NATIONALFUNCTIONALGUIDELINES
for Organic Superfund Methods Data Review
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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 upon to create a substantive or procedural right enforceable by any other
person. The Government may take action that is at a variance with the policies and procedures in this
manual.
This document can be obtained from the EPA's Superfund Analytical Services and Contract Laboratory
Program website at:
https://www.epa.gov/clp/contract-laboratorv-program-national-functional-guidelines-data-review
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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
TIT 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. Initial Calibration Verification 28
V. Continuing Calibration Verification 31
VI. Blanks 34
VII. Deuterated Monitoring Compound 37
VIII. Matrix Spike/Matrix Spike Duplicate 40
IX. Internal Standard 42
X. Target Analyte Identification 45
XI. Target Analyte Quantitation and Reported Contract Required Quantitation Limit 47
XII. Tentatively Identified Compounds 48
XIII. System Performance 51
XIV. Performance Evaluation Sample 52
XV. Regional Quality Assurance and Quality Control 54
XVI. Overall Assessment of Data 55
LOW/MEDIUM VOLATILE DATA REVIEW 57
I. Preservation and Holding Times 59
II. Gas Chromatograph/Mass Spectrometer Instrument Performance Check 63
TIT Initial Calibration 71
IV. Initial Calibration Verification 76
V. Continuing Calibration Verification 79
VI. Blanks 82
VII. Deuterated Monitoring Compound 85
VIII. Matrix Spike/Matrix Spike Duplicate 88
IX. Internal Standard 90
X. Target Analyte Identification 93
XI. Target Analyte Quantitation and Reported Contract Required Quantitation Limit 95
XII. Tentatively Identified Compounds 97
XIII. System Performance 100
XIV. Performance Evaluation Sample 101
XV. Regional Quality Assurance and Quality Control 103
XVI. Overall Assessment of Data 104
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SEMIVOLATILE DATA REVIEW 105
I. Preservation and Holding Times 107
II. Gas Chromatograph/Mass Spectrometer Instrument Performance Check Ill
III. Initial Calibration 119
IV. Initial Calibration Verification 126
V. Continuing Calibration Verification 129
VI. Blanks 132
VII. Deuterated Monitoring Compound 135
VIII. Matrix Spike/Matrix Spike Duplicate 139
IX. Gel Permeation Chromatography Performance Check 141
X. Internal Standard 143
XI. Target Analyte Identification 146
XII. Target Analyte Quantitation and Reported Contract Required Quantitation Limit 148
XIII. Tentatively Identified Compounds 150
XIV. System Performance 153
XV. Performance Evaluation Sample 154
XVI. Regional Quality Assurance and Quality Control 156
XVII. Overall Assessment of Data 157
PESTICIDE DATA REVIEW 159
I. Preservation and Holding Times 161
II. Gas Chromatograph with Electron Capture Detector Instrument Performance Check 166
III. Initial Calibration 171
IV. Continuing Calibration Verification 177
V. Blanks 182
VI. Surrogate 185
VII. Matrix Spike/Matrix Spike Duplicate 187
VIII. Laboratory Control Sample 189
IX. Florisil Cartridge Performance Check 191
X. Gel Permeation Chromatography Performance Check 193
XI. Target Analyte Identification 196
XII. Gas Chromatograph/Mass Spectrometer Confirmation 198
XIII. Target Analyte Quantitation and Reported Contract Required Quantitation Limit 199
XIV. Performance Evaluation Sample 201
XV. Regional Quality Assurance and Quality Control 203
XVI. Overall Assessment of Data 204
AROCLOR DATA REVIEW 205
I. Preservation and Holding Times 207
II. Initial Calibration 210
III. Continuing Calibration Verification 214
IV. Blanks 218
V. Surrogate 221
VI. Matrix Spike/Matrix Spike Duplicate 224
VII. Laboratory Control Sample 226
VIII. Gel Permeation Chromatography Performance Check 228
IX. Target Analyte Identification 231
X. Gas Chromatograph/Mass Spectrometer Confirmation 233
XI. Target Analyte Quantitation and Reported Contract Required Quantitation Limit 234
XII. Performance Evaluation Sample 236
XIII. Regional Quality Assurance and Quality Control 238
XIV. Overall Assessment of Data 239
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, ICV, and CCV for Trace
Volatile Analysis 25
Table 5. Initial Calibration Actions for Trace Volatile Analysis 27
Table 6. ICV Actions for Trace Volatile Analysis 30
Table 7. CCV Actions for Trace Volatile Analysis 33
Table 8. Blank Actions for Trace Volatile Analysis 36
Table 9. Trace Volatile DMCs and Recovery Limits 37
Table 10. DMC Actions for Trace Volatile Analysis 38
Table 11. Trace Volatile DMCs and the Associated Target Analytes 39
Table 12. MS/MSD %R and RPD Limits for Trace Volatile Analysis 41
Table 13. MS/MSD Actions for Trace Volatile Analysis 41
Table 14. Internal Standard Actions for Trace Volatile Analysis 44
Table 15. PE Sample Actions for Trace Volatile Analysis 53
Table 16. Preservation and Holding Time Actions for Low/Medium Volatile Analysis 62
Table 17. Ion Abundance Criteria for BFB 69
Table 18. RRF, %RSD, and %D Acceptance Criteria in Initial Calibration, ICV, and CCV for
Low/Medium Volatile Analysis 73
Table 19. Initial Calibration Actions for Low/Medium Volatile Analysis 75
Table 20. ICV Actions for Low/Medium Volatile Analysis 78
Table 21. CCV Actions for Low/Medium Volatile Analysis 81
Table 22. Blank and TCLP/SPLP LEB Actions for Low/Medium Volatile Analysis 84
Table 23. Low/Medium Volatile DMC Recovery Limits 85
Table 24. DMC Actions for Low/Medium Volatile Analysis 86
Table 25. Low/Medium Volatile DMCs and the Associated Target Analytes 87
Table 26. MS/MSD %R and RPD Limits for Low/Medium Volatile Analysis 89
Table 27. MS/MSD Actions for Low/Medium Volatile Analysis 89
Table 28. Internal Standard Actions for Low/Medium Volatile Analysis 92
Table 29. Percent Solids Actions for Low/Medium Volatile Analysis for Non-Aqueous Samples 96
Table 30. PE Sample Actions for Low/Medium Volatile Analysis 102
Table 31. Preservation and Holding Time Actions for Semivolatile Analysis 109
Table 32. Holding Time Actions for Non-Aqueous Semivolatile TCLP/SPLP Sample Analysis 110
Table 33. Ion Abundance Criteria for DFTPP 117
Table 34. RRF, %RSD, and %D Acceptance Criteria in Initial Calibration, ICV, and CCV for
Semivolatile Analysis 121
Table 35. Initial Calibration Actions for Semivolatile Analysis 125
Table 36. ICV Actions for Semivolatile Analysis 128
Table 37. CCV Actions for Semivolatile Analysis 131
Table 38. Blank and TCLP/SPLP LEB Actions for Semivolatile Analysis 134
Table 39. Semivolatile DMC Recovery Limits 135
Table 40. DMC Actions for Semivolatile Analysis 137
Table 41. Semivolatile DMCs and the Associated Target Analytes 137
Table 42. Semivolatile SIM DMCs and the Associated Target Analytes 138
Table 43. MS/MSD %R and RPD Limits for Semivolatile Analysis 140
Table 44. MS/MSD Actions for Semivolatile Analysis 140
Table 45. Internal Standard Actions for Semivolatile Analysis 145
Table 46. Percent Solids Actions for Semivolatile Analysis for Non-Aqueous Samples 149
Table 47. PE Sample Actions for Semivolatile Analysis 155
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Table 48. Preservation and Holding Time Actions for Pesticide Analysis 164
Table 49. Holding Time Actions for Non-Aqueous Pesticide TCLP/SPLP Sample Analysis 165
Table 50. Resolution Check Mixture 166
Table 51. Performance Evaluation Mixture (PEM) 166
Table 52. Individual Standard Mixtures A and B 167
Table 53. Individual Standard Mixture C 168
Table 54. GC/ECD Instrument Performance Check Actions 170
Table 55. Concentration Levels of Calibration Standards 171
Table 56. Initial Calibration Sequence 1 173
Table 57. Initial Calibration Sequence 2 173
Table 58. Initial Calibration Action for Pesticide Analysis 176
Table 59. CCV Actions for Pesticide Analysis 181
Table 60. Blank and TCLP/SPLP LEB Actions for Pesticide Analysis 184
Table 61. Surrogate Actions for Pesticide Analysis 186
Table 62. MS/MSD %R and RPD Limits for Pesticide Analysis 188
Table 63. MS/MSD Actions for Pesticide Analysis 188
Table 64. LCS %R Limits for Pesticide Analysis 189
Table 65. LCS Actions for Pesticide Analysis 190
Table 66. Florisil Cartridge Performance Check Actions 192
Table 67. GPC Performance Check Actions for Pesticide Analysis 195
Table 68. GC/MS Confirmation Actions 198
Table 69. Percent Solids Actions for Pesticide Analysis for Non-Aqueous Samples 200
Table 70. PE Sample Actions for Pesticide Analysis 202
Table 71. Preservation and Holding Time Actions for Aroclor Analysis 209
Table 72. Initial Calibration Sequence 211
Table 73. Initial Calibration Action for Aroclor Analysis 213
Table 74. CCV Actions for Aroclor Analysis 217
Table 15. Blank Actions for Aroclor Analysis 220
Table 76. Surrogate Actions for Aroclor Analysis 223
Table 77. MS/MSD %R and RPD Limits for Aroclor Analysis 225
Table 78. MS/MSD Actions for Aroclor Analysis 225
Table 79. LCS %R Limits for Aroclor Analysis 226
Table 80. LCS Actions for Aroclor Analysis 227
Table 81. GPC Performance Check Actions for Aroclor Analysis 230
Table 82. GC/MS Confirmation Actions 233
Table 83. Percent Solids Actions for Aroclor Analysis for Non-Aqueous Samples 235
Table 84. PE Sample Actions for Aroclor Analysis 237
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ACRONYMS AND ABBREVIATIONS
I. Terminology
The following acronyms and abbreviations may be found throughout this document. For definitions,
see Appendix A: Glossary at the end of the document.
ARO Aroclors
BFB Bromofluorobenzene
CAS Chemical Abstracts Service
CCS Contract Compliance Screening
CCV Continuing Calibration Verification
CF Calibration Factor
CF Mean Calibration Factor
CLP Contract Laboratory Program
COR Contracting Officer's Representative
CRQL Contract Required Quantitation Limit
CS3 Mid-point Calibration Standard
CSF Complete SDG File
DCB Decachlorobiphenyl
DFTPP Decafluorotriphenylphosphine
DMC Deuterated Monitoring Compound
DQA Data Quality Assessment
DQO Data Quality Objective
EDM EXES Data Manager
EPA United States Environmental Protection Agency
EXES Electronic Data Exchange and Evaluation System
GC Gas Chromatograph or Gas Chromatography
GC/ECD Gas Chromatograph/Electron Capture Detector
GC/MS Gas Chromatograph/Mass Spectrometer or Gas Chromatography/Mass
Spectrometry
GPC Gel Permeation Chromatography
ICAL Initial Calibration
ICV Initial Calibration Verification
INDA Individual Standard Mixture A
INDB Individual Standard Mixture B
INDC Individual Standard Mixture C
IUPAC International Union of Pure and Applied Chemistry
LCS Laboratory Control Sample
LEB Leachate Extraction Blank
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MS
Mass Spectrometer or Mass Spectrometry
MS
Matrix Spike
MSD
Matrix Spike Duplicate
NFG
National Functional Guidelines
NIH
National Institutes of Health
NIST
National Institute of Standards and Technology
OSRTI
Office of Superfund Remediation and Technology Innovation
%Breakdown
Percent Breakdown
%D
Percent Difference
%R
Percent Recovery
%Resolution
Percent Resolution
%RSD
Percent Relative Standard Deviation
%Solids
Percent Solids
PAH
Polycyclic Aromatic Hydrocarbon
PCP
Pentachlorophenol
PCBs
Polychlorinated Biphenyls
PE
Performance Evaluation
PEM
Performance Evaluation Mixture
PEST
Pesticides
P/T
Purge-and-trap
QA
Quality Assurance
QAPP
Quality Assurance Project Plan
QC
Quality Control
RESC
Resolution Check Mixture
RFQ
Request for Quote
RIC
Reconstructed Ion Chromatogram
RPD
Relative Percent Difference
RRF
Relative Response Factor
RRF
Mean Relative Response Factor
RRT
Relative Retention Time
RT
Retention Time
RT
Mean Retention Time
SAP
Sampling and Analysis Plan
SDG
Sample Delivery Group
SEDD
Staged Electronic Data Deliverable
SIM
Selected Ion Monitoring
SMO
Sample Management Office
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SOP
Standard Operating Procedure
sow
Statement of Work
SPLP
Synthetic Precipitation Leaching Procedure
SVOA
Semi volatile s
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
VOA
Volatile s
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 Organic Superfund Methods (Multi-Media,
Multi-Concentration) SOM02.4. The SOW includes analytical methods for Trace Volatiles (Trace
VOA), Low-Medium Volatiles (Low/Med VOA), Semivolatiles (SVOA), Pesticides (PEST), and
Aroclors (ARO).
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, QC audit samples, 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
are affected by site conditions (e.g., sample matrix effects) 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 SOM02.4. 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 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 SOM02.4, although the general types
of QC checks, the evaluation procedures, and the decisions made after consideration of the evaluation
criteria may be applicable to data from any similar method.
While this document is a valuable aid in the 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 the 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 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 EPA's Superfund
Analytical Services and Contract Laboratory Program website at https://www.epa.gov/clp.
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Organic Data Review General
PART A: GENERAL DATA REVIEW
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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) Record, 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 reanalysis; 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 discussion of sample
logistics, preparation, and/or analysis issues between the laboratory, the Contract Laboratory Program
(CLP) Sample Management Office (SMO), and the EPA Region.
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General
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
usability of the analytical data. The reviewer should contact the appropriate EPA Regional CLP
Contracting Officer's Representative (EPA Regional CLP COR) 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 SOM02.4, and 2) automated data validation based
on the criteria in the EPA CLP National Functional Guidelines for Organic Superfund 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 noncompliant data identified in the report. The automated data validation results are
summarized in criteria-based National Functional Guidelines (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 Superfund Analytical Services SMO Portal and may use them in determining
data usability.
For access to the Superfund Analytical Services SMO Portal, refer to the following EPA Superfund
Analytical Services and Contract Laboratory Program web page to contact the EPA Regional CLP
COR from the EPA Region where the data review is being performed and obtain the necessary
username and password information:
https://www.epa.gov/clp/forms/contact-us-about-superfund-analvtical-services-or-contract-laboratorv
-program#tab-3
For concerns or questions regarding the data package, contact the EPA Regional CLP COR from the
EPA 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
Definition
U
The analyte was analyzed for, but was not detected above the level of the reported sample
quantitation limit.
J
The result is an estimated quantity. The associated numerical value is the approximate
concentration of the analyte in the sample.
J+
The result is an estimated quantity, but the result may be biased high.
J-
The result is an estimated quantity, but the result may be biased low.
NJ
The analyte has been "tentatively identified" or "presumptively" as present and the
associated numerical value is the estimated concentration in the sample.
UJ
The analyte was analyzed for, but was not detected. The reported quantitation limit is
approximate and may be inaccurate or imprecise.
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General
Data
Qualifier
Definition
R
The data are unusable. The sample results are rejected due to serious deficiencies in
meeting QC criteria. The analyte may or may not be present in the sample.
C
The target Pesticide or Aroclor analyte identification has been confirmed by Gas
Chromatography/Mass Spectrometry (GC/MS).
X
The target Pesticide or Aroclor analyte identification was not confirmed when GC/MS
analysis was performed.
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 EPA 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),
should be provided together with the laboratory data to the appropriate data recipient(s). A copy of the
Data Review Narrative should also be submitted to the EPA Regional CLP COR assigned oversight
responsibility for the Contractor laboratory.
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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. Initial Calibration Verification 28
V. Continuing Calibration Verification 31
VI. Blanks 34
VII. Deuterated Monitoring Compound 37
VIII. Matrix Spike/Matrix Spike Duplicate 40
IX. Internal Standard 42
X. Target Analyte Identification 45
XI. Target Analyte Quantitation and Reported Contract Required Quantitation Limit 47
XII. Tentatively Identified Compounds 48
XIII. System Performance 51
XIV. Performance Evaluation Sample 52
XV. Regional Quality Assurance and Quality Control 54
XVI. Overall Assessment of Data 55
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Trace VOA
I. Preservation and Holding Times
A. Review Items
Form 1A-OR, Form 1B-OR, Traffic Report/Chain of Custody (TR/COC) Record 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. (SOW SOM02.4 - Exhibit B, Section 3.4;
Exhibit D/Introduction, Section 5.0; Exhibit D/General, Sections 8.0 and 10.1.2.1; and Exhibit D/Trace
VOA, Section 8.0)
B. Objective
The objective is to determine the validity of the analytical results based on the sample conditions 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, Form 1B-OR, and the raw data are identical.
3. Establish technical holding times by comparing the sample collection dates on the TR/COC Record
documentation with the dates of analysis on Form 1A-OR, 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 listed in
SOW SOM02.4 Exhibit C, Table 1 - Trace Volatiles Target Analyte List and Contract
Required Quantitation Limits. 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 but < 10°C, use professional
judgment to qualify detects and non-detects.
2. 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 (J) and non-detects as estimated
(UJ).
3. If a discrepancy is found between the sample analysis date on Form 1A-OR, Form 1B-OR, and the
raw data, perform a more comprehensive review to determine the correct date to be used for
establishing the holding time.
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Trace VOA
4. 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.
5. If samples are not properly preserved and are analyzed outside of the technical holding time of 7
days, qualify detects as estimated (J) and non-detects as unusable (R).
6. If samples are properly preserved and are analyzed within the technical holding time of 14 days,
detects and non-detects should not be qualified.
7. 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).
8. When the holding times are exceeded, annotate in the Data Review Narrative any possible
consequences for the analytical results.
9. If holding times are grossly exceeded, qualify detects as estimated (J) and non-detects as unusable
(R). Note this for United States Environmental Protection Agency Regional Contract Laboratory
Program Contracting Officer's Representative (EPA Regional CLP COR) action. Annotate the
effect of the holding time exceedance on the resulting data in the Data Review Narrative, whenever
possible.
Table 2. Preservation and Holding Time Actions for Trace Volatile Analysis
Criteria
Action
Detect
Non-detect
Sample temperature > 6°C but < 10°C upon receipt
at the laboratory
Use professional
judgment
Use professional
judgment
Sample temperature > 10°C upon receipt at the
laboratory
Use professional
judgment
J*
Use professional
judgment
UJ
Sample not preserved but analyzed within the 7-day
technical holding time
No qualification
No qualification
Samples not preserved and analyzed outside the
7-day technical holding time
J*
R
Sample properly preserved and analyzed within the
14-day technical holding time
No qualification
No qualification
Sample properly preserved but analyzed outside the
14-day technical holding time
J*
R
Holding time grossly exceeded
J*
R
* The true direction of any bias may be unknown in this case. 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).
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Trace VOA
II. Gas Chromatograph/Mass Spectrometer Instrument Performance Check
A. Review Items
Form 5-OR, bromofluorobenzene (BFB) mass spectra, and mass listing. (SOW SOM02.4 - Exhibit B,
Section 3.4 and Exhibit D/Trace VOA, Section 9.2)
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. 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 the injection of BFB;
however, 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.
• Initial Calibration Verification
(ICV) meets ICV 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.
• ICV meets ICV 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:
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 2/
Beginning of 12-hour clock
for Analytical Sequence 3
Ohr
12 hr
24 hr
BFB
Initial Calibration 0.5
Initial Calibration 1.0
Initial Calibration 5.0
Initial Calibration 10
Initial Calibration 20
ICV
Method Blank
Subsequent Samples
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:
Time Material Injected
Analytical Sequence #
Start of 12-hour clock for
Analytical Sequence 1
Ohr
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
25 hr
BFB
Initial Calibration 0.5
Initial Calibration 1.0
Initial Calibration 5.0
Initial Calibration 10
Initial Calibration 20
ICV
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
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
End of 12-hour clock for
Analytical Sequence 1/
Beginning of 12-hour clock
for Analytical Sequence 2
Ohr
12 hr
BFB
CCV A (meets opening CCV
criteria)
Method Blank
Subsequent Samples
CCV B (meets opening CCV
criteria)
Method Blank
Subsequent Samples
1/2
2
2
2
2
2
End of 12-hour clock for
Analytical Sequence 2/
Beginning of 12-hour clock
for Analytical Sequence 3
24 hr
CCV C (meets opening CCV
criteria)
2/3
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Example 4:
Example 4:
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
End of 12-hour clock for
Analytical Sequence 1
Beginning of 12-hour clock
for Analytical Sequence 2
CCV B (meets closing CCV
12 hr criteria; fails opening CCV
criteria)
13 hr BFB
CCV C (meets opening CCV
criteria)
Method Blank
Subsequent Samples
2
2
2
2
2
End of 12-hour clock for
Analytical Sequence 2/
Beginning of 12-hour clock
for Analytical Sequence 3
25 hr
CCV D (meets opening CCV
criteria)
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
Mass
Ion Abundance Criteria
50
15.0-40.0% of mass 95
75
30.0 - 80.0% of mass 95
95
Base peak, 100% relative abundance
96
5.0 - 9.0% of mass 95*
173
Less than 2.0% of mass 174
174
50.0%- 120% of mass 95
175
5.0 -9.0% of mass 174
176
95.0 - 101% of mass 174
177
5.0 -9.0% of mass 176
* All ion abundances must be normalized to 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 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 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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b. Background subtraction must be accomplished using a single scan acquired within 20 scans of
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 CLP, information regarding noncompliant 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,
qualify detects and non-detects in the associated samples as unusable (R). The EPA Regional CLP
COR should be contacted to arrange for 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 action is required.
3. If the laboratory failed to provide the correct forms, or if significant transcription or calculation
errors are found, notify the EPA Regional CLP COR, 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 EPA Regional CLP COR.
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 noncompliant 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 EPA Regional CLP COR action.
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III. Initial Calibration
A. Review Items
Form 6A-OR, quantitation reports, and chromatograms. (SOW SOM02.4 - Exhibit B, Section 3.4 and
Exhibit D/Trace VOA, Sections 7.2.2.1 and 9.3)
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 the ICV, 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, and 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 Solicitation"
of a Modified Analysis may impact some of the preceding evaluation criteria. A copy of
this document should be present in the CSF, when applicable.
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 %RSDs 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.
NOTE: For data obtained from the CLP, information regarding noncompliant ICALs 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, use professional judgment to
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 %RSDs, 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 value in Table 4 for any target analyte, 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
necessary. The following guidelines are recommended:
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.
10. If the laboratory failed to provide adequate calibration information, notify the EPA Regional CLP
COR, 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 EPA Regional CLP COR action.
Table 4. RRF, %RSD, and %D Acceptance Criteria in Initial Calibration, ICV, and CCV for
Trace Volatile Analysis
Analyte
Minimum
RRF
Maximum
%RSD
ICV/Opening
CCV
Maximum
%D'
Closing
CCV
Maximum
%D
Dichlorodifluoromethane
0.010
30.0
±40.0
±50.0
Chloromethane
0.010
30.0
±30.0
±50.0
Vinyl chloride
0.010
30.0
±30.0
±50.0
Bromomethane
0.010
40.0
±30.0
±50.0
Chloroethane
0.010
30.0
±30.0
±50.0
Trichlorofluoromethane
0.010
30.0
±30.0
±50.0
1,1 -Dichloroethene
0.020
30.0
±20.0
±25.0
1,1,2-T richloro-1,2,2-trifluoroethane
0.010
30.0
±30.0
±50.0
Acetone
0.010
40.0
±40.0
±50.0
Carbon disulfide
0.010
20.0
±25.0
±25.0
Methyl acetate
0.010
40.0
±40.0
±50.0
Methylene chloride
0.010
40.0
±30.0
±50.0
trans-1,2-Dichloroethene
0.070
20.0
±20.0
±25.0
Methyl tert-butyl ether
0.010
30.0
±30.0
±50.0
1,1 -Dichloroethane
0.100
20.0
±20.0
±25.0
cis-l,2-Dichloroethene
0.100
20.0
±20.0
±25.0
2-Butanone
0.010
40.0
±40.0
±50.0
Bromochloromethane
0.020
20.0
±20.0
±25.0
Chloroform
0.040
20.0
±20.0
±25.0
1,1,1 -T richloroethane
0.050
30.0
±20.0
±25.0
Cyclohexane
0.100
30.0
±25.0
±50.0
Carbon tetrachloride
0.020
20.0
±25.0
±50.0
Benzene
0.300
20.0
±20.0
±25.0
1,2-Dichloroethane
0.010
20.0
±25.0
±50.0
Trichloroethene
0.100
20.0
±20.0
±25.0
Methylcyclohexane
0.200
30.0
±25.0
±50.0
1,2-Dichloropropane
0.100
20.0
±20.0
±25.0
Bromodichloromethane
0.090
20.0
±20.0
±25.0
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Analyte
Minimum
RRF
Maximum
%RSD
ICV/Opening
CCV
Maximum
%D'
Closing
CCV
Maximum
%D
cis-1,3 -Dichloropropene
0.100
20.0
±20.0
±25.0
4-Methyl -2 -pentanone
0.010
30.0
±30.0
±50.0
Toluene
0.400
20.0
±20.0
±25.0
trans -1,3 -Dichloropropene
0.010
30.0
±20.0
±25.0
1,1,2-T richloroethane
0.040
20.0
±20.0
±25.0
T etrachloroethene
0.100
20.0
±20.0
±25.0
2-Hexanone
0.010
40.0
±40.0
±50.0
Dibromochloromethane
0.050
20.0
±20.0
±25.0
1,2-Dibromoethane
0.010
20.0
±20.0
±25.0
Chlorobenzene
0.400
20.0
±20.0
±25.0
Ethylbenzene
0.500
20.0
±20.0
±25.0
m,p-Xylene
0.200
20.0
±20.0
±25.0
o-Xylene
0.300
30.0
±20.0
±25.0
Styrene
0.200
30.0
±20.0
±25.0
Bromoform
0.010
30.0
±30.0
±50.0
Isopropylbenzene
0.700
30.0
±25.0
±25.0
1,1,2,2-Tetrachloroethane
0.050
20.0
±25.0
±25.0
1,3 -Dichlorobenzene
0.500
20.0
±20.0
±25.0
1,4-Dichlorobenzene
0.700
20.0
±20.0
±25.0
1,2-Dichlorobenzene
0.400
20.0
±20.0
±25.0
1,2-Dibromo-3 -chloropropane
0.010
40.0
±40.0
±50.0
1,2,4-Trichlorobenzene
0.300
30.0
±30.0
±50.0
1,2,3 -T richlorobenzene
0.200
30.0
±40.0
±50.0
Deuterated Monitoring Compounds
Vinyl chloride-d3
0.010
30.0
±30.0
±50.0
Chloroethane-ds
0.010
30.0
±30.0
±50.0
1,1 -Dichloroethene-d2
0.010
30.0
±25.0
±25.0
2-Butanone-ds
0.010
40.0
±40.0
±50.0
Chloroform-d
0.010
20.0
±20.0
±25.0
1,2-Dichloroethane-d4
0.010
20.0
±25.0
±25.0
Benzene-d6
0.030
20.0
±20.0
±25.0
1,2-Dichloropropane-d6
0.100
20.0
±20.0
±25.0
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Analyte
Minimum
RRF
Maximum
%RSD
ICV/Opening
CCV
Maximum
%D'
Closing
CCV
Maximum
%D
Toluene-ds
0.200
20.0
±20.0
±25.0
trans -1,3 -Dichloropropene-cU
0.010
30.0
±25.0
±25.0
2-Hexanone-d5
0.010
40.0
±40.0
±50.0
1,1,2,2- Tetrachloroethane-d2
0.010
20.0
±25.0
±25.0
1,2-Dichlorobenzene-d4
0.060
20.0
±20.0
±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
Action
Detect
Non-detect
Initial Calibration not performed at the
specified frequency and sequence
Use professional
judgment
R
Use professional
judgment
R
Initial Calibration not performed at the
specified concentrations
J
UJ
RRF < Minimum RRF in Table 4 for
target analyte
Use professional
judgment
J+ or R
R
RRF > Minimum RRF in Table 4 for
target analyte
No qualification
No qualification
%RSD > Maximum %RSD in Table 4
for target analyte
J
Use professional
judgment
%RSD < Maximum %RSD in Table 4
for target analyte
No qualification
No qualification
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IV. Initial Calibration Verification
A. Review Items
Form 7A-OR, quantitation reports, and chromatograms. (SOW SOM02.4 - Exhibit B, Section 3.4 and
Exhibit D/Trace VOA, Sections 7.2.2.2 and 9.4)
B. Objective
The objective is to ensure that the instrument is calibrated accurately to produce acceptable qualitative
and quantitative data throughout each analytical sequence by the use of a second-source check
standard.
