REGION I, EPA-NEW ENGLAND DATA VALIDATION FUNCTIONAL GUIDELINES
FOR
EVALUATING ENVIRONMENTAL ANALYSES
U.S. EPA-NEW ENGLAND
Region I
Quality Assurance Unit Staff
Office of Environmental Measurement and Evaluation
Parti
July 1996
Revised December 1996
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TABLE of CONTENTS
Part I - Data Validation Manual The Data Quality System
Attachment A “Quality Assurance for Superfund Environmental Data Collection
Activities” - Publication 9200 2-16FS, February 1993, and “EPA Order
5360 1, Draft 1995 Quality Assurance Order”
1 a ent B “Region I j riered Organic and Inorganic Data Validation Guidelines”, July
1, 1993, DRAFT
Attachment C gion i)CSF Completeness Evidence Audit Program”, July 1991
Attachment D “Specifications and Guidance for Contaminant-Free Sample Containers” -
Publication 9240 05A, EPAJ54O/R-93/051, December 1992
Attachment E “User’s Guide to the Contract Laboratory Program”, EPAJS4O/P-91/002,
January 1991
Attachment F gion I Short Sheets and EPA CLP Information Sheets
Attachment “Training Manual for Reviewing Laboratory Data Package Completeness”,
un 1994.
Attachment Fj PA Region I Performance Evaluation Program Guidance”, July 1996,
L Reii
Attachment I “The Standard Operating Procedures for Submitting Data for Reduced
Payment/Data Rejection”, September 9, 1991
Attachment J Data \‘alidation Report
DQO Summary Form
ii ORDAJ RDA Form
iii. Telephone Log or Regional/Laboratory Communication Form
iv Data Validation Worksheets
v Chain-of-Custody Form
vi Traffic Report
Attachment K Example of Contract Compliance Screening (CCS) Report
Attachment Guidance Document for Completing Region I Data Validation Utilizir g
L iADRE Data Review”, February 1995
Attachment M Example Tier I Validation Cover Letter
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Attachment N Example Tier III Data Validation Reports
Attachment 0 “March 7, 1995 Memorandum to Heidi Horahan, ARCS DPO re CLP-
SOW OLMO3 1 - New Contract Requirements”
Attachment P “The Regional Sample Control Center Guidance for the Contract
Lt; boratory Program (CLP) and Delivery of Analytical Services (DAS)
Program for EPA-New England”, November 1996
Attachment\ ’Region I ARCS Delivery of Analytical Services Pilot Program, Final
L Report Volume II Appendices”, March 15, 1994
Part II - Volatile /Semivolatile Data Validation Functional Guidelines
Appendix A CLP SOW OLMO3 2/Volatile Organic Analysis - Method QC Critena,
Equations, and Definitions
Appendix B CLP SOW OLMO3 2/Semivolatile Organic Analysis - Method QC Criteria,
Equations, and Definitions
Appendix C CLP SOW OLCO2 1/Low Concentration Volatile Organic Analysis -
Method QC Criteria, Equations, and Definitions
Appendix D CLP SOW OLCO2 1/Low Concentration Semivolatile Organic Analysis -
Method QC Criteria, Equations, and Definitions
Appendix E VOA/SV Functional Guidelines Action Tables
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QA UNIT FACT SHEET 12/96
NEW DATA VALIDATION GUIDANCE
WHY: J w data validation guidance, the Region I. EPA-NE Data Validation Functional
Guidelines for Evaluating Environmental Analyses , was written by the QA Unit
Staff to formalize technical direction given since the original Region I Functional
Guidelines were implemented in 1988.
Data validation is necessary to ensure that only data of known and documented
quality are used in making environmental decisions. As such, this guidance serves
as a standard operating procedure that documents our Region’s commitment to
using only scientifically defensible data in environmental decision-making, it
documents compliance with Headquarters’ directives and guidance, and it ensures
that data generated by or for the region are evaluated consistently.
WHAT: The Region I, EPA-NE Data Validation Functional Guidelines for Evaluating
Environmental Analyses is a QA guidance document that describes the data
generation and validation process, including project scoping, sample scheduling,
data review and implementation of corrective actions. The document provides
generic guidance in reviewing multi-media organic and inorganic data and is
applicable to both CLP and non-CLP data.
The “Data Validation Manual: The Data Quality System”, Part I of the document,
details:
• Purpose and objectives of data validation
• Describes the Region I three Tier Data Validation system
• Identifies the roles and responsibilities of each of the following regarding
project scoping, DQO development, sample scheduling, data validation,
data usability and corrective action:
- EPA personnel
- EPA contractors
- States under Cooperative Agreements
- Other Federal Agencies under Interagency Agreements
- Other Federal Agencies performing non-Fund lead work
- Potentially Responsible Parties
• Itemizes the information to be reviewed during data validation
• Specifies the format and components of the Tier I Validation Cover Letter
and the Data Validation Report for Tier II and Tier m validations
• Identifies distribution requirements for the Tier I Validation Cover Letter
and Tier H/Ill Data Validation Reports
Parts II, III and IV are the specific Functional Guideline procedures for evaluating
Volatile/Semivolatile organic analyses by GC/MS, Pesticide/PCB organic analyses
by GC, and Inorganic analyses by ICP and AA, respectively. Parts H and 111 will
replace the Re2ion I Laboratory Data Validation Functional Guidelines for
Evaluating Or2anlcs Analyses . 2/01/88 modified 11/01/88 Part IV will replace
the Region I Laboratory Data Validation Functional Guidelines for Evaluating
Inor anics Analyses , 6/13/88, modified 2/89.
WHO: This new guidance document is intended for use by numerous stakeholders,
including EPA and its contractors. States, Tribes, other Federal Agencies, PRPs,
industry, and the public It serves as a training, instruction, and guidance
document for individuals involved in data generation activities for EPA-New
England ______
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1. TITLE: Region I, EPA-NE Data Validation Functional Guidelines
for Evaluating Environmental Analyses , 12/96; including Part I,
“Data Validation Manual: The Quality System” and Part II,
“Volatile/Semivolatile Data Validation Function Guidelines”
2. IDENTIFICATION NUMBER: N/A
3. ABSTRACT: The Region I, EPA-NE Data Validation Functional
Guidelines for Evaluating Environmental Analyses , 12/96, is a
Quality Assurance guidance document that describes the data
generation and validation process for environmental projects,
including project scoping, sample scheduling, data review and
implementation of corrective actions. The document provides
generic guidance for reviewing multi—media organic data.
