions for Low/Medium Volatile Analysis 75
Table 20. Low/Medium Volatile DMCs and Recovery Limits 76
Table 21. DMC Actions for Low/Medium Volatile Analysis 77
Table 22. Low/Medium Volatile DMCs and the Associated Target Analytes 78
Table 23. MS/MSD %R and RPD Limits for Low/Medium Volatile Analysis 81
Table 24. MS/MSD Actions for Low/Medium Volatile Analysis 81
Table 25. Internal Standard Actions for Low/Medium Volatile Analysis 83
Table 26. Percent Solids Actions for Low/Medium Volatile Analysis for Non-Aqueous Samples 87
Table 27. Preservation and Holding Time Actions for Semivolatile Analysis 99
Table 28. Holding Time Actions for Non-Aqueous Semivolatile TCLP/SPLP Sample Analysis 100
Table 29. Ion Abundance Criteria for DFTPP 107
Table 30. RRF, %RSD and %D Acceptance Criteria in Initial Calibration and CCV for Semivolatile
Analysis 112
Table 31. Initial Calibration Actions for Semivolatile Analysis 115
Table 32. CCV Actions for Semivolatile Analysis 118
Table 33. Blank and TCLP/SPLP LEB Actions for Semivolatile Analysis 121
Table 34. Semivolatile DMC and %R Limits 122
Table 35. DMC Actions for Semivolatile Analysis 124
Table 36. Semivolatile DMCs and the Associated Target Analytes 124
Table 37. Semivolatile SIM DMCs and the Associated Target Analytes 125
Table 38. MS/MSD %Rand RPD Limits for Semivolatile Analysis 127
Table 39. MS/MSD Actions for Semivolatile Analysis 127
Table 40. Internal Standard Actions for Semivolatile Analysis 131
Table 41. Percent Solids Actions for Semivolatile Analysis for Non-Aqueous Samples 135
Table 42. Preservation and Holding Time Actions for Pesticide Analysis 148
Table 43. Holding Time Actions for Non-Aqueous Pesticide TCLP/SPLP Sample Analysis 149
Table 44. Resolution Check Mixture 150
Table 45. Performance Evaluation Mixture (PEM) 150
Table 46. Individual Standard Mixtures A and B 151
Table 47. Individual Standard Mixture C 152
Table 48. GC/ECD Instrument Performance Check Actions 154
Table 49. Concentration Levels of Calibration Standards 155
Table 50. Initial Calibration Sequence 1 157
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Table 51. Initial Calibration Sequence 2 157
Table 52. Initial Calibration Action for Pesticide Analysis 160
Table 53. CCV Actions for Pesticide Analysis 165
Table 54. Blank and TCLP/SPLP LEB Actions for Pesticide Analysis 168
Table 55. Surrogate Actions for Pesticide Analysis 170
Table 56. MS/MSD %R and RPD Limits for Pesticide Analysis 172
Table 57. MS/MSD Actions for Pesticide Analysis 172
Table 58. LCS %R Limits for Pesticide Analysis 173
Table 59. LCS Actions for Pesticide Analysis 174
Table 60. Florisil Cartridge Performance Check Actions 176
Table 61. GPC Performance Check Actions for Pesticide Analysis 178
Table 62. GC/MS Confirmation Actions 181
Table 63. Percent Solids Actions for Pesticide Analysis for Non-Aqueous Samples 183
Table 64. Preservation and Holding Time Actions for Aroclor Analysis 191
Table 65. Initial Calibration Sequence 193
Table 66. Initial Calibration Action for Aroclor Analysis 195
Table 67. CCV Actions for Aroclor Analysis 199
Table 68. Blank Actions for Aroclor Analysis 202
Table 69. Surrogate Actions for Aroclor Analysis 205
Table 70. MS/MSD %R and RPD Limits for Aroclor Analysis 207
Table 71. MS/MSD Actions for Aroclor Analysis 207
Table 72. LCS %R Limits for Aroclor Analysis 208
Table 73. LCS Actions for Aroclor Analysis 209
Table 74. GPC Performance Check Actions for Arolcor Analysis 211
Table 75. GC/MS Confirmation Actions 214
Table 76. Percent Solids Actions for Aroclor Analysis for Non-Aqueous Samples 216
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Organic Data Review
ACRONYMS AND ABBREVIATIONS
I. Terminology
The following acronyms and abbreviations may be found throughout this document. For further
definition, see Appendix A: Glossary at the end of the document.
BFB
CAS
CCS
CCV
CF
CF
CLP
CLPPO
CRQL
CS3
CSF
DCB
DFTPP
DMC
DQA
DQO
EDM
EPA
EXES
GC
GC/ECD
GC/MS
GPC
ICAL
INDA
INDB
INDC
IUPAC
LCS
LEB
MS
MSD
m/z
Bromofluorobenzene
Chemical Abstract Service
Contract Compliance Screening
Continuing Calibration Verification
Calibration Factor
Mean Calibration Factor
Contract Laboratory Program
Contract Laboratory Program Project Officer
Contract Required Quantitation Limit
Mid-point Calibration Standard
Complete SDG File
Decachlorobiphenyl
Decafluorotriphenylphosphine
Deuterated Monitoring Compound
Data Quality Assessment
Data Quality Objective
EXES Data Manager
United States Environmental Protection Agency
Electronic Data Exchange and Evaluation System
Gas Chromatograph
Gas Chromatograph/Electron Capture Detector
Gas Chromatograph/Mass Spectrometer
Gel Permeation Chromatography
Initial Calibration
Individual Standard Mixture A
Individual Standard Mixture B
Individual Standard Mixture C
International Union of Pure and Applied Chemistry
Laboratory Control Sample
Leachate Extraction Blank
Matrix Spike
Matrix Spike Duplicate
Mass-to-Charge Ratio
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Organic Data Review
NFG
NIH
NIST
OSRTI
%Breakdown
%D
%R
%Resolution
%RSD
%Solids
PAH
PCP
PCBs
PE
PEM
PIBLK
QA
QAPP
QC
RESC
RFQ
RIC
RPD
RRF
RRF
RRT
RT
RT
SAP
SDG
SEDD
SIM
SMO
SOP
SOW
SPLP
SVGA
National Functional Guidelines
National Institutes of Health
National Institue of Standards and Technology
Office of Superfund Remediation and Technology Innovation
Percent Breakdown
Percent Difference
Percent Recovery
Percent Resolution
Percent Relative Standard Deviation
Percent Solids
Polycyclic Aromatic Hydrocarbon
Pentachlorophenol
Polychlorinated Biphenyls
Performance Evaluation
Performance Evaluation Mixture
Pesticide Instrument Blank
Quality Assurance
Quality Assurance Project Plan
Quality Control
Resolution Check Mixture
Request for Quote
Reconstructed Ion Chromatogram
Relative Percent Difference
Relative Response Factor
Mean Relative Response Factor
Relative Retention Time
Retention Time
Mean Retention Time
Sampling and Analysis Plan
Sample Delivery Group
Staged Electronic Data Deliverable
Selected Ion Monitoring
Sample Management Office
Standard Operating Procedure
Statement of Work
Synthetic Precipitation Leaching Procedure
Semi volatile s
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Organic Data Review
TAL Target Analyte List
TCLP Toxicity Characteristic Leaching Procedure
TCX Tetrachloro-m-xylene
TIC Tentatively Identified Compound
TR/COC Traffic Report/Chain of Custody
UV Ultraviolet
ZHE Zero Headspace Extraction
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Organic Data Review Introduction
INTRODUCTION
I. Purpose of Document
This document contains guidance to aid the data reviewer in determining the usability of analytical data
generated using the United States Environmental Protection Agency (EPA) Contract Laboratory
Program (CLP) Statement of Work (SOW) for Organics Analysis (Multi-Media, Multi-Concentration)
SOM02.1. The SOW includes Trace Volatiles (Trace VOAs), Low-Medium Volatiles (Low-Med
VOAs), Semivolatiles (SVGAs), Pesticides, and Aroclors analytical methods.
The guidelines presented in this document are designed to assist the data reviewer in evaluating: (a)
whether the analytical data meet the technical and Quality Control (QC) criteria specified in the SOW,
and (b) the usability and extent of bias of any data not meeting these criteria. This document contains
definitive guidance in areas such as blanks, calibration standards, and instrument performance checks
in which performance is fully under a laboratory's control. General guidance is provided to aid the
reviewer in making subjective judgments regarding the use of data that is affected by site conditions
and do not meet SOW-specific requirements.
II. Limitations of Use
This guidance is specific to the review of analytical data generated using CLP SOW SOM02.1. It
applies to the current version of the SOW, as well as future versions that contain editorial changes. To
use this document effectively, the reviewer should have an understanding of the analytical methods and
a general overview of the Sample Delivery Group (SDG) or sample Case at hand. This guidance is not
appropriate for use in conducting contract compliance reviews and should be used with caution in
reviewing data generated using methods other than the CLP SOW SOM02.1, although the general types
of QC checks, the evaluation procedures, and the decisions made after consideration of the evalutation
criteria may be applicable to data from any similar method.
While this document is a valuable aid in the formal data review process, other sources of guidance and
information, along with professional judgment, are useful in determining the ultimate usability of the
data. This is particularly critical in those cases where all data do not meet SOW-specific technical and
QC criteria. To make appropriate judgments, the reviewer needs to gain a complete understanding of
the intended use of the data, and is strongly encouraged to establish a dialogue with the data user prior
to and following the data review, to discuss usability issues and to resolve questions regarding the
review.
III. Document Organization
Following this introduction, the document is presented in two major parts: Part A - General Data
Review, which applies to all methods; and Part B - Method-Specific Data Review. In Part B, each
method is addressed individually in a stand-alone format. A complete list of acronyms used in this
document appears preceding this introduction, and a Glossary is appended as Appendix A.
IV. For Additional Information
For additional information regarding the CLP and the services it provides, refer to the CLP Web site at
http://www.epa.gov/superfund/programs/clp/index.htm
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Organic Data Review General
PART A: GENERAL DATA REVIEW
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Organic Data Review General
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Organic Data Review General
I. Preliminary Review
A preliminary review should be performed on the data, prior to embarking on the method-specific
review (see Part B). During this process, the reviewer should compile the necessary data package
elements to ensure that all of the information needed to determine data usability is available. The
preliminary review also allows the reviewer to obtain an overview of the Case or Sample Delivery
Group (SDG) under review.
This initial review should include, but is not limited to, verification of the exact number of samples,
their assigned number and matrices, and the Contractor laboratory name. It should take into
consideration all the documentation specific to the sample data package, which may include Modified
Analysis requests, the Traffic Report/Chain of Custody (TR/COC) form, the SDG Narrative, and other
applicable documents.
The reviewer should be aware that minor modifications to the Statement of Work (SOW) that have
been made through a Modified Analysis request, to meet site-specific requirements, could affect certain
validation criteria such as the Contract Required Quantitation Limits (CRQLs), initial calibration
(ICAL) levels, and Target Analyte Lists (TALs). Therefore, these modifications should be applied
during the method-specific review (Part B) process.
The Cases or SDGs routinely have unique field quality control (QC) samples that may affect the
outcome of the review. These include field and trip blanks, field duplicates, and Performance
Evaluation (PE) samples which must be identified in the sampling records. The reviewer should verify
that the following information is identified in the sampling records (e.g., TR/COC records, field logs,
and/or contractor tables):
1. The United States Environmental Protection Agency (EPA) Region where the samples were
collected, and
2. The complete list of samples with information on:
a. Sample matrix
b. Field blanks and trip blanks (if applicable)
c. Field duplicates (if applicable)
d. Field spikes (if applicable)
e. PE samples (if applicable)
f Sampling dates
g. Sampling times
h. Shipping dates
i. Preservatives
j. Types of analysis
k. Contractor laboratory
The laboratory's SDG Narrative is another source of general information which includes notable
problems with matrices; insufficient sample volume for analysis or re-analysis; samples received in
broken containers; preservation information; and unusual events. The reviewer should also inspect any
email or telephone/communication logs in the data package detailing any discussions of sample
preparation and/or analysis issues between the laboratory, Contract Laboratory Program (CLP) Sample
Management Office (SMO) and the EPA Region.
The reviewer should also have a copy of the Quality Assurance Project Plan (QAPP), or similar
document, for the project for which samples were analyzed, to assist in the determination of final
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Organic Data Review
General
usability of the analytical data. The reviewer should contact the appropriate Regional CLP Project
Officer (CLP PO) to obtain copies of the QAPP and relevant site information.
For data obtained through the CLP, the Staged Electronic Data Deliverable (SEDD) generated by the
CLP laboratories is subjected to the following reviews via the Electronic Data Exchange and
Evaluation System (EXES): 1) automated data assessment for Contract Compliance Screening (CCS)
based on the technical and QC criteria in CLP SOW SOM02.1, and 2) automated data validation based
on the criteria in the EPA CLP National Functional Guidelines (NFG)for Superfund Organic Methods
Data Review. In addition, completeness checks are manually performed on the hardcopy data. The
automated CCS results and hardcopy data issues are subsequently included in a CCS defect report that
is provided to the laboratory. The laboratory may then submit a reconciliation package for any missing
items, or to correct non-compliant data identified in the report. The automated data validation results
are summarized in criteria-based NFG reports that are provided to the EPA Regions. The data reviewer
can access the CCS and NFG reports through the EXES Data Manager (EDM) via the SMO Portal and
may use them in determining data usability.
For more information about EXES and EDM, refer to the following CLP Web site:
http://www.epa.gov/superfund/programs/clp/data_assessment.htm
For access to the SMO Portal, refer to the following CLP Web site to contact the CLP PO from the
Region where the data review is being performed and obtain the necessary username and password
information:
http: //www. epa.gov/superfund/programs/clp/contacts .htm
For concerns or questions regarding the data package, contact the CLP PO from the Region where the
samples were collected.
II. Data Qualifier Definitions
The following definitions provide brief explanations of the national qualifiers assigned to results during
the data review process. The reviewer should use these qualifiers as applicable. If the reviewer chooses
to use additional qualifiers, a complete explanation of those qualifiers should accompany the data
review.
Table 1. Data Qualifiers and Definitions
Data
Qualifier
U
J
J+
J-
NJ
UJ
R
C
Definition
The analyte was analyzed for, but was not detected above the level of the reported sample
quantitation limit.
The result is an estimated quantity. The associated numerical value is the approximate
concentration of the analyte in the sample.
The result is an estimated quantity, but the result may be biased high.
The result is an estimated quantity, but the result may be biased low.
The analyte has been "tentatively identified" or "presumptively" as present and the
associated numerical value is the estimated concentration in the sample.
The analyte was analyzed for, but was not detected. The reported quantitation limit is
approximate and may be inaccurate or imprecise.
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.
The target Pesticide or Aroclor analyte identification has been confirmed by Gas
Chromatograph/Mass Spectrometer (GC/MS).
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Organic Data Review General
Data
Qualifier
X
Definition
The target Pesticide or Aroclor
analysis was performed.
analyte identification
was not confirmed when GC/MS
III. Data Review Narrative
The reviewer should complete a Data Review Narrative that includes comments that address the
problems identified during the review process and state the limitations of the data associated with a
Case or SDG. The CLP Sample Numbers, analytical methods, extent of the problem(s), and assigned
qualifiers should also be listed in the document.
The Data Review Narrative, including the Organic Data Review Summary form (see Appendix B) must
accompany the laboratory data forwarded to the appropriate data recipient(s). A copy of the Data
Review Narrative should also be submitted to the CLP PO assigned oversight responsibility for the
Contractor laboratory.
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Organic Data Review
PART B: METHOD-SPECIFIC DATA REVIEW
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Organic Data Review Trace VOA
TRACE VOLATILE DATA REVIEW
The Trace Volatile organic data requirements to be reviewed during validation are listed below:
I. Preservation and Holding Times 13
II. Gas Chromatograph/Mass Spectrometer Instrument Performance Check 15
III. Initial Calibration 23
IV. Continuing Calibration Verification 28
V. Blanks 31
VI. Deuterated Monitoring Compound 34
VII. Matrix Spike/Matrix Spike Duplicate 37
VIII. Internal Standard 39
IX. Target Analyte Identification 41
X. Target Analyte Quantitation and Reported Contract Required Quantitation Limit 43
XI. Tentatively Identified Compounds 44
XII. System Performance 47
XIII. Regional Quality Assurance and Quality Control 48
XIV. Overall Assessment of Data 49
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Organic Data Review Trace VOA
I. Preservation and Holding Times
A. Review Items
Form 1A-OR, Form 1B-OR, Traffic Report/Chain of Custody (TR/COC) documentation, Form DC-1,
raw data, and the Sample Delivery Group (SDG) 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 condition and the
holding time of the sample.
C. Criteria
1. Technical holding time is determined from the date of field sample collection to the date of sample
analysis.
2. Samples should be in proper condition with shipping container temperatures at < 6°C upon receipt
at the laboratory. The samples shall be protected from light and refrigerated at < 6°C (but not
frozen) from the time of receipt at the laboratory until sample analysis.
3. The technical holding time criteria for aqueous samples that are properly cooled at < 6°C without
any indications of being preserved is 7 days.
4. The technical holding time criteria for aqueous samples that are properly cooled at < 6°C and
acid-preserved with HC1 to a pH of < 2 is 14 days.
D. Evaluation
1. Review the SDG Narrative to determine if the samples were properly preserved and arrived at the
laboratory in proper condition (e.g., received intact, appropriate sample temperature at receipt, pH,
and absence of air bubbles or detectable headspace). If there is an indication of problems with the
samples, the sample integrity may be compromised.
2. Verify that the analysis dates on Form 1A-OR and Form 1B-OR and the raw data/SDG file are
identical.
3. Establish technical holding times by comparing the sample collection dates on the TR/COC
documentation with the dates of analysis on Form 1A-OR and Form 1B-OR and the raw data. Also
consider information contained in the Complete SDG File (CSF) as it may be helpful in the
assessment.
a. These evaluation guidelines are intended to address the integrity of data for all analytes in
Statement of Work (SOW) Exhibit C for Trace Volatile Organics. If the data user is interested
in only a subset of the analytes and has data supporting analyte stability over longer holding
times, then those longer times may be applied prior to data qualification under Section E,
below. This information should be made part of the Data Review Narrative for evidentiary
purposes.
E. Action
1. If samples are received with shipping container temperatures > 6°C, use professional judgment to
qualify detects and non-detects.
2. If a discrepancy is found between the sample analysis date on Form 1A-OR and Form 1B-OR and
the one on the raw data, perform a more comprehensive review to determine the correct date to be
used for establishing the holding time.
3. If samples are not properly preserved but are analyzed within the technical holding time of 7 days,
detects and non-detects should not be qualified.
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Organic Data Review
Trace VGA
4. If samples are not properly preserved and are analyzed outside of the technical holding time of 7
days, qualify detects as estimated low (J-) and non-detects as unusable (R).
5. If samples are properly preserved and are analyzed within the technical holding time of 14 days,
detects and non-detects should not be qualified.
6. If samples are properly preserved, but are analyzed outside of the technical holding time of 14 days,
qualify detects as estimated (J) and non-detects as unusable (R). Use caution in determining
whether some detected analytes should be qualified as estimated low (J-) or as estimated high (J+),
based on knowledge of individual analyte stability on interactions (i.e., dehydrohalogenation).
7. When the holding times are exceeded, annotate in the Data Review Narrative any possible
consequences for the analytical results.
8. If holding times are grossly exceeded, qualify detects as estimated low (J-) and non-detects as
unusable (R). Note this for Contract Laboratory Program Project Officer (CLP PO) action.
Annotate the effect of the holding time exceedance on the resulting data in the Data Review
Narrative, whenever possible.
9. If samples are received with shipping container temperatures > 10°C, use professional judgment to
determine the reliability of the data, or qualify detects as estimated low (J-) and non-detects as
estimated (UJ).
Table 2. Preservation and Holding Time Actions for Trace Volatile Analysis
Criteria
Sample temperature > 6 C upon receipt at the
laboratory
Sample not preserved but analyzed within the 7-day
technical holding time
Samples not preserved and analyzed outside the
7-day technical holding time
Sample properly preserved and analyzed within the
14-day technical holding time
Sample properly preserved but analyzed outside the
14-day technical holding time
Holding time grossly exceeded
Action
Detect
Use professional
judgment
No qualification
J-
No qualification
J*
J-
Non-detect
Use professional
judgment
No qualification
R
No qualification
R
R
* The true direction of any bias may be unknown in this case. Use professional judgment based on
knowledge of the chemistry of the analytes in the sample, or do not assign a direction to the bias.
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Organic Data Review
Trace VGA
II.
Gas Chromatograph/Mass Spectrometer Instrument Performance Check
A. Review Items
Form 5-OR, bromofluorobenzene (BFB) mass spectra, and mass listing.
B. Objective
The objective of performing Gas Chromatograph/Mass Spectrometer (GC/MS) instrument
performance checks is to ensure adequate mass resolution, identification, and to some degree,
sensitivity, and to document this level of performance prior to analyzing any sequence of standards or
samples.
C. Criteria
1. Sufficient amount of the BFB instrument performance check solution (up to 50 ng BFB on-column)
must be injected once at the beginning of each 12-hour period, during which samples, blanks, or
standards are to be analyzed. The 12-hour period begins with either the injection of BFB, or in
cases where a closing Continuing Calibration Verification (CCV) can be used as an opening CCV,
the 12-hour period begins with the injection of the opening CCV.
Listed below are examples of acceptable analytical sequences incorporating the use of the opening
and/or closing CCV. Use these examples as a guide for the possible analytical sequences that can
be expected.
Conditions for When
Example Sequence is
Appropriate:
Acceptable Criteria That Must
Be Met:
Notes:
Use Example 1 if time
remains on the 12-hour
clock after the initial
calibration sequence.
BFB tunes meet instrument
performance criteria.
The five Initial Calibration
standards meet initial
calibration criteria.
CCV A meets both opening
and closing CCV criteria.
CCV B meets closing CCV
criteria.
The requirement of starting the
new 12-hour clock for Analytical
Sequence 2 with a new BFB tune
is waived if CCV A meets opening
CCV criteria. If CCV B meets
opening CCV criteria, a method
blank and subsequent samples
may be analyzed immediately
after CCV B.
Use Example 2 if time
remains on the 12-hour
clock after the initial
calibration sequence.
BFB tunes meet instrument
performance criteria.
The five Initial Calibration
standards meet initial
calibration criteria.
CCV A meets closing CCV
criteria (but does not meet
opening CCV criteria).
CCV B meets opening CCV
criteria.
CCV C meets closing CCV
criteria.
CCV A does not meet opening
CCV criteria. Therefore a new
BFB tune must be performed,
immediately followed by CCV B
before a method blank and any
samples may be analyzed. In this
case, the new 12-hour clock and
Analytical Sequence 2 begins with
the injection of the new BFB tune.
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Conditions for When
Example Sequence is
Appropriate:
Acceptable Criteria That Must
Be Met:
Notes:
Use Example 3 if more
than 12 hours have
elapsed since the most
recent initial calibration
or closing CCV,
OR
if the most recent closing
CCV was not or could
not be used as an
opening CCV.
BFB tunes meet instrument
performance criteria.
CCV A meets opening CCV
criteria.
CCV B meets both opening
and closing CCV criteria.
CCV C meets both opening
and closing CCV criteria.
The requirement of starting the
new 12-hour clock for Analytical
Sequence 2 with a new BFB tune
is waived if CCV B meets opening
CCV criteria. If CCV C meets
opening CCV criteria, a method
blank and subsequent samples
may be analyzed immediately
after CCV B.
Use Example 4 if more
than 12-hours have
elapsed since the most
recent initial calibration
or closing CCV,
OR
if the most recent closing
CCV was not or could
not be used as an
opening CCV.
BFB tunes meet instrument
performance criteria.
CCV A meets opening CCV
criteria.
CCV B meets closing CCV
criteria (but does not meet
opening CCV criteria).
CCV C meets opening CCV
criteria.
CCV D meets both opening
and closing CCV criteria.
CCV B does not meet opening
CCV criteria. Therefore a new
BFB tune must be performed,
immediately followed by CCV C
before a method blank and any
samples may be analyzed. In this
case, the new 12-hour clock and
Analytical Sequence 2 begins with
the injection of the new BFB tune.
The requirement of starting the
new 12-hour clock for Analytical
Sequence 3 with a new BFB tune
is waived if CCV D meets opening
CCV criteria. If CCV D meets
opening CCV criteria, a method
blank and subsequent samples
may be analyzed immediately
after CCV D.
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Example 1:
Example 1:
Start of 12-hour clock for
Analytical Sequence 1
Time Material Injected
0 hr BFB
Initial Calibration 0.5
Initial Calibration 1.0
Initial Calibration 5.0
Initial Calibration 10
Initial Calibration 20
Method Blank
Subsequent Samples
•
•
•
.
Analytical
Sequence #
1
1
1
1
1
1
1
1
1
1
1
1
End of 12-hour clock for
Analytical Sequence I/
Beginning of 12-hour clock
for Analytical Sequence 2
12 hr
End of 12-hour clock for
Analytical Sequence 21
Beginning of 12-hour clock
for Analytical Sequence 3
24 hr
CCV A (meets opening CCV
criteria)
Method Blank
Subsequent Samples
CCV B (meets opening CCV
criteria)
1/2
2
2
2
2
2
2
2/3
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Example 2:
Example 2:
Start of 12-hour clock for
Analytical Sequence 1
Time Material Injected
0 hr BFB
Initial Calibration 0.5
Initial Calibration 1.0
Initial Calibration 5.0
Initial Calibration 10
Initial Calibration 20
Method Blank
Subsequent Samples
•
•
•
.
Analytical
Sequence #
1
1
1
1
1
1
1
1
1
1
1
1
End of 12-hour clock for
Analytical Sequence 1
Beginning of 12-hour
clock for Analytical
Sequence 2
, ~ ,
13 hr
End of 12-hour clock for
Analytical Sequence 2
CCV A (meets closing CCV criteria;
fails opening CCV criteria)
BFB
CCV B (meets opening CCV
criteria)
Method Blank
Subsequent Samples
2
2
2
2
2
2
25 hr CCV C (meets closing CCV criteria)
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Example 3:
Example 3: Time Material Injected
Start of 12-hour clock for ,
,,.,,., . Dm r>rr>
Analytical Sequence 1
CCV A (meets opening CCV
criteria)
Method Blank
Subsequent Samples
•
•
•
•
Analytical
Sequence #
1
1
1
1
1
1
1
1
End of 12-hour clock for
Analytical Sequence I/
Beginning of 12-hour clock
for Analytical Sequence 2
12 hr
End of 12-hour clock for
Analytical Sequence 21
Beginning of 12-hour clock
for Analytical Sequence 3
24
CCV B (meets opening CCV
criteria)
Method Blank
Subsequent Samples
CCV C (meets opening CCV
criteria)
1/2
2
2
2
2
2
2/3
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Example 4:
Example 4: Time Material Injected
Start of 12-hour clock for ,
,,.,,., . Dm r>rr>
Analytical Sequence 1
CCV A (meets opening CCV criteria)
Method Blank
Subsequent Samples
•
•
•
Analytical
Sequence #
1
1
1
1
1
1
1
End of 12-hour clock for
Analytical Sequence 1
Beginning of 12-hour
clock for Analytical
Sequence 2
End of 12-hour clock for
Analytical Sequence 21
Beginning of 12-hour
clock for Analytical
Sequence 3
12 hr
13 hr
CCV B (meets closing CCV criteria;
fails opening CCV criteria)
BFB
CCV C (meets opening CCV criteria)
Method Blank
Subsequent Samples
25 hr CCV D (meets opening CCV criteria)
2
2
2
2
2
2
2/3
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2. The BFB instrument performance check must meet the ion abundance criteria listed in Table 3.
Table 3. Ion Abundance Criteria for BFB
m/z
50
75
95
96
173
174
175
176
177
Ion Abundance Criteria
15. 0-40.0% of mass 95
30.0 -80.0% of mass 95
Base peak, 100% relative abundance
5. 0-9.0% of mass 95*
Less than 2.0% of mass 174
5 0.0% -120% of mass 95
5. 0-9.0% of mass 174
95.0 -101% of mass 174
5. 0-9.0% of mass 176
* All ion abundances must be normalized to mass-to-charge (m/z) 95, the nominal base peak, even
though the ion abundance of m/z 174 may be up to 120% that of m/z 95.
D. Evaluation
1. Verify that the BFB Instrument Performance Check solution is analyzed at the specified frequency
and sequence.
2. Compare the data presented on Form 5 -OR for each Instrument Performance Check with each mass
listing submitted to ensure the following:
a. Form 5-OR is present and completed for each required BFB at the specified frequency.
b. The laboratory has not made transcription errors on Forms 5-OR. If there are major differences
between the mass listing and the data on Form 5-OR, a more in-depth review of the data is
required. This may include obtaining and reviewing additional information from the
laboratory.
c. The appropriate number of significant figures has been reported (number of significant figures
given for each ion in the ion abundance criteria column) and that rounding is correct.
d. The laboratory has not made any calculation errors.
3. Verify from the raw data (mass listing) that the mass assignment is correct and that the mass listing
is normalized to the specified m/z of 95, 174 and 176, respectively.
4. Verify that the ion abundance criteria are met. The ion abundance for m/z 173, 175, 176, and 177
are calculated by normalizing to the specified m/z. The critical ion abundance criteria for BFB are
the relative abundance ratios of m/z 95/96, 174/175, 174/176, and 176/177. The relative abundance
ratios of m/z 50 and 75 are of lower importance for target analytes than for Tentatively Identified
Compounds (TICs).
5. If possible, verify that spectra are generated using appropriate background subtraction techniques.
Since the BFB spectrum is obtained from chromatographic peaks that should be free from
co-elution problems, background subtraction should be performed in accordance with the
following procedure:
a. Three scans (the peak apex scan and the scans immediately preceding and following the apex)
are acquired and averaged.
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Organic Data Review Trace VOA
b. Background subtraction must be accomplished using a single scan no more than 20 scans prior
to the elution of BFB, but the BFB peak must not be subtracted as part of the background.
NOTE: All mass spectrometer instrument conditions must be identical to those used for sample
analysis. Background subtraction actions resulting in spectral distortions for the sole
purpose of meeting the method specifications are contrary to the Quality Assurance (QA)
objectives, and are therefore unacceptable.
NOTE: For data obtained from the Contract Laboratory Program (CLP), information regarding
non-compliant BFB instrument performance checks can be obtained from the National
Functional Guidelines (NFG) reports and may be used as part of the evaluation process.
E. Action
1. If the instrument performance check is not analyzed at the specified frequency and sequence,
contact the Regional CLP PO to arrange for a reanalysis of all affected samples.
a. In the event that samples cannot be reanalyzed, examine all calibrations associated with the
sequence to evaluate whether proper qualitative criteria were achievable. If so, it may be
possible to salvage usable data from the sequence. Otherwise, qualify the data as unusable (R).
2. If minor transcription errors are found to be insignificant to data quality and can be corrected on a
copy of the form, no further actions are required.
3. If the laboratory failed to provide the correct forms, or if significant transcription or calculation
errors are found, notify the Regional CLP PO, who may contact the laboratory to request the
necessary information. If the information is not available, use professional judgment to assess the
data, and notify the laboratory's CLP PO.
4. If the mass assignment is in error (e.g., m/z 96 is indicated as the base peak rather than m/z 95),
qualify detects and non-detects in the associated samples as unusable (R).
5. If the ion abundance criteria in Table 3 are not met, use professional judgment to qualify detects
and non-detects in the associated samples.
6. Annotate decisions to use analytical data associated with non-compliant BFB instrument
performance checks in the Data Review Narrative.
7. If the instrument performance check criteria are achieved using techniques other than those
described in Section II.D.5, obtain additional information to evaluate the performance and
procedures. Note any concerns (e.g., use of inappropriate technique for background subtraction) or
questions for laboratory CLP PO action.
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III. Initial Calibration
A. Review Items
Form 6A-OR, quantitation reports, and chromatograms.
B. Objective
The objective of initial calibration (ICAL) is to ensure that the instrument is capable of producing
acceptable qualitative and quantitative data.
C. Criteria
1. ICAL should be performed at the specified frequency and sequence. Each GC/MS system must be
calibrated with a minimum of five concentrations to determine instrument sensitivity and the
linearity of GC/MS response for the purgeable target analytes and Deuterated Monitoring
Compounds (DMCs).
a. ICAL standards must be analyzed prior to any analysis of samples and required blanks and
within 12 hours of the associated instrument performance check at the beginning of each
analytical sequence, or as necessary if the CCV acceptance criteria are not met.
b. ICAL standards must contain all required target analytes and DMCs at concentrations of 0.50,
1.0, 5.0, 10, and 20 (ig/L for non-ketones, 5.0, 10, 50, 100 and 200 (ig/L for ketones.
c. All three xylene isomers (o-, m-, and p-xylene) must be present in calibration standards.
d. Concentrations for o-xylene must be at 0.50, 1.0, 5.0, 10 and 20 (ig/L, while the total
concentrations of the m- plus the p-xylene isomers must be at 0.50, 1.0, 5.0, 10, and 20 (ig/L.
2. The Relative Response Factor (RRF), mean RRF (RRF) and Percent Relative Standard Deviation
(%RSD) must be calculated for each target analyte and DMC according to the SOW.
3. The RRF for each target analyte and DMC in each ICAL standard must be > Minimum RRF value
in Table 4.
4. The %RSD of the ICAL RRF for each target analyte and DMC must be < Maximum %RSD value
in Table 4.
NOTE: The technical acceptance criteria specified in a "Request for Quote (RFQ) for Modified
Analysis" may impact some of the preceding evaluation criteria. A copy of this document
should be present in the SDG, when applicable. Refer to the CLP home page at
http://www.epa.gov/oerrpage/superfund/programs/clp/modifiedanalyses.htm for the
specific method flexibility requirements.
D. Evaluation
1. Verify that the ICAL is performed at the specified frequency and sequence.
2. Verify that the correct concentrations of the target analytes and DMCs are used in each ICAL
standard.
3. Verify that the RRF, RRF, and %RSD for each target analyte and DMC are reported on Form
6A-OR. Recalculate the RRFs, RRFs and %RSD for at least one target analyte and DMC
associated with each internal standard, and verify that the recalculated values agree with the
laboratory reported values on Form 6A-OR.
4. Verify that the RRF is > Minimum RRF value in Table 4 for each target analyte and DMC.
5. Verify that the %RSD is < Maximum %RSD value in Table 4 for each target analyte and DMC.
October 2013 23
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Organic Data Review Trace VOA
NOTE: For data obtained from the CLP, information regarding non-compliant ICALs can be
obtained from the NFG reports and may be used as part of the evaluation process.
E. Action
1. If the ICAL is not performed at the specified frequency and sequence, qualify detects and
non-detects in the associated samples as unusable (R).
2. If the ICAL is not performed at the specified concentrations, qualify detects in the associated
samples as estimated (J) and non-detects in the associated samples as estimated (UJ).
3. If errors are detected in the calculations of the RRFs, RRF or %RSD, perform a more
comprehensive recalculation.
4. If the RRF is < Minimum RRF value in Table 4 for any target analyte, use professional judgment to
qualify detects in the associated samples as estimated high (J+) or unusable (R) and non-detects in
the associated samples as unusable (R).
5. If the RRF is > Minimum RRF value in Table 4 for any target analyte, detects and non-detects in the
associated samples should not be qualified.
6. If the %RSD is > Maximum %RSD value in Table 4 for any target analyte, qualify detects in the
associated samples as estimated (J). Use professional judgment to qualify non-detects in the
associated samples.
7. If the %RSD is < Maximum %RSD for any target analyte in Table 4, detects and non-detects in the
associated samples should not be qualified.
8. No qualification of the data is necessary based on the DMC RRF, RRF, and %RSD data alone. Use
professional judgment to evaluate the DMC RRF, RRF, and %RSD data in conjunction with the
DMC recoveries to determine the need for data qualification.
9. Based on the project-specific Data Quality Objectives (DQOs), a more in-depth review may be
considered using the following guidelines:
a. If the %RSD criteria of any target analyte 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.
b. If the high-point of the ICAL curve is outside of the %RSD criteria (e.g., due to saturation):
i. Qualify detects in the associated samples with analyte concentrations greater than the
high-point concentration as estimated (J).
ii. Detects in the associated samples with analyte concentrations within the calibration range
should not be qualified.
iii. Non-detects in the associated samples should not be qualified.
c. If the low-point of the ICAL curve is outside of the %RSD criteria:
i. Qualify detects in the associated samples with analyte concentrations in the non-linear
range as estimated (J).
ii. Detects in the associated samples with analyte concentrations within the calibration range
should not be qualified.
iii. 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.
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10. If the laboratory failed to provide adequate calibration information, notify the Regional CLP PO,
who may contact the laboratory to request the necessary information. If the information is not
available, use professional judgment to assess the data.
11. Annotate the potential effects on the reported data due to exceeding the ICAL criteria in the Data
Review Narrative.
12. If the ICAL criteria are grossly exceeded, note this for laboratory CLP PO action.
Table 4. RRF, %RSD and %D Acceptance Criteria in Initial Calibration and CCV for Trace
Volatile Analysis
Analyte
Dichlorodifluoromethane
Chloromethane
Vinyl chloride
Bromomethane
Chloroethane
Trichlorofluoromethane
1 , 1 -Dichloroethene
1 , 1 ,2-Trichloro- 1 ,2,2-trifluoroethane
Acetone
Carbon disulfide
Methyl acetate
Methylene chloride
trans-l,2-Dichloroethene
Methyl tert-butyl ether
1 , 1 -Dichloroethane
cis-l,2-Dichloroethene
2-Butanone
Bromochloromethane
Chloroform
1,1,1 -Trichloroethane
Cyclohexane
Carbon tetrachloride
Minimum
RRF
0.010
0.010
0.010
0.010
0.010
0.010
0.020
0.010
0.010
0.010
0.010
0.010
0.070
0.010
0.100
0.100
0.010
0.020
0.040
0.050
0.100
0.020
Maximum
%RSD
30.0
30.0
30.0
40.0
30.0
30.0
30.0
30.0
40.0
20.0
40.0
40.0
20.0
30.0
20.0
20.0
40.0
20.0
20.0
30.0
30.0
20.0
Opening
Maximum
%ol
±40.0
±30.0
±30.0
±30.0
±30.0
±30.0
±20.0
±30.0
±40.0
±25.0
±40.0
±30.0
±20.0
±30.0
±20.0
±20.0
±40.0
±20.0
±20.0
±20.0
±25.0
±25.0
Closing
Maximum
%D
±50.0
±50.0
±50.0
±50.0
±50.0
±50.0
±25.0
±50.0
±50.0
±25.0
±50.0
±50.0
±25.0
±50.0
±25.0
±25.0
±50.0
±25.0
±25.0
±25.0
±50.0
±50.0
October 2013
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Analyte
Benzene
1 ,2-Dichloroethane
Trichloroethene
Methylcyclohexane
1 ,2-Dichloropropane
Bromodichloromethane
cis- 1 ,3 -Dichloropropene
4-Methyl -2 -pentanone
Toluene
trans -1,3 -Dichloropropene
1 , 1 ,2-Trichloroethane
Tetrachloroethene
2-Hexanone
Dibromochloromethane
1 ,2-Dibromoethane
Chlorobenzene
Ethylbenzene
m,p-Xylene
o-Xylene
Styrene
Bromoform
Isopropylbenzene
1 , 1 ,2,2-Tetrachloroethane
1 , 3 -Dichlorobenzene
1 ,4-Dichlorobenzene
1 ,2-Dichlorobenzene
1 ,2-Dibromo-3 -chloropropane
1 ,2,4-Trichlorobenzene
Minimum
RRF
0.300
0.010
0.100
0.200
0.100
0.090
0.100
0.010
0.400
0.010
0.040
0.100
0.010
0.050
0.010
0.400
0.500
0.200
0.300
0.200
0.010
0.700
0.050
0.500
0.700
0.400
0.010
0.300
Maximum
%RSD
20.0
20.0
20.0
30.0
20.0
20.0
20.0
30.0
20.0
30.0
20.0
20.0
40.0
20.0
20.0
20.0
20.0
20.0
30.0
30.0
30.0
30.0
20.0
20.0
20.0
20.0
40.0
30.0
Opening
Maximum
%ol
±20.0
±25.0
±20.0
±25.0
±20.0
±20.0
±20.0
±30.0
±20.0
±20.0
±20.0
±20.0
±40.0
±20.0
±20.0
±20.0
±20.0
±20.0
±20.0
±20.0
±30.0
±25.0
±25.0
±20.0
±20.0
±20.0
±40.0
±30.0
Closing
Maximum
%D
±25.0
±50.0
±25.0
±50.0
±25.0
±25.0
±25.0
±50.0
±25.0
±25.0
±25.0
±25.0
±50.0
±25.0
±25.0
±25.0
±25.0
±25.0
±25.0
±25.0
±50.0
±25.0
±25.0
±25.0
±25.0
±25.0
±50.0
±50.0
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Analyte
1,2,3-Trichlorobenzene
Minimum
RRF
0.200
Maximum
%RSD
30.0
Opening
Maximum
%ol
±40.0
Closing
Maximum
%D
±50.0
Deuterated Monitoring Compound
Vinyl chloride-d3
Chloroethane-d5
1 , 1 -Dichloroethene-d2
2-Butanone-d5
Chloroform-d
1 ,2-Dichloroethane-d4
Benzene -d6
1 ,2-Dichloropropane-d6
Toluene-d8
trans -1,3 -Dichloropropene-d4
1,1,2,2- Tetrachloroethane-d2
l,2-Dichlorobenzene-d4
0.010
0.010
0.010
0.010
0.010
0.010
0.030
0.100
0.200
0.010
0.010
0.060
30.0
30.0
30.0
40.0
20.0
20.0
20.0
20.0
20.0
30.0
20.0
20.0
±30.0
±30.0
±25.0
±40.0
±20.0
±25.0
±20.0
±20.0
±20.0
±25.0
±25.0
±20.0
±50.0
±50.0
±25.0
±50.0
±25.0
±25.0
±25.0
±25.0
±25.0
±25.0
±25.0
±25.0
1 If a closing CCV is acting as an opening CCV, all target analytes must meet the requirements for an
opening CCV.
Table 5. Initial Calibration Actions for Trace Volatile Analysis
Criteria
Initial Calibration not performed at
specified frequency and sequence
Initial Calibration not performed at the
specified concentrations
RRF < Minimum RRF in Table 4 for
target analyte
RRF > Minimum RRF in Table 4 for
target analyte
%RSD > Maximum %RSD in Table 4
for target analyte
%RSD < Maximum %RSD in Table 4
for target analyte
Action
Detect
Use professional
judgment
R
J
Use professional
judgment
J+orR
No qualification
J
No qualification
Non-detect
Use professional
judgment
R
UJ
R
No qualification
Use professional
judgment
No qualification
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Organic Data Review Trace VOA
IV. Continuing Calibration Verification
A. Review Items
Form 7A-OR, quantitation reports, and chromatograms.
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. Criteria
1. The calibration for each GC/MS system used for analysis must be verified at the beginning and end
of every 12-hour period of operation. The 12-hour period begins with the injection of BFB,
followed by the injection of the opening CCV solution. After the injection of all samples and
required blanks, and before the end of the 12-hour period, injection of the closing CCV is required.
The closing CCV used to bracket the end of a 12-hour analytical sequence may be used as the
opening CCV for a new 12-hour analytical sequence, provided that all technical acceptance criteria
for an opening CCV are met.
2. The CCV standards must contain all required target analytes and DMCs at the mid-point
concentration (CSS) of the ICAL.
3. For an opening or a closing CCV, the RRF for each target analyte and DMC must be > the
Minimum RRF value in Table 4.
4. The Percent Difference (%D) between the ICAL RRF and the opening CCV RRF must be within
the Opening Maximum %D limits in Table 4 for each target analyte and DMC.
5. For a closing CCV, the %D between the ICAL RRF and the CCV RRF must be within Closing
Maximum %D limits in Table 4 for each target analyte and DMC.
D. Evaluation
1. Verify that the CCV is analyzed at the specified frequency and sequence and that the CCV is
associated to the correct ICAL. Also verify that the correct ICAL is represented in the data package
and meets SOW criteria, as described in Section III.
2. Verify that the mid-point standard CSS from the ICAL is used as an opening or closing CCV.
3. Verify that the RRF and %D for each target analyte and DMC are reported on Form 7A-OR.
Recalculate RRF and %D for at least one target analyte and DMC associated with each internal
standard and verify that the recalculated values agree with the laboratory reported values on Form
7A-OR
4. For an opening or a closing CCV, verify that the RRFs for all target analytes and DMCs are > the
Minimum RRF values in Table 4.
5. For an opening CCV, verify that the %Ds are within the Opening Maximum %D limits in Table 4
for the target analytes and DMCs.
6. For a closing CCV, verify that the %Ds are within the Closing Maximum %D limits in Table 4 for
the target analytes and DMCs.
NOTE: For data obtained from the CLP, information regarding non-compliant CCVs can be
obtained from the NFG reports and may be used as part of the evaluation process.
E. Action
1. If the CCV is not performed at the specified frequency, qualify detects and non-detects as unusable
(R). Contact the Regional CLP PO to request that the laboratory repeat the analysis, if holding
times have not expired and there are remaining sample vials. Preanalysis is not possible, carefully
October 2013 28
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Organic Data Review Trace VOA
evaluate all other available information, including the quality of analyte peak shapes and mass
spectral matches, stability of internal standard Retention Times (RTs) and areas in each affected
sample, 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).
2. If the CCV is not performed at the specified concentration, use professional judgment to qualify
detects and non-detects. Special consideration should be given to sample results at the opposite
extreme of the calibration range if this defect is noted.
3. If errors are detected in the calculations of either the RRF or the %D, perform a more
comprehensive recalculation.
4. For an opening or a closing CCV, if the RRF is < the Minimum RRF value in Table 4 for any target
analyte, carefully evaluate the qualitative data associated with positively identified analytes and use
professional judgment to qualify detects as estimated (J) or unusable (R) and qualify non-detects as
unusable (R).
5. For an opening or a closing CCV, if the RRF is > the Minimum RRF value in Table 4 for any target
analyte, detects and non-detects should not be qualified.
a. Take special note of any extreme deviation in RRF and evaluate RT data peak shapes and areas
for insconsistencies that may indicate a chromatographic co-elution. If this is suspected, the
contaminant may also be present in samples and blanks. Use professional judgment to qualify
affected data appropriately.
6. For an opening CCV, if the %D is outside the Opening Maximum %D limits in Table 4 for any
target analyte, qualify detects as estimated (J) and non-detects as estimated (UJ).
7. For a closing CCV, if the %D is outside the Closing Maximum %D limits in Table 4 for any target
analyte, qualify detects as estimated (J) and non-detects as estimated (UJ).
8. For an opening CCV, if the %D is within the inclusive range of the Opening Maximum %D limits
in Table 4 for any target analyte, detects and non-detects should not be qualified.
9. For a closing CCV, if the %D is within the inclusive range of the Closing Maximum %D limits in
Table 4 for any target analyte, detects and non-detects should not be qualified.
10. No qualification of the data is necessary on DMC RRF and/or %D alone. Use professional
judgment to evaluate the DMC RRF and %D data in conjunction with the DMC recoveries to
determine the need for data qualification.
11. If the laboratory has failed to provide adequate calibration information, contact the Regional CLP
PO, who may contact the laboratory and request the necessary information. If the information is
not available, use professional judgment to assess the data. Referto E.I, above, for additional steps.
12. Note the potential effects on the data due to CCV criteria exceedance in the Data Review Narrative.
13. If CCV criteria are grossly exceeded, note this for laboratory CLP PO action.
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Table 6. CCV Actions for Trace Volatile Analysis
Criteria for Opening CCV
CCV not performed at required
frequency
CCV not performed at specified
concentration
RRF < the Minimum RRF in
Table 4 for target analytes
RRF > the Minimum RRF in
Table 4 for target analytes
%D outside the Opening
Maximum %D limits in Table 4
for target analytes
%D within the inclusive Opening
Maximum %D limits in Table 4
for target analytes
Criteria for Closing CCV
CCV not performed at
required frequency
CCV not performed at
specified concentration
RRF < Minimum RRF in
Table 4 for target analytes
RRF > Minimum RRF in
Table 4 for target analytes
%D outside the Closing
Maximum %D limits in
Table 4 for target analytes
%D within the inclusive
Opening Maximum %D
limits in Table 4 for target
analytes
Action
Detect
Use
professional
judgment
R
Use
professional
judgment
Use
professional
judgment
JorR
No
qualification
J
No
qualification
Non-detect
Use
professional
judgment
R
Use
professional
judgment
R
No
qualification
UJ
No
qualification
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V. Blanks
A. Review Items
Form 1A-OR, Form 1B-OR, Form 4-OR, chromatograms, and quantitation 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. Criteria
The criteria for evaluation of blanks should apply to any blank associated with the samples (e.g.,
method blanks, storage blank, field blanks, etc.). If problems with any blank exist, all associated data
must be carefully evaluated to determine whether or not there is an inherent variability in the data or if
the problem is an isolated occurrence not affecting other data.