C. Criteria
1. The accuracy of the calibration for each GC/MS system used for analysis must be verified at the
frequency of one ICV standard analysis per initial calibration analytical sequence. The ICV is
analyzed after the last ICAL standard analysis and prior to a blank, sample, or an applicable CCV
analysis.
2. The ICV standard must contain all required target analytes, from an alternate source or a different
lot than that used for the ICAL standards and the DMCs, at or near the mid-point concentration
(CS3) of the ICAL.
3. For an ICV, 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 ICV RRF must be within the
ICV/Opening CCV Maximum %D limits in Table 4 for each target analyte and DMC.
D. Evaluation
1. Verify that the ICV standard is analyzed at the specified frequency and sequence, and that it is
associated with 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 concentrations of the target analytes and the DMCs in the ICV are at or near the
mid-point standard CS3 from the ICAL.
3. Verify that the RRF and %D for each target analyte and DMC are reported on Form 7A-OR.
Recalculate the 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. Verify that the RRFs for each target analyte and DMC in the ICV are > Minimum RRF values in
Table 4.
5. Verify that the %Ds are within the ICV/Opening CCV Maximum %D limits in Table 4 for each
target analyte and DMC.
NOTE: For data obtained from the CLP, information regarding a noncompliant ICV can be
obtained from the NFG reports and may be used as part of the evaluation process.
E. Action
1. If the ICV is not performed at the specified frequency, use professional judgment to qualify detects
and non-detects. Contact the EPA Regional CLP COR 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 quality of analyte peak
shapes and mass spectral matches, the 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.
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2. If the ICV 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. If the RRF in an ICV is < 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).
a. Take special note of any extreme deviation in the RRF and evaluate RT data, peak shapes, and
areas of the target analytes and associated internal standards for inconsistencies that may
indicate a chromatographic co-elution. If this is suspected, the contaminant may also be
present in samples and blanks. Also review the documentation of the preparation of the ICV
standard. Use professional judgment to qualify affected data appropriately.
5. If the RRF in an ICV is > Minimum RRF value in Table 4 for any target analyte, detects and
non-detects should not be qualified.
6. If the %D in an ICV is outside the ICV/Opening CCV Maximum %D limits in Table 4 for any
target analyte, qualify detects as estimated (J) and non-detects as estimated (UJ).
7. If the %D in an ICV is within the inclusive range of the ICV/Opening CCV Maximum %D limits in
Table 4 for any target analyte, detects and non-detects should not be qualified.
8. No qualification of the data is necessary based on the 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.
9. If the laboratory has failed to provide adequate calibration information, contact the EPA Regional
CLP COR, who may contact the laboratory to request the necessary information. If the information
is not available, use professional judgment to assess the data. Refer to E.l, above, for additional
steps.
10. Note the potential effects on the data due to ICV criteria exceedance in the Data Review Narrative.
11. If the ICV criteria are grossly exceeded, note this for EPA Regional CLP COR action.
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Table 6. ICV Actions for Trace Volatile Analysis
Criteria for ICV
Action
Detect
Non-detect
ICV not performed at the specified
frequency and sequence
Use professional
judgment
Use professional
judgment
ICV not performed at the specified
concentration
Use professional
judgment
Use professional
judgment
RRF < Minimum RRF in Table 4
for target analyte
Use professional
judgment
J or R
R
RRF > Minimum RRF in Table 4
for target analyte
No qualification
No qualification
%D outside the ICV/Opening
CCV Maximum %D limits in
Table 4 for target analyte
J
UJ
%D within the inclusive
ICV/Opening CCV Maximum
%D limits in Table 4 for target
analyte
No qualification
No qualification
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V. Continuing Calibration Verification
A. Review Items
Form 7A-OR, quantitation reports, and chromatograms. (SOW SOM02.4 - Exhibit B, Section 3.4 and
Exhibit D/Trace VOA, Sections 7.2.2.1 and 9.5)
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 or near the mid-point
concentration (CS3) 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 %D between the ICAL RRF and the opening CCV RRF must be within the ICV/Opening CCV
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 the Closing
CCV 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 it is associated
with 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 CS3 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 the 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 each target analyte and DMC are
> Minimum RRF values in Table 4.
5. For an opening CCV, verify that the %Ds are within the ICV/Opening CCV Maximum %D limits
in Table 4 for each target analyte and DMC.
6. For a closing CCV, verify that the %Ds are within the Closing CCV Maximum %D limits in Table
4 for each target analyte and DMC.
NOTE: For data obtained from the CLP, information regarding noncompliant CCVs 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 CCV is not performed at the specified frequency, qualify detects and non-detects as unusable
(R). Contact the EPA Regional CLP COR 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 quality of analyte peak shapes and
mass spectral matches, the stability of internal standard 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 < 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).
a. Take special note of any extreme deviation in the RRF and evaluate RT data, peak shapes, and
areas of the target analytes and associated internal standards for inconsistencies that may
indicate a chromatographic co-elution. If this is suspected, the contaminant may also be
present in samples and blanks. Also review the documentation of the preparation of the CCV
standard. Use professional judgment to qualify affected data appropriately.
5. For an opening or a closing CCV, if the RRF is > Minimum RRF value in Table 4 for any target
analyte, detects and non-detects should not be qualified.
6. For an opening CCV, if the %D is outside the ICV/Opening CCV 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 CCV 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 ICV/Opening CCV 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 CCV 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 based on the 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 EPA Regional
CLP COR, who may contact the laboratory to request the necessary information. If the information
is not available, use professional judgment to assess the data. Refer to E. 1, above, for additional
steps.
12. Note the potential effects on the data due to CCV criteria exceedance in the Data Review Narrative.
13. If the CCV criteria are grossly exceeded, note this for EPA Regional CLP COR action.
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Table 7. CCV Actions for Trace Volatile Analysis
Criteria for Opening CCV
Criteria for Closing CCV
Action
Detect
Non-detect
CCV not performed at the
specified frequency and
sequence
CCV not performed at the
specified frequency
Use professional
judgment
J or R
Use professional
judgment
UJ orR
CCV not performed at the
specified concentration
CCV not performed at the
specified concentration
Use professional
judgment
Use professional
judgment
RRF < Minimum RRF in
Table 4 for target analyte
RRF < Minimum RRF in
Table 4 for target analyte
Use professional
judgment
J or R
R
RRF > Minimum RRF in
Table 4 for target analyte
RRF > Minimum RRF in
Table 4 for target analyte
No qualification
No qualification
%D outside the ICV/Opening
CCV Maximum %D limits in
Table 4 for target analyte
%D outside the Closing CCV
Maximum %D limits in
Table 4 for target analyte
J
UJ
%D within the inclusive
ICV/Opening CCV Maximum
%D limits in Table 4 for target
analyte
%D within the inclusive
Closing CCV Maximum %D
limits in Table 4 for target
analyte
No qualification
No qualification
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VI. Blanks
A. Review Items
Form 1A-OR, Form 1B-OR, Form 4-OR, chromatograms, and quantitation reports. (SOW SOM02.4 -
Exhibit B, Section 3.4 and Exhibit D/Trace VOA, Section 12.1)
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, the ICV, or the opening 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 an SDG, and stored with the samples
until analysis. The storage blank must be analyzed once per SDG after all sample analyses within
an 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 blank must not exceed its Contract Required
Quantitation Limit (CRQL) (2x CRQLs for Methylene chloride, Acetone, and 2-Butanone). TIC
concentration in any blank 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. Data concerning the field blanks are not evaluated as part of the Contract Compliance Screening
(CCS) process. 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 CCS
process. Information regarding the noncompliant 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 EPA
Regional CLP COR 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 EPA 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 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 (> 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 but
< Blank Results at sample results and qualify as non-detect (U) or as unusable (R). Use
professional judgment to qualify sample results that are > CRQLs and > Blank Results or > 2x
result in method blank for Methylene chloride, Acetone, and 2-Butanone.
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) concentrations) 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 EPA
Regional CLP COR 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 8 should
apply.
9. If gross contamination exists with blank results that are > ICAL CS5 concentrations, qualify detects
as unusable (R). If the contamination is suspected of having an effect on the sample results, note it
for EPA Regional CLP COR action.
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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 8. Blank Actions for Trace Volatile Analysis
Blank Type
Blank Result
Sample Result
Action
Detect
Non-detect
No qualification
< CRQL
Report at CRQL and qualify as
non-detect (U)
< CRQL
> CRQL or > 2x Blank Result
for Methylene chloride,
Acetone, and 2-Butanone
Use professional judgment
Method,
< CRQL
Report at CRQL and qualify as
non-detect (U)
Storage,
Field, Trip,
Instrument*
> CRQL
> CRQL but < Blank Result
Report at sample result and
qualify as non-detect (U) or
unusable (R)
> CRQL and > Blank Result or
> 2x Blank Result for
Methylene chloride, Acetone,
and 2-Butanone
Use professional judgment
Gross
contamination
Detect
Report at sample result and
qualify as unusable (R)
TIC > 0.5 jig/L
Detect
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 TICs concentration exceeding 100 (ig/L.
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VII. Deuterated Monitoring Compound
A. Review Items
Form 2A-OR, Form 2B-OR quantitation reports, and chromatograms. (SOW SOM02.4 - Exhibit B,
Section 3.4 and Exhibit D/Trace VOA, Sections 7.2.2.4 and 11.2.5)
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 9, 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 9.
Table 9. Trace Volatile DMCs and Recovery Limits
DMC
Recovery Limits (%)
Vinyl chloride-d3
40 - 130
Chloroethane-ds
65 - 130
1,1 -Dichloroethene-d2
60 - 125
2-Butanone-ds
40 - 130
Chloroform-d
70 - 125
1,2-Dichloroethane-d4
70 - 130
Benzene-d6
70 - 125
1,2-Dichloropropane-d6
60 - 140
Toluene-ds
70-130
trans-1,3 -Dichloropropene-d4
55 - 130
2-Hexanone-ds
45 - 130
1,1,2,2-T etrachloroethane-d2
65 - 120
1,2-Dichlorobenzene-d4
80 - 120
NOTE: The recovery limits for any of the compounds listed in Table 9 may be expanded at any
time during the period of performance if the EPA determines that the limits are too
restrictive.
D. Evaluation
1. Check the 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 time s.
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 noncompliant 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
EPA Regional CLP COR 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 9) in samples, qualify the associated target analytes
listed in Table 11 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 < 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 9) in a blank, special consideration should be taken to
evaluate 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 EPA Regional CLP COR action.
Table 10. DMC Actions for Trace Volatile Analysis
Criteria
Action
Detect
Non-detect
%R< 10%
J-
R
10% < %R < Lower Acceptance Limit
J-
UJ
Lower Acceptance Limit < %R < Upper Acceptance
Limit
No qualification
No qualification
%R > Upper Acceptance Limit
J+
No qualification
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Table 11. Trace Volatile DMCs and the Associated Target Analytes
Vinyl chloride-d3 (DMC-1)
Chloroethane-ds (DMC-2)
l,l-Dichloroethene-d2 (DMC-3)
Vinyl chloride
Dichlorodifluoromethane
Chloromethane
Bromomethane
Chloroethane
Carbon disulfide
trans-1,2-Dichloroethene
cis-l,2-Dichloroethene
1,1 -Dichloroethene
2-Butanone-ds (DMC-4)
Chloroform-d (DMC-5)
l,2-Dichloroethane-d4 (DMC-6)
Acetone
2-Butanone
1,1 -Dichloroethane
Bromochloromethane
Chloroform
Dibromochloromethane
Bromoform
Trichlorofluoromethane
1,1,2-T richloro-1,2,2-trifluoroethane
Methyl acetate
Methylene chloride
Methyl-tert-butyl ether
1,1,1 -T richloroethane
Carbon tetrachloride
1,2-Dibromoethane
1,2-Dichloroethane
Benzene-d6 (DMC-7)
l,2-Dichloropropane-d6
(DMC-8)
Toluene-ds (DMC-9)
Benzene
Cyclohexane
Methylcyclohexane
1,2-Dichloropropane
Bromodichloromethane
Trichloroethene
Toluene
T etrachloroethene
Ethylbenzene
o-Xylene
m,p-Xylene
Styrene
Isopropylbenzene
trans-l,3-Dichloropropene-d4
(DMC-10)
2-Hexanone-ds (DMC-11)
l,l,2,2-Tetrachloroethane-d2
(DMC-12)
cis-1,3 -Dichloropropene
trans -1,3 -Dichloropropene
1,1,2-Trichloroethane
4-Methyl-2-pentanone
2-Hexanone
1,1,2,2,-T etrachloroethane
1,2-Dibromo -3 -chloropropane
l,2-Dichlorobenzene-d4
(DMC-13)
Chlorobenzene
1,3 -Dichlorobenzene
1,4-Dichlorobenzene
1,2-Dichlorobenzene
1,2,4-Trichlorobenzene
1,2,3 -Trichlorobenzene
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VIII. Matrix Spike/Matrix Spike Duplicate
A. Review Items
SDG Cover Page, Form 3A-OR, chromatograms, and quantitation reports. (SOW SOM02.4 - Exhibit
B, Section 3.4 and Exhibit D/Trace VOA, Sections 7.2.2.5 and 12.2)
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 samples should be analyzed per matrix or per SDG.
NOTE: Data for MS and MSDs will not be present unless requested by the EPA 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 12.
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 3A-OR and verify that they are within the limits listed
in Table 12.
NOTE: For data obtained from the CLP, the preceding criteria, including the requested MS/MSD
spiking analytes and spiking levels specified in Exhibit D - Trace Concentrations of
Volatile Organic Compounds Analysis, Section 7.2.2.5, of the SOW, are evaluated as part
of the CCS process. Information regarding the noncompliant 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 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 EPA
Regional CLP COR action. It is not likely that data qualification will be warranted if 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 was used for the MS/MSD analysis, note this for EPA Regional CLP
COR 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 the 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 12, 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:
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If the MS/MSD %R is < 20%, qualify detects as estimated (J) and non-detects as unusable (R).
If the MS/MSD %R is > 20% and < lower acceptance limit, qualify detects as estimated (J) and
non-detects as estimated (UJ).
If the MS/MSD %R or RPD is > lower acceptance limit and < upper acceptance limit, detects
and non-detects should not be qualified.
If the MS/MSD %R or RPD is > upper acceptance limit, qualify detects as estimated (J).
Non-detects should not be qualified.
Table 12. MS/MSD %R and RPD Limits for Trace Volatile Analysis
Analyte
%R
RPD
1,1 -Dichloroethene
61 - 145
0-14
Benzene
76 - 127
0-11
Trichloroethene
71 - 120
0-14
Toluene
76 - 125
0-13
Chlorobenzene
75 - 130
0-13
Table 13. MS/MSD Actions for Trace Volatile Analysis
Criteria
Action
Detect
Non-detect
%R < 20%
J
R
20% < %R< Lower Acceptance Limit
J
UJ
Lower Acceptance Limit < %R or RPD < Upper
Acceptance Limit
No qualification
No qualification
%R or RPD > Upper Acceptance Limit
J
No qualification
a.
b.
c.
d.
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IX. Internal Standard
A. Review Items
Form 8A-OR, quantitation reports, and chromatograms. (SOW SOM02.4 - Exhibit B, Section 3.4 and
Exhibit D/Trace VOA, Sections 7.2.2.6, 11.3.5, and 11.3.6)
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 compound from the
associated opening CCV or the mid-point standard CS3 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 CS3 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 RT and area
response of each internal standard compound in a sample or blank are reported on 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 noncompliant internal standard area response or RT
can be obtained from the NFG reports and may be used as part of the evaluation process.
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E. Action
NOTE: Apply the action to the target analytes in the samples or blanks that are associated to the
noncompliant internal standard compound in Table 14. The internal standard and the
associated target analytes are in Exhibit D - Trace Concentrations of Volatile Organic
Compounds Analysis, Table 9, of the SOW.
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 CS3 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 CS3 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 CS3 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 CS3 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 CS3
from the associated ICAL of an internal standard compound is > 10.0 seconds, qualify detects and
non-detects as unusable (R). The EPA Regional CLP COR should be contacted to arrange for
reanalysis.
8. If the RT shift between sample/blank and the associated opening CCV or mid-point standard CS3
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 EPA Regional CLP COR action.
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Table 14. Internal Standard Actions for Trace Volatile Analysis
Criteria
Action
Detect
Non-detect
Area response < 20% of the opening CCV or mid-point
standard CS3 from ICAL
J+
R
20% < Area response < 50% of the opening CCV or
mid-point standard CS3 from ICAL
J+
UJ
50% < Area response < 200% of the opening CCV or
mid-point standard CS3 from ICAL
No qualification
No qualification
Area response > 200% of the opening CCV or mid-point
standard CS3 from ICAL
J-
No qualification
RT shift between sample/blank and opening CCV or
mid-point standard CS3 from ICAL > 10.0 seconds
R
R
RT shift between sample/blank and opening CCV or
mid-point standard CS3 from ICAL < 10.0 seconds
No qualification
No qualification
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X. Target Analyte Identification
A. Review Items
Form 1A-OR, quantitation reports, mass spectra, and chromatograms. (SOW SOM02.4 - Exhibit B,
Section 3.4 and Exhibit D/Trace VOA, Section 11.1.1)
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 CS3 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
CS3 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 CS3 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 |ig/L for non-ketones, 200 |ig/L for ketones), non-target compounds
at concentrations >100 (ig/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 noncompliant 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 the 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 the 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 EPA Regional CLP COR 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.
(SOW SOM02.4 - Exhibit B, Section 3.4 and Exhibit D/Trace VOA, Sections 11.2.1, 11.2.2, and
11.2.4)
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 noncompliant 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 EPA Regional CLP COR, 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 CRQL calculations, perform a more comprehensive
recalculation.
3. If sample results are < CRQLs and > MDLs, qualify as estimated (I).
4. Note numerous or significant failures to accurately quantify the target analytes, or to properly
evaluate and adjust CRQLs, for EPA Regional CLP COR action.
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XII. Tentatively Identified Compounds
A. Review Items
Form 1B-OR, chromatograms, library search printouts, and spectra for the TIC candidates. (SOW
SOM02.4 - Exhibit B, Section 3.4 and Exhibit D/Trace VOA, Sections 11.1.2 and 11.2.3)
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 (NIST) (2011 release or later), 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 an 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
"probable 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.
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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
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 (straight-chain or branched) or CnFhn (cyclic)
that contains 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 an 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 EPA Regional CLP COR 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 EPA Regional CLP COR action.
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XIII. System Performance
A. Review Items
Form 8A-OR and chromatograms. (SOW SOM02.4 - Exhibit B, Section 3.4 and Exhibit D/Trace
VOA, Section 11.1)
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 EPA
Regional CLP COR action.
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XIV. Performance Evaluation Sample
A. Review Items
Form 1A-OR, TR/COC Record documentation, preparation logs, instrument printouts, and raw data.
(SOW SOM02.4 - Exhibit B, Section 3.4 and Exhibit F, Section 4.1)
B. Objective
The objective is to determine the validity of the analytical results based on the recovery of the PE
sample(s).
C. Criteria
1. Matrix-specific PE samples shall be analyzed utilizing the same analytical methods and Quality
Assurance/Quality Control (QA/QC) procedures as employed for the samples, at a frequency to be
determined by each EPA Region for each site. PE samples must be analyzed in an SDG containing
field samples for the Case, using the same procedures, reagents, and instrumentation.
D. Evaluation
1. Verify, using Form 1A-OR, preparation logs, and raw data, that the PE samples were analyzed with
the field samples and field blanks in the SDG.
2. Verify, using Form 1A-OR, that the PE sample results are within the warning limits (95%
confidence interval) and action limits (99% confidence interval).
3. If a significant number (i.e., half or more) of the analytes in the PE samples fall outside of the 95%
warning or 99% action criteria, or a number of false positive results are reported, evaluate the
overall impact on the data.
E. Action
NOTE: If the PE sample criteria are not met, the laboratory performance and method accuracy are
in question. Use professional judgment to determine if the data should be qualified or
rejected. The following guidance is suggested for qualifying sample data associated with a
PE sample that does not meet the required criteria.
For a PE sample that does not meet the technical criteria, apply the action to all samples in
the same preparation batch. If the concentration of any analyte in a PE sample is not
comparable to the analyte's concentration in the field samples or field blanks (i.e., it is
much higher or much lower than the concentration in these samples), the action may be
applied to only those samples in which the analyte's concentration is comparable to the PE
sample concentration.
1. If the PE sample was not analyzed with the field samples and field blanks, use professional
judgment to determine if the associated sample results should be qualified. Obtain additional
information from the laboratory, if necessary. If a laboratory fails to analyze the PE sample(s)
provided with field samples and field blanks, or if a laboratory consistently fails to generate
acceptable PE sample results, record the situation in the Data Review Narrative, and note it for EPA
Regional CLP COR action.
2. If the PE sample results are outside the lower warning limits but inside the lower action limits,
qualify detects as estimated low (I-) and non-detects as estimated (UI).
3. If the PE sample results are outside the lower action limits, qualify detects as estimated low (I-) and
non-detects as unusable (R).
4. If the PE sample results are within the limits, detects and non-detects should not be qualified.
5. If the PE sample results are outside the upper warning limits but inside the upper action limits,
qualify detects as estimated high (I+). Non-detects should not be qualified.
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6. If the PE sample results are outside the upper action limits, qualify detects as estimated high (J+).
Non-detects should not be qualified.
7. Annotate the potential effects on the data due to out-of-control PE sample results in the Data
Review Narrative.
Table 15. PE Sample Actions for Trace Volatile Analysis
Criteria
Action
Detect
Non-detect
PE sample results outside lower warning limits but inside
lower action limits
J-
UJ
PE sample results outside lower action limits
J-
R
PE sample results within limits
No qualification
No qualification
PE sample results outside upper warning limits but inside
upper action limits
J+
No qualification
PE sample results outside upper action limits
J+
No qualification
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XV. Regional Quality Assurance and Quality Control
A. Review Items
Form 1A-OR, chromatograms, TR/COC Record documentation, quantitation reports, and other raw
data from QA/QC samples. (SOW SOM02.4 - Exhibit B, Sections 2.4 and 3.4)
B. Objective
The objective is to use results from the analysis of EPA Regional QA/QC samples such as field
duplicates, blind spikes, and blind blanks to determine the validity of the analytical results.
C. Criteria
Criteria are determined by each EPA Region.
1. The frequency of EPA Regional QA/QC samples should be defined in the project QAPP.
2. Performance criteria for EPA Regional QA/QC samples should also be defined in the project
QAPP.
3. The EPA Region may provide the laboratory with PE samples to be analyzed with each SDG.
These samples may include blind spikes and/or blind blanks. The laboratory must analyze a PE
sample when provided by the EPA Region. Refer to Section VI, above, for blanks criteria. Refer to
Section XIV, above, for PE samples criteria.
4. The RPD between field duplicates shall fall within the specific limits in the EPA Region's SOP or
project QAPP.
D. Evaluation
1. Evaluation procedures must follow the EPA Region's SOP for data review.
2. Determine whether the results of EPA Regional QA/QC samples impact all samples in the project
or only those directly associated (i.e., in the same SDG, collected on the same day, prepared
together, or contained in the same analytical sequence).
3. 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 EPA Region's SOP or
project QAPP.
4. Determine whether poor precision is the fault of the laboratory, or a result of sample
non-homogeneity in the field. Laboratory observations of sample appearance may become
important in these situations.
E. Action
1. Any action must be in accordance with EPA Regional specifications and the criteria for acceptable
field duplicate sample results.
2. Note unacceptable results for field duplicate samples for EPA Regional CLP COR action.
3. In general, for EPA Regional QA/QC performance not within QAPP specification, qualify detects
as estimated (J) and non-detects as estimated (UJ). The impact on overall data quality should be
assessed after consultation with the data user and/or field personnel. Contact the EPA Regional
CLP COR if reanalysis of samples is required.
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XVI. 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 equations, as
listed in the method. All sample results must be within the linear calibration ranges per the
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 Data Reporting 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 EPA Regional CLP COR 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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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 59
II. Gas Chromatograph/Mass Spectrometer Instrument Performance Check 63
III. Initial Calibration 71
IV. Initial Calibration Verification 76
V. Continuing Calibration Verification 79
VI. Blanks 82
VII. Deuterated Monitoring Compound 85
VIII. Matrix Spike/Matrix Spike Duplicate 88
IX. Internal Standard 90
X. Target Analyte Identification 93
XI. Target Analyte Quantitation and Reported Contract Required Quantitation Limit 95
XII. Tentatively Identified Compounds 97
XIII. System Performance 100
XIV. Performance Evaluation Sample 101
XV. Regional Quality Assurance and Quality Control 103
XVI. Overall Assessment of Data 104
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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) Record 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. (SOW SOM02.4 - Exhibit
B, Section 3.4; Exhibit D/Introduction, Section 5.0; Exhibit D/General, Sections 8.0, 10.1.2.1, and
10.2.2.4.4; and Exhibit D/Low/Med VOA, Section 8.0)
B. Objective
The objective is to determine the validity of the analytical results based on the sample conditions 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. Aqueous samples, TCLP/SPLP aqueous and aqueous filtrate samples,
TCLP/SPLP leachate samples, and 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. 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 filtrate 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 purge-and-trap (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 Record 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, Form 1B-OR, and the raw data 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 Record
documentation with the dates of analysis on Form 1A-OR, Form 1B-OR, and the raw data. 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 aH analytes listed in
SOW SOM02.4 Exhibit C, Table 2 - Low/Medium Volatiles Target Analyte List and Contract
Required Quantitation Limits. 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 but < 10°C, use professional
judgment to qualify detects and non-detects.
2. 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 (J) and non-detects as estimated
(UJ).
3. 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.
4. If the TCLP/SPLP ZHE procedure is performed outside the extraction technical holding time of 14
days, qualify detects as estimated (J) and non-detects as unusable (R).
5. If a discrepancy is found between the sample analysis date on Form 1A-OR, Form 1B-OR, and the
raw data, perform a more comprehensive review to determine the correct date for establishing the
holding time.
6. 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.
7. If TCLP/SPLP aqueous filtrate samples and TCLP/SPLP leachate samples are analyzed within the
technical holding time of 7 days, detects and non-detects should not be qualified.
8. If aqueous samples are not properly preserved and are analyzed outside of the technical holding
time of 7 days, qualify detects as estimated (J) and non-detects as unusable (R).
9. If TCLP/SPLP aqueous filtrate samples and TCLP/SPLP leachate samples are analyzed outside of
the technical holding time of 7 days, qualify detects as estimated (J) and non-detects as unusable
(R).
10. 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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11. 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).
12. 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.
13. 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 (J) and non-detects as unusable (R).
14. 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.
15. 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).
16. When the holding times are exceeded, annotate in the Data Review Narrative any possible
consequences for the analytical results.
17. If holding times are grossly exceeded, qualify detects as estimated (J) and non-detects as unusable
(R). Note this for United States Environmental Protection Agency Regional Contract Laboratory
Program Contracting Officer's Representative (EPA Regional CLP COR) action. Annotate the
effect of the holding time exceedance on the resulting data in the Data Review Narrative, whenever
possible.