Part I of the functional guidelines, “Data Validation Manual: The
Quality System” describes the following:
• The purpose and objectives of data validation.
• The Region I three-tier data validation system.
• The roles and responsibilities for EPA personnel, EPA
contractors, state agencies, other federal agencies, and
Potentially Responsible Parties involved in project scoping,
DQO development, sample scheduling, data validation, data
usability, and corrective actions.
• The information to be reviewed during data validation.
• The format and components of the Tier I Validation Cover
Letter and the Data Validation Report for Tier II and Tier
III validations.
• The distribution requirements for Tier I Cover Letters and
Tier Il/Ill Data Validation Reports
Part II of the functional guidelines, “Volatile/Semivolatile Data
Validation Functional Guidelines”, describes the specific
procedures for evaluating Volatile and Seniivolatile organic
analyses generated by GC/MS. It replaces the Volatile and
Semivolatile parts of the Region I Laboratory Data Validation
Functional Guidelines for Evaluating Organic Analyses , 2/01/88
modified 11/01/88.
Parts III and Part IV of the 12/96 functional guidelines will
cover Pesticide/PCB analyses by GC and Inorganic analyses by ICP
and AA, respectively. Parts III and IV will be added to this
site at a later date.
4. PURPOSE: This guidance, Region I, EPA-NE Data Validation
Functional Guidelines for Evaluating Environmental Analyses ,
12/96, was written by the QA Unit Staff in Region I to formalize
technical direction given since the original Region I data
validation functional guidelines were implemented in 1988. Data
validation is necessary to ensure that only data of known and
documented quality are used in making environmental decisions.
As such, this guidance serves as a standard operating procedure
-------
that documents our Region’s commitment to using only
scientifically defensible data in environmental decision-making.
It documents compliance with Headquarters’ directives and
guidance and it ensures that data generated by or for Region I
are evaluated consistently.
5. ORIGINATOR: Quality Assurance Unit, Office of Environmental
Measurement & Evaluation, EPA-New England
6. PUBLICATION DATE: TO BE ENTERED LATER
7. ACCESS CONSTRAINTS: N/A
8. AVAILABILITY:
These documents may be downloaded from this site. For the
Attachments, when an electronic version of the files are not
available, hardcopies of the documents may be ordered from the
addresses shown on the cover pages of the Attachments.
a. Distributor: Downloadable Files
b. Order Process: Downloadable Files
c. Technical Prerequisites: None
d. Automated Linkages: None
e. Downloadable Files: See attached list
9. COVERAGE: Primarily Limited to New England, with limited for
all of U.S. (Regions and Laboratories).
l0.TIME PERIOD OF COVERAGE: Current version is 12/96. Documents
will be updated periodically.
ll.POINT OF CONTACT FOR FURTHER INFORNATION:
Steve Stodola
EPA-New England
60 Westview Street
Lexington, MA 02173
TEL: (781) 860—4634
FAX: (781) 860—4642
EMAIL: stodola. steve@epamail . epa. gov
12 .RESPONSIBLE PARTY:
Deborah Szaro/Moira Lataille
Quality Assurance Officers
EPA-New England
60 Westview Street
Lexington, MA 02173
TEL: (781) 860—4312
FAX: (781) 860—4642
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EMAIL: szaro.deb@epan ail.epa.gov
lataille .inoira@epainail . epa. gov
13.DATE OF CREATION: [ To be added later]
14.AGENCY SUPPLEMENTAL INFORMATION: None
15.EXPIRATION DATE: None
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- Preface
The Region 1, EPA-New England Data Validation Functional Guidelines for Evaluating Environmental
Analyses , consists of Part I, the “Data Validation Manual: The Data Quality System”, December 1996
Revision, Part II, “Volatile/Sernivolatile Data Validation Functional Guidelines”, December 1996, and
Parts III, “Pesticide/PCB Data Validation Functional Guidelines” and IV, “Inorganic Data Validation
Functional Guidelines”, which are not yet released. This Preface will be updated with the finalization
of Part II, the release of Parts III and IV and any subsequent revisions or additions, and will accompany
those revised documents.
This document was written by the QA Unit Staff of Region I, EPA New-England to formalize technical
direction given since the original Region I Functional Guidelines were implemented in 1988. Data
validation is necessary to ensure that only data of known and documented quality are used in making
environmental decisions. As such, this guidance serves as a standard operating procedure that documents
Region l’s commitment to using only scientifically defensible data in environmental decision-making, it
documents compliance with Headquarters’ directives and guidance, and it ensures that data generated by
or for the region are evaluated consistently. Part I, the “Data Validation Manual: The Data Quality
System’ includes by attachment other Regional and National Quality Assurance guidance documents
utilized in conjunction with this new guidance to support Region L’s data quality system.
12/96 Revision
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REGION I, EPA-NEW ENGLAND DATA VALIDATION FUNCTIONAL GUIDELINES FOR
EVALUATING ENVIRONMENTAL ANALYSES
DATA VALIDATION MANUAL. THE DATA QUALITY SYSTEM PART I
VOLATILE/SEMIVOLATILE DATA VALIDATION
FUNCTIONAL GUIDELINES . . . . . PART II
PESTICIDE/PCB DATA VALIDATION
FUNCTIONAL GUIDELINES, (under development) PART HI
INORGANIC DATA VALIDATION
FUNCTIONAL GUIDELINES, (under development) . . . PART IV
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REGION I, EPA-NEW ENGLAND DATA VALIDATION FUNCTIONAL
GUIDELINES FOR EVALUATING ENVIRONMENTAL ANALYSES
TABLE OF CONTENTS
Part I-Data Validation Manual: The Data Quality System
1 Introduction . . . .
2 Definition of Data Validauon .
3 Purpose of Data Validation
4 Region I, EPA-New England Data Validation Functional Guidelines
13 Distribution of Data Validation Reports and Tier I
Validation Cover Letters . .