1. Method blank analyses must be performed at the specified frequency and sequence. A method
blank must be analyzed once every 12-hour period and prior to any sample analysis, and after all
ICAL standards or CCV. The method blank must be analyzed on each GC/MS system used for
sample analysis within an entire analytical sequence.
2. The method blank, like any other sample in the SDG, must meet the technical acceptance criteria
for sample analysis.
3. A storage blank analysis must be performed at the specified frequency and sequence. A storage
blank must be prepared upon receipt of the first samples from a SDG, and stored with the samples
until analysis. The storage blank must be analyzed once per SDG after all sample analyses within a
SDG are completed.
4. An instrument blank must be analyzed immediately after any sample that has target analytes
exceeding the calibration range or non-target compounds exceeding 100 (ig/L.
5. The concentration of a target analyte in any blanks must not exceed its Contract Required
Quantitation Limits (CRQL) (2x CRQLs for Methylene chloride, Acetone and 2-Butanone). TIC
concentration in any blanks must be < 0.5 (ig/L.
D. Evaluation
1. Verify that method blanks are analyzed at the specified frequency and sequence. The Method
Blank Summary (Form 4-OR) may be used to identify the samples associated with each method
blank.
2. Verify that a storage blank has been analyzed at the specified frequency and sequence.
3. Verify that the instrument blank analysis has been performed following any sample analysis where
a target analyte(s) is/are reported at high concentration(s).
4. Review the results of all associated blanks on the forms and raw data (chromatograms and
quantitation reports) to evaluate the presence of target analytes and non-target compounds in the
blanks.
5. Evaluate field or trip blanks in a manner similar to that used for the method blanks.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the Contract
Compliance Screening (CCS) process. Information regarding the non-compliant blank can
be obtained from the NFG reports and may be used as part of the evaluation process.
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E. Action
1. If the appropriate blanks are not analyzed at the correct frequency, use professional judgment to
determine if the associated sample data should be qualified; obtain additional information from the
laboratory, if necessary. Record the situation in the Data Review Narrative and note it for
laboratory CLP PO action.
2. 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 Quality Assurance Project Plan (QAPP). 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 having the highest concentration of a contaminant. Do not correct the results by
subtracting any blank value.
3. For any blank (including method blank), if a target analyte is detected, but is not detected in the
sample, non-detects should not be qualified.
4. For any method blank reported with results < CRQLs, report sample results that are < CRQLs at the
CRQLs and qualify as non-detect (U). For any method blank reported with results < CRQLs, use
professional judgment to qualify sample results that are > CRQLs (> 2x result in method blank for
Methylene Chloride, Acetone and 2-Butanone). Positive results in samples, especially those near
but above the CRQL, may be biased high by low level contamination in the method blank, and
should be considered as estimated (J+).
5. For any method blank reported with results > CRQLs, report sample results that are < CRQLs at the
CRQLs and qualify as non-detect (U).
6. For any method blank reported with results > CRQLs, report sample results that are > CRQLs (> 2x
result in method blank for Methylene Chloride, Acetone and 2-Butanone) but < Blank Results at
the CRQLs and qualified as non-detect (U) or as unusable (R). Use professional judgment to
qualify sample results that are > CRQLs (> 2x result in method blank for Methylene Chloride,
Acetone and 2-Butanone) and > Blank Results.
7. If an instrument blank is not analyzed following a sample analysis which contains analyte(s) at high
concentration(s) exceeding the calibration range, evaluate the analyte(s) concentration(s) in the
samples, analyzed immediately after the sample with high analyte(s) concentration(s), for
carryover. Use professional judgment to determine if instrument cross-contamination has affected
any positive target analyte identification(s). If instrument cross-contamination is suggested and
suspected of having an effect on the sample results or calibration performance, note it for
laboratory CLP PO action.
8. If any analytes are detected in the storage, field, or trip blanks, the following is recommended:
a. Review the associated method blank data to determine if the same analytes are also detected in
the method blank.
i. If the analytes are detected at comparable levels in the method blank, the source of the
contamination may be in the analytical system. Apply the recommended actions for the
method blank.
ii. If the analytes are not detected in the method blank, the source of contamination may be in
the storage area or in the field, or contamination may have occurred during sample
transport. Consider all associated samples for possible cross-contamination.
iii. For storage, field, or trip blanks, the sample result qualifications listed in Table 7 should
apply.
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9. If gross contamination exists with blank results that are > ICAL CSS concentrations, qualify detects
as unusable (R). If the contamination is suspected of having an effect on the sample results, note it
for laboratory CLP PO action.
10. For any blank (including method blank) reported with TICs (non-target compounds) concentrations
that are > 0.5 (ig/L, use professional judgment to qualify sample results.
11. 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 occurrence
can be detected when contaminants are found in the diluted sample result, but are absent in the
undiluted sample.
Table 7. Blank Actions for Trace Volatile Analysis
Blank Type
Method,
Storage,
Field, Trip,
Instrument*
Blank Result
Detect
CRQL
Gross
contamination*
TIC > 0.5(ig/L
Sample Result
Non-detect
CRQL or > 2x Blank Result
for Methylene Chloride,
Acetone and 2-Butanone
CRQL but < Blank Result
> CRQL and > Blank Result or
> 2x Blank Result for
Methylene Chloride, Acetone
and 2-Butanone
Detect
Detect
Action
No qualification
Report at CRQL and qualify
as non-detect (U)
Use professional judgment
Report at CRQL and qualify
as non-detect (U)
Report at sample result and
qualify as non-detect (U) or
unusable (R)
Use professional judgment
Report at sample result and
qualify as unusable (R)
Use professional judgment
Qualifications based on instrument blank results affect only the sample analyzed immediately after
the sample that has target analyte concentration exceeding the calibration range (ICAL CSS
concentration) or TICs concentration exceeding 100 (ig/L.
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VI. Deuterated Monitoring Compound
A. Review Items
Form 2A-OR, Form 2B-OR quantitation reports, and chromatograms.
B. Objective
The objective is to evaluate the DMC Percent Recovery (%R) to ensure that the analytical method is
efficient.
C. Criteria
1. All samples and blanks are spiked with the DMCs listed in Table 8, just prior to sample purging, to
measure the DMC %R.
2. The %R for each DMC should be calculated correctly according to the method.
3. The %R for each DMC in samples and blanks must be within the limits in Table 8.
Table 8. Trace Volatile DMCs and Recovery Limits
DMC
Vinyl chloride -d3
Chloroethane-d5
1 , 1 -Dichloroethene-d2
2-Butanone-d5
Chloroform-d
1 ,2-Dichloroethane-d4
Benzene -d6
1 ,2-Dichloropropane-d6
Toluene-d8
trans- 1 ,3 -Dichloropropene-d4
2-Hexanone-d5
1 , 1 ,2,2-Tetrachloroethane-d2
1 ,2-Dichlorobenzene-d4
Recovery Limits (%)
40-130
65-130
60-125
40-130
70-125
70-130
70-125
60-140
70-130
55-130
45-130
65-120
80-120
NOTE: The recovery limits for any of the compounds listed in Table 8 may be expanded at any
time during the period of performance if the United States Environmental Protection
Agency (EPA) determines that the limits are too restrictive.
D. Evaluation
1. Check raw data (e.g., chromatograms and quantitation reports) to verify the recoveries on the
Deuterated Monitoring Compound Recovery Form 2A-OR and Form 2B-OR.
2. Check for any calculation or transcription errors; verify that the DMC recoveries were calculated
correctly using the equation in the method and that the recalculated values agree with the laboratory
reported values on Form 2A-OR and Form 2B-OR.
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3. Whenever there are two or more analyses for a particular sample, use professional judgment to
determine which analysis has the most acceptable data to report. Considerations include, but are
not limited to:
a. DMC recovery (marginal versus gross deviation).
b. Technical holding times.
c. Comparison of the target analyte results reported in each sample analysis.
d. Other QC information, such as performance of internal standards.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the non-compliant DMC %Rs can be obtained from the
NFG reports and may be used as part of the evaluation process.
E. Action
1. If a DMC was not added to the samples and blanks or the concentrations of DMCs in the samples
and blanks are not as specified, use professional judgment to qualify detects and non-detects. The
Regional CLP PO should be contacted to arrange for reanalysis, if possible.
2. If errors are detected in the calculations of %R, perform a more comprehensive recalculation. It
may be necessary to have the laboratory resubmit the data after making corrections.
3. If any DMC %R is outside the limits (Table 8) in samples, qualify the associated analytes listed in
Table 10 considering the existence of interference in the raw data. Considerations include, but are
not limited to:
a. If the DMC %R is < 10%, qualify detects as estimated low (J-) and non-detects as unusable (R).
b. If the DMC %R is > 10% and < the lower acceptance limit, qualify detects as estimated low (J-)
and non-detects as estimated (UJ).
c. If the DMC %R is > lower acceptance limit and < upper acceptance limit, detects and
non-detects should not be qualified.
d. If the DMC %R is > upper acceptance limit, qualify detects as estimated high (J+).
Non-detects should not be qualified.
4. If any DMC %R is outside the limits (Table 8) in a blank, special consideration should be taken to
evaluate the validity of 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.
For example, if one or more samples in the analytical sequence show acceptable DMC %Rs, the
blank problem may be considered as an isolated occurrence. However, even if this judgment
allows some use of the affected data, note analytical problems for laboratory CLP PO action.
Table 9. DMC Recovery Actions for Trace Volatile Analysis
Criteria
%R<10%
10% < %R < Lower Acceptance Limit
Lower Acceptance Limit < %R < Upper Acceptance
Limit
%R > Upper Acceptance Limit
Action
Detect
J-
J-
No qualification
J+
Non-detect
R
UJ
No qualification
No qualification
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Table 10. Trace Volatile DMCs and the Associated Target Analytes
Chloroethane-d5 (DMC)
Dichlorodifluoromethane
Chloromethane
Bromomethane
Chloroethane
Carbon disulfide
trans -1,3 -Dichloropropene-d4
(DMC)
cis- 1 ,3 -Dichloropropene
trans -1,3 -Dichloropropene
1 , 1 ,2-Trichloroethane
2-Butanone-d5 (DMC)
Acetone
2-Butanone
Vinyl chloride-d3 (DMC)
Vinyl chloride
l,2-Dichloroethane-d4 (DMC)
Trichlorofluoromethane
1 , 1 ,2-Trichloro- 1 ,2,2-trifluoroethane
Methyl acetate
Methylene chloride
Methyl-tert-butyl ether
1,1,1 -Trichloroethane
Carbon tetrachloride
1 ,2-Dibromoethane
1 ,2-Dichloroethane
l,2-Dichloropropane-d6 (DMC)
Cyclohexane
Methylcyclohexane
1 ,2-Dichloropropane
Bromodichloromethane
Chloroform-d (DMC)
1 , 1 -Dichloroethane
Bromochloromethane
Chloroform
Dibromochloromethane
Bromoform
1 , 1 -Dichloroethene-d2 (DMC)
1 , 1 -Dichloroethene
trans-l,2-Dichloroethene
cis-l,2-Dichloroethene
Benzene-d6 (DMC)
Benzene
l,2-Dichlorobenzene-d4 (DMC)
Chlorobenzene
1 ,3 -Dichlorobenzene
1 ,4-Dichlorobenzene
1 ,2-Dichlorobenzene
1 ,2,4-Trichlorobenzene
1 ,2,3 -Trichlorobenzene
2-Hexanone-d5 (DMC)
4-Methyl-2-pentanone
2-Hexanone
1 , 1 ,2,2-Tetrachloroethane-d2
(DMC)
1 , 1 ,2,2,-Tetrachlororethane
1 ,2-Dibromo-3 -chloropropane
Toluene-d8 (DMC)
Trichloroethene
Toluene
Tetrachloroethene
Ethylbenzene
o-Xylene
m,p-Xylene
Styrene
Isopropylbenzene
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VII. Matrix Spike/Matrix Spike Duplicate
A. Review Items
Cover Page, Form 3A-OR, chromatograms, and quantitation reports.
B. Objective
The objective of the 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. Criteria
1. If requested, MS/MSD samples shall be prepared and analyzed at the specified frequency. One pair
of MS/MSD should be analyzed per matrix or per SDG.
NOTE: Data for MS and MSDs will not be present unless requested by the Region.
2. Samples identified as field blanks or Performance Evaluation (PE) samples cannot be used for
spiked sample analysis.
3. The MS/MSD %R and the Relative Percent Difference (RPD) between MS and MSD results
should be calculated according to the method.
4. The MS/MSD %R and RPD should be within the acceptance limits in Table 11.
D. Evaluation
1. Verify that the requested MS/MSD samples were analyzed at the required frequency.
2. Verify that a field blank or PE sample was not used for MS/MSD analysis.
3. Verify that the recalculated MS/MSD %R and RPD values agree with the laboratory reported
values on Form 3A-OR.
4. Inspect the MS/MSD %R and RPD on Form 3 A-OR and verify that they are within the limits listed
in Table 11.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the non-compliant MS/MSD %Rs or RPDs can be
obtained from the NFG reports and may be used as part of the evaluation process.
E. Action
1. If requested MS/MSD samples are not analyzed at the specified frequency, use professional
judgment to determine the impact on sample data, if any; obtain additional information from the
laboratory, if necessary. Record the situation in the Data Review Narrative and note it for
laboratory CLP PO action. It is not likely that data qualification will be warranted if the frequency
requirement is not met. Carefully consider all factors, known and unknown, about method
performance on the matrix at hand, in lieu of MS/MSD data.
2. If a field blank or PE sample was used for the MS/MSD analysis, note this for laboratory CLP PO
action. All of the other QC data must then be carefully checked. Use professional judgment when
evaluating the data.
3. If the MS/MSD %R or RPD is outside the acceptance limits in Table 11, qualify the detects and
non-detects in the original sample to include consideration of the existence of interference in the
raw data. Considerations include, but are not limited to:
a. If the MS/MSD %R is < 20%, qualify detects as estimated (J) and non-detects as unusable (R).
b. If the MS/MSD %R is > 20% and < the lower acceptance limit, qualify detects as estimated (J)
and non-detects as estimated (UJ).
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c. If MS/MSD %R or RPD is > lower acceptance limit and < upper acceptance limit, detects and
non-detects should not be qualified.
d. If the MS/MSD%R or RPD is > the upper acceptance limit, qualify detects as estimated (J).
Non-detects should not be qualified.
Table 11. MS/MSD %R and RPD Limits for Trace Volatile Analysis
Analyte
1 , 1 -Dichloroethene
Benzene
Trichloroethene
Toluene
Chlorobenzene
%R
61 - 145
76 - 127
71 - 120
76 - 125
75 - 130
RPD
0-14
0-11
0-14
0-13
0-13
Table 12. MS/MSD Actions for Trace Volatile Analysis
Criteria
%R < 20%
20% < %R< Lower Acceptance Limit
Lower Acceptance Limit < %R or RPD < Upper
Acceptance Limit
%R or RPD > Upper Acceptance Limit
Action
Detect
J
J
No qualification
J
Non-detect
R
UJ
No qualification
No qualification
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VIII. Internal Standard
A. Review Items
Form 8A-OR, quantitation reports, and chromatograms.
B. Objective
The objective is to evaluate the internal standard performance to ensure that GC/MS sensitivity and
response are stable during each analysis.
C. Criteria
1. The internal standard solution must be added to all samples and blanks at the specified
concentration. The internal standard solution must contain all internal standard compounds
specified in the method.
2. The area response of each internal standard compound in all samples and blanks must be within the
inclusive ranges of 50.0 - 200% of the area response of the same internal standard compound from
the associated opening CCV or the mid-point standard CSS from the associated ICAL.
3. The RT of the internal standard compound in the sample or blank must not vary more than ±10.0
seconds from the RT of the same internal standard compound in the associated opening CCV or
mid-point standard CSS from the associated ICAL.
D. Evaluation
1. Verify that all required internal standard compounds were added to sample and blank analyses at
the specified concentrations.
2. Check the raw data (e.g., chromatograms and quantitation reports) to verify that the RTs and area
response of each internal standard compound in a sample or blank are reported on the Internal
Standard Area and Retention Time Summary Form 8A-OR.
3. Verify that the RTs and area responses for all internal standard compounds are within the specified
criteria. If internal standard RTs are significantly different from the associated CCV or ICAL
midpoint, i.e., more than 10 seconds, the internal standard peak may have been misidentified, but
most likely a change in the chromatographic system should be suspected. This could be an
improper desorb/injection cycle, a leak in the purge/trap/GC system, or the effect of a highly
contaminated matrix. Normally, the area counts will also suffer in this situation, but even if they
appear unaffected, both quantitative and qualitative results should be considered highly suspect.
4. If there is a reanalysis for a particular sample, determine which analysis is the best data to report.
Considerations include, but are not limited to:
a. Magnitude and direction of the internal standard area response shift.
b. Magnitude and direction of the internal standard RT shift.
c. Technical holding times.
d. Comparison of the values of the target analytes reported in each method.
e. Other QC information.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the non-compliant internal standard area response or RT
can be obtained from the NFG reports and may be used as part of the evaluation process.
E. Action
NOTE: Apply the action to the target analytes in the samples or blanks that are associated to the
non-compliant internal standard compound in Table 13. The internal standard and the
associated target analytes are in Exhibit D Trace VOA Section 17 Table 9 of the SOW.
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1. If the required internal standard compounds were not added to a sample or blank, qualify detects
and non-detects as unusable (R).
2. If the required internal standard compound was not analyzed at the specified concentration in a
sample or blank, use professional judgment to qualify detects and non-detects.
3. If the area response of an internal standard compound in a sample or blank is < 20% of the area
response of the same internal standard compound in the associated opening CCV or mid-point
standard CSS from the associated ICAL, qualify detects as estimated high (J+) and non-detects as
unusable (R).
4. If the area response of an internal standard compound in a sample or blank is > 20 % and < 50% of
the area response of the same internal standard compound in the associated opening CCV or
mid-point standard CSS from the associated ICAL, qualify detects as estimated high (J+) and
non-detects as estimated (UJ).
5. If the area response of an internal standard compound in a sample or blank is within the inclusive
range of 50-200% of the area response of the same internal standard compound in the associated
opening CCV or mid-point standard CSS from the associated ICAL, detects and non-detects should
not be qualified.
6. If the area response of an internal standard compound in a sample or blank is > 200% of the area
response of the same internal standard compound in the associated opening CCV or mid-point
standard CSS from the associated ICAL, qualify detects as estimated low (J-). Non-detects should
not be qualified.
7. If the RT shift between sample/blank and the associated opening CCV or mid-point standard CSS
from the associated ICAL of an internal standard compound is > 10.0 seconds, qualify detects and
non-detects as unusable (R). The Regional CLP PO should be contacted to arrange for reanalysis.
8. If the RT shift between sample/blank and the associated opening CCV or mid-point standard CSS
from the associated ICAL of an internal standard compound is < 10.0 seconds, detects and
non-detects should not be qualified.
9. If the internal standard performance criteria are grossly exceeded, annotate the potential effects on
the data in the Data Review Narrative and note it for laboratory CLP PO action.
Table 13. Internal Standard Actions for Trace Volatile Analysis
Criteria
Area response < 20% of the opening CCV or mid-point
standard CSS from initial calibration
20% < Area response < 50% of the opening CCV or
mid-point standard CSS from initial calibration
50% < Area response < 200% of the opening CCV or
mid-point standard CSS from initial calibration
Area response > 200% of the opening CCV or mid-point
standard CSS from initial calibration
RT shift between sample/blank and opening CCV or
mid-point standard CSS from initial calibration > 10.0
seconds
RT shift between sample/blank and opening CCV or
mid-point standard CSS from initial calibration < 10.0
seconds
Action
Detect
J+
J+
No qualification
J-
R
No qualification
Non-detect
R
UJ
No qualification
No qualification
R
No qualification
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IX. Target Analyte Identification
A. Review Items
Form 1A-OR, quantitation reports, mass spectra, and chromatograms.
B. Objective
The objective is to provide acceptable GC/MS qualitative analysis to minimize the number of erroneous
analyte identifications.
C. Criteria
1. The mass spectrum of the analyte from the sample analysis must match that of the same analyte in
the associated opening CCV or mid-point standard CSS from the associated ICAL according to the
following criteria:
a. All ions present in the calibration standard mass spectrum must be present in the sample
spectrum at a relative intensity > 10%.
b. The relative intensities of these ions must agree within ±20% between the standard and sample
spectra (e.g., for an ion with an abundance of 50% in the standard spectrum, the corresponding
sample ion abundance must be between 30-70%).
c. Ions present at > 10% in the sample mass spectrum, but not present in the standard spectrum,
must be evaluated by a reviewer experienced in mass spectral interpretation.
2. The Relative Retention Time (RRT) for a positively identified target analyte must be within ±0.06
RRT units of the RRT for the same analyte in the associated opening CCV or mid-point standard
CSS from the associated ICAL.
D. Evaluation
1. Verify that the positively identified target analyte mass spectrum meets the specified criteria. If
not, examine the sample target analyte spectra for the presence of interference at one or more mass
fragment peaks. Although the presence of a co-eluting interferent may preclude positive
identification of the analyte, the presumptive evidence of its presence may be useful information to
include in the Data Review Narrative.
2. Verify that the RRT of the positively identified target analyte is within ±0.06 RRT units of the RRT
for the same analyte in the associated opening CCV or mid-point standard CSS from the associated
ICAL.
3. Be aware of situations when sample carryover is a possibility and use professional judgment to
determine if instrument cross-contamination has affected any positive analyte identification. An
instrument blank must be analyzed after a sample containing target analytes with concentrations
exceeding the ICAL range (20 ug/L for non-ketones, 200 ug/L for ketones), non-target compounds
at concentrations > 100 ug/L, or saturated ions from an analyte (excluding the analyte peaks in the
solvent front).
4. Verify that peaks are correctly identified as target analytes, TICs, DMCs, or internal standards on
the chromatogram for samples and blanks.
5. Verify that there is no erroneous analyte identification, either false positive or false negative, for
each target analyte. The positively identified target analytes can be more easily detected for false
positives than false negatives. More information is available for false positives due to the
requirement for submittal of data supporting positive identifications. Non-detected target analytes,
on the other hand, are more difficult to assess. One example of the detection of false negatives is
reporting a target analyte as a TIC.
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NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the non-compliant TICs can be obtained from the CCS
report and may be used as part of the evaluation process.
NOTE: A target analyte reported as a false negative may not have the best match in a TIC search of
a contaminated sample, but its mass spectrum may be present under that of a reported TIC.
E. Action
1. If the positively identified target analyte mass spectrum does not meet the specified criteria, qualify
detect as unusable (R) or report the result at CRQL and qualify as non-detect (U).
2. If the RRT for a positively identified target analyte is outside the specified RRT windows, qualify
detect as unusable (R) or report the result at CRQL and qualify as non-detect (U).
3. If it is determined that cross-contamination has occurred, use professional judgment to qualify
detects. Annotate any changes made to the reported analytes due to either false positive or negative
identifications, or concerns regarding target analyte identifications, in the Data Review Narrative.
Note the necessity for numerous or significant changes for laboratory CLP PO action.
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X. Target Analyte Quantitation and Reported Contract Required Quantitation Limit
A. Review Items
Form 1A-OR, sample preparation sheets, SDG Narrative, quantitation reports, and chromatograms.
B. Objective
The objective is to ensure that the reported results and CRQLs for target analytes are accurate.
C. Criteria
1. Target analyte results and sample specific CRQLs must be calculated according to the correct
equations.
2. Target analyte RRF must be calculated using the correct associated internal standard, as listed in
the method. Quantitation must be based on the quantitation ion (m/z) specified in the method for
both the internal standards and target analytes. Target analyte result must be calculated using the
RRF from the associated ICAL.
D. Evaluation
1. Verify that the results for all positively identified analytes are calculated and reported by the
laboratory.
2. Verify that the CRQLs are calculated for the non-detects and reported accordingly.
3. Verify that the correct internal standard, quantitation ion, and RRF are used to calculate the
reported results.
4. Verify that the same internal standard, quantitation ion, and RRF are used consistently.
5. Verify that the sample-specific CRQLs have been calculated and adjusted to reflect original sample
mass/volume and any applicable dilutions.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the non-compliant results or CRQLs can be obtained from
the CCS report and may be used as part of the evaluation process.
E. Action
1. If any discrepancies are found, contact the Regional CLP PO, who may contact the laboratory to
obtain additional information that could resolve any differences. If a discrepancy remains
unresolved, use professional judgment to decide which value is the most accurate and to determine
whether qualification of the data is warranted. Annotate the reasons for any data qualification in
the Data Review Narrative.
2. If errors are detected in results and CRQLs calculations, perform a more comprehensive
recalculation.
3. If sample results are < CRQLs and > MDLs, qualify as estimated (J).
4. Note numerous or significant failures to accurately quantify the target analytes, or to properly
evaluate and adjust CRQLs, for laboratory CLP PO action.
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XI. Tentatively Identified Compounds
A. Review Items
Form 1B-OR, chromatograms, library search printouts, and spectra for the TIC candidates.
B. Objective
The objective is to provide tentative identifications to chromatographic peaks that are not identified as
target analytes, DMCs, or internal standards.
C. Criteria
For each sample, the laboratory must conduct a mass spectral search of the National Institute of
Standards and Technology/U.S. Environmental Protection Agency/National Institutes of Heath
[(NIST/EPA/NH) 2011 release or later], and/or Wiley (2011 release or later), or equivalent mass
spectral library, and report the possible identity for up to 30 of the largest peaks that are not DMCs,
internal standards, or target analytes. The peak for a TIC should have an area or height > 10% of the
area or height of the nearest internal standard. The estimated concentration for a TIC is calculated
similarly to that for a target analyte, using total ion areas for the TIC and the internal standard, and
assuming a RRF of 1.0.
1. Guidelines for tentative identification are as follows:
a. Major ions (> 10% Relative Intensity) in the reference spectrum should be present in the
sample spectrum.
b. The relative intensities of the major ions should agree within ±20% between the sample and the
reference spectra.
c. Molecular ions present in the reference spectrum should be present in the sample spectrum.
d. Non-target compounds receiving a library search match of 85% or higher are considered a
"likely match." The compound should be reported unless the mass spectral interpretation
specialist feels there is evidence not to report the compound as identified by the library search
program. The laboratory should include the justification for not reporting a compound as listed
by the search program in the SDG Narrative.
e. If the library search produces more than one compound > 85%, the compound with the highest
percent match (report first compound if percent match is the same for two or more compounds)
should be reported, unless the mass spectral interpretation specialist feels that the highest
match compound should not be reported, or another compound with a lower match should be
reported. The laboratory should include the justification for not reporting the compound with
the highest spectral match within the SDG Narrative. DMCs, internal standards, and target
analytes should not be reported as TICs.
f If the library search produces a series of obvious isomer compounds with library search
matches > 85%, the compound with the highest library search percent match (or the first
compound if the library search matches are the same) should be reported. The laboratory
should note in the SDG Narrative that the exact isomer configuration, as reported, may not be
accurate.
g. If the library search produces no match > 85%, and in the technical judgment of the mass
spectral interpretation specialist, no valid tentative identification can be made, the compound
should be reported as unknown. The mass spectral specialist should give additional
classification of the unknown compound, if possible (e.g., unknown aromatic, unknown
hydrocarbon, unknown acid type, unknown chlorinated compound). If probable molecular
weights can be distinguished, they should be included.
h. The Chemical Abstracts Service (CAS) registry number is the unique identifier for each
chemical compound. As the rules of chemical nomenclature have changed overtime, each
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chemical substance is liable to have several names or synonyms [i.e., trade or brand name(s);
generic or common name(s); trivial or systematic; or International Union of Pure and Applied
Chemistry (IUPAC) name(s)]. Whether synonyms or other names are created for this
compound, the CAS registry number will remain unchanged. The CAS registry number is
simply an identifier which has no structural significance. Regardless of RTs, if the library
search produces two or more compounds at or above 85% with the same CAS Number, the
compound with the highest percent match (report first compound if the percent match is the
same for two or more compounds) should be reported unless the mass spectral interpretation
specialist feels there is just evidence not to report the compound with the highest match.
i. If the library search produces only one and the same compound (i.e., the same CAS registry
number) with the match at or above 85% at two different RTs, the compound having the
highest percent match should be reported as TIC and the other one could be reported as
unknown. If both TICs have the same percent match for the same compound, one of the TICs
could be reported as unknown. Such justifications should be included in the SDG Narrative.
j. Alkanes are not to be reported as TICs on Form 1B-OR. An alkane is defined as any
hydrocarbon with the generic formula CnH2n+2 containing only C-H and C-C single bonds.
When the preceding alkanes are tentatively identified, the concentration(s) should be estimated
and the analytes reported as alkanes by class (i.e., straight-chain, branched, cyclic, as a series,
or as applicable) in the SDG Narrative. Total alkanes concentration should be reported on
Form 1B-OR.
D. Evaluation
1. Verify that the laboratory has generated a library search for all required peaks in the
chromatograms for samples and blanks.
2. Verify that TIC peaks present in samples are not found in blanks. When a low-level, non-target
compound that is a common artifact or laboratory contaminant is detected in a sample, a thorough
check of blank chromatograms may require looking for peaks which are < 10% of the internal
standard height, but present in the blank chromatogram at a similar RRT.
3. Verify that mass spectra for all reported TICs are present for every sample and blank.
4. Review ions present in the sample spectrum, but not in the reference spectrum, for possible
background contamination, interference, or presence of coeluting compounds.
5. Review ions present in the reference spectrum, but not in the sample spectrum, for possible
subtraction from the sample spectrum because of background contamination or coeluting
compounds. Data system library reduction programs can sometimes create these discrepancies.
6. Consider all reasonable choices since TIC library searches often yield several candidate
compounds having a close matching score.
7. Be aware of common laboratory artifacts/contaminants and their sources (e.g., Aldol condensation
products, solvent preservatives, and reagent contaminants). These may be present in blanks and not
reported as sample TICs, such as:
a. Common laboratory contaminants include CO2 (m/z 44), siloxanes (m/z 73), diethyl ether,
hexane, certain freons, and phthalates at levels < 100 (ig/L.
b. Solvent preservatives include cyclohexene (a methylene chloride preservative). Related
by-products include cyclohexanone, cyclohexenone, cyclohexanol, cyclohexenol,
chlorocyclohexene, and chlorocyclohexanol.
c. Aldol condensation reaction products of acetone include: 4-hydroxy-4-methyl-2-pentanone,
4-methyl-2-penten-2-one, and 5,5-dimethyl-2(5H)-furanone.
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8. A target analyte may be identified by non-target library search procedures, even though it is not
identified as a target analyte (false negative). If the total area quantitation method is used, request
that the laboratory recalculate the result using the proper quantitation ion and RRF.
a. A non-target compound may be incorrectly identified by the instrument's target analyte data
processor as a target analyte (false positive). When this happens, the non-target library search
procedure will not detect the false positive as a TIC. In this case, request that the laboratory
properly identify the analyte as a TIC and recalculate the result using the total area quantitation
method and a RRF of 1.0.
b. Evaluate other sample chromatograms and check for both false negatives and false positives to
determine if the occurrence is isolated or systematic.
9. Verify that the TIC concentration is calculated using an RRF of 1.0.
E. Action
1. If the library search match for a TIC is > 85%, qualify the TIC as tentatively identified with
estimated concentration (NJ).
2. If the library search match for a TIC is < 85%, qualify the TIC as unknown with estimated
concentration (J).
3. General actions related to the review of TIC results are as follows:
a. If it is determined that a tentative identification of a non-target compound is unacceptable,
change the tentative identification to "unknown" or another appropriate identification, and
qualify the result as estimated (J).
b. If a library search or proper calculation was not performed for all contractually-required peaks,
the Regional CLP PO may request the data from the laboratory.
c. Use professional judgment to determine whether a library search result for a TIC represents a
reasonable identification. If there is more than one possible match, report the result as "either
compound X or compound Y." If there is a lack of isomer specificity, change the TIC result to
a non-specific isomer result (e.g., 1,3,5-trimethyl benzene to trimethyl benzene isomer) or to a
compound class (e.g., 2-methyl, 3-ethyl benzene to a substituted aromatic compound).
d. Other Case factors may influence TIC judgments. If a sample TIC match is poor, but other
samples have a TIC with a valid library match, similar RRT, and the same ions, infer
identification information from the other sample TIC results.
4. Annotate any changes made to the reported data or any concerns regarding TIC identifications in
the Data Review Narrative.
5. Note any failure to properly evaluate and report TICs for laboratory CLP PO action.
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XII. System Performance
A. Review Items
Form 8A-OR and chromatograms.
B. Objective
The objective is to ensure that the system is stable during the analytical sequence to produce quality
data.
C. Criteria
There are no specific criteria for system performance.
D. Evaluation
1. Abrupt discrete shifts in the Reconstructed Ion Chromatogram (RIC) baseline may indicate a
change in the instrument's sensitivity or in the zero setting. A baseline "shift" could indicate a
decrease in sensitivity in the instrument or an increase in the instrument zero, possibly causing
target compounds at or near the detection limit to miss detection. A baseline "rise" could indicate
problems such as a change in the instrument zero, a leak, or degradation of the column.
2. Poor chromatographic performance affects both qualitative and quantitative results. Indications of
substandard performance include:
a. High RIC background levels or shifts in Absolute RTs of internal standards.
b. Excessive baseline rise at elevated temperature.
c. Extraneous peaks.
d. Loss of resolution.
e. Peak tailing or peak splitting that may result in inaccurate quantitation.
3. A drift in instrument sensitivity may occur during the 12-hour period and may be an indication of
possible internal standard spiking problems. This could be discerned by examination of the internal
standard area on Form 8A-OR for trends such as a continuous or near-continuous increase or
decrease in the internal standard area over time.
E. Action
1. Use professional judgment to qualify the data if it is determined that system performance has
degraded during sample analyses.
2. Note any degradation of system performance which significantly affected the data for laboratory
CLP PO action.
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XIII. Regional Quality Assurance and Quality Control
A. Review Items
Form 1A, chromatograms, TR/COC documentation, quantitation reports, and other raw data from
QA/QC samples.
B. Objective
The objective is to use results from the analysis of the Regional QA/QC samples including field
duplicates, PE samples, blind spikes, and blind blanks to determine the validity of the analytical results.
C. Criteria
Criteria are determined by each Region.
1. PE sample frequency may vary.
2. The target analytes present in the PE sample must be correctly identified and quantified.
3. The RPD between field duplicates shall fall within the specific limits in the Region's Standard
Operating Procedure (SOP) or project QAPP.
D. Evaluation
1. Evaluation procedures must follow the Region's SOP for data review. Each Region will handle the
evaluation of PE samples on an individual basis.
2. Verify that each target analyte in the PE sample is properly identified and that each result is
calculated correctly.
3. Verify that the acceptance criteria for the specific PE sample are met, if available.
4. Calculate the RPD between field duplicates and provide this information in the Data Review
Narrative. Also verify that the value falls within the specific limits in the Region's SOP or project
QAPP.
E. Action
1. Any action must be in accordance with Regional specifications and the criteria for acceptable PE or
field duplicate sample results.
2. Note unacceptable results for PE or field duplicate samples for laboratory CLP PO action.
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XIV. Overall Assessment of Data
A. Review Items
Entire data package, data review results, and (if available), the QAPP and Sampling and Analysis Plan
(SAP).
B. Objective
The objective is to provide the overall assessment on data quality and usability.
C. Criteria
1. Review all available materials to assess the overall quality of the data, keeping in mind the additive
nature of analytical problems.
2. Reported analyte concentrations must be quantitated according to the appropriate analytical
method, as listed in the method. All sample results must be within the linear calibration ranges per
methods.
D. Evaluation
Examine the raw data to verify that the correct calculation of the sample results was reported by the
laboratory. Analysis logs, instrument printouts, etc., should be compared to the reported sample results
recorded on the appropriate Organic Summary Forms (Form 1A-OR through Form 8A-OR).
1. Evaluate any technical problems which have not been previously addressed.
2. Examine the raw data for any anomalies (e.g, baseline shift).
3. Verify that the appropriate method is used in sample analysis.
4. Verify that there are no transcription or reduction errors.
5. Verify that target analyte results fall within the calibrated ranges.
6. If appropriate information is available, use professional judgment to assess the usability of the data
in order to assist the data user in avoiding inappropriate use of the data. Review all available
information, including the QAPP (specifically the acceptance and performance criteria), SAP, and
communication with the data user that concerns the intended use and desired quality of these data.
E. Action
1. Use professional judgment to determine if there is any need to qualify data which were not
qualified based on the QC criteria previously discussed.
2. Use professional judgment to qualify sample results and non-detects if the MDL exceeds the
CRQL.
3. If a sample is not diluted properly when sample results exceed the upper limit of the calibration
range, qualify sample results as estimated (J).
4. Write a brief Data Review Narrative to give the user an indication of the limits of the analytical
data.
5. Note any inconsistency of the data with the SDG Narrative for laboratory CLP PO action. If
sufficient information on the intended use and required quality of the data is available, include an
assessment of the usability of the data within the given context. This may be used as part of a
formal Data Quality Assessment (DQA).
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Organic Data Review Low/Medium VGA
LOW/MEDIUM VOLATILE DATA REVIEW
The Low/Medium Volatile organic data requirements to be reviewed during validation are listed below:
I. Preservation and Holding Times 53
II. Gas Chromatograph/Mass Spectrometer Instrument Performance Check 57
III. Initial Calibration 65
IV. Continuing Calibration Verification 70
V. Blanks 73
VI. Deuterated Monitoring Compound 76
VII. Matrix Spike/Matrix Spike Duplicate 80
VIII. Internal Standard 82
IX. Target Analyte Identification 84
X. Target Analyte Quantitation and Reported Contract Required Quantitation Limit 86
XI. Tentatively Identified Compounds 88
XII. System Performance 91
XIII. Regional Quality Assurance and Quality Control 92
XIV. Overall Assessment of Data 93
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Organic Data Review Low/Medium VGA
I. Preservation and Holding Times
A. Review Items
Form 1A-OR, Form 1B-OR, Traffic Report/Chain of Custody (TR/COC) documentation, Form DC-1,
preparation sheet, raw data, and the Sample Delivery Group (SDG) 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 condition and the
holding time of the sample.
C. Criteria
1. Technical holding time is determined from the date of sample collection to the date of sample
analysis for aqueous and non-aqueous (soil and sediment) samples that are not designated for
Toxicity Characteristic Leaching Procedure (TCLP)/ Synthetic Precipitation Leaching Procedure
(SPLP) Zero Headspace Extraction (ZHE) procedures. The extraction technical holding time for
samples designated for TCLP/SPLP is determined from the date of sample collection to the date of
sample extraction.
2. For TCLP/SPLP leachate samples, technical holding time is determined from the date of
TCLP/SPLP ZHE completion to the date of TCLP/SPLP leachate sample analysis.
3. Samples should be in proper condition with shipping container temperatures at < 6°C upon receipt
at the laboratory. The aqueous, TCLP/SPLP aqueous samples, TCLP/SPLP leachate samples,
preserved non-aqueous samples shall be protected from light and refrigerated at < 6°C (but not
frozen) from the time of receipt at the laboratory. The unpreserved soil samples and samples
received in field core sampling/storage containers (Encore or equivalent) shall be protected from
light and stored at < -7°C, from the time of receipt at the laboratory.
4. The extraction technical holding time criteria for samples designated for TCLP/SPLP is 14 days.
5. The technical holding time criteria for aqueous samples that are properly cooled at < 6°C, but
without any indications of being preserved, is 7 days.
6. The technical holding time criteria for TCLP/SPLP aqueous samples and TCLP/SPLP leachate
samples that are properly cooled at < 6°C is 7 days.
7. The technical holding time criteria for aqueous samples that are properly cooled at < 6°C, and
acid-preserved with HC1 to a pH of < 2, is 14 days.
8. Samples received in field core sampling/storage containers should be transferred, immediately
upon receipt, to a pre-prepared closed-system P/T vial and either be analyzed within 24 hours of
sample receipt, or stored at < -7°C and analyzed within 14 days.
9. The technical holding time criteria for non-aqueous samples that are frozen at < -7°C, but not
preserved with NaHSO,is 14 days.
10. The technical holding time criteria for non-aqueous samples that are properly cooled at < 6°C (but
not frozen) and preserved with NaHSO, is 14 days.
11. The technical holding time criteria for non-aqueous samples that are properly cooled at < 6°C (but
not frozen), and preserved with methanol, is 14 days.
12. Samples received in field core sampling/storage containers should be transferred, immediately
upon receipt, to a pre-prepared closed system P/T vial and analyzed or frozen within 24 hours of
receipt.
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D. Evaluation
1. Review the SDG Narrative to determine if the samples were properly preserved and arrived at the
laboratory in proper condition (e.g., received intact, appropriate sample temperature at receipt, pH,
and absence of air bubbles or detectable headspace). If there is an indication of problems with the
samples, the sample integrity may be compromised.
2. Establish the TCLP/SPLP ZHE procedure technical holding times by comparing the sample
collection dates on the TR/COC documentation with the dates of extraction in the preparation
sheet. Also consider information contained in the Complete SDG File (CSF) as it may be helpful in
the assessment.
3. Verify that the analysis dates on Form 1A-OR and Form 1B-OR and the raw data/SDG file are
identical.
4. Establish technical holding times for TCLP/SPLP leachate samples by comparing the dates on the
extraction sheet with the dates of analysis on Form 1A-OR and Form 1B-OR.
5. Establish technical holding times by comparing the sample collection dates on the TR/COC
documentation with the dates of analysis on Form 1A-OR and Form 1B-OR. Also consider
information contained in the CSF as it may be helpful in the assessment.
a. These evaluation guidelines are intended to address the integrity of data for all analytes in
Statement of Work (SOW) Exhibit C for Low/Med Volatile Organics. If the data user is
interested in only a subset of the analytes and has data supporting analyte stability over longer
holding times, then those longer times may be applied prior to data qualification under Section
E, below. This information should be made part of the Data Review Narrative for evidentiary
purposes.
E. Action
1. If samples are received with shipping container temperatures > 6°C, use professional judgment to
qualify detects and non-detects.
2. If the TCLP/SPLP ZHE procedure is performed within the extraction technical holding time of 14
days, detects and non-detects should not be qualified.
3. If the TCLP/SPLP ZHE procedure is performed outside the extraction technical holding time of 14
days, qualify detects as estimated low (J-) and non-detects as unusable (R). Use caution in
determining whether some detected analytes should be qualified as estimated low (J-) or as
estimated high (J+), based on knowledge of individual analyte stability or interactions (i.e.
dehydrohalogenation).
4. If a discrepancy between the sample analysis date and that on raw data is found, perform a more
comprehensive review to determine the correct date for establishing holding time.
5. If aqueous samples are not properly preserved, but the samples are analyzed within the technical
holding time of 7 days, detects and non-detects should not be qualified.
6. If TCLP/SPLP aqueous samples and TCLP/SPLP leachate samples are analyzed within the
technical holding time of 7 days, detects and non-detects should not be qualified.
7. If aqueous samples are not properly preserved and are analyzed outside of the technical holding
time of 7 days, qualify detects as estimated low (J-) and non-detects as unusable (R).
8. If TCLP/SPLP aqueous samples and TCLP/SPLP leachate samples are analyzed outside of the
technical holding time of 7 days, qualify detects as estimated low (J-) and non-detects as unusable
(R).
9. If aqueous samples are properly preserved and are analyzed within the technical holding time of 14
days, detects and non-detects should not be qualified.
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10. If aqueous samples are properly preserved, but are analyzed outside of the technical holding time of
14 days, qualify detects as estimated (J) and non-detects as unusable (R). Use caution in
determining whether some detected analytes should be qualified as estimated low (J-) or as
estimated high (J+), based on knowledge of individual analyte stability or interactions (i.e.
dehydrohalogenation).
11. If non-aqueous samples are not properly preserved, and the samples are analyzed within the
technical holding time of 14 days, detects and non-detects should not be qualified.
12. If non-aqueous samples are not properly preserved, and the samples are analyzed outside the
technical holding time of 14 days, qualify detects as estimated low (J-) and non-detects as unusable
(R).
13. If non-aqueous samples are properly preserved, and the samples are analyzed within the technical
holding time of 14 days, detects and non-detects should not be qualified.
14. If non-aqueous samples are properly preserved, and the samples are analyzed outside the technical
holding time of 14 days, qualify detects as estimated (J) and non-detects as unusable (R). Use
caution in determining whether some detected analytes should be qualified as estimated low (J-) or
as estimated high (J+), based on knowledge of individual analyte stability or interactions (i.e.,
dehydrohalogenation).
15. When the holding times are exceeded, annotate in the Data Review Narrative any possible
consequences for the analytical results.
16. If holding times are grossly exceeded, qualify detects as estimated low (J-) and non-detects as
unusable (R). Note this for Contract Laboratory Program Project Officer (CLP PO) action.
Annotate the effect of the holding time exceedance on the resulting data in the Data Review
Narrative, whenever possible.
17. If samples are received with shipping container temperatures > 10°C, use professional judgment to
determine the reliability of the data or qualify detects as estimated low (J-) and non-detects as
estimated (UJ).
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Low/Medium VGA
Table 14. Preservation and Holding Time Actions for Low/Medium Volatile Analysis
Criteria
Sample temperature > 6°C upon receipt at the
laboratory
TCLP/SPLP ZHE performed within the 14-day
technical holding time
TCLP/SPLP ZHE performed outside the 14-day
technical holding time
Aqueous sample not preserved but analyzed within
the 7-day technical holding time
TCLP/SPLP aqueous and TCLP/SPLP leachate
samples analyzed within 7-day technical holding
time
Aqueous sample not preserved and analyzed outside
the 7-day technical holding time
TCLP/SPLP aqueous and TCLP/SPLP leachate
sample analyzed outside 7-day technical holding
time
Aqueous or TCLP/SPLP leachate sample properly
preserved and analyzed within the 14-day technical
holding time
Aqueous or TCLP/SPLP leachate sample properly
preserved but analyzed outside the 14-day technical
holding time
Non-aqueous sample preserved and analyzed within
the 14-day technical holding time
Non-aqueous sample properly preserved but
analyzed outside the 14-day technical holding time
Holding times grossly exceeded
Action
Detect
Use professional
judgment
No qualification
J-
No qualification
No qualification
J-
J-
No qualification
J*
No qualification
J*
J-
Non-detect
Use professional
judgment
No qualification
R
No qualification
No qualification
R
R
No qualification
R
No qualification
R
R
The true direction of any bias may be unknown in this case. Use professional judgement based on
knowledge of the chemistry of the analytes in the sample, or do not assign a direction to the bias.
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II.
Gas Chromatograph/Mass Spectrometer Instrument Performance Check
A.
B.
Review Items
Form 5-OR, bromofluorobenzene (BFB) mass spectra, and mass listing.
Objective
The objective of performing Gas Chromatograph/Mass Spectrometer (GC/MS) instrument
performance checks is to ensure adequate mass resolution, identification, and to some degree,
sensitivity, and to document this level of performance prior to analyzing any sequence of standards or
samples.
C. Criteria
1. A sufficient amount of the BFB instrument performance check solution (up to 50 ng BFB
on-column) must be injected once at the beginning of each 12-hour period, during which samples,
blanks, or standards are to be analyzed. The 12-hour period begins with either the injection of BFB,
or in cases where a closing Continuing Calibration Verification (CCV) can be used as an opening
CCV, the 12-hour clock begins with the injection of the opening CCV.
Listed below are examples of acceptable analytical sequences incorporating the use of the opening
and/or closing CCV. Use these examples as a guide for the possible analytical sequences that can be
expected.
Conditions for When
Example Sequence is
Appropriate:
Acceptable Criteria That Must
Be Met:
Notes:
Use Example 1 if time
remains on the 12-hour
clock after the initial
calibration sequence.
BFB tunes meet instrument
performance criteria.
The five Initial Calibration
standards meet initial
calibration criteria.
CCV A meets both opening
and closing CCV criteria.
CCV B meets closing CCV
criteria.
The requirement of starting the
new 12-hour clock for
Analytical Sequence 2 with a
new BFB tune is waived if CCV
A meets opening CCV criteria.
If CCV B meets opening CCV
criteria, a method blank and
subsequent samples may be
analyzed immediately after
CCVB.
Use Example 2 if time
remains on the 12-hour
clock after the initial
calibration sequence.
BFB tunes meet instrument
performance criteria.
The five Initial Calibration
standards meet initial
calibration criteria.
CCV A meets closing CCV
criteria (but does not meet
opening CCV criteria).
CCV B meets opening CCV
criteria.
CCV C meets closing CCV
criteria.
CCV A does not meet opening
CCV criteria. Therefore, a new
BFB tune must be performed,
immediately followed by CCV
B before the method blank and
any samples may be analyzed.
In this case, the new 12-hour
clock and Analytical Sequence
2 begins with the injection of
the new BFB tune.