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Table 16. Preservation and Holding Time Actions for Low/Medium Volatile Analysis
Criteria
Action
Detect
Non-detect
Sample temperature > 6°C but < 10°C upon receipt
at the laboratory
Use professional
judgment
Use professional
judgment
Sample temperature > 10°C upon receipt at the
laboratory
Use professional
judgment
J*
Use professional
judgment
UJ
TCLP/SPLP ZHE procedure performed within the
14-day technical holding time
No qualification
No qualification
TCLP/SPLP ZHE procedure performed outside the
14-day technical holding time
J*
R
Aqueous sample not preserved but analyzed within
the 7-day technical holding time
No qualification
No qualification
TCLP/SPLP aqueous filtrate sample and
TCLP/SPLP leachate sample analyzed within 7-day
technical holding time
No qualification
No qualification
Aqueous sample not preserved and analyzed outside
the 7-day technical holding time
J*
R
TCLP/SPLP aqueous filtrate sample and
TCLP/SPLP leachate sample analyzed outside
7-day technical holding time
J*
R
Aqueous sample properly preserved and analyzed
within the 14-day technical holding time
No qualification
No qualification
Aqueous sample properly preserved but analyzed
outside the 14-day technical holding time
J*
R
Non-aqueous sample preserved and analyzed within
the 14-day technical holding time
No qualification
No qualification
Non-aqueous sample properly preserved but
analyzed outside the 14-day technical holding time
J*
R
Non-aqueous sample not properly preserved but
analyzed within the 14-day technical holding time
No qualification
No qualification
Non-aqueous sample not properly preserved and
analyzed outside the 14-day technical holding time
J*
R
Holding time grossly exceeded
J*
R
* The true direction of any bias may be unknown in this case. 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).
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II. Gas Chromatograph/Mass Spectrometer Instrument Performance Check
A. Review Items
Form 5-OR, bromofluorobenzene (BFB) mass spectra, and mass listing. (SOW SOM02.4 - Exhibit B,
Section 3.4 and Exhibit D/Low/Med VOA, Section 9.2)
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. 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 the injection of BFB;
however, 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.
• Initial Calibration Verification
(ICV) meets ICV 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.
• ICV meets ICV 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
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 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. 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 1/
Beginning of 12-hour clock
for Analytical Sequence 2
End of 12-hour clock for
Analytical Sequence 2/
Beginning of 12-hour clock
for Analytical Sequence 3
0 hr BFB
Initial Calibration 5.0
Initial Calibration 10
Initial Calibration 50
Initial Calibration 100
Initial Calibration 200
ICV
Method Blank
Subsequent Samples
12 hr CCV ^ (meets opening CCV
criteria)
Method Blank
Subsequent Samples
24 hr CCV B (meets opening CCV
criteria)
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
0 hr BFB
End of 12-hour clock for
Analytical Sequence 1
Beginning of 12-hour clock
for Analytical Sequence 2
12 hr
End of 12-hour clock for
Analytical Sequence 2
25 hr
Initial Calibration 5.0
Initial Calibration 10
Initial Calibration 50
Initial Calibration 100
Initial Calibration 200
ICV
Method Blank
Subsequent Samples
CCV A (meets closing CCV
criteria, fails opening CCV
criteria)
13 hr BFB
CCV B (meets opening CCV
criteria)
Method Blank
Subsequent Samples
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
End of 12-hour clock for
Analytical Sequence 1/
Beginning of 12-hour clock
for Analytical Sequence 2
0 hr BFB
CCV A (meets opening CCV
criteria)
Method Blank
Subsequent Samples
12 hr CCV ® (meets opening CCV
criteria)
Method Blank
Subsequent Samples
1/2
2
2
2
2
2
End of 12-hour clock for
Analytical Sequence 2/
Beginning of 12-hour clock
for Analytical Sequence 3
24 hr CCV C (meets opening CCV
criteria)
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
Ohr
12 hr
BFB
CCV A (meets opening CCV
criteria)
Method Blank
Subsequent Samples
CCV B (meets closing CCV
criteria, fails opening CCV
criteria)
13 hr BFB
CCV C (meets opening CCV
criteria)
Method Blank
Subsequent Samples
2
2
2
2
2
End of 12-hour clock for
Analytical Sequence 2/
Beginning of 12-hour clock
for Analytical Sequence 3
25 hr CCV D (meets opening CCV
criteria)
2/3
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2. The BFB instrument performance check must meet the ion abundance criteria listed in Table 17.
Table 17. Ion Abundance Criteria for BFB
Mass
Ion Abundance Criteria
50
15.0-40.0% of mass 95
75
30.0 - 80.0% of mass 95
95
Base peak, 100% relative abundance
96
5.0 - 9.0% of mass 95*
173
Less than 2.0% of mass 174
174
50.0%- 120% of mass 95
175
5.0-9.0% of mass 174
176
95.0- 101% of mass 174
177
5.0-9.0% of mass 176
* All ion abundances must be normalized to 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 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 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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b. Background subtraction must be accomplished using a single scan acquired within 20 scans of
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 CLP, information regarding noncompliant 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 the 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 EPA Regional CLP
COR should be contacted to arrange for reanalysis of all affected samples.
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 action is required.
3. If the laboratory failed to provide the correct forms, or if significant transcription or calculation
errors are found, notify the EPA Regional CLP COR, 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 EPA Regional CLP COR.
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 17 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 noncompliant 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 EPA Regional CLP COR action.
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III. Initial Calibration
A. Review Items
Form 6A-OR, quantitation reports, and chromatograms. (SOW SOM02.4 - Exhibit B, Section 3.4 and
Exhibit D/Low/Med VOA, Sections 7.2.2.1 and 9.3)
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 the ICV, 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 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 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 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 18.
4. The %RSD of the ICAL RRF for each target analyte and DMC must be < Maximum %RSD value
in Table 18.
NOTE: The technical acceptance criteria specified in a "Request for Quote (RFQ) for Solicitation"
of a Modified Analysis may impact some of the preceding evaluation criteria. A copy of
this document should be present in the CSF, when applicable.
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 %RSDs 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 18 for each target analyte and DMC.
5. Verify that the %RSD is < Maximum %RSD value in Table 18 for each target analyte and DMC.
NOTE: For data obtained from the CLP, information regarding noncompliant 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, use professional judgment to
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 %RSDs, perform a more
comprehensive recalculation.
4. If the RRF is < Minimum RRF value in Table 18 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 18 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 18 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 18 for any target analyte, 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
necessary. The following guidelines are recommended:
a. If the %RSD criteria of any target analytes are not met and the %RSD criteria are still not
satisfied after eliminating either the high or the low-point of the ICAL:
i. Qualify detects in the associated samples as estimated (J).
ii. Use professional judgment to qualify non-detects in the associated samples.
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 EPA Regional CLP
COR, 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 EPA Regional CLP COR action.
Table 18. RRF, %RSD, and %D Acceptance Criteria in Initial Calibration, ICV, and CCV for
Low/Medium Volatile Analysis
Analyte
Minimum
RRF
Maximum
%RSD
ICV/Opening
CCV
Maximum
%D'
Closing
CCV
Maximum
%D
Dichlorodifluoromethane
0.010
25.0
±40.0
±50.0
Chloromethane
0.010
20.0
±30.0
±50.0
Vinyl chloride
0.010
20.0
±25.0
±50.0
Bromomethane
0.010
40.0
±30.0
±50.0
Chloroethane
0.010
40.0
±25.0
±50.0
Trichlorofluoromethane
0.010
40.0
±30.0
±50.0
1,1 -Dichloroethene
0.060
20.0
±20.0
±25.0
1,1,2-Trichloro-1,2,2-trifluoroethane
0.050
25.0
±25.0
±50.0
Acetone
0.010
40.0
±40.0
±50.0
Carbon disulfide
0.100
20.0
±25.0
±25.0
Methyl acetate
0.010
40.0
±40.0
±50.0
Methylene chloride
0.010
40.0
±30.0
±50.0
trans-1,2-Dichloroethene
0.100
20.0
±20.0
±25.0
Methyl tert-butyl ether
0.100
40.0
±25.0
±50.0
1,1 -Dichloroethane
0.300
20.0
±20.0
±25.0
cis-1,2-Dichloroethene
0.200
20.0
±20.0
±25.0
2-Butanone
0.010
40.0
±40.0
±50.0
Bromochloromethane
0.100
20.0
±20.0
±25.0
Chloroform
0.300
20.0
±20.0
±25.0
1,1,1 -Trichloroethane
0.050
20.0
±25.0
±25.0
Cyclohexane
0.010
40.0
±25.0
±50.0
Carbon tetrachloride
0.100
20.0
±25.0
±25.0
Benzene
0.200
20.0
±20.0
±25.0
1,2-Dichloroethane
0.070
20.0
±20.0
±25.0
Trichloroethene
0.200
20.0
±20.0
±25.0
Methylcyclohexane
0.050
40.0
±25.0
±50.0
1,2-Dichloropropane
0.200
20.0
±20.0
±25.0
Bromodichloromethane
0.300
20.0
±20.0
±25.0
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Analyte
Minimum
RRF
Maximum
%RSD
ICV/Opening
CCV
Maximum
%D'
Closing
CCV
Maximum
%D
cis-1,3 -Dichloropropene
0.300
20.0
±20.0
±25.0
4-Methyl-2-pentanone
0.030
25.0
±30.0
±50.0
Toluene
0.300
20.0
±20.0
±25.0
trans-1,3 -Dichloropropene
0.200
20.0
±20.0
±25.0
1,1,2-Trichloroethane
0.200
20.0
±20.0
±25.0
T etrachloroethene
0.100
20.0
±20.0
±25.0
2-Hexanone
0.010
40.0
±40.0
±50.0
Dibromochloromethane
0.200
20.0
±20.0
±25.0
1,2-Dibromoethane
0.200
20.0
±20.0
±25.0
Chlorobenzene
0.400
20.0
±20.0
±25.0
Ethylbenzene
0.400
20.0
±20.0
±25.0
m,p-Xylene
0.200
20.0
±20.0
±25.0
o-Xylene
0.200
20.0
±20.0
±25.0
Styrene
0.200
20.0
±20.0
±25.0
Bromoform
0.100
20.0
±25.0
±50.0
Isopropylbenzene
0.400
20.0
±25.0
±25.0
1,1,2,2-T etrachloroethane
0.200
20.0
±25.0
±25.0
1,3 -Dichlorobenzene
0.500
20.0
±20.0
±25.0
1,4-Dichlorobenzene
0.600
20.0
±20.0
±25.0
1,2-Dichlorobenzene
0.600
20.0
±20.0
±25.0
1,2-Dibromo -3 -chloropropane
0.010
25.0
±30.0
±50.0
1,2,4-Trichlorobenzene
0.400
20.0
±30.0
±50.0
1,2,3 -T richlorobenzene
0.400
25.0
±30.0
±50.0
Deuterated Monitoring Compounds
Vinyl chloride-d3
0.010
20.0
±30.0
±50.0
Chloroethane-ds
0.010
40.0
±30.0
±50.0
1,1 -Dichloroethene-d2
0.050
20.0
±25.0
±25.0
2-Butanone-ds
0.010
40.0
±40.0
±50.0
Chloroform-d
0.300
20.0
±20.0
±25.0
1,2-Dichloroethane-d4
0.060
20.0
±25.0
±25.0
Benzene-d6
0.300
20.0
±20.0
±25.0
1,2-Dichloropropane-d6
0.200
20.0
±20.0
±25.0
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Analyte
Minimum
RRF
Maximum
%RSD
ICV/Opening
CCV
Maximum
%D'
Closing
CCV
Maximum
%D
Toluene-ds
0.300
20.0
±20.0
±25.0
trans-1,3 -Dichloropropene-d4
0.200
20.0
±20.0
±25.0
2-Hexanone-ds
0.010
40.0
±40.0
±50.0
1,1,2,2-T etrachloroethane-d2
0.200
20.0
±25.0
±25.0
1,2-Dichlorobenzene-d4
0.400
20.0
±20.0
±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 19. Initial Calibration Actions for Low/Medium Volatile Analysis
Criteria
Action
Detect
Non-detect
Initial Calibration not performed at the specified
frequency and sequence
Use professional
judgment
R
Use professional
judgment
R
Initial Calibration not performed at the specified
concentrations
J
UJ
RRF < Minimum RRF in Table 18 for target
analyte
Use professional
judgment
J+ or R
R
RRF > Minimum RRF in Table 18 for target
analyte
No qualification
No qualification
%RSD > Maximum %RSD in Table 18 for
target analyte
J
Use professional
judgment
%RSD < Maximum %RSD in Table 18 for
target analyte
No qualification
No qualification
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IV. Initial Calibration Verification
A. Review Items
Form 7A-OR, quantitation reports, and chromatograms. (SOW SOM02.4 - Exhibit B, Section 3.4 and
Exhibit D/Low/Med VOA, Sections 7.2.2.2 and 9.4)
B. Objective
The objective is to ensure that the instrument is calibrated accurately to produce acceptable qualitative
and quantitative data throughout each analytical sequence by the use of a second-source check
standard.
C. Criteria
1. The accuracy of the calibration for each GC/MS system used for analysis must be verified at the
frequency of one ICV standard analysis per initial calibration analytical sequence. The ICV is
analyzed after the last ICAL standard analysis and prior to a blank, sample, or an applicable CCV
analysis.
2. The ICV standard must contain all required target analytes, from an alternate source or a different
lot than that used for the ICAL standards and DMCs, at or near the mid-point concentration (CS3)
of the ICAL.
3. For an ICV, the RRF for each target analyte and DMC must be > the Minimum RRF values in Table
18.
4. The Percent Difference (%D) between the ICAL RRF and the ICV RRF must be within the
ICV/Opening CCV Maximum %D limits in Table 18 for each target analyte and DMC.
D. Evaluation
1. Verify that the ICV standard is analyzed at the specified frequency and sequence, and that it is
associated with 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 concentrations of the target analytes and the DMCs in the ICV are at or near the
mid-point standard CS3 from the ICAL.
3. Verify that the RRF and %D for each target analyte and DMC are reported on Form 7A-OR.
Recalculate the 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. Verify that the RRFs for each target analyte and DMC in the ICV are > Minimum RRF values in
Table 18.
5. Verify that the %Ds are within the ICV/Opening CCV Maximum %D limits in Table 18 for each
target analyte and DMC.
NOTE: For data obtained from the CLP, information regarding the noncompliant ICV can be
obtained from the NFG reports and may be used as part of the evaluation process.
E. Action
1. If the ICV is not performed at the specified frequency, use professional judgment to qualify detects
and non-detects. Contact the EPA Regional CLP COR 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 quality of analyte peak
shapes and mass spectral matches, the 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.
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2. If the ICV 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. If the RRF in an ICV is < Minimum RRF value in Table 18 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).
a. Take special note of any extreme deviation in the RRF and evaluate RT data, peak shapes, and
areas of the target analytes and associated internal standards for inconsistencies that may
indicate a chromatographic co-elution. If this is suspected, the contaminant may also be
present in samples and blanks. Also review the documentation of the preparation of the ICV
standard. Use professional judgment to qualify affected data appropriately.
5. If the RRF in an ICV is > Minimum RRF value in Table 18 for any target analyte, detects and
non-detects should not be qualified.
6. If the %D in an ICV is outside the ICV/Opening CCV Maximum %D limits in Table 18 for any
target analyte, qualify detects as estimated (J) and non-detects as estimated (UJ).
7. If the %D in an ICV is within the inclusive range of the ICV/Opening CCV Maximum %D limits in
Table 18 for any target analyte, detects and non-detects should not be qualified.
8. No qualification of the data is necessary based on the 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.
9. If the laboratory has failed to provide adequate calibration information, contact the EPA Regional
CLP COR, who may contact the laboratory to request the necessary information. If the information
is not available, use professional judgment to assess the data. Refer to E. 1, above, for additional
steps.
10. Note the potential effects on the data due to ICV criteria exceedance in the Data Review Narrative.
11. If the ICV criteria are grossly exceeded, note this for EPA Regional CLP COR action.
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Table 20. ICV Actions for Low/Medium Volatile Analysis
Criteria for ICV
Action
Detect
Non-detect
ICV not performed at the specified
frequency and sequence
Use professional
judgment
Use professional
judgment
ICV not performed at the specified
concentration
Use professional
judgment
Use professional
judgment
RRF < Minimum RRF in Table 18
for target analyte
Use professional
judgment
J or R
R
RRF > Minimum RRF in Table 18
for target analyte
No qualification
No qualification
%D outside the ICV/Opening
CCV Maximum %D limits in
Table 18 for target analyte
J
UJ
%D within the inclusive
ICV/Opening CV Maximum %D
limits in Table 18 for target
analyte
No qualification
No qualification
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V. Continuing Calibration Verification
A. Review Items
Form 7A-OR, quantitation reports, and chromatograms. (SOW SOM02.4 - Exhibit B, Section 3.4 and
Exhibit D/Low/Med VOA, Sections 7.2.2.1 and 9.5)
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 CCV are met.
2. The CCV standards must contain all required target analytes and DMCs at or near the mid-point
concentration (CS3) 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 18.
4. The %D between the ICAL RRF and the opening CCV RRF must be within the ICV/Opening CCV
Maximum %D limits in Table 18 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
CCV Maximum %D limits in Table 18 for each target analyte and DMC.
D. Evaluation
1. Verify that the CCV is analyzed at the specified frequency and sequence, and that it is associated
with 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 CS3 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 the 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 each target analyte and DMC are
> Minimum RRF values in Table 18.
5. For an opening CCV, verify that the %Ds are within the ICV/Opening CCV Maximum %D limits
in Table 18 for each target analyte and DMC.
6. For a closing CCV, verify that the %Ds are within the Closing CCV Maximum %D limits in Table
18 for each target analyte and DMC.
NOTE: For data obtained from the CLP, information regarding the noncompliant CCV 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 CCV is not performed at the specified frequency, qualify detects and non-detects as unusable
(R). Contact the EPA Regional CLP COR 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 quality of analyte peak shapes and
mass spectral matches, the stability of internal standard 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 < Minimum RRF value in Table 18 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).
a. Take special note of any extreme deviation in the RRF and evaluate RT data, peak shapes, and
areas of the target analytes and associated internal standards for inconsistencies that may
indicate a chromatographic co-elution. If this is suspected, the contaminant may also be
present in samples and blanks. Also review the documentation of the preparation of the CCV
standard. Use professional judgment to qualify affected data appropriately.
5. For an opening or a closing CCV, if the RRF is > Minimum RRF value in Table 18 for any target
analyte, detects and non-detects should not be qualified.
6. For an opening CCV, if the %D is outside the ICV/Opening CCV Maximum %D limits in Table 18
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 CCV Maximum %D limits in Table 18 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 ICV/Opening CCV Maximum
%D limits in Table 18 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 CCV Maximum %D limits
in Table 18 for any target analyte, detects and non-detects should not be qualified.
10. No qualification of the data is necessary based on the 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 EPA Regional
CLP COR, who may contact the laboratory to request the necessary information. If the information
is not available, use professional judgment to assess the data. Refer to E. 1, above, for additional
steps.
12. Note the potential effects on the data due to CCV criteria exceedance in the Data Review Narrative.
13. If the CCV criteria are grossly exceeded, note this for EPA Regional CLP COR action.
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Table 21. CCV Actions for Low/Medium Volatile Analysis
Criteria for Opening CCV
Criteria for Closing CCV
Action
Detect
Non-detect
CCV not performed at the
specified frequency and
sequence
CCV not performed at the
specified frequency
Use
professional
judgment
J or R
Use
professional
judgment
UJ orR
CCV not performed at the
specified concentration
CCV not performed at the
specified concentration
Use
professional
judgment
Use
professional
judgment
Use
RRF < Minimum RRF in
Table 18 for target analyte
RRF < Minimum RRF in
Table 18 for target analyte
professional
judgment
J or R
R
RRF > Minimum RRF in
Table 18 for target analyte
RRF > Minimum RRF in
Table 18 for target analyte
No
qualification
No
qualification
%D outside the ICV/Opening
CCV Maximum %D limits in
Table 18 for target analyte
%D outside the Closing CCV
Maximum %D limits in Table
18 for target analyte
J
UJ
%D within the inclusive
ICV/Opening CCV Maximum
%D limits in Table 18 for
target analyte
%D within the inclusive
Closing CCV Maximum %D
limits in Table 18 for target
analyte
No
qualification
No
qualification
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VI. Blanks
A. Review Items
Form 1A-OR, Form 1B-OR, Form 4-OR, chromatograms, and quantitation reports. (SOW SOM02.4 -
Exhibit B, Section 3.4 and Exhibit D/Low/Med VOA, Section 12.1)
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 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, the ICV, or the opening 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 an SDG, and stored with the samples
until analysis. The storage blank must be analyzed once per SDG after all sample analyses within
an 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 200 (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 blank must be < 5.0 (ig/L for water (0.0050 mg/L for TCLP leachate) and <5.0
(ig/kg for soil/sediment 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 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 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.
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6. Data concerning the field blanks are not evaluated as part of the Contract Compliance Screening
(CCS) process. 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 CCS
process. Information regarding the noncompliant 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 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 EPA
Regional CLP COR 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 EPA 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 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 that are
< 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 but
< Blank Results at sample results and qualify as non-detect (U) or as unusable (R). Use
professional judgment to qualify sample results that are > CRQLs and > Blank Results or > 2x
results in method blank for Methylene chloride, Acetone, and 2-Butanone.
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) concentrations) 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 EPA
Regional CLP COR 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.
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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 and storage, field, or trip blanks, the sample result qualifications
listed in Table 22 should apply if supported by the project QAPP.
9. If gross contamination exists with blank results that are > ICAL CS5 concentrations, qualify detects
as unusable (R). If the contamination is suspected of having an effect on the sample results, note it
for EPA Regional CLP COR action.
10. For any blank (including method blank) reported with TICs (non-target compounds) concentrations
that are >5.0 (ig/L for water (0.0050 mg/L for TCLP leachate) or > 5.0 j^ig/kg for soil/sediment
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 22. Blank and TCLP/SPLP LEB Actions for Low/Medium Volatile Analysis
Blank Type
Blank Result
Sample Result
Action
Method,
TCLP/SPLP
LEB, Storage,
Field, Trip,
Instrument*
Detect
Non-detect
No qualification
< CRQL
< CRQL
Report at CRQL and qualify as
non-detect (U)
> CRQL or > 2x Blank Result
for Methylene chloride,
Acetone, and 2-Butanone
Use professional judgment
> CRQL
< CRQL
Report at CRQL and qualify as
non-detect (U)
> CRQL but < Blank Result
Report at sample result and
qualify as non-detect (U) or
unusable (R)
> CRQL and > Blank Result or
> 2x Blank Result for
Methylene chloride, Acetone,
and 2-Butanone
Use professional judgment
Gross
contamination
Detect
Report at sample result and
qualify as unusable (R)
TIC >5.0 ng/L
(water) or 0.0050
mg/L (TCLP
leachate)
or
TIC >5.0 (ig/kg
(soil/sediment)
Detect
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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VII. Deuterated Monitoring Compound
A. Review Items
Form 2A-OR, Form 2B-OR quantitation reports, and chromatograms. (SOW SOM02.4 - Exhibit B,
Section 3.4 and Exhibit D/Low/Med VOA, Sections 7.2.2.4 and 11.2.5)
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 23, 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 23.
Table 23. Low/Medium Volatile DMC Recovery Limits
%R for
%R for
DMC
Water
Soil/Sediment
Sample
Sample
Vinyl chloride-d3
60 - 135
30 - 150
Chloroethane-ds
70-130
30-150
1,1 -Dichloroethene-d2
60 - 125
45-110
2-Butanone-ds
40 - 130
20 - 135
Chloroform-d
70 - 125
40 - 150
1,2-Dichloroethane-d4
70 - 125
70 - 130
Benzene-d6
70 - 125
20-135
1,2-Dichloropropane-d6
70 - 120
70 - 120
Toluene-ds
80 - 120
30-130
trans-1,3 -Dichloropropene-d4
60 - 125
30-135
2-Hexanone-ds
45 - 130
20 - 135
1,1,2,2-T etrachloroethane-d2
65 - 120
45 - 120
1,2-Dichlorobenzene-d4
80 - 120
75 - 120
NOTE: The recovery limits for any of the compounds listed in Table 23 may be expanded at any
time during the period of performance if the EPA determines that the limits are too
restrictive.
D. Evaluation
1. Check the 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 time s.
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 noncompliant 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 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
EPA Regional CLP COR 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 23) in samples, qualify the associated target analytes
listed in Table 25 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 < 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 23) 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 EPA Regional CLP COR action.
Table 24. DMC Actions for Low/Medium Volatile Analysis
Criteria
Action
Detect
Non-detect
%R< 10%
J-
R
10% < %R < Lower Acceptance Limit
J-
UJ
Lower Acceptance Limit < %R < Upper Acceptance
Limit
No qualification
No qualification
%R > Upper Acceptance Limit
J+
No qualification
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Table 25. Low/Medium Volatile DMCs and the Associated Target Analytes
Vinyl chloride-d3 (DMC-1)
Chloroethane-ds (DMC-2)
l,l-Dichloroethene-d2 (DMC-3)
Vinyl chloride
Dichlorodifluoromethane
Chloromethane
Bromomethane
Chloroethane
Carbon disulfide
trans-1,2-Dichloroethene
cis-l,2-Dichloroethene
1,1 -Dichloroethene
2-Butanone-ds (DMC-4)
Chloroform-d (DMC-5)
l,2-Dichloroethane-d4 (DMC-6)
Acetone
2-Butanone
1,1 -Dichloroethane
Bromochloromethane
Chloroform
Dibromochloromethane
Bromoform
Trichlorofluoromethane
1,1,2-T richloro-1,2,2-trifluoroethane
Methyl acetate
Methylene chloride
Methyl-tert-butyl ether
1,1,1 -T richloroethane
Carbon tetrachloride
1,2-Dibromoethane
1,2-Dichloroethane
Benzene-d6 (DMC-7)
l,2-Dichloropropane-d6
(DMC-8)
Toluene-ds (DMC-9)
Benzene
Cyclohexane
Methylcyclohexane
1,2-Dichloropropane
Bromodichloromethane
Trichloroethene
Toluene
T etrachloroethene
Ethylbenzene
o-Xylene
m,p-Xylene
Styrene
Isopropylbenzene
trans-l,3-Dichloropropene-d4
(DMC-10)
2-Hexanone-ds (DMC-11)
l,l,2,2-Tetrachloroethane-d2
(DMC-12)
cis-1,3 -Dichloropropene
trans -1,3 -Dichloropropene
1,1,2-Trichloroethane
4-Methyl-2-pentanone
2-Hexanone
1,1,2,2,-T etrachloroethane
1,2-Dibromo -3 -chloropropane
l,2-Dichlorobenzene-d4
(DMC-13)
Chlorobenzene
1,3 -Dichlorobenzene
1,4-Dichlorobenzene
1,2-Dichlorobenzene
1,2,4-Trichlorobenzene
1,2,3 -Trichlorobenzene
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VIII. Matrix Spike/Matrix Spike Duplicate
A. Review Items
SDG Cover Page, Form 3A-OR, chromatograms, and quantitation reports. (SOW SOM02.4 - Exhibit
B, Section 3.4 and Exhibit D/Low/Med VOA, Sections 7.2.2.5 and 12.2)
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 samples should be analyzed per matrix or per SDG.
NOTE: Data for MS and MSDs will not be present unless requested by the EPA 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 26.
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 3A-OR and verify that they are within the limits listed
in Table 26.
NOTE: For data obtained from the CLP, the preceding criteria, including the requested MS/MSD
spiking analytes and spiking levels specified in Exhibit D - Low/Medium Concentrations
of Volatile Organic Compounds Analysis, Section 7.2.2.5, of the SOW, are evaluated as
part of the CCS process. Information regarding the noncompliant 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 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 EPA
Regional CLP COR action. It is not likely that data qualification will be warranted if 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 was used for the MS/MSD analysis, note this for EPA Regional CLP
COR 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 the 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 26, 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:
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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 < lower acceptance limit, qualify detects as estimated (J) and
non-detects as estimated (UJ).