14 EPA Data Validation Oversight/Methods Review Program
CLP Data Validation - Roles & Responsibilities
Overview of the Data Validation Process for CLP Data
Overview of the )ata Validation Process for Non-CLP Data Generated for EPA
Data Validation Criteria Flow Chart for EPA Superfund Data
Attachment A
Attachment B
Attachment C
Attachment D
Attachment E
Attachment F
Attachment G
Attachment H
Attachment I
“Quality Assurance for Superfund Environmental Data Collection Activities” -
Publication 9200 2-I6FS, February 1993, and “EPA Order 5360.1, Draft 1995
Quality Assurance Order”
“Region I Tiered Organic and Inorganic Data Validation Guidelines”, July 1, 1993,
DRAFT
“Region I CSF Completeness Evidence Audit Program”, July 1991.
“Specifications and Guidance for Contaminant-Free Sample Containers” - Publication
9240 0-05A, EPA/540/R-93/05 1, December 1992
“User’s Guide to the Contract Laboratory Program”, EPA/540/P-91/002, Januar
199 1.
Region I Short Sheets and EPA CLP Information Sheets
“Training Manual for Reviewing Laboratory Data Package Completeness”, June
1994.
“EPA Region I Performance Evaluation Program Guidance”, July 1996, Revision
‘Standard Operating Procedures for Submitting Data for Reduced Payment/Data
Rejection’, September 9, 1991
DV
DV
DV
MANUAL-i
MANUAL-I
MANUAL-2
for Evaluating Environmental Analyses .
5 General Overview of the Data Validation Process
6 Summary of Data Validation Objectives
7 Roles and Responsibilities
8 Information Reviewed During the Data Validation Process
9 Communication Networks
10. The Tier I Validation Cover Letter . . .
11 The Data Validation Report (Tiers II and III)
12 Internal Review of Validation Documents . . . . .
DV MANUAL-3
DV MANUAL-S
DV MANUAL-7
DV MANUAL-8
DV MANUAL-21
DV MANUAL-33
DV MANUAL-40
DV MANUAL-44
DV MANUAL-54
DV MANUAL-55
DV MANUAL-56
Figure 1
Figure 2
Figure 3
Figure 4
TOC-1
12/96 Revision
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Attachment J Data Validation Report - Blank Forms
i. DQO Summary Form
ii. ORDA/IRDA Form
iii. Telephone Log or Regional/Laboratory Communication Form
iv. Data Validation Worksheets
v Chain-of-Custody Form
vi. Traffic Report
Attachment K Example of Contract Compliance Screening (CCS) Report
Attachment L ‘Guidance Document for Completing Region I Data Validation Utilizing CADRE
Data Review”, February 1995.
Attachment M Example Tier I Validation Cover Letter
Attachment N Example Tier III Data Validation Reports
Attachment 0 “March 7, 1995 Memorandum to Heidi Horahan, ARCS DPO re CLP-SOW
OLMO3. 1-New Contract Requirements.”
Attachment P ‘The Regional Sample Control Center Guidance for the Contract Laboratory Program
(CLP) and Delivery of Analytical Services (DAS) Program for EPA-New England”,
November 1996.
Attachment Q ‘Region I ARCS Delivery of Analytical Services Pilot Program, Final Report
Volume II. Appendices’, 15 March 1994.
TOC-2 12/96 Revision
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I I.
Ill
IV
V
VI
VII
VIII.
Ix
x
x l
X II.
x1II.
X IV.
XV.
XVI
XVII
Appendices
Appendix A
Appendix B
Appendix C
Appendix D
Appendix E
TABLE OF CONTENTS (continued)
Part Il-Volatile/Semivolatile Data Validation Functional Guidelines
• VOA/S V-I-i
• VOA/S V-H-i
VOA/S V-Ill-i
VOA/S V-IV-i
VOA/SV-V- 1
VOA/SV-V1-1
VOA/SV-VII- 1
VOA/SV-Vffl- 1
VOA/SV-IX- 1
VOA/SV-X- 1
VOA/SV-XJ-1
VOA/SV-XII- 1
VOA/SV-Xffl- 1
VOA/SV-XIV. 1
VOA/SV-XV- 1
VOA/SV-XVJ- 1
VOA/SV-XVH-1
OLMO3.1/Volatiles method QC criteria, equations, and definitions
OLMO3.1/Semivolatiles method QC criteria, equations, and definitions
OLCO2.O/Volatiles method QC criteria, equations, and definitions
OLCO2 0/Semivolatiles method QC criteria, equations, and definitions
VOA/SV Functional Guidelines Action Tables
II,
III
[ V
V
VI.
VII.
VIII.
IX
x
XI
XII.
XIII
X IV
XV
Appendices
Appendix F
Appendix G
Appendix H
Part IlI-Pestic ide/PCB Data Validation Functional Guidelines
Pest ’PCB-I-I
Pest/PCB-II- 1
• Pest/PCB-III-1
Pest/PC B-IV- I
PestIPCB-V- 1
• . Pest/PCB-VI-1
• . Pest/PCB-Xll- 1
Pest/PCB-VIH-1
Pest/PC B-IX- I
Pest/PCB-X-1
• Pest/PCB-XJ-l
• Pesc/PCB-XII-1
Pest/PCB-XIII-1
Pest/PC B-XIV- I
Pest/PCB-XV- 1
OLMO3 1/Pesticides/Aroclors method QC criteria, equations, and definitions
OLCO2 0/Pesucides/Aroclors method QC criteria, equations, and definitions
Pest/PCB Functional Guidelines Action Tables
Preservation and Technical Holding Times
GC/MS Instrument Performance Check (Tuning)
Initial Calibration . . .
Continuing Calibration
Blanks .
Surrogate Compounds
Internal Standards •
Matrix Spike/Matrix Spike Duplicate
Field Duplicates
Sensitivity Check • • . • • .
PE Samples/Accuracy Check
Target Compound Identification
Compound Quantitation and Reported Quantitation Limits
Tentatively Identified Compounds
Semivolaule Cleanup .
System Performance . . .
Overall Evaluation of Data
Preservation and Technical Holding Times
GC/ECD Instrument Performance Check
Initial Calibration . . . . . .
Continuing Calibration
Blanks ,
Surrogate Compounds
Pesticide Cleanup . .
Matrix Spike/Matrix Spike Duplicate .
Field Duplicates
Sensitivity Check .
PE Samples/Accuracy Check . . . . .
Target Compound Identification • • •
Compound Quantitation and Reported Quanutation Limits
System Performance . . . . . • . •
Overall Evaluation of Data • . .