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Conditions for When
Example Sequence is
Appropriate:
Acceptable Criteria That Must
Be Met:
Notes:
Use Example 3 if more
than 12 hours have elapsed
since the most recent
initial calibration or
closing CCV,
OR
if the most recent closing
CCV was not or could not
be used as an opening
CCV.
BFB tunes meet instrument
performance criteria.
CCV A meets opening CCV
criteria.
CCV B meets both opening
and closing CCV criteria.
CCV C meets both opening
and closing CCV criteria.
The requirement of starting the
new 12-hour clock for
Analytical Sequence 2 with a
new BFB tune is waived if CCV
B meets opening CCV criteria.
If CCV C meets opening CCV
criteria, a method blank and
subsequent samples may be
analyzed immediately after
CCVB.
Use Example 4 if more
than 12 hours have elapsed
since the most recent
initial calibration or
closing CCV,
OR
if the most recent closing
CCV was not or could not
be used as an opening
CCV.
BFB tunes meet instrument
performance criteria.
CCV A meets opening CCV
criteria.
CCV B meets closing CCV
criteria (but does not meet
opening CCV criteria).
CCV C meets opening CCV
criteria.
CCV D meets both opening
and closing CCV criteria.
Because CCV B does not meet
opening CCV criteria before the
method blank and any samples
may be analyzed, a new BFB
tune must be performed,
immediately followed by CCV
C. In this case, the new 12-hour
clock and Analytical Sequence
2 begins with the injection of
the new BFB tune. The
requirement of starting the new
12-hour clock for Analytical
Sequence 3 with a new BFB
tune is waived if CCV D meets
opening CCV criteria. If CCV
D meets opening CCV criteria,
a method blank and subsequent
samples may be analyzed
immediately after CCV D.
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Example 1:
Example 1:
Time Material Injected
Analytical Sequence #
Start of 12-hour clock for
Analytical Sequence 1
End of 12-hour clock for
Analytical Sequence I/
Beginning of 12-hour clock
for Analytical Sequence 2
End of 12-hour clock for
Analytical Sequence 21
Beginning of 12-hour clock
for Analytical Sequence 3
0 hr BFB
12 h
24
Initial Calibration 5.0
Initial Calibration 10
Initial Calibration 50
Initial Calibration 100
Initial Calibration 200
Method Blank
Subsequent Samples
L (meets opening
criteria)
Method Blank
Subsequent Samples
CCV B (meets opening CCV
criteria)
1
1
1
1
1
1
1
1
1
1
1
1/2
2
2
2
2
2
2
2/3
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Example 2:
Example 2:
Time Material Injected
Analytical Sequence
#
Start of 12-hour clock for
,,.,,., .
Analytical Sequence 1
,
Dm
End of 12-hour clock for
Analytical Sequence 1
Beginning of 12-hour
clock for Analytical
Sequence 2
12 hr
13 hr
End of 12-hour clock for
Analytical Sequence 2
BFB
Initial Calibration 5.0
Initial Calibration 10
Initial Calibration 50
Initial Calibration 100
Initial Calibration 200
Method Blank
Subsequent Samples
CCV A (meets closing CCV
criteria, fails opening CCV criteria)
BFB
CCV B (meets opening CCV
criteria)
Method Blank
Subsequent Samples
25 hr
CCV C (meets closing CCV
criteria)
2
2
2
2
2
2
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Example 3:
Example 3:
Time Material Injected
Analytical Sequence
#
Start of 12-hour clock for
Analytical Sequence 1
0 hr BFB
CCV A (meets opening CCV
criteria)
Method Blank
Subsequent Samples
•
•
•
.
1
1
1
1
1
1
1
1
End of 12-hour clock for
Analytical Sequence I/
Beginning of 12-hour clock
for Analytical Sequence 2
12 hr
End of 12-hour clock for
Analytical Sequence 21
Beginning of 12-hour clock
for Analytical Sequence 3
24
CCV B (meets opening CCV
criteria)
Method Blank
Subsequent Samples
CCV C (meets opening CCV
criteria)
1/2
2
2
2
2
2
2/3
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Example 4:
Example 4:
Time Material Injected
Analytical Sequence
#
Start of 12-hour clock for
Analytical Sequence 1
End of 12-hour clock for
Analytical Sequence 1
Beginning of 12-hour
clock for Analytical
Sequence 2
End of 12-hour clock for
Analytical Sequence 21
Beginning of 12-hour
clock for Analytical
Sequence 3
Ohr
12 hr
13 hr
25 hr
BFB
CCV A (meets opening CCV
criteria)
Method Blank
Subsequent Samples
CCV B (meets closing CCV criteria,
fails opening CCV criteria)
BFB
CCV C (meets opening CCV
criteria)
Method Blank
Subsequent Samples
CCV D (meets opening CCV
criteria)
1
2
2
2
2
2
2/3
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2. The BFB instrument performance check must meet the ion abundance criteria listed in Table 15.
Table 15. Ion Abundance Criteria for BFB
Mass
50
75
95
96
173
174
175
176
177
Ion Abundance Criteria
15.0 -40.0% of mass 95
30.0 -80.0% of mass 95
Base peak, 100% relative abundance
5.0 -9.0% of mass 95*
Less than 2.0% of mass 174
5 0.0% -120% of mass 95
5.0 -9.0% of mass 174
95.0 -101% of mass 174
5.0 -9.0% of mass 176
* All ion abundances must be normalized to mass-to-charge (m/z) 95, the nominal base peak, even
though the ion abundance of m/z 174 may be up to 120% that of m/z 95.
D. Evaluation
1. Verify that the BFB Instrument Performance Check solution is analyzed at the specified frequency
and sequence.
2. Compare the data presented on Form 5-OR for each Instrument Performance Check with each mass
listing submitted to ensure the following:
a. Form 5-OR is present and completed for each required BFB at the specified frequency.
b. The laboratory has not made transcription errors between the data and the form. If there are
major differences between the mass listing and Form 5-OR, a more in-depth review of the data
is required. This may include obtaining and reviewing additional information from the
laboratory.
c. The appropriate number of significant figures has been reported (number of significant figures
given for each ion in the ion abundance criteria column) and that rounding is correct.
d. The laboratory has not made any calculation errors.
3. Verify from the raw data (mass listing) that the mass assignment is correct and that the mass listing
is normalized to m/z 95.
4. Verify that the ion abundance criteria are met. The criteria for m/z 173, 175, 176, and 177 are
calculated by normalizing to the specified m/z. The critical ion abundance criteria for BFB are the
relative abundance ratios of m/z 95/96, 174/175, 174/176, and 176/177. The relative abundance
ratios of m/z 50 and 75 are of lower importance for target analytes than for Tentatively Identified
Compounds (TICs).
5. If possible, verify that spectra are generated using appropriate background subtraction techniques.
Since the BFB spectrum is obtained from chromatographic peaks that should be free from
co-elution problems, background subtraction should be performed in accordance with the
following procedure:
a. Three scans (the peak apex scan and the scans immediately preceding and following the apex)
are acquired and averaged.
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b. Background subtraction must be accomplished using a single scan no more than 20 scans prior
to the elution of BFB, but the BFB peak must not be subtracted as part of the background.
NOTE: All mass spectrometer instrument conditions must be identical to those used for sample
analysis. Background subtraction actions resulting in spectral distortions for the sole
purpose of meeting the method specifications are contrary to the Quality Assurance (QA)
objectives, and are therefore unacceptable.
NOTE: For data obtained from the Contract Laboratory Program (CLP), information regarding
non-compliant BFB instrument performance check can be obtained from the National
Functional Guidelines (NFG) reports and may be used as part of the evaluation process.
E. Action
1. If instrument performance check is not analyzed at the specified frequency and sequence, contact
the Regional CLP PO to arrange for reanalysis of any samples involved.
a. In the event the samples cannot be reanalyzed, examine all calibrations associated with the
sequence to evaluate whether proper qualitative criteria were achievable. If so, it may be
possible to salvage usable data from the sequence. Otherwise, qualify the data as unusable (R).
2. If minor transcription errors are found to be insignificant to data quality and can be corrected on a
copy of the form, no further actions are required.
3. If the laboratory failed to provide the correct forms or significant transcription or calculation errors
are found, notify the Regional CLP PO, who may contact the laboratory to request the necessary
information. If the information is not available, use professional judgment to assess the data, and
notify the laboratory's CLP PO.
4. If mass assignment is in error (e.g., m/z 96 is indicated as the base peak rather than m/z 95), qualify
detects and non-detects in the associated samples as unusable (R).
5. If the ion abundance criteria in Table 15 are not met, use professional j udgment to qualify detects
and non-detects in the associated samples.
6. Annotate decisions to use analytical data associated with non-compliant BFB instrument
performance checks in the Data Review Narrative.
7. If the instrument performance check criteria are achieved using techniques other than those
described in Section II.D.5, obtain additional information to evaluate performance and procedures.
Note any concerns or questions for laboratory CLP PO action.
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III. Initial Calibration
A. Review Items
Form 6A-OR, quantitation reports, and chromatograms.
B. Objective
The objective of initial calibration (ICAL) is to ensure that the instrument is capable of producing
acceptable qualitative and quantitative data.
C. Criteria
1. ICAL should be performed at the specified frequency and sequence. Each GC/MS system must be
calibrated with a minimum of five concentrations to determine instrument sensitivity and the
linearity of GC/MS response for the purgeable target analytes and Deuterated Monitoring
Compounds (DMCs).
a. ICAL standards must be analyzed prior to any analysis of samples and required blanks and
within 12 hours of the associated instrument performance check at the beginning of each
analytical sequence, or as necessary if the CCV acceptance criteria are not met.
b. ICAL standards must contain all required target analytes and DMCs at concentrations of 5.0,
10, 50, 100, and 200 (ig/L for non-ketones, and 10, 50, 100, 200 and 400 (ig/L forketones.
c. All three xylene isomers (o-, m-, and p-xylene) must be present in calibration standards.
d. Concentrations for o-xylene must be at 5.0, 10, 50, 100 and 200 (ig/L, while the total
concentrations of the m- plus the p-xylene isomers must be at 5.0, 10, 50, 100, and 200 (ig/L.
2. The Relative Response Factor (RRF), mean RRF (RRF) and the Percent Relative Standard
Deviation (%RSD) must be calculated for each target analyte and DMC accordingly.
3. The RRF for each target analyte and DMC in each ICAL standard must be > Minimum RRF value
in Table 16.
4. The %RSD of the ICAL RRF for each target analyte and DMC must be < Maximum %RSD values
in Table 16.
NOTE: The technical acceptance criteria in a "Request for Quote (RFQ) for Modified Analysis"
may impact some of the preceding evaluation criteria. A copy of the modified analysis
should be present in the SDG, when applicable. Refer to the CLP home page at
http://www.epa.gov/oerrpage/superfund/programs/clp/modifiedanalyses.htm for the
specific method flexibility requirements.
D. Evaluation
1. Verify that the ICAL is performed at the specified frequency and sequence.
2. Verify that the correct concentrations of the target analytes and DMCs are used in each ICAL
standard.
3. Verify that the RRF, RRF, and %RSD for each target analyte and DMC are reported in Form
6A-OR. Recalculate the RRFs, RRFs, and %RSD for at least one target analyte and DMC
associated with each internal standard, and verify that the recalculated values agree with the
laboratory reported values on Form 6A-OR.
4. Verify that RRF is > Minimum RRF values in Table 16 for each target analyte and DMC.
5. Verify that %RSDs are < Maximum %RSD values in Table 16 for each target analyte and DMC.
NOTE: For data obtained from the CLP, information regarding non-compliant ICAL can be
obtained from the NFG reports and may be used as part of the evaluation process.
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E. Action
1. If the ICAL is not performed at the specified frequency and sequence, qualify detects and
non-detects in the associated samples as unusable (R).
2. If the ICAL is not performed at the specified concentrations, qualify detects in the associated
samples as estimated (J) and non-detects in the associated samples as estimated (UJ).
3. If errors are detected in the calculations of the RRFs, RRFs, or %RSD, perform a more
comprehensive recalculation.
4. If the RRF is < Minimum RRF value in Table 16 for any target analyte, use professional judgment
to qualify detects in the associated samples as estimated high (J+) or unusable (R) and non-detects
in the associated samples as unusable (R).
5. If the RRF is > Minimum RRF value in Table 16 for any target analyte, detects and non-detects in
the associated samples should not be qualified.
6. If the %RSD is > Maximum %RSD value in Table 16 for any target analyte, qualify detects in the
associated samples as estimated (J). Use professional judgment to qualify non-detects in the
associated samples.
7. If the %RSD is < Maximum %RSD value in Table 16 for any target analyte, detects and
non-detects in the associated samples should not be qualified.
8. No qualification of the data is necessary on the DMC RRF, RRF, and %RSD data alone. Use
professional judgment to evaluate the DMC RRF, RRF, and %RSD data in conjunction with the
DMC recoveries to determine the need for data qualification.
9. Based on the project-specific Data Quality Objectives (DQOs), a more in-depth review may be
considered using the following guidelines:
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.
b. If the high-point of the ICAL curve is outside of the %RSD criteria (e.g., due to saturation):
i. Qualify detects in the associated samples with analyte concentrations greater than the
high-point concentration as estimated (J).
ii. Detects in the associated samples with analyte concentrations within the calibration range
should not be qualified.
iii. Non-detects in the associated samples should not be qualified.
c. If the low-point of the ICAL curve is outside of the %RSD criteria:
i. Qualify detects in the associated samples with analyte concentrations in the non-linear
range as estimated (J).
ii. Detects in the associated samples with analyte concentrations within the calibration range
should not be qualified.
iii. 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.
10. If the laboratory failed to provide adequate calibration information, notify the Regional CLP PO,
who may contact the laboratory to request the necessary information. If the information is not
available, use professional judgment to assess the data.
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11. Annotate the potential effects on the reported data due to exceeding the ICAL criteria in the Data
Review Narrative.
12. If the ICAL criteria are grossly exceeded, note this for laboratory CLP PO action.
Table 16. RRF, %RSD, and %D Acceptance Criteria in Initial Calibration and CCV for
Low/Medium Volatile Analysis
Analyte
Dichlorodifluoromethane
Chloromethane
Vinyl chloride
Bromomethane
Chloroethane
Trichlorofluoromethane
1 , 1 -Dichloroethene
1 , 1 ,2-Trichloro- 1 ,2,2-trifluoroethane
Acetone
Carbon disulfide
Methyl acetate
Methylene chloride
trans-l,2-Dichloroethene
Methyl tert-butyl ether
1 , 1 -Dichloroethane
cis-l,2-Dichloroethene
2-Butanone
Bromochloromethane
Chloroform
1,1,1 -Trichloroethane
Cyclohexane
Carbon tetrachloride
Benzene
1 ,2-Dichloroethane
Trichloroethene
Methylcyclohexane
1 ,2-Dichloropropane
Bromodichloromethane
Minimum
RRF
0.010
0.010
0.010
0.010
0.010
0.010
0.060
0.050
0.010
0.100
0.010
0.010
0.100
0.100
0.300
0.200
0.010
0.100
0.300
0.050
0.010
0.100
0.200
0.070
0.200
0.050
0.200
0.300
Maximum
%RSD
25.0
20.0
20.0
40.0
40.0
40.0
20.0
25.0
40.0
20.0
40.0
40.0
20.0
40.0
20.0
20.0
40.0
20.0
20.0
20.0
40.0
20.0
20.0
20.0
20.0
40.0
20.0
20.0
Opening
Maximum
VoD1
±40.0
±30.0
±25.0
±30.0
±25.0
±30.0
±20.0
±25.0
±40.0
±25.0
±40.0
±30.0
±20.0
±25.0
±20.0
±20.0
±40.0
±20.0
±20.0
±25.0
±25.0
±25.0
±20.0
±20.0
±20.0
±25.0
±20.0
±20.0
Closing
Maximum
%D
±50.0
±50.0
±50.0
±50.0
±50.0
±50.0
±25.0
±50.0
±50.0
±25.0
±50.0
±50.0
±25.0
±50.0
±25.0
±25.0
±50.0
±25.0
±25.0
±25.0
±50.0
±25.0
±25.0
±25.0
±25.0
±50.0
±25.0
±25.0
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Analyte
cis- 1 ,3 -Dichloropropene
4-Methyl -2 -pentanone
Toluene
trans -1,3 -Dichloropropene
1 , 1 ,2-Trichloroethane
Tetrachloroethene
2-Hexanone
Dibromochloromethane
1 ,2-Dibromoethane
Chlorobenzene
Ethylbenzene
m,p-Xylene
o-Xylene
Styrene
Bromoform
Isopropylbenzene
1 , 1 ,2,2-Tetrachloroethane
1 , 3 -Dichlorobenzene
1 ,4-Dichlorobenzene
1 ,2-Dichlorobenzene
1 ,2-Dibromo-3 -chloropropane
1 ,2,4-Trichlorobenzene
1,2,3-Trichlorobenzene
Minimum
RRF
0.300
0.030
0.300
0.200
0.200
0.100
0.010
0.200
0.200
0.400
0.400
0.200
0.200
0.200
0.100
0.400
0.200
0.500
0.600
0.600
0.010
0.400
0.400
Maximum
%RSD
20.0
25.0
20.0
20.0
20.0
20.0
40.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
25.0
20.0
25.0
Opening
Maximum
VoD1
±20.0
±30.0
±20.0
±20.0
±20.0
±20.0
±40.0
±20.0
±20.0
±20.0
±20.0
±20.0
±20.0
±20.0
±25.0
±25.0
±25.0
±20.0
±20.0
±20.0
±30.0
±30.0
±30.0
Closing
Maximum
%D
±25.0
±50.0
±25.0
±25.0
±25.0
±25.0
±50.0
±25.0
±25.0
±25.0
±25.0
±25.0
±25.0
±25.0
±50.0
±25.0
±25.0
±25.0
±25.0
±25.0
±50.0
±50.0
±50.0
Deuterated Monitoring Compound
Vinyl chloride-ds
Chloroethane-d5
1 , 1 -Dichloroethene-d2
2-Butanone-d5
Chloroform-d
1 ,2-Dichloroethane-d4
Benzene -d6
1 ,2-Dichloropropane-d6
Toluene -ds
0.010
0.010
0.050
0.010
0.300
0.060
0.300
0.200
0.300
20.0
40.0
20.0
40.0
20.0
20.0
20.0
20.0
20.0
±30.0
±30.0
±25.0
±40.0
±20.0
±25.0
±20.0
±20.0
±20.0
±50.0
±50.0
±25.0
±50.0
±25.0
±25.0
±25.0
±25.0
±25.0
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Analyte
trans -1,3 -Dichloropropene-d4
2-Hexanone-d5
1 , 1 ,2,2-Tetrachloroethane-d2
l,2-Dichlorobenzene-d4
Minimum
RRF
0.200
0.010
0.200
0.400
Maximum
%RSD
20.0
40.0
20.0
20.0
Opening
Maximum
VoD1
±20.0
±40.0
±25.0
±20.0
Closing
Maximum
%D
±25.0
±50.0
±25.0
±25.0
1 If a closing CCV is acting as an opening CCV, all target analytes and DMCs must meet the
requirements for an opening CCV.
Table 17. Initial Calibration Actions for Low/Medium Volatile Analysis
Criteria
Initial Calibration not performed at specified
frequency and sequence
Initial Calibration not performed at the specified
concentrations
RRF < Minimum RRF in Table 16 for target
analyte
RRF > Minimum RRF in Table 16 for target
analyte
%RSD > Maximum %RSD in Table 16 for
target analyte
%RSD < Maximum %RSD in Table 16 for
target analyte
Action
Detect
Use professional
judgment
R
J
Use professional
judgment
J+orR
No qualification
J
No qualification
Non-detect
Use professional
judgment
R
UJ
R
No qualification
Use professional
judgment
No qualification
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IV. Continuing Calibration Verification
A. Review Items
Form 7A-OR, quantitation reports, and chromatograms.
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. Criteria
1. The calibration for each GC/MS system used for analysis must be verified at the beginning and end
of every 12-hour period of operation. The 12-hour period begins with the injection of BFB,
followed by the injection of the opening CCV solution. After the injection of all samples and
required blanks, and before the end of the 12-hour period, injection of the closing CCV is required.
The closing CCV used to bracket the end of a 12-hour analytical sequence may be used as the
opening CCV for a new 12-hour analytical sequence, provided that all technical acceptance criteria
of an opening CCVare met.
2. The CCV standards must contain all required target analytes and DMCs at the mid-point
concentration (CSS) of the ICAL.
3. For an opening or a closing CCV, the RRF for each target analyte and DMC must be > the
Minimum RRF values in Table 16.
4. The Percent Difference (%D) between the ICAL RRF and the opening CCV RRF must be within
the Opening Maximum %D limits in Table 16 for each target analyte and DMC.
5. For a closing CCV, the %D between the ICAL RRF and the CCV RRF must be within the Closing
Maximum %D limits in Table 16 for each target analyte and DMC.
D. Evaluation
1. Verify that the CCV is analyzed at the specified frequency and sequence and that the CCV is
associated to the correct ICAL. Also verify that the correct ICAL is represented in the data package
and meets SOW criteria, as described in Section III.
2. Verify that the mid-point standard CSS from the ICAL is used as an opening or a closing CCV.
3. Verify that the RRF and %D for each target analyte and DMC are reported on Form 7A-OR.
Recalculate RRF and %D for at least one target analyte and DMC associated with each internal
standard and verify that the recalculated values agree with the laboratory reported values on Form
7A-OR
4. For an opening or a closing CCV, verify that the RRFs for all target analytes and DMCs are > the
Minimum RRF values in Table 16.
5. For an opening CCV, verify that the %Ds are within the Opening Maximum %D limits in Table 16
for the target analytes and DMCs.
6. For a closing CCV, verify that the %Ds are within the Closing Maximum %D limits in Table 16 for
all target analytes and DMCs.
NOTE: For data obtained from the CLP, information regarding the non-compliant CCV can be
obtained from the NFG reports and may be used as part of the evaluation process.
E. Action
1. If the CCV is not performed at the specified frequency, qualify detects and non-detects as unusable
(R). Contact the Regional CLP PO to request that the laboratory repeat the analysis, if holding
times have not expired and there are remaining sample vials. If reanalysis is not possible, carefully
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evaluate all other available information, including the the quality of analyte peak shapes and mass
spectral matches, stability of internal standard retention times (RTs) and areas in each affected
sample, 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).
2. If the CCV is not performed at the specified concentration, use professional judgment to qualify
detects and non-detects. Special consideration should be given to sample results at the opposite
extreme of the calibration range if this defect is noted.
3. If errors are detected in the calculations of either the RRF or the %D, perform a more
comprehensive recalculation.
4. For an opening or a closing CCV, if the RRF is < the Minimum RRF value in Table 16 for any
target analyte, carefully evaluate the qualitative data associated with positively identified analytes
and use professional judgment to qualify detects as estimated (J) or unusable (R), and qualify
non-detects as unusable (R).
5. For an opening or a closing CCV, if the RRF is > Minimum RRF value in Table 16 for any target
analyte, detects and non-detects should not be qualified.
6. For an opening CCV, if the %D is outside the Opening Maximum %D limits in Table 16 for any
target analyte, qualify detects as estimated (J) and non-detects as estimated (UJ).
a. Take special note of any extreme deviation in RRF and evaluate RT data peak shapes, and areas
for inconsistencies that may indicate a chromatographic co-elution. If this is suspected, the
contaminant may also be present in samples and blanks. Use professional judgement to qualify
affected data appropriately.
7. For a closing CCV, if the %D is outside the Closing Maximum %D limits in Table 16 for any target
analyte, qualify detects as estimated (J) and non-detects as estimated (UJ).
8. For an opening CCV, if the %D is within the inclusive range of the Opening Maximum %D limits
in Table 16 for any target analyte, detects and non-detects should not be qualified.
9. For closing CCV, if the %D is within the inclusive range of the Closing Maximum %D limits in
Table 16 for any target analyte, detects and non-detects should not be qualified.
10. No qualification of the data is necessary on DMC RRF and/or %D alone. Use professional
judgment to evaluate the DMC RRF and %D data in conjunction with the DMC recoveries to
determine the need for data qualification.
11. If the laboratory has failed to provide adequate calibration information, contact the Regional CLP
PO, who may contact the laboratory to request the necessary information. If the information is not
available, use professional judgment to assess the data.
12. Annotate the potential effects on the data due to CCV criteria exceedance in the Data Review
Narrative.
13. If CCV criteria are grossly exceeded, note this for laboratory CLP PO action.
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Table 18. CCV Actions for Low/Medium Volatile Analysis
Criteria for Opening CCV
CCV not performed at
required frequency
CCV not performed at
specified concentration
RRF < Minimum RRF in
Table 16 for target analyte
RRF > Minimum RRF in
Table 16 for target analyte
%D outside the Opening
Maximum %D limits in Table
16 for target analyte
%D within the inclusive
Opening Maximum %D limits
in Table 16 for target analyte
Criteria for Closing CCV
CCV not performed at
required frequency
CCV not performed at
specified concentration
RRF < Minimum RRF in
Table 16 for target analyte
RRF > Minimum RRF in
Table 16 for target analyte
%D outside the Closing
Maximum %D limits in Table
16 for target analyte
%D within the inclusive
Closing Maximum %D limits
in Table 16 for target analyte
Action
Detect
Use
professional
judgment
R
Use
professional
judgment
Use
professional
judgment
JorR
No
qualification
J
No
qualification
Non- detect
Use
professional
judgment
R
Use
professional
judgment
R
No
qualification
UJ
No
qualification
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V. Blanks
A. Review Items
Form 1A-OR, Form 1B-OR, Form 4-OR, chromatograms, and quantitation 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. Criteria
The criteria for evaluation of blanks should apply to any blank associated with the samples (e.g.,
method blanks, storage blanks, field blanks, etc.). If problems with any blank exist, all associated data
must be carefully evaluated to determine whether or not there is an inherent variability in the data or if
the problem is an isolated occurrence not affecting other data.
1. Method blanks analyses must be performed at the specified frequency and sequence. A method
blank must be analyzed once every 12-hour period and prior to any sample analysis and after all
ICAL standards or CCV. The method blank must be analyzed on each GC/MS system used for
sample analysis within an entire analytical sequence.
2. The method blank, like any other sample in the SDG, must meet the technical acceptance criteria
for sample analysis.
3. The TCLP/SPLP ZHE leachate extraction blank (LEB) must be prepared and analyzed at the
specified frequency and sequence.
4. A storage blank analysis must be performed at the specified frequency and sequence. A storage
blank must be prepared upon receipt of the first samples from a SDG, and stored with the samples
until analysis. The storage blank must be analyzed once per SDG after all sample analyses within a
SDG are complete.
5. An instrument blank must be analyzed immediately after any sample that has target analytes
exceeding the calibration range or non-target compounds exceeding 100 (ig/L.
6. The concentration of a target analyte in any blank must not exceed its Contract Required
Quantitation Limit (CRQL) (2x CRQLs for Methylene chloride, Acetone, and 2-Butanone). TIC
concentration in any blanks must be < 5.0 (ig/L for water and < 5.0 (ig/kg for soil matrices.
D. Evaluation
1. Verify that method blanks are analyzed at the specified frequency and sequence. The Method Blank
Summary (Form 4-OR) may be used to identify the samples associated with each method blank.
2. Verify that applicable TCLP/SPLP extraction blanks are analyzed at the specified frequency and
sequence. The Method Blank Summary (Form 4-OR) may be used to identify the samples
associated with each TCLP/SPLP LEB.
3. Verify that a storage blank has been analyzed at the specified frequency and sequence.
4. Verify that the instrument blank analysis has been performed following any sample analysis where
a target analyte(s) is/are reported at high concentration(s).
5. Review the results of all associated blanks on the forms and raw data (chromatograms and
quantitation reports) to evaluate the presence of target analytes and non-target compounds in the
blanks.
6. Evaluate field or trip blanks in the manner similar to that used for the method blanks.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the Contract
Compliance Screening (CCS) process. Information regarding the non-compliant blank can
be obtained from the NFG reports and may be used as part of the evaluation process.
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E. Action
1. If the appropriate blanks are not analyzed at the correct frequency, use professional judgment to
determine if the associated sample data should be qualified; obtain additional information from the
laboratory, if necessary. Record the situation in the Data Review Narrative and note it for CLP PO
action.
2. 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 Quality Assurance Project Plan (QAPP). At a minimum, contamination found in field
blanks should be documented in the Data Review Narrative. In instances where more than one of
blank is associated with a given sample, qualification should be based upon a comparison with the
associated blank having the highest concentration of a contaminant. Do not correct the results by
subtracting any blank value.
3. For any blank (including method blank), if a target analyte is detected, but it is not detected in the
sample, non-detects should not be qualified.
4. For any method blank reported with results < CRQLs, report sample results that are < CRQLs at the
CRQLs and qualify as non-detect (U). For any method blank reported with results < CRQLs, use
professional judgment to qualify sample results that are > CRQLs (> 2x result in method blank for
Methylene Chloride, Acetone and 2-Butanone). Positive results in samples, especially those near
but above the CRQL, may be biased high by low level contamination in the method blank, and
should be considered as estimated (J+).
5. For any method blank reported with results > CRQLs, report sample results that are < CRQLs at the
CRQLs and qualify as non-detect (U).
6. For any method blank reported with results > CRQLs, report sample results that are > CRQLs (> 2x
results in method blank for Methylene Chloride, Acetone and 2-Butanone) but < Blank Results,
qualified as non-detect (U) or as unusable (R). Use professional judgment to qualify sample results
that are > CRQLs (> 2x results in method blank for Methylene Chloride, Acetone and 2-Butanone)
and > Blank Results.
7. If an instrument blank is not analyzed following a sample analysis which contains analyte(s) at high
concentration(s) exceeding the calibration range, evaluate the analyte(s) concentration(s) in sample
analyzed immediately after the sample with high analyte(s) concentration(s) for carryover. Use
professional judgment to determine if instrument cross-contamination has affected any positive
target analyte identification(s). If instrument cross-contamination is suggested and suspected of
having an effect on the sample results or calibration performance, note it for laboratory CLP PO
action.
8. If any analytes are detected in the storage, field, or trip blanks, the following is recommended:
a. Review the associated method blank data to determine if the same analytes are also detected in
the method blank.
i. If the analytes are detected at comparable levels in the method blank, the source of the
contamination may be in the analytical system. Apply the recommended actions for the
method blank.
ii. If the analytes are not detected in the method blank, the source of contamination may be in
the storage area or in the field; or contamination may have occurred during sample
transport. Consider all associated samples for possible cross-contamination.
iii. For TCLP/SPLP LEBs, storage, field, or trip blanks, sample result qualifications listed in
Table 19 should apply.
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9. If gross contamination exists with blank results that are > ICAL CSS concentrations, qualify detects
as unusable (R). If the contamination is suspected of having an effect on the sample results, note it
for laboratory CLP PO action.
10. For any blank (including method blank) reported with TICs (non-target compounds) concentrations
that are > 5.0 (ig/L for water or > 5.0 (ig/kg for soil matrices, use professional judgment to qualify
sample results.
11. 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.
Table 19. Blank and TCLP/SPLP LEB Actions for Low/Medium Volatile Analysis
Blank Type
Method,
TCLP/SPLP
LEB,
Storage,
Field, Trip,
Instrument*
Blank Result
Detect
< CRQL*
> CRQL*
Gross
contamination*
TIC>5.0ug/L
(water)
and
TIC>5.0(ig/kg
(soil)
Sample Result
Non-detect
CRQL or > 2x Blank Result
for Methylene Chloride,
Acetone and 2-Butanone
CRQL but < Blank Result
> CRQL and > Blank Result or
> 2x Blank Result for
Methylene Chloride, Acetone
and 2-Butanone
Detect
Detect
Action
No qualification
Report at CRQL and qualify
as non-detect (U)
Use professional judgment
Report at CRQL and qualify
as non-detect (U)
Report sample result and
qualify as non-detect (U) or
unusable (R)
Use professional judgment
Report at sample result and
qualify as unusable (R)
Use professional judgment
Qualifications based on instrument blank results affect only the sample analyzed immediately after
the sample that has target analyte concentration exceeding the calibration range (ICAL CS5
concentration) or TIC exceeding 200 (ig/L.
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VI. Deuterated Monitoring Compound
A. Review Items
Form 2A-OR, Form 2B-OR quantitation reports, and chromatograms.
B. Objective
The objective is to evaluate the DMC Percent Recovery (%R) to ensure that the analytical method is
efficient.
C. Criteria
1. All samples and blanks are spiked with the DMCs listed in Table 20, just prior to sample purging, to
measure the DMC %R.
2. The %R for each DMC should be calculated correctly according to the method.
3. The %R for each DMC in samples and blanks must be within the limits in Table 20.
Table 20. Low/Medium Volatile DMCs and Recovery Limits
DMC
Vinyl chloride -d3
Chloroethane-d5
1 , 1 -Dichloroethene-d2
2-Butanone-d5
Chloroform-d
1 ,2-Dichloroethane-d4
Benzene -d6
1 ,2-Dichloropropane-d6
Toluene-d8
trans- 1 ,3 -Dichloropropene-d4
2-Hexanone-d5
1 , 1 ,2,2-Tetrachloroethane-d2
1 ,2-Dichlorobenzene-d4
%R for Water
Sample
60-135
70-130
60-125
40-130
70-125
70-125
70-125
70-120
80-120
60-125
45-130
65-120
80-120
%R for Soil
Sample
30-150
30-150
45-110
20-135
40-150
70-130
20-135
70-120
30-130
30-135
20-135
45-120
75-120
NOTE:
The recovery limits for any of the compounds listed in Table 20 may be expanded at any
time during the period of performance if the United States Environmental Protection
Agency (EPA) determines that the limits are too restrictive.
D. Evaluation
1. Check raw data (e.g., chromatograms and quantitation reports) to verify the recoveries on the
Deuterated Monitoring Compound Recovery Form 2A-OR and Form 2B-OR.
2. Check for any calculation or transcription errors. Verify that the DMC recoveries were calculated
correctly using the equation in the method and that the recalculated values agree with the laboratory
reported values on Form 2A-OR and Form 2B-OR.
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3. Whenever there are two or more analyses for a particular sample, use professional judgment to
determine which analysis has the most acceptable data to report. Considerations include, but are
not limited to:
a. DMC recovery (marginal versus gross deviation).
b. Technical holding times.
c. Comparison of the target analyte results reported in each sample analysis.
d. Other QC information, such as performance of internal standards.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the non-compliant DMC %R can be obtained from the
NFG reports and may be used as part of the evaluation process.
E. Action
1. If a DMC is not added in the samples and blanks or the concentrations of DMCs in the samples and
blanks are not as specified, use professional judgment to qualify detects and non-detects. The
Regional CLP PO should be contacted to arrange for reanalysis, if possible.
2. If errors are detected in the calculations of %R, perform a more comprehensive recalculation. It
may be necessary to have the laboratory resubmit the data after making corrections.
3. If any DMC %R is outside the limits (Table 20) in samples, qualify the associated analytes listed in
Table 22 considering the existence of interference in the raw data. Considerations include, but are
not limited to:
a. If the DMC %R is < 10%, qualify detects as estimated low (J-) and non-detects as unusable (R).
b. If the DMC %R is > 10% and < the lower acceptance limit, qualify detects as estimated low (J-)
and non-detects as estimated (UJ).
c. If the DMC %R is > lower acceptance limit and < upper acceptance limit, detects and
non-detects should not be qualified.
d. If the DMC %R is > upper acceptance limit, qualify detects as estimated high (J+).
Non-detects should not be qualified.
4. If any DMC %R is outside the limits (Table 20) in a blank, 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.
For example, if one or more samples in the analytical sequence show acceptable DMC %Rs, the
blank problem may be considered as an isolated occurrence. However, even if this judgment
allows some use of the affected data, note analytical problems for laboratory CLP PO action.
Table 21. DMC Actions for Low/Medium Volatile Analysis
Criteria
%R<10%
10% < %R < Lower Acceptance Limit
Lower Acceptance Limit < %R < Upper Acceptance
Limit
%R > Upper Acceptance Limit
Action
Detect
J-
J-
No qualification
J+
Non-detect
R
UJ
No qualification
No qualification
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Table 22. Low/Medium Volatile DMCs and the Associated Target Analytes
Chloroethane-d5 (DMC)
Dichlorodifluoromethane
Chloromethane
Bromomethane
Chloroethane
Carbon disulfide
trans -1,3 -Dichloropropene-d4
(DMC)
cis- 1 ,3 -Dichloropropene
trans -1,3 -Dichloropropene
1 , 1 ,2-Trichloroethane
2-Butanone-d5 (DMC)
Acetone
2-Butanone
Vinyl chloride-d3 (DMC)
Vinyl chloride
l,2-Dichloroethane-d4 (DMC)
Trichlorofluoromethane
1,1,2-Trichloro-
1 ,2,2-trifluoroethane
Methyl acetate
l,2-Dichloropropane-d6 (DMC)
Cyclohexane
Methylcyclohexane
1 ,2-Dichloropropane
Bromodichloromethane
Chloroform-d (DMC)
1 , 1 -Dichloroethane
Bromochloromethane
Chloroform
Dibromochloromethane
Bromoform
l,l-Dichloroethene-d2 (DMC)
trans- 1,2-Dichloroethene
cis-l,2-Dichloroethene
1 , 1 -Dichloroethene
Benzene-d6 (DMC)
Benzene
l,2-Dichlorobenzene-d4 (DMC)
Chlorobenzene
1 , 3 -Dichlorobenzene
1 ,4-Dichlorobenzene
1 ,2-Dichlorobenzene
1 ,2,4-Trichlorobenzene
1 ,2,3 -Trichlorobenzene
2-Hexanone-d5 (DMC)
4-Methyl -2 -pentanone
2-Hexanone
1 , 1 ,2,2-Tetrachloroethane-d2
(DMC)
1 , 1 ,2,2,-Tetrachlororethane
1 ,2-Dibromo-3 -chloropropane
Toluene-d8 (DMC)
Trichloroethene
Toluene
Tetrachloroethene
Ethylbenzene
o-Xylene
m,p-Xylene
Styrene
Isopropylbenzene
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Methylene chloride
Methyl-tert-butyl ether
1,1,1 -Trichloroethane
Carbon tetrachloride
1,2-Dibromoethane
1,2-Dichloroethane
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VII. Matrix Spike/Matrix Spike Duplicate
A. Review Items
Cover Page, Form 3A-OR, chromatograms, and quantitation reports.
B. Objective
The objective of the 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. Criteria
1. If requested, MS/MSD samples should be prepared and analyzed at the specified frequency. One
pair of MS/MSD should be analyzed per matrix or per SDG.
NOTE: Data for MS and MSDs will not be present unless requested by the Region.
2. Samples identified as field blanks or Performance Evaluation (PE) samples cannot be used for
spiked sample analysis.
3. The MS/MSD %R and the Relative Percent Difference (RPD) between MS and MSD results
should be calculated according to the method.
4. The MS/MSD %R and RPD should be within the acceptance limits in Table 23.
D. Evaluation
1. Verify that requested MS/MSD samples were analyzed at the required frequency.
2. Verify that a field blank or PE sample was not used for MS/MSD analysis.
3. Verify that the recalculated MS/MSD %R and RPD values agree with the laboratory reported
values on Form 3A-OR.
4. Inspect the MS/MSD %R and RPD on Form 3 A-OR and verify that they are within the limits listed
in Table 23.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the non-compliant MS/MSD %R or RPD can be obtained
from the NFG reports and may be used as part of the evaluation process.
E. Action
1. If the requested MS/MSD samples were not analyzed at the specified frequency, use professional
judgment to determine the impact on sample data, if any; obtain additional information from the
laboratory, if necessary. Record the situation in the Data Review Narrative and note it for
laboratory CLP PO action. It is not likely that data qualification will be warranted if any of the
frequency requirements are not met. Carefully consider all factors, known and unknown, about
method performance on the matrix at hand, in lieu of MS/MSD data.
2. If a field blank or PE sample is used for the MS/MSD analysis, note this for laboratory CLP PO
action. All of the other QC data must then be carefully checked. Use professional judgment when
evaluating the data.
3. If the MS/MSD %R or RPD is outside the acceptance limits in Table 23, qualify the detects and
non-detects in the original sample to include the consideration of the existence of interference in the
raw data. Considerations include, but are not limited to:
a. If the MS/MSD %R is < 20%, qualify detects as estimated (J) and non-detects as unusable (R).
b. If the MS/MSD %R is > 20% and < the lower acceptance limit, qualify detects as estimated (J)
and non-detects as estimated (UJ).
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c. If the MS/MSD %R or RPD is > lower acceptance limit and < upper acceptance limit, detects
and non-detects should not be qualified.
d. If the MS/MSD%R or RPD is > the upper acceptance limit, qualify detects as estimated (J).
Non-detects should not be qualified.
Table 23. MS/MSD %R and RPD Limits for Low/Medium Volatile Analysis
Analyte
1 , 1 -Dichloroethene
Trichloroethene
Benzene
Toluene
Chlorobenzene
%R for Water
Sample
61 - 145
71 - 120
76 - 127
76 - 125
75 - 130
RPD for Water
Sample
0-14
0-14
0-11
0-13
0-13
%R for
Soil/Sediment
Sample
59 - 172
62 - 137
66 - 142
59-139
60-133
RPD for
Soil/Sediment
Sample
0-22
0-24
0-21
0-21
0-21
Table 24. MS/MSD Actions for Low/Medium Volatile Analysis
Criteria
%R < 20%
20% < %R< Lower Acceptance Limit
Lower Acceptance Limit < %R or RPD < Upper
Acceptance Limit
%R or RPD> Upper Acceptance Limit
Action
Detect
J
J
No qualification
J
Non-detect
R
UJ
No qualification
No qualification
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VIII. Internal Standard
A. Review Items
Form 8A-OR, quantitation reports, and chromatograms.
B. Objective
The objective is to evaluate the internal standard performance to ensure that GC/MS sensitivity and
response are stable during each analysis.
C. Criteria
1. The internal standard solution must be added to all samples and blanks at the specified
concentration. The internal standard solution must contain all internal standard compounds
specified in the method.
2. The area response of each internal standard compound in all samples and blanks must be within the
inclusive ranges of 50-200% of the area response of the same internal standard from the associated
opening CCV or the mid-point standard CSS from the associated ICAL.
3. The RT of the internal standard compound in the sample or blank must not vary more than ±10.0
seconds from the RT of the same internal standard compound in the associated opening CCV or
mid-point standard CSS from the associated ICAL.
D. Evaluation
1. Verify that all required internal standard compounds were added to sample and blank analyses at
the specified concentrations.
2. Check raw data (e.g., chromatograms and quantitation reports) to verify that the RT and area
response of each internal standard compound in a sample or blank are reported on the Internal
Standard Area and Retention Time Summary Form 8A-OR.
3. Verify that the RTs and area responses for all internal standard compounds are within the specified
criteria. If internal standard RTs are significantly different from the associated CCV or ICAL
midpoint, i.e., more than 10 seconds, the internal standard peak may have been misidentified, but
most likely a change in the chromatographic system should be suspected. This could be an
improper desorb/injection cycle, a leak in the purge/trap/GC system, or the effect of a highly
contaminated matrix. Normally, the area counts will also suffer in this situation, but even if they
appear unaffected, both quantitative and qualitative results should be considered highly suspect.
4. If there is a reanalysis for a particular sample, determine which analysis is the best data to report.
Considerations include, but are not limited to:
a. Magnitude and direction of the internal standard area response shift.
b. Magnitude and direction of the internal standard RT shift.
c. Technical holding times.
d. Comparison of the values of the target analytes reported in each method.
e. Other QC information.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the non-compliant internal standard area response or RT
can be obtained from the NFG reports and may be used as part of the evaluation process.
E. Action
NOTE: Apply the action to the target analytes in samples or blanks that are associated to the
non-compliant internal standard compound. The internal standard and the associated target
analytes are in Exhibit D Low/Med VOA Section 17 Table 9 of the SOW.
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1. If required internal standard compounds are not added to a sample or blank, qualify detects and
non-detects as unusable (R).
2. If the required internal standard compound is not analyzed at the specified concentration in a
sample or blank, use professional judgment to qualify detects and non-detects.
3. If the area response of an internal standard compound in a sample or blank is < 20% of the area
response of the same internal standard compound in the associated opening CCV or mid-point
standard CSS from the associated ICAL, qualify detects as estimated high (J+) and non-detects as
unusable (R).
4. If the area response of an internal standard compound in a sample or blank is > 20%, and < 50% of
the area response of the same internal standard in the associated opening CCV or mid-point
standard CSS from the associated ICAL, qualify detects as estimated high (J+) and non-detects as
unusable (UJ).
5. If the area response of an internal standard compound in a sample or blank is within the inclusive
range of 50-200% of the area response of the same internal standard compound in the associated
opening CCV or mid-point standard CSS from the associated ICAL, detects and non-detects should
not be qualified.
6. If the area response of an internal standard compound in a sample or blank is > 200% of the area
response of the same internal standard compound in the associated opening CCV or mid-point
standard CSS from the associated ICAL, qualify detects as estimated low (J-). Non-detects should
not be qualified.
7. If the RT shift between sample/blank and the associated opening CCV or mid-point standard CSS
from the associated ICAL of an internal standard compound is > 10.0 seconds, qualify detects and
non-detects as unusable (R). The Regional CLP PO should be contacted to arrange for reanalysis.
8. If the RT shift between sample/blank and the associated opening CCV or mid-point standard CSS
from the associated ICAL of an internal standard compound is < 10.0 seconds, detects and
non-detects should not be qualified.
9. If the internal standard performance criteria are grossly exceeded, annotate the potential effects on
the data in the Data Review Narrative and note it for laboratory CLP PO action.
Table 25. Internal Standard Actions for Low/Medium Volatile Analysis
Criteria
Area response < 20% of the opening CCV or mid-point
standard CSS from initial calibration
20% < area response < 50% of the opening CCV or mid-point
standard CSS from initial calibration
50% < area response < 200% of the opening CCV or
mid-point standard CSS from initial calibration
Area response > 200% of the opening CCV or mid-point
standard CSS from initial calibration
RT shift between sample/blank and opening CCV or
mid-point standard CSS from initial calibration > 10.0
seconds
RT shift between sample/blank and opening CCV or
mid-point standard CSS from initial calibration < 10.0
seconds
Action
Detect
J+
J+
No qualification
J-
R
No qualification
Non-detect
R
UJ
No qualification
No qualification
R
No qualification
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IX. Target Analyte Identification
A. Review Items
Form 1A-OR, quantitation reports, mass spectra, and chromatograms.
B. Objective
The objective is to provide acceptable GC/MS qualitative analysis to minimize the number of erroneous
analyte identifications.
C. Criteria
1. The mass spectrum of the analyte from the sample analysis must match that of the same analyte in
the associated opening CCV or mid-point standard CSS from the associated ICAL according to the
following criteria:
a. All ions present in the calibration standard mass spectrum must be present in the sample
spectrum at relative intensity > 10%.
b. The relative intensities of these ions must agree within ±20% between the standard and sample
spectra (e.g., for an ion with an abundance of 50% in the standard spectrum, the corresponding
sample ion abundance must be between 30-70%).
c. Ions present at > 10% in the sample mass spectrum, but not present in the standard spectrum,
must be evaluated by a reviewer experienced in mass spectral interpretation.
2. The Relative Retention Time (RRT) for a positively identified target analyte must be within ±0.06
RRT units of the RRT for the same analyte in the associated opening CCV or mid-point standard
CSS from the associated ICAL.
D. Evaluation
1. Verify that the positively identified target analyte mass spectrum meets the specified criteria. If not,
examine the sample target analyte spectra for the presence of interference at one or more mass
fragment peaks. Although the presence of a co-eluting interferent may preclude positive
identification of the analyte, the presumptive evidence of its presence may be useful information to
include in the Data Review Narrative.
2. Verify that the RRT of the positively identified target analyte is within ±0.06 RRT units of the RRT
for the same analyte in the associated opening CCV or mid-point standard CSS from the associated
ICAL.
3. Be aware of situations when sample carryover is a possibility and use professional judgment to
determine if instrument cross-contamination has affected any positive analyte identification. An
instrument blank must be analyzed after a sample containing target analytes with concentrations
exceeding the ICAL range (200 ug/L for non-ketones, 400 ug/L for ketones), non-target
compounds at concentrations > 200 ug/L, or saturated ions from an analyte (excluding the analyte
peaks in the solvent front).
4. Verify that peaks are correctly identified as target analytes, TICs, DMCs, or internal standards on
the chromatogram for samples and blanks.
5. Verify that there is no erroneous analyte identification, either false positive or false negative, for
each target analyte. The positively identified target analytes can be more easily detected for false
positives than false negatives. More information is available for false positives due to the
requirement for submittal of data supporting positive identifications. Non-detected target analytes,
on the other hand, are more difficult to assess. One example of the detection of false negatives is
reporting a target analyte as a TIC.
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NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the non-compliant TICs can be obtained from the CCS
report and may be used as part of the evaluation process.
NOTE: A target analyte reported as a false negative may not have the best match in a TIC search of
a contaminated sample, but its mass spectrum may be present under that of a reported TIC.