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 > upper acceptance limit, qualify detects as estimated (J).
Non-detects should not be qualified.
Table 26. MS/MSD %R and RPD Limits for Low/Medium Volatile Analysis
Analyte
%R for
Water Sample
RPD for
Water Sample
%R for
Soil/Sediment
Sample
RPD for
Soil/Sediment
Sample
1,1 -Dichloroethene
61 - 145
0-14
59-172
0-22
Trichloroethene
71 - 120
0 - 14
62-137
0-24
Benzene
76 - 127
0 - 11
66 - 142
0-21
Toluene
76 - 125
0 - 13
59-139
0-21
Chlorobenzene
75 - 130
0 - 13
60-133
0-21
Table 27. MS/MSD Actions for Low/Medium Volatile Analysis
Criteria
Action
Detect
Non-detect
%R < 20%
J
R
20% < %R < Lower Acceptance Limit
J
UJ
Lower Acceptance Limit < %R or RPD < Upper
Acceptance Limit
No qualification
No qualification
%R or RPD > Upper Acceptance Limit
J
No qualification
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IX. Internal Standard
A. Review Items
Form 8A-OR, quantitation reports, and chromatograms. (SOW SOM02.4 - Exhibit B, Section 3.4 and
Exhibit D/Low/Med VOA, Sections 7.2.2.6, 11.3.5, and 11.3.6)
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 compound from the
associated opening CCV or the mid-point standard CS3 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 CS3 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 RT and area
response of each internal standard compound in a sample or blank are reported on 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 time s.
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 noncompliant internal standard area response or RT
can be obtained from the NFG reports and may be used as part of the evaluation process.
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E. Action
NOTE: Apply the action to the target analytes in samples or blanks that are associated to the
noncompliant internal standard compound in Table 28. The internal standard and the
associated target analytes are in Exhibit D - Low/Medium Concentrations of Volatile
Organic Compounds Analysis, Table 9, of the SOW.
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 CS3 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 CS3 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 CS3 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 CS3 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 CS3
from the associated ICAL of an internal standard compound is > 10.0 seconds, qualify detects and
non-detects as unusable (R). The EPA Regional CLP COR should be contacted to arrange for
reanalysis.
8. If the RT shift between sample/blank and the associated opening CCV or mid-point standard CS3
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 EPA Regional CLP COR action.
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Table 28. Internal Standard Actions for Low/Medium Volatile Analysis
Criteria
Action
Detect
Non-detect
Area response < 20% of the opening CCV or mid-point
standard CS3 from ICAL
J+
R
20% < Area response < 50% of the opening CCV or
mid-point standard CS3 from ICAL
J+
UJ
50% < Area response < 200% of the opening CCV or
mid-point standard CS3 from initial calibration
No qualification
No qualification
Area response > 200% of the opening CCV or mid-point
standard CS3 from ICAL
J-
No qualification
RT shift between sample/blank and opening CCV or
mid-point standard CS3 from ICAL > 10.0 seconds
R
R
RT shift between sample/blank and opening CCV or
mid-point standard CS3 from ICAL < 10.0 seconds
No qualification
No qualification
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X. Target Analyte Identification
A. Review Items
Form 1A-OR, quantitation reports, mass spectra, and chromatograms. (SOW SOM02.4 - Exhibit B,
Section 3.4 and Exhibit D/Low/Med VOA, Section 11.1.1)
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 CS3 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
CS3 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 CS3 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 |ig/L for non-ketones, 400 |ig/L for ketones), non-target
compounds at concentrations > 200 (ig/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 noncompliant 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 the 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 the 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 EPA Regional CLP COR 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.
(SOW SOM02.4 - Exhibit B, Section 3.4 and Exhibit D/Low/Med VOA, Sections 11.2.1, 11.2,2, and
11.2.4)
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 Percent Solids
(%Solids), 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 noncompliant 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 EPA Regional CLP COR, 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 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 the %Solids for a soil/sediment sample is < 10.0%, use professional judgment to qualify detects
and non-detects.
4. If the %Solids for a soil/sediment sample is > 10.0% and < 30.0%, use professional judgment to
qualify detects and non-detects.
5. If the %Solids for a soil/sediment sample is > 30.0%, detects and non-detects should not be
qualified.
6. If sample results are < CRQLs and > MDLs, qualify as estimated (I).
7. Note numerous or significant failures to accurately quantify the target analytes, or to properly
evaluate and adjust CRQLs, for EPA Regional CLP COR action.
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Table 29. Percent Solids Actions for Low/Medium Volatile Analysis for Non-Aqueous Samples
Criteria
Action
Detects
Non-detects
%Solids < 10.0%
Use professional judgment
Use professional judgment
10.0% <%Solids< 30.0%
Use professional judgment
Use professional judgment
%Solids > 30.0%
No qualification
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. (SOW
SOM02.4 - Exhibit B, Section 3.4 and Exhibit D/Low/Med VOA, Sections 11.1.2 and 11.2.3)
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 (NIST) (2011 release or later), 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 an 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
"probable 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.
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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
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 (straight-chain or branched) or CnFhn (cyclic)
that contains 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 an 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 is not performed for all contractually-required peaks,
the EPA Regional CLP COR 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 EPA Regional CLP COR action.
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XIII. System Performance
A. Review Items
Form 8A-OR and chromatograms. (SOW SOM02.4 - Exhibit B, Section 3.4 and Exhibit D/Low/Med
VOA, Section 11.1)
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 EPA
Regional CLP COR action.
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XIV. Performance Evaluation Sample
A. Review Items
Form 1A-OR, TR/COC Record documentation, preparation logs, instrument printouts, and raw data.
(SOW SOM02.4 - Exhibit B, Section 3.4 and Exhibit F, Section 4.1)
B. Objective
The objective is to determine the validity of the analytical results based on the recovery of the PE
sample(s).
C. Criteria
1. Matrix-specific PE samples shall be analyzed utilizing the same analytical methods and Quality
Assurance/Quality Control (QA/QC) procedures as employed for the samples, at a frequency to be
determined by each EPA Region for each site. PE samples must be analyzed in an SDG containing
field samples for the Case, using the same procedures, reagents, and instrumentation.
D. Evaluation
1. Verify, using Form 1A-OR, preparation logs, and raw data, that the PE samples were analyzed with
the field samples and field blanks in the SDG.
2. Verify, using Form 1A-OR, that the PE sample results are within the warning limits (95%
confidence interval) and action limits (99% confidence interval).
3. If a significant number (i.e., half or more) of the analytes in the PE samples fall outside of the 95%
warning or 99% action criteria, or a number of false positive results are reported, evaluate the
overall impact on the data.
E. Action
NOTE: If the PE sample criteria are not met, the laboratory performance and method accuracy are
in question. Use professional judgment to determine if the data should be qualified or
rejected. The following guidance is suggested for qualifying sample data associated with a
PE sample that does not meet the required criteria.
For a PE sample that does not meet the technical criteria, apply the action to all samples in
the same preparation batch. If the concentration of any analyte in a PE sample is not
comparable to the analyte's concentration in the field samples or field blanks (i.e., it is
much higher or much lower than the concentration in these samples), the action may be
applied to only those samples in which the analyte's concentration is comparable to the PE
sample concentration.
1. If the PE sample was not analyzed with the field samples and field blanks, use professional
judgment to determine if the associated sample results should be qualified. Obtain additional
information from the laboratory, if necessary. If a laboratory fails to analyze the PE sample(s)
provided with field samples and field blanks, or if a laboratory consistently fails to generate
acceptable PE sample results, record the situation in the Data Review Narrative, and note it for EPA
Regional CLP COR action.
2. If the PE sample results are outside the lower warning limits but inside the lower action limits,
qualify detects as estimated low (I-) and non-detects as estimated (UI).
3. If the PE sample results are outside the lower action limits, qualify detects as estimated low (I-) and
non-detects as unusable (R).
4. If the PE sample results are within the limits, detects and non-detects should not be qualified.
5. If the PE sample results are outside the upper warning limits but inside the upper action limits,
qualify detects as estimated high (I+). Non-detects should not be qualified.
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6. If the PE sample results are outside the upper action limits, qualify detects as estimated high (J+).
Non-detects should not be qualified.
7. Annotate the potential effects on the data due to out-of-control PE sample results in the Data
Review Narrative.
Table 30. PE Sample Actions for Low/Medium Volatile Analysis
Criteria
Action
Detect
Non-detect
PE sample results outside lower warning limits but inside
lower action limits
J-
UJ
PE sample results outside lower action limits
J-
R
PE sample results within limits
No qualification
No qualification
PE sample results outside upper warning limits but inside
upper action limits
J+
No qualification
PE sample results outside upper action limits
J+
No qualification
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XV. Regional Quality Assurance and Quality Control
A. Review Items
Form 1A-OR, chromatograms, TR/COC Record documentation, quantitation reports, and other raw
data from QA/QC samples. (SOW SOM02.4 - Exhibit B, Sections 2.4 and 3.4)
B. Objective
The objective is to use results from the analysis of EPA Regional QA/QC samples such as field
duplicates, blind spikes, and blind blanks to determine the validity of the analytical results.
C. Criteria
Criteria are determined by each EPA Region.
1. The frequency of EPA Regional QA/QC samples should be defined in the project QAPP.
2. Performance criteria for EPA Regional QA/QC samples should also be defined in the project
QAPP.
3. The EPA Region may provide the laboratory with PE samples to be analyzed with each SDG.
These samples may include blind spikes and/or blind blanks. The laboratory must analyze a PE
sample when provided by the EPA Region. Refer to Section VI, above, for blanks criteria. Refer to
Section XIV, above, for PE samples criteria.
4. The RPD between field duplicates shall fall with the specific limits in the EPA Region's SOP or
project QAPP.
D. Evaluation
1. Evaluation procedures must follow the EPA Region's SOP for data review.
2. Determine whether the results of EPA Regional QA/QC samples impact all samples in the project
or only those directly associated (i.e., in the same SDG, collected on the same day, prepared
together, or contained in the same analytical sequence).
3. 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 EPA Region's SOP or
project QAPP.
4. Determine whether poor precision is the fault of the laboratory, or a result of sample
non-homogeneity in the field. Laboratory observations of sample appearance may become
important in these situations.
E. Action
1. Any action must be in accordance with EPA Regional specifications and the criteria for acceptable
field duplicate sample results.
2. Note unacceptable results for field duplicate samples for EPA Regional CLP COR action.
3. In general, for EPA Regional QA/QC performance not within QAPP specification, qualify detects
as estimated (J) and non-detects as estimated (UJ). The impact on overall data quality should be
assessed after consultation with the data user and/or field personnel. Contact the EPA Regional
CLP COR if reanalysis of samples is required.
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XVI. 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 equations, as
listed in the method. All sample results must be within the linear calibration ranges per the
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 Data Reporting 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 EPA Regional CLP COR 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 (SVOA) organic data requirements to be reviewed during validation are listed below:
I. Preservation and Holding Times 107
II. Gas Chromatograph/Mass Spectrometer Instrument Performance Check Ill
III. Initial Calibration 119
IV. Initial Calibration Verification 126
V. Continuing Calibration Verification 129
VI. Blanks 132
VII. Deuterated Monitoring Compound 135
VIII. Matrix Spike/Matrix Spike Duplicate 139
IX. Gel Permeation Chromatography Performance Check 141
X. Internal Standard 143
XI. Target Analyte Identification 146
XII. Target Analyte Quantitation and Reported Contract Required Quantitation Limit 148
XIII. Tentatively Identified Compounds 150
XIV. System Performance 153
XV. Performance Evaluation Sample 154
XVI. Regional Quality Assurance and Quality Control 156
XVII. Overall Assessment of Data 157
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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) Record documentation, Form
DC-1, raw data, sample extraction sheets, and the Sample Delivery Group (SDG) Narrative checking
for: pH, shipping container temperature, holding time, and other sample conditions. (SOW SOM02.4 -
Exhibit B, Section 3.4; Exhibit D/Introduction, Section 5.0; Exhibit D/General, Sections 8.0, 10.1.2.1,
and 10.2.2.4.4; and Exhibit D/SVOA, Section 8.0)
B. Objective
The objective is to determine the validity of the analytical results based on the sample conditions 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 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. 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 filtrate
samples, and TCLP/SPLP leachate samples that are properly preserved is 7 days.
5. The extraction technical holding time criteria for soil/sediment 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 and
aqueous filtrate sample extracts, is 40 days.
D. Evaluation
1. Review the SDG Narrative and the TR/COC Record 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, Form 1B-OR,
and the raw data are identical.
3. Establish extraction technical holding times for samples, excluding TCLP/SPLP leachate samples,
by comparing the sample collection dates on the TR/COC Record documentation with the dates of
extraction on Form 1A-OR, Form 1B-OR, and the sample extraction sheets.
4. Establish extraction technical holding times for TCLP/SPLP leachate samples by comparing the
sample collection dates on the TR/COC Record documentation with the dates of extraction on
sample extraction sheets.
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5. Establish extraction technical holding times for TCLP/SPLP leachate samples by comparing the
dates of TCLP/SPLP extraction on the extraction sheets with the dates of extraction on Form
1A-OR, Form IB-OR, and the preparation 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 extraction is performed within the 14-day extraction technical holding time for
preserved and not properly preserved soil/sediment samples designated for TCLP/SPLP, detects
and non-detects should not be qualified.
3. If TCLP/SPLP extraction is performed outside the 14-day extraction technical holding time for
preserved and not properly preserved soil/sediment 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 the
raw data, perform a more comprehensive review, contacting the laboratory if necessary through the
United States Environmental Protection Agency Regional Contract Laboratory Program
Contracting Officer's Representative (EPA Regional CLP COR), to determine the correct dates for
establishing the technical holding time.
5. If an aqueous sample, TCLP/SPLP aqueous filtrate 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 sample, TCLP/SPLP aqueous filtrate sample, or TCLP/SPLP leachate sample is not
properly preserved, extraction is performed outside the 7-day technical holding time, and/or 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 sample, TCLP/SPLP aqueous filtrate 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 sample, TCLP/SPLP aqueous filtrate sample, or TCLP/SPLP leachate sample is
properly preserved, extraction is performed outside the 7-day technical holding time, and/or the
extract is analyzed outside the 40-day technical holding time, consider all evidence of
compromised extract integrity (such as evaporation or 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/or the extract is analyzed outside the 40-day technical holding time,
use professional judgment to qualify detects and non-detects.
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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.
12. If a non-aqueous sample is properly preserved, extraction is performed outside the 14-day technical
holding time, and/or 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 EPA Regional CLP
COR action. Annotate the effect of the holding time exceedance on the resulting data in the Data
Review Narrative, whenever possible.
Table 31. Preservation and Holding Time Actions for Semivolatile Analysis
Matrix
Preserved
Criteria
Action
Detect
Non-detect
< 7 days (for extraction) and
< 40 days (for analysis)
No
TCLP/SPLP aqueous filtrate
sample and TCLP/SPLP
leachate sample extracted
within the 7-day technical
holding time
Use professional
judgment
Use professional
judgment
> 7 days (for extraction) and/or
> 40 days (for analysis)
Aqueous
No
TCLP/SPLP aqueous filtrate
sample and TCLP/SPLP
leachate sample not extracted
within the 7-day technical
holding time
J
R
< 7 days (for extraction) and
< 40 days (for analysis)
Yes
TCLP/SPLP aqueous filtrate
sample and TCLP/SPLP
leachate sample extracted
within the 7-day technical
holding time
No qualification
No qualification
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Matrix
Preserved
Criteria
Action
Detect
Non-detect
Aqueous
Yes
> 7 days (for extraction) and/or
> 40 days (for analysis)
Use professional
judgment
Use professional
judgment
TCLP/SPLP aqueous filtrate
sample and TCLP/SPLP
leachate sample not extracted
within the 7-day technical
holding time
Yes/No
Holding time grossly exceeded
J-
Use professional
judgment
R
Non-aqueous
No
<14 days (for extraction) and
< 40 days (for analysis)
Use professional
judgment
Use professional
judgment
No
>14 days (for extraction) and/or
> 40 days (for analysis)
Use professional
judgment
Use professional
judgment
Yes
<14 days (for extraction) and
< 40 days (for analysis)
No qualification
No qualification
Yes
>14 days (for extraction) and/or
> 40 days (for analysis)
J-
R
Yes/No
Holding time grossly exceeded
J-
Use professional
judgment
R
Table 32. Holding Time Actions for Non-Aqueous Semivolatile TCLP/SPLP Sample Analysis
Preserved
Criteria
Action
Detect
Non-detect
No
TCLP/SPLP extraction
performed within the
14-day technical holding
time
No qualification
No qualification
No
TCLP/SPLP extraction not
performed within the
14-day technical holding
time
J-
R
Yes
TCLP/SPLP extraction
performed within the
14-day technical holding
time
No qualification
No qualification
Yes
TCLP/SPLP extraction not
performed within the
14-day technical holding
time
J-
R
Yes/No
Holding time grossly
exceeded
J-
Use professional
judgment
R
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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. (SOW SOM02.4
- Exhibit B, Section 3.4 and Exhibit D/SVOA, Section 9.2)
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 the injection of DFTPP; however, 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.
• Initial Calibration Verification
(ICV) meets ICV 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.
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Conditions for When
Example Sequence is
Appropriate:
Acceptable Criteria That Must
Be Met:
Notes:
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.
• ICV meets ICV 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.
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:
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 2/
Beginning of 12-hour clock
for Analytical Sequence 3
0 hr DFTPP
Initial Calibration 5.0
Initial Calibration 10
Initial Calibration 20
Initial Calibration 40
Initial Calibration 80
ICV
Method Blank
Subsequent Samples
12 hr CCV ^ (meets opening CCV
criteria)
Method Blank
Subsequent Samples
24 hr CCV B (meets opening CCV
criteria)
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
0 hr DFTPP
End of 12-hour clock for
Analytical Sequence 1
Beginning of 12-hour clock
for Analytical Sequence 2
12 hr
End of 12-hour clock for
Analytical Sequence 2
25 hr
Initial Calibration 5.0
Initial Calibration 10
Initial Calibration 20
Initial Calibration 40
Initial Calibration 80
ICV
Method Blank
Subsequent Samples
CCV A (meets closing CCV
criteria, fails opening CCV
criteria)
13 hr DFTPP
CCV B (meets opening CCV
criteria)
Method Blank
Subsequent Samples
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
End of 12-hour clock for
Analytical Sequence 1/
Beginning of 12-hour clock
for Analytical Sequence 2
0 hr DFTPP
CCV A (meets opening CCV
criteria)
Method Blank
Subsequent Samples
12 hr CCV ® (meets opening CCV
criteria)
Method Blank
Subsequent Samples
1/2
2
2
2
2
2
End of 12-hour clock for
Analytical Sequence 2/
Beginning of 12-hour clock
for Analytical Sequence 3
24 hr CCV C (meets opening CCV
criteria)
2/3
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Example 4:
Example 4:
Time Material Injected
Analytical Sequence #
Start of 12-hour clock for
Analytical Sequence 1
0 hr DFTPP
CCV A (meets opening CCV
criteria)
Method Blank
Subsequent Samples
End of 12-hour clock for
Analytical Sequence 1
Beginning of 12-hour clock
for Analytical Sequence 2
CCV B (meets closing CCV
12 hr criteria, fails opening CCV
criteria)
13 hr DFTPP
CCV C (meets opening CCV
criteria)
Method Blank
Subsequent Samples
2
2
2
2
2
End of 12-hour clock for
Analytical Sequence 2/
Beginning of 12-hour clock
for Analytical Sequence 3
25 hr CCV D (meets opening CCV
criteria)
2/3
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2. The DFTPP instrument performance check must meet the ion abundance criteria listed in Table 33.
Table 33. Ion Abundance Criteria for DFTPP
Mass
Ion Abundance Criteria
51
10.0-80.0% of mass 198
68
Less than 2.0% of mass 69
69
Present
70
Less than 2.0% of mass 69
127
10.0-80.0% of mass 198
197
Less than 2.0% of mass 198
198
Base peak, 100% relative abundance*
199
5.0 -9.0% of mass 198
275
10.0 -60.0% of mass 198
365
Greater than 1.0% of mass 198
441
Present, but less than mass 443
442
Greater than 50.0% of mass 198
443
15.0 -24.0% of mass 442
* All ion abundances must be normalized to m/z 198, the nominal base peak, even though the ion
abundance of m/z 442 may exceed that of m/z 198.
D. Evaluation
1. Verify that the 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 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 ion abundance 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 198/199 and 442/443. For the 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 acquired within 20 scans of
the elution of DFTPP, but the DFTPP 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 CLP, information regarding noncompliant 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 the 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 EPA Regional CLP
COR should be contacted to arrange for 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 action is required.
3. If the laboratory failed to provide the correct forms, or if significant transcription or calculation
errors are found, notify the EPA Regional CLP COR, 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 EPA Regional CLP COR.
4. If the 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 the ion abundance criteria in Table 33 are not met, use professional judgment to qualify detects
and non-detects in the associated samples.
6. If the 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 the 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 noncompliant 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 EPA Regional CLP COR action.
For example, the issue shall be noted for the EPA Regional CLP COR 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. (SOW SOM02.4 - Exhibit B, Section 3.4 and
Exhibit D/SVOA, Sections 7.2.2.1 and 9.3)
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 the ICV, 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-one target analytes and
six DMCs listed in Section C.l.c, and DMC 1,4-Dioxane-ds. For 1,4-Dioxane and
l,4-Dioxane-d8, the calibration standard concentrations are at 2.0, 4.0, 8.0, 16, and 32 ng/ |_iL.
c. The ICAL standard concentrations are at 10, 20, 40, 80, and 160 ng/(.iL for twenty-one target
analytes and six DMCs: Benzaldehyde, Phenol, Bis(2-chloroethyl) ether, 2-Methylphenol,
2,2'-Oxybis(l-chloropropane), Acetophenone, 4-Chloroaniline, Caprolactam,
Hexachlorocyclopentadiene, Atrazine, Carbazole, Fluoranthene, 3,3'-Dichlorobenzidine,
Di-n-octylphthalate, 2,4-Dinitrophenol, PCP, 4-Methylphenol, 4,6-Dinitro-2-methylphenol,
3-Nitroaniline, 4-Nitroaniline, 4-Nitrophenol, Phenol-ds, Bis(2-chloroethyl) ether-ds,
4-Methylphenol-ds, 4-Chloroaniline-d4, 4-Nitrophenol-d4, and 4,6-Dinitro-2-methylphenol-d2.
For the optional analysis of Polycyclic 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 RRF (RRF), and 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 34.
4. The %RSD of the ICAL RRF for each target analyte and DMC must be < Maximum %RSD value
in Table 34.
NOTE: The technical acceptance criteria specified in a "Request for Quote (RFQ) for Solicitation"
of a Modified Analysis may impact some of the preceding evaluation criteria. A copy of
this document should be present in the Complete SDG File (CSF), when applicable.
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.
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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 %RSDs 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 34 for each target analyte and DMC.
5. Verify that the %RSD is < Maximum %RSD value in Table 34 for each target analyte and DMC.
NOTE: For data obtained from the CLP, information regarding noncompliant 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, use professional judgment to
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 %RSDs, perform a more
comprehensive recalculation.
4. If the RRF is < Minimum RRF value in Table 34 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 34 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 34 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 34 for any target analyte, 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
necessary. The following guidelines are recommended:
a. If the %RSD criteria of any target analytes are not met and the %RSD criteria are still not
satisfied after eliminating either the high or the low-point of the ICAL:
i. Qualify detects in the associated samples as estimated (J).
ii. Use professional judgment to qualify non-detects in the associated samples.
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 EPA Regional CLP
COR, 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 EPA Regional CLP COR action.
Table 34. RRF, %RSD, and %D Acceptance Criteria in Initial Calibration, ICV, and CCV for
Semivolatile Analysis
Analyte
Minimum
RRF
Maximum
%RSD
ICV/Opening
CCV
Maximum
%D'
Closing
CCV
Maximum
%D
1,4-Dioxane
0.010
40.0
±40.0
±50.0
Benzaldehyde
0.100
40.0
±40.0
±50.0
Phenol
0.080
20.0
±20.0
±25.0
Bis(2-chloroethyl) ether
0.100
20.0
±20.0
±25.0
2-Chlorophenol
0.200
20.0
±20.0
±25.0
2-Methylphenol
0.010
20.0
±20.0
±25.0
3-Methylphenol
0.010
20.0
±20.0
±25.0
2,2'-Oxybis-( 1 -chloropropane)
0.010
20.0
±25.0
±50.0
Acetophenone
0.060
20.0
±20.0
±25.0
4-Methylphenol
0.010
20.0
±20.0
±25.0
N-Nitroso-di-n-propylamine
0.080
20.0
±25.0
±25.0
Hexachloroethane
0.100
20.0
±20.0
±25.0
Nitrobenzene
0.090
20.0
±20.0
±25.0
Isophorone
0.100
20.0
±20.0
±25.0
2-Nitrophenol
0.060
20.0
±20.0
±25.0
2,4-Dimethylphenol
0.050
20.0
±25.0
±50.0
Bis(2-chloroethoxy) methane
0.080
20.0
±20.0
±25.0
2,4-Dichlorophenol
0.060
20.0
±20.0
±25.0
Naphthalene
0.200
20.0
±20.0
±25.0
4-Chloroaniline
0.010
40.0
±40.0
±50.0
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Analyte
Minimum
RRF
Maximum
%RSD
ICV/Opening
CCV
Maximum
%D'
Closing
CCV
Maximum
%D
Hexachlorobutadiene
0.040
20.0
±20.0
±25.0
Caprolactam
0.010
40.0
±30.0
±50.0
4-Chloro-3 -methylphenol
0.040
20.0
±20.0
±25.0
2-Methylnaphthalene
0.100
20.0
±20.0
±25.0
Hexachlorocyclopentadiene
0.010
40.0
±40.0
±50.0
2,4,6-Trichlorophenol
0.090
20.0
±20.0
±25.0
2,4,5-Trichlorophenol
0.100
20.0
±20.0
±25.0
l,l'-Biphenyl
0.200
20.0
±20.0
±25.0
2-Chloronaphthalene
0.300
20.0
±20.0
±25.0
2-Nitroaniline
0.060
20.0
±25.0
±25.0
Dimethylphthalate
0.300
20.0
±20.0
±25.0
2,6-Dinitrotoluene
0.080
20.0
±20.0
±25.0
Acenaphthylene
0.400
20.0
±20.0
±25.0
3-Nitroaniline
0.010
20.0
±25.0
±50.0
Acenaphthene
0.200
20.0
±20.0
±25.0
2,4-Dinitrophenol
0.010
40.0
±50.0
±50.0
4-Nitrophenol
0.010
40.0
±40.0
±50.0
Dibenzofuran
0.300
20.0
±20.0
±25.0
2,4-Dinitrotoluene
0.070
20.0
±20.0
±25.0
Diethylphthalate
0.300
20.0
±20.0
±25.0
1,2,4,5-Tetrachlorobenzene
0.100
20.0
±20.0
±25.0
4-Chlorophenyl-phenylether
0.100
20.0
±20.0
±25.0
Fluorene
0.200
20.0
±20.0
±25.0
4-Nitroaniline
0.010
40.0
±40.0
±50.0
4,6-Dinitro-2-methylphenol
0.010
40.0
±30.0
±50.0
4-Bromophenyl-phenyl ether
0.070
20.0
±20.0
±25.0
N-Nitrosodiphenylamine
0.100
20.0
±20.0
±25.0
Hexachlorobenzene
0.050
20.0
±20.0
±25.0
Atrazine
0.010
40.0
±25.0
±50.0
Pentachlorophenol
0.010
40.0
±40.0
±50.0
Phenanthrene
0.200
20.0
±20.0
±25.0
Anthracene
0.200
20.0
±20.0
±25.0
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Analyte
Minimum
RRF
Maximum
%RSD
ICV/Opening
CCV
Maximum
%D'
Closing
CCV
Maximum
%D
Carbazole
0.050
20.0
±20.0
±25.0
Di -n-butylphthalate
0.500
20.0
±20.0
±25.0
Fluoranthene
0.100
20.0
±20.0
±25.0
Pyrene
0.400
20.0
±25.0
±50.0
Butylbenzylphthalate
0.100
20.0
±25.0
±50.0
3,3 '-Dichlorobenzidine
0.010
40.0
±40.0
±50.0
Benzo(a)anthracene
0.300
20.0
±20.0
±25.0
Chrysene
0.200
20.0
±20.0
±50.0
Bis(2-ethylhexyl) phthalate
0.200
20.0
±25.0
±50.0
Di -n-octylphthalate
0.010
40.0
±40.0
±50.0
Benzo(b)fluoranthene
0.010
20.0
±25.0
±50.0
Benzo(k)fluoranthene
0.010
20.0
±25.0
±50.0
Benzo(a)pyrene
0.010
20.0
±20.0
±50.0
Indeno( 1,2,3 -cd)pyrene
0.010
20.0
±25.0
±50.0
Dibenzo(a,h)anthracene
0.010
20.0
±25.0
±50.0
Benzo(g,h,i)perylene
0.010
20.0
±30.0
±50.0
2,3,4,6-Tetrachlorophenol
0.040
20.0
±20.0
±50.0
Selective Ion Monitoring
Naphthalene
0.600
20.0
±25.0
±25.0
2-Methylnaphthalene
0.300
20.0
±20.0
±25.0
Acenaphthylene
0.900
20.0
±20.0
±25.0
Acenaphthene
0.500
20.0
±20.0
±25.0
Fluorene
0.700
20.0
±25.0
±50.0
Phenanthrene
0.300
20.0
±25.0
±50.0
Anthracene
0.400
20.0
±25.0
±50.0
Fluoranthene
0.400
20.0
±25.0
±50.0
Pyrene
0.500
20.0
±30.0
±50.0
Benzo(a)anthracene
0.400
20.0
±25.0
±50.0
Chrysene
0.400
20.0
±25.0
±50.0
Benzo(b)fluoranthene
0.100
20.0
±30.0
±50.0
Benzo(k)fluoranthene
0.100
20.0
±30.0
±50.0
Benzo(a)pyrene
0.100
20.0
±25.0
±50.0
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Analyte
Minimum
RRF
Maximum
%RSD
ICV/Opening
CCV
Maximum
%D'
Closing
CCV
Maximum
%D
Indeno( 1,2,3 -cd)pyrene
0.100
20.0
±40.0
±50.0
Dibenzo(a,h)anthracene
0.010
25.0
±40.0
±50.0
Benzo(g,h,i)perylene
0.020
25.0
±40.0
±50.0
Pentachlorophenol
0.010
40.0
±50.0
±50.0
Deuterated Monitoring Compounds
1,4-Dioxane-ds
0.010
20.0
±25.0
±50.0
Phenol-ds
0.010
20.0
±25.0
±25.0
Bis-(2-chloroethyl) ether-ds
0.100
20.0
±20.0
±25.0
2-Chlorophenol-d4
0.200
20.0
±20.0
±25.0
4-Methylphenol-ds
0.010
20.0
±20.0
±25.0
4-Chloroaniline-d4
0.010
40.0
±40.0
±50.0
Nitrobenzene-ds
0.050
20.0
±20.0
±25.0
2-Nitrophenol-d4
0.050
20.0
±20.0
±25.0
2,4-Dichlorophenol-d3
0.060
20.0
±20.0
±25.0
Dimethylphthalate-d6
0.300
20.0
±20.0
±25.0
Acenaphthylene-ds
0.400
20.0
±20.0
±25.0
4-Nitrophenol-d4
0.010
40.0
±40.0
±50.0
Fluorene-dio
0.100
20.0
±20.0
±25.0
4,6-Dinitro-2-methylphenol-d2
0.010
40.0
±30.0
±50.0
Anthracene-dio
0.300
20.0
±20.0
±25.0
Pyrene-dio
0.300
20.0
±25.0
±50.0
Benzo(a)pyrene-di2
0.010
20.0
±20.0
±50.0
Fluoranthene-dio (SIM)
0.400
20.0
±25.0
±50.0
2-Methylnaphthalene-dio (SIM)
0.300
20.0
±20.0
±25.0
1 If a closing CCV is acting as an opening CCV, all target analytes must meet the requirements for an
opening CCV.