TOC-3
12/96 Revision
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Part IV-Inor anic Data Validation Functional Guidelines
This document is under development. In the interim, validators must use the information in Part I,
the ‘Data Validation Manual: The Data Quality System” for the data validation process and
deliverables but use procedures contained in “Region I Laboratory Data Validation Functional
Guidelines for Evaluating Inorganic Analyses’, 6/13/88, modified 2/89, to validate inorganic data
generated by or submitted to EPA-NE.
TOC-4 12/96 Revision
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PART I - DATA VALIDATION MANUAL: THE DATA QUALITY SYSTEM
U.S. EPA-NEW ENGLAND
Region I
Quality Assurance Unit Staff
Office of Environmental Measurement and Evaluation
July 1996
Revised December 1996
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PART I - DATA VALIDATION MANUAL: THE DATA QUALITY SYSTEM
1.0 Introduction
2 0 Definition of Data Validation
3 0 Purpose of Data Validation
4 0 Region I, EPA-New England Data Validation Functional Guidelines for Evaluating
Environmental Analyses
5 0 General Overview of the Data Validation Process
6 0 Summary of Data Validation Objectives
7 0 Roles and Responsibilities
7 1 EPA-NE Delivery of Analytical Services (DAS) Team (Quality Assurance Unit-
Office of Environmental Measurement and Evaluation)
7.1.1 EPA-NE CLP-Technical Project Officer
7 1.2 EPA-NE Data Validation Chemist
7 1.3 EPA-NE Performance Evaluation Chemist
7.1.4 EPA-NE Regional Sample Control Center
7 2 EPA-NE Site Managers
7 3 CLP National Program Office
7.3.1 NPO Sample Scheduling and Coordination Contract (currently Contract
Laboratory Analytical Services Support [ CLASS], formerly Sample
Management Office)
7.3 2 NPO Quality Assurance Technical Support Contract (QATS)
7 4 Potentially Responsible Parties (Non Fund-lead)
7 5 Other Federal Agencies (Non Fund-lead)
7 6 Other Federal Agencies (Fund-lead)
7 7 States (State-leadlFund-lead)
7 8 EPA Field Sampling Contractors (Fund-lead and PRP/Federal Facility Oversight)
7 8.1 EPA Field Sampling Contractor Lead Chemist
7 8 2 Data Validator
8 0 Information Reviewed During the Data Validation Process
8. 1 Project Scoping Information
8.1 1 Objective
8 1 2 Requirements
8 1 3 Evaluation
8.14 Action
8 2 The Data Package
8 2 1 Objective
8 2 2 Requirements
8 2 3 Evaluation
8 2 4 Action
DVM-TOC-1 12/96 Revision
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8 3 Field Sampling Information
8.3.1 Field QAJQC Samples
8.3.2 Sample Descriptions
8 4 CLP Laboratory Contract Compliance Screening (CCS)
8.4.1 Objective
8.4.2 Requirements
8.4.3 Evaluation
8.4.4 Action
8.5 Performance Evaluation Samples
8.5.1 Objective
8.5 2 Requirements
8.5 3 Evaluation
8.5.4 Action
8 6 Computer-Aided Review and Evaluation (CADRE) Reports
8.6.1 Objective
8 6 2 Requirements
8.6.3 Evaluation
8.6.4 Action
9 0 Communication Networks
9.1 The CLP-RSCC Communication Network
9.1.1 Objective
9.1.2 Requirements
9.1.3 Procedure
9.1.4 Action
9.2 The Regional/Laboratory Communication Network
9.2.1 Objective
9.2.2 Requirements
9.2.3 Procedure
9.2 4 Action
9 3 The CLP-TPO Commumcation Network
10.0 The Tier I Validation Cover Letter
10 1 Objective
10 2 Components of the Tier I Validation Cover Letter
10 2. 1 Cover Letter
10.2.2 Attachments
10 3 Initiating the Tier I Validation Procedure
11 0 The Data Validation Report (Tiers II and III)
111 Objective
11 2 Components of the Data Validation Report
11 2 1 Organic/Inorganic Regional Data Assessment Form (ORDA/IRDA)
11.2 2 Data Validation Memorandum (DVM)
11 2.3 Standard Data Validation Worksheets
11 2.4 Support Documentation
11 2.5 CSF Audit
11.26 DQO Summary Form
DVM-TOC-2 12/96 Revision
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11.3 Initiating the Tier II and Tier III Data Validation Process
11.3 1 Reviewing the Data Package Narrative/Cover Page
11.3.2 Generating Data Summary Tables
11.3.3 Usage of Qualifier Codes on the Data Summary Table
12 0 Internal Review of Validation Documents
12 1 Senior Validator Review
12 2 Lead Chemist Review
13 0 Distribution of Data Validation Reports and Tier I Validation Cover Letters
14.0 EPA Data Validation Oversight/Methods Review Program
Figure 1 CLP Data Validation. Roles & Responsibilities
Figure 2. Overview of the Data Validation Process for CLP Data
Figure 3. Overview of the Data Validation Process for Non-CLP Data Generated for EPA
Figure 4. Data Validation Criteria Flow Chart for EPA Superfund Data
Attachment A “Quality Assurance for Superfund Environmental Data Collection Activities”
Publication 9200.2-L6FS, February 1993, and “EPA Order 5360.1, Draft 1995
Quality Assurance Order’.
Attachment B “Region I Tiered Organic and Inorganic Data Validation Guidelines’, July 1, 1993,
DRAFT.
Attachment C “Region I CSF Completeness Evidence Audit Program”, July 1991
Attachment D “Specifications and Guidance for Contaminant-Free Sample Containers” . Publication
9240.0-05A, EPA/540/R-93/05 1, December 1992.
Attachment E “User’s Guide to the Contract Laboratory Program”, EPA/5401P-91f002, January
1991.
Attachment F Region I Short Sheets and EPA CLP Information Sheets.
Attachment G “Training Manual for Reviewing Laboratory Data Package Completeness”, June
1994.
Attachment H “EPA Region I Performance Evaluation Program Guidance”, July 1996, Revision.
Attachment I “Standard Operating Procedures for Submitting Data for Reduced Payment/Data
Rejection”, September 9, 1991.