E. Action
1. If the positively identified target analyte mass spectrum does not meet the specified criteria, qualify
detect as unusable (R) or report the result at CRQL and qualify as non-detect (U).
2. If the RRT for a positively identified target analyte is outside the specified RRT windows, qualify
detects as unusable (R) or report the result at CRQL and qualify as non-detect (U).
3. If it is determined that cross-contamination has occurred, use professional judgment to qualify
detects. Annotate any changes made to the reported analytes due to either false positive or negative
identifications, or concerns regarding target analyte identifications in the Data Review Narrative.
Note the necessity for numerous or significant changes for laboratory CLP PO action.
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X. Target Analyte Quantitation and Reported Contract Required Quantitation Limit
A. Review Items
Form 1A-OR, sample preparation sheets, SDG Narrative, quantitation reports, and chromatograms.
B. Objective
The objective is to ensure that the reported results and CRQLs for target analytes are accurate.
C. Criteria
1. Target analyte results and sample specific CRQLs must be calculated according to the correct
equations.
2. Target analyte RRF must be calculated using the correct associated internal standard, as listed in
the method. Quantitation must be based on the quantitation ion (m/z) specified in the method for
both the internal standards and target analytes. Target analyte result must be calculated using the
RRF from the associated ICAL.
D. Evaluation
1. Verify that the results for all positively identified analytes are calculated and reported by the
laboratory. Verify that the CRQLs are calculated for the non-detects and reported accordingly.
2. Verify that the correct internal standard, quantitation ion, and RRF are used to calculate the
reported results.
3. Verify that the same internal standard, quantitation ion, and RRF are used consistently.
4. Verify that the sample specific CRQLs have been calculated and adjusted to reflect Percent Solids
(%Solids), original sample mass/volume, and sample dilutions.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the non-compliant results or CRQLs can be obtained from
the CCS report and may be used as part of the evaluation process
E. Action
1. If any discrepancies are found, contact the Regional CLP PO, who may contact the laboratory to
obtain additional information that could resolve any differences. If a discrepancy remains
unresolved, use professional judgment to decide which value is the most accurate and whether
qualification of data is warranted. Annotate the reasons for any data qualification in the Data
Review Narrative.
2. If errors are detected in results and CRQL calculations, perform a more comprehensive
recalculation.
3. If %Solids for a soil sample is < 10.0%, use professional judgment to qualify detects and
non-detects.
4. If %Solids for a soil sample is > 10.0 and < 30.0%, use professional judgment to qualify detects and
non-detects.
5. If %Solids for a soil sample is > 30.0%, detects and non-detects should not be qualified.
6. If sample results are < CRQLs and > MDLs, qualify as estimated (J).
7. Note numerous or significant failures to accurately quantify the target analytes, or to properly
evaluate and adjust CRQLs, for laboratory CLP PO action.
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Low/Medium VGA
Table 26. Percent Solids Actions for Low/Medium Volatile Analysis for Non-Aqueous Samples
Criteria
%Solids<10.0%
10.0% < %Solids < 30.0%
%Solids > 30.0%
Action
Detects
Use professional judgment
Use professional judgment
No qualification
Non-detects
Use professional judgment
Use professional judgment
No qualification
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XI. Tentatively Identified Compounds
A. Review Items
Form 1B-OR, chromatograms, library search printouts, and spectra for the TIC candidates.
B. Objective
The objective is to provide tentative identifications to chromatographic peaks that are not identified as
target analytes, DMCs, or internal standards.
C. Criteria
For each sample, the laboratory must conduct a mass spectral search of the National Institute of
Standards and Technology/U.S. Environmental Protection Agency/National Institutes of Heath
[(NIST/EPA/NH) 2011 release or later], and/or Wiley (2011 release or later), or equivalent mass
spectral library, and report the possible identity for up to 30 of the largest peaks that are not DMCs,
internal standards, or target analytes. The peak for a TIC should have an area or height > 10% of the
area or height of the nearest internal standard. The estimated concentration for a TIC is calculated
similarly to that for a target analyte, using total ion areas for the TIC and the internal standard, and
assuming a RRF of 1.0.
1. Guidelines for tentative identification are as follows:
a. Major ions (> 10% Relative Intensity) in the reference spectrum should be present in the
sample spectrum.
b. The relative intensities of the major ions should agree within ±20% between the sample and the
reference spectra.
c.
1^-L^l^llVV^ OJJ^VLICI.
Molecular ions present in the reference spectrum should be present in the sample spectrum.
TWT j. j. i_ •• _ i :i I. j._i- _j?o£-n/ I. • i • i i_
Non-target compounds receiving a library search match of 85% or higher are considered a
"likely match." The compound should be reported unless the mass spectral interpretation
specialist feels there is evidence not to report the compound as identified by the library search
program. The laboratory should include the justification for not reporting a compound as listed
by the search program in the SDG Narrative.
e. If the library search produces more than one compound > 85%, the compound with the highest
percent match (report first compound if percent match is the same for two or more compounds)
should be reported, unless the mass spectral interpretation specialist feels that the highest
match compound should not be reported, or another compound with a lower match should be
reported. The laboratory should include the justification for not reporting the compound with
the highest spectral match within the SDG Narrative. DMCs, internal standards, and target
analytes should not be reported as TICs.
f If the library search produces a series of obvious isomer compounds with library search
matches > 85%, the compound with the highest library search percent match (or the first
compound if the library search matches are the same) should be reported. The laboratory
should note in the SDG Narrative that the exact isomer configuration, as reported, may not be
accurate.
g. If the library search produces no matches > 85% and, in the technical judgment of the mass
spectral interpretation specialist no valid tentative identification can be made, the compound
should be reported as unknown. The mass spectral specialist should give additional
classification of the unknown compound, if possible (e.g., unknown aromatic, unknown
hydrocarbon, unknown acid type, unknown chlorinated compound). If probable molecular
weights can be distinguished, they should be included.
h. The Chemical Abstracts Service (CAS) registry number is the unique identifier for each
chemical compound. As the rules of chemical nomenclature have changed overtime, each
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chemical substance is liable to have several names or synonyms [i.e., trade or brand name(s);
generic or common name(s); trivial or systematic; or International Union of Pure and Applied
Chemistry (IUPAC) name(s)]. Whether synonyms or other names are created for this
compound, the CAS registry number will remain unchanged. The CAS registry number is
simply an identifier which has no structural significance. Regardless of RTs, if the library
search produces two or more compounds at or above 85% with the same CAS number, the
compound with the highest percent match (report first compound if the percent match is the
same for two or more compounds) should be reported unless the mass spectral interpretation
specialist feels there is just evidence not to report the compound with the highest match.
i. If the library search produces only one and the same compound (i.e., the same CAS registry
number) with the match at or above 85% at two different RTs, the compound having the
highest percent match should be reported as TIC and the other one could be reported as
unknown. If both TICs have the same percent match for the same compound, one of the TICs
could be reported as unknown. Such justifications should be included in the SDG Narrative.
j. Alkanes are not to be reported as TICs on Form 1B-OR. An alkane is defined as any
hydrocarbon with the generic formula CnH2n+2 containing only C-H and C-C single bonds.
When the preceding alkanes are tentatively identified, the concentration(s) should be estimated
and the analytes reported as alkanes by class (i.e., straight-chain, branched, cyclic, as a series,
or as applicable) in the SDG Narrative. Total alkanes concentration should be reported on
Form 1B-OR.
D. Evaluation
1. Verify that the laboratory has generated a library search for all required peaks in the
chromatograms for samples and blanks.
2. Verify that TIC peaks present in samples are not found in blanks. When a low-level, non-target
compound that is a common artifact or laboratory contaminant is detected in a sample, a thorough
check of blank chromatograms may require looking for peaks which are < 10% of the internal
standard height, but present in the blank chromatogram at a similar RRT.
3. Verify that mass spectra for all reported TICs are present for every sample and blank.
4. Review ions present in the sample spectrum, but not in the reference spectrum, for possible
background contamination, interference, or presence of coeluting compounds.
5. Review ions present in the reference spectrum, but not in the sample spectrum, for possible
subtraction from the sample spectrum because of background contamination or coeluting
compounds. Data system library reduction programs can sometimes create these discrepancies.
6. Consider all reasonable choices since TIC library searches often yield several candidate
compounds having a close matching score.
7. Be aware of common laboratory artifacts/contaminants and their sources (e.g., Aldol condensation
products, solvent preservatives, and reagent contaminants). These may be present in blanks and not
reported as sample TICs, such as:
a. Common laboratory contaminants include CO2 (m/z 44), siloxanes (m/z 73), diethyl ether,
hexane, certain freons, and phthalates at levels < 100 (ig/L.
b. Solvent preservatives include cyclohexene (a methylene chloride preservative). Related
by-products include cyclohexanone, cyclohexenone, cyclohexanol, cyclohexenol,
chlorocyclohexene, and chlorocyclohexanol.
c. Aldol condensation reaction products of acetone include: 4-hydroxy-4-methyl-2-pentanone,
4-methyl-2-penten-2-one, and 5,5-dimethyl-2(5H)-furanone.
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8. A target analyte may be identified by non-target library search procedures, even though it is not
identified as a target analyte (false negative). If the total area quantitation method is used, request
that the laboratory recalculate the result using the proper quantitation ion and RRF.
a. A non-target compound may be incorrectly identified by the instrument's target analyte data
processor as a target analyte (false positive). When this happens, the non-target library search
procedure will not detect the false positive as a TIC. In this case, request that the laboratory
properly identify the analyte as a TIC and recalculate the result using the total area quantitation
method and a RRF of 1.0.
b. Evaluate other sample chromatograms and check for both false negatives and false positives to
determine if the occurrence is isolated or systematic.
9. Verify that the TIC concentration is calculated using an RRF of 1.0.
E. Action
1. If the library search match for a TIC is > 85%, qualify the TIC as tentatively identified with
estimated concentration (NJ).
2. If the library search match for a TIC is < 85%, qualify the TIC as unknown with estimated
concentration (J).
3. General actions related to the review of TIC results are as follows:
a. If it is determined that a tentative identification of a non-target compound is unacceptable,
change the tentative identification to "unknown" or another appropriate identification, and
qualify the result as estimated (J).
b. If library search or proper calculation is not performed for all contractually-required peaks, the
Regional CLP PO may request the data from the laboratory.
c. Use professional judgment to determine whether a library search result for a TIC represents a
reasonable identification. If there is more than one possible match, report the result as "either
compound X or compound Y." If there is a lack of isomer specificity, change the TIC result to
a non-specific isomer result (e.g., 1,3,5-trimethyl benzene to trimethyl benzene isomer) or to a
compound class (e.g., 2-methyl, 3-ethyl benzene to a substituted aromatic compound).
d. Other Case factors may influence TIC judgments. If a sample TIC match is poor, but other
samples have a TIC with a valid library match, similar RRT, and the same ions, infer
identification information from the other sample TIC results.
4. Note any changes made to the reported data or any concerns regarding TIC identifications in the
Data Review Narrative.
5. Note any failure to properly evaluate and report TICs for laboratory CLP PO action.
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XII. System Performance
A. Review Items
Form 8A-OR and chromatograms.
B. Objective
The objective is to ensure that the system is stable during the analytical sequence to produce quality
data.
C. Criteria
There are no specific criteria for system performance.
D. Evaluation
1. Abrupt discrete shifts in the Reconstructed Ion Chromatogram (RIC) baseline may indicate a
change in the instrument's sensitivity or the zero setting. A baseline "shift" could indicate a
decrease in sensitivity in the instrument or an increase in the instrument zero, possibly causing
target compounds at or near the detection limit to miss detection. A baseline "rise" could indicate
problems such as a change in the instrument zero, a leak, or degradation of the column.
2. Poor chromatographic performance affects both qualitative and quantitative results. Indications of
substandard performance include:
a. High RIC background levels or shifts in Absolute RTs of internal standards.
b. Excessive baseline rise at elevated temperature.
c. Extraneous peaks.
d. Loss of resolution.
e. Peak tailing or peak splitting that may result in inaccurate quantitation.
3. A drift in instrument sensitivity may occur during the 12-hour period and may be an indication of
possible internal standard spiking problems. This could be discerned by examination of the internal
standard area on Form 8A-OR for trends such as a continuous or near-continuous increase or
decrease in the internal standard area over time.
E. Action
1. Use professional judgment to qualify the data if it is determined that system performance has
degraded during sample analyses.
2. Note any degradation of system performance which significantly affected the data for laboratory
CLP PO action.
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XIII. Regional Quality Assurance and Quality Control
A. Review Items
Form 1A, chromatograms, TR/COC documentation, quantitation reports, and other raw data from
QA/QC samples.
B. Objective
The objective is to use results from the analysis of the Regional QA/QC samples including field
duplicates, PE samples, blind spikes, and blind blanks to determine the validity of the analytical results.
C. Criteria
Criteria are determined by each Region.
1. PE sample frequency may vary.
2. The target analytes present in the PE sample must be correctly identified and quantified.
3. The RPD between field duplicates shall fall with the specific limits in the Region's Standard
Operating Procedure (SOP) or project QAPP.
D. Evaluation
1. Evaluation procedures must follow the Region's SOP for data review. Each Region will handle the
evaluation of PE samples on an individual basis.
2. Verify that the target analyte in PE sample is properly identified and that the result is calculated
correctly.
3. Verify that the acceptance criteria for the specific PE sample are met, if available.
4. Calculate the RPD between field duplicates and provide this information in the Data Review
Narrative. Also verify that the value falls within the specific limits in the Region's SOP or project
QAPP.
E. Action
1. Any action must be in accordance with Regional specifications and the criteria for acceptable PE or
field duplicate sample results.
2. Note unacceptable results for PE or field duplicate samples for laboratory CLP PO action.
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XIV. Overall Assessment of Data
A. Review Items
Entire data package, data review results, and (if available), the QAPP and Sampling and Analysis Plan
(SAP).
B. Objective
The objective is to provide the overall assessment on data quality and usability.
C. Criteria
1. Review all available materials to assess the overall quality of the data, keeping in mind the additive
nature of analytical problems.
2. Reported analyte concentrations must be quantitated according to the appropriate analytical
method, as listed in the method. All sample results must be within the linear calibration ranges per
methods.
D. Evaluation
Examine the raw data to verify that the correct calculation of the sample results was reported by the
laboratory. Analysis logs, instrument printouts, etc., should be compared to the reported sample results
recorded on the appropriate Organic Summary Forms (Form 1A-OR through Form 8A-OR).
1. Evaluate any technical problems which have not been previously addressed.
2. Examine the raw data for any anomalies (e.g, baseline shift).
3. Verify that the appropriate method is used in sample analysis.
4. Verify that there are no transcription or reduction errors.
5. Verify that target analyte results fall within the calibrated ranges.
6. If appropriate information is available, use professional judgment to assess the usability of the data
in order to assist the data user in avoiding inappropriate use of the data. Review all available
information, including the QAPP (specifically the acceptance and performance criteria), SAP, and
communication with the data user that concerns the intended use and desired quality of these data.
E. Action
1. Use professional judgment to determine if there is any need to qualify data which were not
qualified based on the QC criteria previously discussed.
2. Use professional judgment to qualify sample results and non-detects if the MDL exceeds the
CRQL.
3. If a sample is not diluted properly when sample results exceed the upper limit of the calibration
range, qualify sample results as estimated (J).
4. Write a brief Data Review Narrative to give the user an indication of the limitations of the
analytical data.
5. Note any inconsistency of the data with the SDG Narrative for laboratory CLP PO action. If
sufficient information on the intended use and required quality of the data is available, include an
assessment of the usability of the data within the given context. This may be used as part of a
formal Data Quality Assessment (DQA).
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SEMIVOLATILE DATA REVIEW
The Semivolatile (SVGA) organic data requirements to be reviewed during validation are listed below:
I. Preservation and Holding Times 97
II. Gas Chromatograph/Mass Spectrometer Instrument Performance Check 101
III. Initial Calibration 109
IV. Continuing Calibration Verification 116
V. Blanks 119
VI. Deuterated Monitoring Compound 122
VII. Matrix Spike/Matrix Spike Duplicate 126
VIII. Gel Permeation Chromatography Performance Check 128
IX. Internal Standard 130
X. Target Analyte Identification 132
XI. Target Analyte Quantitation and Reported Contract Required Quantitation Limit 134
XII. Tentatively Identified Compounds 136
XIII. System Performance 139
XIV. Regional Quality Assurance and Quality Control 140
XV. Overall Assessment of Data 141
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I. Preservation and Holding Times
A. Review Items
Form 1A-OR, Form 1B-OR, Traffic Report/Chain of Custody (TR/COC) documentation, raw data,
sample extraction sheets, and the Sample Delivery Group (SDG) 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 sample condition and the
holding time of the sample.
C. Criteria
1. The extraction technical holding time is determined from the date of sample collection to the date
of sample extraction for aqueous and non-aqueous (soil and sediment) samples that are not
designated for Toxicity Characteristic Leaching Procedure (TCLP)/ Synthetic Precipitation
Leachate Procedure (SPLP) procedures. The extraction technical holding time for samples
designated for TCLP/SPLP is determined from the date of sample collection to the date of
TCLP/SPLP extraction.
2. For TCLP/SPLP leachate samples, extraction technical holding time is determined from the date of
TCLP/SPLP procedure completion to the date of the leachate sample extraction by the specified
preparation methods for aqueous samples. The analysis technical holding time is determined from
the date of sample extraction completion to the date of sample analysis.
3. Samples shall be in proper condition with shipping container temperatures at < 6°C upon receipt at
the laboratory. All aqueous and non-aqueous samples shall be protected from light and refrigerated
at < 6°C (but not frozen) from the time of receipt at the laboratory. The sample extracts shall be
stored at < 6°C (but not frozen) from the time of the extraction completion until analysis.
4. The extraction technical holding time criteria for aqueous samples, TCLP/SPLP aqueous samples,
and TCLP/SPLP leachate samples that are properly preserved is 7 days.
5. The extraction technical holding time criteria for soil samples designated for TCLP/SPLP is 14
days.
6. The extraction technical holding time criteria for non-aqueous samples that are properly preserved
is 14 days.
7. The analysis technical holding time criteria for extracts including TCLP/SPLP leachate sample
extract is 40 days.
D. Evaluation
1. Review the SDG Narrative and the TR/COC documentation to determine if the samples are
received intact and iced. If there is an indication of problems with the samples, the sample integrity
may be compromised.
2. Verify that the extraction dates and the analysis dates for samples on Form 1A-OR and Form
IB-OR and the raw data/SDG File are identical.
3. Establish extraction technical holding times for samples excluding TCLP/SPLP leachate by
comparing the sample collection dates on the TR/COC documentation with the dates of extraction
on Form 1A-OR and Form IB-OR, and the sample extraction sheets.
4. Establish extraction technical holding times for samples undergone TCLP/SPLP procedure by
comparing the sample collection dates on the TR/COC documentation with the dates of extraction
on sample extraction sheets.
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5. Establish extraction technical holding times for TCLP/SPLP leachates by comparing the dates of
TCLP/SPLP extraction on extraction sheets with the dates of extraction on Form 1A-OR, Form
IB-OR and preparative extraction log.
6. Determine the analysis technical holding times for samples after the completion of extraction by
comparing the dates of extraction with the dates of analysis on Form 1A-OR and Form 1B-OR, as
well as from the analytical run logs.
E. Action
1. If samples are received with shipping container temperatures > 6°C, use professional judgment to
qualify detects and non-detects.
2. If TCLP/SPLP is performed within the 14-day extraction technical holding time for soil samples
designated for TCLP/SPLP, detects and non-detects should not be qualified.
3. If TCLP/SPLP is performed outside the 14-day extraction technical holding time for soil samples
designated for TCLP/SPLP, qualify detects as estimated low (J-) and non-detects as unusable (R).
Use caution in determining whether some detected analytes should be qualified as estimated low
(J-) or as estimated high (J+), based on knowledge of individual analyte stability or interactions.
4. If discrepancies are found between the sample extraction date or analysis date and the date on raw
data, perform a more comprehensive review, contacting the laboratory if necessary through the
Regional Contract Laboratory Program Project Officer (CLP PO), to determine the correct dates
for establishing technical holding times.
5. If an aqueous, TCLP/SPLP aqueous sample, or TCLP/SPLP leachate sample is not properly
preserved, but extraction is performed within the 7-day technical holding time, and the extract is
analyzed within the 40-day technical holding time, consider the extent of temperature excursion in
addition to overall sample integrity and use professional judgment to qualify detects and
non-detects.
6. If an aqueous, TCLP/SPLP aqueous sample, or TCLP/SPLP leachate sample is not properly
preserved, extraction is performed outside the 7-day technical holding time, and the extract is
analyzed outside the 40-day technical holding time, qualify detects as estimated (J) and non-detects
as unusable (R). Use caution in determining whether some detected analytes should be qualified as
estimated low (J-) or as estimated high (J+), based on knowledge of individual analyte stability or
interactions.
7. If an aqueous, TCLP/SPLP aqueous sample, or TCLP/SPLP leachate sample is properly preserved,
extraction is performed within the 7-day technical holding time, and the extract is analyzed within
the 40-day technical holding time, detects and non-detects should not be qualified.
8. If an aqueous, TCLP/SPLP aqueous sample, or TCLP/SPLP leachate sample is properly preserved,
extraction is performed outside the 7-day technical holding time, and the extract is analyzed outside
the 40-day technical holding time, consider all evidence of compromised extract integrity (such as
evaporation, refrigeration), in addition to overall sample integrity and use professional judgment to
qualify the data, in particular the direction of the bias.
9. If a non-aqueous sample is not properly preserved, extraction is performed within the 14-day
technical holding time, and the extract is analyzed within the 40-day technical holding time, use
professional judgment to qualify detects and non-detects.
10. If a non-aqueous sample is not properly preserved, extraction is performed outside the 14-day
technical holding time, and the extract is analyzed outside the 40-day technical holding time, use
professional judgment to qualify detects and non-detects.
11. If a non-aqueous sample is properly preserved, extraction is performed within the 14-day technical
holding time, and the extract is analyzed within the 40-day technical holding time, detects and
non-detects should not be qualified.
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12. If a non-aqueous sample is properly preserved, extraction is performed outside the 14-day technical
holding time, and the extract is analyzed outside the 40-day technical holding time, qualify detects
as estimated low (J-) and non-detects as unusable (R). Use caution in determining whether some
detected analytes should be qualified as estimated low (J-) or as estimated high (J+), based on
knowledge of individual analyte stability or interactions.
13. Note the effect of exceeding the holding time on the resulting data in the Data Review Narrative,
whenever possible.
14. If technical holding times are grossly exceeded, qualify detects as estimated low (J-) and use
professional judgment to qualify non-detects as unusable (R). Note this for CLP PO action.
15. If samples are received with shipping container temperatures > 10°C, use professional judgment to
qualify detects and non-detects.
Table 27. Preservation and Holding Time Actions for Semivolatile Analysis
Matrix
Aqueous
Preserved
No
No
Yes
Yes
Yes/No
Criteria
< 7 days (for extraction) and
< 40 days (for analysis)
TCLP/SPLP aqueous and
TCLP/SPLP leachate
samples extracted within the
7-day technical holding
time
> 7 days (for extraction) and
> 40 days (for analysis)
TCLP/SPLP aqueous and
TCLP/SPLP leachate
samples not extracted
within the 7-day technical
holding time
< 7 days (for extraction) and
< 40 days (for analysis)
TCLP/SPLP aqueous and
TCLP/SPLP leachate
sampes extracted within the
7-day technical holding
time
> 7 days (for extraction) and
> 40 days (for analysis)
TCLP/SPLP aqueous and
TCLP/SPLP leachate
samples not extracted
within the 7-day technical
holding time
Holding time grossly
exceeded
Action
Detect
Non-Detect
Use professional judgment
J
Use professional
judgment
No qualification
J
J
UJ
UJorR
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Matrix
Non-aqueous
Preserved
No
No
Yes
Yes
Yes/No
Criteria
< 14 days (for extraction)
and < 40 days (for analysis)
> 14 days (for extraction)
and > 40 days (for analysis)
< 14 days (for extraction)
and < 40 days (for analysis)
> 14 days (for extraction)
and > 40 days (for analysis)
Holding time grossly
exceeded
Action
Detect
Non-Detect
Use professional judgment
J
Use professional
judgment
No qualification
J
J
UJ
UJorR
Table 28. Holding Time Actions for Non-Aqueous Semivolatile TCLP/SPLP Sample Analysis
Preserved
No
No
Yes
Yes
Yes/No
Criteria
TCLP/SPLP performed
within the 14-day technical
holding time
TCLP/SPLP not performed
within the 14-day technical
holding time
TCLP/SPLP performed
within the 14-day technical
holding time
TCLP/SPLP not performed
within the 14-day technical
holding time
Holding time grossly
exceeded
Action
Detect
Non-Detect
Use professional judgment
J
Use professional
judgment
No qualification
J
J
UJ
UJorR
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II. Gas Chromatograph/Mass Spectrometer Instrument Performance Check
A. Review Items
Form 5-OR, decafluorotriphenylphosphine (DFTPP) mass spectra, and mass listing.
B. Objective
The objective of performing Gas Chromatograph/Mass Spectrometer (GC/MS) instrument
performance checks is to ensure adequate mass resolution, identification, and to some degree,
sensitivity, and to document this level of performance prior to analyzing any sequence of standards or
samples.
C. Criteria
NOTE:
This requirement does not apply when samples are analyzed by the Selected Ion
Monitoring (SIM) technique.
1. A sufficient amount of the instrument performance check solution (50 ng DFTPP on-column) must
be analyzed at the specified frequency and sequence. It must be injected once at the beginning of
each 12-hour period, during which samples, blanks, or standards are to be analyzed. The 12-hour
period begins with either the injection of DFTPP, or in cases where a closing Continuing
Calibration Verification (CCV) can be used as an opening CCV, the 12-hour period begins with the
injection of the opening CCV.
Listed below are examples of acceptable analytical sequences incorporating the use of the opening
and/or closing CCV. Use these examples as a guide for the possible analytical sequences that can
be expected.
Conditions for When
Example Sequence is
Appropriate:
Acceptable Criteria That Must
Be Met:
Notes:
Use Example 1 if time
remains on the 12-hour
clock after the initial
calibration sequence.
DFTPP tunes meet instrument
performance criteria.
The five Initial Calibration
standards meet initial
calibration criteria.
CCV A meets both opening
and closing CCV criteria.
CCV B meets closing CCV
criteria.
The requirement of starting the
new 12-hour clock for Analytical
Sequence 2 with a new DFTPP
tune is waived if CCV A meets
opening CCV criteria. If CCV B
meets opening CCV criteria, a
method blank and subsequent
samples may be analyzed
immediately after CCV B.
Use Example 2 if time
remains on the 12-hour
clock after the initial
calibration sequence.
DFTPP tunes meet instrument
performance criteria.
The five Initial Calibration
standards meet initial
calibration criteria.
CCV A meets closing CCV
criteria (but does not meet
opening CCV criteria).
CCV B meets opening CCV
criteria.
CCV C meets closing CCV
criteria.
CCV A does not meet opening
CCV criteria. Therefore a new
DFTPP tune must be performed,
immediately followed by CCV B,
before the method blank and any
samples may be analyzed. In this
case, the new 12-hour clock and
Analytical Sequence 2 begins
with the injection of the new
DFTPP tune.
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Conditions for When
Example Sequence is
Appropriate:
Acceptable Criteria That Must
Be Met:
Notes:
Use Example 3 if more
than 12 hours have
elapsed since the most
recent initial calibration
or closing CCV,
OR
if the most recent closing
CCV was not or could
not be used as an
opening CCV.
DFTPP tunes meet instrument
performance criteria.
CCV A meets opening CCV
criteria.
CCV B meets both opening
and closing CCV criteria.
CCV C meets both opening
and closing CCV criteria.
The requirement of starting the
new 12-hour clock for Analytical
Sequence 2 with a new DFTPP
tune is waived if CCV B meets
opening CCV criteria. If CCV C
meets opening CCV criteria, a
method blank and subsequent
samples may be analyzed
immediately after CCV B.
Use Example 4 if more
than 12 hours have
elapsed since the most
recent initial calibration
or closing CCV,
OR
if the most recent closing
CCV was not or could
not be used as an
opening CCV.
DFTPP tunes meet instrument
performance criteria.
CCV A meets opening CCV
criteria.
CCV B meets closing CCV
criteria (but does not meet
opening CCV criteria).
CCV C meets opening CCV
criteria.
CCV D meets both opening
and closing CCV criteria.
CCV B does not meet opening
CCV criteria. Therefore a new
DFTPP tune must be performed,
immediately followed by CCV C,
before the method blank and any
samples may be analyzed. In this
case, the new 12-hour clock and
Analytical Sequence 2 begins
with the injection of the new
DFTPP tune. The requirement of
starting the new 12-hour clock for
Analytical Sequence 3 with a new
DFTPP tune is waived if CCV D
meets opening CCV criteria. If
CCV D meets opening CCV
criteria, a method blank and
subsequent samples may be
analyzed immediately after CCV
D.
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Example 1:
Example 1:
Start of 12-hour clock for
Analytical Sequence 1
End of 12-hour clock for
Analytical Sequence I/
Beginning of 12-hour clock
for Analytical Sequence 2
End of 12-hour clock for
Analytical Sequence 21
Beginning of 12-hour clock
for Analytical Sequence 3
Time Material Injected
0 hr DFTPP
Initial Calibration 5.0
Initial Calibration 10
Initial Calibration 20
Initial Calibration 40
Initial Calibration 80
Method Blank
Subsequent Samples
12 hr CCV A (meets opening CCV criteria)
Method Blank
Subsequent Samples
24 hr CCV B (meets opening CCV criteria)
Analytical
Sequence #
1
1
1
1
1
1
1
1
1
1
1
1
1/2
2
2
2
2
2
2
2/3
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Example 2:
Example 2:
Start of 12-hour clock for
Analytical Sequence 1
End of 12-hour clock for
Analytical Sequence 1
Beginning of 12-hour
clock for Analytical
Sequence 2
Time Material Injected
0 hr
, ~ ,
13 hr
DFTPP
Initial Calibration 5.0
Initial Calibration 10
Initial Calibration 20
Initial Calibration 40
Initial Calibration 80
Method Blank
Subsequent Samples
CCV A (meets closing CCV criteria,
fails opening CCV criteria)
DFTPP
CCV B (meets opening CCV
criteria)
Method Blank
Subsequent Samples
Analytical
Sequence #
1
1
1
1
1
1
1
1
1
1
1
1
2
2
2
2
2
2
End of 12-hour clock for
Analytical Sequence 2
25 hr CCV C (meets closing CCV criteria)
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Example 3:
Example 3:
Start of 12-hour clock for
Analytical Sequence 1
Time Material Injected
End of 12-hour clock for
Analytical Sequence I/
Beginning of 12-hour clock
for Analytical Sequence 2
End of 12-hour clock for
Analytical Sequence 21
Beginning of 12-hour clock
for Analytical Sequence 3
Ohr
12 hr
24 hr
DFTPP
CCV A (meets opening CCV
criteria)
Method Blank
Subsequent Samples
CCV B (meets opening CCV
criteria)
Method Blank
Subsequent Samples
CCV C (meets opening CCV
criteria)
Analytical
Sequence #
1
1
1
1
1
1
1
1/2
2
2
2
2
2
2/3
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Example 4:
Example 4:
Start of 12-hour clock for
Analytical Sequence 1
End of 12-hour clock for
Analytical Sequence 1
Beginning of 12-hour
clock for Analytical
Sequence 2
End of 12-hour clock for
Analytical Sequence 21
Beginning of 12-hour
clock for Analytical
Sequence 3
Time Material Injected
Ohr
12 hr
13 hr
DFTPP
CCV A (meets opening CCV criteria)
Method Blank
Subsequent Samples
CCV B (meets closing CCV criteria,
fails opening CCV criteria)
DFTPP
CCV C (meets opening CCV criteria)
Method Blank
Subsequent Samples
25 hr CCV D (meets opening CCV criteria)
Analytical
Sequence #
1
1
1
1
1
1
1
2
2
2
2
2
2
2/3
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2. The DFTPP instrument performance check must meet the ion abundance criteria provided in Table
29.
Table 29. Ion Abundance Criteria for DFTPP
Mass
51
68
69
70
127
197
198
199
275
365
441
442
443
Ion Abundance Criteria
10.0 -80.0% of mass 198
Less than 2.0% of mass 69
Present
Less than 2.0% of mass 69
10.0- 80.0% of mass 198
Less than 2.0% of mass 198
Base peak, 100% relative abundance*
5.0 -9.0% of mass 198
10.0 -60.0% of mass 198
Greater than 1.0% of mass 198
Present, but less than mass 443
Greater than 5 0.0% of mass 198
15.0 -24.0% of mass 442
* All ion abundances must be normalized to mass-to-charge (m/z) 198, the nominal base peak, even
though the ion abundance of m/z 442 may be up to 100% that of m/z 198.
D. Evaluation
1. Verify that DFTPP Instrument Performance Check is analyzed at the specified frequency and
sequence.
2. Compare the data presented on Form 5 -OR for each Instrument Performance Check with each mass
listing submitted to ensure the following:
a. Form 5-OR is present and completed for each required DFTPP at the specified frequency.
b. The laboratory has not made transcription errors between the data and the form. If there are
major differences between the mass listing and Forms 5-OR, a more in-depth review of the data
is required. This may include obtaining and reviewing additional information from the
laboratory.
c. The appropriate number of significant figures has been reported (number of significant figures
given for each ion in the ion abundance criteria column) and that rounding is correct.
d. The laboratory has not made any calculation errors.
3. Verify from the raw data (mass spectral listing) that the mass assignment is correct and that the
mass listing is normalized to m/z 198.
4. Verify that the ion abundance criteria are met. The criteria for m/z 68, 70, 441, and 443 are
calculated by normalizing to the specified m/z. The critical ion abundance criteria for DFTPP are
the relative abundance ratios of m/z ratios for 198/199 and 442/443. Forthe ions at m/z 51, 127,
and 275, the actual relative abundance is not as critical. The relative abundance of m/z 365 is
present and > 1.0%.
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5. If possible, verify that spectra are generated using appropriate background subtraction techniques.
Since the DFTPP spectrum is obtained from chromatographic peaks that should be free from
co-elution problems, background subtraction should be performed in accordance with the
following procedure:
a. Three scans (the peak apex scan and the scans immediately preceding and following the apex)
are acquired and averaged.
b. Background subtraction must be accomplished using a single scan no more than 20 scans prior
to the elution of DFTPP. Do not subtract the DFTPP peak as part of the background.
NOTE: All mass spectrometer instrument conditions must be identical to those used for sample
analysis. Background subtraction actions resulting in spectral distortions for the sole
purpose of meeting the method specifications are contrary to the Quality Assurance (QA)
objectives, and are therefore unacceptable.
NOTE: For data obtained from the Contract Laboratory Program (CLP), information regarding
non-compliant DFTPP instrument performance check can be obtained from the National
Functional Guidelines (NFG) reports and may be used as part of the evaluation process.
E. Action
1. If instrument performance check is not analyzed at the specified frequency and sequence, qualify
detects and non-detects in the associated samples as unusable (R). The Regional CLP PO should be
contacted to arrange for reanalysis of any samples involved.
a. In the event that samples cannot be renanalyzed, examine all calibrations associated with the
sequence to evaluate whether proper qualitative criteria were achievable. If so, it may be
possible to salvage usable data from the sequence. Otherwise, qualify the data as unusable (R).
2. If minor transcription errors are found to be insignificant to data quality and can be corrected on a
copy of the form, no further actions are required.
3. If the laboratory has failed to provide the correct forms or significant transcription or calculation
errors are found, notify the Regional CLP PO, who may contact the laboratory to request the
necessary information. If the information is not available, use professional judgment to assess the
data, and notify the laboratory's CLP PO.
4. If mass assignment is in error (e.g., m/z 197 is indicated as the base peak rather than m/z 198),
qualify detects and non-detects in the associated samples as unusable (R).
5. If ion abundance criteria in Table 29 are not met, use professional judgment to qualify detects and
non-detects in the associated samples.
6. If ion abundance criteria is not met for ions at m/z 51, 127, and 275, detects and non-detects should
not be qualified.
7. If ion abundance at m/z 365 is zero, minimum detection limits may be affected. On the other hand,
if m/z 365 is present, but ion abundance is < 1.0%, detects and non-detects should not be qualified.
8. Annotate decisions to use analytical data associated with non-compliant DFTPP instrument
performance checks in the Data Review Narrative.
9. If instrument performance check criteria are achieved using alternate techniques other than
described in Section II.D.5, obtain additional information to evaluate the performance and
procedures. Note any concerns or questions for laboratory CLP PO action.
For example, the issue shall be noted for laboratory CLP PO action when an inappropriate
technique such as background subtracting from the solvent front or from another region of the
chromatogram rather than from the DFTPP peak is used to obtain background subtraction.
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III. Initial Calibration
A. Review Items
Form 6A-OR, quantitation reports, and chromatograms.
B. Objective
The objective of initial calibration (ICAL) is to ensure that the instrument is capable of producing
acceptable qualitative and quantitative data.
C. Criteria
1. ICAL shall be performed at the specified frequency and sequence. Each GC/MS system must be
calibrated with a minimum of five concentrations to determine instrument sensitivity and the
linearity of GC/MS response for the purgeable target analytes and Deuterated Monitoring
Compounds (DMCs).
a. ICAL standards must be analyzed prior to any analysis of samples and required blanks, and
within 12 hours of the associated instrument performance check at the beginning of each
analytical sequence; or as necessary if the CCV acceptance criteria are not met.
b. ICAL standards must contain all required target analytes and DMCs at specified
concentrations. The calibration standards are to be prepared at 5.0, 10,20,40, and 80 ng/(iL for
each target analyte and associated DMCs, except 1,4-Dioxane, twenty target analytes and two
DMCs listed in Section C.l.c and DMC l,4-Dioxane-d8. For 1,4-Dioxane and
l,4-Dioxane-d8, the calibration standard concentrations are at 2.5, 5.0, 10, 20, and 40 ng/ (iL.
c. The ICAL standard concentrations are at 10, 20, 40, 80, and 160 ng/(iL for twenty target
analytes and two DMCs: Benzaldehyde; Phenol; Bis(2-chloroethyl) ether; 2-Methylphenol;
2,2'-Oxybis(l—chloropropane); Caprolactam; Hexachlorocyclopentadiene; Atrazine;
Carbazole; Fluoranthene; 3,3'-Dichlorobenzidine; Di-n-octylphthalate; 2,4-Dinitrophenol;
Pentachlorophenol (PCP); 4-Methylphenol; 4,6-Dinitro-2-methylphenol; 3-Nitroaniline;
4-Nitroaniline; 4-Nitrophenol; 4,6-Dinitro-2-methylphenol; 4-Nitrophenol-d4;
4-Methylphenol-d8
d. For the optional analysis of Fob/cyclic Aromatic Hydrocarbons (PAHs) and PCP using the
SIM technique, the calibration standard concentrations are at 0.10, 0.20, 0.40, 0.80, and 1.6
ng/(iL for each target analyte of interest and the associated DMCs. PCP concentrations are at
0.20, 0.40, 0.80, 1.6 and 3.2 ng/^L.
2. The Relative Response Factor (RRF), Mean Relative Response Factor (RRF) and the Percent
Relative Standard Deviation (%RSD) must be calculated for each target analyte and DMC
accordingly.
3. The RRF for each target analyte and DMC in each ICAL standard must be > Minimum RRF value
in Table 30.
4. The %RSD of the ICAL RRF for each target analyte and DMC must be < Maximum %RSD values
in Table 30.
NOTE: The technical acceptance criteria in the modified analysis of the method may impact some
of the preceding evaluation criteria. A copy of the modified analysis should be present in
the SDG. Refer to the CLP home page at
http://www.epa.gov/oerrpage/superfund/programs/clp/modifiedanalvses.htm for the
specific method flexibility requirements.
D. Evaluation
1. Verify that the ICAL is performed at the specified frequency and sequence.
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2. Verify that the correct concentrations of the target analytes and DMCs are used in each ICAL
standard.
3. Verify that the RRF, RRF and %RSD for each target analyte and DMC are calculated correctly and
that the recalculated values agree with the laboratory reported values on Form 6A-OR. Recalculate
the RRFs, RRFs and %RSD for at least one target analyte and DMC associated with each internal
standard.
4. Verify that RRFs are > Minimum RRF values in Table 30 for the target analytes and DMCs.
5. Verify that the %RSDs are < Maximum %RSD values in Table 30 for all target analytes and
DMCs.
NOTE: For data obtained from the CLP, information regarding non-compliant ICAL can be
obtained from the NFG reports and may be used as part of the evaluation process.
E. Action
1. If the ICAL is not performed at the specified frequency and sequence, qualify detects and
non-detects in the associated samples as unusable (R).
2. If the ICAL is not performed at the specified concentrations, qualify detects in the associated
samples as estimated (J) and non-detects in the associated samples as estimated (UJ).
3. If errors are detected in the calculations of the RRFs, RRF or %RSD, perform a more
comprehensive recalculation.
4. If the RRF is < Minimum RRF value in Table 30 for any target analyte, use professional judgment
to qualify detects in the associated samples as estimated high (J+) or unusable (R) and non-detects
in the associated samples as unusable (R).
5. If the RRF is > Minimum RRF value in Table 30 for any target analyte, detects and non-detects in
the associated samples should not be qualified.
6. If the %RSD is > Maximum %RSD value in Table 30 for any target analyte, qualify detects in the
associated samples as estimated (J). Use professional judgment to qualify non-detects in the
associated samples.
7. If the %RSD is < Maximum %RSD value in Table 30 for any target analyte, detects and
non-detects in the associated samples should not be qualified.
8. No qualification of the data is necessary on the DMC RRF, RRF and %RSD data alone. Use
professional judgment to evaluate the DMC RRF, RRF and %RSD data in conjunction with the
DMC recoveries to determine the need for data qualification.
9. Based on the project-specific Data Quality Objectives (DQOs), a more in-depth review may be
considered using the following guidelines:
a. If %RSD criteria of any target analytes are not met, and if %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.
b. If the high-point of the ICAL curve is outside of the %RSD criteria (e.g., due to saturation):
i. Qualify detects in the associated samples with analyte concentrations greater than the
high-point concentration as estimated (J).
ii. Detects in the associated samples with analyte concentrations within the calibration range
should not be qualified.
iii. Non-detects in the associated samples should not be qualified.
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c. If the low-point of the ICAL curve is outside of the %RSD criteria:
i. Qualify detects in the associated samples with analyte concentrations in the non-linear
range as estimated (J).
ii. Detects in the associated samples with analyte concentrations within the calibration range
should not be qualified.
iii. 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.
10. If the laboratory failed to provide adequate calibration information, notify the Regional CLP PO,
who may contact the laboratory and request the necessary information. If the information is not
available, use professional judgment to assess the data.
11. Annotate the potential effects on the reported data due to exceeding the ICAL criteria in the Data
Review Narrative.
12. If the ICAL criteria are grossly exceeded, note this for laboratory CLP PO action.
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Table 30. RRF, %RSD and %D Acceptance Criteria in Initial Calibration and CCV for Semivolatile
Analysis
Analyte
1,4-Dioxane
Benzaldehyde
Phenol
Bis(2-chloroethyl)ether
2-Chlorophenol
2-Methylphenol
3-Methylphenol
2,2'-Oxybis-(l-chloropropane)
Acetophenone
4-Methylphenol
N-Nitroso-di-n-propylamine
Hexachloroethane
Nitrobenzene
Isophorone
2-Nitrophenol
2,4-Dimethylphenol
Bis(2-chloroethoxy)methane
2,4-Dichlorophenol
Naphthalene
Hexachlorobutadiene
Caprolactam
4-Chloro-3-methylphenol
2-Methylnaphthalene
Hexachlorocyclopentadiene
2,4,6-Trichlorophenol
2,4,5 -Trichlorophenol
l,l'-Biphenyl
2-Chloronaphthalene
2-Nitroaniline
Dimethylphthalate
2,6-Dinitrotoluene
Minimum
RRF
0.010
0.100
0.080
0.100
0.200
0.010
0.010
0.010
0.060
0.010
0.080
0.100
0.090
0.100
0.060
0.050
0.080
0.060
0.200
0.040
0.010
0.040
0.100
0.010
0.090
0.100
0.200
0.300
0.060
0.300
0.080
Maximum
%RSD
40.0
40.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
40.0
20.0
20.0
40.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
Opening
Maximum
%ol
+ 40.0
+ 40.0
+ 20.0
+ 20.0
+ 20.0
+ 20.0
+ 20.0
+ 25.0
+ 20.0
+ 20.0
+ 25.0
+ 20.0
+ 20.0
+ 20.0
+ 20.0
+ 25.0
+ 20.0
+ 20.0
+ 20.0
+ 20.0
+ 30.0
+ 20.0
+ 20.0
+ 40.0
+ 20.0
+ 20.0
+ 20.0
+ 20.0
+ 25.0
+ 20.0
+ 20.0
Closing
Maximum
%D
+ 50.0
+ 50.0
+ 25.0
+ 25.0
+ 25.0
+ 25.0
+ 25.0
+ 50.0
+ 25.0
+ 25.0
+ 25.0
+ 25.0
+ 25.0
+ 25.0
+ 25.0
+ 50.0
+ 25.0
+ 25.0
+ 25.0
+ 25.0
+ 50.0
+ 25.0
+ 25.0
+ 50.0
+ 25.0
+ 25.0
+ 25.0
+ 25.0
+ 25.0
+ 25.0
+ 25.0
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Semivolatiles
Analyte
Acenaphthylene
3-Nitroaniline
Acenaphthene
2,4-Dinitrophenol
4-Nitrophenol
Dibenzofuran
2,4-Dinitrotoluene
Diethylphthalate
1,2,4,5-Tetrachlorobenzene
4-Chlorophenyl-phenylether
Fluorene
4-Nitroaniline
4,6-Dinitro-2-methylphenol
4-Bromophenyl-phenyl ether
N-Nitrosodiphenylamine
Hexachlorobenzene
Atrazine
Pentachlorophenol
Phenanthrene
Anthracene
Carbazole
Di-n-butylphthalate
Fluoranthene
Pyrene
Butylbenzylphthalate
3,3' -Dichlorobenzidine
Benzo(a)anthracene
Chrysene
Bis(2-ethylhexyl) phthalate
Di-n-octylphthalate
Benzo(b)fluoranthene
Benzo(k)fluoranthene
Minimum
RRF
0.400
0.010
0.200
0.010
0.010
0.300
0.070
0.300
0.100
0.100
0.200
0.010
0.010
0.070
0.100
0.050
0.010
0.010
0.200
0.200
0.050
0.500
0.100
0.400
0.100
0.010
0.300
0.200
0.200
0.010
0.010
0.010
Maximum
%RSD
20.0
20.0
20.0
40.0
40.0
20.0
20.0
20.0
20.0
20.0
20.0
40.0
40.0
20.0
20.0
20.0
40.0
40.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
40.0
20.0
20.0
20.0
40.0
20.0
20.0
Opening
Maximum
%ol
+ 20.0
+ 25.0
+ 20.0
+ 50.0
+ 40.0
+ 20.0
+ 20.0
+ 20.0
+ 20.0
+ 20.0
+ 20.0
+ 40.0
+ 30.0
+ 20.0
+ 20.0
+ 20.0
+ 25.0
+ 40.0
+ 20.0
+ 20.0
+ 20.0
+ 20.0
+ 20.0
+ 25.0
+ 25.0
+ 40.0
+ 20.0
+ 20.0
+ 25.0
+ 40.0
+ 25.0
+ 25.0
Closing
Maximum
%D
+ 25.0
+ 50.0
+ 25.0
+ 50.0
+ 50.0
+ 25.0
+ 25.0
+ 25.0
+ 25.0
+ 25.0
+ 25.0
+ 50.0
+ 50.0
+ 25.0
+ 25.0
+ 25.0
+ 50.0
+ 50.0
+ 25.0
+ 25.0
+ 25.0
+ 25.0
+ 25.0
+ 50.0
+ 50.0
+ 50.0
+ 25.0
+ 50.0
+ 50.0
+ 50.0
+ 50.0
+ 50.0
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Analyte
Benzo(a)pyrene
Indeno( 1,2,3 -cd)pyrene
Dibenzo(a,h)anthracene
Benzo(g,h,i)perylene
2,3,4,6-Tetrachlorophenol
Minimum
RRF
0.010
0.010
0.010
0.010
0.040
Maximum
%RSD
20.0
20.0
20.0
20.0
20.0
Opening
Maximum
%ol
+ 20.0
+ 25.0
+ 25.0
+ 30.0
+ 20.0
Closing
Maximum
%D
+ 50.0
+ 50.0
+ 50.0
+ 50.0
+ 50.0
Analytes
Naphthalene
2-Metylnapthalene
Acenaphthylene
Acenaphthene
Fluorene
Phenanthrene
Anthracene
Fluoranthene
Pyrene
Benzo(a)anthracene
Chyrsene
Benzo(b)fluoranthene
Benzo(k)fluoranthene
Benzo(a)pyrene
Indeno( 1,2,3 -cd)pyrene
Dibenzo(a,h)anthracene
Benzo(g,h,i)perylene
Pentachlorophenol
0.600
0.300
0.900
0.500
0.700
0.300
0.400
0.400
0.500
0.400
0.400
0.100
0.100
0.100
0.100
0.010
0.020
0.010
20.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
25.0
25.0
40.0
+ 25.0
+ 20.0
+ 20.0
+ 20.0
+ 25.0
+ 25.0
+ 25.0
+ 25.0
+ 30.0
+ 25.0
+ 25.0
+ 30.0
+ 30.0
+ 25.0
+ 40.0
+ 40.0
+ 40.0
+ 50.0
+ 25.0
+ 25.0
+ 25.0
+ 25.0
+ 50.0
+ 50.0
+ 50.0
+ 50.0
+ 50.0
+ 50.0
+ 50.0
+ 50.0
+ 50.0
+ 50.0
+ 50.0
+ 50.0
+ 50.0
+ 50.0
Deuterated Monitoring Compounds
l,4-Dioxane-d8
Phenol-d5
Bis-(2-chloroethyl)ether-d8
2-Chlorophenol-d4
4-Methylphenol-ds
Nitrobenzene -d5
2-Nitrophenol-d4
2,4-Dichlorophenol-d3
Dimethylphthalate -d6
0.010
0.010
0.100
0.200
0.010
0.050
0.050
0.060
0.300
20.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
20.0
+ 25.0
+ 25.0
+ 20.0
+ 20.0
+ 20.0
+ 20.0
+ 20.0
+ 20.0
+ 20.0
+ 50.0
±25.0
+ 25.0
+ 25.0
+ 25.0
+ 25.0
+ 25.0
+ 25.0
+ 25.0
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Analyte
Acenaphthylene -ds
4-Nitrophenol-d4
Fluorene-dio
4,6-Dinitro-2-methylphenol-d2
Anthracene-dio
Pyrene-dio
Benzo(a)pyrene-di2
Fluoranthene-dio (SIM)
2-Methylnapthalene-d10 (SIM)
Minimum
RRF
0.400
0.010
0.100
0.010
0.300
0.300
0.010
0.400
0.300
Maximum
%RSD
20.0
40.0
20.0
40.0
20.0
20.0
20.0
20.0
20.0
Opening
Maximum
%ol
+ 20.0
+ 40.0
+ 20.0
+ 30.0
+ 20.0
+ 25.0
+ 20.0
+ 25.0
+ 20.0
Closing
Maximum
%D
+ 25.0
+ 50.0
+ 25.0
+ 50.0
+ 25.0
+ 50.0
+ 50.0
+ 50.0
+ 25.0
1 If a closing CCV is acting as an opening CCV, all target analytes must meet the requirements for an
opening CCV.