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Table 35. Initial Calibration Actions for Semivolatile Analysis
Criteria
Action
Detect
Non-detect
Initial Calibration not performed at the specified
frequency and sequence
Use professional
judgment
R
Use professional
judgment
R
Initial Calibration not performed at the specified
concentrations
J
UJ
RRF < Minimum RRF in Table 34 for target
analyte
Use professional
judgment
J+ or R
R
RRF > Minimum RRF in Table 34 for target
analyte
No qualification
No qualification
%RSD > Maximum %RSD in Table 34 for target
analyte
J
Use professional
judgment
%RSD < Maximum %RSD in Table 34 for target
analyte
No qualification
No qualification
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IV. Initial Calibration Verification
A. Review Items
Form 7A-OR, quantitation reports, and chromatograms. (SOW SOM02.4 - Exhibit B, Section 3.4 and
Exhibit D/SVOA, Sections 7.2.2.2 and 9.4)
B. Objective
The objective is to ensure that the instrument is calibrated accurately to produce acceptable qualitative
and quantitative data throughout each analytical sequence by the use of a second-source check
standard.
C. Criteria
1. The accuracy of the calibration for each GC/MS system used for analysis must be verified at the
frequency of one ICV standard analysis per initial calibration analytical sequence. The ICV is
analyzed after the last ICAL standard analysis and prior to a blank, sample, or an applicable CCV
analysis.
2. The ICV standard must contain all required target analytes, from an alternate source or a different
lot than that used for the ICAL standards and DMCs, at or near the mid-point concentration (CS3)
of the ICAL.
3. For an ICV, the RRFs for each target analyte and DMC must be > the Minimum RRF values in
Table 34.
4. The Percent Difference (%D) between the ICAL RRF and the ICV RRF must be within the
ICV/Opening CCV Maximum %D limits in Table 34 for each target analyte and DMC.
D. Evaluation
1. Verify that the ICV standard is analyzed at the specified frequency and sequence, and that it is
associated with 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 concentrations of the target analytes and the DMCs in the ICV are at or near the
mid-point standard CS3 from the ICAL.
3. Verify that the RRF and %D for each target analyte and DMC are reported on Form 7A-OR.
Recalculate the 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. Verify that the RRFs for each target analyte and DMC in the ICV are > Minimum RRF values in
Table 34.
5. Verify that the %Ds are within the ICV/Opening CCV Maximum %D limits in Table 34 for each
target analyte and DMC.
NOTE: For data obtained from the CLP, information regarding the noncompliant ICV can be
obtained from the NFG reports and may be used as part of the evaluation process.
E. Action
1. If the ICV is not performed at the specified frequency, use professional judgment to qualify detects
and non-detects. Contact the EPA Regional CLP COR 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 quality of analyte peak
shapes and mass spectral matches, the 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.
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2. If the ICV 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. If the RRF in an ICV is < Minimum RRF value in Table 34 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).
a. Take special note of any extreme deviation in the RRF and evaluate RT data, peak shapes, and
areas of the target analytes and associated internal standards for inconsistencies that may
indicate a chromatographic co-elution. If this is suspected, the contaminant may also be
present in samples and blanks. Also review the documentation of the preparation of the ICV
standard. Use professional judgment to qualify affected data appropriately.
5. If the RRF in an ICV is > Minimum RRF value in Table 34 for any target analyte, detects and
non-detects should not be qualified.
6. If the %D in an ICV is outside the ICV/Opening CCV Maximum %D limits in Table 34 for any
target analyte, qualify detects as estimated (J) and non-detects as estimated (UJ).
7. If the %D in an ICV is within the inclusive range of the ICV/Opening CCV Maximum %D limits in
Table 34 for any target analyte, detects and non-detects should not be qualified.
8. No qualification of the data is necessary based on the 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.
9. If the laboratory has failed to provide adequate calibration information, contact the EPA Regional
CLP COR, who may contact the laboratory to request the necessary information. If the information
is not available, use professional judgment to assess the data. Refer to E. 1, above, for additional
steps.
10. Note the potential effects on the data due to ICV criteria exceedance in the Data Review Narrative.
11. If the ICV criteria are grossly exceeded, note this for EPA Regional CLP COR action.
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Table 36. ICV Actions for Semivolatile Analysis
Criteria for ICV
Action
Detect
Non-detect
ICV not performed at the specified
frequency and sequence
Use professional
judgment
Use professional
judgment
ICV not performed at the specified
concentration
Use professional
judgment
Use professional
judgment
RRF < Minimum RRF in Table 34 for
target analyte
Use professional
judgment
J or R
R
RRF > Minimum RRF in Table 34 for
target analyte
No qualification
No qualification
%D outside the ICV/Opening CCV
Maximum %D limits in Table 34 for
target analyte
J
UJ
%D within the inclusive ICV/Opening
CCV Maximum %D limits in Table 34
for target analyte
No qualification
No qualification
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V. Continuing Calibration Verification
A. Review Items
Form 7A-OR, quantitation reports, and chromatograms. (SOW SOM02.4 - Exhibit B, Section 3.4 and
Exhibit D/SVOA, Sections 7.2.2.1 and 9.5)
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 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. The CCV standards must contain all required target analytes and DMCs at or near the mid-point
concentration (CS3) 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 34.
4. The %D between the ICAL RRF and the opening CCV RRF must be within the ICV/Opening CCV
Maximum %D limits in Table 34 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
CCV Maximum %D limits in Table 34 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 it is associated with 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 CS3 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 the 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 each target analyte and DMC are
> Minimum RRF values in Table 34.
5. For an opening CCV, verify that the %Ds are within the ICV/Opening CCV Maximum %D limits
in Table 34 for each target analyte and DMC.
6. For a closing CCV, verify that the %Ds are within the Closing CCV Maximum %D limits in Table
34 for each target analyte and DMC.
NOTE: For data obtained from the CLP, information regarding the noncompliant CCV 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 CCV is not performed at the specified frequency, qualify detects and non-detects as unusable
(R). Contact the EPA Regional CLP COR 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 quality of analyte peak shapes and
mass spectral matches, the stability of internal standard 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 < Minimum RRF value in Table 34 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).
a. Take special note of any extreme deviation in the RRF and evaluate RT data, peak shapes, and
areas of the target analytes and associated internal standards for inconsistencies that may
indicate a chromatographic co-elution. If this is suspected, the contaminant may also be
present in samples and blanks. Also review the documentation of the preparation of the CCV
standard. Use professional judgment to qualify affected data appropriately.
5. For opening or a closing CCV, if the RRF is > Minimum RRF value in Table 34 for any target
analyte, detects and non-detects should not be qualified.
6. For an opening CCV, if the %D is outside the ICV/Opening CCV Maximum %D limits in Table 34
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 CCV Maximum %D limits in Table 34 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 ICV/Opening CCV Maximum
%D limits in Table 34 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 CCV Maximum %D limits
in Table 34 for any target analyte, detects and non-detects should not be qualified.
10. No qualification of the data is necessary based on the 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 EPA Regional
CLP COR, who may contact the laboratory to request the necessary information. If the information
is not available, use professional judgment to assess the data. Refer to E. 1, above, for additional
steps.
12. Note the potential effects on the data due to CCV criteria exceedance in the Data Review Narrative.
13. If the CCV criteria are grossly exceeded, note this for EPA Regional CLP COR action.
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Table 37. CCV Actions for Semivolatile Analysis
Criteria for Opening CCV
Criteria for Closing CCV
Action
Detect
Non-detect
CCV not performed at the
specified frequency and sequence
CCV not performed at the
specified frequency
Use
professional
judgment
J or R
Use
professional
judgment
UJ orR
CCV not performed at the
specified concentration
CCV not performed at the
specified concentration
Use
professional
judgment
Use
professional
judgment
Use
RRF < Minimum RRF in Table 34
for target analyte
RRF < Minimum RRF in Table 34
for target analyte
professional
judgment
J or R
R
RRF > Minimum RRF in Table 34
for target analyte
RRF > Minimum RRF in Table 34
for target analyte
No
qualification
No
qualification
%D outside the ICV/Opening
CCV Maximum %D limits in
Table 34 for target analyte
%D outside the Closing CCV
Maximum %D limits in Table 34
for target analyte
J
UJ
%D within the inclusive
ICV/Opening CCV Maximum
%D limits in Table 34 for target
analyte
%D within the inclusive Closing
CCV Maximum %D limits in
Table 34 for target analyte
No
qualification
No
qualification
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VI. Blanks
A. Review Items
Form 1A-OR, Form 1B-OR, Form 4-OR, chromatograms, and quantitation reports. (SOW SOM02.4 -
Exhibit B, Section 3.4 and Exhibit D/SVOA, Section 12.1)
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 semivolatile 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 blank analyses 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 Leachate Extraction Blank (LEB) 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 blanks must be < 5.0 ug/L for water (0.0050 mg/L
for TCLP leachate) or 170 ug/kg for soil/sediment 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 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. 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 noncompliant 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 EPA Regional CLP COR 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) or EPA 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 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 at sample 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 LEBs and field blanks, sample result qualifications listed in Table 38 should apply
if supported by the project QAPP.
7. If gross contamination exists with blank results that are > ICAL CS5 concentrations, qualify detects
as unusable (R). If the contamination is suspected of having an effect on the sample results, note it
for EPA Regional CLP COR action.
8. For any blank (including method blank) reported with TICs (non-target compounds) concentrations
that are >5.0 ug/L for water (0.0050 mg/L for TCLP leachate) and 170 ug/kg for soil/sediment
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 38. Blank and TCLP/SPLP LEB Actions for Semivolatile Analysis
Blank Type
Blank Result
Sample Result
Action
Detect
Non-detect
No qualification
< CRQL
< CRQL
Report at CRQL and qualify
as non-detect (U)
> CRQL
Use professional judgment
< CRQL
Report at CRQL and qualify
as non-detect (U)
Method,
> CRQL
> CRQL but < Blank Result
Report at sample result and
qualify as non-detect (U) or as
unusable (R)
TCLP/SPLP
LEB, Field
> CRQL and > Blank Result
Use professional judgment
Gross
contamination
Detect
Report at sample result and
qualify as unusable (R)
TIC >5.0 ug/L
(water) or 0.0050
mg/L (TCLP
leachate)
or
TIC >170 ug/kg
(soil/sediment)
Detect
Use professional judgment
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VII. Deuterated Monitoring Compound
A. Review Items
Form 2A-OR, Form 2B-OR quantitation reports, and chromatograms. (SOW SOM02.4 - Exhibit B,
Section 3.4 and Exhibit D/SVOA, Sections 7.2.2.5 and 11.2.4)
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 39, prior to the sample extraction
procedure, to measure DMC %R.
2. The %R for each DMC shall be calculated correctly according to the method.
3. The %R for each DMC in samples and blanks must be within the limits in Table 39.
Table 39. Semivolatile DMC Recovery Limits
DMC
%R For Water
Sample
%R For Soil/Sediment
Sample
1,4-Dioxane-ds
40-110
40-110
Phenol-ds
10-130
10 - 130
Bis(2-chloroethyl) ether-ds
25 - 120
10 - 150
2-Chlorophenol-d4
20 - 130
15 - 120
4-Methylphenol-ds
25 - 125
10 - 140
4-Chloroaniline-d4
1 - 146*
1 - 145*
Nitrobenzene-ds
20 - 125
10 - 135
2-Nitrophenol-d4
20 - 130
10-120
2,4-Dichlorophenol-d3
20 - 120
10 - 140
Dimethylphthalate -d6
25 - 130
10 - 145
Acenaphthylene-ds
10 - 130
15 - 120
4-Nitrophenol-d4
10 - 150
10-150
Fluorene-dio
25 - 125
20 - 140
4,6-Dinitro-2-methylphenol-d2
10-130
10 - 130
Anthracene-dio
25 - 130
10 - 150
Pyrene-dio
15 - 130
10 - 130
Benzo(a)pyrene-di2
20-130
10 - 140
Fluoranthene-dio (SIM)
30 - 130
30-130
2-Methylnaphthalene-dio (SIM)
30 - 130
20 - 140
* Limits are advisory.
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D. Evaluation
1. Check the 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.
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 time s.
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 noncompliant 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 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
EPA Regional CLP COR 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 39) in samples, qualify the associated target analytes
listed in Table 41 and SIM target analytes in Table 42 considering the existence of interference in
the raw data. Considerations include, but are not limited to:
a. If the DMC %R in the undiluted sample analysis 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 the DMC %R in the undiluted sample analysis is > 10% (excluding DMCs with 10% as a
lower acceptance limits) and < lower acceptance limit, qualify detects as estimated low (J-) and
non-detects as estimated (UJ).
c. If the DMC %R in the diluted sample analysis is < lower acceptance limit, use professional
judgment to qualify detects and non-detects.
d. If the DMC %R is > lower acceptance limit and < upper acceptance limit, detects and
non-detects should not be qualified.
e. 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 39) 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 EPA Regional CLP COR action.
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Table 40. DMC Actions for Semivolatile Analysis
Criteria
Action
Detect
Non-detect
%R < 10% (excluding DMCs with 10% as a lower
acceptance limit, undiluted sample analysis)
J-
R
10% < %R (excluding DMCs with 10% as a lower
acceptance limit, undiluted sample analysis) < Lower
Acceptance Limit
J-
UJ
%R < Lower Acceptance Limit (diluted sample analysis)
Use professional
judgment
Use professional
judgment
Lower Acceptance limit < %R < Upper Acceptance Limit
No qualification
No qualification
%R > Upper Acceptance Limit
J+
No qualification
Table 41. Semivolatile DMCs and the Associated Target Analytes
1,4-Dioxane-ds (DMC-1)
Phenol-d5(DMC-2)
Bis(2-Chloroethyl) ether-ds
(DMC-3)
1,4-Dioxane
Benzaldehyde
Bis(2-chloroethyl) ether
Phenol
2,2'-Oxybis( 1 -chloropropane)
Bis(2-chloroethoxy) methane
2-Chlorophenol-d4 (DMC-4)
4-Methylphenol-ds (DMC-5)
4-Chloroaniline-d4 (DMC-6)
2-Chlorophenol
2-Methylphenol
3-Methylphenol
4-Methylphenol
2,4-Dimethylphenol
4-Chloroaniline
Nitrobenzene-ds (DMC-7)
2-Nitrophenol-d4 (DMC-8)
2,4-Dichlorophenol-d3 (DMC-9)
Acetophenone
Isophorone
2,4-Dichlorophenol
N-Nitroso-di-n-propylamine
2-Nitrophenol
Hexachlorobutadiene
Hexachloroethane
4-Chloro-3 -methylphenol
Hexachlorocyclopentadiene
2,4,6-Trichlorophenol
Nitrobenzene
2,4,5-Trichlorophenol
2,6-Dinitrotoluene
1,2,4,5-Tetrachlorobenzene
2,4-Dinitrotoluene
* Pentachlorophenol
N-Nitrosodiphenylamine
2,3,4,6-Tetrachlorophenol
3,3 '-Dichlorobenzidine
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Dimethylphthalate-d6 (DMC-10)
Acenaphthylene-ds (DMC-11)
4-Nitrophenol-d4 (DMC-12)
Caprolactam
*Naphthalene
2-Nitroaniline
l,l'-Biphenyl
* 2-Methylnaphthalene
3-Nitroaniline
Dimethylphthalate
2-Chloronaphthalene
2,4-Dinitrophenol
Diethylphthalate
* Acenaphthylene
4-Nitrophenol
Di-n-butylphthalate
*Acenaphthene
4-Nitroaniline
Butylbenzylphthalate
Bis(2-ethylhexyl) phthalate
Di-n-octylphthalate
Fluorene-dio (DMC-13)
4,6-Dinitro-2-methylphenol-d2
(DMC-14)
Anthracene-dio (DMC-15)
Dibenzofuran
4,6-Dinitro-2-methylphenol
Hexachlorobenzene
*Fluorene
Atrazine
4-Chlorophenyl-phenylether
*Phenanthrene
4-Bromophenyl-phenylether
* Anthracene
Carbazole
Pyrene-dio (DMC-16)
Benzo(a)pyrene-di2 (DMC-17)
*Fluoranthene
* Benzo(b)fluoranthene
*Pyrene
* Benzo(k)fluoranthene
* Benzo(a)anthracene
*Benzo(a)pyrene
*Chrysene
* Indeno( 1,2,3 -cd)pyrene
* Dibenzo(a,h)anthracene
* Benzo(g,h,i)perylene
* Included in optional Target Analyte List (TAL) of PAHs and PCP only.
Table 42. Semivolatile SIM DMCs and the Associated Target Analytes
Fluoranthene-dio
(DMC-1)
2-Methylnaphthalene-dio
(DMC-2)
Fluoranthene
Naphthalene
Pyrene
2-Methylnaphthalene
Benzo(a)anthracene
Acenaphthylene
Chrysene
Acenaphthene
Benzo(b)fluoranthene
Fluorene
Benzo(k)fluoranthene
Pentachlorophenol
Benzo(a)pyrene
Phenanthrene
Indeno( 1,2,3 -cd)pyrene
Anthracene
Dibenzo(a,h)anthracene
Benzo(g,h,i)perylene
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VIII. Matrix Spike/Matrix Spike Duplicate
A. Review Items
SDG Cover Page, Form 3A-OR, chromatograms, and quantitation reports. (SOW SOM02.4 - Exhibit
B, Section 3.4 and Exhibit D/SVOA, Sections 7.2.2.6 and 12.2)
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 samples should be analyzed per matrix or per SDG.
NOTE: Data for MS and MSDs will not be present unless requested by the EPA 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 shall be within the acceptance limits in Table 43.
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 3A-OR and verify that they are within the limits listed
in Table 43.
NOTE: For data obtained from the CLP, the preceding criteria, including the requested MS/MSD
spiking analytes and spiking levels specified in Exhibit D - Semivolatile Organic
Compounds Analysis, Section 7.2.2.6.1, of the SOW, are evaluated as part of the CCS
process. Information regarding the noncompliant 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 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 EPA
Regional CLP COR action. It is not likely that data qualification will be warranted if 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 was used for the MS/MSD analysis, note this for EPA Regional CLP
COR 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 the 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 43, 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:
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If the 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).
If the 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).
If the MS/MSD %R or RPD is > lower acceptance limit and < upper acceptance limit, detects
and non-detects should not be qualified.
If the MS/MSD %R or RPD is > upper acceptance limit, qualify detects as estimated (J).
Non-detects should not be qualified.
Table 43. MS/MSD %R and RPD Limits for Semivolatile Analysis
Compound
%R for
Water Sample
RPD for
Water Sample
%R for
Soil/Sediment
Sample
RPD for
Soil/Sediment
Sample
Phenol
12-110
0-42
26-90
0-35
2-Chlorophenol
27 - 123
0-40
25 - 102
0-50
N-Nitroso-di-n-propylamine
41 - 116
0-38
41 - 126
0-38
4-Chloro-3 -methylphenol
23-97
0-42
26 - 103
0-33
Acenaphthene
46-118
0-31
31 - 137
0-19
4-Nitrophenol
10-80
0-50
11 - 114
0-50
2,4-Dinitrotoluene
24-96
0-38
28-89
0-47
Pentachlorophenol
9 - 103
0-50
17-109
0-47
Pyrene
26 - 127
0-31
35 - 142
0-36
Table 44. MS/MSD Actions for Semivolatile Analysis
Criteria
Action
Detect
Non-detect
%R < 10% (excluding spiked analyte with %R lower
limit of 10% or less)
J
R
10% < %R (excluding spiked analyte with %R lower
limit of 10% or less) < Lower Acceptance Limit
J
UJ
Lower Acceptance Limit < %R or RPD < Upper
Acceptance Limit
No qualification
No qualification
%R or RPD > Upper Acceptance Limit
J
No qualification
a.
b.
c.
d.
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IX. 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. (SOW SOM02.4 - Exhibit B, Section 3.4 and Exhibit
D/SVOA, Section 10.3)
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
calibration verification solution fails to meet criteria, 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. 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 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; and 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 EPA Regional CLP COR.
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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 subj ect to erratic performance. The expected result may
be an unknown bias in the data. Contact the EPA Regional CLP COR 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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X. Internal Standard
A. Review Items
Form 8A-OR, quantitation reports, and chromatograms. (SOW SOM02.4 - Exhibit B, Section 3.4 and
Exhibit D/SVOA, Sections 7.2.2.7, 11.3.5, and 11.3.6)
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 compound from the
associated opening CCV or the mid-point standard CS3 from the associated ICAL.
3. The RT of the internal standard compound in the sample or blank must not vary more than ±30.0
seconds from the RT of the same internal standard compound in the associated opening CCV or
mid-point standard CS3 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 RT and area
response of each internal standard compound in a sample or blank are reported on 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 30 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 time s.
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 noncompliant internal standard area response or RT
can be obtained from the NFG reports and may be used as part of the evaluation process.
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E. Action
NOTE: Apply the action to the target analytes in samples or blanks that are associated to the
noncompliant internal standard compound in Table 45. The internal standard and the
associated target analytes are in Exhibit D - Semivolatile Organic Compounds Analysis,
Tables 9 and 10, of the SOW.
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 CS3 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 CS3 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 CS3 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 CS3 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 CS3
from the associated ICAL of an internal standard compound is > 30.0 seconds, qualify detects and
non-detects as unusable (R). The EPA Regional CLP COR should be contacted to arrange for
reanalysis.
8. If the RT shift between sample/blank and the associated opening CCV or mid-point standard CS3
from the associated ICAL of an internal standard compound is < 30.0 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 EPA Regional CLP COR action.
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Table 45. Internal Standard Actions for Semivolatile Analysis
Criteria
Action
Detect
Non-detect
Area response < 20% of the opening CCV or mid-point
standard CS3 from ICAL
J+
R
20% < Area response < 50% of the opening CCV or
mid-point standard CS3 from ICAL
J+
UJ
50% < Area response < 200% of the opening CCV or
mid-point standard CS3 from ICAL
No qualification
No qualification
Area response > 200% of the opening CCV or mid-point
standard CS3 from ICAL
J-
No qualification
RT shift between sample/blank and opening CCV or
mid-point standard CS3 from ICAL > 30.0 seconds
R
R
RT shift between sample/blank and opening CCV or
mid-point standard CS3 from ICAL < 30.0 seconds
No qualification
No qualification
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XI. Target Analyte Identification
A. Review Items
Form 1A-OR, quantitation reports, mass spectra, and chromatograms. (SOW SOM02.4 - Exhibit B,
Section 3.4 and Exhibit D/SVOA, Section 11.1.1)
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 CS3 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
CS3 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 CS3 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. 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.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the noncompliant 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.
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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 the 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 the 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 EPA Regional CLP COR action.
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XII. Target Analyte Quantitation and Reported Contract Required Quantitation Limit
A. Review Items
Form 1A-OR, sample preparation sheets, SDG Narrative, quantitation reports, and chromatograms.
(SOW SOM02.4 - Exhibit B, Section3.4 and Exhibit D/SVOA, Sections 11.2.1, 11.2.1.6, and 11.2 3)
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 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.
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 Percent Solids
(%Solids), original sample mass/volume, and any applicable dilutions.
a. For soil/sediment samples that are high in moisture (i.e., < 30% solids), 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 noncompliant 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 EPA Regional CLP COR, 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 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 the %Solids for a soil/sediment sample is < 10.0%, use professional judgment to qualify detects
and non-detects.
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4. If the %Solids for a soil/sediment sample is > 10.0% and < 30%, use professional judgment to
qualify detects and non-detects.
5. If the %Solids for a soil/sediment 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 EPA Regional CLP COR action.
Table 46. Percent Solids Actions for Semivolatile Analysis for Non-Aqueous Samples
Criteria
Action
Detects
Non-detects
%Solids < 10.0%
Use professional judgment
Use professional judgment
10.0% <%Solids< 30.0%
Use professional judgment
Use professional judgment
%Solids > 30.0%
No qualification
No qualification
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XIII. Tentatively Identified Compounds
A. Review Items
Form 1B-OR, chromatograms, library search printouts, and spectra for the TIC candidates. (SOW
SOM02.4 - Exhibit B, Section 3.4 and Exhibit D/SVOA, Sections 11.1.2 and 11.2.2)
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 (NIST) (2011 release or later), 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 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 an 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
"probable 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.