Attachment J Data Validation Report . Blank Forms
i. DQO Summary Form
ii. ORDA/IRDA Form
iii. Telephone Log or Regional/Laboratory Communication Form
iv Data Validation Worksheets
v. Chain-of-Custody Form
vi. Traffic Report
Attachment K Example of Contract Compliance Screening (CCS) Report
Attachment L “Guidance Document for Completing Region I Data Validation Utilizing CADRE
Data Review”, February 1995
Attachment M Example Tier I Validation Cover Letter
Attachment N Example Tier Ill Data Validation Reports
Attachment 0 ‘March 7, 1995 Memorandum to Heidi Horahan, ARCS DPO re CLP-SOW
OLMO3 1-New Contract Requirements
Attachment P “The Regional Sample Control Center Guidance for the Contract Laboratory Program
(CLP) and Delivery of Analytical Services (DAS) Program for EPA-New England”,
November 1996.
Attachment Q “Region I ARCS Delivery of Analytical Services Pilot Program, Final Report
Volume II Appendices”, 15 March 1994.
DVM-TOC-3 12/96 Revision
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PART I
DATA VALIDATION MANUAL: THE DATA QUALITY SYSTEM
1.0 INTRODUCTION
The Region I, EPA-New England Data Validation Functional Guidelines for Evaluating
Environmental Analyses , consists of Part!, the “Data Validation Manual: The Data Quality System”,
and Parts II, III and IV, the specific Functional Guideline procedures for validating multi-media
organic and inorganic data. Additional Functional Guideline procedures will be prepared as needed
The data validation guidance presented in this document is intended to ensure that data of known
quality are provided to both Superfund and non-Superfund EPA-NE program personnel. It is
applicable to data generated for all Superfund work performed by EPA, Potentially Responsible
Parties (PRPs), other Federal Agencies, States, and for oversight activities performed by EPA-NE.
En addition, it is applicable to data generated for all non-Superfund work performed by EPA, other
Federal Agencies, and State, Tribal and industrial partners and voluntary monitors.
These data validation procedures are not limited to Contract Laboratory Program (CLP) data. They
can be employed regardless of the mechanism used to generate the data and the program for which
they were generated. They may be modified to Suit any organic or inorganic sample separation
procedure, including chromatographic techniques such as gas chromatography or ion chromatography,
and any analytical method including performance-based methods utilizing a variety of detectors The
data validation guidelines in Part II -IV of this document are not limited to aqueous and soil/sediment
matrices but may be modified to evaluate other environmental matrices including, but not limited to,
oil, fly ash, biological tissue and air.
2.0 DEFINITION OF DATA VALIDATION
Data validation, the first step in assessing data quality, is a standardized review process for judging
the analytical quality and usefulness of a discrete set of chemical data. Thus, data validation
identifies the ‘analytical error” associated with a data set. Data validation can also identify some
(e g , incorrect preservation techniques), but not all of the “sampling error” associated with a data
set The sum of the “analytical error” and the “sampling error” is known as the “measurement
error”, as per Equation 1.
Equation 1 Measurement Error = Sampling Error + Analytical Error
The “measurement error” is used in conjunction with “sampling variability” (spatial variability of
pollutant concentrations) to determine “total error” or “total uncertainty” associated with a data set,
as per Equation 2. It should be noted that “sampling error” and “sampling variability” usually
contribute a greater percentage of the ‘total error” associated with a sampling event than the
“analytical error”
DV MANUAL - 1 12/96
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PART I
Equation 2: Total Error (uncertainty) = Measurement Error + Sampling Variability
Once the “total uncertainty’ has been estimated, the end user can assess the usability of a data set in
the context of previously developed project Data Quality Objectives (DQOs). For additional QA
Guidance, refer to EPA Order 5360.1 and Publication 9200.2- 16FS contained in Attachment A.
Data validation can be viewed as a decision making process during which established quality control
criteria are applied to the data. During this process, individual sample results are either accepted,
rejected or qualified. Data which meet all the validation criteria are accepted as unqualified and can
be used as needed, assuming that no problems occurred during the sampling events Data which are
rejected (R) for not meeting one or more of the validation criteria cannot be used at all. Some data
fall into the grey area between accepted and rejected. These data are qualified as “estimated” (J) to
indicate that one or more of the validation criteria were not met. Estimated data may or may not be
usable depending on the intended use of the data. In general, estimated (J) data can be used after
examining the reasons for data qualification and its impact on the achievement of the project DQOs
Estimated data, however, should not be used indiscriminately
The end product of data validation is data of known and defensible analytical quality
and, therefore, data should not be assessed for usability and used in environmental
decision maldng until after completion of the data validation process.
3.0 PURPOSE OF DATA VALIDATION
Data validation serves many purposes. As previously discussed, the primary purpose of data
validation is to assess and summarize the quality and defensibility of the laboratory’s analytical data
for the end users: site managers, risk assessors, hydrogeologists, and lawyers. The data validation
process focuses on evaluating the analytical laboratory’s performance so that the “analytical error’
associated with a data set can be determined. It provides a technical judgment on the validity of the
laboratory results as a first step in determining their overall usability and legal defensibility. To this
end, the data validator may be required to consult with the sampler in an effort to identify field
problems For example, incorrect preservation procedures result in “sampling error” and contribute
o the overall “measurement error’ associated with a data set. The data validation process does not
include consideration of “sampling variability”; this is left to the end user in the final assessment
of data usability.
Second, for data generated under the Superfund Contract Laboratory Program, data validation assists
the Region I Technical Proect Officer (TPO) in monitoring Regional CLP laboratory performance
If a laboratory fails to produce contractually-compliant data, then payment to the laboratory may be
reduced or denied by procedures initiated by the EPA Field Sampling Contractor and recommended
to the National Program Office (NPO) by the CLP-TPO. The TPO can also recommend that the CLP
Contracting Officer take contract action against a contractually non-compliant laboratory.
Similarly, for data generated by non-CLP laboratories, data validation assists those organizations
procuring analytical services in monitoring laboratory performance. If a non-CLP laboratory fails
to produce contractually-compliant data, then payment to the laboratory may be reduced or denied
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It is important to emphasize that the purpose of data validation is to identify “analytical error” and
not to make final determinations about the overall usability of the data for a project. The end user
of the data must specify the overall Data Quality Objectives (DQOs) for the project during the up-
front scoping process. Then, during data validation, the effect of individual analytical problems on
the accuracy and precision of the data is detailed for specific analytes and proper qualifiers are
applied to the data. Validation is just the first step in deciding whether or not data for a particular
sample can be used for a specific purpose. Ultimately, only the end user can assess usability based
on the “measurement error” and “sampling variability’ associated with the data package. The project
chemist andJor validator, however, are generally consulted by the end user to interpret decisions
made with regard to measurement error during the usability determination.