Table 31. Initial Calibration Actions for Semivolatile Analysis
Criteria
Initial Calibration not performed at specified
frequency and sequence
Initial Calibration not performed at the specified
concentrations
RRF < Minimum RRF in Table 30 for target
analyte
RRF > Minimum RRF in Table 30 for target
analyte
%RSD > Maximum %RSD in Table 30 for target
analyte
%RSD < Maximum %RSD in Table 30 for target
analyte
Action
Detect
Use professional
judgment
R
J
Use professional
judgment
J+orR
No qualification
J
No qualification
Non- detect
Use professional
judgment
R
UJ
R
No qualification
Use professional
judgment
No qualification
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IV. Continuing Calibration Verification
A. Review Items
Form 7A-OR, quantitation reports, and chromatograms.
B. Objective
The objective is to ensure that the instrument continues to meet the sensitivity and linearity criteria to
produce acceptable qualitative and quantitative datathroughout each analytical sequence.
C. Criteria
1. The calibration for each GC/MS system used for analysis must be verified at the beginning and end
of every 12-hour period of operation. The 12-hour period begins with the injection of DFTPP,
followed by the injection of the opening CCV solution. After the injection of all samples and
required blanks, and before the end of the 12-hour period, injection of the closing CCV is required.
The closing CCV used to bracket the end of a 12-hour analytical sequence may be used as the
opening CCV for a new 12-hour analytical sequence, provided that all technical acceptance criteria
are met for an opening CCV.
2. CCV standards must contain all required target analytes and DMCs at the mid-point concentration
CSS of the ICAL.
3. For an opening or a closing CCV, the RRFs for the target analytes and DMCs must be > the
Minimum RRF values in Table 30.
4. The Percent Difference (%D) between the ICAL RRF and the opening CCV RRF must be within
the Opening Maximum %D limits in Table 30 for each target analyte and DMC.
5. For a closing CCV, the %D between the ICAL RRF and the CCV RRF must be within the Closing
Maximum %D limits in Table 30 for each target analyte and DMC.
D. Evaluation
1. Verify that the CCV is analyzed at the specified frequency (an opening and closing CCV must be
analyzed within a 12-hour period) and sequence and that the CCV is associated to the correct
ICAL.
2. Verify that the mid-point standard CS3 from the ICAL is used as an opening or a closing CCV.
3. Verify that the RRF and %D for all target analytes and DMCs are calculated correctly and the
recalculated values agree with the laboratory reported values on Form 7A-OR. Recalculate RRF
and %D for at least one target analyte and DMC associated with each internal standard.
4. For an opening or a closing CCV, verify that the RRFs are > the Minimum RRF values in Table 30
for all target analytes and DMCs.
5. For an opening CCV, verify that the %Ds are within the Opening Maximum %D limits in Table 30
for the target analytes and DMCs.
6. For a closing CCV, verify that the %Ds are within the Closing Maximum %D limits in Table 30 for
all target analytes and DMCs.
NOTE: For data obtained from the CLP, information regarding the non-compliant CCV can be
obtained from the NFG reports and may be used as part of the evaluation process.
E. Action
1. If the CCV is not performed at the specified frequency, qualify detects and non-detects as unusable
(R). Contact the Regional CLP PO to request that the laboratory repeat the analysis, if holding
times have not expired and there are remaining sample vials. If reanalysis is not possible, carefully
evaluate all other available information, including the the quality of analyte peak shapes and mass
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spectral matches, stability of internal standard retention times (RTs) and areas in each affected
sample, and compare to the most recent calibration performed on the same instrument under the
same conditions. Using this information and professional judgement, 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).
2. If the CCV is not performed at the specified concentration, use professional judgment to qualify
detects and non-detects. Special consideration should be given to sample results at the opposite
extreme of the calibration range if this defect is noted.
3. If errors are detected in the calculations of either the RRF or the %D, perform a more
comprehensive recalculation.
4. For an opening or a closing CCV, if RRF is < Minimum RRF value in Table 30 for any target
analyte, carefully evaluate the qualitative data associated with positively identified analytes and use
professional judgment to qualify detects as estimated (J) or unusable (R) and qualify non-detects as
unusable (R).
5. For opening or a closing CCV, if RRF is > Minimum RRF value in Table 30 for any target analyte,
detects and non-detects should not be qualified.
a. Take special note of any extreme deviation in RRF and evaluate RT data, peak shapes, and
areas for inconsistencies that may indicate a chromatographic co-elution. If this is suspected,
the contaminant may also be present in samples and blanks. Use professional judgment to
qualify affected data appropriately.
6. For an opening CCV, if %D is outside the Opening Maximum %D limits in Table 30 for any target
analyte, qualify detects as estimated (J) and non-detects as estimated (UJ).
7. For a closing CCV, if %D is outside the Closing Maximum %D limits in Table 30 for any target
analyte, qualify detects as estimated (J) and non-detects as estimated (UJ).
8. For an opening CCV, if %D is within the inclusive range of the Opening Maximum %D limits in
Table 30 for any target analyte, detects and non-detects should not be qualified. For closing CCV,
if %D is within the inclusive range of the Closing Maximum %D limits in Table 30 for any target
analyte, detects and non-detects should not be qualified.
9. No qualification of the data is necessary on DMC RRF and/or %D alone. Use professional
judgment to evaluate the DMC RRF and %D data in conjunction with the DMC recoveries to
determine the need for data qualification.
10. If the laboratory has failed to provide adequate calibration information, contact the Regional CLP
PO, who may contact the laboratory and request the necessary information. If the information is
not available, use professional judgment to assess the data.
11. Annotate the potential effects on the data due to CCV criteria exceedance in the Data Review
Narrative.
12. If CCV criteria are grossly exceeded, note this for laboratory CLP PO action.
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Table 32. CCV Actions for Semivolatile Analysis
Criteria for Opening CCV
CCV not performed at required
frequency and sequence
CCV not performed at specified
concentration
RRF < Minimum RRF in Table 30
for target analyte
RRF > Minimum RRF in Table 30
for target analyte
%D outside the Opening
Maximum %D limits in Table 30
for target analyte
%D within the inclusive Opening
Maximum %D limits in Table 30
for target analyte
Criteria for Closing CCV
CCV not performed at required
frequency
CCV not performed at specified
concentration
RRF < Minimum RRF in Table 30
for target analyte
RRF > Minimum RRF in Table 30
for target analyte
%D outside the Closing Maximum
%D limits in Table 30 for target
analyte
%D within the inclusive Closing
Maximum %D limits in Table 30
for target analyte
Action
Detect
Use
professional
judgment
R
Use
professional
judgment
Use
professional
judgment
JorR
No
qualification
J
No
qualification
Non- detect
Use
professional
judgment
R
Use
professional
judgment
R
No
qualification
UJ
No
qualification
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V. Blanks
A. Review Items
Form 1A-OR, Form 1B-OR, Form 4-OR, chromatograms, and quantitation 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. Criteria
The criteria for evaluation of blanks should apply to any blank associated with the samples (e.g.,
method blanks, field blanks, etc.). If problems with any blank exist, all associated data must be
carefully evaluated to determine whether or not there is an inherent variability in the data or if the
problem is an isolated occurrence not affecting other data. Whereas previous guidelines recommended
special criteria to discount possible false positives of common SVGA laboratory contaminants
(phthalate esters), recent CLP data have shown less than a 1% probability that levels of these
contaminants from a contaminating source will exceed the Contract Required Quantitation Limit
(CRQL).
1. Method blanks must be performed at the specified frequency and sequence. A method blank must
be extracted per matrix each time samples are extracted. The number of samples extracted with
each method blank shall not exceed 20 field samples. The method blank must be extracted by the
same procedure used to extract samples and analyzed on each GC/MS system under the same
conditions used to analyze associated samples.
2. The method blank, like any other sample in the SDG, must meet the technical acceptance criteria
for sample analysis.
3. The TCLP/SPLP extraction blank must be prepared and analyzed at the specified frequency and
sequence.
4. The concentration of a target analyte in any blank must not exceed its CRQL. Tentatively
Identified Compound (TIC) concentration in any blank must be < 5.0 ug/L for water or 170 ug/Kg
for soil matrices.
D. Evaluation
1. Verify that method blanks are extracted at the specified frequency and analyzed at the required
sequence. The Method Blank Summary (Form 4-OR) may be used to identify the samples
associated with each method blank.
2. Verify that applicable TCLP/SPLP extraction blanks are analyzed at the specified frequency and
sequence. The Method Blank Summary (Form 4-OR) may be used to identify the samples
associated with each TCLP/SPLP extraction blank.
3. Data concerning the field blanks are not evaluated as part of the Contract Compliance Screening
(CCS) process. Evaluations on field or trip blanks should be similar to the method blanks.
4. Review the results of all associated blanks on the forms and raw data (chromatograms and
quantitation reports) to evaluate the presence of target analytes and non-target compounds in the
blanks.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the non-compliant blank can be obtained from the NFG
reports and may be used as part of the evaluation process.
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E. Action
1. If the appropriate blanks are not extracted at the correct frequency and/or analyzed at the correct
sequence, use professional judgment to determine if the associated sample data should be qualified;
obtain additional information from the laboratory, if necessary. Record the situation in the Data
Review Narrative and note it for CLP PO action.
2. Action regarding unsuitable blank results depends on the circumstances and origin of the blank.
Verify that the data qualification decisions based on field quality control (QC) are supported by the
project Quality Assurance Project Plan (QAPP). 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 having the highest concentration of a contaminant. Do not correct the results by
subtracting any blank value.
3. For any blank (including method blank), if a target analyte is detected, but it is not detected in the
sample, non-detects should not be qualified.
4. For any method blank reported with results < CRQLs, report sample results that are < CRQLs at the
CRQLs and qualify as non-detect (U). For any method blank reported with results that are <
CRQLs, use professional judgment to qualify sample results that are > CRQLs. Positive results in
samples, especially those near but above the CRQL, may be biased high by low level
contamination in the method blanks, and should be considered as estimated (J+).
5. For any method blank reported with results > CRQLs, report sample results that are < CRQLs at the
CRQLs and qualify as non-detect (U). For any method blank reported with results > CRQLs, report
at sample results that are > CRQLs but < Blank Results, and qualify as non-detect (U) or unusable
(R). Use professional judgment to qualify sample results that are > CRQLs and > Blank Results.
6. For TCLP/SPLP extraction blanks and field blanks, sample result qualifications listed in Table 33
should apply if supported by the project QAPP.
7. If gross contamination exists with blank results that are > ICAL CSS concentrations, qualify detects
as unusable (R). If the contamination is suspected of having an effect on the sample results note it
for laboratory CLP PO action.
8. For any blank (including method blank) reported with TICs (non-target compounds) concentrations
that are > 5.0 ug/L for water and 170 ug/kg for soil matrices, use professional judgment to qualify
sample results.
9. 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.
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Table 33. Blank and TCLP/SPLP LEB Actions for Semivolatile Analysis
Blank Type
Method,
TCLP/SPLP
LEB, Field
Blank Result
Detect
CRQL
Grossly high
TIC>5.0ug/L
(water)
or
TIC> 170ug/Kg
(soil)
Sample Result
Non-detect
CRQL
CRQL but < Blank Result
> CRQL and > Blank Result
Detect
Detect
Action
No qualification
Report at CRQL and qualify
as non-detect (U)
Use professional judgment
Report at CRQL and qualify
as non-detect (U)
Report at sample results and
qualify as non-detect (U) or as
unusable (R)
Use professional judgment
Report at sample results and
qualify as unusable (R)
Use professional judgment
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VI. Deuterated Monitoring Compound
A. Review Items
Form 2A-OR, Form 2B-OR quantitation reports, and chromatograms.
B. Objective
The objective is to evaluate DMC percent recovery (%R) to ensure that the analytical method is
efficient.
C. Criteria
1. All samples and blanks are spiked with DMCs listed in Table 34 prior to sample extraction
procedure to measure DMC %R.
2. %R for each DMC shall be calculated correctly according to the method.
3. %R for each DMC in samples and blanks must be within the limits in Table 34.
Table 34. Semivolatile DMC and %R Limits
DMC
l,4-Dioxane-d8
Phenol-d5
Bis(2-chloroethyl)ether-d8
2-Chlorophenol-d4
4-Methylphenol-d8
Nitrobenzene-ds
2-Nitrophenol-d4
2,4-Dichlorophenol-d3
Dimethylphthalate -d6
Acenaphthylene-d8
4-Nitrophenol-d4
Fluorene-dio
4,6-Dinitro-2-methylphenol-d2
Anthracene-dio
Pyrene-dio
Benzo(a)pyrene-di2
Fluoranthene-dio (SIM)
2-Methylnapthalene-djo (SIM)
%R For Water
Samples
40-110
10-130
25-120
20-130
25-125
20-125
20-130
20-120
25-130
10-130
10-150
25-125
10-130
25-130
15-130
20-130
30-130
30-130
%R For Soil Samples
40-110
10-130
10-150
15-120
10-140
10-135
10-120
10-140
10-145
15-120
10-150
20-140
10-130
10-150
10-130
10-140
30-130
20-140
D. Evaluation
1. Check raw data (e.g., chromatograms and quantitation reports) to verify that the recoveries are on
the Deuterated Monitoring Compound Recovery Form 2A-OR and Form 2B-OR.
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2. Check for any calculation or transcription errors. Verify that the DMC recoveries are calculated
correctly using the equation in the method and that the recalculated values agree with the laboratory
reported values on Form 2A-OR and Form 2B-OR.
3. Whenever there are two or more analyses for a particular sample, use professional judgment to
determine which analysis has the most acceptable data to report. Considerations include, but are
not limited to:
a. DMC recovery (marginal versus gross deviation).
b. Technical holding times.
c. Comparison of the target analyte results reported in each sample analysis.
d. Other QC information, such as performance of internal standards.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the non-compliant DMC %R can be obtained from the NFG
reports and may be used as part of the evaluation process.
E. Action
1. If a DMC is not added in the samples and blanks or the concentrations of DMCs in the samples and
blanks are not as specified, use professional judgment to qualify detects and non-detects. The
Regional CLP PO should be contacted to arrange for reanalysis, if possible.
2. If errors are detected in the calculations of %R, perform a more comprehensive recalculation. It
may be necessary to have the laboratory resubmit the data after making corrections.
3. If any DMC %R is outside the limits (Table 34) in samples, qualify the associated SVGA target
analytes listed in Table 36 and SVGA SIM target analytes in Table 37 considering the existence of
interference in the raw data. Considerations include, but are not limited to:
a. If DMC %R is < 10% (excluding DMCs with 10% as a lower acceptance limits), qualify
detects as estimated low (J-) and non-detects as unusable (R).
b. If DMC %R is > 10% (excluding DMCs with 10% as a lower acceptance limits) and < the
lower acceptance limit, qualify detects as estimated low (J-) and non-detects as estimated (UJ).
c. If DMC %R is > lower acceptance limit and < upper acceptance limit, detects and non-detects
should not be qualified.
d. If DMC%R is > upper acceptance limit, qualify detects as estimated high (J+). Non-detects
should not be qualified.
4. If DMC %R is outside the limits (Table 34) in a blank, special consideration shall be given to 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.
For example, if one or more samples in the analytical sequence show acceptable DMC %Rs, the
blank problem may be considered as an isolated occurrence. However, even if this judgment
allows some use of the affected data, note analytical problems for laboratory CLP PO action.
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Table 35. DMC Actions for Semivolatile Analysis
Criteria
%R < 10% (excluding DMCs with 10% as a lower
acceptance limit)
10% < %R (excluding DMCs with 10% as a lower
acceptance limit) < Lower Acceptance Limit
Lower Acceptance limit < %R < Upper Acceptance Limit
%R > Upper Acceptance Limit
Action
Detect
J-
J-
No qualification
J+
Non-detect
R
UJ
No qualification
No qualification
Table 36. Semivolatile DMCs and the Associated Target Analytes
l,4-Dioxane-d8 (DMC-1)
1,4-Dioxane
2-Chlorophenol-d4(DMC-4)
2-Chlorophenol
2-Nitrophenol-d4(DMC-7)
Isophorone
2-Nitrophenol
Acenaphthylene-d8(DMC-10)
*Naphthalene
* 2-Methylnaphthalene
2-Chloronaphthalene
*Acenaphthylene
*Acenaphthene
4,6-Dinitro-2-methylphenol-d2
(DMC-13)
4,6-Dinitro-2-methylphenol
Phenol-d5(DMC-2)
Benzaldehyde
Phenol
4-Methylphenol-d8(DMC-5)
2-Methylphenol
3-Methylphenol
4-Methylphenol
2,4-Dimethylphenol
2,4-Dichlorophenol-d3(DMC-8)
2,4-Dichlorophenol
Hexachlorobutadiene
Hexachlorocyclopentadiene
4-Chloro-3 -methylphenol
2,4,6-Trichlorophenol
2,4,5-Trichlorophenol
1, 2,4,5 -Tetrachlorobenzene
* Pentachlorophenol
2,3,4,6-Tetrachlorophenol
4-Nitrophenol-d4(DMC-ll)
2-Nitroaniline
3-Nitroaniline
2,4-Dinitrophenol
4-Nitrophenol
4-Nitroaniline
Anthracene-dio(DMC-14)
Hexachlorobenzene
Atrazine
Bis(2-Chloroethyl)
ether-d8(DMC-3)
Bis(2-chloroethyl)ether
2,2'-Oxybis( 1 -chloropropane)
Bis(2-chloroethoxy)methane
Nitrobenzene-ds(DMC-6)
Acetophenone
N-Nitroso-di-n-propylamine
Hexachloroethane
Nitrobenzene
2,6-Dinitrotoluene
2,4-Dinitrotoluene
N-Nitrosodiphenylamine
Dimethylphthalate-d6(DMC-9)
Caprolactam
l,l'-Biphenyl
Dimethylphthalate
Diethylphthalate
Di-n-butylphthalate
Butylbenzylphthalate
Bis(2-ethylhexyl) phthalate
Di-n-octylphthalate
Fluorene-d10(DMC-12)
Dibenzofuran
*Fluorene
4-Chlorophenyl-phenylether
4-Bromophenyl-phenylether
Carbazole
Pyrene-d10(DMC-15)
*Fluoranthene
*Pyrene
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Benzo(a)pyrene-di2(DMC-16)
3 ,3 '-Dichlorobenzidine
* Benzo(b)fluoranthene
* Benzo(k)fluoranthene
* Benzo(a)pyrene
* Indeno( 1 ,2,3 -cd)pyrene
* Dibenzo(a,h)anthracene
* Benzo(g,h,i)perylene
*Phenanthrene
* Anthracene
* Benzo(a)anthracene
*Chrysene
* Included in optional Target Analyte List (TAL) of PAHs and PCP only.
Table 37. Semivolatile SIM DMCs and the Associated Target Analytes
Fluoranthene-dlO
(DMC-1)
Fluoranthene
Pyrene
Benzo(a)anthracene
Chrysene
Benzo(b)fluoranthene
Benzo(k)fluoranthene
Benzo(a)pyrene
Indeno( 1 ,2,3 -cd)pyrene
Dibenzo(a,h)anthracene
Benzo(g,h,i)perylene
2-Methylnapthalene-dlO
(DMC-2)
Napthalene
2-Methylnapthalene
Acenapthylene
Acenaphthene
Fluorene
Pentachlorophenol
Phenanthrene
Anthracene
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VII. Matrix Spike/Matrix Spike Duplicate
A. Review Items
Cover Page, Form 3A-OR, chromatograms, and quantitation reports.
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. Criteria
1. If requested, MS/MSDs shall be prepared and analyzed at specified frequency. One pair of
MS/MSD shall be analyzed per matrix or per SDG.
NOTE: Data for MS and MSDs will not be present unless requested by the Region.
2. Samples identified as field blanks or Performance Evaluation (PE) samples cannot be used for
spiked sample analysis.
3. MS/MSD %R and the Relative Percent Difference (RPD) between MS and MSD results shall be
calculated according to the method.
4. MS/MSD %R and RPD shall be within the acceptance limits in Table 38.
D. Evaluation
1. Verify that requested MS/MSD samples are analyzed at the required frequency.
2. Verify that a field blank or PE sample is not used for MS/MSD analysis.
3. Verify that the recalculated MS/MSD %R and RPD values agree with the laboratory reported
values on Form 3A-OR.
4. Inspect MS/MSD %R and RPD on Form 3A-OR and verify that they are within the limits in Table
38.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the non-compliant MS/MSD %R or RPD can be obtained
from the NFG reports and may be used as part of the evaluation process.
E. Action
1. If requested MS/MSD samples are not analyzed at the specified frequency, use professional
judgment to determine the impact on sample data, if any; obtain additional information from the
laboratory, if necessary. Record the situation in the Data Review Narrative and note it for
laboratory CLP PO action. It is not likely that data qualification will be warranted if the frequency
requirement is not met. Carefully consider all factors, known and unknown, about method
performance on the matrix at hand, in lieu of MS/MSD data.
2. If a field blank or PE sample is used for the MS/MSD analysis, note this for laboratory CLP PO
action. All of the other QC data must then be carefully checked. Use professional judgment when
evaluating the data.
3. If the MS/MSD %R or RPD is outside the acceptance limits in Table 38, qualify the detects and
non-detects in the original sample to include the consideration of the existence of interference in the
raw data. Considerations include, but are not limited to:
a. If MS/MSD %R is < 10% (excluding spiked analyte with %R lower limit of 10% or less),
qualify detects as estimated (J) and non-detects as unusable (R).
b. If MS/MSD %R is > 10% (excluding spiked analyte with %R lower limit of 10% or less) and <
the lower acceptance limit, qualify detects as estimated (J) and non-detects as estimated (UJ).
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c. If MS/MSD %R or RPD is > lower acceptance limit and < upper acceptance limit, detects and
non-detects should not be qualified.
d. If MS/MSD%R or RPD is > the upper acceptance limit, qualify detects as estimated (J).
Non-detects should not be qualified.
Table 38. MS/MSD %R and RPD Limits for Semivolatile Analysis
Compound
Phenol
2-Chlorophenol
N-Nitroso-di-n-propylamine
4-Chloro-3 -methylphenol
Acenaphthene
4-Nitrophenol
2,4-Dinitrotoluene
Pentachlorophenol
Pyrene
%R for Water
Samples
12-110
27 - 123
41-116
23-97
46-118
10-80
24-96
9-103
26 - 127
RPD for
Water
Samples
0-42
0-40
0-38
0-42
0-31
0-50
0-38
0-50
0-31
%R for
Soil/Sediment
Samples
26-90
25 - 102
41 - 126
26 - 103
31-137
11-114
28-89
17-109
35 - 142
RPD for
Soil/Sediment
Samples
0-35
0-50
0-38
0-33
0-19
0-50
0-47
0-47
0-36
Table 39. MS/MSD Actions for Semivolatile Analysis
Criteria
%R < 10% (excluding spiked analyte with %R lower
limit of 10% or less)
10% < %R (excluding spiked analyte with %R lower
limit of 10% or less) < Lower Acceptance Limit
Lower Acceptance Limit < %R or RPD < Upper
Acceptance Limit
%R or RPD > Upper Acceptance Limit
Action
Detect
J
J
No qualification
J
Non-detect
R
UJ
No qualification
No qualification
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VIII. Gel Permeation Chromatography Performance Check
A. Review Items
Form 9B-OR, two ultraviolet (UV) traces, Gel Permeation Chromatography (GPC) cleanup blank
quantitation reports, and chromatograms.
B. Objective
The objective is to evaluate GPC cleanup efficiency.
C. Criteria
1. GPC is used for the cleanup of all non-aqueous sample extracts and for aqueous sample extracts
that contain high molecular weight components that interfere with the analysis of the target
analytes.
2. Each GPC system must be calibrated prior to processing samples for GPC cleanup; or when the
GPC CCV solution fails to meet criteria; or when the column is changed or channeling occurs; and
once every 7 days when in use.
3. The GPC calibration is acceptable if the two UV traces meet the following requirements:
a. Peaks must be observed and symmetrical for all compounds in the calibration solution.
b. Corn oil and the phthalate peaks exhibit > 85% resolution.
c. The phthalate and methoxychlor peaks exhibit > 85% resolution.
d. Methoxychlor and perylene peaks exhibit > 85% resolution.
e. Perylene and sulfur peaks must not be saturated and should exhibit > 90% baseline resolution.
f. The RT shift is < 5% between UV traces for Bis(2-ethylhexyl) phthalate and perylene.
4. A GPC blank must be analyzed after each GPC calibration. The concentration for any target
analyte in the GPC blank must not exceed the CRQL.
5. The calibration verification must be performed at least once every 7 days according to the
specifications.
D. Evaluation
1. Verify that the GPC calibration is performed at the specified frequency.
2. Verify that there are two UV traces present and that the RT shift for Bis(2-ethylhexyl) phthalate and
perylene is < 5%.
3. Verify that the SVGA target analytes in the GPC calibration standard are present and the peaks are
symmetrical in both UV traces meeting the minimum resolution requirements.
4. Verify that no target analyte in the GPC blank exceeds the CRQL.
5. Verify that the GPC calibration verification is performed at the specified frequency.
E. Action
1. If GPC calibration and calibration verification criteria are not met, examine the raw data for the
presence of high molecular weight contaminants; examine subsequent sample data for unusual
peaks. Use professional judgment to qualify the data. If the laboratory chooses to analyze samples
under unacceptable GPC criteria, notify the laboratory CLP PO.
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a. If the RT shift of Bis(2-ethlhexyl) phthalate and perylene is > 5%, the GPC unit may be in an
unstable temperature environment and subj ect to erratic performance. The expected result may
be an unknown bias in the data. Contact the Regional CLP PO to arrange for sample reanalysis.
2. Annotate the potential effects on the sample data resulting from the GPC cleanup analyses not
yielding acceptable results in the Data Review Narrative.
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IX. Internal Standard
A. Review Items
Form 8A-OR, quantitation reports, and chromatograms.
B. Objective
The objective is to evaluate the internal standard performance to ensure that GC/MS sensitivity and
response are stable during each analysis.
C. Criteria
1. The internal standard solution must be added to all samples and blanks at the specified
concentration. The internal standard solution must contain all internal standard compounds
specified in the method.
2. The area response of each internal standard compound in all samples and blanks must be within the
inclusive ranges of 50-200% of the area response of the same internal standard from the associated
opening CCV or the mid-point standard CSS from the associated ICAL.
3. The RT of the internal standard compound in the sample or blank must not vary more than ±10.0
seconds from the RT of the same internal standard in the associated opening CCV or mid-point
standard CSS from the associated ICAL.
D. Evaluation
1. Verify that all required internal standard compounds are added to sample and blank analyses at the
specified concentrations.
2. Check raw data (e.g., chromatograms and quantitation reports) to verify that RT and area response
of each internal standard compound in a sample or blank are reported on Internal Standard Area and
Retention Time Summary Form 8A-OR.
3. Verify that RTs and area responses for all internal standard compounds are within the specified
criteria. If internal standard RTs are signicantly different from the associated CCV or ICAL
midpoint, i.e., more than 10 seconds, the internal standard peak may have been misidentified, but
most likely a change in the chromatographic system should be suspected. This could be an
improper injection, a leak in the GC system, or the effect of a highly contaminated matrix.
Normally, the area counts will also suffer in this situation, but even if they appear unaffected, both
quantitative and qualitative results should be considered highly suspect.
4. If there is a reanalysis for a particular sample, determine which analysis is the best data to report.
Considerations include, but are not limited to:
a. Magnitude and direction of the internal standard area response shift.
b. Magnitude and direction of the internal standard RT shift.
c. Technical holding times.
d. Comparison of the values of the target analytes reported in each method.
e. Other QC information.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the non-compliant internal standard area response or RT
can be obtained from the NFG reports and may be used as part of the evaluation process.
E. Action
NOTE: Apply the action to the target analytes in samples or blanks that are associated to the
non-compliant internal standard compound (Table 40). The internal standard and the
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associated target analytes are in Exhibit D SVGA Section 17 Table 9 and 10 of the
Statement of Work (SOW).
1. If required internal standard compounds are not added to a sample or blank, qualify detects and
non-detects as unusable (R).
2. If the required internal standard compound is not analyzed at the specified concentration in a
sample or blank, use professional judgment to qualify detects and non-detects.
3. If the area response of an internal standard compound in a sample or blank is < 20% of the area
response of the same internal standard in the associated opening CCV or mid-point standard CSS
from the associated ICAL, qualify detects as estimated high (J+) and non-detects as unusable (R).
4. If the area response of an internal standard compound in a sample or blank is > 20 % and < 50% of
the area response of the same internal standard in the associated opening CCV or mid-point
standard CSS from the associated ICAL, qualify detects as estimated high (J+) and non-detects as
estimated (UJ).
5. If the area response of an internal standard compound in a sample or blank is within the inclusive
range of 50-200% of the area response of the same internal standard in the associated opening CCV
or mid-point standard CSS from the associated ICAL, detects and non-detects should not be
qualified.
6. If the area response of an internal standard compound in a sample or blank is > 200% of the area
response of the same internal standard in the associated opening CCV or mid-point standard CSS
from the associated ICAL, qualify detects as estimated low (J-). Non-detects should not be
qualified.
7. If the RT shift between sample/blank and the associated opening CCV or mid-point standard CSS
from the associated ICAL of an internal standard compound is > 10.0 seconds, qualify detects and
non-detects as unusable (R). The Regional CLP PO should be contacted to arrange for reanalysis.
8. If the RT shift between sample/blank and the associated opening CCV or mid-point standard CSS
from the associated ICAL of an internal standard compound is < 10.0 seconds, detects and
non-detects should not be qualified.
9. If the internal standard performance criteria are grossly exceeded, annotate the potential effects on
the data in the Data Review Narrative and note it for laboratory CLP PO action.
Table 40. Internal Standard Actions for Semivolatile Analysis
Criteria
Area response < 20% of the opening CCV or mid-point
standard CSS from ICAL
20% < Area response < 50% of the opening CCV or
mid-point standard CSS from ICAL
50% < Area response < 200% of the opening CCV or
mid-point standard CSS from ICAL
Area response > 200% of the opening CCV or mid-point
standard CSS from ICAL
RT shift between sample/blank and opening CCV or
mid-point standard CSS from ICAL > 10.0 seconds
RT shift between sample/blank and opening CCV or
mid-point standard CSS from ICAL < 10.0 seconds
Action
Detect
J+
J+
No qualification
J-
R
No qualification
Non-detect
R
UJ
No qualification
No qualification
R
No qualification
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X. Target Analyte Identification
A. Review Items
Form 1A-OR, quantitation reports, mass spectra, and chromatograms.
B. Objective
The objective is to provide acceptable GC/MS qualitative analysis to minimize the number of erroneous
analyte identifications.
C. Criteria
1. The mass spectrum of the analyte from the sample analysis must match that of the same analyte in
the associated opening CCV or mid-point standard CSS from the associated ICAL according to the
following criteria:
a. All ions present in the calibration standard mass spectrum must be present in the sample
spectrum at relative intensity > 10%.
b. The relative intensities of these ions must agree within ±20% between the standard and sample
spectra (e.g., for an ion with an abundance of 50% in the standard spectrum, the corresponding
sample ion abundance must be between 30-70%).
c. Ions present at > 10% in the sample mass spectrum, but not present in the standard spectrum,
must be evaluated by a reviewer experienced in mass spectral interpretation.
2. The Relative Retention Time (RRT) for a positively identified target analyte must be within ±0.06
RRT units of the RRT for the same analyte in the associated opening CCV or mid-point standard
CSS from the associated ICAL.
D. Evaluation
1. Verify that the positively identified target analyte mass spectrum meets the specified criteria. If
not, examine the sample target analyte spectra for the presence of interference at one or more mass
fragment peaks. Although the presence of a co-eluting interferent may preclude positive
identification of the analyte, the presumptive evidence of its presence may be useful information to
include in the Data Review Narrative.
2. Verify that the RRT of the positively identified target analyte is within ±0.06 RRT units of the RRT
for the same analyte in the associated opening CCV or mid-point standard CSS from the associated
ICAL.
3. Verify that peaks are correctly identified as target analytes, TICs, DMCs, or internal standards on
the chromatogram for samples and blanks.
4. Verify that there is no erroneous analyte identification, either false positive or false negative, for
each target analyte. The positively identified target analyte can be more easily detected for false
positives than false negatives. More information is available for false positives due to the
requirement for submittal of data supporting positive identifications. For non-detected target
analyte, on the other hand, is more difficult to assess. One example of the detection of false
negatives is reporting a target analyte as a TIC.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the non-compliant TICs can be obtained from the CCS
report and may be used as part of the evaluation process.
NOTE: Target analytes reported as false negatives may not have the best match in a TIC search of
a contaminated sample, but its mass spectrum may be present under that of a reported TIC.
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E. Action
1. If the positively identified target analyte mass spectrum does not meet the specified criteria,
qualify detect as unusable (R) or report the result at CRQL and qualify as non-detect (U).
2. If the RRT for a positively identified target analyte is outside the specified RRT windows, qualify
detects as unusable (R) or report the result at CRQL and qualify as non-detect (U).
3. If it is determined that cross-contamination has occurred, use professional judgment to qualify
detects. Annotate any changes made to the reported analytes due to either false positive or negative
identifications or concerns regarding target analyte identifications in the Data Review Narrative.
Note the necessity for numerous or significant changes for laboratory CLP PO action.
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XI. Target Analyte Quantitation and Reported Contract Required Quantitation Limit
A. Review Items
Form 1A-OR, sample preparation sheets, SDG Narrative, quantitation reports, and chromatograms.
B. Objective
The objective is to ensure that the reported results and CRQLs for target analytes are accurate.
C. Criteria
1. Target analyte results, as well as the sample specific CRQLs, must be calculated according to the
correct equations.
2. Target analyte RRF must be calculated using the correct associated internal standard , as listed in
the method. Quantitation must be based on the quantitation ion (m/z) specified in the method for
both the internal standards and target analytes. Target analyte result must be calculated using the
RRF from the associated ICAL.
D. Evaluation
1. Verify that the results for all positively identified analytes are calculated and reported by the
laboratory. Verify that the CRQLs are calculated for the non-detects and reported accordingly.
2. Verify that the correct internal standard, quantitation ion, and RRF are used to calculate the
reported results.
3. Verify that the same internal standard, quantitation ion, and RRF are used consistently.
4. Verify that the sample specific CRQLs have been calculated and adjusted to reflect Percent Solids
(%Solids) and sample dilutions.
a. For soil/sediment samples that are high in moisture (i.e., < 30% solid), evaluation of the
presence of each analyte depends on the anticipated interaction between the analyte and the
total matrix, as well as how the sample was processed.
b. If the phases of a sample were separated and processed separately, no particular qualification
on the grounds of matrix distribution is warranted.
c. If a soil/sediment sample was processed by eliminating most of the water, analytes that are
highly water soluble under ambient conditions may be severely impacted such that their
presence cannot be completely evaluated.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the non-compliant results or CRQLs can be obtained from
the CCS report and may be used as part of the evaluation process
E. Action
1. If any discrepancies are found, contact the Regional CLP PO, who may contact the laboratory to
obtain additional information that could resolve any differences. If a discrepancy remains
unresolved, use professional judgment to decide which value is the most accurate and whether
qualification of data is warranted. Annotate the reasons for any data qualification in the Data
Review Narrative.
2. If errors are detected in results and CRQL calculations, perform a more comprehensive
recalculation.
3. If %Solids for a soil sample is < 10.0%, use professional judgment to qualify detects and
non-detects.
4. If %Solids for a soil sample is > 10.0% and < 30%, use professional judgment to qualify detects and
non-detects.
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5. If %Solids for a soil sample is > 30.0%, detects and non-detects should not be qualified.
6. If sample results are < CRQL and > MDL, qualify as estimated (J).
7. Note numerous or significant failures to accurately quantify the target analytes, or to properly
evaluate and adjust CRQLs, for laboratory CLP PO action.
Table 41. Percent Solids Actions for Semivolatile Analysis for Non-Aqueous Samples
Criteria
%Solids< 10.0%
10.0% < %Solids < 30.0%
%Solids > 30.0%
Action
Detects
Use professional judgment
Use professional judgment
No qualification
Non-detects
Use professional judgment
Use professional judgment
No qualification
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XII. Tentatively Identified Compounds
A. Review Items
Form 1B-OR, chromatograms, library search printouts, and spectra for the TIC candidates.
B. Objective
The objective is to provide tentative identifications to chromatographic peaks that are not identified as
target analytes, DMCs, or internal standards.
C. Criteria
For each sample, the laboratory must conduct a mass spectral search of the National Institute of
Standards and Technology/U.S. Environmental Protection Agency/National Institutes of Heath
[(NIST/EPA/NH) 2011 release or later], and/or Wiley (2011 release or later), or equivalent mass
spectral library, and report the possible identity for up to 30 of the largest peaks which are not DMCs,
internal standards, or target analytes. The peak for a TIC shall have an area or height > 10% of the area
or height of the nearest internal standard. Estimated concentration for a TIC is calculated similarly to
that for a target analyte, using total ion areas for the TIC and the internal standard, and assuming a RRF
of 1.0.
1. Guidelines for tentative identification are as follows:
a. Major ions (> 10% Relative Intensity) in the reference spectrum should be present in the
sample spectrum.
b. The relative intensities of the major ions should agree within ±20% between the sample and the
reference spectra.
c.
1^-L^l^llVV^ OJJ^VLICI.
Molecular ions present in the reference spectrum should be present in the sample spectrum.
TWT j. j. i_ •• _ i :i I. j._i- _j?o£-n/ I. • i • i i_
Non-target compounds receiving a library search match of 85% or higher are considered a
"likely match." The compound should be reported unless the mass spectral interpretation
specialist feels there is evidence not to report the compound as identified by the library search
program. The laboratory should include the justification for not reporting a compound as listed
by the search program in the SDG Narrative.
e. If the library search produces more than one compound > 85%, the compound should be
reported with the highest percent match (report first compound if percent match is the same for
two or more compounds), unless the mass spectral interpretation specialist feels that the highest
match compound should not be reported or another compound with a lower match should be
reported. The laboratory should include the justification for not reporting the compound with
the highest spectral match within the SDG Narrative. DMCs, internal standards, and target
analytes should not be reported as TICs.
f. If the library search produces a series of obvious isomer compounds with library search
matches > 85%, the compound with the highest library search percent match (or the first
compound if the library search matches are the same) should be reported. The laboratory
should note in the SDG Narrative that the exact isomer configuration, as reported, may not be
accurate.
g. If the library search produces no matches > 85%, and in the technical judgment of the mass
spectral interpretation specialist, no valid tentative identification can be made, the compound
should be reported as unknown. The mass spectral specialist should give additional
classification of the unknown compound, if possible (e.g., unknown aromatic, unknown
hydrocarbon, unknown acid type, unknown chlorinated compound). If probable molecular
weights can be distinguished, they should be included.
h. The Chemical Abstracts Service (CAS) registry number is the unique identifier for each
chemical compound. As the rules of chemical nomenclature have changed overtime, each
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chemical substance is liable to have several names or synonyms [i.e., trade or brand name(s);
generic or common name(s); trivial or systematic; or International Union of Pure and Applied
Chemistry (IUPAC) name(s)]. Whether synonyms or other names are created for this
compound, the CAS registry number will remain unchanged. The CAS registry number is
simply an identifier which has no structural significance. Regardless of RTs, if the library
search produces two or more compounds at or above 85% with the same CAS number, the
compound with the highest percent match (report first compound if the percent match is the
same for two or more compounds) should be reported unless the mass spectral interpretation
specialist feels there is just evidence not to report the compound with the highest match.
i. If the library search produces only one and the same compound (i.e., the same CAS registry
number) with the match at or above 85% at two different RTs, the compound having the
highest percent match should be reported as TIC and the other one could be reported as
unknown. If both TICs have the same percent match for the same compound, one of the TICs
could be reported as unknown. Such justifications should be included in the SDG Narrative.
j. Alkanes are not to be reported as TICs on Form 1B-OR. An alkane is defined as any
hydrocarbon with the generic formula CnH2n+2 containing only C-H and C-C single bonds.
When the preceding alkanes are tentatively identified, the concentration(s) should be estimated
and the analytes reported as alkanes by class (i.e., straight-chain, branched, cyclic, as a series,
or as applicable) in the SDG Narrative. Total alkanes concentration should be reported on
Form 1B-OR
D. Evaluation
1. Verify that the laboratory has generated a library search for all required peaks in the
chromatograms for samples and blanks.
2. Verify that TIC peaks present in samples are not found in blanks. When a low-level, non-target
compound that is a common artifact or laboratory contaminant is detected in a sample, a thorough
check of blank chromatograms may require looking for peaks which are < 10% of the internal
standard height, but present in the blank chromatogram at a similar RRT.
3. Verify that mass spectra for all reported TICs are present for every sample and blank.
4. Review ions present in the sample spectrum, but not in the reference spectrum, for possible
background contamination, interference, or presence of coeluting compounds.
5. Review ions present in the reference spectrum, but not in the sample spectrum, for possible
subtraction from the sample spectrum because of background contamination or coeluting
compounds. Data system library reduction programs can sometimes create these discrepancies
6. Consider all reasonable choices since TIC library searches often yield several candidate
compounds having a close matching score.
7. Be aware of common laboratory artifacts/contaminants and their sources (e.g., Aldol condensation
products, solvent preservatives, and reagent contaminants). These may be present in blanks and not
reported as sample TICs, such as:
a. Common laboratory contaminants include CO2 (m/z 44), siloxanes (m/z 73), diethyl ether,
hexane, certain freons, and phthalates at levels < 100 (ig/L.
b. Solvent preservatives include cyclohexene (a methylene chloride preservative). Related
by-products include cyclohexanone, cyclohexenone, cyclohexanol, cyclohexenol,
chlorocyclohexene, and chlorocyclohexanol.
c. Aldol condensation reaction products of acetone include: 4-hydroxy-4-methyl-2-pentanone,
4-methyl-2-penten-2-one, and 5,5-dimethyl-2(5H)-furanone.
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8. A target analyte may be identified by non-target library search procedures, even though it is not
identified as a target analyte (false negative). If the total area quantitation method is used, request
that the laboratory recalculate the result using the proper quantitation ion and RRF.
a. A non-target compound may be incorrectly identified by the instrument's target analyte data
processor as a target analyte (false positive). When this happens, the non-target library search
procedure will not detect the false positive as a TIC. In this case, request that the laboratory
properly identify the analyteas a TIC and recalculate the result using the total area quantitation
method and a RRF of 1.0.
b. Evaluate other sample chromatograms and check for both false negatives and false positives to
determine if the occurrence is isolated or systematic.
9. Verify that the TIC concentration is calculated using an RRF of 1.0.
E. Action
1. If the library search match for a TIC is > 85%, qualify the TIC as tentatively identified with
estimated concentration (NJ).
2. If the library search match for a TIC is < 85%, qualify the TIC as unknown with estimated
concentration (J).
3. General actions related to the review of TIC results are as follows:
a. If it is determined that a tentative identification of a non-target compound is unacceptable,
change the tentative identification to "unknown" or another appropriate identification, and
qualify the result as estimated (J).
b. If library search or proper calculation is not performed for all contractually-required peaks, the
Regional CLP PO may request the data from the laboratory.
c. Use professional judgment to determine whether a library search result for a TIC represents a
reasonable identification. If there is more than one possible match, report the result as "either
compound X or compound Y." If there is a lack of isomer specificity, change the TIC result to
a non-specific isomer result (e.g., 1,3,5-trimethyl benzene to trimethyl benzene isomer) or to a
compound class (e.g., 2-methyl, 3-ethyl benzene to a substituted aromatic compound).
d. Other Case factors may influence TIC judgments. If a sample TIC match is poor, but other
samples have a TIC with a valid library match, similar RRT, and the same ions, infer
identification information from the other sample TIC results.
4. Note any changes made to the reported data or any concerns regarding TIC identifications in the
Data Review Narrative.
5. Note any failure to properly evaluate and report TICs for laboratory CLP PO action.
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XIII. System Performance
A. Review Items
Form 8A-OR and chromatograms.
B. Objective
The objective is to ensure that the system is stable during the analytical sequence to produce quality
data.
C. Criteria
There are no specific criteria for system performance.
D. Evaluation
1. Abrupt discrete shifts in the Reconstructed Ion Chromatogram (RIC) baseline may indicate a
change in the instrument's sensitivity or the zero setting. A baseline "shift" could indicate a
decrease in sensitivity in the instrument or an increase in the instrument zero, possibly causing
target compounds at or near the detection limit to miss detection. A baseline "rise" could indicate
problems such as a change in the instrument zero, a leak, or degradation of the column.
2. Poor chromatographic performance affects both qualitative and quantitative results. Indications of
substandard performance include:
a. High RIC background levels or shifts in Absolute RTs of internal standards.
b. Excessive baseline rise at elevated temperature.
c. Extraneous peaks.
d. Loss of resolution.
e. Peak tailing or peak splitting that may result in inaccurate quantitation.
3. A drift in instrument sensitivity may occur during the 12-hour period and may be an indication of
possible internal standard spiking problems. This could be discerned by examination of the internal
standard area on Form 8A-OR for trends such as a continuous or near-continuous increase or
decrease in the internal standard area over time.
E. Action
1. Use professional judgment to qualify the data if it is determined that system performance has
degraded during sample analyses.
2. Note any degradation of system performance which significantly affected the data for CLP PO
action.
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XIV. Regional Quality Assurance and Quality Control
A. Review Items
Form 1A, chromatograms, TR/COC documentation, quantitation reports, and other raw data from
QA/QC samples.
B. Objective
The objective is to use results from the analysis of the Regional QA/QC samples including field
duplicates, PE samples, blind spikes, and blind blanks to determine the validity of the analytical results.
C. Criteria
Criteria are determined by each Region.
1. PE sample frequency may vary.
2. The target analytes present in the PE sample must be correctly identified and quantified.
3. The RPD between field duplicates shall fall with the specific limits in the Region's Standard
Operating Procedure (SOP) or project QAPP.
D. Evaluation
1. Evaluation procedures must follow the Region's SOP for data review. Each Region will handle the
evaluation of PE samples on an individual basis.
2. Verify that the target analyte in PE sample is properly identified and that the result is calculated
correctly.
3. Verify that the acceptance criteria for the specific PE sample are met, if available.
4. Calculate the RPD between field duplicates and provide this information in the Data Review
Narrative. Also verify that the value falls within the specific limits in the Region's SOP or project
QAPP.