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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
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 (straight-chain or branched) or CnFhn (cyclic)
that contains 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 an 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 is not performed for all contractually-required peaks,
the EPA Regional CLP COR 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 EPA Regional CLP COR action.
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XIV. System Performance
A. Review Items
Form 8A-OR and chromatograms. (SOW SOM02.4 - Exhibit B, Section 3.4 and Exhibit D/SVOA,
Section 11.1)
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 EPA
Regional CLP COR action.
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XV. Performance Evaluation Sample
A. Review Items
Form 1A-OR, TR/COC Record documentation, preparation logs, instrument printouts, and raw data.
(SOW SOM02.4 - Exhibit B, Section 3.4 and Exhibit F, Section 4.1)
B. Objective
The objective is to determine the validity of the analytical results based on the recovery of the PE
sample(s).
C. Criteria
1. Matrix-specific PE samples shall be analyzed utilizing the same analytical methods and Quality
Assurance/Quality Control (QA/QC) procedures as employed for the samples, at a frequency to be
determined by each EPA Region for each site. PE samples must be analyzed in an SDG containing
field samples for the Case, using the same procedures, reagents, and instrumentation.
D. Evaluation
1. Verify, using Form 1A-OR, preparation logs, and raw data, that the PE samples were analyzed with
the field samples and field blanks in the SDG.
2. Verify, using Form 1A-OR, that the PE sample results are within the warning limits (95%
confidence interval) and action limits (99% confidence interval).
3. If a significant number (i.e., half or more) of the analytes in the PE samples fall outside of the 95%
warning or 99% action criteria, or a number of false positive results are reported, evaluate the
overall impact on the data.
E. Action
NOTE: If the PE sample criteria are not met, the laboratory performance and method accuracy are
in question. Use professional judgment to determine if the data should be qualified or
rejected. The following guidance is suggested for qualifying sample data associated with a
PE sample that does not meet the required criteria.
For a PE sample that does not meet the technical criteria, apply the action to all samples in
the same preparation batch. If the concentration of any analyte in a PE sample is not
comparable to the analyte's concentration in the field samples or field blanks (i.e., it is
much higher or much lower than the concentration in these samples), the action may be
applied to only those samples in which the analyte's concentration is comparable to the PE
sample concentration.
1. If the PE sample was not analyzed with the field samples and field blanks, use professional
judgment to determine if the associated sample results should be qualified. Obtain additional
information from the laboratory, if necessary. If a laboratory fails to analyze the PE sample(s)
provided with field samples and field blanks, or if a laboratory consistently fails to generate
acceptable PE sample results, record the situation in the Data Review Narrative, and note it for EPA
Regional CLP COR action.
2. If the PE sample results are outside the lower warning limits but inside the lower action limits,
qualify detects as estimated low (J-) and non-detects as estimated (UJ).
3. If the PE sample results are outside the lower action limits, qualify detects as estimated low (J-) and
non-detects as unusable (R).
4. If the PE sample results are within the limits, detects and non-detects should not be qualified.
5. If the PE sample results are outside the upper warning limits but inside the upper action limits,
qualify detects as estimated high (J+). Non-detects should not be qualified.
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6. If the PE sample results are outside the upper action limits, qualify detects as estimated high (J+).
Non-detects should not be qualified.
7. Annotate the potential effects on the data due to out-of-control PE sample results in the Data
Review Narrative.
Table 47. PE Sample Actions for Semivolatile Analysis
Criteria
Action
Detect
Non-detect
PE sample results outside lower warning limits but inside
lower action limits
J-
UJ
PE sample results outside lower action limits
J-
R
PE sample results within limits
No qualification
No qualification
PE sample results outside upper warning limits but inside
upper action limits
J+
No qualification
PE sample results outside upper action limits
J+
No qualification
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XVI. Regional Quality Assurance and Quality Control
A. Review Items
Form 1A-OR, chromatograms, TR/COC Record documentation, quantitation reports, and other raw
data from QA/QC samples. (SOW SOM02.4 - Exhibit B, Sections 2.4 and 3.4)
B. Objective
The objective is to use results from the analysis of EPA Regional QA/QC samples such as field
duplicates, blind spikes, and blind blanks to determine the validity of the analytical results.
C. Criteria
Criteria are determined by each EPA Region.
1. The frequency of EPA Regional QA/QC samples should be defined in the project QAPP.
2. Performance criteria for EPA Regional QA/QC samples should also be defined in the project
QAPP.
3. The EPA Region may provide the laboratory with PE samples to be analyzed with each SDG.
These samples may include blind spikes and/or blind blanks. The laboratory must analyze a PE
sample when provided by the EPA Region. Refer to Section VI, above, for blanks criteria. Refer to
Section XV, above, for PE samples criteria.
4. The RPD between field duplicates shall fall with the specific limits in the EPA Region's SOP or
project QAPP.
D. Evaluation
1. Evaluation procedures must follow the EPA Region's SOP for data review.
2. Determine whether the results of EPA Regional QA/QC samples impact all samples in the project
or only those directly associated (i.e., in the same SDG, collected on the same day, prepared
together, or contained in the same analytical sequence).
3. 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 EPA Region's SOP or
project QAPP.
4. Determine whether poor precision is the fault of the laboratory, or a result of sample
non-homogeneity in the field. Laboratory observations of sample appearance may become
important in these situations.
E. Action
1. Any action must be in accordance with EPA Regional specifications and the criteria for acceptable
field duplicate sample results.
2. Note unacceptable results for field duplicate samples for EPA Regional CLP COR action.
3. In general, for EPA Regional QA/QC performance not within QAPP specification, qualify detects
as estimated (J) and non-detects as estimated (UJ). The impact on overall data quality should be
assessed after consultation with the data user and/or field personnel. Contact the EPA Regional
CLP COR if reanalysis of samples is required.
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XVII. 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 equations, as
listed in the method. All sample results must be within the linear calibration ranges per the
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 Data Reporting 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 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 EPA Regional CLP COR 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 161
II. Gas Chromatograph with Electron Capture Detector Instrument Performance Check 166
III. Initial Calibration 171
IV. Continuing Calibration Verification 177
V. Blanks 182
VI. Surrogate 185
VII. Matrix Spike/Matrix Spike Duplicate 187
VIII. Laboratory Control Sample 189
IX. Florisil Cartridge Performance Check 191
X. Gel Permeation Chromatography Performance Check 193
XI. Target Analyte Identification 196
XII. Gas Chromatograph/Mass Spectrometer Confirmation 198
XIII. Target Analyte Quantitation and Reported Contract Required Quantitation Limit 199
XIV. Performance Evaluation Sample 201
XV. Regional Quality Assurance and Quality Control 203
XVI. Overall Assessment of Data 204
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I. Preservation and Holding Times
A. Review Items
Form 1A-OR, Traffic Report/Chain of Custody (TR/COC) documentation, Form DC-1, raw data,
sample extraction sheets, and the Sample Delivery Group (SDG) Narrative checking for: pH, shipping
container temperature, holding time, and other sample conditions. (SOW SOM02.4 - Exhibit B,
Section 3.4; Exhibit D/Introduction, Section 5.0; Exhibit D/General, Sections 8.0, 10.1.2.1, and
10.2.2.4.4; and Exhibit D/PEST, Section 8.0)
B. Objective
The objective is to determine the validity of the analytical results based on the sample conditions 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. 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 filtrate
samples, and TCLP/SPLP leachate samples that are properly preserved is 7 days.
5. The extraction technical holding time criteria for soil/sediment 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 and
aqueous filtrate sample extracts, is 40 days.
D. Evaluation
1. Review the SDG Narrative and the TR/COC Record 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
are identical.
3. Establish extraction technical holding times for samples excluding TCLP/SPLP leachate samples
by comparing the sample collection dates on the TR/COC Record documentation with the dates of
extraction on Form 1A-OR and the sample extraction sheets.
4. Establish extraction technical holding times for TCLP/SPLP leachate samples by comparing the
sample collection dates on the TR/COC Record documentation with the dates of extraction on
sample extraction sheets.
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5. Establish extraction technical holding times for TCLP/SPLP leachate samples by comparing the
dates of TCLP/SPLP extraction on the extraction sheets with the dates of extraction on Form
1A-OR and the preparation 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 extraction technical holding time for
preserved and not properly preserved soil/sediment samples designated for TCLP/SPLP, detects
and non-detects should not be qualified.
3. If TCLP/SPLP extraction is performed outside the 14-day extraction technical holding time for
preserved and not properly preserved soil/sediment 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 the
raw data, perform a more comprehensive review, contacting the laboratory if necessary through the
United States Environmental Protection Agency Regional Contract Laboratory Program
Contracting Officer's Representative (EPA Regional CLP COR), to determine the correct dates for
establishing the technical holding time.
5. If an aqueous sample, TCLP/SPLP aqueous filtrate 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 sample, TCLP/SPLP aqueous filtrate sample, or TCLP/SPLP leachate sample is not
properly preserved, extraction is performed outside the 7-day technical holding time, and/or 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 sample, TCLP/SPLP aqueous filtrate 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 sample, TCLP/SPLP aqueous filtrate sample, or TCLP/SPLP leachate sample is
properly preserved, extraction is performed outside the 7-day technical holding time, and/or the
extract is analyzed outside the 40-day technical holding time, consider all evidence of
compromised extract integrity (such as evaporation or 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/or the extract is analyzed outside the 40-day technical holding time,
use professional judgment to qualify detects and non-detects.
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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.
12. If a non-aqueous sample is properly preserved, extraction is performed outside the 14-day
technical holding time, and/or 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. 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 (J) and use
professional judgment to qualify non-detects as unusable (R). Note this for EPA Regional CLP
COR action. Annotate the effect of the holding time exceedance on the resulting data in the Data
Review Narrative, wherever possible.
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Table 48. Preservation and Holding Time Actions for Pesticide Analysis
Matrix
Preserved
Criteria
Action
Detect
Non-detect
< 7 days (for extraction) and
< 40 days (for analysis)
No
TCLP/SPLP aqueous filtrate
sample and TCLP/SPLP
leachate sample extracted
within the 7-day technical
holding time
Use professional
judgment
Use professional
judgment
> 7 days (for extraction) and/or
> 40 days (for analysis)
No
TCLP/SPLP aqueous filtrate
sample and TCLP/SPLP
leachate sample not extracted
within the 7-day technical
holding time
J
R
Aqueous
< 7 days (for extraction) and
< 40 days (for analysis)
Yes
TCLP/SPLP aqueous filtrate
sample and TCLP/SPLP
leachate sample extracted
within the 7-day technical
holding time
No qualification
No qualification
> 7 days (for extraction) and/or
> 40 days (for analysis)
Yes
TCLP/SPLP aqueous filtrate
sample and TCLP/SPLP
leachate sample not extracted
within the 7-day technical
holding time
Use professional
judgment
Use professional
judgment
Yes/No
Holding time grossly exceeded
J
Use professional
judgment
R
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Matrix
Preserved
Criteria
Action
Detect
Non-detect
No
<14 days (for extraction) and
< 40 days (for analysis)
Use professional
judgment
Use professional
judgment
No
>14 days (for extraction) and/or
> 40 days (for analysis)
Use professional
judgment
Use professional
judgment
Non-aqueous
Yes
<14 days (for extraction) and
< 40 days (for analysis)
No qualification
No qualification
Yes
>14 days (for extraction) and/or
> 40 days (for analysis)
J-
Use professional
judgment
R
Yes/No
Holding time grossly exceeded
J
Use professional
judgment
R
Table 49. Holding Time Actions for Non-Aqueous Pesticide TCLP/SPLP Sample Analysis
Preserved
Criteria
Action
Detect
Non-detect
No
TCLP/SPLP extraction
performed within the
14-day technical holding
time
No qualification
No qualification
No
TCLP/SPLP extraction not
performed within the
14-day technical holding
time
J-
Yes
TCLP/SPLP extraction
performed within the
14-day technical holding
time
No qualification
No qualification
Yes
TCLP/SPLP extraction not
performed within the
14-day technical holding
time
J-
Yes/No
Holding time grossly
exceeded
J
Use professional
judgment
R
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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. (SOW SOM02.4 - Exhibit B,
Section 3.4 and Exhibit D/PEST, Section 9.0)
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 50:
Table 50. Resolution Check Mixture
trans-Chlordane
Endrin ketone
Endosulfan I
Methoxychlor
4,4'-DDE
Endosulfan II
Dieldrin
Heptachlor-epoxide
Endosulfan sulfate
cis-Chlordane
alpha-BHC
4,4'-DDD
beta-BHC
4,4'-DDT
delta-BHC
Endrin
gamma-BHC
Endrin aldehyde
Aldrin
Tetrachloro-m-xylene (surrogate)
Heptachlor
Decachlorobiphenyl (surrogate)
b. The resolution between two adjacent peaks in the 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 51:
Table 51. Performance Evaluation Mixture (PEM)
gamma-BHC
Endrin
alpha-BHC
Methoxychlor
4,4'-DDT
Tetrachloro-m-xylene (surrogate)
beta-BHC
Decachlorobiphenyl (surrogate)
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b. The resolution between any two adjacent peaks in the ICAL and Continuing Calibration
Verification (CCV) PEMs must be > 90% on each GC column.
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 the 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 52) or INDC (see Table 53) can be used. This is determined by the
analysis of the RESC to see if the criteria in II. C. 1 .b are met. If Individual Standard
Mixtures A and B are used, follow the procedure in 2e. If INDC is used, follow the
procedure in 2f.
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 52.
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 52. Individual Standard Mixtures A and B
Individual Standard Mixture A
Individual Standard Mixture B
alpha-BHC
beta-BHC
Heptachlor
delta-BHC
gamma-BHC
Aldrin
Endosulfan I
Heptachlor-epoxide
Dieldrin
cis-Chlordane
Endrin
trans-Chlordane
4,4'-DDD
4,4'-DDE
4,4'-DDT
Endosulfan sulfate
Methoxychlor
Endrin aldehyde
Tetrachloro-m-xylene (surrogate)
Endrin ketone
Decachlorobiphenyl (surrogate)
Endosulfan II
Tetrachloro-m-xylene (surrogate)
Decachlorobiphenyl (surrogate)
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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 53.
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 53. Individual Standard Mixture C
alpha-BHC
4,4'-DDD
beta-BHC
4,4'-DDE
delta-BHC
4,4'-DDT
gamma-BHC
Dieldrin
Aldrin
Endrin
Heptachlor
Endosulfan sulfate
Heptachlor-epoxide
Endrin ketone
cis-Chlordane
Endrin aldehyde
trans-Chlordane
Methoxychlor
Endosulfan I
Tetrachloro-m-xylene (surrogate)
Endosulfan II
Decachlorobiphenyl (surrogate)
D. Evaluation
1. Resolution Check Mixture
a. Verify that the RESC is analyzed at the specified frequency and sequence.
b. Check the RESC data and Form 6G-OR to verify that if INDA and INDB are used in the
analytical sequence, and that the %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, the %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 the PEM is analyzed at the specified frequency and sequence.
b. Check the ICAL and CCV PEM data and Form 6G-OR to verify that the %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.
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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.
NOTE: For data obtained from the CLP, the preceding criteria are evaluated as part of the Contract
Compliant Screening (CCS) process. Information regarding the noncompliant
%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 the RESC is not performed at the specified sequence or frequency, use professional judgment
to qualify detects and non-detects.
b. If the RESC %Resolution criteria are not met, qualify detects as presumptively present with
estimated concentration (NJ) and non-detects as unusable (R).
2. Performance Evaluation Mixture
a. If the PEM is not performed at the specified frequency and sequence, qualify detects and
non-detects as unusable (R).
b. If the PEM %Resolution criteria are not met, qualify detects as presumptively present with
estimated concentration (NJ) and non-detects as unusable (R).
c. If the 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'-DDD 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).
d. If the 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 the mid-point Individual Standard Mixture CS3 is not performed at the specified frequency,
qualify detects and non-detects as unusable (R).
4. If the 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 EPA Regional CLP COR.
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Table 54. GC/ECD Instrument Performance Check Actions
Criteria
Action
Detect
Non-detect
RESC not performed at the specified frequency and
sequence
Use professional
judgment
Use professional
judgment
RESC
% Resolution < 60.0%
(INDA/INDB)
RESC
% Resolution < 80.0%
(INDC, primary column)
% Resolution < 50.0%
(INDC, secondary column)
NJ
R
PEM not performed at the specified frequency and
sequence
R
R
PEM %Resolution < 90.0%
NJ
R
PEM: 4,4'-DDT %Breakdown > 20.0% and 4,4'-DDT is
detected
J for 4,4'-DDT,
4,4'-DDD, and
4,4'-DDE
No qualification
PEM: 4,4'-DDT %Breakdown > 20.0% and 4,4'-DDT is
not detected
NJ for 4,4'-DDD and
4,4'-DDE
R for 4,4'- DDT
PEM: Endrin %Breakdown > 20.0% and Endrin is
detected
J for Endrin, Endrin
aldehyde, and Endrin
ketone
No qualification
PEM: Endrin %Breakdown > 20.0% and Endrin is not
detected
NJ for Endrin
aldehyde and Endrin
ketone
R for Endrin
PEM: Combined %Breakdown > 30%
Apply qualifiers as
described above
considering degree of
individual
breakdown.
Apply qualifiers as
described above
considering degree of
individual
breakdown.
CS3 INDA/INDB or INDC not performed at the specified
frequency
R
R
%Resolution < 90.0%
(CS3 INDA and INDB)
%Resolution < 80.0% (CS3
INDC, primary column)
%Resolution < 50.0% ( CS3
INDC, secondary column)
NJ
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. (SOW SOM02.4 - Exhibit B, Section 3.4 and Exhibit D/PEST, Sections 7.2.2 and
9.3)
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. 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 a specific
sequence as in the recommended Sequence 1 or 2 in Tables 56 and 57.
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 55.
3. A single-point Toxaphene calibration at low standard should be included in the initial calibration at
a minimum. Optionally, all five-point ICAL standards at Toxaphene concentration levels in Table
55 may be included in the ICAL as in Sequence 1 or 2 in Tables 56 and 57. When Toxaphene is
identified in any sample analysis with a single-point ICAL, a 5-point calibration must be performed
for Toxaphene qualitative and quantitative 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 55. Concentration Levels of Calibration Standards
Analyte
Concentration (ng/mL)
CS1
CS2
CS3
CS4
CS5
alpha-BHC
5.0
10
20
40
80
gamma-BHC
5.0
10
20
40
80
Heptachlor
5.0
10
20
40
80
Endosulfan I
5.0
10
20
40
80
Dieldrin
10
20
40
80
160
Endrin
10
20
40
80
160
4,4'-DDD
10
20
40
80
160
4,4'-DDT
10
20
40
80
160
Methoxychlor
50
100
200
400
800
beta-BHC
5.0
10
20
40
80
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Analyte
Concentration (ng/mL)
CS1
CS2
CS3
CS4
CS5
delta-BHC
5.0
10
20
40
80
Aldrin
5.0
10
20
40
80
Heptachlor-epoxide
5.0
10
20
40
80
4,4'-DDE
10
20
40
80
160
Endosulfan II
10
20
40
80
160
Endosulfan sulfate
10
20
40
80
160
Endrin ketone
10
20
40
80
160
Endrin aldehyde
10
20
40
80
160
cis-Chlordane
5.0
10
20
40
80
trans-Chlordane
5.0
10
20
40
80
Tetrachloro-m-xylene
(surrogate)
5.0
10
20
40
80
Decachlorobiphenyl
(surrogate)
10
20
40
80
160
Toxaphene
500
1000
2000
4000
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 a 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 the %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 56. Initial Calibration Sequence 1
Initial Calibration Sequence 1
1.
Resolution Check
2.
PEM
3.
Toxaphene CS1
4.
Toxaphene CS2
5.
Toxaphene CS3
6.
Toxaphene CS4
7.
Toxaphene CS5
8.
CS1 Individual Standard Mixture C
9.
CS2 Individual Standard Mixture C
10.
CS3 Individual Standard Mixture C
11.
CS4 Individual Standard Mixture C
12.
CS5 Individual Standard Mixture C
13.
Instrument Blank
14.
PEM
Table 57. Initial Calibration Sequence 2
Initial Calibration Sequence 2
1.
Resolution Check
2.
PEM
3.
Toxaphene CS1
4.
Toxaphene CS2
5.
Toxaphene CS3
6.
Toxaphene CS4
7.
Toxaphene CS5
8.
CS 1 Individual Standard Mixture A
9.
CS 1 Individual Standard Mixture B
10.
CS2 Individual Standard Mixture A
11.
CS2 Individual Standard Mixture B
12.
CS3 Individual Standard Mixture A
13.
CS3 Individual Standard Mixture B
14.
CS4 Individual Standard Mixture A
15.
CS4 Individual Standard Mixture B
16.
CS5 Individual Standard Mixture A
17.
CS5 Individual Standard Mixture B
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Initial Calibration Sequence 2
18.
Instrument Blank
19.
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 the 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 a
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 the 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 INDC data and Form 6B-OR to review the calculated RT windows
for calculation and transcription errors.
4. Check the Toxaphene ICAL standard data and Form 6D-OR to verify that five maj or 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 deflections between 50-100% of
full scale.
6. Check and recalculate the CFs, CFs, and %RSDs 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 Form 6C-OR and Form 6E-OR. If errors are detected, perform a more
comprehensive recalculation and review.
7. Verify that the %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: For data obtained from the CLP, the preceding criteria are evaluated as part of the CCS
process. Information regarding the noncompliant RT windows and %RSDs 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 or sequence, use professional judgment to
qualify detects and non-detects. Contact the EPA Regional CLP COR to arrange for reanalysis, if
possible, or note in the Data Review Narrative for later EPA Regional CLP COR 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. Contact the EPA Regional CLP COR to arrange for a revised report, or note in the
Data Review Narrative for later EPA Regional CLP COR action.
5. If the %RSD for any target analyte or surrogate is outside the acceptance limits, qualify detects as
estimated (J). Use professional judgment to qualify non-detects.
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6. If the %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
necessary. The following guidelines are recommended:
a. If the %RSD criteria of any target analytes are not met, and if 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.
8. If the laboratory failed to provide adequate calibration information, notify the EPA Regional CLP
COR, 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 EPA Regional CLP COR to arrange for
reanalysis, if possible, or note it in the Data Review Narrative for later EPA Regional CLP COR
action.
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Table 58. Initial Calibration Action for Pesticide Analysis
Criteria
Action
Detect
Non-detect
Initial calibration not performed or not
performed at specified frequency and
sequence
Contact the EPA Regional
CLP COR for reanalysis or
use professional judgment
Contact the EPA Regional
CLP COR for reanalysis or
use professional judgment
Initial calibration not performed at the
specified concentrations
Contact the EPA Regional
CLP COR for reanalysis or
use professional judgment
Contact the EPA Regional
CLP COR for reanalysis or
use professional judgment
RT windows incorrect
Or
Chromatogram criteria not met
Contact the EPA Regional
CLP COR for reanalysis or
use professional judgment
Contact the EPA Regional
CLP COR for reanalysis or
use professional judgment
%RSD outside acceptance limits*
J
Use professional judgment
%RSD within acceptance limits*
No qualification
No qualification
* %RSD < 20.0% for single component target analytes except alpha-BHC and delta-BHC.
%RSD < 25.0% for alpha-BHC and delta-BHC.
%RSD < 30.0% for Toxaphene peaks.
%RSD < 20.0% for surrogates (TCX and DCB).
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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. (SOW
SOM02.4 - Exhibit B, Section 3.4 and Exhibit D/PEST, Sections 7.2.2 and 9.4)
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 CS3 for INDA and INDB or INDC 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 CS3 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 CS3 Toxaphene Standard.
2. The CCV PEM standard must contain the specified target analytes and surrogates at the specified
concentration.
3. The CCV CS3 standards must contain all required target analytes and surrogates at or near 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 CS3
of INDA and INDB or INDC must be within the RT windows determined from the ICAL. If the
CCV CS3 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.
The %Breakdown of 4,4'-DDT, %Breakdown of Endrin, and combined %Breakdown of 4,4'-DDT
and Endrin must be calculated accordingly for the CCV PEM.
6. The %D between the CF and CF from the associated ICAL for each target analyte and surrogate in
CCV CS3 and the CF %D for each Toxaphene peak in the applicable CCV CS3 must be calculated
accordingly.
7. The %D for each single component target analyte and surrogate in the CCV PEM must be in the
inclusive range of ±25.0%.
8. The %Breakdown of 4,4'-DDT and %Breakdown of Endrin in the CCV PEM must be < 20.0%, and
the combined %Breakdown of 4,4'-DDT and Endrin in the CCV PEM must be < 30.0%.
9. The %D for each target analyte and surrogate in the CCV CS3 must be in the inclusive range of
±25.0%.
10. The %D for each Toxaphene peak in the applicable the CCV CS3 must be in the inclusive range of
±25.0%.
11. Instrument blanks paired with either a PEM or CS3 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 CS3 standard 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 CS3 standard (including Toxaphene CS3) are analyzed at the
specified frequency and sequence, and that each CCV standard is associated to the correct ICAL.
2. Verify that specified target analytes and surrogates at the correct concentrations are included in the
CCV PEM.
3. Verify that the mid-point standard CS3 from the ICAL is used for the CCV and the specified target
analytes and surrogates are included in each CS3 standard.
4. Verify that the absolute RT for each single component target analyte and surrogate in the CCV
PEM and CS3 standard of INDA and INDB or INDC are within the RT windows determined from
the ICAL. Verify that the absolute RT for each Toxaphene peak in the applicable CS3 standard is
within the RT window determined from the ICAL.
5. Verify that the %D for each single component target analyte and surrogate in the CCV PEM is
calculated correctly; that the %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 the %D
for at least one target analyte, surrogate, and all three %Breakdowns in each CCV PEM.
6. Verify that the %D for each target analyte and surrogate in the CCV CS3 and the CF %D for each
Toxaphene peak in the applicable CCV CS3 are calculated correctly, and that the recalculated
values agree with the laboratory reported values on Form 7C-OR and Form 7D-OR, respectively.
Recalculate the %D for at least one target analyte, surrogate, and all five Toxaphene peaks in each
CS3 standard.
7. Verify that the %D for each single component target analyte and surrogate in the CCV PEM are in
the inclusive range of ±25.0%.
8. Verify that the %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 the %D for each target analyte and surrogate in CCV CS3 are in the inclusive range of
±25.0%.
10. Verify that the %D for each Toxaphene peak in the applicable CCV CS3 is in the inclusive range of
±25.0%.
11. Verify that the instrument blanks paired with either the PEM or CS3 standard are analyzed at the
specified frequency and sequence, and that the concentration of each target analyte in the
instrument blank is not exceeding the CRQL.
12. Verify that the time elapsed between the injection of an instrument blank as opening CCV and the
injection of either a PEM or CS3 as closing CCV is within 14 hours.
13. Verify that the time elapsed between the injection of an instrument blank as opening CCV and the
injection of the last sample or blank in the same analytical sequence is within 12 hours.
NOTE: For data obtained from the CLP, information regarding the noncompliant CCV 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 CCV PEM or CS3 is not performed at the specified frequency and sequence, contact the EPA
Regional CLP COR to request that the laboratory repeat the analysis if holding times have not
expired and there is extract remaining. If reanalysis is not possible, carefully evaluate all other
available information, including the quality of analyte peak shapes and RT match of surrogates on
both columns, and compare to the most recent calibration performed on the same instrument under
the same conditions. Using this information and professional judgment, the reviewer may be able
to justify unqualified acceptance of qualitative results and qualification of all quantitative results as
estimated (J). Otherwise, qualify all detects and non-detects as unusable (R).