4.0 REGION I, EPA-NEW ENGLAND DATA VALIDATION FUNCTIONAL GUIDELINES
FOR EVALUATING ENVIRONMENTAL ANALYSES
All Superfund data generated for and/or used by EPA-NE must be validated in accordance with the
most recent revision of the Region I, EPA-NE Data Validation Functional Guidelines for Evaluating
Environmental Analyses , and this requirement should be clearly documented in the project Quality
Assurance Project Plan (QAPjP) or Sampling and Analysis Plan (SAP). Any deviation from this
stated data validation policy must be documented and justified in the site QAPjP or SAP and approved
by the Agency.
If CLP methods are used to generate site data, then the Region I, EPA-NE Data
Validation Functional Guidelines for Evaluating Environmental Analyses must be used
without deviation for the data validation process.
If non-CLP methods are used to generate site data and modified validation criteria are
necessary to validate those data, then all deviations to the Region I. EPA-NE Data
Validation Functional Guidelines for Evaluating Environmental Analyses must be
documented in an approved QAPJP or SAP specific to that site.
The Region I, EPA-NE Data Validation Functional Guidelines for Evaluating Environmental Analyses
is based on the U S. EPA Contract Laboratory Program National Functional Guidelines for Or amc
Data Review , February 1994 and the U S EPA Contract Laboratory Program National Functional
Guidelines for Inorganic Data Review , February 1994, but has been modified to provide generic
guidance for reviewing any organic data generated by gas chromatography (GC) or gas
chromatography/mass spectrometry (GC/MS) and any inorganic data generated by Atomic Absorption
(AA) or Inductively Coupled Plasma (ICP) spectrometry.
In some aspects, this document is equivalent to a standard operating procedure (SOP). In other, more
subjective areas, only general guidance is offered due to the complexities and uniqueness of data
relative to specific samples. Those areas where specific validation procedures are appropriate have
definitive performance requirements established in the contract or the method These requirements
are not sample dependent, they specify performance on parameters that should be fully under a
laboratory’s control, such as laboratory blanks, calibration standards, performance evaluation standard
materials. GC/MS mass calibration, peak shape and resolution.
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Other performance requirements, such as the frequency of Quality Control (QC) actions, are
dependent on the contract or the method, the number of samples, sample preparation technique, time
of analysis, etc , and are not identical for every case or batch of samples. Individual case
requirements and the impact of non-conformance must be addressed on a case-by-case basis;
therefore, no specific guidance is provided. For example, the CLP organic contract requirement that
a laboratory blank analysis be performed a minimum of once every twelve hours of analysis time
must be translated into the number of blanks required for a specific set of samples. The data
validator may have to consider the impact on data quality for a sample analyzed thirteen hours after
a blank, in terms of the quality of that particular sample data.
For some CLP data, a Contract Compliance Screening (CCS) automated review is performed by the
CLP NPO Sample Scheduling and Coordination Contract (currently Contract Laboratory Analytical
Services Support [ CLASS], formerly Sample Management Office) to assess both technical and
contractual deficiencies as presented by the laboratory in an electronic format. CCS is available to
the validator and can be utilized to assist in data validation and in determining reduced value/data
rejection recommendations (See Section 8.4 for additional information). However, for some CLP
data (i.e., dioxin) and for all EPA-generated non-CLP data, a contractual screen is not performed by
the CLP National Program Office. In the future, those organizations procunng analytical services
may choose to implement their own contractual screening procedures. Until that time, the validator
must assess both technical and contractual deficiencies in order to determine analytical quality as well
as contractual non-compliance. Contractually non-compliant data, which are unusable for making site
decisions and are considered ‘unacceptable” to the Region, should be considered for reduced payment
or data rejection/non-payment to ensure that EPA does not pay for “unacceptable” data.
At times, there may be an urgent need to use data which do not meet all contract requirements and
technical criteria. Use of these data does j constitute either a new requirement standard or Ml
acceptance of the data. Any decision to utilize data that are contractually non-compliant is strictly
to facilitate the progress of projects requiring the availability of the data. A laboratory submitting
non-compliant data may be required to re-extract and/or reanalyze samples and/or resubmit data even
if the previously submitted data have been utilized due to urgent program needs. Data that are not
fully usable may be recommended far reduced payment if those data are contractually non-compliant.
Data that are rejected due to contractual non-compliance should be returned to the laboratory and
payment denied. Data that have been rejected and returned to the laboratory cannot be used by the
Region in site decisions.
If the nature of the sample itself limits the attainment of contract or method quality control and/or
validation specifications, appropriate allowances must be made. The overriding concern of the
Agency is to obtain data which are technically valid, legally defensible, of known quality, and
ultimately usable in making site decisions.
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5.0 GENERAL OVERVIEW OF THE DATA VALIDATION PROCESS
In order to perform data validation, certain quality control (QC) checks and analytical procedures
must be performed in association with the analysis of the environmental samples. Examination of
the results of these checks and procedures allows the trained validator to determine the analytical
quality of the data in question.
To provide data of known quality, the data validator should: 1) review the data package to ensure
that it contains all the required documents and forms, 2) assess the results of all QC checks and
procedures, and 3) examine the raw data in detail to verify the accuracy of all information presented
by the laboratory These three levels of review constitute the Region I Tiered Validation approach.
Refer to Attachment B, Region I Tiered Organic and Inorganic Data Validation Guidelines , July 1,
1993, Draft or most recent revision. Note that the tiered validation procedures specific to the Region
I. EPA-NE Data Validation Functional Guidelines for Evaluating Environmental Analyses have been
incorporated into the text in each section of Parts II-IV.