E. Action
1. Any action must be in accordance with Regional specifications and the criteria for acceptable PE or
field duplicate sample results.
2. Note unacceptable results for PE or field duplicate samples for laboratory CLP PO action.
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XV. Overall Assessment of Data
A. Review Items
Entire data package, data review results, and (if available), the QAPP and Sampling and Analysis Plan
(SAP).
B. Objective
The objective is to provide the overall assessment on data quality and usability.
C. Criteria
1. Review all available materials to assess the overall quality of the data, keeping in mind the additive
nature of analytical problems.
2. Reported analyte concentrations must be quantitated according to the appropriate analytical
method, as listed in the method. All sample results must be within the linear calibration ranges per
methods.
D. Evaluation
Examine the raw data to verify that the correct calculation of the sample results was reported by the
laboratory. Analysis logs, instrument printouts, etc., should be compared to the reported sample results
recorded on the appropriate Organic Summary Forms (Form 1A-OR through Form 9B-OR).
1. Evaluate any technical problems which have not been previously addressed.
2. Examine the raw data for any anomalies (e.g, baseline shift).
3. Verify appropriate method is used in sample analysis.
4. Verify that there are no transcription or reduction errors.
5. Verify that target analyte results fall within the calibrated ranges.
6. If appropriate information is available, use professional judgment to assess the usability of the data
to to assist the data user in avoiding inappropriate use of the data. Review all available information,
including the QAPP (specifically the acceptance and performance criteria), SAP, and
communication with the data user that concerns the intended use and desired quality of these data.
E. Action
1. Use professional judgment to determine if there is any need to qualify data which were not
qualified based on the QC criteria previously discussed.
2. Use professional judgment to qualify sample results and non-detects if the MDL exceeds the
CRQL.
3. If a sample is not diluted properly when sample results exceed the upper limit of the calibration
range, qualify sample results as estimated (J).
4. Write a brief Data Review Narrative to give the user an indication of the limitations of the
analytical data.
5. Note any inconsistency of the data with the SDG Narrative for CLP PO action. If sufficient
information on the intended use and required quality of the data is available, include an assessment
of the usability of the data within the given context. This may be used as part of a formal Data
Quality Assessment (DQA).
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PESTICIDE DATA REVIEW
The Pesticide organic data requirements to be reviewed during validation are listed below:
I. Preservation and Holding Times 145
II. Gas Chromatograph with Electron Capture Detector Instrument Performance Check 150
III. Initial Calibration 155
IV. Continuing Calibration Verification 161
V. Blanks 166
VI. Surrogate 169
VII. Matrix Spike/Matrix Spike Duplicate 171
VIII. Laboratory Control Sample 173
IX. Florisil Cartridge Performance Check 175
X. Gel Permeation Chromatography Performance Check 177
XI. Target Analyte Identification 179
XII. Gas Chromatograph/Mass Spectrometer Confirmation 181
XIII. Target Analyte Quantitation and Reported Contract Required Quantitation Limit 182
XIV. Regional Quality Assurance and Quality Control 184
XV. Overall Assessment of Data 185
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I. Preservation and Holding Times
A. Review Items
Form 1A-OR, Traffic Report/Chain of Custody (TR/COC) documentation, raw data, sample extraction
sheets, and the Sample Delivery Group (SDG) Narrative checking for: pH; shipping container
temperature; holding time; and other sample conditions.
B. Objective
The objective is to ascertain the validity of the analytical results based on sample condition and the
holding time of the sample.
C. Criteria
1. The extraction technical holding time is determined from the date of sample collection to the date
of sample extraction for aqueous and non-aqueous (soil and sediment) samples that are not
designated for Toxicity Characteristic Leachate Procedure (TCLP)/Synthetic Precipitation
Leachate Procedure (SPLP) procedures. The extraction technical holding time for samples
designated for TCLP/SPLP is determined from the date of sample collection to the date of
TCLP/SPLP extraction.
2. For TCLP/SPLP leachate samples, extraction technical holding time is determined from the date of
TCLP/SPLP procedure completion to the date of the leachate sample extraction by the specified
preparation methods for aqueous samples. The analysis technical holding time is determined from
the date of sample extraction completion to the date of sample analysis.
3. Samples should be in proper condition with shipping container temperatures at < 6°C upon receipt
at the laboratory. All aqueous and non-aqueous samples shall be protected from light and
refrigerated at < 6°C, (but not frozen) from the time of receipt at the laboratory. The sample
extracts shall be stored at < 6°C (but not frozen) from the time of the extraction completion until
analysis.
4. The extraction technical holding time criteria for aqueous samples, TCLP/SPLP aqueous samples,
and TCLP/SPLP leachate samples that are properly preserved is 7 days.
5. The extraction technical holding time criteria for soil samples designated for TCLP/SPLP is 14
days.
6. The extraction technical holding time criteria for non-aqueous samples that are properly preserved
is 14 days.
7. The analysis technical holding time criteria for extracts, including TCLP/SPLP leachate sample
extracts, that are properly preserved is 40 days.
D. Evaluation
1. Review the SDG Narrative and the TR/COC documentation to determine if the samples are
received intact and iced. If there is an indication of problems with the samples, the sample integrity
may be compromised.
2. Verify that the extraction dates and the analysis dates for samples on Form 1A-OR and the raw
data/SDG file are identical.
3. Establish extraction technical holding times for sample excluding TCLP/SPLP leachate by
comparing the sample collection dates on the TR/COC documentation with the dates of extraction
on Form 1A-OR and the sample extraction sheets.
4. Establish extraction technical holding times for samples undergone TCLP/SPLP procedure by
comparing the sample collection dates on the TR/COC documentation with the dates of extraction
on sample extraction sheets.
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5. Establish extraction technical holding times for TCLP/SPLP leachates by comparing the dates of
TCLP/SPLP extraction on TCLP/SPLP extraction sheets with the dates of extraction on Form
1A-OR and preparative extraction log.
6. Determine the analysis technical holding times for samples after the completion of extraction by
comparing the dates of extraction with the dates of analysis on Form 1A-OR, as well as from the
analytical run logs.
E. Action
1. If samples are received with shipping container temperatures > 6°C, use professional judgment to
qualify detects and non-detects.
2. If TCLP/SPLP extraction is performed within the 14-day technical holding time for soil samples
designated for TCLP/SPLP, detects and non-detects should not be qualified.
3. If TCLP/SPLP extraction is performed outside the 14-day technical holding time for soil samples
designated for TCLP/SPLP, qualify detects as estimated low (J-) and non-detects as unusable (R).
Use caution in determining whether some detected analytes should be qualified as estimated low
(J-) or as estimated (J+), based on knowledge of individual analyte stability or interactions.
4. If discrepancies are found between the sample extraction date or analysis date and the date on raw
data, perform a more comprehensive review contacting the laboratory if necessary, through the
Regional Contract Laboratory Program Project Officer (CLP PO), to determine the correct dates
for establishing technical holding times.
5. If an aqueous, TCLP/SPLP aqueous sample, or TCLP/SPLP leachate sample is not properly
preserved, but extraction is performed within the 7-day technical holding time, and the extract is
analyzed within the 40-day technical holding time, consider the extent of temperature excursion in
addition to overall sample integrity and use professional judgment to qualify detects and
non-detects.
6. If an aqueous, TCLP/SPLP aqueous sample, or TCLP/SPLP leachate sample is not properly
preserved and extraction is performed outside the 7-day technical holding time, and the extract is
analyzed outside the 40-day technical holding time, qualify detects as estimated (J) and non-detects
as unusable (R). Use caution in determining whether some detected analytes should be qualified as
estimated low (J-) or estimated high (J+), based on knowledge of individual analyte stability or
interactions.
7. If an aqueous, TCLP/SPLP aqueous sample, or TCLP/SPLP leachate sample is properly preserved,
extraction is performed within the 7-day technical holding time, and the extract is analyzed within
the 40-day technical holding time, detects and non-detects should not be qualified.
8. If an aqueous, TCLP/SPLP aqueous sample, or TCLP/SPLP leachate sample is properly preserved,
but extraction is performed outside the 7-day technical holding time, and the extract is analyzed
outside the 40-day technical holding time, consider all evidence of compromised extract integrity
(such as evaporation, refrigeration), in addition to overall sample integrity and use professional
judgment to qualify the data, in particular the direction of the bias.
9. If a non-aqueous sample is not properly preserved, but extraction is performed within the 14-day
technical holding time, and the extract is analyzed within the 40-day technical holding time, use
professional judgment to qualify detects and non-detects.
10. If a non-aqueous sample is not properly preserved, and extraction is performed outside the 14-day
technical holding time, and the extract is analyzed outside the 40-day technical holding time, use
professional judgment to qualify detects and non-detects.
11. If non-aqueous sample is properly preserved, and extraction is performed within the 14-day
technical holding time, and the extract is analyzed within the 40-day technical holding time, detects
and non-detects should not be qualified.
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12. If non-aqueous sample is properly preserved, but extraction is performed outside the 14-day
technical holding time, and the extract is analyzed outside the 40-day technical holding time,
qualify detects as estimated low (J-) and non-detects as unusable (R). Use caution in determining
whether some detected analytes should be qualified as estimated low (J-) or estimated high (J+),
based on knowledge of individual analyte stability or interactions.
13. Annotate the effect of exceeding the holding time on the resulting data in the Data Review
Narrative, whenever possible.
14. If technical holding times are grossly exceeded, qualify detects as estimated (J). Use professional
judgment to qualify non-detects as unusable (R). Note this for laboratory CLP PO action.
15. If samples are received with shipping container temperatures > 10°C, use professional judgment to
qualify detects and non-detects.
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Table 42. Preservation and Holding Time Actions for Pesticide Analysis
Matrix
Aqueous
Non-aqueous
Preserved
No
No
Yes
Yes
Yes/No
No
No
Yes
Yes
Yes/No
Criteria
< 7 days (for extraction) and
< 40 days (for analysis)
TCLP/SPLP aqueous and
TCLP/SPLP leachate
sample extracted within the
7-day technical holding
time
> 7 days (for extraction) and
> 40 days (for analysis)
TCLP/SPLP aqueous and
TCLP/SPLP leachate
sample not extracted within
the 7-day technical holding
time
< 7 days (for extraction) and
< 40 days (for analysis)
TCLP/SPLP aqueous and
TCLP/SPLP leachate
sample extracted within the
7-day technical holding
time
> 7 days (for extraction) and
> 40 days (for analysis)
TCLP/SPLP aqueous and
TCLP/SPLP leachate
sample not extracted within
the 7-day technical holding
time
Holding time grossly
exceeded
< 14 days (for extraction)
and < 40 days (for analysis)
> 14 days (for extraction)
and > 40 days (for analysis)
< 14 days (for extraction)
and < 40 days (for analysis)
> 14 days (for extraction)
and > 40 days (for analysis)
Holding time grossly
exceeded
Action
Detect
Non-Detect
Use professional judgment
J
Use professional
judgment
No qualification
J
J
UJ
UJorR
Use professional judgment
J
Use professional
judgment
No qualification
J
J
UJ
UJorR
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Table 43. Holding Time Actions for Non-Aqueous Pesticide TCLP/SPLP Sample Analysis
Preserved
No
No
Yes
Yes
Yes/No
Criteria
TCLP/SPLP performed
within the 14-day technical
holding time
TCLP/SPLP not performed
within the 14-day technical
holding time
TCLP/SPLP performed
within the 14-day technical
holding time
TCLP/SPLP not performed
within the 14-day technical
holding time
Holding time grossly
exceeded
Action
Detect
Non-Detect
Use professional judgment
J
Use professional
judgment
No qualification
J
J
UJ
UJorR
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II. Gas Chromatograph with Electron Capture Detector Instrument Performance Check
A. Review Items
Form 6G-OR, Form 7B-OR, chromatograms, and data system printouts.
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. Criteria
1. Resolution Check Mixture
a. The Resolution Check Mixture (RESC) is analyzed at the beginning of every initial calibration
(ICAL) sequence on each GC column and instrument used for analysis. The RESC contains
the following target analytes and surrogates listed in Table 44:
Table 44. Resolution Check Mixture
trans -Chlordane
Endosulfan I
4,4'-DDE
Dieldrin
Endosulfan sulfate
alpha-BHC
beta-BHC
delta-BHC
gamma-BHC
Aldrin
Heptachlor
Endrin ketone
Methoxychlor
Endosulfan II
Heptachlor-epoxide
cis-Chlordane
4,4'-DDD
4,4'-DDT
Endrin
Endrin aldehyde
Tetrachloro-m-xylene (surrogate)
Decachlorobiphenyl (surrogate)
b. The resolution between two adjacent peaks in RESC must be > 80.0% for all analytes for the
primary column, and > 50.0% for the confirmation column in order to use Individual Standard
Mixture C (INDC). If Individual Standard Mixture A (INDA) and Individual Standard Mixture
B (INDB) are used, the resolution between two adjacent peaks must be > 60.0%.
2. Performance Evaluation Mixture
a. The Performance Evaluation Mixture (PEM) is analyzed at the beginning (following the
Resolution Check Standard) and at the end of the ICAL sequence. The PEM analysis must
bracket one end of each 12-hour analytical period. The PEM contains the following target
analytes and surrogates listed in Table 45:
Table 45. Performance Evaluation Mixture (PEM)
gamma-BHC
alpha-BHC
4,4'-DDT
beta-BHC
Endrin
Methoxychlor
Tetrachloro-m-xylene (surrogate)
Decachlorobiphenyl (surrogate)
b. The resolution between any two adjacent peaks in the ICAL and Continuing Calibration
Verification (CCV) PEMs must be > 90% on each GC column.
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c. The Percent Breakdown (%Breakdown) is the amount of decomposition that 4,4'-DDT and
Endrin undergo when analyzed on the GC column. For Endrin, the %Breakdown is determined
by the presence of Endrin aldehyde and/or Endrin ketone in the PEM. For 4,4'-DDT, the
%Breakdown is determined by the presence of 4,4'-DDD and/or 4,4'-DDE in the PEM.
i. The %Breakdown of 4,4'-DDT and Endrin in the PEMs must each be < 20.0% on each GC
column.
ii. The combined %Breakdown for 4,4'-DDT and Endrin in PEMs must be < 30.0% on each
GC column.
d. Mid-point Individual Standard Mixtures A and B or C
i. The resolution capabilities of the GC/ECD system used will dictate whether INDA and
INDB (see Table 46) or INDC (see Table 47) can be used. This is determined by the
analysis of the RESC to see if the criteria in Il.C.l.b are met. If Individual Standard
Mixtures A and B are used, follow the procedure in 3e. If INDC is used, follow the
procedure in 3f
e. Mid-point Individual Standard Mixtures A and B
i. The mid-point INDA/INDB are analyzed as part of the ICAL. The ICAL mid-point CS3
standards, INDA and INDB, must be analyzed to bracket one end of the subsequent
12-hour analytical sequence for the associated ICAL sequence containing INDA and
INDB standards. The Individual Standard Mixtures contain the target analytes and
surrogates listed in Table 46.
ii. The Percent Resolution (%Resolution) between any two adjacent peaks in the mid-point
concentration of INDA and INDB in the ICAL and the subsequent CCVs must be > 90.0%
on each column.
Table 46. Individual Standard Mixtures A and B
Individual Standard Mixture A
alpha-BHC
Heptachlor
gamma-BHC
Endosulfan I
Dieldrin
Endrin
4,4'-DDD
4,4'-DDT
Methoxychlor
Tetrachloro-m-xylene (surrogate)
Decachlorobiphenyl (surrogate)
Individual Standard Mixture B
beta-BHC
delta-BHC
Aldrin
Heptachlor-epoxide
cis-Chlordane
trans -Chlordane
4,4'-DDE
Endosulfan sulfate
Endrin aldehyde
Endrin ketone
Endosulfan II
Tetrachloro-m-xylene (surrogate)
Decachlorobiphenyl (surrogate)
f. Mid-point Individual Standard Mixture C
i. The mid-point INDC is analyzed as part of the ICAL. The ICAL mid-point CS3 standard,
INDC, must be analyzed to bracket one end of the subsequent 12-hour analytical sequence
for the associated ICAL sequence containing INDC standards. The INDC contains target
analytes and surrogates listed in Table 47.
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ii. The %Resolution between any two adjacent peaks in the mid-point concentration of INDC
in the ICAL and CCV must be > 80.0% for the primary column and > 50.0% for the
secondary column.
Table 47. Individual Standard Mixture C
alpha-BHC
beta-BHC
delta-BHC
gamma-BHC
Aldrin
Heptachlor
Heptachlor-epoxide
cis-Chlordane
trans-Chlordane
Endosulfan I
Endosulfan II
4,4'-DDD
4,4'-DDE
4,4'-DDT
Dieldrin
Endrin
Endosulfan sulfate
Endrin ketone
Endrin aldehyde
Methoxychlor
Tetrachloro-m-xylene
Decachlorobiphenyl
D. Evaluation
1. Resolution Check Mixture
a. Verify that RESC is analyzed at the specified frequency and sequence.
b. Check RESC data and Form 6G-OR to verify that if INDA and INDB are used in the analytical
sequence, and that %Resolution between two adjacent peaks for the required target analytes
and surrogates in RESC is > 60.0% on both GC columns.
c. Verify that if INDC is used in the analytical sequence, %Resolution between two adjacent
peaks for the required analytes and surrogates in RESC is > 80.0% on the primary column and
> 50.0% on the secondary column.
2. Performance Evaluation Mixture
a. Verify that PEM is analyzed at the specified frequency and sequence.
b. Check the ICAL and CCV PEM data and Form 6G-OR to verify that %Resolution between
adjacent peaks is > 90.0% on both GC columns.
c. Check Form 7B-OR to verify that the %Breakdown of 4,4'-DDT is < 20.0%, the %Breakdown
of Endrin is < 20.0%, and the combined %Breakdown of 4,4'-DDT and Endrin is < 30.0% in all
PEMs on both GC columns.
3. Mid-point Individual Standard Mixtures A and B
a. Check the ICAL and CCV mid-point INDA and INDB data on Form 6G-OR to verify that the
resolution between adjacent peaks is > 90.0% on both GC columns.
4. Mid-point Individual Standard Mixture C
a. Check the ICAL and CCV mid-point INDC data on Form 6G-OR to verify that the resolution
between adjacent peaks is > 80.0% for the primary column and 50.0% for the secondary
column.
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NOTE: For data obtained from the Contract Laboratory Program (CLP), the preceding criteria are
evaluated as part of the Contract Compliant Screening (CCS) process. Information
regarding the non-compliant Resolution and %Breakdown can be obtained from the
National Functional Guidelines (NFG) reports and may be used as part of the evaluation
process.
E. Action
1. Resolution Check Mixture
a. If RESC is not performed at the specified sequence or frequency, use professional judgment to
qualify detects and non-detects.
b. If RESC %Resolution criteria are not met, qualify detects as presumptively present with
estimated concentration (NJ) and non-detects as unusable (R).
2. Performance Evalutaion Mixture
a. If PEM is not performed at the specified frequency and sequence, qualify detects and
non-detects as unusable (R).
b. If PEM resolution criteria are not met, qualify detects as presumptively present with estimated
concentration (NJ) and non-detects as unusable (R).
c. If 4,4'-DDT %Breakdown is > 20.0%,qualify detected 4,4'-DDT, 4,4'-DDD and 4'4'-DDE as
estimated (J). When 4,4'-DDT is not detected, but 4,4'-ODD and 4,4'-DDE are detected,
qualify non-detected 4,4'-DDT as unusable (R) and detected 4,4'-ODD and 4,4'-DDE as
presumptively present with estimated concentration (NJ).
d. If Endrin %Breakdown > 20.0%, qualify detected Endrin, Endrin aldehyde, and Endrin ketone
as estimated (J). When Endrin is not detected, but Endrin aldehyde and Endrin ketone are
detected, qualify non-detected Endrin as unusable (R) and detected Endrin aldehyde and
Endrin ketone as presumptively present with estimated concentration (NJ).
e. If the combined %Breakdown for 4,4'-DDT and Endrin is > 30.0%, consider the degree of
individual breakdown of 4,4'-DDT and Endrin and qualify as in sections II.E.2.C and II.E.2.d
accordingly.
3. Mid-point Individual Standard Mixtures (A and B) or (C)
a. If mid-point Individual Standard Mixture CS3 is not performed at the specified frequency,
qualify detects and non-detects as unusable (R).
4. If mid-point Individual Standard Mixture CS3 resolution criteria are not met, qualify detects as
presumptively present with estimated concentration (NJ) and non-detects as unusable (R).
5. Annotate the potential effects on the sample data resulting from the instrument performance check
criteria in the Data Review Narrative.
6. If the laboratory has repeatedly failed to comply with the requirements for linearity, resolution, or
4,4'-DDT/Endrin %Breakdown, notify the laboratory CLP PO.
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Table 48. GC/ECD Instrument Performance Check Actions
Criteria
RESC not performed at the specified frequency and
sequence
RESC
% Resolution <60.0%
(INDA/INDB)
PEM not performed at the
sequence
RESC
% Resolution <80.0%
(INDC, primary column)
% Resolution <50.0%
(INDC) secondary column)
specified frequency and
PEM %Resolution < 90.0%
PEM: 4,4'-DDT %Breakdown > 20.0% and 4,4'-DDT is
detected
PEM: 4,4'-DDT %Breakdown > 20.0% and 4,4'-DDT is
not detected
PEM: Endrin %Breakdown > 20.0% and Endrin is
detected
PEM: Endrin %Breakdown > 20.0% and Endrin is not
detected
PEM: Combined %Breakdown > 30%
CSS INDA/INDB or INDC not performed at the specified
frequency
%Resolution < 90.0%
(CSS INDA and INDB)
%Resolution < 80.0% (CSS
INDC, primary column)
%Resolution < 50.0% ( CSS
INDC, secondary column)
Action
Detect
Use professional
judgment
NJ
R
NJ
J for 4,4'-DDT,
4,4 '-ODD,
4,4'-DDE
R for 4,4'- DDT
J for Endrin,
Endrin aldehyde,
Endrin ketone
R for Endrin
Apply qualifiers as
described above
considering degree
of individual
breakdown.
R
NJ
Non-detect
Use professional
judgment
R
R
R
No qualification
NJ for 4,4'-DDD and
4,4'-DDE
No qualification
NJ for aldehyde and
Endrin ketone
Apply qualifiers as
described above
considering degree of
individual
breakdown.
R
R
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III. Initial Calibration
A. Review Items
Form 6B-OR, Form 6C-OR, Form 6D-OR, Form 6E-OR, Form 6F-OR, chromatograms, and data
system printouts.
B. Objective
The objective of ICAL is to ensure that the instrument is capable of producing acceptable qualitative
and quantitative data.
C. Criteria
1. INDA/INDB or INDC must be analyzed at five concentration levels during the ICAL on each GC
column and instrument used for analysis. The ICAL shall be performed following specific
sequence as in the recommended Sequence 1 or 2 in Tables 50 and 51.
2. The five concentration level standards containing all single component target analytes and
surrogates shall be prepared in either Individual Standard Mixtures A and B or Individual Mixture
C at the concentration levels listed in Table 49.
3. A single-point Toxaphene calibration at low standard should be included in the intial calibration at
a minimum. Optionally, all five-point ICAL standards at Toxaphene concentration levels in Table
49 may be included in the ICAL as in Sequence 1 or 2 in Tables 50 and 51. When Toxaphene is
identified in any sample analysis with a single-point ICAL, a 5-point calibration must be performed
for Toxaphene qualitative and quantitive analysis in the sample reanalysis.
4. The Mean Retention Times (RTs) of each single component target analyte and surrogates are
determined from the five-point ICAL. For Toxaphene, Retention Times (RTs) are determined for
five major peaks. The peaks chosen must not share the same RT Window as any single component
target analyte. The RT for the surrogates is measured from each INDA and INDB.
5. An RT Window must be calculated for each single component target analyte, each Toxaphene peak
and each surrogate, accordingly.
NOTE: At least one chromatogram from each of the Individual Standard Mixtures (A and B) or (C)
must yield peaks that give recorder deflections between 50-100% of full scale.
Table 49. Concentration Levels of Calibration Standards
Analyte
alpha-BHC
gamma-BHC
Heptachlor
Endosulfan I
Dieldrin
Endrin
4,4'-DDD
4,4'-DDT
Methoxychlor
beta-BHC
Concentration (ng/mL)
CS1
5.0
5.0
5.0
5.0
10
10
10
10
50
5.0
CS2
10
10
10
10
20
20
20
20
100
10
CS3
20
20
20
20
40
40
40
40
200
20
CS4
40
40
40
40
80
80
80
80
400
40
CSS
80
80
80
80
160
160
160
160
800
80
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Analyte
delta-BHC
Aldrin
Heptachlor-epoxide
4,4'-DDE
Endosulfan II
Endosulfan sulfate
Endrin ketone
Endrin aldehyde
cis-Chlordane
trans-Chlordane
Tetrachloro-m-xylene
(surrogate)
Decachlorobiphenyl
(surrogate)
Toxaphene
Concentration (ng/mL)
CS1
5.0
5.0
5.0
10
10
10
10
10
5.0
5.0
5.0
10
500
CS2
10
10
10
20
20
20
20
20
10
10
10
20
1000
CS3
20
20
20
40
40
40
40
40
20
20
20
40
2000
CS4
40
40
40
80
80
80
80
80
40
40
40
80
4000
CSS
80
80
80
160
160
160
160
160
80
80
80
160
8000
6. Calibration Factors (CFs) must be calculated for each single component target analyte, each of the
five major Toxaphene peaks, and each surrogate in the ICAL standard. Mean Calibration Factor
(CF) must be calculated accordingly for the 5-point ICAL.
7. The Percent Relative Standard Deviation (%RSD) of the CFs for each of the single component
target analytes must be < 20.0%, except for alpha-BHC and delta-BHC. The %RSD of the CFs for
alpha-BHC and delta-BHC must be < 25.0%. The %RSD of the CFs for each of the Toxaphene
peaks must be < 30.0% when 5-point ICAL is performed. The %RSD of the CFs for the two
surrogates [tetrachloro-m-xylene (TCX) and decachlorobiphenyl (DCB)] must be < 30.0%.
NOTE: Either peak area or peak height may be used to calculate the CFs that are, in turn, used to
calculate %RSD. However, the type of peak measurement used to calculate each CF for a
given compound must be consistent. For example, if peak area is used to calculate the
low-point CF for Endrin, the mid-point and high-point CFs for Endrin must also be
calculated using peak area.
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Table 50. Initial Calibration Sequence 1
Initial Calibration Sequence 1
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
Resolution Check
Performance Evaluation Mixture
(PEM)
Toxaphene CS1
Toxaphene CS2
Toxaphene CS3
Toxaphene CS4
Toxaphene CSS
CS 1 Individual Standard Mixture
CS2 Individual Standard Mixture
CS3 Individual Standard Mixture
CS4 Individual Standard Mixture
CSS Individual Standard Mixture
C
C
C
C
C
Instrument Blank
PEM
Table 51. Initial Calibration Sequence 2
Initial Calibration Sequence 2
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
Resolution Check
Performance Evaluation Mixture (PEM)
Toxaphene CS1
Toxaphene CS2
Toxaphene CS3
Toxaphene CS4
Toxaphene CSS
CS 1 Individual Standard Mixture A
CS 1 Individual Standard Mixture B
CS2 Individual Standard Mixture A
CS2 Individual Standard Mixture B
CS3 Individual Standard Mixture A
CS3 Individual Standard Mixture B
CS4 Individual Standard Mixture A
CS4 Individual Standard Mixture B
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Initial Calibration Sequence 2
16.
17.
18.
19.
CSS Individual Standard Mixture A
CSS Individual Standard Mixture B
Instrument Blank
PEM
NOTE: For ICAL Sequence 2, Individual Standards for Mixture B may be analyzed before
corresponding Individual Standards for Mixture A.
D. Evaluation
1. Verify that ICAL is performed at the specified frequency and sequence. Verify that the proper
ICAL sequence (1 or 2) is used depending on if INDC or INDA/INDB is used. Verify that
single-point Toxaphene calibration at low standard is included in the ICAL or a 5-point Toxaphene
calibration is included in either one of the ICAL sequence 1 and 2.
2. Check raw data for each standard in the ICAL to verify that the concentration for each single
component target analyte, Toxaphene, and surrogate is at the specified concentration level.
3. Check the INDA/INDB data or Individual Standard Mixture C data and Form 6B-OR to review the
calculated RT Windows for calculation and transcription errors.
4. Check Toxaphene ICAL standard data and Form 6D-ORto verify that five major peaks are used for
identification, and RT Windows are calculated as specified. Verify that the peaks chosen do not
share the same RT Window as any single component target analyte in any Individual Standard
Mixture.
5. Check the chromatograms and verify that at least one chromatogram from each of the INDA/INDB,
INDC, or Toxaphene standard yields peaks registering recorder/printer deflections between
50-100% of full scale.
6. Check and recalculate the CFs, CFs, and %RSD for one or more single component target analytes
in INDA/INDB, INDC, or Toxaphene standard. Verify that the recalculated values agree with the
reported values on Forms 6C-OR and 6E-OR. If errors are detected, perform a more
comprehensive recalculation and review.
7. Verify that %RSD for each single component target analyte, each of the five major Toxaphene
peaks and each surrogate in the initial standard is within the acceptance limits.
NOTE:
E. Action
For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the non-compliant RT windows and %RSD can be
obtained from the NFG reports and may be used as part of the evaluation process.
1. If ICAL is not performed at the specified frequency or sequence, use professional judgment to
qualify detects and non-detects. Contact the Regional CLP PO to arrange for reanalysis, if
possible, or note in the Data Review Narrative for later CLP PO action.
2. If the ICAL is not performed at the specified concentrations, use professional judgment to qualify
detects and non-detects. This is especially critical for the low-level standards and non-detects.
3. If errors are detected in the calculations of RT Windows, CFs, CFs, or %RSD, perform a more
comprehensive recalculation.
4. If the chromatogram display criteria are not met, use professional judgment to qualify detects and
non-detects.
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5. If %RSD for any target analyte or surrogate is outside the accptacne limits, qualify detects as
estimated (J). Use professional judgment to qualify non-detects.
6. If %RSD for all target analytes are within the acceptance limits, detects and non-detects should not
be qualified.
7. Based on the project-specific Data Quality Objectives (DQOs), a more in-depth review may be
considered using the following guidelines:
a. If %RSD criteria of any target analytes are not met, and if %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.
b. If the high-point of the ICAL curve is outside of the %RSD criteria (e.g., due to saturation):
i. Qualify detects in the associated samples with analyte concentrations greater than the
high-point concentration as estimated (J).
ii. Detects in the associated samples with analyte concentrations within the calibration range
should not be qualified.
iii. Non-detects in the associated samples should not be qualified.
c. If the low-point of the ICAL curve is outside of the %RSD criteria:
i. Qualify detects in the associated samples with analyte concentrations in the non-linear
range as estimated (J).
ii. Detects in the associated samples with analyte concentrations within the calibration range
should not be qualified.
iii. 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.
8. If the laboratory failed to provide adequate calibration information, notify the Regional CLP PO,
who may contact the laboratory to request the necessary information. If the information is not
available, use professional judgment to assess the data.
9. Annotate the potential effects on the reported data due to exceeding the ICAL criteria in the Data
Review Narrative.
10. If the ICAL criteria are grossly exceeded, contact the Regional CLP PO to arrange for reanalysis, if
possible, or note it in the Data Review Narrative for later CLP PO action.
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Table 52. Initial Calibration Action for Pesticide Analysis
Criteria
Initial calibration not performed or not
performed at specified frequency and
sequence
Initial calibration not performed at the
specified concentrations
RT Windows incorrect,
Or chromatogram criteria not met
%RSD outside acceptance limits*
%RSD within acceptance limits*
Action
Detect
Contact CLP PO for
reanalysis or use
professional judgment
Contact CLP PO for
reanalysis or use
professional judgment
Contact CLP PO for
reanalysis or use
professional judgment
J
No qualification
Non-detect
Contact CLP PO for
reanalysis or use
professional judgment
Contact CLP PO for
reanalysis or use
professional judgment
Contact CLP PO for
reanalysis or use
professional judgment
Use professional judgment
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).
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IV. Continuing Calibration Verification
A. Review Items
Form 7B-OR, Form 7C-OR, Form 7D-OR, chromatograms, and data system printouts.
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. Criteria
1. The calibration for each GC/ECD system used for analysis must be verified at the beginning and
end of every 12-hour period of operation. A CCV consisting of the analyses of instrument blanks,
the PEM, and the mid-point ICAL standard CSS for Individual Standard Mixtures A and B or
Individual Standard Mixture C is performed. The opening and closing CCVs consist of an injection
of an instrument blank followed by either an injection of an PEM or mid-point concentration of
INDA and INDB or INDC in an alternating fashion (i.e., if the PEM is part of the opening CCV, the
mid-point ICAL standard CSS for INDA and INDB or INDC must be part of the closing CCV). For
Toxaphene analyses under a five-point calibration, the sequence must end with an instrument blank
and a CSS Toxaphene Standard.
2. CCV PEM standard must contain the specified target analytes and surrogates at the specified
concentration.
3. CCV CSS standards must contain all required target analytes and surrogates at the mid-point
standard concentration of the ICAL.
4. The Absolute RT for each single component target analyte and surrogate in the CCV PEM and CSS
of Individual Standard Mixtures A and B or Individual Standard Mixture C must be within the RT
Windows determined from the ICAL. If the CCV CSS of Toxaphene is required, the absolute RT
for each Toxaphene peak must be within the RT Windows determined from the ICAL.
5. The Percent Difference (%D) between the calculated amount and the nominal amount (amount
added) for each single component target analyte and surrogate in the CCV PEM must be calculated.
%Breakdown of 4,4'-DDT, %Breakdown of Endrin and combined %Breakdown of 4,4'-DDT and
Endrin must be calculated accordingly for CCV PEM.
6. %D between the CF and CF from the associated ICAL for each target analyte and surrogate in CCV
CSS and the CF %D for each Toxaphene peak in the applicable CCV CSS must be calculated
accordingly.
7. %D for each single component target analyte and surrogate in the CCV PEM must be in the
inclusive range of ±25.0%.
8. %Breakdown of 4,4'-DDT and %Breakdown of Endrin in CCV PEM must be < 20.0% and
combined %Breakdown of 4,4'-DDT and Endrin in CCV PEM must be < 30.0%.
9. %D for each target analyte and surrogate in CCV CSS must be in the inclusive range of ±25.0%.
10. %D for each Toxaphene peak in the applicable CCV CSS must be in the inclusive range of
±25.0%.
11. Instrument blanks paired with either PEM or CSS standard must bracket the 12-hour analytical
sequence. The concentration of each target analyte in the instrument blank must not exceed the
Contract Required Quantitation Limit (CRQL).
12. No more than 14 hours may elapse from the injection of the instrument blank that begins an
analytical sequence (opening CCV) and the injection of either a PEM or CSS that ends an analytical
sequence (closing CCV).
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13. No more than 12 hours may elapse from the injection of the instrument blank that begins an
analytical sequence (opening CCV) and the injection of the last sample or blank that is part of the
same analytical sequence.
D. Evaluation
1. Verify that the CCV PEM and CSS including Toxaphene CSS are analyzed at the specified
frequency and sequence and that each CCV standard is associated to the correct ICAL.
2. Verify that specified target analyates and surrogates at the correct concentrations are included in
CCV PEM.
3. Verify that the mid-point standard CSS from the ICAL is used for CCV and the specified target
analytes and surrogates are included in each CSS standard.
4. Verify that the absolute RT for each single component target analyte and surrogate in the CCV
PEM and CSS of Individual Standard Mixtures A and B or Individual Standard Mixture C are
within the RT Windows determined from the ICAL. Verify that the absolute RT for each
Toxaphene peak in the applicable CSS standard is within the RT Window determined from the
ICAL.
5. Verify that %D for each single component target analyte and surrogate in the CCV PEM is
calculated correctly; that %Breakdown of 4,4'-DDT, %Breakdown of Endrin and combined
%Breakdown of 4,4'-DDT and Endrin in the CCV PEM are calculated correctly; and that the
recalculated values agree with the laboratory reported values on Form 7B-OR. Recalculate %D for
at least one target analyte, surrogate, and all three %Breakdowns in each CCV PEM.
6. Verify that %D for each target analyte and surrogate in CCV CSS and the CF %D for each
Toxaphene peak in the applicable CCV CSS are calculated correctly, and that the recalculated
values agree with the laboratory reported values on Form 7C-OR and Form 7D-OR, respectively.
Recalculate %D for at least one target analyte, surrogate, and all five Toxaphene peaks in each CSS
standard.
7. Verify that %D for each single component target analyte and surrogate in the CCV PEM are in the
inclusive range of ±25.0%.
8. Verify that %Breakdown of 4,4' -DDT and %Breakdown of Endrin in CCV PEM are < 20.0% and
that the combined %Breakdown of 4,4'-DDT and Endrin in CCV PEM is < 30.0%,
9. Verify that %D for each target analyte and surrogate in CCV CSS are in the inclusive range of
±25.0%.
10. Verify that %D for each Toxaphene peak in the applicable CCV CSS is in the inclusive range of
±25.0%.
11. Verify that the instrument blanks paired with either PEM or CSS standard are analyzed at the
specified frequency and sequence and that the concentration of each target analyte in the instrument
blank is not exceeding CRQL.
12. Verify that the time elapse between the injection of an instrument blank as opening CCV and the
injection of either a PEM or CSS as closing CCV is within 14 hours.
13. Verify that the time elapse between the injection of an instrument blank as opening CCV and the
injection of the last sample or blank in the same analytical sequence is within 12 hours.
NOTE: For data obtained from the CLP, information regarding the non-compliant CCV can be
obtained from the NFG reports and may be used as part of the evaluation process.
E. Action
1. If the CCV PEM or CSS is not performed at the specified frequency and sequence, contact the
Regional CLP PO to request that the laboratory repeat the analysis if holding times have not
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expired and there is extract remaining. If reanalysis is not possible, carefully evaluate all other
available information, including the 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).
2. If the CCV PEM is not performed at the specified concentration, use professional judgment to
qualify detects and non-detects.
3. If the CCV CSS is not performed at the specified concentration, use professional judgment to
qualify detects and non-detects.
4. If the RT of any target analyte in CCV PEM and CSS standard is outside RT Window, carefully
evaluate the associated sample results. All samples injected after the last in-control standard are
potentially affected.
a. For non-detected target analytes in the affected samples, check 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 are present, non-detects should not be qualified.
ii. If any peaks are present close to the expected RT Window of the analytes of interest, use
professional judgment to qualify the non-detects as presumptively present with estimated
concentration (NJ).
b. For detected target analytes in the affected samples, check 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 package may be examined for the presence of three or more standards
containing the target analytes of interest that were run within the analytical sequence during
which the sample was analyzed. If three or more such standards are present, the RT Window
can be re-evaluated using the RTs of the standards.
i. If the peaks in the affected sample fall within the revised window, qualify detects as
presumptively present with estimated concentration (NJ).
ii. If the problem of concern remains unresolved, qualify detects as unusable (R).
5. If errors are detected in the calculations of either %D or %Breakdown in CCV PEM, perform a
more comprehensive recalculation.
6. If errors are detected in the calculations of %D in any CSS standard or %D for any Toxaphene peak
in the applicable CCV CSS, perform a more comprehensive recalculation. Contact the Regional
CLP PO to arrange for data resubmittal and note it in the Data Review Narrative for later CLP PO
action.
7. If %D for any target analyte in CCV PEM is outside the limits, qualify detects as estimated (J) and
non-detects as estimated (UJ).
8. If 4,4'-DDT %Breakdown is > 20.0%, qualify detected 4,4'-DDT, 4,4'-DDD and 4'4'-DDE as
estimated (J). When 4,4'-DDT is not detected, but 4,4'-ODD and 4,4'-DDE are detected, qualify
non-detected 4,4'-DDT as unusable (R) and detected 4,4'-DDD and 4,4'-DDE as presumptively
present with estimated concentration (NJ).
9. If Endrin %Breakdown > 20.0%, qualify detected Endrin, Endrin aldehyde and Endrin ketone as
estimated (J). When Endrin is not detected, but Endrin aldehyde and Endrin ketone are detected,
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qualify non-detected Endrin as unusable (R) and detected Endrin aldehyde and Endrin ketone as
presumptively present with estimated concentration (NJ).
10. If the combined %Breakdown for 4,4'-DDT and Endrin is > 30.0%, consider the degree of
individual breakdown of 4,4'-DDT and Endrin and qualify as in sections FV.E.8 and FV.E.9
accordingly.
11. If %D for any target analyte in CCV CSS is outside the limits, qualify detects as estimated (J) and
non-detects as estimated (UJ).
12. If time elapse between the injection of an instrument blank as opening CCV and the injection of
either a PEM or CSS as closing CCV exceeds 14 hours, carefully evaluate instrument stability
during the entire sequence to decide whther 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).
13. If time elapse 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 whther 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).
14. If RT for each target analyte in PEM and CSS standards are within the RT windows, and %D for
the specified target analyte and %Breakdown in PEM are within the respective limits, and %D for
each target analyte in CCV CSS is within the limits, detects and non-detects should not be qualified.
15. No qualification of the data is necessary on surrogate %D alone. Use professional judgment to
evaluate the surrogate %D data in conjunction with surrogate recoveries to determine the need for
data qualification.
16. If instrument blank as part of CCV is not performed at the specified frequency and sequence or
instrument blank does not meet the concentration criteria, refer to Section V. Blanks for data
qualfications.
17. If the laboratory has failed to provide adequate calibration information, contact the Regional CLP
PO, who may contact the laboratory and request the necessary information. If the information is
not available, use professional judgment to assess the data.
18. Annotate the potential effects on the data due to CCV criteria exceedance in the Data Review
Narrative.
19. If CCV criteria are grossly exceeded, note this for laboratory CLP PO action.
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Table 53. CCV Actions for Pesticide Analysis
Criteria
CCV PEM and CSS not performed at correct
frequency and sequence
CCV PEM not performed at specified
concentration
CCV CSS not performed at the specified
concentration
RT outside the RT window
PEM %D outside the limits
PEM: 4,4'-DDT %Breakdown >20.0% and
4,4'-DDT is detected
PEM: 4,4'-DDT %Breakdown >20.0% and
4,4'-DDT is not detected
PEM: Endrin %Breakdown >20.0% and
Endrin is detected
PEM: Endrin %Breakdown >20.0% and
Endrin is not detected
PEM: Combined %Breakdown >30%
CSS %D outside the limits
Time elapse between opening CCV Pesticide
Instrument Blank and closing CCV PEM or
CSS exceeds 14 hr
Time elapse between opening CCV Pesticide
Instrument Blank and last sample or blank
exceeds 12 hr
RT, PEM %D, PEM %Breakdown, CSS %D,
time elapse within limits
Action
Detect
Contact CLP PO for
reanalysis or use
professional judgment
Contact CLP PO for
reanalysis or use
professional judgment
Contact CLP PO for
reanalysis or use
professional judgment
Use professional judgment
J
J for 4,4'-DDT, 4,4 '-ODD,
4,4'-DDE
R for 4,4'- DDT
J for Endrin,
Endrin aldehyde, Endrin
ketone
R for Endrin
Apply qualifiers as
described above considering
degree of individual
breakdown.
J
Use professional judgment
Use professional judgment
No qualification
Non-detect
Contact CLP PO for
reanalysis or use
professional judgment
Contact CLP PO for
reanalysis or use
professional judgment
Contact CLP PO for
reanalysis or use
professional judgment
Use professional judgment
UJ
No qualification
NJ for 4,4'-DDD and
4,4'-DDE
No qualification
NJ for aldehyde and Endrin
ketone
Apply qualifiers as
described above considering
degree of individual
breakdown.
UJ
Use professional judgment
Use professional judgment
No qualification
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V. Blanks
A. Review Items
Form 1A-OR, Form 4-OR, chromatograms, and quantitation 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. Criteria
The criteria for evaluation of blanks should apply to any blank associated with the samples (e.g.,
method blanks, instrument blanks, sulfur cleanup blank, field blanks, etc.). If problems with any blank
exist, all associated data must be carefully evaluated to determine whether or not there is an inherent
variability in the data or if the problem is an isolated occurrence not affecting other data.
1. Method blanks must be performed at the specified frequency and sequence. A method blank must
be extracted per matrix each time when samples are extracted. The number of samples extracted
with each method blank shall not exceed 20 field samples. The method blank must be extracted by
the same procedure used to extract samples and analyzed on each GC system under the same
conditions used to analyze associated samples.
2. The method blank, like any other sample in the SDG, must meet the technical acceptance criteria
for sample analysis.
3. An acceptable instrument blank must be analyzed at the beginning and ending of an analytical
sequence in which samples are analyzed, immediately prior to the analysis of the PEM or mid-point
INDA/INDB or INDC, used as CCV.
4. A sulfur cleanup blank must be analyzed whenever part of a set of the extracted samples requires
sulfur cleanup. If the entire set of samples associated with a method blank requires sulfur cleanup,
the method blank also serves the purpose of a sulfur cleanup blank and a separate sulfur cleanup
blank is not required.
5. TCLP/SPLP leachate extraction blank (LEB) must be prepared and analyzed at the specified
frequency and sequence.
6. The concentration of a target analyte in any blanks must not exceed its CRQL.
D. Evaluation
1. Verify that method blanks are extracted at the specified frequency and analyzed at the required
sequence. The Method Blank Summary (Form 4-OR) may be used to identify the samples
associated with each method blank.
2. Verify that applicable TCLP/SPLP LEBs are analyzed at the specified frequency and sequence.
The Method Blank Summary (Form 4-OR) may be used to identify the samples associated with
each TCLP/SPLP LEB.
3. Verify that instrument blanks are analyzed at the specified frequency and sequence.
4. Verify that the sulfur cleanup blank is analyzed when part of a set of samples extracted together
requires sulfur cleanup. The Method Blank Summary (Form 4-OR) may be used to identify the
samples associated with the sulfur cleanup blank.
5. Data concerning the field blanks are not evaluated as part of the CCS process. Evaluations on field
or trip blanks should be similar to the method blanks.
6. Review the results of all associated blanks on the forms and raw data (chromatograms and
quantitation reports) to evaluate the presence of target analytes in the blanks.
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NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the non-compliant blank can be obtained from the NFG
reports and may be used as part of the evaluation process.
E. Action
1. If the appropriate blanks are not extracted at the correct frequency and/or analyzed at the correct
sequence, use professional judgment to determine if the associated sample data should be qualified;
obtain additional information from the laboratory, if necessary. Record the situation in the Data
Review Narrative and note it for CLP PO action.
2. 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 Quality Assurance Project Plan (QAPP) or Regional Standard Operating Procedure (SOP).
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 having the highest concentration of a
contaminant.. Do not correct the results by subtracting any blank value.
3. For any blank (including method blank), if a target analyte is detected, but it is not detected in the
sample, non-detects should not be qualified.
4. For any method blank reported with results < CRQLs, report sample results that are < CRQLs at the
CRQLs and qualify as non-detect (U). For any method blank reported with results that are <
CRQLs, use professional judgment to qualify sample results that are > CRQLs. Positive results in
samples, especially those near but above the CRQL, may be biased high by low level
contamination in the method blank, and should be considered as estimated (J+).
5. For any method blank reported with results > CRQLs, report sample results that are < CRQLs at the
CRQLs and qualify as non-detect (U). For any sample reported with results > CRQLs but < Blank
Results, report sample results and qualify as non-detect (U) or unusable (R). Use professional
judgment to qualify sample results that > CRQLs and > Blank Results.
6. For TCLP/SPLP LEBs, sulfur cleanup blank, instrument blanks, and field blanks, sample result
qualifications listed in Table 54 should apply if supported by the project QAPP.
7. If gross contamination exists with blank results that are > ICAL CSS concentrations, qualify detects
as unusable (R). If the contamination is suspected of having an effect on the sample results, note it
for CLP PO action.
8. 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.
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Table 54. Blank and TCLP/SPLP LEB Actions for Pesticide Analysis
Blank Type
Method,
TCLP/SPLP LEB,
Sulfur cleanup,
Instrument, Field
Blank Result
Detects
CRQL
Gross
contamination
Sample Result
Nondetect
CRQL
CRQL but < Blank Result
> CRQL and > Blank Result
Detects
Action
No qualification
Report at CRQL and qualify
as non-detect (U)
Use professional judgment
Report at CRQL and qualify
as non-detect (U)
Report at sample results and
qualify as non-detect (U) or
as unusable (R)
Use professional judgment
Report at sample results and
qualify as unusable (R)
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VI. Surrogate
A. Review Items
Form 2C-OR, Form 8B-OR, chromatograms, and data system printouts.
B. Objective
The objective is to evaluate surrogate percent recovery (%R) to ensure that the analytical method is
efficient.
C. Criteria
1. Surrogate spiking solution containing two surrogates, TCX and DCB, is added to all samples,
including Matrix Spike (MS)/Matrix Spike Duplicates (MSDs), Laboratory Control Samples
(LCSs), and blanks to measure the surrogate recovery. The surrogates are also added to all the
standards to monitor RTs.