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 CS3 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 the CCV PEM and CS3 standard is outside the RT window,
carefully evaluate the associated sample results. All samples injected after the last in-control
standard are potentially affected.
a. For non-detected target analytes in the affected samples, check the sample chromatograms that
may contain any peaks that are close to the expected RT window of the target analytes of
interest.
i. If no peaks 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 the sample chromatograms that may
contain any peaks that are close to the expected RT window of the target analytes of interest.
If the peaks are close to the expected RT window of the pesticide of interest, it may require
additional effort to determine if sample peaks represent the target analytes of interest.
For example, the data 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 windows
can be re-evaluated using the RTs of the standards.
i. If the peaks 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).
5. If errors are detected in the calculations of either the %D or %Breakdown in the CCV PEM,
perform a more comprehensive recalculation.
6. If errors are detected in the calculations of the %D in any CS3 standard or %D for any Toxaphene
peak in the applicable CCV CS3, perform a more comprehensive recalculation. Contact the EPA
Regional CLP COR to arrange for data resubmittal and note it in the Data Review Narrative for
later EPA Regional CLP COR action.
7. If the %D for any target analyte in the CCV PEM is outside the limits, qualify detects as estimated
(J) and non-detects as estimated (UJ).
8. If the 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'-DDD 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).
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9. If the 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).
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 IV.E.8 and IV.E.9
accordingly.
11. If the %D for any target analyte in CCV CS3 is outside the limits, qualify detects as estimated (J)
and non-detects as estimated (UJ).
12. If the time elapsed between the injection of an instrument blank as opening CCV and the injection
of either a PEM or CS3 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 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 the time elapsed between the injection of an instrument blank as opening CCV and the injection
of the last sample or blank in the same analytical sequence exceeds 12 hours, carefully evaluate
instrument stability during the entire sequence to decide whether degradation has occurred,
including column bleed, RTs, peak shapes, and surrogate recovery. If system degradation has been
found, qualify positive results as estimated (J). If any possibility exists for either false positives or
false negatives, qualify non-detects as unusable (R).
14. If the RT for each target analyte in PEM and CS3 standards are within the RT windows, and the %D
for the specified target analyte and %Breakdown in PEM are within the respective limits, and the
%D for each target analyte in CCV CS3 is within the limits, detects and non-detects should not be
qualified.
15. No qualification of the data is necessary based on the 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 an instrument blank as part of the 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
qualifications.
17. If the laboratory has failed to provide adequate calibration information, contact the EPA Regional
CLP COR, who may contact the laboratory to request the necessary information. If the information
is not available, use professional judgment to assess the data.
18. Note the potential effects on the data due to CCV criteria exceedance in the Data Review Narrative.
19. If the CCV criteria are grossly exceeded, note this for EPA Regional CLP COR action.
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Table 59. CCV Actions for Pesticide Analysis
Criteria
Action
Detect
Non-detect
CCV PEM and CS3 not performed at the
correct frequency and sequence
Contact the EPA Regional
CLP COR for reanalysis or
use professional judgment
Contact the EPA Regional
CLP COR for reanalysis or
use professional judgment
CCV PEM not performed at the specified
concentration
Contact the EPA Regional
CLP COR for reanalysis or
use professional judgment
Contact the EPA Regional
CLP COR for reanalysis or
use professional judgment
CCV CS3 not performed at the specified
concentration
Contact the EPA Regional
CLP COR for reanalysis or
use professional judgment
Contact the EPA Regional
CLP COR for reanalysis or
use professional judgment
RT outside the RT window
Use professional judgment
Use professional judgment
PEM %D outside the limits
J
UJ
PEM: 4,4'-DDT %Breakdown >20.0% and
4,4'-DDT is detected
J for 4,4'-DDT, 4,4'-DDD,
and 4,4'-DDE
No qualification
PEM: 4,4'-DDT %Breakdown >20.0% and
4,4'-DDT is not detected
NJ for 4,4'-DDD and
4,4'-DDE
R for 4,4'-DDT
PEM: Endrin %Breakdown >20.0% and
Endrin is detected
J for Endrin, Endrin
aldehyde, and Endrin ketone
No qualification
PEM: Endrin %Breakdown >20.0% and
Endrin is not detected
NJ for Endrin aldehyde and
Endrin ketone
R for Endrin
PEM: Combined %Breakdown >30%
Apply qualifiers as
described above considering
degree of individual
breakdown
Apply qualifiers as
described above considering
degree of individual
breakdown
CS3 %D outside the limits
J
UJ
Time elapsed between opening CCV Pesticide
Instrument Blank and closing CCV PEM or
CS3 exceeds 14 hours
Use professional judgment
Use professional judgment
Time elapsed between opening CCV Pesticide
Instrument Blank and last sample or blank
exceeds 12 hours
Use professional judgment
Use professional judgment
RT, PEM %D, PEM %Breakdown, CS3 %D,
and time elapsed within limits
No qualification
No qualification
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V. Blanks
A. Review Items
Form 1A-OR, Form 4-OR, chromatograms, and quantitation reports. (SOW SOM02.4 - Exhibit B,
Section 3.4 and Exhibit D/PEST, Section 12.1)
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 blank analyses 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 end 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 the 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 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 noncompliant 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 EPA Regional CLP COR 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 EPA 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 method blank reported with results > CRQLs, report
sample results that are > CRQLs but < Blank Results at sample results and qualify as non-detect (U)
or as unusable (R). Use professional judgment to qualify sample results that > CRQLs and
> Blank Results.
6. For TCLP/SPLP LEBs, sulfur cleanup blanks, instrument blanks, and field blanks, sample result
qualifications listed in Table 60 should apply if supported by the project QAPP.
7. If gross contamination exists with blank results that are > ICAL CS5 concentrations, qualify detects
as unusable (R). If the contamination is suspected of having an effect on the sample results, note it
for EPA Regional CLP COR 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 60. Blank and TCLP/SPLP LEB Actions for Pesticide Analysis
Blank Type
Blank Result
Sample Result
Action
Method,
TCLP/SPLP LEB,
Sulfur cleanup,
Instrument, Field
Detects
Non-detect
No qualification
< CRQL
< CRQL
Report at CRQL and qualify as
non-detect (U)
> CRQL
Use professional judgment
> CRQL
< CRQL
Report at CRQL and qualify as
non-detect (U)
> CRQL but < Blank Result
Report at sample result and
qualify as non-detect (U) or as
unusable (R)
> CRQL and > Blank Result
Use professional judgment
Gross
contamination
Detect
Report at sample result 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. (SOW SOM02.4 - Exhibit B,
Section 3.4 and Exhibit D/PEST, Sections 7.2.2.7 and 11.2.6)
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 the CCV, all samples (including MS/MSD and 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. The %R for the surrogates TCX and DCB in all samples, including MS/MSDs, LCSs, and all
blanks, must be calculated accordingly.
4. The %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 the 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 time s.
c. Comparison of the results 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 noncompliant 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 the
sample or blank, use professional judgment to qualify detects and non-detects. Contact the EPA
Regional CLP COR to arrange for reanalysis, if possible.
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2. If surrogate RTs in the PEMs, Individual Standard Mixtures, samples, and blanks are outside of the
RT windows, use professional judgment to qualify detects and non-detects.
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 the %R, perform a more comprehensive recalculation. It
may be necessary to have the laboratory resubmit the data after making corrections.
5. If the %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 the %R for any surrogate in undiluted sample is < 10%, qualify detects as estimated low (J-) and
non-detects as unusable (R).
7. If the %Rfor any surrogate in diluted sample is < 10%, use professional judgment to qualify detects
and non-detects.
8. If the %R for any surrogate is > 10% and < 30%, qualify detects as estimated low (J-) and
non-detects as estimated (UJ).
9. If the %R for both surrogates are > 30% and < 150%, detects and non-detects should not be
qualified.
10. If the %R for any surrogate is > 150% but < 200%, qualify detects as estimated high (J+).
Non-detects should not be qualified.
11. If the %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 EPA Regional CLP COR action even if this judgment
allows some use of the affected data.
Table 61. Surrogate Actions for Pesticide Analysis
Criteria
Action*
Detect
Non-detect
RT out of RT window
Use professional judgment
Use professional judgment
RT within RT window
No qualification
No qualification
%R < 10% (undiluted sample)
J-
R
%R < 10% (diluted sample)
Use professional judgment
Use professional judgment
10% < %R < 30%
J-
UJ
30% < %R < 150%
No qualification
No qualification
150% < %R < 200%
J+
No qualification
%R > 200%
J+
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
SDG Cover Page, Form 3A-OR, chromatograms, and quantitation reports. (SOW SOM02.4 - Exhibit
B, Section 3.4 and Exhibit D/PEST, Sections 7.2.2.8 and 12.2)
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 the specified frequency. One pair of MS/MSD
samples 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. 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 shall be within the acceptance limits in Table 62.
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 3A-OR and verify that they are within the limits listed
in Table 62.
NOTE: For data obtained from the CLP, the preceding criteria, including the required MS/MSD
spiking analytes and spiking levels specified in Exhibit D - Pesticides Analysis, Table 7, of
the SOW, are evaluated as part of the CCS process. Information regarding the
noncompliant 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 were 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 EPA Regional CLP COR action. It is not
likely that data qualification will be warranted if 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 was used for the MS/MSD analysis, note this for EPA Regional CLP
COR 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 the 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 62, 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:
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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 < lower acceptance limit, qualify detects as estimated (J) and
non-detects as estimated (UJ).
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 > upper acceptance limit, qualify detects as estimated (J).
Non-detects should not be qualified.
Table 62. MS/MSD %R and RPD Limits for Pesticide Analysis
Analyte
%R for
Water Sample
RPD for
Water Sample
%R for
Soil Sample
RPD for
Soil Sample
gamma-BHC (Lindane)
56 - 123
0-15
46 - 127
0-50
Heptachlor
40 - 131
0-20
35 - 130
0-31
Aldrin
40 - 120
0-22
34-132
0-43
Dieldrin
52 - 126
0-18
31 - 134
0-38
Endrin
56-121
0-21
42 - 139
0-45
4,4'-DDT
38 - 127
0-27
23 - 134
0-50
Table 63. MS/MSD Actions for Pesticide Analysis
Criteria
Action
Detect
Non-detect
%R < 20%
J
R
20% < %R < Lower Acceptance Limit
J
UJ
Lower Acceptance Limit < %R or
RPD < Upper Acceptance Limit
No qualification
No qualification
%R or RPD > Upper Acceptance Limit
J
No qualification
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VIII. Laboratory Control Sample
A. Review Items
Form 3B-OR, chromatograms, and data system printouts. (SOW SOM02.4 - Exhibit B, Section 3.4
and Exhibit D/PEST, Sections 7.2.2.9 and 12.3)
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. The LCS should be extracted
and analyzed per matrix or per SDG. The 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 64 and the surrogates at the specified
concentrations in the method (Table 7 in the SOW).
4. The %R for each spiked analyte in the LCS must be calculated according to the method.
5. The %R for each spiked analyte must be within the acceptance limits in Table 64.
Table 64. LCS %R Limits for Pesticide Analysis
Analyte
%R Limits
gamma-BHC
50-120
Heptachlor epoxide
50-150
Dieldrin
30-130
4,4'-DDE
50-150
Endrin
50-120
Endosulfan sulfate
50 - 120
trans-Chlordane
30-130
NOTE: The %R limits for any spiked analyte in the LCS may be expanded at any time during the
period of performance if the 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 the 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 the %R of each
target analyte in the LCS is calculated correctly and that the recalculated %R values agree with that
reported on Form 3B-OR.
4. Verify that the %R of each target analyte in the 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 noncompliant LCS %R 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 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 EPA Regional
CLP COR 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 the 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 the 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 < 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 > 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 65. LCS Actions for Pesticide Analysis
Criteria
Action
Detect
Non-detect
LCS not performed at the specified frequency or
concentration
Use professional
judgment
Use professional
judgment
%R < Lower Acceptance Limit
J-
R
Lower Acceptance Limit < %R < Upper
Acceptance Limit
No qualification
No qualification
%R > Upper Acceptance Limit
J+
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. (SOW SOM02.4 - Exhibit
B, Section 3.4 and Exhibit D/PEST, Section 10.3.2)
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. The %R for each target analyte and surrogate in INDA must be calculated according to the method.
4. The %R limits for the target analytes and surrogates in the INDA are 80-120%, and < 5% for
2,4,5-trichlorophenol. If INDC is used, the %R limits for target analytes and surrogates in INDC
shall be evaluated.
D. Evaluation
1. Verify that the Florisil Cartridge Performance Check is performed at the specified frequency.
2. Check the 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 the %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 the %R for the target analytes and surrogates in the Florisil Cartridge 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 noncompliant %R in the 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 the Florisil Cartridge Performance Check is not performed at the specified frequency, use
professional judgment to qualify detects and non-detects.
2. If the 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 the %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 the %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 the %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 the %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 the %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 the %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.
5. Annotate the potential effects on the sample data resulting from the Florisil Cartridge Performance
Check analysis not yielding acceptable results in the Data Review Narrative.
Table 66. Florisil Cartridge Performance Check Actions
Criteria
Action
Detect
Non-detect
Florisil Cartridge Performance Check not
performed at specified frequency or
concentration
Use professional
judgment
Use professional
judgment
%R < 10% (target analytes)
Use professional
judgment
R
10% < %R < 80% (target analytes)
J
UJ
80% < %R < 120% (target analytes)
No qualification
No qualification
%R > 120% (target analytes)
Use professional
judgment
No qualification
%R> 5% (2,4,5-trichlorophenol)
Use professional
judgment
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. (SOW SOM02.4 - Exhibit B, Section 3.4 and Exhibit
D/PEST, Section 10.3.1)
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
calibration verification 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. 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, LCSs, 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. The %R for each target analyte in the GPC calibration verification must be calculated according to
the method.
8. The %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 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 the %R for target analytes are calculated correctly and the %R values agree with that on
Form 9B-OR.
7. Verify that the %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 noncompliant %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 EPA Regional CLP COR.
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 EPA Regional CLP COR 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 the %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 the %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 the %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 the %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 the %R is > 120% for any target analytes and 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.
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Table 67. GPC Performance Check Actions for Pesticide Analysis
Criteria
Action
Detect
Non-detect
GPC Performance Check not
performed at the specified frequency
or concentration
Use professional judgment
Use professional judgment
%R < 10% (target analytes)
Use professional judgment
R
10% < %R < 80% (target analytes)
J
UJ
80% < %R < 120% (target analytes)
No qualification
No qualification
%R > 120% (target analytes)
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. (SOW
SOM02.4 - Exhibit B, Section 3.4 and Exhibit D/PEST, Section 11.1.1)
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, the %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), Form
10A-OR, and 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 the 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 the %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-homogeneity as causes for the difference.
E. Action
1. If the qualitative criteria for both columns are not met, all target analyte s 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 the 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 the %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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XII. Gas Chromatograph/Mass Spectrometer Confirmation
A. Review Items
Form 1A-OR, Form 10A-OR, Form 10B-OR, chromatograms, and data system printouts. (SOW
SOM02.4 - Exhibit B, Section 3.4 and Exhibit D/PEST, Section 11.1.2)
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 a 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), Form
10A-OR, and Form 10B-OR.
2. Check the 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.l).
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 noncompliant 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 an X or as non-detect (U). Explain in the Data Review Narrative that
the analyte should be considered non-detect because it could not be confirmed.
Table 68. GC/MS Confirmation Actions
Criteria
Action for Detects
Analyte confirmed by GC/MS
C
Analyte indicated but not confirmed by GC/MS
X or U
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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.
(SOW SOM02.4 - Exhibit B, Section 3.4 and Exhibit D/PEST, Sections 11.2.2 and 11.2.4)
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 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), original sample mass/volume, and any applicable dilutions.
a. For soil/sediment samples that are high in moisture (i.e., < 30% solids), 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 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 noncompliant 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 EPA Regional CLP COR, 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 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 the %Solids for a soil/sediment sample is < 10.0%, use professional judgment to qualify detects
and non-detects.
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4. If the %Solids for a soil/sediment sample is > 10.0% and < 30.0%, use professional judgment to
qualify detects and non-detects.
5. If the %Solids for a soil/sediment 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 EPA Regional CLP COR action.
Table 69. Percent Solids Actions for Pesticide Analysis for Non-Aqueous Samples
Criteria
Action
Detect
Non-detect
%Solids < 10.0%
Use professional judgment
Use professional judgment
10.0% <%Solids< 30.0%
Use professional judgment
Use professional judgment
%Solids > 30.0%
No qualification
No qualification
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XIV. Performance Evaluation Sample
A. Review Items
Form 1A-OR, TR/COC Record documentation, preparation logs, instrument printouts, and raw data.
(SOW SOM02.4 - Exhibit B, Section 3.4 and Exhibit F, Section 4.1)
B. Objective
The objective is to determine the validity of the analytical results based on the recovery of the PE
sample(s).
C. Criteria
1. Matrix-specific PE samples shall be analyzed utilizing the same analytical methods and Quality
Assurance/Quality Control (QA/QC) procedures as employed for the samples, at a frequency to be
determined by each EPA Region for each site. PE samples must be analyzed in an SDG containing
field samples for the Case, using the same procedures, reagents, and instrumentation.
D. Evaluation
1. Verify, using Form 1A-OR, preparation logs, and raw data, that the PE samples were analyzed with
the field samples and field blanks in the SDG.
2. Verify, using Form 1A-OR, that the PE sample results are within the warning limits (95%
confidence interval) and action limits (99% confidence interval).
3. If a significant number (i.e., half or more) of the analytes in the PE samples fall outside of the 95%
warning or 99% action criteria, or a number of false positive results are reported, evaluate the
overall impact on the data.
E. Action
NOTE: If the PE sample criteria are not met, the laboratory performance and method accuracy are
in question. Use professional judgment to determine if the data should be qualified or
rejected. The following guidance is suggested for qualifying sample data associated with a
PE sample that does not meet the required criteria.
For a PE sample that does not meet the technical criteria, apply the action to all samples in
the same preparation batch. If the concentration of any analyte in a PE sample is not
comparable to the analyte's concentration in the field samples or field blanks (i.e., it is
much higher or much lower than the concentration in these samples), the action may be
applied to only those samples in which the analyte's concentration is comparable to the PE
sample concentration.
1. If the PE sample was not analyzed with the field samples and field blanks, use professional
judgment to determine if the associated sample results should be qualified. Obtain additional
information from the laboratory, if necessary. If a laboratory fails to analyze the PE sample(s)
provided with field samples and field blanks, or if a laboratory consistently fails to generate
acceptable PE sample results, record the situation in the Data Review Narrative, and note it for EPA
Regional CLP COR action.
2. If the PE sample results are outside the lower warning limits but inside the lower action limits,
qualify detects as estimated low (I-) and non-detects as estimated (UI).
3. If the PE sample results are outside the lower action limits, qualify detects as estimated low (I-) and
non-detects as unusable (R).
4. If the PE sample results are within the limits, detects and non-detects should not be qualified.
5. If the PE sample results are outside the upper warning limits but inside the upper action limits,
qualify detects as estimated high (I+). Non-detects should not be qualified.
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6. If the PE sample results are outside the upper action limits, qualify detects as estimated high (J+).
Non-detects should not be qualified.
7. Annotate the potential effects on the data due to out-of-control PE sample results in the Data
Review Narrative.
Table 70. PE Sample Actions for Pesticide Analysis
Criteria
Action
Detect
Non-detect
PE sample results outside lower warning limits but inside
lower action limits
J-
UJ
PE sample results outside lower action limits
J-
R
PE sample results within limits
No qualification
No qualification
PE sample results outside upper warning limits but inside
upper action limits
J+
No qualification
PE sample results outside upper action limits
J+
No qualification
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XV. Regional Quality Assurance and Quality Control
A. Review Items
Form 1A-OR, chromatograms, TR/COC Record documentation, quantitation reports, and other raw
data from QA/QC samples. (SOW SOM02.4 - Exhibit B, Sections 2.4 and 3.4)
B. Objective
The objective is to use results from the analysis of EPA Regional QA/QC samples such as field
duplicates, blind spikes, and blind blanks to determine the validity of the analytical results.
C. Criteria
Criteria are determined by each EPA Region.
1. The frequency of EPA Regional QA/QC samples should be defined in the project QAPP.
2. Performance criteria for EPA Regional QA/QC samples should also be defined in the project
QAPP.
3. The EPA Region may provide the laboratory with PE samples to be analyzed with each SDG.
These samples may include blind spikes and/or blind blanks. The laboratory must analyze a PE
sample when provided by the EPA Region. Refer to Section V, above, for blanks criteria. Refer
to Section XIV, above, for PE samples criteria.
4. The RPD between field duplicates shall fall with the specific limits in the EPA Region's SOP or
project QAPP.
D. Evaluation
1. Evaluation procedures must follow the EPA Region's SOP for data review.
2. Determine whether the results of EPA Regional QA/QC samples impact all samples in the project
or only those directly associated (i.e., in the same SDG, collected on the same day, prepared
together, or contained in the same analytical sequence).
3. 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 EPA Region's SOP or
project QAPP.
4. Determine whether poor precision is the fault of the laboratory, or a result of sample
non-homogeneity in the field. Laboratory observations of sample appearance may become
important in these situations.
E. Action
1. Any action must be in accordance with EPA Regional specifications and the criteria for acceptable
field duplicate sample results.
2. Note unacceptable results for field duplicate samples for EPA Regional CLP COR action.
3. In general, for EPA Regional QA/QC performance not within QAPP specification, qualify detects
as estimated (J) and non-detects as estimated (UJ). The impact on overall data quality should be
assessed after consultation with the data user and/or field personnel. Contact the EPA Regional
CLP COR if reanalysis of samples is required.
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XVI. 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 equations, as
listed in the method. All sample results must be within the linear calibration ranges per the
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 Data Reporting 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 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 EPA Regional CLP COR 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 207
II. Initial Calibration 210
III. Continuing Calibration Verification 214
IV. Blanks 218
V. Surrogate 221
VI. Matrix Spike/Matrix Spike Duplicate 224
VII. Laboratory Control Sample 226
VIII. Gel Permeation Chromatography Performance Check 228
IX. Target Analyte Identification 231
X. Gas Chromatograph/Mass Spectrometer Confirmation 233
XI. Target Analyte Quantitation and Reported Contract Required Quantitation Limit 234
XII. Performance Evaluation Sample 236
XIII. Regional Quality Assurance and Quality Control 238
XIV. Overall Assessment of Data 239
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I. Preservation and Holding Times
A. Review Items
Form 1A-OR, Traffic Report/Chain of Custody (TR/COC) Record documentation, Form DC-1, raw
data, sample extraction sheets, and the Sample Delivery Group (SDG) Narrative checking for: pH,
shipping container temperature, holding time, and other sample conditions. (SOW SOM02.4 - Exhibit
B, Section 3.4; Exhibit D/Introduction, Section 5.0; Exhibit D/General, Sections 8.0, 10.1.2.1, and
10.2.2.4.4; and Exhibit D/ARO, Section 8.0)
B. Objective
The objective is to determine the validity of the analytical results based on the sample conditions 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. Sample extracts shall be stored
at < 6°C (but not frozen) from the time of the extraction completion until analysis.
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 Record 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
are identical.
3. 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.
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 the
raw data, perform a more comprehensive review, contacting the laboratory if necessary through the
United States Environmental Protection Agency Regional Contract Laboratory Program
Contracting Officer's Representative (EPA Regional CLP COR), to determine the correct dates for
establishing the technical holding time.
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3. If an aqueous 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, use
professional judgment to qualify detects and non-detects.
4. If an aqueous sample is not properly preserved, but extraction is performed outside the 7-day
technical holding time, and/or 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 preserved, 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.
6. If an aqueous sample is properly preserved, but extraction is performed outside the 1-year technical
holding time, and/or 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 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.
8. If a non-aqueous sample is not properly preserved, but extraction is performed outside the 14-day
technical holding time and/or 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 preserved, 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 preserved, but extraction is performed outside the 1-year
technical holding time and/or 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
EPA Regional CLP COR, to determine the correct dates for establishing the technical holding time.
12. Note 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 EPA Regional CLP
COR 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.
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Table 71. Preservation and Holding Time Actions for Aroclor Analysis
Matrix
Preserved
Criteria
Action
Detect
Non-detect
Aqueous
No
< 7 days (for extraction) and
< 40 days (for analysis)
Use professional
judgment
Use professional
judgment
No
> 7 days (for extraction) and/or
> 40 days (for analysis)
J
Use professional
judgment
Yes
< 1 year (for extraction) and
< 40 days (for analysis)
No qualification
No qualification
Yes
> 1 year (for extraction) and/or
> 40 days (for analysis)
J
U
Yes/No
Holding time grossly exceeded
J
Use professional
judgment
UJ orR
Non-aqueous
No
<14 days (for extraction) and
< 40 days (for analysis)
Use professional
judgment
Use professional
judgment
No
>14 days (for extraction) and/or
> 40 days (for analysis)
J
Use professional
judgment
Yes
< 1 year (for extraction) and
< 40 days (for analysis)
No qualification
No qualification
Yes
> 1 year (for extraction) and/or
> 40 days (for analysis)
J
U
Yes/No
Holding time grossly exceeded
J
Use professional
judgment
UJ orR
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II. Initial Calibration
A. Review Items
Form 6D-OR, Form 6E-OR, Form 6F-OR, chromatograms, and data system printouts. (SOW
SOM02.4 - Exhibit B, Section 3.4 and Exhibit D/ARO, Sections 7.2.2 and 9.3)
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 72. 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 tetrachloro-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 RT s of each of the five maj or peaks (three maj or 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. The 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 the %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
CS1 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 72. Initial Calibration Sequence
1.
Aroclor 1221 CS1
2.
Aroclor 1232 CS1
3.
Aroclor 1242 CS1
4.
Aroclor 1248 CS1
5.
Aroclor 1254 CS1
6.
Aroclor 1262 CS1
7.
Aroclor 1268 CS1
8.
Aroclor 1016/1260 (100 ng/mL) CS1
9.
Aroclor 1016/1260 (200 ng/mL) CS2
10.
Aroclor 1016/1260 (400 ng/mL) CS3
11.
Aroclor 1016/1260 (800 ng/mL) CS4
12.
Aroclor 1016/1260 (1600 ng/mL) CS5
13.
Instrument blank
D. Evaluation
1. Verify that the 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 in the ICAL 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-ORto verify that
the RT windows, CFs, CFs, and %RSDs are calculated correctly. Recalculate the CFs and %RSDs
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 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 CLP, the preceding criteria are evaluated as part of the Contract
Compliance Screening (CCS) process. Information regarding the noncompliant 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 EPA Regional CLP COR to arrange for reanalysis, if
possible, or note it in the Data Review Narrative for later EPA Regional CLP COR 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.
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4. If the chromatogram display criteria are not met, use professional judgment to qualify detects and
non-detects. Contact the EPA Regional CLP COR to arrange for a revised report, or note in the
Data Review Narrative for later EPA Regional CLP COR action.
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 the %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
necessary. The following guidelines are recommended:
a. If the %RSD criteria of any target analytes are not met, and if 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.
8. If the laboratory failed to provide adequate calibration information, notify the EPA Regional CLP
COR, 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 EPA Regional CLP COR to arrange for
reanalysis, if possible, or note it in the Data Review Narrative for later EPA Regional CLP COR
action.
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Table 73. Initial Calibration Action for Aroclor Analysis
Criteria
Action
Detect
Non-detect
Initial calibration not performed or not
performed at specified frequency and
sequence
Contact the EPA Regional
CLP COR for reanalysis or
use professional judgment
Contact the EPA Regional
CLP COR for reanalysis or
use professional judgment
Initial calibration not performed at the
specified concentrations
Contact the EPA Regional
CLP COR for reanalysis or
use professional judgment
Contact the EPA Regional
CLP COR for reanalysis or
use professional judgment
RT windows incorrect
Or
Chromatogram criteria not met
Contact the EPA Regional
CLP COR for reanalysis or
use professional judgment
Contact the EPA Regional
CLP COR for reanalysis or
use professional judgment
%RSD outside acceptance limits
J
Use professional judgment
%RSD within acceptance limits
No qualification
No qualification
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III. Continuing Calibration Verification
A. Review Items
Form 7D-OR, chromatograms, and data system printouts. (SOW SOM02.4 - Exhibit B, Section 3.4
and Exhibit D/ARO, Sections 7.2.2 and 9.4)
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 (CS3) 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 CS3 of Aroclor 1016/1260. If an Aroclor analyte other than 1016 or 1260 is
detected in any samples, a mid-point ICAL standard CS3 of that specific Aroclor analyte must be
analyzed as part of the opening and closing CCV.