Data completeness is the first item checked during validation. The validator needs all the laboratory
documents in order to verify the accuracy of sample analysis results reported by the laboratory and
to ensure the legal defensibility of the data. Prior to submitting sample results, the laboratory must
do a complete file purge. In the CLP, this is known as the Complete SDG File (CSF) purge. This
purge assembles all the supporting documentation and deliverables needed to substantiate the reported
results that are used in site decisions and/or litigation support. If any part of the complete file purge
information is not present, then the validator or designated Regional representative contacts the
laboratory to obtain the missing documentation. This process ensures that all the required
deliverables are present in the package. If missing deliverables are not obtained at this time, in all
likelihood they will never be recovered. Since any data package has the potential of being used in
court for enforcement or to support a site decision, all CLP and non-CLP data packages must be
routinely checked for completeness. Refer to Attachment C for Region I CSF Completeness Evidence
Audit Program , July 3, 1991 or most recent revision. The validator should evaluate any
Performance Evaluation sample results to assess potential usability issues, as part of the first
step in data validation.
Second, the reported results of all QC checks and analytical procedures are evaluated. Items such
as holding times, sample preservation techniques, QC sample results, etc., are assessed. QC samples
are designed to identify problems in three specific areas: laboratory/instrument performance, sample
preparationlmatrix effects, and field performance. The validator checks laboratory and instrument
performance by reviewing items such as laboratory blank contamination and instrument calibration.
Unusual matrix effects can be detected by examining the results from matrix spike/matrix spike
duplicates (MS/MSD), surrogate spike recoveries, and interial standard responses. These matrix
effects can be caused by high concentrations of non-target analytes which mask the analytes of
interest High levels of peat or clay can bind the target analytes to produce unwanted matrix effects
Potential problems originating from field sampling work are assessed by examining the field
duplicate, equipment blank, and trip blank results. It should be noted that field QC checks cannot
completely assess the “error’ associated with field sampling procedures. If the evaluation of QC
checks indicate laboratory or field problems, then the validator must discuss the:r impact on the data
in the Data Validation Memorandum and qualify the sample results in accordance with the guidance
in Parts II. III and IV of this document
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Last, the validator examines the raw data in detail to verify the accuracy of the results reported by
the laboratory Reported sample concentrations are checked by recalculating about 10% of the
original calculations unless problems warrant further investigation. Proper identification of all the
analytes is confirmed by examining the laboratory instrument print-outs. The validator is responsible
for resolving discrepancies in the reported data with the laboratory and obtaining resubmictals from
the laboratory whenever necessary. Occasionally, the identification and concentration of target
analytes reported in the samples may need to be changed upon validation.
In summary, the data validation process involves the following three steps:
Tier I: The data package is checked for completeness. The DC-2 Form (Inventory Sheet)
is completed and signed. This ensures that the data set is complete for potential use
in court. The PE sample results are evaluated to assess potential usability issues
For Tier I validations, a Tier I Validation Cover Letter is produced by the validator.
Tier II: The results of the QC checks, analytical procedures and PE sample results are
assessed and applied to the data set. This will result in the proper qualifiers being
applied to the data. For Tier II validations, a Data Validation Report is produced by
the validator.
Tier III: The raw data are examined in detail to check for calculation, compound
identification, and/or transcription errors. For Tier Ill validations, a Data Validation
Report is produced by the validator.
The validation tier used to validate each data package must be documented in the first paragraph of
either the Tier I Validation Cover Letter for Tier I validations, or the Data Validation Memorandum
from the Data Validation Report for Tier II and Tier ifi validations. For Tier I validations, the Tier
I Validation Cover Letter must document the site-specific justification for limiting the validation to
Tier I and the validator’s evaluation of the PE sample results.
En general, validation should be completed within 21 days of receipt of the data package from the
laboratory. This enables the user and/or site manager to assess contractual compliance and data
usability in order to make timely site decisions. Accelerated site schedules may necessitate shorter
turnaround times for validation. In general, the completion of a Data Validation Report should not
be delayed because the laboratory failed to forward a resubrruttal. In most cases, the Data Validation
Report should be completed, the laboratory omission noted, and the data qualified using professional
judgment. When/If the resubmittal is received, an amendment to the original Data Validation Report
should be forwarded.
In some cases, the validator must wait for critical information before the validation can be completed
In these cases, the user and/or site manager must be notified of the delay. If validation reports are
time critical, the site manager may request that a partially completed Data Validation Report be
generated Subsequently, an amendment should be written to incorporate all late resubmittals
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6.0 SUMMARY OF DATA VALIDATION OBJECTIVES
Data validation must concurrently accomplish the following:
• Assess and summarize the analytical quality and defensibility of data for the end user.
• Document for the historical record all factors contributing to “analytical error’ that
ultimately affect data usability, such as: data discrepancies, poor laboratory practices
that impact data quality, site locations for which samples were difficult to analyze,
i.e., matrix effects Also, document any “sampling error” that may be identified by
the data validation process, such as, contaminated trip or equipment blanks, incorrect
storage or preservation techniques, improper sampling containers, and improper
sampling techmques, i.e., headspace in VOA containers.
• Assist Regional TPOs in monitoring CLP laboratory performance for contract
administration.
• Assist in monitoring any laboratory’s performance of CLP methods in generating data
for submittal to EPA.
• Assist in monitoring any laboratory’s performance of non-CLP methods in generating
data directly for EPA or for submittal to EPA.
• Identify contractually non-compliant data that are unusable by the Region. For CLP
data, a letter documenting the contractual non-compliances and recommending
reduced payment or data rejection must be written and addressed to the CLP-TPO,
in accordance with EPA-NE Standard Operatina Procedures for Submitting Data for
Reduced Payment/Data Rejection , September 1991 (Attachment fl. For non-CLP
data generated directly for EPA, i.e., under the DAS program, contractually non-
compliant data should also be identified and documented so that contractual action
can be taken to ensure that the Region does not pay for unusable, cornractually non-
compliant data. In general, contractually non-compliant data should always be
identified and documented to support any contractual action taken by the data
requestor.
• Provide information concerning the effectiveness of analytical methods and SOWs,
and identify problems requiring method revision and/or resolution
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7.0 ROLES AND RESPONSIBILITIES
The end users of the data are responsible at the time of project scoping for determining the validation
criteria, including validation Tier, that are necessary to support the achievement of project DQOs
The question then arises as to who is responsible for performrig data validation. In general, whoever
collects field samples at the site is also responsible for validating the analytical data. An exception
exists when the organization collecting the samples uses their own internal laboratory to analyze the
samples; in this situation an independent third party must validate the data. In general, EPA Field
Sampling Contractors working on Fund-lead sites are responsible for validating the results for samples
that they collect. States working on Fund-lead sites under Cooperative Agreements with EPA are
responsible for validating their own samples. Likewise, other government agencies working on Fund-
lead sites under Interagency Agreements are responsible for validating results for samples that they
collect from their sites, i.e., the Army Corp of Engineers. For non Fund-lead sites, PRPs and
Federal Facilities traditionally have been required to use an independent third party for data
validation.