2. The RTs of the surrogates in each PEM, mid-point Individual Standard Mixtures A and B or
Individual Standard Mixture C used for CCV, all samples (including MS and MSB, LCS), and all
blanks must be within the calculated RT Windows. TCX must be within ±0.05 minutes, and DCB
must be within ±0.10 minutes of the RTs determined from the ICAL.
3. %R for the surrogates TCX and DCB in all samples including MS and MSDs, LCSs and all blanks
must be calculated accordingly.
4. %R for each surrogate must be in the inclusive range of 30-150% for all samples, including MS and
MSDs, LCSs and all blanks.
D. Evaluation
1. Check raw data (e.g., chromatograms and data system printouts) to verify that the surrogates are
added at the specified concentrations to all samples and blanks.
2. Check the raw data (e.g., chromatograms and data system printouts) to verify that the surrogate RTs
on Form 8B-OR are within the RT windows.
3. Check the raw data (e.g., chromatograms and data system printouts) to verify that the surrogate %R
for each sample and blank is on Form 2C-OR.
4. Check for any calculation or transcription errors. Verify that the surrogate recoveries are calculated
correctly using the equation in the method.
5. Whenever there are two or more analyses for a particular sample, use professional judgment to
determine which analyses is the most accurate data to report. Considerations include, but are not
limited to:
a. Surrogate recovery (marginal versus gross deviation).
b. Technical holding times.
c. Comparison of the values of the target compounds reported in each sample analysis.
d. Other QC information, such as surrogate recoveries and/or RTs in blanks and standards.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the non-compliant surrogate recovery can be obtained
from the NFG reports and may be used as part of the evaluation process.
E. Action
1. If surrogates are not added to any sample or blank, or surrogate concentration is incorrect in sample
or blank, use professional judgment to qualify detects and non-detects. Contact the Regional CLP
PO to arrange for reanalysis, if possible.
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2. If surrogate RTs in PEMs, Individual Standard Mixtures, samples, and blanks are outside of the RT
Windows, use professional judgment to qualify detects and non-detects. It may be necessary to
have the laboratory resubmit the data after making corrections.
3. If surrogate RTs are within RT windows, detects and non-detects should not be qualified.
4. If errors are detected in the calculations of %R, perform a more comprehensive recalculation.
5. If %R for any surrogate is outside the acceptance limits, consider the existence of coelution and
interference in the raw data. Use professional judgment to qualify data as surrogate recovery
problems may not directly apply to target analytes.
6. If %R for any surrogate in undiluted sample is < 10%, qualify detects as estimated low (J-) and
non-detects as unusable (R).
7. If %R for any surrogate in diluted sample is < 10%, use professional judgment to qualify detects
and non-detects.
8. If %R for any surrogate is > 10%, and < 30%, qualify detects as estimated low (J-) and non-detects
as estimated (UJ).
9. If %R for both surrogates are > 30%, and < 150%, detects and non-detects should not be qualified.
10. If %R for any surrogate is > 150% but < 200%, qualify detects as estimated high (J+). Non-detects
should not be qualified.
11. If %R for any surrogate is > 200%, qualify detects as estimated high (J+). Use professional
judgment to qualify non-detects.
12. In the special case of a blank analysis with surrogate %R outside the acceptance limits, give special
consideration to qualify 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.
For example, 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. Note analytical problems for laboratory CLP PO action even if this judgment allows
some use of the affected data.
Table 55. Surrogate Actions for Pesticide Analysis
Criteria
RT out of RT window
RT within RT window
%R < 10% (undiluted sample)
%R < 10% (diluted sample)
10%<%R<30%
30%<%R<150%
150%<%R<200%
%R > 200%
Action*
Detect
Use professional judgment
No qualification
J-
Use professional judgment
J-
No qualification
J+
J+
Non-detect
Use professional judgment
No qualification
R
Use professional judgment
UJ
No qualification
No qualification
Use professional judgment
* Use professional judgment in qualifying data, as surrogate recovery problems may not directly
apply to target analytes.
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VII. Matrix Spike/Matrix Spike Duplicate
A. Review Items
Cover Page, Form 3A-OR, chromatograms, and quantitation reports.
B. Objective
The objective of MS/MSD analysis is to evaluate the effect of each sample matrix on the sample
preparation procedures and the measurement methodology.
C. Criteria
1. MS/MSD samples shall be prepared and analyzed at specified frequency. One pair of MS/MSD
shall be analyzed per matrix or per SDG.
2. Samples identified as field blanks or Performance Evaluation (PE) samples cannot be used for
MS/MSD sample analysis.
3. MS/MSD %R and the Relative Percent Difference (RPD) between MS and MSD results shall be
calculated according to the method.
4. MS/MSD %R and RPD shall be within the acceptance limits in Table 56.
D. Evaluation
1. Verify that requested MS/MSD samples are analyzed at the required frequency.
2. Verify that a field blank or PE sample is not used for MS/MSD analysis.
3. Verify that the recalculated MS/MSD %R and RPD values agree with the laboratory reported
values on Form 3A-OR.
4. Check MS/MSD %R and RPD on Form 3A-OR and verify that they are within the limits in Table
56.
NOTE: For data obtained from the CLP, the preceding criteria, including the required MS/MSD
spiking analytes and spiking levels specified in Table 7 of the Statement of Work (SOW),
are evaluated as part of the CCS process. Information regarding the non-compliant
MS/MSD %R or RPD can be obtained from the NFG reports and may be used as part of the
evaluation process.
E. Action
1. If requested MS/MSD samples are not analyzed at the specified frequency, or were spiked with the
wrong analytes or at the wrong concentrations, use professional judgment to determine the impact
on sample data, if any; obtain additional information from the laboratory, if necessary. Record the
situation in the Data Review Narrative and note it for CLP PO action. It is not likely that data
qualification will be warranted if the frequency criteria is not met. Carefully consider all factors,
known and unknown, about method performance on the matrix at hand, in lieu of MS/MSD data.
2. If a field blank or PE sample is used for the MS/MSD analysis, note this for CLP PO action. All of
the other QC data must then be carefully checked. Use professional judgment when evaluating the
data.
3. If errors are detected in the calculations of MS/MSD %R or RPD, perform a more comprehensive
recalculation.
4. If the MS/MSD %R or RPD is outside the acceptance limits in Table 57, qualify detects and
non-detects in the original sample to include the consideration of the existence of interference in the
raw data. Considerations include, but are not limited to:
a. If MS/MSD %R is < 20%, qualify detects as estimated (J) and non-detects as unusable (R).
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b. If MS/MSD %R is > 20% and < the lower acceptance limit, qualify detects as estimated (J) and
non-detects as estimated (UJ).
c. If MS/MSD %R or RPD is > lower acceptance limit and < upper acceptance limit, detects and
non-detects should not be qualified.
d. If MS/MSD%R or RPD is > the upper acceptance limit, qualify detects as estimated (J).
Non-detects should not be qualified.
Table 56. MS/MSD %R and RPD Limits for Pesticide Analysis
Analyte
gamma-BHC (Lindane)
Heptachlor
Aldrin
Dieldrin
Endrin
4,4'-DDT
%R for
Water
Sample
56 - 123
40-131
40 - 120
52 - 126
56-121
38-127
RPD for
Water
Sample
0-15
0-20
0-22
0-18
0-21
0-27
%R for Soil
Sample
46 - 127
35-130
34-132
31-134
42 - 139
23 - 134
RPD for Soil
Sample
0-50
0-31
0-43
0-38
0-45
0-50
Table 57. MS/MSD Actions for Pesticide Analysis
Criteria
%R < 20%
20% < %R < Lower Acceptance Limit
Lower Acceptance Limit < %R;
RPD < Upper Acceptance Limit
%R or RPD > Upper Acceptance
Limit
Action
Detect
J
J
No qualification
J
Non-detect
R
UJ
No qualification
No qualification
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VIII. Laboratory Control Sample
A. Review Items
Form 3B-OR, chromatograms, and data system printouts.
B. Objective
The objective is to evaluate the accuracy of the analytical method and laboratory performance.
C. Criteria
1. An LCS must be prepared and analyzed at the specified frequency. LCS should be extracted and
analyzed per matrix or per SDG. LCS should be extracted using the same procedures as the
samples and method blank.
2. The requirements below apply independently to each GC column and to all instruments used for
these analyses. Quantitation must be performed on each GC column.
3. The LCS must contain the target analytes in Table 58 and the surrogates at the specified
concentrations in the method (Table 7 in the SOW).
4. %R for each spiked analyte in LCS must be calculated according to the method.
5. %R for each spiked analyte must be within the acceptance limits in Table 58.
Table 58. LCS %R Limits for Pesticide Analysis
Analyte
gamma-BHC
Heptachlor epoxide
Dieldrin
4,4'-DDE
Endrin
Endosulfan sulfate
trans -Chlordane
%R
50
50
30
50
50
50
30
Limits
-120
-150
-130
-150
-120
-120
-130
NOTE:
The %R limits for any spiked analyte in the LCS may be expanded at any time during the
period of performance if the United States Environmental Protection Agency (EPA)
determines that the limits are too restrictive.
6. All samples prepared and analyzed with an LCS that does not meet the technical acceptance criteria
in the method will require re-extraction and reanalysis.
D. Evaluation
1. Verify that LCS is prepared and analyzed at the specified frequency.
2. Check the raw data (e.g., chromatograms and data system printouts) to verify that the LCS is spiked
with the specified target analytes at the method specified concentrations (Table 7 in the SOW).
3. Check the raw data (e.g., chromatograms and data system printouts) to verify that %R of each
target analyte in LCS is calculated correctly and that the recalculated %R values agree with that
reported on Form 3B-OR.
4. Verify that %R of each target analyte in LCS is within the specified acceptance limits.
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NOTE:
E. Action
For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the non-compliant LCS %R can be obtained from the NFG
reports and may be used as part of the evaluation process.
1. If LCS is not performed at the specified frequency, use professional judgment to qualify detects and
non-detects in the associated samples.
NOTE: If an LCS sample is not analyzed at the specified frequency, use professional judgment to
determine the impact on sample data; obtain additional information from the laboratory, if
necessary. Record the situation in the Data Review Narrative and note it for CLP PO
action. It is not likely that data qualification will be warranted if the frequency requirement
is not met. Carefully consider all factors, known and unknown, about method
performance, in lieu of LCS data.
2. If LCS is not performed at the specified concentration, use professional judgment to qualify detects
and non-detects in the associated samples.
3. If errors are detected in the calculations of LCS %R, perform a more comprehensive recalculation.
4. If the LCS %R criteria are not met, qualify the specific target analyte in the associated samples.
a. If the LCS %R is < the lower acceptance limit, qualify detects as estimated low (J-) and
non-detects as unusable (R).
b. If the LCS %R is > lower acceptance limit and < upper acceptance limit, detects and
non-detects should not be qualified.
c. If the LCS %R is > the upper acceptance limit, qualify detects as estimated high (J+).
Non-detects should not be qualified.
d. Use professional judgment to qualify analytes other than those included in the LCS.
e. Take into account the analyte class, analyte recovery efficiency, analytical problems associated
with each analyte, and comparability in the performance of the LCS analyte to the non-LCS
analyte.
Table 59. LCS Actions for Pesticide Analysis
Criteria
LCS not performed at the specified frequency or
concentration
%R < Lower Acceptance Limit
Lower Acceptance Limit < %R < Upper
Acceptance Limit
%R > Upper Acceptance Limit
Action
Detect
Use professional
judgment
J-
No qualification
J+
Non-Detect
Use professional
judgment
R
No qualification
No qualification
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IX. Florisil Cartridge Performance Check
A. Review Items
Form 9A-OR, Florisil raw data, chromatograms, and data system printouts.
B. Objective
The objective is to evaluate the performance of the Florisil cartridge used for Florisil cleanup procedure
on sample extracts.
C. Criteria
1. The performance of each lot of Florisil cartridges used for sample cleanup must be evaluated at
least once, or every six months (whichever is most frequent).
2. The Florisil cartridge performance check standard solution must contain 2,4,5-trichlorophenol and
the mid-point concentration of INDA or INDC as specified in the method.
3. %R for each target analyte and surrogate in INDA must be calculated according to the method.
4. The %R limits the target analytes and surrogates in the INDA are 80-120%, and < 5% for
2,4,5-trichlorophenol. If INDC is used, %R limits for target analytes and surrogates in INDC shall
be evaluated.
D. Evaluation
1. Verify that Florisil cartridge performance check is performed at the specified frequency.
2. Check raw data for the Florisil cartridge performance check analysis to verify that the
concentrations of analytes are correct.
3. Check the raw data for the Florisil cartridge performance check results and verify that %R for each
analyte and surrogate are calculated correctly and agree with that on Form 9A-OR. Verify that
there are no transcription errors.
4. Verify that %R for the target analytes and surrogates in the performance check solution are within
80-120%, and the recovery of 2,4,5-trichlorophenol is < 5%.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the non-compliant %Rin Florisil cartridge performance
check can be obtained from the NFG reports and may be used as part of the evaluation
process.
E. Action
1. If Florisil Cartridge Performance Check is not performed at the specified frequency, use
professional judgment to qualify detects and non-detects.
2. If Florisil Cartridge Performance Check 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 %R in the Florisil Cartridge Performance Check,
perform a more comprehensive recalculation.
4. If the Florisil Cartridge Performance Check criteria are not met, examine the raw data for the
presence of polar interferences and use professional judgment in qualifying the data as follows:
a. If %R is < 10% for any of target analyte in the Florisil Cartridge Performance Check, use
professional judgment to qualify detects. Qualify non-detects as unusable (R).
b. If %R is > 10% and < 80% for any target analyte in the Florisil Cartridge Performance Check,
qualify detects as estimated (J) and non-detects as estimated (UJ).
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c. If %R is > 80% and < 120% for all target analytes in the Florisil Cartridge Performance Check,
detects and non-detects should not be qualified.
d. If %R is > 120% for any target analyte in the Florisil Cartridge Performance Check, use
professional judgment to qualify detects. Non-detects should not be qualified.
e. If %R of 2,4,5-trichlorophenol in the Florisil Cartridge Performance Check is > 5%, use
professional judgment to qualify detects and non-detects, considering interference on the
sample chromatogram.
Annotate potential effects on the sample data resulting from the Florisil Cartridge Performance
Check analysis not yielding acceptable results in the Data Review Narrative.
Table 60. Florisil Cartridge Performance Check Actions
Criteria
Florisil Cartridge Performance Check not
performed at specified frequency or
concentration
%R < 10% (target analytes)
10% < %R < 80% (target analytes)
80% < %R < 120% (target analytes)
%R > 120% (target analytes)
%R > 5% (2,4,5-trichlorophenol)
Action
Detect
Use professional
judgment
Use professional
judgment
J
No qualification
Use professional
judgment
Use professional
judgment
Non-Detect
Use professional
judgment
R
UJ
No qualification
No qualification
Use professional
judgment
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X. Gel Permeation Chromatography Performance Check
A. Review Items
Form 9B-OR, two ultraviolet (UV) traces, Gel Permeation Chromatography (GPC) raw data,
chromatograms, and data system printouts.
B. Objective
The objective is to evaluate GPC cleanup efficiency.
C. Criteria
1. GPC is used for the cleanup of all non-aqueous sample extracts and for aqueous sample extracts
that contain high molecular weight components that interfere with the analysis of the target
analytes.
2. Each GPC system must be calibrated prior to processing samples for GPC cleanup or when the
GPC CCV solution fails to meet criteria or when the column is changed or channeling occurs, and
once every 7 days when in use.
3. The GPC calibration is acceptable if the two UV traces meet the following requirements:
a. Peaks must be observed and symmetrical for all compounds in the calibration solution.
b. Corn oil and the phthalate peaks exhibit > 85% resolution.
c. The phthalate and methoxychlor peaks exhibit > 85% resolution.
d. Methoxychlor and perylene peaks exhibit > 85% resolution.
e. Perylene and sulfur peaks must not be saturated and should exhibit > 90% baseline resolution.
f. The RT shift is < 5% between UV traces for Bis(2-ethylhexyl) phthalate and perylene.
4. A GPC blank must be analyzed after each GPC calibration. The concentration for any target
analyte in the GPC blank must not exceed the CRQL.
5. GPC calibration verification must be performed at least once every 7 days (immediately following
the GPC Calibration) whenever samples (including MS/MSDs, LCS, and blanks) are cleaned up
using the GPC.
6. The GPC calibration verification solution must contain the target analytes gamma-BHC (Lindane),
Heptachlor, Aldrin, 4,4'-DDT, Endrin, and Dieldrin in Methylene Chloride at the concentrations
specified in the method (Table 7 in SOW).
7. %R for each target analyte in the GPC calibration verification must be calculated according to the
method.
8. %R for each target analyte in the GPC calibration verification must be in the inclusive range of
80-120%.
D. Evaluation
1. Verify that the GPC calibration is performed at the specified frequency.
2. Verify that there are two UV traces present and that the RT shift for Bis(2-ethylhexyl) phthalate and
perylene is < 5%.
3. Verify that the pesticide target analytes in the GPC calibration standard are present and the peaks
are symmetrical in both UV traces meeting the minimum resolution requirements.
4. Verify that no target analyte in the GPC blank exceeds the CRQL.
5. Verify that the GPC calibration verification is performed at the specified frequency and
concentrations.
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6. Verify that %R for target analytes are calculated correctly and %R values agree with that on Form
9B-OR.
7. Verify that %R for target analytes are within the acceptance limits.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the non-compliant %R in the GPC calibration verification
can be obtained from the NFG reports and may be used as part of the evaluation process.
E. Action
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 sample data for
unusual peaks; and use professional judgment to qualify the data. If the laboratory chooses to
analyze samples under unacceptable GPC criteria, notify the CLP PO.
a. If the RT shift of Bis(2-ethylhexyl) phthalate and perylene is > 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. Contact the CLP PO to arrange for sample re-analysis.
2. If GPC calibration verification is not performed at the specified frequency, use professional
judgment to qualify detects and non-detects.
3. If GPC calibration verification is not performed at the specified concentrations, use professional
judgment to qualify detects and non-detects.
4. If errors are detected in the calculations of %R in the GPC calibration verification, perform a more
comprehensive recalculation.
5. If GPC calibration verification criteria are not met, examine the raw data and qualify data as
follows:
a. If %R is < 10% for any target analytes and surrogates in the GPC calibration verification, use
professional judgment to qualify detects. Qualify non-detects as unusable (R).
b. If %R is > 10% and < 80% for any target analytes and surrogates in the GPC calibration
verification, qualify detects as estimated (J) and non-detects as estimated (UJ).
c. If %R is > 80% and < 120% for all target analytes and surrogates in the GPC calibration
verification, detects and non-detects should not be qualified.
d. If %R is > 120% for any target analytes and surrogates surrogates in the GPC calibration
verification, use professional judgment to qualify detects. Non-detects should not be qualified.
6. Annotate potential effects on the sample data resulting from the GPC cleanup analyses not yielding
acceptable results in the Data Review Narrative.
Table 61. GPC Performance Check Actions for Pesticide Analysis
Criteria
GPC Performance Check not
performed at the specified frequency
or concentration
%R < 10% (target analytes)
10% < %R < 80% (target analytes)
80% < %R < 120% (target analytes)
%R > 120% (target analytes)
Action
Detect
Use professional judgment
Use professional judgment
J
Non-Detect
Use professional judgment
R
UJ
No qualification
Use professional judgment
No qualification
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XI. Target Analyte Identification
A. Review Items
Form 1A-OR, Form 10A-OR, Form 10B-OR, chromatograms, and data system printouts.
B. Objective
The objective is to provide acceptable GC/ECD qualitative analysis to minimize the number of
erroneous analyte identifications.
C. Criteria
1. The RTs of both of the surrogates and reported target analytes in each sample must be within the
calculated RT Windows on both columns. TCX must be within ±0.05 minutes of the RT
determined from the ICAL, and DCB must be within ±0.10 minutes of the RT determined from the
ICAL.
2. For detected single component target analytes and Toxaphene, %D between the concentrations on
two GC columns must be calculated according to the method. The %D for any detected target
analyte should be < 25.0% to have high confidence in the identification.
3. When no analytes are identified in a sample, the chromatograms from the analyses of the sample
extract must use the same scaling factor as was used for the low-point standard of the ICAL
associated with those analyses.
4. Chromatograms must display detected single component target analytes in the sample and the
largest peak of Toxaphene detected in the sample at less than full scale.
5. If an extract must be diluted, chromatograms must display single component target analyte peaks
between 10-100% of full scale, and the chosen five Toxaphene peaks between 25-100% of full
scale.
6. For any sample, the baseline of the chromatogram must return to below 50% of full scale before the
elution time of alpha-BHC, and also return to below 25% of full scale after the elution time of
alpha-BHC and before the elution time of DCB.
7. If a chromatogram is replotted electronically to meet these requirements, the scaling factor used
must be displayed on the chromatogram, and both the initial chromatogram and the replotted
chromatogram must be submitted in the data package.
D. Evaluation
1. Review Form 1A-OR, the associated raw data (chromatograms and data system printouts) and
Form lOA-ORand Form 10B-OR.
a. Verify that the reported target analytes as detects are identified correctly by comparing the
sample chromatograms to the tabulated results and verifying peak measurements and RTs.
b. Verify that non-detects by a review of the sample chromatograms.
c. Check the associated blank data for potential interferences (to evaluate sample data for false
positives) and check the calibration data for adequate RT Windows (to evaluate sample data for
false positives and false negatives).
d. For Toxaphene, compare the RTs and relative peak height ratios of the five major peaks in the
appropriate standard chromatograms.
e. Compare the Toxaphene peaks identified in the sample to determine that the RTs do not
overlap with the RTs of any other target analytes or with chromatographic interferences from
the sample matrix.
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2. Verify that the %D results were calculated correctly and that the recalculated %D agrees with that
reported on Forms lOA-ORor 10B-OR, as appropriate.
3. Verify that the %D for any target analyte is < 25.0%. If target %D is > 25.0% for any target analyte,
evaluate the impact of the presence of an interfering compound, and whether the interference
precludes confirmation of the target analyte. Also, evaluate the possibility of poor precision or
non-homogeniety as causes for the difference.
E. Action
1. If the qualitative criteria for both columns are not met, all target analytes that are reported as detects
should be qualified as non-detect (U). Use professional judgment to assign an appropriate
quantitation limit using the following guidance:
a. If the detected target analyte peak is sufficiently outside the RT window determined from the
associated ICAL, the reported values may be a false positive and should be replaced with the
sample CRQL value.
b. If the detected target analyte peak poses an interference with potential detection of another
target peak, the reported value should be considered and qualified as unusable (R).
2. If a peak is identified in both GC column analyses that falls within the appropriate RT windows, but
the analyte is reported as a non-detect, the analyte may be a false negative. Use professional
judgment to decide if the analyte should be included and reported as detect. Annotate all
conclusions made regarding target analyte identification in the Data Review Narrative.
3. If the Toxaphene peak RT windows determined from the calibration overlap with single component
target analytes or chromatographic interferences, use professional judgment to qualify the data.
4. If Toxaphene exhibits a marginal pattern-matching quality, use professional judgment to determine
if the differences are due to environmental "weathering" (i.e., degradation of the earlier eluting
peaks relative to the later eluting peaks). If the presence of Toxaphene is strongly suggested, report
results as presumptively present with estimated concentration (NJ).
5. If errors are detected in the calculations of %D for any target analyte, perform a more
comprehensive recalculation.
6. If an interfering compound is indicated, consider the potential for co-elution and use professional
judgment to determine how best to report. It is recommended to either report the analyte as positive
at the lower value, qualified as tentative (N), or as non-detect (U) at CRQL.
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XII. Gas Chromatograph/Mass Spectrometer Confirmation
A. Review Items
Form 1A-OR, Form 10A-OR, Form 10B-OR, chromatograms, and data system printouts.
B. Objective
The objective is to ensure the accuracy of the positive identification of a target analyte.
C. Criteria
1. Gas Chromatography/Mass Spectrometer (GC/MS) confirmation is required when a positively
identified target analyte has on-column concentration meeting the specified criterion on both GC
columns. For single component target analyte, GC/MS shall be performed for analyte
concentration > 5.0 ng/(iL. For Toxaphene, GC/MS shall be performed for at least one peak
concentration > 125 ng/(iL.
2. GC/MS confirmation may be accomplished by one of three general means:
a. Examination of the semivolatile GC/MS library search results [i.e., Tentatively Identified
Compound (TIC) data];
b. A second analysis of the semivolatile extract; or
c. Analysis of the pesticide extract, following any solvent exchange and concentration steps that
may be necessary.
D. Evaluation
1. Review Form 1A-OR, the associated raw data (chromatograms and data system printouts) and
Form 10A-OR and Form 10B-OR
2. Check quantitation report to verify that GC/MS confirmation is required by ensuring that the
on-column concentration criteria are met (criteria indicated in Section C.I).
3. Verify that GC/MS confirmation is completed as specified in the method.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding non-compliant GC/MS can be obtained from the CCS
report and may be used as part of the evaluation process.
E. Action
1. If an analyte was confirmed by GC/MS, qualify as confirmed (C).
2. If a sufficient quantity of an analyte was indicated and GC/MS confirmation was attempted but was
not confirmed, qualify as (X) or non-detect (U). Explain in the Data Review Narrative that the
analyte should be considered non-detect because it could not be confirmed.
Table 62. GC/MS Confirmation Actions
Criteria
Analyte confirmed by GC/MS
Analyte indicated by not confirmed by GC/MS
Action for Detects
C
XorU
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XIII. Target Analyte Quantitation and Reported Contract Required Quantitation Limit
A. Review Items
Form 1A-OR, sample preparation sheets, SDG Narrative, quantitation reports, and chromatograms.
B. Objective
The objective is to ensure that the reported results and CRQLs for target analytes are accurate.
C. Criteria
1. Target analyte results, as well as the sample specific CRQLs, must be calculated according to the
correct equations.
2. Target analyte CF must be calculated using the correct associated ICAL. Target analyte result must
be calculated using the CF from the associated ICAL.
D. Evaluation
1. Verify that the results for all positively identified analytes are calculated and reported by the
laboratory.
2. Verify that the CRQLs are calculated for the non-detects and reported accordingly.
3. Verify that the correct CF is used to calculate the reported results.
4. Verify that the same CF is used consistently for all sample result calculations.
5. Verify that the sample-specific CRQLs have been calculated and adjusted to reflect Percent Solids
(%Solids) and sample dilutions.
a. For soil/sediment samples that are high in moisture (i.e., < 30% solid), evaluation of the
presence of each analyte depends on the anticipated interaction between the analyte and the
total matrix, as well as how the sample was processed.
b. If the phases of a sample were separated and processed separately, no particular qualification
on the grounds of matrix distribution is warranted.
c. If a soil/sediment sample was processed by eliminating most of the water, analytes that are
highly water soluble under ambient conditions may be severely impacted such that their
presence cannot be completely evaluated.
6. Verify that recalculated results and CRQLs agree with that reported by the laboratory.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the non-compliant results or CRQLs can be obtained from
the CCS report and may be used as part of the evaluation process.
E. Action
1. If any discrepancies are found, contact the Regional CLP PO, who may contact the laboratory to
obtain additional information that could resolve any differences. If a discrepancy remains
unresolved, use professional judgment to decide which value is the most accurate. Under these
circumstances, use professional judgment to determine that qualification of data is warranted.
Annotate the reasons for any data qualification in the Data Review Narrative.
2. If errors are detected in results and CRQL calculations, perform a more comprehensive
recalculation.
3. If %Solids for a soil sample is < 10.0%, use professional judgment to qualify detects and
non-detects.
4. If %Solids for a soil sample is > 10.0% and < 30.0%, use professional judgment to qualify detects
and non-detects.
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5. If %Solids for a soil sample is > 30.0%, detects and non-detects should not be qualified.
6. If sample results are < CRQLs and > MDLs, qualify as estimated (J).
7. Note numerous or significant failures to accurately quantify the target analytes, or to properly
evaluate and adjust CRQLs, for laboratory CLP PO action.
Table 63. Percent Solids Actions for Pesticide Analysis for Non-Aqueous Samples
Criteria
%Solids< 10.0%
10.0% < %Solids < 30.0%
%Solids > 30.0%
Action
Detect
Use professional judgment
Use professional judgment
No qualification
Non- detect
Use professional judgment
Use professional judgment
No qualification
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XIV. Regional Quality Assurance and Quality Control
A. Review Items
Form 1A, chromatograms, TR/COC documentation, quantitation reports, and other raw data from
Quality Assurance/Quality Control (QA/QC) samples.
B. Objective
The objective is to use results from the analysis of the Regional QA/QC samples including field
duplicates, PE samples, blind spikes, and blind blanks to determine the validity of the analytical results.
C. Criteria
Criteria are determined by each Region.
1. PE sample frequency may vary.
2. The target analytes present in the PE sample must be correctly identified and quantified.
3. The RPD between field duplicates shall fall with the specific limits in the Region's SOP or project
QAPP.
D. Evaluation
1. Evaluation procedures must follow the Region's SOP for data review. Each Region will handle the
evaluation of PE samples on an individual basis.
2. Verify that the target analyte in PE sample is properly identified and that the result is calculated
correctly.
3. Verify that the acceptance criteria for the specific PE sample are met, if available.
4. Calculate the RPD between field duplicates and provide this information in the Data Review
Narrative. Also verify that the value falls within the specific limits in the Region's SOP or project
QAPP.
E. Action
1. Any action must be in accordance with Regional specifications and the criteria for acceptable PE or
field duplicate sample results.
2. Note unacceptable results for PE or field duplicate samples for CLP PO action.
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XV. Overall Assessment of Data
A. Review Items
Entire data package, data review results, and (if available), the QAPP and Sampling and Analysis Plan
(SAP).
B. Objective
The objective is to provide the overall assessment on data quality and usability.
C. Criteria
1. Review all available materials to assess the overall quality of the data, keeping in mind the additive
nature of analytical problems.
2. Reported analyte concentrations must be quantitated according to the appropriate analytical
method, as listed in the method. All sample results must be within the linear calibration ranges per
methods.
D. Evaluation
Examine the raw data to verify that the correct calculation of the sample results was reported by the
laboratory. Analysis logs, instrument printouts, etc., should be compared to the reported sample results
recorded on the appropriate Organic Summary Forms (Form 1A-OR through Form 10B-OR).
1. Evaluate any technical problems which have not been previously addressed.
2. Examine the raw data for any anomalies (e.g, baseline shift).
3. Verify appropriate method is used in sample analysis.
4. Verify that there are no transcription or reduction errors.
5. Verify that target analyte results fall within the calibrated ranges.
6. If appropriate information is available, use professional judgment to assess the usability of the data
to to assist the data user in avoiding inappropriate use of the data. Review all available information,
including the QAPP (specifically the acceptance and performance criteria), SAP, and
communication with the data user that concerns the intended use and desired quality of these data.
E. Action
1. Use professional judgment to determine if there is any need to qualify data which were not
qualified based on the QC criteria previously discussed.
2. Use professional judgment to qualify sample results and non-detects if the MDL exceeds CRQL.
3. If a sample is not diluted properly when sample results exceed the upper limit of the calibration
range, qualify sample results as estimated (J).
4. Write a brief Data Review Narrative to give the user an indication of the limitations of the
analytical data.
5. Note any inconsistency of the data with the SDG Narrative for CLP PO action. If sufficient
information on the intended use and required quality of the data is available, include an assessment
of the usability of the data within the given context. This may be used as part of a formal Data
Quality Assessment (DQA).
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AROCLOR DATA REVIEW
The Aroclor organic data requirements to be reviewed during validation are listed below:
I. Preservation and Holding Times 189
II. Initial Calibration 192
III. Continuing Calibration Verification 196
IV. Blanks 200
V. Surrogate 203
VI. Matrix Spike/Matrix Spike Duplicate 206
VII. Laboratory Control Sample 208
VIII. Gel Permeation Chromatography Performance Check 210
IX. Target Analyte Identification 212
X. Gas Chromatograph/Mass Spectrometer Confirmation 214
XI. Target Analyte Quantitation and Reported Contract Required Quantitation Limit 215
XII. Regional Quality Assurance and Quality Control 217
XIII. Overall Assessment of Data 218
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I. Preservation and Holding Times
A. Review Items
Form 1A-OR, Traffic Report/Chain of Custody (TR/COC) documentation, raw data, sample extraction
sheets, and the Sample Delivery Group (SDG) 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 sample condition and the
holding time of the sample.
C. Criteria
1. The extraction technical holding time is determined from the date of sample collection to the date
of sample extraction. The analysis technical holding time is determined from the date of sample
extraction completion to the date of sample analysis.
2. Samples shall be in proper condition with shipping container temperatures at < 6°C upon receipt at
the laboratory. All aqueous and non-aqueous samples shall be protected from light and refrigerated
at < 6°C (but not frozen) from the time of receipt at the laboratory. The sample extracts shall be
stored at < 6°C (but not frozen) from the time of the extraction completion.
3. The extraction technical holding time criteria for aqueous samples that are not properly preserved is
7 days.
4. The extraction technical holding time criteria for non-aqueous samples that are not properly
preserved is 14 days.
5. The extraction technical holding time criteria for aqueous and soil samples that are properly
preserved is 1 year.
6. The analysis technical holding time criteria for sample extracts that are not properly preserved is 40
days.
7. The analysis technical holding time criteria for sample extracts that are properly preserved is 40
days.
D. Evaluation
1. Review the SDG Narrative and the TR/COC documentation to determine if the samples are
received intact and iced. If there is an indication of problems with the samples, the sample integrity
may be compromised.
2. Verify that the extraction dates and the analysis dates for samples on Form 1A-OR and the raw
data/SDG file are identical.
3. To determine the analysis technical holding times for samples, after the completion of extraction,
the dates of extraction are compared with the dates of analysis on Form 1A-OR.
E. Action
1. If samples are received with shipping container temperatures > 6°C, use professional judgment to
qualify detects and non-detects.
2. If discrepancies are found between the sample extraction date or analysis date and the date on raw
data, perform a more comprehensive review to determine the correct dates to be used for
establishing technical holding times.
3. If an aqueous sample is not properly cooled, but extraction is performed within the 7-day technical
holding time and the extract is analyzed within the 40-day technical holding time, use professional
judgment to qualify detects and non-detects.
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4. If an aqueous sample is not properly cooled, but extraction is performed outside the 7-day technical
holding time, and the extract is analyzed outside the 40-day technical holding time, detects should
be qualified as estimated (J). Use professional judgment to qualify non-detects.
5. If an aqueous sample is properly cooled and extraction is performed within the 1-year technical
holding time, and the extract is analyzed within the 40-day technical holding time, detects should
not be qualified.
6. If an aqueous sample is properly cooled, but extraction is performed outside the 1-year technical
holding time, and the extract is analyzed outside the 40-day technical holding time, qualify detects
as estimated (J) and non-detects as estimated (UJ).
7. If a non-aqueous sample is not properly cooled, but extraction is performed within the 14-day
technical holding time and the extract is analyzed within the 40-day technical holding time, use
professional judgment to qualify detects and non-detects.
8. If a non-aqueous sample is not properly cooled, but extraction is performed outside the 14-day
technical holding time and the extract is analyzed outside the 40-day technical holding time, detects
should be qualified as estimated (J). Use professional judgment to qualify non-detects.
9. If a non-aqueous sample is properly cooled, and extraction is performed within the 1 -year technical
holding time and the extract is analyzed within the 40 day technical holding time, detects and
non-detects should not be qualified.
10. If a non-aqueous sample is properly cooled, but extraction is performed outside the 1-year
technical holding time and the extract is analyzed outside the 40 day technical holding time, qualify
detects as estimated low (J) and non-detects as estimated (UJ).
11. If discrepancies are found between the sample extraction date or analysis date and the date on the
raw data, perform a more comprehensive review, contacting the laboratory if necessary through the
Regional Contract Laboratory Program Project Officer (CLP PO), to determine the correct dates
for establishing technical holding times.
12. Annotate the effect of exceeding the holding time on the resulting data in the Data Review
Narrative, whenever possible.
13. If technical holding times are grossly exceeded, qualify detects as estimated (J). Use professional
judgment to qualify non-detects as estimated (UJ) or unusable (R). Note it for CLP PO action. Use
caution in determining whether some detected analytes should be qualified as estimated low (J-) or
estimated high (J+), based on knowledge of individual analyte stability or interactions. Exceedance
of holding time limits may not indicate a low bias for all Aroclors.
14. If samples are received with shipping container temperatures > 10°C, use professional judgment to
qualify detects and non-detects.
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Table 64. Preservation and Holding Time Actions for Aroclor Analysis
Matrix
Aqueous
Non-aqueous
Preserved
No
No
Yes
Yes
Yes/No
No
No
Yes
Yes
Yes/No
Criteria
< 7 days (for extraction) and
< 40 days (for analysis)
> 7 days (for extraction) and
> 40 days (for analysis)
< 1 year (for extraction) and
< 40 days (for analysis)
> 1 year (for extraction) and
> 40 days (for analysis)
Holding time grossly
exceeded
< 14 days (for extraction)
and < 40 days (for analysis)
> 14 days (for extraction)
and > 40 days (for analysis)
< 1 year (for extraction) and
< 40 days (for analysis)
> 1 year (for extraction) and
> 40 days (for analysis)
Holding time grossly
exceeded
Action
Detect
Non-Detect
Use professional judgment
J
Use professional
judgment
No qualification
J
J
UJ
UJorR
Use professional judgment
J
Use professional
judgment
No qualification
J
J-
UJ
UJorR
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II. Initial Calibration
A. Review Items
Form 6D-OR, Form 6E-OR, Form 6F-OR, chromatograms, and data system printouts.
B. Objective
The objective of initial calibration (ICAL) is to ensure that the instrument is capable of producing
acceptable qualitative and quantitative data.
C. Criteria
1. A five-point ICAL is performed for Aroclor 1016/1260. Either single or five-point calibration shall
be performed for the other Arocloranalytes. Aroclors 1221, 1232, 1242, 1248, 1254, 1262 or 1268
are calibrated at the lowest concentration (CS1) for pattern recognition at the Contract Required
Quantitation Limit (CRQL). If Aroclors 1221, 1232, 1242, 1248, 1254, 1262 or 1268 are identified
in a sample with a single-point ICAL, a valid five-point ICAL is required for confirming the
identification and quantitation of the specific detected Aroclor analyte.
2. The ICAL must be performed following a specific sequence listed in Table 65. Single-point
Aroclor calibration may be made before or after the analysis of the five-point Aroclor calibration.
Each Aroclor standard shall be analyzed before the analysis of any sample or blank.
3. The concentrations for Aroclors in the five ICAL standards shall be at 100, 200, 400, 800, and 1600
ng/mL. The concentrations for surrogates in the five ICAL standards shall be at 5.0, 10, 20, 40 and
80 ng/mL for tetracholor-m-xylene (TCX), and 10, 20, 40, 80 and 160 ng/mL for
decachlorobiphenyl (DCB). The single-point ICAL standard for all Aroclors other than Aroclor
1016/1260 should be at 100 ng/mL.
4. The Mean Retention Times (RTs) of each of the five major peaks of Aroclors 1016 and 1260 and
the Retention Time (RT) of the surrogates are determined from the five-point ICAL. For Aroclor
1221, the RT of each of the three major peaks and the RT of the surrogates are determined from the
single-point standard ICAL standard. For the other six Aroclors, 1232, 1242, 1248, 1254, 1262 or
1268, the RT of each of the five major peaks and the RT of the surrogates are determined from the
single-point standard ICAL_If Aroclors 1221, 1232, 1242, 1248, 1254, 1262 or 1268, are
identified in a sample, the RTs of each of the five major peaks (three major peaks for Aroclor 1221)
and the RT of the surrogates are determined from the five-point ICAL.
5. An RT Window must be calculated as ±0.07 for each of the five major Aroclor peaks (three major
peaks for Aroclor 1221), and ±0.05 and ±0.10 for the surrogates TCX and DCB, respectively.
6. The chromatograms of the standards for the Aroclors analyzed during the ICAL sequence must
display the peaks chosen for identification of each analyte at greater than 25% of full scale, but less
than 100% of full scale.
7. Mean Calibration Factor (CF) must be calculated for the five major peaks for each Aroclor (three
major peaks for Aroclor 1221), as well as for the surrogates, in the 5-point ICAL.
8. The Percent Relative Standard Deviation (%RSD) of the Calibration Factors (CFs) for the five
major peaks of each of the Aroclor analytes must be < 20.0%. The %RSD of the CFs for the two
surrogates must be < 20.0%.
NOTE: Either peak area or peak height may be used to calculate the CFs that are, in turn, used to
calculate %RSD. However, the type of peak measurement used to calculate each CF for a
given compound must be consistent. For example, if peak area is used to calculate the CS 1
CF for a given peak of a certain Aroclor, the remaining CFs for the same peak in the
remaining standards (CS2-CS5) for that Aroclor must also be calculated using peak area.
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Table 65. Initial Calibration Sequence
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
Aroclor
Aroclor
Aroclor
Aroclor
Aroclor
Aroclor
Aroclor
Aroclor
Aroclor
Aroclor
Aroclor
Aroclor
1221 CS1
1232 CS1
1242CS1
1248 CS1
1254 CS1
1262 CS1
1268 CS1
1016/1260
1016/1260
1016/1260
1016/1260
1016/1260
(100
(200
(400
(800
ng/mL)
ng/mL)
ng/mL)
ng/mL)
CS1
CS2
CS3
CS4
(1600ng/mL)CS5
Instrument blank
D. Evaluation
1. Verify that ICAL is performed at the specified frequency and sequence. Verify that the proper
ICAL sequence is used and that either single-point calibration for Aroclors other than Aroclor
1016/1260 is included in the ICAL, or a 5-point calibration for a specific Aroclor is included.
2. Check the raw data (chromatograms and data system printouts) for each standard to verify that each
of the standards is analyzed at the specified concentrations for Aroclor analytes and surrogates.
3. Check the Aroclor Standards data and Form 6D-OR, Form 6E-OR, and Form 6F-OR to verify that
the RT Windows, CFs, CFs, and %RSDs are calculated correctly. Recalculate the CFs and %RSD
for one or more Aroclors and verify that the recalculated values agree with that reported by the
laboratory and there are no transcription errors.
4. Check the chromatograms and verify that at least one chromatogram from each of the Aroclor
Standards yields peaks registering recorder/printer deflections between 25-100% of full scale.
5. Verify that the %RSD for the CFs are within the acceptance limits.
NOTE: For data obtained from the Contract Laboratory Program (CLP), the preceding criteria are
evaluated as part of the Contract Compliance Screening (CCS) process. Information
regarding the non-compliant RT windows and %RSD can be obtained from the National
Functional Guidelines (NFG) reports and may be used as part of the evaluation process.
E. Action
1. If ICAL is not performed at the specified frequency and sequence, use professional judgment to
qualify detects and non-detects. Contact the Regional CLP PO to arrange for reanalysis, if possible,
or note it in the Data Review Narrative for later CLP PO action.
2. If the ICAL standards are not performed at the specified concentrations, use professional judgment
to qualify detects and non-detects. This is especially critical for the low-level standards and
non-detects.
3. If errors are detected in the calculations of RT Windows, CFs, CFs, or %RSDs, perform a more
comprehensive recalculation.
4. If the chromatogram display criteria are not met, use professional judgment to evaluate the effect
on the data.
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5. If the %RSD for any target analyte peak used for Aroclor analyte identification is outside the
acceptance limits, qualify detects as estimated (J) . Use professional judgment to qualify
non-detects.
6. If %RSD for all target analyte peaks used for Aroclor analyte identification are within the
acceptance limits, detects and non-detects should not be qualified.
7. Based on the project-specific Data Quality Objectives (DQOs), a more in-depth review may be
considered using the following guidelines:
a. If %RSD criteria of any target analytes are not met, and if %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.
b. If the high-point of the ICAL curve is outside of the %RSD criteria (e.g., due to saturation):
i. Qualify detects in the associated samples with analyte concentrations greater than the
high-point concentration as estimated (J).
ii. Detects in the associated samples with analyte concentrations within the calibration range
should not be qualified.
iii. Non-detects in the associated samples should not be qualified.
c. If the low-point of the ICAL curve is outside of the %RSD criteria:
i. Qualify detects in the associated samples with analyte concentrations in the non-linear
range as estimated (J).
ii. Detects in the associated samples with analyte concentrations within the calibration range
should not be qualified.
iii. 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.
8. If the laboratory failed to provide adequate calibration information, notify the Regional CLP PO,
who may contact the laboratory to request the necessary information. If the information is not
available, use professional judgment to assess the data.
9. Annotate the potential effects on the reported data due to exceeding the ICAL criteria in the Data
Review Narrative.
10. If the ICAL criteria are grossly exceeded, note this for laboratory CLP PO action.
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Table 66. Initial Calibration Action for Aroclor Analysis
Criteria
Initial calibration not performed or not
performed at specified frequency and
sequence
Initial calibration not performed at the
specified concentrations
RT Windows incorrect,
Or chromatogram criteria not met
%RSD outside acceptance limits
%RSD within acceptance limits
Action
Detect
Contact CLP PO for
reanalysis or
use professional judgment
Contact CLP PO for
reanalysis or
use professional judgment
Contact CLP PO for
reanalysis or
use professional judgment
J
No qualification
Non- detect
Contact CLP PO for
reanalysis or
use professional judgment
Contact CLP PO for
reanalysis or
use professional judgment
Contact CLP PO for
reanalysis or
use professional judgment
Use professional judgment
No qualification
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III. Continuing Calibration Verification
A. Review Items
Form 7D-OR, chromatograms, and data system printouts.
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. Criteria
1. A Continuing Calibration Verification (CCV) consisting of the analyses of instrument blanks, and
the mid-point concentration (CSS) of Aroclor standards must be performed at the beginning
(opening CCV) and end (closing CCV) of each 12-hour analytical sequence. The opening and
closing CCVs consist of an injection of an instrument blank followed by an injection of mid-point
ICAL standard CSS of Aroclor 1016/1260. If an Aroclor analyte other than 1016 or 1260 is
detected in any samples, a mid-point ICAL standard CSS of that specific Aroclor analyte must be
analyzed as part of the opening and closing CCV.
2. CCV CSS standards must contain all required target analytes and surrogates at the mid-point
standard concentration of the ICAL.
3. The RT for each Aroclor target analyte and surrogate in the CCV CSS standard must be within the
RT windows determined from the ICAL.
4. Percent Difference (%D) between the CF and CF from the associated ICAL for each of the five
major Aroclor target analyte peaks (three majorpeaks for Aroclor 1221) and surrogate in CCV CSS
must be calculated accordingly.
5. For the opening CCV, or closing CCV that is used as an opening CCV for the next 12-hour period,
the %D for each of the five peaks (three major peaks for Aroclor 1221) used to identify an Aroclor
and surrogates in CSS Aroclor standard must be in the inclusive range of ±25.0% and ±30.0%,
respectively.
6. For a closing CCV, %D for each of the five peaks (three major peaks for Aroclor 1221) used to
identify an Aroclor and surrogates in CSS Aroclor standard must be in the inclusive range of
±50.0%.
7. Instrument blanks paired with CSS standard must bracket the 12-hour analytical sequence. The
concentration of each target analyte in the instrument blank must not exceed CRQL.
8. No more than 14 hours may elapse from the injection beginning the opening CCV (instrument
blank) and the injection ending the closing CCV (CSS Aroclor Standard).
9. No more than 12 hours may elapse from the injection of the instrument blank that begins an
analytical sequence (opening CCV) and the injection of the last sample or blank that is part of the
same analytical sequence.
D. Evaluation
1. Verify that the CCV is performed at the specified frequency and sequence.
2. Verify that the CCV CSS standard is performed at the specified concentrations.
3. Verify that the RTs for each Aroclor peak and for surrogate in CSS standard are within the RT
Windows.
4. Check the data for each of the Aroclors and surrogates in CSS standards on Form 7D-OR and verify
that the CFs and %Ds are calculated correctly. Recalculate the CFs and %D for one or more
Aroclor peaks and verify that the recalculated values agree with that reported by the laboratory and
there are no transcription errors.
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5. Verify that %D for each of the five peaks (three major peaks for Aroclor 1221) used to identify an
Aroclor analyte and surrogates in the opening CCV CSS Aroclor Standard, or a closing CCV used
as an opening CCV for the next analytical sequence, are within the acceptance limits (± 25.0% and
± 30.0% for target analytes and surrogates, respectively).
6. Verify that %D for each of the five peaks (three major peaks for Aroclor 1221) used to identify an
Aroclor analyte and surrogates in the closing CCV CSS Aroclor Standard are within the acceptance
limits (±50.'
7. Verify that the instrument blanks paired with the CSS standard are analyzed at the specified
frequency and sequence and that the concentration of each target analyte in the instrument blank is
not exceeding CRQL.
8. Verify that the time elapse between the injection of an instrument blank as opening CCV and the
injection of that last CSS Aroclor standard as closing CCV is within 14 hours.