2. The CCV CS3 standards must contain all required target analytes and surrogates at or near the
mid-point standard concentration of the ICAL.
3. The RT for each Aroclor target analyte and surrogate in the CCV CS3 standard must be within the
RT windows determined from the ICAL.
4. The Percent Difference (%D) between the CF and CF from the associated ICAL for each of the five
major Aroclor target analyte peaks (three major peaks for Aroclor 1221) and surrogate in the CCV
CS3 standard 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 the CS3 Aroclor Standard must be in the inclusive range of ±25.0% and ±30.0%,
respectively.
6. For a closing CCV, the %D for each of the five peaks (three major peaks for Aroclor 1221) used to
identify an Aroclor and surrogates in the CS3 Aroclor Standard must be in the inclusive range of
±50.0%.
7. Instrument blanks paired with the CS3 standard must bracket the 12-hour analytical sequence. The
concentration of each target analyte in the instrument blank must not exceed the 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 (CS3 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 CS3 standard is performed at the specified concentrations.
3. Verify that the RTs for each Aroclor peak and for surrogate in the CS3 standard are within the RT
windows.
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4. Check the data for each of the Aroclors and surrogates in the CS3 standards on Form 7D-OR and
verify that the CFs and %Ds are calculated correctly. Recalculate the CFs and %Ds for one or more
Aroclor peaks and verify that the recalculated values agree with that reported by the laboratory and
that there are no transcription errors.
5. Verify that the %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 CS3 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 the %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 CS3 Aroclor Standard are within the
acceptance limits (± 50.0%).
7. Verify that the instrument blanks paired with the CS3 standard are analyzed at the specified
frequency and sequence and that the concentration of each target analyte in the instrument blank is
not exceeding the CRQL.
8. Verify that the time elapsed between the injection of an instrument blank as opening CCV and the
injection of that last CS3 Aroclor Standard as closing CCV is within 14 hours.
9. Verify that the time elapsed between the injection of an instrument blank as opening CCV and the
injection of the last sample or blank in the same analytical sequence is within 12 hours.
NOTE: For data obtained from the CLP, information regarding the noncompliant 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 EPA Regional
CLP COR to request that the laboratory repeat the analysis, if holding times have not expired and
there is extract remaining. If reanalysis is not possible, carefully evaluate all other available
information, including the quality of analyte peak shapes and RT match of surrogates on both
columns, and compare to the most recent calibration performed on the same instrument under the
same conditions. Using this information and professional judgment, the reviewer may be able to
justify unqualified acceptance of qualitative results and qualification of all quantitative results as
estimated (J). Otherwise, qualify all detects and non-detects as unusable (R).
2. If the CCV is not performed at the specified concentrations, use professional judgment to qualify
detects and non-detects.
3. If the RTs for any Aroclor target analyte peak or surrogate in the CS3 standard are outside the RT
windows and match peak pattern, 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 the 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 the sample chromatograms that may
contain any peaks that are close to the expected RT window of the target analytes of interest.
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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
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 the CF or %D in any CCV CS3 standard, perform
a more comprehensive recalculation. Contact the EPA Regional CLP COR to arrange for data
resubmittal and note it in the Data Review Narrative for later EPA Regional CLP COR action.
5. If the %D for any Aroclor target analyte peak in CCV CS3 standard is outside the limits, qualify
detects as estimated (J) and non-detects as estimated (UJ).
6. If the time elapsed between the injection of an instrument blank as opening CCV and the injection
of the last required CS3 standard 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 has been found, qualify
positive results as estimated (J). If any possibility exists for either false positives or false negatives,
qualify non-detects as unusable (R).
7. If the time elapsed between the injection of an instrument blank as opening CCV and the injection
of the last sample or blank in the same analytical sequence exceeds 12 hours, carefully evaluate
instrument stability during the entire sequence to decide whether degradation has occurred,
including column bleed, RTs, peak shapes, and surrogate recovery. If system degradation has been
found, qualify positive results as estimated (J). If any possibility exists for either false positives or
false negatives, qualify non-detects as unusable (R).
8. If the RT for each target analyte peak in CS3 standards are within the RT windows or the %D for
each target analyte peak in CCV CS3 is within the limits, detects and non-detects should not be
qualified.
9. No qualification of the data is necessary based on the 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 an 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
qualifications.
11. If the laboratory has failed to provide adequate calibration information, contact the EPA Regional
CLP COR, who may contact the laboratory to request the necessary information. If the information
is not available, use professional judgment to assess the data.
12. Note the potential effects on the data due to CCV criteria exceedance in the Data Review Narrative.
13. If the CCV criteria are grossly exceeded, note this for EPA Regional CLP COR action.
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Table 74. CCV Actions for Aroclor Analysis
Criteria
Action
Detect
Non-detect
CCV CS3 not performed at the correct
frequency and sequence
Contact the EPA Regional
CLP COR for reanalysis or
use professional judgment
Contact the EPA Regional
CLP COR for reanalysis or
use professional judgment
CCV CS3 not performed at the specified
concentration
Contact the EPA Regional
CLP COR for reanalysis or
use professional judgment
Contact the EPA Regional
CLP COR for reanalysis or
use professional judgment
RT outside the RT window
Use professional judgment
Use professional judgment
CS3 %D outside the limits
J
UJ
Time elapsed between opening CCV
instrument blank and closing CCV CS3
exceeds 14 hours
Use professional judgment
Use professional judgment
Time elapsed between opening CCV
instrument blank and last sample or blank
exceeds 12 hours
Use professional judgment
Use professional judgment
RT, CS3 %D, and time elapsed within limits
No qualification
No qualification
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IV. Blanks
A. Review Items
Form 1A-OR, Form 4-OR, chromatograms, and quantitation reports. (SOW SOM02.4 - Exhibit B,
Section 3.4 and Exhibit D/ARO, Section 12.1)
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 blank samples 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 CS3 used as the 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 noncompliant 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 EPA Regional CLP COR 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 EPA 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 method blank reported with results > CRQLs, report
sample results that are > CRQLs but < Blank Results at sample results and qualify as non-detect (U)
or as unusable (R). Use professional judgment to qualify sample results > CRQLs and > Blank
Results.
6. For Sulfur cleanup blanks, instrument blanks, and field blanks, sample result qualifications listed in
Table 75 should apply if supported by the project QAPP.
7. If gross contamination exists with blank results that are > ICAL CS5 concentrations, qualify detects
as unusable (R). If the contamination is suspected of having an effect on the sample results, note it
for EPA Regional CLP COR 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 75. Blank Actions for Aroclor Analysis
Blank Type
Blank Result
Sample Result
Action
Detects
Non-detect
No qualification
< CRQL
< CRQL
Report at CRQL and qualify
as non-detect (U)
> CRQL
Use professional judgment
Method, Sulfur
cleanup, Instrument,
Field
< CRQL
Report at CRQL and qualify
as non-detect (U)
> CRQL
> CRQL but < Blank Result
Report at sample result and
qualify as non-detect (U) or as
unusable (R)
> CRQL and > Blank Result
Use professional judgment
Gross
contamination
Detect
Report at sample result 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. (SOW SOM02.4 - Exhibit B,
Section 3.4 and Exhibit D/ARO, Sections 7.2.2.4 and 11.2.5)
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 CS3 standard, all samples (including MS/MSD and 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. The %R for the surrogates TCX and DCB in all samples, including MS/MSDs, LCSs, and all
blanks, must be calculated accordingly.
4. The %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 the 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 time s.
c. Comparison of the results 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 noncompliant 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 the
sample or blank, use professional judgment to qualify detects and non-detects. Contact the EPA
Regional CLP COR to arrange for reanalysis, if possible.
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2. If surrogate RTs in CCV CS3 standards, samples, and blanks are outside of the RT windows, use
professional judgment to qualify detects and non-detects.
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 the %R, perform a more comprehensive recalculation. It
may be necessary to have the laboratory resubmit the data after making corrections.
5. If the %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, the %R for TCX must meet the acceptance
criteria.
7. If the %R for any surrogate in undiluted sample is < 10%, qualify detects as estimated low (J-) and
non-detects as unusable (R).
8. If the %R for any surrogate in diluted sample is < 10%, use professional judgment to qualify detects
and non-detects.
9. If the %R for any surrogate is > 10%, and < 30%, qualify detects as estimated low (J-) and
non-detects as estimated (UJ).
10. If the %R for both surrogates are > 30% and < 150%, detects and non-detects should not be
qualified.
11. If the %R for any surrogate is > 150% but < 200%, qualify detects as estimated high (J+).
Non-detects should not be qualified.
12. If the %R for any surrogate is > 200%, qualify detects as estimated high (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 EPA Regional CLP COR action even if this judgment
allows some use of the affected data.
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Table 76. Surrogate Actions for Aroclor Analysis
Criteria
Action*
Detect
Non-detect
RT out of RT window
Use professional judgment
Use professional judgment
RT within RT window
No qualification
No qualification
%R < 10% (undiluted sample)
J-
R
%R < 10% (diluted sample)
Use professional
judgment**
Use professional
judgment**
10% < %R < 30%
J-
UJ
30% < %R < 150%
No qualification
No qualification
150% < %R < 200%
J+
No qualification
%R > 200%
J+
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
SDG Cover Page, Form 3A-OR, chromatograms, and quantitation reports. (SOW SOM02.4 - Exhibit
B, Section 3.4 and Exhibit D/ARO, Sections 7.2.2.5 and 12.2)
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 the specified frequency. One pair of MS/MSD
samples 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. 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 77.
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 3A-OR and verify that they are within the limits listed
in Table 77.
NOTE: For data obtained from the CLP, the preceding criteria, including the required MS/MSD
spiking analytes and spiking levels in Exhibit D - Aroclors Analysis, Table 5, of the SOW,
are evaluated as part of the CCS process. Information regarding the noncompliant
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 were 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 EPA Regional CLP COR action. It is not
likely that data qualification will be warranted if 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 was used for the MS/MSD analysis, note this for EPA Regional CLP
COR 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 the 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 77, 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:
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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 < lower acceptance limit, qualify detects as estimated (J) and
non-detects as estimated (UJ).
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 > upper acceptance limit, qualify detects as estimated (J).
Non-detects should not be qualified.
Table 77. MS/MSD %R and RPD Limits for Aroclor Analysis
Analyte
%R for
Water and Soil Sample
RPD for
Water and Soil Sample
Aroclor 1016
29-135
0-15
Aroclor 1260
29-135
0-20
Table 78. MS/MSD Actions for Aroclor Analysis
Criteria
Action
Detect
Non-detect
%R < 20%
J
R
20% < %R < Lower Acceptance Limit
J
UJ
Lower Acceptance Limit < %R or
RPD < Upper Acceptance Limit
No qualification
No qualification
%R or RPD > Upper Acceptance Limit
J
No qualification
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VII. Laboratory Control Sample
A. Review Items
Form 3B-OR, chromatograms, and data system printouts. (SOW SOM02.4 - Exhibit B, Section 3.4
and Exhibit D/ARO, Sections 7.2.2.6 and 12.3)
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. The LCS should be extracted
and analyzed per matrix or per SDG. The 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 79 and the surrogates at the specified
concentrations in the method (Table 5 in the SOW).
4. The %R for each spiked analyte in the LCS must be calculated according to the method.
5. The %R for each spiked analyte must be within the acceptance limits in Table 79.
Table 79. LCS %R Limits for Aroclor Analysis
Analyte
%Recovery for
Water and Soil Sample
Aroclor 1016
50-150
Aroclor 1260
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 the 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 the %R of each
target analyte in the LCS is calculated correctly and that the recalculated %R values agree with that
reported on Form 3B-OR.
4. Verify that the %R of each target analyte in the 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 noncompliant LCS %R can be obtained from the NFG
reports and may be used as part of the evaluation process.
E. Action
1. If the 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 EPA Regional
CLP COR 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 the 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 the 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 < 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 > 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 80. LCS Actions for Aroclor Analysis
Criteria
Action
Detect
Non-detect
LCS not performed at the specified frequency or
concentration
Use professional
judgment
Use professional
judgment
%R < Lower Acceptance Limit
J-
R
Lower Acceptance Limit < %R < Upper
Acceptance Limit
No qualification
No qualification
%R > Upper Acceptance Limit
J+
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. (SOW SOM02.4 - Exhibit B, Section 3.4 and Exhibit
D/ARO, Section 10.3.1)
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
calibration verification 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. 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, LCSs, and blanks) are cleaned up
using the GPC.
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. The %R for each target analyte in the GPC calibration verification must be calculated according to
the method.
8. The %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 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 the %R for target analytes are calculated correctly and the %R values agree with that on
Form 9B-OR.
7. Verify that the %R for target analytes is 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 noncompliant %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 EPA Regional CLP COR.
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 subj ect to erratic performance. The expected result may
be an unknown bias in the data. Contact the EPA Regional CLP COR 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 the %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 the %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 the %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 the %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 the %R is > 120% for any target analytes and 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.
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Table 81. GPC Performance Check Actions for Aroclor Analysis
Criteria
Action
Detect
Non-detect
GPC Performance Check not
performed at the specified frequency
or concentration
Use professional judgment
Use professional judgment
%R < 10% (target analytes)
Use professional judgment
R
10% < %R < 80% (target analytes)
J
UJ
80% < %R < 120% (target analytes)
No qualification
No qualification
%R > 120% (target analytes)
Use professional judgment
No qualification
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IX. Target Analyte Identification
A. Review Items
Form 1A-OR, Form 10B-OR, chromatograms, and data system printouts. (SOW SOM02.4 - Exhibit
B, Section 3.4 and Exhibit D/ARO, Section 11.1.1)
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, the %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 major peaks (three major
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 the 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 results were 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 the %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
non-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 the 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 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 an Aroclor is strongly suggested, report
results as presumptively present with estimated concentration (NJ).
5. If errors are detected in the calculations of the %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. (SOW SOM02.4 - Exhibit
B, Section 3.4 and Exhibit D/ARO, Section 11.1.2)
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 Polychlorinated
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. Gas Chromatography/Mass Spectrometry (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 the 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.l).
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 noncompliant 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 an X or as 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 82. GC/MS Confirmation Actions
Criteria
Action for Detects
Analyte confirmed by GC/MS
C
Analyte indicated but not confirmed by GC/MS
X or U
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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.
(SOW SOM02.4 - Exhibit B, Section 3.4 and Exhibit D/ARO, Sections 11.2.2 and 11.2.3)
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 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), sample mass/volume, and any applicable dilutions.
a. For soil/sediment samples that are high in moisture (i.e., < 30% solids), 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 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 noncompliant 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 EPA Regional CLP COR, 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 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 the %Solids for a soil/sediment sample is < 10.0%, use professional judgment to qualify detects
and non-detects.
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4. If the %Solids for a soil/sediment sample is > 10% and < 30.0%, use professional judgment to
qualify detects and non-detects.
5. If the %Solids for a soil/sediment 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 EPA Regional CLP COR action.
Table 83. Percent Solids Actions for Aroclor Analysis for Non-Aqueous Samples
Criteria
Action
Detect
Non-detect
%Solids < 10.0%
Use professional judgment
Use professional judgment
10.0% <%Solids< 30.0%
Use professional judgment
Use professional judgment
%Solids > 30.0%
No qualification
No qualification
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XII. Performance Evaluation Sample
A. Review Items
Form 1A-OR, TR/COC Record documentation, preparation logs, instrument printouts, and raw data.
(SOW SOM02.4 - Exhibit B, Section 3.4 and Exhibit F, Section 4.1)
B. Objective
The objective is to determine the validity of the analytical results based on the recovery of the PE
sample(s).
C. Criteria
1. Matrix-specific PE samples shall be analyzed utilizing the same analytical methods and Quality
Assurance/Quality Control (QA/QC) procedures as employed for the samples, at a frequency to be
determined by each EPA Region for each site. PE samples must be analyzed in an SDG containing
field samples for the Case, using the same procedures, reagents, and instrumentation.
D. Evaluation
1. Verify, using Form 1A-OR, preparation logs, and raw data, that the PE samples were analyzed with
the field samples and field blanks in the SDG.
2. Verify, using Form 1A-OR, that the PE sample results are within the warning limits (95%
confidence interval) and action limits (99% confidence interval).
3. If a significant number (i.e., half or more) of the analytes in the PE samples fall outside of the 95%
warning or 99% action criteria, or a number of false positive results are reported, evaluate the
overall impact on the data.
E. Action
NOTE: If the PE sample criteria are not met, the laboratory performance and method accuracy are
in question. Use professional judgment to determine if the data should be qualified or
rejected. The following guidance is suggested for qualifying sample data associated with a
PE sample that does not meet the required criteria.
For a PE sample that does not meet the technical criteria, apply the action to all samples in
the same preparation batch. If the concentration of any analyte in a PE sample is not
comparable to the analyte's concentration in the field samples or field blanks (i.e., it is
much higher or much lower than the concentration in these samples), the action may be
applied to only those samples in which the analyte's concentration is comparable to the PE
sample concentration.
1. If the PE sample was not analyzed with the field samples and field blanks, use professional
judgment to determine if the associated sample results should be qualified. Obtain additional
information from the laboratory, if necessary. If a laboratory fails to analyze the PE sample(s)
provided with field samples and field blanks, or if a laboratory consistently fails to generate
acceptable PE sample results, record the situation in the Data Review Narrative, and note it for EPA
Regional CLP COR action.
2. If the PE sample results are outside the lower warning limits but inside the lower action limits,
qualify detects as estimated low (J-) and non-detects as estimated (UJ).
3. If the PE sample results are outside the lower action limits, qualify detects as estimated low (J-) and
non-detects as unusable (R).
4. If the PE sample results are within the limits, detects and non-detects should not be qualified.
5. If the PE sample results are outside the upper warning limits but inside the upper action limits,
qualify detects as estimated high (J+). Non-detects should not be qualified.
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6. If the PE sample results are outside the upper action limits, qualify detects as estimated high (J+).
Non-detects should not be qualified.
7. Annotate the potential effects on the data due to out-of-control PE sample results in the Data
Review Narrative.
Table 84. PE Sample Actions for Aroclor Analysis
Criteria
Action
Detect
Non-detect
PE sample results outside lower warning limits but inside
lower action limits
J-
UJ
PE sample results outside lower action limits
J-
R
PE sample results within limits
No qualification
No qualification
PE sample results outside upper warning limits but inside
upper action limits
J+
No qualification
PE sample results outside upper action limits
J+
No qualification
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XIII. Regional Quality Assurance and Quality Control
A. Review Items
Form 1A-OR, chromatograms, TR/COC Record documentation, quantitation reports, and other raw
data from QA/QC samples. (SOW SOM02.4 - Exhibit B, Sections 2.4 and 3.4)
B. Objective
The objective is to use results from the analysis of EPA Regional QA/QC samples such as field
duplicates, blind spikes, and blind blanks to determine the validity of the analytical results.
C. Criteria
Criteria are determined by each EPA Region.
1. The frequency of EPA Regional QA/QC samples should be defined in the project QAPP.
2. Performance criteria for EPA Regional QA/QC samples should also be defined in the project
QAPP.
3. The EPA Region may provide the laboratory with PE samples to be analyzed with each SDG.
These samples may include blind spikes and/or blind blanks. The laboratory must analyze a PE
sample when provided by the EPA Region. Refer to Section IV, above, for blanks criteria. Refer to
Section XII, above, for PE samples criteria.
4. The RPD between field duplicates shall fall with the specific limits in the EPA Region's SOP or
project QAPP.
D. Evaluation
1. Evaluation procedures must follow the EPA Region's SOP for data review.
2. Determine whether the results of EPA Regional QA/QC samples impact all samples in the project
or only those directly associated (i.e., in the same SDG, collected on the same day, prepared
together, or contained in the same analytical sequence).
3. 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 EPA Region's SOP or
project QAPP.
4. Determine whether poor precision is the fault of the laboratory, or a result of sample
non-homogeneity in the field. Laboratory observations of sample appearance may become
important in these situations.
E. Action
1. Any action must be in accordance with EPA Regional specifications and the criteria for acceptable
field duplicate sample results.
2. Note unacceptable results for field duplicate samples for EPA Regional CLP COR action.
3. In general, for EPA Regional QA/QC performance not within QAPP specification, qualify detects
as estimated (J) and non-detects as estimated (UJ). The impact on overall data quality should be
assessed after consultation with the data user and/or field personnel. Contact the EPA Regional
CLP COR if reanalysis of samples is required.
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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 equations, as
listed in the method. All sample results must be within the linear calibration ranges per the
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 Data Reporting 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 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 EPA Regional CLP COR 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
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 GC system.
Aroclor - A trademarked name for a mixture of polychlorinated biphenyls (PCBs) used in a variety of
applications including additives in lubricants, heat transfer dielectric fluids, adhesives, etc.
Blank - An analytical sample that has negligible or unmeasurable amounts of a substance of interest. The
blank is designed to assess specific sources of contamination. Types of blanks may include calibration
blanks, instrument blanks, method blanks, and field blanks. See the 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 organic analyses.
Calibration F actor (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) - A single parameter or multi-parameter standard solution
prepared by the analyst and used to verify the stability of the instrument calibration with time, and the
instrument performance during the analysis of samples. The CCV can be one of the calibration standards.
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 U.S. 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.
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 United States Environmental Protection Agency (EPA)
Contract Laboratory Program (CLP) Statement of Work (SOW) for Organic Superfund Methods
(Multi-Media, Multi-Concentration) SOM02.4. 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 check 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.
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Appendix A: Glossary
EPA Regional CLP Contracting Officer's Representative (EPA Regional CLP COR) - The EPA
official who monitors assigned CLP laboratories (either inside or outside of the Regional CLP COR's
respective Region), responds to and identifies problems in laboratory operations, and participants in
on-site laboratory audits.
Field Blank - A blank used to provide information about contaminants that may be introduced during
sample collection sample shipment, and in the laboratory. A field blank includes trip blanks, rinsate blanks,
bottle blanks, equipment blanks, preservative blanks, decontamination blanks, etc.
Field Sample - A portion of material to be analyzed that is contained in single or multiple containers and
identified by a unique EPA sample number.
14-Hour Time Period - For pesticide and Aroclor analyses, the 14-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 (VOA water and low-soil),
volatized from the sample extract (VOA medium soil), or injected as extracts (SVOA, PEST, and ARO). In
VOA and SVOA analysis, the analytes are detected by a Mass Spectrometer (MS). In Pesticide and Aroclor
analysis, the analytes 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 for a series of different concentrations; used to define
the quantitative response, linearity, and dynamic range of the instrument to target analytes.
Initial Calibration Verification (ICV) - Analysis of the calibration standard from an alternate source or a
different lot than that used for the initial calibration (ICAL) standards at the mid-point CS3 concentration of
the ICAL standards to ensure the instrument is calibrated accurately.
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 (for
volatiles), or sample extract aliquot (for semivolatiles), at a known concentration, prior to analysis. Internal
standards are used to monitor instrument performance and quantitation of target compounds.
Laboratory Control Sample (LCS) - A reference matrix spiked with target analytes at known
concentrations. LCSs are analyzed using the same sample preparation, reagents, and analytical methods
employed for the EPA samples received.
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 under study. Matrix effects
may affect purging/extraction efficiencies, and consequently affect Deuterated Monitoring Compound
(DMC)/surrogate recoveries and cause interference for the qualitative and quantitative analyses of the
target analytes.
Matrix Spike (MS) - Aliquot of the sample (aqueous/water or soil/sediment) fortified (spiked) with known
quantities of specific compounds and subjected to the entire analytical procedure to indicate the
appropriateness of the method for the matrix by measuring recovery.
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Appendix A: Glossary
Matrix Spike Duplicate (MSD) - A second aliquot of the same sample as the Matrix Spike (MS) (above)
that is spiked in order to determine the precision of the method.
Method Blank - A clean reference matrix sample (i.e., reagent water or purified sodium sulfate) spiked
with internal standards, and surrogate standards [or Deuterated Monitoring Compounds (DMCs) for
volatile and semi volatile], 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.
Percent Difference (%D) - The difference between two values calculated as a percentage of one of the
values.
Percent Relative Standard Deviation (%RSD) - The Percent Relative Standard Deviation is calculated
from the standard deviation and mean measurement of either Relative Response Factors (RRFs) or
Calibration Factors (CFs) from initial calibration standards. Percent Relative Standard Deviation indicates
the 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 a measure 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 water or soil 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 (GC); a plot of total ion current versus Retention Time (RT).
Relative Percent Difference (RPD) - The relative percent difference is based on the mean of the two
values, and is reported as an absolute value (i.e., always expressed as a positive number or zero).
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 analyte's RT falling within the
specified RT window established for that analyte. 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 20 field samples [excluding Performance Evaluation (PE) samples] within a Case; or
• Each 7 calendar day period (3 calendar day period for 7-day turnaround) during which field
samples in a Case are received (said period beginning with the receipt of the first sample in the
SDG).
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Appendix A: Glossary
• All samples scheduled with the same level of deliverables.
• In addition, all samples and/or sample fractions assigned to an SDG must be scheduled under the
same contractual turnaround time. Preliminary Results have no impact on defining the SDG.
Samples may be assigned to SDGs by matrix (i.e., all soil/sediment samples in one SDG, all aqueous/water
samples in another) at the discretion of the laboratory. Laboratories shall take all precautions to meet the 20
sample per SDG criteria.
Sample Management Office (SMO) - A Contractor-operated facility operated under the SMO contract,
awarded and administered by the EPA.
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 (TR/COC) Record
which documents information on that sample.
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.
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 an SDG have been analyzed. It is used to
determine the level of contamination acquired during storage.
Sulfur 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. Surrogates are 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 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 completed by
the sampler, which accompanies the sample during shipment to the laboratory and is used to document
sample identity, sample chain of custody, sample condition, and sample receipt by the laboratory.
Trip Blank - A blank used to provide information about contaminants that may be introduced during
sample transport.
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Appendix A: Glossary
Twelve-hour Time Period - The 12-hour time period for Gas Chromatograph/Mass Spectrometer
(GC/MS) system instrument performance check, standards calibration (initial, initial calibration
verification, or continuing calibration), 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 and Aroclor analyses performed by Gas
Chromatography/Electron Capture Detection (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 12 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.
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Appendix A: Glossary
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Appendix B
APPENDIX B: ORGANIC DATA REVIEW SUMMARY
CASE NO.
SITE
LABORATORY
NO. OF SAMPLES/MATRIX
MA NO.
SDGNo.
SOW NO.
REGION
REVIEWER NAME
COMPLETION DATE
EPA REGIONAL CLP COR ACTION
FY I
Review Criteria
Method
TRACE
VOA
LOW/MED
VOA
SVOA
PEST
AROCLOR
Preservation and Holding Times
GC/MS or GC/ECD Instrument
Performance Check
Initial Calibration
Initial Calibration Verification
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Appendix B
Review Criteria
Method
TRACE
VOA
LOW/MED
VOA
SVOA
PEST
AROCLOR
Continuing Calibration
Verification
Blanks
Deuterated Monitoring
Compound or Surrogate Spikes
Matrix Spike/Matrix Spike
Duplicate
Laboratory Control Sample
Regional QA/QC
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Appendix B
Review Criteria
Method
TRACE
VOA
LOW/MED
VOA
SVOA
PEST
AROCLOR
Internal Standards
GPC Performance Check
Florisil Cartridge Performance
Check
Target Analyte Identification
GC/MS Confirmation
Target Analyte Quantitation and
Reported CRQLs
Tentatively Identified Compounds
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Appendix B
Review Criteria
Method
TRACE
VOA
LOW/MED
VOA
SVOA
PEST
AROCLOR
System Performance
Overall Assessment of Data
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