9. Verify that the time elapse between the injection of an instrument blank as opening CCV and the
injection of the last sample or blank in the same analytical sequence is within 12 hours.
NOTE: For data obtained from the CLP, information regarding the non-compliant CCV can be
obtained from the NFG reports and may be used as part of the evaluation process.
E. Action
1. If the CCV is not performed at the specified frequency and sequence, contact the Regional CLP PO
to request that the laboratory repeat the analysis if holding times have not expired and there is
extract remaining. Preanalysis is not possible, carefully evaluate all other available information,
including the 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 judgement, 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).
2. If CCV is not performed at the specified concentrations, use professional judgment to qualify
detects and non-detects.
3. If RTs for any Aroclor target anayte peak or surrogate in CSS standard are outside the RT Windows
and match peak pattern, use professional judgment to the associated sample results. All samples
injected after the last in-control standard are potentially affected.
a. For non-detected target analytes in the affected samples, check sample chromatograms that
may contain any peaks that are close to the expected RT Window of the target analyte peaks of
interest.
i. If no peaks used for Aroclor 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 judgment to qualify the non-detects as presumptively present with estimated
concentration (NJ).
b. For detected target analytes in the affected samples, check 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 Aroclor of interest, it may require
additional effort to determine if sample peaks represent the target analytes of interest. Peak
pattern recognition is used as a means of identifying the Aroclor target analytes.
For example, the data package may be examined for the presence of three or more standards
containing the target analytes of interest that were run within the analytical sequence during
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which the sample was analyzed. If three or more such standards are present, the RT Windows
can be re-evaluated using the RTs of the standards.
i. If the peaks used for Aroclor analyte identification in the affected sample fall within the
revised windows, qualify detects as presumptively present with estimated concentration
(NJ).
ii. If the problem of concern remains unresolved, qualify detects as unusable (R).
4. If errors are detected in the calculations of either CF or %D in any CCV CSS standard, perform a
more comprehensive recalculation. Contact the Regional CLP PO to arrange for data resubmittal
and note it in the Data Review Narrative for later CLP PO action.
5. If %D for any Aroclor target analyte peak in CCV CSS standard is outside the limits, qualify detects
as estimated (J) and non-detects as estimated (UJ).
6. If time elapse between the injection of an instrument blank as opening CCV and the injection of the
last required CSS as closing CCV exceeds 14 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 is found, qualify positive results as estimated
(J). If any possibility exists for either false positives or false negatives, qualify non-detects as
unsuable (R).
7. If time elapse 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 is 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. If RT for each target analyte peak in CSS standards are within the RT windows or %D for each
target analyte peak in CCV CSS is within the limits, detects and non-detects should not be
qualified.
9. No qualification of the data is necessary on surrogate %D alone. Use professional judgment to
evaluate the surrogate %D data in conjunction with surrogate recoveries to determine the need for
data qualification.
10. If instrument blank as part of CCV is not performed at the specified frequency and sequence, or
instrument blank does not meet the concentration criteria, refer to Section IV. Blanks for data
qualfications.
11. If the laboratory has failed to provide adequate calibration information, contact the Regional CLP
PO, who may contact the laboratory to request the necessary information. If the information is not
available, use professional judgment to assess the data.
12. Annotate the potential effects on the data due to CCV criteria exceedance in the Data Review
Narrative.
13. If CCV criteria are grossly exceeded, note this for laboratory CLP PO action.
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Table 67. CCV Actions for Aroclor Analysis
Criteria
CCV CSS not performed at correct frequency
and sequence
CCV CSS not performed at the specified
concentration
RT outside the RT window
CSS %D outside the limits
Time elapse between opening CCV
instrument blank and closing CCV CSS
exceeds 14 hr
Time elapse between opening CCV
instrument blank and last sample or blank
exceeds 12 hr
RT, CSS %D, time elapse within limits
Action
Detect
Contact CLP PO for
reanalysis or use
professional judgment
Contact CLP PO for
reanalysis or use
professional judgment
Use professional judgment
J
Use professional judgment
Use professional judgment
No qualification
Non-detect
Contact CLP PO for
reanalysis or use
professional judgment
Contact CLP PO for
reanalysis or use
professional judgment
Use professional judgment
UJ
Use professional judgment
Use professional judgment
No qualification
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IV. Blanks
A. Review Items
Form 1A-OR, Form 4-OR, chromatograms, and quantitation 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. Criteria
The criteria for evaluation of blanks should apply to any blank associated with the samples (e.g.,
method blanks, instrument blanks, sulfur cleanup blank, field blanks, etc.). If problems with any blank
exist, all associated data must be carefully evaluated to determine whether or not there is an inherent
variability in the data or if the problem is an isolated occurrence not affecting other data.
1. Method blanks must be performed at the specified frequency and sequence. A method blank must
be extracted per matrix each time when samples are extracted. The number of samples extracted
with each method blank shall not exceed 20 field samples. The method blank must be extracted by
the same procedure used to extract samples and must be analyzed on each Gas Chromatograph
(GC) system under the same conditions used to analyze associated samples.
2. The method blank, like any other sample in the SDG, must meet the technical acceptance criteria
for sample analysis.
3. An acceptable instrument blank must be analyzed at the beginning and ending of an analytical
sequence in which samples are analyzed, immediately prior to the analysis of the Aroclor
1016/1260 CSS used as CCV.
4. A sulfur cleanup blank must be analyzed whenever part of a set of the extracted samples requires
sulfur cleanup. If the entire set of samples associated with a method blank requires sulfur cleanup,
the method blank also serves the purpose of a sulfur cleanup blank and a separate sulfur cleanup
blank is not required.
5. The concentration of a target analyte in any blanks must not exceed its CRQL.
D. Evaluation
1. Verify that method blanks are extracted at the specified frequency and analyzed at the required
sequence. The Method Blank Summary (Form 4-OR) may be used to identify the samples
associated with each method blank.
2. Verify that instrument blanks are analyzed at the specified frequency and sequence.
3. Verify that the sulfur cleanup blank is analyzed when part of a set of samples extracted together
requires sulfur cleanup. The Method Blank Summary (Form 4-OR) may be used to identify the
samples associated with the sulfur cleanup blank.
4. Data concerning the field blanks are not evaluated as part of the CCS process. Evaluations on field
or trip blanks should be similar to the method blanks.
5. Review the results of all associated blanks on the forms and raw data (chromatograms and
quantitation reports) to evaluate the presence of target analytes in the blanks.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the non-compliant blank can be obtained from the NFG
reports and may be used as part of the evaluation process.
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E. Action
1. If the appropriate blanks are not extracted at the correct frequency and/or analyzed at the correct
sequence, use professional judgment to determine if the associated sample data should be qualified;
obtain additional information from the laboratory, if necessary. Record the situation in the Data
Review Narrative and note it for laboratory CLP PO action.
2. 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 Quality Assurance Project Plan (QAPP) or Regional Standard Operating Procedure (SOP).
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 having the highest concentration of a
contaminant. Do not correct the results by subtracting any blank value.
3. For any blank (including method blank), if a target analyte is detected, but it is not detected in the
sample, non-detects should not be qualified.5
4. For any method blank reported with results < CRQLs, report sample results that are < CRQLs at the
CRQLs and qualify as non-detect (U). For any method blank reported with results that are <
CRQLs, use professional judgment to qualify sample results that are > CRQLs. Positive results in
samples, especially those near but above CRQL, may be biased high by low level contamination in
the method blank, and should be considred as estimated (J+).
5. For any blank reported with results > CRQLs, report sample results that are < CRQLs at the CRQLs
and qualify as non-detect (U). For any blank reported with results > CRQLs, report at sample
results that are > CRQL but < Blank Results, and qualify as non-detect (U) or unusable (R). Use
professional judgment to qualify sample results > CRQLs and > Blank Results.
6. For Sulfur cleanup blank, instrument blanks and field blanks, sample result qualifications listed in
Table 68 should apply if supported by the project QAPP.
7. If gross contamination exists with Blank Results that are > ICAL CSS concentrations, qualify
detects as unusable (R). If the contamination is suspected of having an effect on the sample results,
note it for laboratory CLP PO action.
8. 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.
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Table 68. Blank Actions for Aroclor Analysis
Blank Type
Method, Sulfur
cleanup, Instrument,
Field
Blank Result
Detects
CRQL
Gross
contamination
Sample Result
Non-detect
CRQL
CRQL but < Blank Result
> CRQL and > Blank Result
Detects
Action
No qualification
Report at CRQL and qualify
as non-detect (U)
Use professional judgment
Report at CRQL and qualify
as non-detect (U)
Report at sample results and
qualify as non-detect(U) or as
unusable (R)
Use professional judgment
Report at sample results and
qualify as unusable (R)
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V. Surrogate
A. Review Items
Form 2C-OR, Form 8B-OR, chromatograms, and data system printouts.
B. Objective
The objective is to evaluate surrogate percent recovery (%R) to ensure that the analytical method is
efficient.
C. Criteria
1. Surrogate spiking solution containing two surrogates, TCX and DCB, is added to all samples,
including Matrix Spike (MS)/Matrix Spike Duplicates (MSDs), Laboratory Control Samples
(LCSs), and blanks to measure the surrogate recovery. The surrogates are also added to all the
standards to monitor RTs.
2. The RTs of the surrogates in each CCV CSS standard, all samples (including MS and MSB, LCS),
and all blanks must be within the calculated RT Windows. TCX must be within ±0.05 minutes, and
DCB must be within ±0.10 minutes of the RTs determined from the ICAL.
3. %R for the surrogates TCX and DCB in all samples including MS and MSDs, LCSs and all blanks
must be calculated accordingly.
4. %R for each surrogate must be in the inclusive range of 30-150% for all samples, including
MS/MSDs, LCSs and all blanks.
D. Evaluation
1. Check raw data (e.g., chromatograms and data system printouts) to verify that the surrogates are
added at the specified concentrations to all samples and blanks.
2. Check the raw data (e.g., chromatograms and data system printouts) to verify that the surrogate RTs
on Form 8B-OR are within the RT windows.
3. Check the raw data (e.g., chromatograms and data system printouts) to verify that the surrogate %R
for each sample and blank is on Form 2C-OR.
4. Check for any calculation or transcription errors; verify that the surrogate recoveries are calculated
correctly using the equation in the method.
5. Whenever there are two or more analyses for a particular sample, use professional judgment to
determine which analyses are the most accurate data to report. Considerations include, but are not
limited to:
a. Surrogate recovery (marginal versus gross deviation).
b. Technical holding times.
c. Comparison of the values of the target compounds reported in each sample analysis.
d. Other QC information, such as surrogate recoveries and/or RTs in blanks and standards.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the non-compliant surrogate recovery can be obtained
from the NFG reports and may be used as part of the evaluation process.
E. Action
1. If surrogates are not added to any sample or blank, or surrogate concentration is incorrect in sample
or blank, use professional judgment to qualify detects and non-detects. The Regional CLP PO
should be contacted to arrange for reanalysis, if possible.
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2. If surrogate RTs in CCV CSS standards, samples, and blanks are outside of the RT windows, use
professional judgment to qualify detects and non-detects. It may be necessary to have the
laboratory resubmit the data after making corrections.
3. If surrogate RTs are within RT windows, detects and non-detects should not be qualified.
4. If errors are detected in the calculations of %R, perform a more comprehensive recalculation.
5. If %R for any surrogate is outside the acceptance limits, consider the existence of coelution and
interference in the raw data. Use professional judgment to qualify data, as surrogate recovery
problems may not directly apply to target analytes.
6. If Aroclor 1262 or 1268 is detected in a sample, the %R of the DCB surrogate is advisory for both
column analyses of the specific sample. However, %R for TCX must meet the acceptance criteria.
7. If %R for any surrogate in undiluted sample is < 10%, qualify detects as estimated low (J-) and
non-detects as unusable (R).
8. If %R for any surrogate in diluted sample is < 10%, use professional judgment to qualify detects
and non-detects.
9. If %R for any surrogate is > 10%, and < 30%, qualify detects as estimated low (J-) and non-detects
as estimated (UJ).
10. If %R for both surrogates are > 30%, and < 150%, detects and non-detects should not be qualified.
11. If %R for any surrogate is > 150% but < 200%, qualify detects as estimated high (J+). Non-detects
should not be qualified.
12. If %R for any surrogate is > 200%, qualify detects as estimated (J). Use professional judgment to
qualify non-detects.
13. In the special case of a blank analysis with surrogate %R outside the acceptance limits, give special
consideration to qualify 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.
For example, 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. Note analytical problems for laboratory CLP PO action even if this judgment allows
some use of the affected data.
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Table 69. Surrogate Actions for Aroclor Analysis
Criteria
RT out of RT window
RT within RT window
%R < 10% (undiluted sample )
%R < 10% (diluted sample )
10%<%R<30%
30%<%R<150%
150%<%R<200%
%R > 200%
Action*
Detect
Use professional judgment
No qualification
J-
Use professional judgment
J-
No qualification
J+
J+
Non-detect
Use professional judgment
No qualification
R
Use professional judgment
UJ
No qualification
No qualification
Use professional judgment
* %R of the DCB surrogate is advisory for both column analyses of samples with detected Aroclor
1262 or 1268.
** Use professional judgment in qualifying data, as surrogate recovery problems may not directly
apply to target analytes.
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VI. Matrix Spike/Matrix Spike Duplicate
A. Review Items
Cover Page, Form 3A-OR, chromatograms, and quantitation reports.
B. Objective
The objective of MS/MSD analysis is to evaluate the effect of each sample matrix on the sample
preparation procedures and the measurement methodology.
C. Criteria
1. MS/MSD samples should be prepared and analyzed at specified frequency. One pair of MS/MSD
should be analyzed per matrix or per SDG.
2. Samples identified as field blanks or Performance Evaluation (PE) samples cannot be used for
MS/MSD sample analysis.
3. MS/MSD %R and the Relative Percent Difference (RPD) between MS and MSD results should be
calculated according to the method.
4. MS/MSD %R and RPD should be within the acceptance limits in Table 70.
D. Evaluation
1. Verify that requested MS/MSD samples are analyzed at the required frequency.
2. Verify that a field blank or PE sample is not used for MS/MSD analysis.
3. Verify that the recalculated MS/MSD %R and RPD values agree with the laboratory reported
values on Form 3A-OR.
4. Check MS/MSD %R and RPD on Form 3A-OR and verify that they are within the limits in Table
70.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the non-compliant MS/MSD %R or RPD can be obtained
from the NFG reports and may be used as part of the evaluation process.
E. Action
1. If MS/MSD samples are not analyzed at the specified frequency, use professional judgment to
determine the impact on sample data, if any; it may be necessary to obtain additional information
from the laboratory. Record the situation in the Data Review Narrative and note it for laboratory
CLP PO action. It is not likely that data qualification will be warranted if the frequency
requirement is not met. Carefully consider all factors, known and unknown, about method
performance on the matrix at hand, in lieu of MS/MSD data.
2. If a field blank or PE sample is used for the MS/MSD analysis, note this for laboratory CLP PO
action. All of the other QC data must then be carefully checked. Use professional judgment when
evaluating the data.
3. If errors are detected in the calculations of MS/MSD %R or RPD, perform a more comprehensive
recalculation.
4. If the MS/MSD %R or RPD is outside the acceptance limits in Table 70, qualify detects and
non-detects in the original sample to include the consideration of the existence of interference in the
raw data. Considerations include, but are not limited to:
a. If MS/MSD %R is < 20%, qualify detects as estimated (J) and non-detects as unusable (R).
b. If MS/MSD %R is > 20% and < the lower acceptance limit, qualify detects as estimated (J) and
non-detects as estimated (UJ).
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c. If MS/MSD %R or RPD is > lower acceptance limit and < upper acceptance limit, detects and
non-detects should not be qualified.
d. If MS/MSD%R or RPD is > the upper acceptance limit, qualify detects as estimated (J).
Non-detects should not be qualified.
Table 70. MS/MSD %R and RPD Limits for Aroclor Analysis
Analyte
AR1016
AR1260
%R Water and
Soil Sample
29-135
29-135
RPD Water and
Soil Sample
0-15
0-20
Table 71. MS/MSD Actions for Aroclor Analysis
Criteria
%R < 20%
20% < %R < Lower Acceptance Limit
Lower Acceptance Limit < %R;
RPD < Upper Acceptance Limit
%R or RPD > Upper Acceptance Limit
Action
Detect
J
J
No qualification
J
Non-detect
R
UJ
No qualification
No qualification
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VII. Laboratory Control Sample
A. Review Items
Form 3B-OR, chromatograms, and data system printouts.
B. Objective
The objective is to evaluate the accuracy of the analytical method and laboratory performance.
C. Criteria
1. An LCS must be prepared and analyzed at the specified frequency. LCS should be extracted and
analyzed per matrix or per SDG. LCS should be extracted using the same procedures as the
samples and method blank.
2. The requirements below apply independently to each GC column and to all instruments used for
these analyses. Quantitation must be performed on each GC column.
3. The LCS must contain the target analytes in Table 72 and the surrogates at the specified
concentrations in the method [Table 5 in the Statement of Work (SOW)].
4. The %R for each spiked analyte in LCS must be calculated according to the method.
5. The %R for each spiked analyte must be within the acceptance limits in Table 72.
Table 72. LCS %R Limits for Aroclor Analysis
Analyte
Aroclor 1016
Aroclor 1260
%Recovery
Water and Soil Sample
50-150
50-150
6. All samples prepared and analyzed with an LCS that does not meet the technical acceptance criteria
in the method will require re-extraction and reanalysis.
D. Evaluation
1. Verify that LCS is prepared and analyzed at the specified frequency.
2. Check the raw data (e.g., chromatograms and data system printouts) to verify that the LCS is spiked
with the specified target analytes at the method specified concentrations (Table 5 in the SOW).
3. Check the raw data (e.g., chromatograms and data system printouts) to verify that %R of each
target analyte in LCS is calculated correctly and that the recalculated %R values agree with that
reported on Form 3B-OR.
4. Verify that %R of each target analyte in LCS is within the specified acceptance limits.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the non-compliant LCS %R can be obtained from the NFG
reports and may be used as part of the evaluation process.
E. Action
1. If LCS is not performed at the specified frequency, use professional judgment to qualify detects and
non-detects in the associated samples.
NOTE: If an LCS sample is not analyzed at the specified frequency, use professional judgment to
determine the impact on sample data; obtain additional information from the laboratory, if
necessary. Record the situation in the Data Review Narrative and note it for laboratory
CLP PO action. It is not likely that data qualification will be warranted if the frequency
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requirement is not met. Carefully consider all factors, known and unknown, about method
performance, in lieu of LCS data.
2. If LCS is not performed at the specified concentration, use professional judgment to qualify detects
and non-detects in the associated samples.
3. If errors are detected in the calculations of LCS %R, perform a more comprehensive recalculation.
4. If the LCS %R criteria are not met, qualify the specific target analyte in the associated samples.
a. If the LCS %R is < the lower acceptance limit, qualify detects as estimated low (J-) and
non-detects as unusable (R).
b. If the LCS %R is > lower acceptance limit and < upper acceptance limit, detects and
non-detects should not be qualified.
c. If the LCS %R is > the upper acceptance limit, qualify detects as estimated high (J+).
Non-detects should not be qualified.
d. Use professional judgment to qualify analytes other than those included in the LCS.
e. Take into account the analyte class, analyte recovery efficiency, analytical problems associated
with each analyte, and comparability in the performance of the LCS analyte to the non-LCS
analyte.
Table 73. LCS Actions for Aroclor Analysis
Criteria
%R < Lower Acceptance Limit
Lower Acceptance Limit < %R < Upper
Acceptance Limit
%R > Upper Acceptance Limit
Action
Detect
J-
No qualification
J+
Non-Detect
R
No qualification
No qualification
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VIII. Gel Permeation Chromatography Performance Check
A. Review Items
Form 9B-OR, two ultraviolet (UV) traces, Gel Permeation Chromatography (GPC) cleanup blank
quantitation reports, and chromatograms.
B. Objective
The objective is to evaluate GPC cleanup efficiency.
C. Criteria
1. GPC is used for the cleanup of all non-aqueous sample extracts and for aqueous sample extracts
that contain high molecular weight components that interfere with the analysis of the target
analytes.
2. Each GPC system must be calibrated prior to processing samples for GPC cleanup, when the GPC
CCV solution fails to meet criteria, when the column is changed, when channeling occurs, and once
every 7 days when in use.
3. The GPC calibration is acceptable if the two UV traces meet the following requirements:
a. Peaks must be observed and symmetrical for all compounds in the calibration solution.
b. Corn oil and the phthalate peaks exhibit > 85% resolution.
c. The phthalate and methoxychlor peaks exhibit > 85% resolution.
d. Methoxychlor and perylene peaks exhibit > 85% resolution.
e. Perylene and sulfur peaks must not be saturated and should exhibit > 90% baseline resolution.
f The RT shift is < 5% between UV traces for Bis(2-ethylhexyl) phthalate and perylene.
4. A GPC blank must be analyzed after each GPC calibration. The concentration for any target
analyte in the GPC blank must not exceed the CRQL.
5. The calibration verification must be performed at least once every 7 days according to the
specifications.
6. The GPC calibration verification solution must contain Aroclor 1016 and Aroclor 1260 at the
specified concentrations in the method (0.4 (ig/mL).
7. %R for each target analyte in the GPC calibration verification must be calculated according to the
method.
8. %R for each target analyte in the GPC calibration verification must be in the inclusive range of
80-120%.
D. Evaluation
1. Verify that the GPC calibration is performed at the specified frequency.
2. Verify that there are two UV traces present and that the RT shift for Bis(2-ethylhexyl) phthalate and
perylene is < 5%.
3. Verify that the target analytes in the GPC calibration standard are present and the peaks are
symmetrical in both UV traces meeting the minimum resolution requirements.
4. Verify that no target analyte in the GPC blank exceeds the CRQL.
5. Verify that the GPC calibration verification is performed at the specified frequency.
6. Verify that the %R for target analytes are calculated correctly and the %R values agree with that on
Form 9B-OR
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7. Verify that the %R for target analytes is within the acceptance limits.
E. Action
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 sample data for
unusual peaks; and use professional judgment to qualify the data. If the laboratory chooses to
analyze samples under unacceptable GPC criteria, notify the CLP PO.
a. If the RT shift of Bis(2-ethylhexyl) phthalate and perylene is > 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. Contact the Regional CLP PO to arrange for sample reanalysis.
2. If GPC calibration verification is not performed at the specified frequency, use professional
judgment to qualify detects and non-detects.
3. If GPC calibration verification is not performed at the specified concentrations, use professional
judgment to qualify detects and non-detects.
4. If errors are detected in the calculations of %R in the GPC calibration verification, perform a more
comprehensive recalculation.
5. If GPC calibration verification criteria are not met, examine the raw data and qualify data as
follows:
a. If %R is < 10% for any target analytes and surrogates in the GPC calibration verification, use
professional judgment to qualify detects. Qualify non-detects as unusable (R).
b. If %R is > 10% and < 80% for any target analytes and surrogates in the GPC calibration
verification, qualify detects as estimated (J) and non-detects as estimated (UJ).
c. If %R is > 80% and < 120% for all target analytes and surrogates in the GPC calibration
verification, detects and non-detects should not be qualified.
d. If %R is > 120% for any target analytes and surrogates surrogates in the GPC calibration
verification, use professional judgment to qualify detects. Non-detects should not be qualified.
6. Annotate the potential effects on the sample data resulting from the GPC cleanup analyses not
yielding acceptable results in the Data Review Narrative.
NOTE: For data obtained from the CLP, information regarding the non-compliant CCV can be
obtained from the NFG reports and may be used as part of the evaluation.
Table 74. GPC Performance Check Actions for Arolcor Analysis
Criteria
%R < 10% (target analytes)
10%< %R < 80% (target analytes)
80% < %R < 120% (target analytes)
%R > 120% (target analytes)
Action
Detect
Use professional judgment
J
No qualification
Use professional judgment
Non-Detect
R
UJ
No qualification
No qualification
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IX. Target Analyte Identification
A. Review Items
Form 1A-OR, Form 10B-OR, chromatograms, and data system printouts.
B. Objective
The objective is to provide acceptable Gas Chromatograph/Electron Capture Detector (GC/ECD)
qualitative analysis to minimize the number of erroneous analyte identifications.
C. Criteria
1. The RTs of both of the surrogates and reported target analytes with five major peaks (three major
peaks for Aroclor 1221) in each sample must be within the calculated RT windows on both
columns. TCX must be within ±0.05 minutes of the RT determined from the ICAL, and DCB must
be within ±0.10 minutes of the RT determined from the ICAL.
2. For detected target analytes, %D between the concentrations on two GC columns must be
calculated according to the method. The %D for any detected target analyte should be < 25.0% to
have high confidence in the identification.
3. When no analytes are identified in a sample, the chromatograms from the analyses of the sample
extract must use the same scaling factor as was used for the low-point standard of the ICAL
associated with those analyses.
4. Chromatograms must display the largest peak of any Aroclors detected in the sample at less than
full scale.
5. If an extract must be diluted, chromatograms must display the five chosen maj or peaks (three maj or
peaks for Aroclor 1221) for an analyte between 25-100% of full scale.
6. If a chromatogram is replotted electronically to meet these requirements, the scaling factor used
must be displayed on the chromatogram, and both the initial chromatogram and the replotted
chromatogram must be submitted in the data package.
D. Evaluation
1. Review Form 1A-OR, the associated raw data (chromatograms and data system printouts) and
Form 10B-OR
a. Verify that the reported target analytes as detects are identified correctly with five major peaks
(three major peaks for Aroclor 1221) by comparing the sample chromatograms to the tabulated
results and verifying peak measurements and RTs.
b. Verify non-detects by a review of the sample chromatograms.
c. Check the associated blank data for potential interferences (to evaluate sample data for false
positives) and check the calibration data for adequate RT windows (to evaluate sample data for
false positives and false negatives).
2. Verify that the %D for any target analyte is calculated correctly and that the recalculated %D agrees
with that reported on Form 10B-OR.
3. Verify that the %D for any target analyte is < 25.0%. If target %D is > 25% for any target analyte
evaluate the impact of the presence of an interfering compound and whether the interference
precludes confirmation of the target analyte. Also, evaluate the possibility of poor precision or
ono-homogeneity as causes for the difference.
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E. Action
1. If the qualitative criteria for both columns are not met, all target analytes that are reported as detects
should be qualified as non-detect (U). Use professional judgment to assign an appropriate
quantitation limit using the following guidance:
a. If the detected target analyte peak is sufficiently outside the RT window determined from the
associated ICAL, the reported value may be a false positive and should be replaced with the
sample CRQL value.
b. If the detected target analyte peak poses an interference with potential detection of another
target peak, the reported value should be considered and qualified as unusable (R).
2. If five major peaks (three major peaks for Aroclor 1221) are identified in both GC column analyses
that fall within the appropriate RT windows, but the analyte is reported as a non-detect, the analyte
may be a false negative. Use professional judgment to decide if the analyte should be included and
reported as detect. Annotate all conclusions made regarding target analyte identification in the
Data Review Narrative.
3. If the Aroclor peak RT windows determined from the calibration overlap with single component
target analytes or chromatographic interferences, use professional judgment to qualify the data.
4. If an Aroclor exhibits amarginal pattern-matching quality, use professional judgment to determine
if the differences are due to environmental "weathering" (i.e., degradation of the earlier eluting
peaks relative to the later eluting peaks). If the presence of an Aroclor is strongly suggested, report
results as presumptively present with estimated concentration (NJ).
5. If errors are detected in the calculations of %D for any target analyte, perform a more
comprehensive recalculation.
6. If an interfering compound is indicated, consider the potential for co-elution and use professional
judgment to determine how best to report. It is recommended to either report the analyte as positive
at the lower value, qualified as tentative (N), or as non-detect (U) at the CRQL.
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X. Gas Chromatograph/Mass Spectrometer Confirmation
A. Review Items
Form 1A-OR, Form 10B-OR, chromatograms, and data system printouts.
B. Objective
The objective is to ensure the accuracy of the positive identification of a target analyte. In the case of
Aroclors, the objective is to obtain sufficient information to confirm the presence of Fob/chlorinated
Biphenyls (PCBs) in a sample, not necessarily to confirm which Aroclor is present. This should be
accomplished by pattern matching on each of two GC columns in the GC/ECD analysis.
C. Criteria
1. GC/MS confirmation is required when a positively identified target analyte has on-column
concentration meeting the specified criterion on both GC columns. GC/MS shall be performed for
at least one peak concentration > 10 ng/(iL.
2. GC/MS confirmation may be accomplished by one of three general means:
a. Examination of the semivolatile GC/MS library search results [i.e., Tentatively Identified
Compound (TIC) data];
b. A second analysis of the semivolatile extract; or
c. Analysis of the Aroclor extract, following any solvent exchange and concentration steps that
may be necessary.
D. Evaluation
1. Review Form 1A-OR, the associated raw data (chromatograms and data system printouts) and
Form 10B-OR
2. Check quantitation report to verify that GC/MS confirmation is required by ensuring that the
on-column concentration criteria are met.
3. Verify that GC/MS confirmation is completed as specified in the method.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding non-compliant GC/MS can be obtained from the CCS
report and may be used as part of the evaluation process.
E. Action
1. If an analyte was confirmed by GC/MS, qualify as confirmed (C).
2. If a sufficient quantity of an analyte was indicated and GC/MS confirmation was attempted but was
not confirmed, qualify with special qualified (X) or non-detect (U). Explain in the Data Review
Narrative that the analyte should be considered a non-detect because it could not be confirmed.
Table 75. GC/MS Confirmation Actions
Criteria
Analyte confirmed by GC/MS
Analyte indicated, but not confirmed by GC/MS
Action for Detects
C
XorU
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XI. Target Analyte Quantitation and Reported Contract Required Quantitation Limit
A. Review Items
Form 1A-OR, sample preparation sheets, SDG Narrative, quantitation reports, and chromatograms.
B. Objective
The objective is to ensure that the reported results and CRQLs for target analytes are accurate.
C. Criteria
1. Target analyte results, as well as the sample specific CRQLs, must be calculated according to the
correct equations.
2. Target analyte CF must be calculated using the correct associated ICAL. Target analyte result must
be calculated using the CF from the associated ICAL.
D. Evaluation
1. Verify that the results for all positively identified analytes are calculated and reported by the
laboratory. Verify that the CRQLs are calculated for the non-detects and reported accordingly.
2. Verify that the correct CF is used to calculate the reported results.
3. Verify that the same CF is used consistently for all sample result calculations.
4. Verify that the sample-specific CRQLs have been calculated and adjusted to reflect Percent Solids
(%Solids) and sample dilutions.
a. For soil/sediment samples that are high in moisture (i.e., < 30% solid), evaluation of the
presence of each analyte depends on the anticipated interaction between the analyte and the
total matrix, as well as how the sample was processed.
b. If the phases of a sample were separated and processed separately, the results may be
mathematically recombined or reported separately. No particular qualification on the grounds
of matrix distribution is warranted.
c. If a soil/sediment sample was processed by eliminating most of the water, analytes that are
highly soluble under ambient conditions may be severely impacted such that their presence
cannot be completely evaluated.
5. Verify that recalculated results and CRQLs agree with that reported by the laboratory.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the non-compliant results or CRQLs can be obtained from
the CCS report and may be used as part of the evaluation process.
E. Action
1. If any discrepancies are found, contact the Regional CLP PO, who may contact the laboratory to
obtain additional information that could resolve any differences. If a discrepancy remains
unresolved, use professional judgment to decide which value is the most accurate. Under these
circumstances, use professional judgment to determine that qualification of data is warranted.
Annotate the reasons for any data qualification in the Data Review Narrative.
2. If errors are detected in results and CRQL calculations, perform a more comprehensive
recalculation.
3. If %Solids for a soil sample is < 10.0%, use professional judgment to qualify detects and
non-detects.
4. If %Solids for a soil sample is > 10% and < 30.0%, use professional judgment to qualify detects and
non-detects.
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5. If %Solids for a soil sample is > 30.0%, detects and non-detects should not be qualified.
6. If sample results are < CRQLs and > MDLs, qualify as estimated (J).
7. Note numerous or significant failures to accurately quantify the target analytes, or to properly
evaluate and adjust CRQLs, for laboratory CLP PO action.
Table 76. Percent Solids Actions for Aroclor Analysis for Non-Aqueous Samples
Criteria
%Solids<10.0%
10.0% < %Solids < 30.0%
%Solids > 30.0%
Action
Detect
Use professional judgment
Use professional judgment
No qualification
Non-detect
Use professional judgment
Use professional judgment
No qualification
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XII. Regional Quality Assurance and Quality Control
A. Review Items
Form 1A, chromatograms, TR/COC documentation, quantitation reports, and other raw data from
Quality Assurance/Quality Control (QA/QC) samples.
B. Objective
Regional QA/QC samples refer to any QA and/or QC samples initiated by the Region, including field
duplicates, PE samples, blind spikes, and blind blanks. The use of these QA/QC samples is highly
recommended (e.g., the use of field duplicates can provide information on sampling precision and
homogeneity).
C. Criteria
Criteria are determined by each Region.
1. PE sample frequency may vary.
2. The target analytes present in the PE sample must be correctly identified and quantified.
3. The RPD between field duplicates shall fall with the specific limits in the Region's SOP or project
QAPP.
D. Evaluation
1. Evaluation procedures must follow the Region's SOP for data review. Each Region will handle the
evaluation of PE samples on an individual basis.
2. Verify that the target analyte in the PE sample is properly identified and that the result is calculated
correctly.
3. Verify that the acceptance criteria for the specific PE sample are met, if available.
4. Calculate the RPD between field duplicates and provide this information in the Data Review
Narrative. Also verify that the value falls within the specific limits in the Region's SOP or project
QAPP.
E. Action
1. Any action must be in accordance with Regional specifications and the criteria for acceptable PE or
field duplicate sample results.
2. Note unacceptable results for PE or field duplicate samples for laboratory CLP PO action.
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XIII. Overall Assessment of Data
A. Review Items
Entire data package, data review results, and (if available), the QAPP, and Sampling and Analysis Plan
(SAP).
B. Objective
The objective is to provide the overall assessment on data quality and usability.
C. Criteria
1. Review all available materials to assess the overall quality of the data, keeping in mind the additive
nature of analytical problems.
2. Reported analyte concentrations must be quantitated according to the appropriate analytical
method, as listed in the method. All sample results must be within the linear calibration ranges per
methods.
D. Evaluation
Examine the raw data to verify that the correct calculation of the sample results was reported by the
laboratory. Analysis logs, instrument printouts, etc., should be compared to the reported sample results
recorded on the appropriate Organic Summary Forms (Form 1A-OR through Form 10B-OR).
1. Evaluate any technical problems which have not been previously addressed.
2. Examine the raw data for any anomalies (e.g, baseline shift).
3. Verify appropriate method is used in sample analysis.
4. Verify that there are no transcription or reduction errors.
5. Verify that target analyte results fall within the calibrated ranges.
6. If appropriate information is available, use professional judgment to assess the usability of the data
to to assist the data user in avoiding inappropriate use of the data. Review all available information,
including the QAPP (specifically the acceptance and performance criteria), SAP, and
communication with the data user that concerns the intended use and desired quality of these data.
E. Action
1. Use professional judgment to determine if there is any need to qualify data which were not
qualified based on the QC criteria previously discussed.
2. Use professional judgment to qualify sample results and non-detects if the MDL exceeds CRQL.
3. If a sample is not diluted properly when sample results exceed the upper limit of the calibration
range, qualify sample results as estimated (J).
4. Write a brief Data Review Narrative to give the user an indication of the analytical indications of
the data.
5. Note any inconsistency of the data with the SDG Narrative for laboratory CLP PO action. If
sufficient information on the intended use and required quality of the data is available, include an
assessment of the usability of the data within the given context. This may be used as part of a
formal Data Quality Assessment (DQA).
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APPENDIX A: GLOSSARY
Analysis Date/Time - The date and military time (24-hour clock) of the injection of the sample, standard,
or blank into the Gas Chromatograph/Mass Spectrometer (GC/MS) or Gas Chromatograph (GC) system.
Aroclor - A trademarked name for a mixture of poly chlorinated biphenyls (PCBs) used in a variety of
applications including additives in lubricants, heat transfer dielectric fluids, adhesives, etc.
Blank - An analytical sample designed to assess specific sources of contamination. See individual
definitions for types of blanks.
Breakdown - A measure of the decomposition of certain analytes (DDT and Endrin) into by-products.
4-Bromofluorobenzene (BFB) - The compound chosen to establish mass spectrometer instrument
performance for volatile analyses.
Calibration Factor (CF) - A measure of the Gas Chromatographic response of a target analyte to the mass
injected.
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).
Contamination - A component of a sample or an extract that is not representative of the environmental
source of the sample. Contamination may stem from other samples, sampling equipment, while in transit,
from laboratory reagents, laboratory environment, or analytical instruments.
Continuing Calibration Verification (CCV) - Analytical standard run every 12 hours to verify that the
instrument response at the concentration of the standard is within acceptable limits.
Contract Compliance Screening (CCS) - A screening of electronic and hardcopy data deliverables for
completeness and compliance with the contract. This screening is performed under the United States
Environmental Protection Agency (EPA) direction by the Sample Management Office (SMO) Contractor.
Contract Laboratory Program (CLP) - Supports the EPA's Superfund effort by providing a range of
state-of-the-art chemical analytical services of known and documented quality. This program is directed by
the Analytical Services Branch (ASB) of the Office of Superfund Remediation and Technology Innovation
(OSRTI) of the EPA.
Contract Laboratory Program Project Officer (CLP PO) - The Regional EPA official responsible for
monitoring laboratory performance and/or requesting analytical data or services from a Contract
Laboratory Program (CLP) laboratory.
Contractual Holding Time ~ 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.
Decafluorotriphenylphosphine (DFTPP) - Compound chosen to establish mass spectrometer instrument
performance for semivolatile analysis.
Deuterated Monitoring Compound (DMC) - Compound added to every volatile and semivolatile
calibration standard, blank, and sample used to evaluate the efficiency of the extraction/purge and trap
procedures, and the performance of the Gas Chromatograph/Mass Spectrometer (GC/MS) systems. DMCs
are isotopically labeled (deuterated) analogs of native target analytes. DMCs are not expected to be
naturally detected in the environmental media.
Field Blank - A blank used to provide information about contaminants that may be introduced during
sample collection.
Field Sample - A portion of material to be analyzed that is contained in single or multiple containers and
identified by a unique sample number.
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Organic Data Review Appendix A: Glossary
14-Hour Time Period - For pesticide and Aroclor analyses, the fourteen-hour time period begins at the
injection of the beginning of the sequence for an opening Continuing Calibration Verification (CCV)
(instrument blank) and must end with the injection of the closing sequence of the closing CCV [Individual
standard A, B, or C or Performance Evaluation Mixture (PEM)]. The time period ends after 14 hours have
elapsed according to the system clock.
Gas Chromatograph (GC) - The instrument used to separate analytes on a stationary phase within a
chromatographic column. The analytes are volatized directly from the sample (volatile), or injected as
extracts (semivolatile, pesticides, and Aroclors). In volatile and semivolatile analyses, the compounds are
detected by a Mass Spectrometer. In pesticide and Aroclors analyses, the compounds are detected by an
Electron Capture Detector (ECD).
Gas Chromatograph/Electron Capture Detector (GC/ECD) - A Gas Chromatograph (GC) equipped
with an Electron Capture Detector (ECD). This is one of the most sensitive gas chromatographic detectors
or halon-containing compounds such as organochlorine pesticides and polychlorinated biphenyls.
Initial Calibration - Analysis of analytical standards at different concentrations to define the linear range
of an analytical instrument [e.g., Gas Chromatograph/Mass Spectrometer (GC/MS), Gas
Chromatograph/Electron Capture Detector (GC/ECD)].
Instrument Blank - A blank designed to determine the level of contamination either associated with the
analytical instruments, or resulting from carryover.
Internal Standards - Compounds added to every volatile and semivolatile standard, blank, sample, or
sample extract, including the Laboratory Control Sample (LCS), at a known concentration, prior to
analysis. Internal standards are used to monitor instrument performance and quantitation of target
compounds.
Laboratory Control Sample (LCS) - The LCS is an internal laboratory Quality Control (QC) sample
designed to assess [on a Sample Delivery Group (SDG)-by-SDG basis] the capability of the contractor to
perform the analytical method.
m/z - Mass-to-charge ratio, synonymous with "m/e".
Matrix - The predominant material of which the sample to be analyzed is composed. For the purpose of
this document, the sample matrix is either aqueous or non-aqueous.
Matrix Effect - In general, the effect of a particular matrix on the constituents with which it contacts.
Matrix effects may prevent efficient purging/extraction of target analytes, and may affect DMC and
surrogate recoveries. In addition, non-target analytes may be extracted from the matrix causing
interferences.
Matrix Spike (MS) - Aliquot of the sample fortified (spiked) with known quantities of specific compounds
and subjected to the entire analytical procedure in order to indicate the appropriateness of the method for
the matrix by measuring recovery.
Matrix Spike Duplicate (MSD) - A second aliquot of the same sample that is fortified (spiked) with
known quantities of specific compounds and subjected to the entire analytical procedure in order to
determine precision of the method.
Method Blank - A reagent aqueous sample spiked with internal standards, and surrogate standards (or
DMCs for volatile and semivolatile), that is carried throughout the entire analytical procedure. The method
blank is used to define the level of contamination associated with the processing and analysis of samples.
Narrative (SDG Narrative) - Portion of the data package which includes laboratory, contract, Case and
sample number identification, and descriptive documentation of any problems encountered in processing
the samples, along with corrective action taken and problem resolution.
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Percent Difference (%D) - The difference between two values (usually a true value and a found value),
calculated as a percentage of the true value. The Percent Difference indicates both the direction and the
magnitude of the difference (i.e., the Percent Difference may be either negative, positive, or zero).
Percent Relative Standard Deviation (%RSD) - The Percent Relative Standard Deviation is calculated
from the standard deviation and mean measurement of either RRFs or CFs from initial calibration
standards. Percent Relative Standard Deviation indicates precision of a set of measurements.
Performance Evaluation Mixture (PEM) - A calibration solution of specific analytes used to evaluate
both recovery and Percent Breakdown as measures of performance.
Polychlorinated Biphenyls (PCBs) - A group of toxic, persistent chemicals used in electrical transformers
and capacitors for insulating purposes, and in gas pipeline systems as a lubricant. The sale and new use of
PCBs were banned by law in 1979.
Purge-and-Trap (Device) - Analytical technique (device) used to isolate volatile (purgeable) organics by
stripping the compounds from aqueous by a stream of inert gas, trapping the compounds on an adsorbent
such as a porous polymer trap, and thermally desorbing the trapped compounds onto the Gas
Chromatographic column.
Reconstructed Ion Chromatogram (RIC) - A mass spectral graphical representation of the separation
achieved by a Gas Chromatograph; a plot of total ion current versus Retention Time (RT).
Relative Percent Difference (RPD) - The difference between two values, calculated as a percent relative
to the mean of the two values.
Relative Response Factor (RRF) - A measure of the mass spectral response of an analyte relative to its
associated internal standard. RRFs are determined by analysis of standards and are used in the calculation
of concentrations of analytes in samples.
Relative Retention Time (RRT) - The ratio of the Retention Time (RT) of a compound to that of a
standard (such as an internal standard).
Resolution - Also termed separation or percent resolution, the separation between peaks on a
chromatogram, calculated by dividing the depth of the valley between the peaks by the peak height of the
smaller peak being resolved, multiplied by 100.
Resolution Check Mixture - A solution of specific analytes used to determine resolution of adjacent
peaks; used to assess instrumental performance.
Retention Time (RT) - The time a target analyte is retained on a Gas Chromatograph (GC) column before
elution. The identification of a target analyte is dependent on a target compound's RT falling within the
specified RT Window established for that compound. The RT is dependent on the nature of the column's
stationary phase, column diameter, temperature, flow rate, and other parameters.
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:
• Each Case of field samples received, or
• Each twenty (20) field samples (excluding Performance Evaluation (PE) samples) within a
Case, or
• Each seven (7) calendar day period [three (3) calender day period for seven (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).
In addition, all samples and/or sample fractions assigned to an SDG must have been scheduled under the
same contractual turnaround time. Preliminary Results have no impact on defining the SDG.
Sample Management Office (SMO) - A contractor-operated facility operated under the Contract
Laboratory Analytical Services Support (CLASS) contract, awarded and administered by the EPA.
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Organic Data Review Appendix A: Glossary
Sample Number (EPA Sample Number) - A unique identification number designated by the EPA to each
sample. An EPA Sample Number appears on the Traffic Report/Chain of Custody Record (TR/COC)
which documents information on that sample.
Semivolatile Compounds - Compounds amenable to analysis by extraction of the sample with an organic
solvent. Used synonymously with Base/Neutral/Acid (BNA) compounds.
Statement of Work (SOW)- A document which specifies how laboratories analyze samples under a
particular Contract Laboratory Program (CLP) analytical program.
Storage Blank - Reagent water (two 40.0 mL aliquots) or clean sand stored with volatile samples in a
Sample Delivery Group (SDG). It is analyzed after all samples in that SDG have been analyzed; and it is
used to determine the level of contamination acquired during storage.
Sulfur Cleanup Blank - A modified method blank that is prepared only when some of the samples in a
batch are subjected to sulfur cleanup. It is used to determine the level of contamination associated with the
sulfur cleanup procedure. When all of the samples are subjected to sulfur cleanup, the method blank serves
this purpose. When none of the samples are subjected to sulfur cleanup, no sulfur cleanup blank is required.
Surrogates (Surrogate Standard) - For pesticides and Aroclors, compounds added to every blank,
sample [including Laboratory Control Sample (LCS)], Matrix Spike/Matrix Spike Duplicate (MS/MSD),
and standard; used to evaluate analytical efficiency by measuring recovery. Surrogates are not expected to
be detected in environmental media.
Target Analyte List (TAL) - A list of analytes designated by the Statement of Work (SOW) for analysis.
Technical Holding Time - The maximum length of time that a sample may be held from the collection date
until extraction and/or analysis.
Tentatively Identified Compound (TIC) - Compounds detected in samples that are not target compounds,
internal standards, Deuterated Monitoring Compounds (DMCs), or surrogates. Up to thirty (30) peaks, not
including those identified as alkanes (those greater than 10% of the peak area or height of the nearest
internal standard), are subjected to mass spectral library searches for tentative identification.
Traffic Report/Chain of Custody Record (TR/COC) - An EPA sample identification form filled out by
the sampler, which accompanies the sample during shipment to the laboratory and which documents sample
condition and receipt by the laboratory.
Trip Blank - A blank used to provide information about contaminants that may be introduced during
sample transport.
Twelve-hour Time Period - The twelve (12)-hour time period for Gas Chromatograph/Mass
Spectrometer (GC/MS) system instrument performance check, standards calibration [initial or Continuing
Calibration Verification (CCV)], and method blank analysis begins at the moment of injection of the
Decafluorotriphenylphosphine (DFTPP) or 4-Bromofluorobenzene (BFB) analysis that the laboratory
submits as documentation of instrument performance. The time period ends after 12 hours have elapsed
according to the system clock. For pesticide analyses performed by Gas Chromatograph/Electron Capture
Detector (GC/ECD), the 12-hour time period in the analytical sequence begins at the moment of injection of
the instrument blank that precedes sample analyses, and ends after twelve hours have elapsed according to
the system clock.
Volatile Compounds - Compounds amenable to analysis by the purge-and-trap technique. Used
synonymously with purgeable compounds.
October 2013 A-4
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Organic Data Review
APPENDIX B: ORGANIC DATA REVIEW SUMMARY
CASE NO.
LABORATORY
SDGNO.
REVIEWER NAME
CLP PO: ACTION
SITE
NO. OF SAMPLES/MATRIX
SOW NO. REGION
COMPLETION DATE
FYI
Review Criteria
Preservation
GC/MS or GC/ECD Instrument
Performance Check
Initial Calibration
Continuing Calibration
Verification
Blanks
Method
TRACE
VGA
LOW/MED
VGA
SVGA
PEST
AROCLOR
October 2013
B-l
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Organic Data Review
Review Criteria
Deuterated Monitoring
Compound or Surrogate Spikes
Matrix Spike/Matrix Spike
Duplicate
Laboratory Control Sample
Regional QA/QC
Internal Standards
GPC Performance Check
Method
TRACE
VGA
LOW/MED
VGA
SVGA
PEST
AROCLOR
October 2013
B-2
-------
Organic Data Review
Review Criteria
Florisil Cartridge Performance
Check
Target Analyte Identification
GC/MS Confirmation
Target Analyte Quantitation and
Reported CRQLs
Tentatively Identified Compounds
System Performance
Method
TRACE
VGA
LOW/MED
VGA
SVGA
PEST
AROCLOR
October 2013
B-3
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Organic Data Review
Review Criteria
Overall Assessment of Data
Method
TRACE
VGA
LOW/MED
VGA
SVGA
PEST
AROCLOR
October 2013
B-4
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