When an EPA Field Sampling Contractor performs PRP or Federal Facility oversight, duplicates
(splits) for approximately 10% of the PRP’s or Federal Facility’s samples are analyzed by EPA. The
PRP or Federal Facility must validate the data for the samples which it collects. If after PRP or
Federal Facility validation, the two sets of data agree within the predetermined limits presented in
the EPA-approved QAPJP andlor SAP, then the EPA oversight contractor data may not need to be
validated. If they do not agree within the predetermined limits, then the EPA oversight contractor
data must also be validated to investigate the cause of the discrepancy. Further corrective actions
may be necessary to identify the source of the discrepancy.
7 1 EPA-NE Delivery of Analytical Services (DAS) Team (Quality Assurance Unit-Office of
Environmental Measurement and Evaluation)
The EPA-NE DAS Team located within the Quality Assurance Unit of the Office of Environmental
Measurement and Evaluation (OEME) is responsible for developing data validation guidance, training
EPA Field Sampling Contractors in data validation, and operating an oversight program to ensure that
EPA Field Sampling Contractors are performing data validation in accordance with EPA-NE policy
The DAS Team also provides technical assistance concerning analytical methods, data validation and
data usability to EPA Site Managers and EPA Field Sampling Contractor Lead Chemists. Technical
assistance is also offered to the States, Tribal and industrial partners, other Federal Agencies, the
public, and PRPs through the responsible EPA Site Manager.
In general, OEME does not perform site-specific data validation with the exception of OEME
sampling events and all dioxin/furan samples collected by EPA personnel and EPA Field Sampling
Contractors
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The EPA-NE DAS Team acts as the Regional contact point for all CLP matters and maintains the
EPA-NE Performance Evaluation Sample Program.
7.1 1. EPA-NE CLP-Technica! Project Officer
The CLP Technical Project Officer (TPO) is responsible for moniwnng the CLP contract
laboratories within EPA-NE. This includes responding to the laboratory’s technical
questions: reviewing laboratory performance trend information and data reviews provided by
the National Program Office (NPO) and other Regional TPOs; discussing and documenting
CLP laboratory performance problems; tracking laboratory corrective action
requests/responses; assessing the adequacy of a CLP laboratory’s corrective action response;
recommending contract action to the Administrative Project Officer (APO) and Contracting
Officer (CO); conducting routine and problem resolution on-site audits; and monitoring the
continued effectiveness of corrective actions implemented by the laboratory.
The CLP-TPO is also responsible for: reviewing and developing Superfund analytical
methods and CLP SOWs; reviewing and developing CLP policies, guidance and procedures;
disseminating information concerning CLP operation and available services; and participating
in workgroups to revise and/or write analytical methods, National Functional Guidelines and
other national QA guidance.
7.1 2. EPA-NE Data Validation Chemist
The Data Validation Chemist (DV Chemist) is responsible for all aspects of data validation
within the Region, including: revising regional data validation Functional Guidelines;
providing guidance in using the Region I, EPA-NE Data Validation Functional Guidelines
for Evaluating Environmental Analyses ; writing reduced payment and data rejection
recommendation letters to the CLP-APO; and directing the Regional Data Validation
OversighiiMethod.s Review Program Through the Regional Data Validation
OversighcIMethods Review Program, the DV Chemist identifies analytical issues/problems
and needed corrective actions in order to reduce systematic “analytical error”. Sampling
issues and needed corrective actions are also identified in order to reduce systematic
‘sampling error”. This program also helps to identify inherent problems in the analytical
methods that require programmatic changes.
7. 1.3 EPA-NE Performance Evaluation Chemist
The Performance Evaluation Chemist (PE Chemist) is responsible for all aspects of the
Performance Evaluation Program within the Region, including: preparing, stocking,
distributing, and tracking PE samples, scoring EPA-provided PE sample results and providing
PES Score Reports to the data validators: and trending laboratory performance on PE
samples
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7.1.4 EPA-NE Regional Sample Control Center
The EPA-NE Regional Sample Control Center (RSCC) serves as the central paint of contact
for questions concerning Superfund sampling efforts utilizing the CLP and any future EPA-
NE analytical contracts. CLP and EPA-generated non-CLP (i.e., DAS) samples are
collected, preserved, packaged, and shipped in accordance with EPA-NE, DOT, and NPO
policy as described in EPA-NE Standard Operating Procedures (SOPs) and guidance
documents pertaining to this subject and as documented itt the EPA-approved QAPjP and/or
SAP. Refer to Attachments D and E for selected guidance on the subject.
The responsibilities of the EPA-NE RSCC include: scheduling CLP sample analysis slots
with the NPO Sample Scheduling and Coordination Contract to correspond with the projected
demand for analytical services; providing CL? sample tags, sample labels, custody seals, and
CLP COCICLP Traffic Report Forms for EPA Field Sampling Contractors; coordinating
with the NPO Sample Scheduling and Coordination Contract during sampling and sample
shipment, and resolving any shipment problems concerning the CLP samples; receiving CLP
data from laboratories and distributing Complete SDG Files (CSFs) to Region I Field
Sampling Contractors for validation; and maintaining the New England Sample Tracking
System (NESTS) database which tracks information pertaining to CLP and EPA-generated
non-CLP samples delivered for EPA under the DAS mechanism.
7 2 EPA-NE Site Managers
EPA Site Managers include Site Assessment Managers (SAMs), Remedial Project Managers (RPMs),
On-Scene Coordinators (OSCs) and RCRA Facility Managers (RFMs). They work in the EPA-NE
Office of Site Remediation and Restoration (OSR.R) and have primary responsibility for directing
and/or overseeing response efforts and coordinating all actions at Superfund and RCRA corrective
action sites. The SAMs, RPMs, OSCs, and RFMs establish the project Data Quality Objectives
(DQOs) for their sites.
EPA Site Managers coordinate scoping meetings, assembling all technical personnel and data users
to help identify the appropriate analytical methods, detection levels, level of quality assurance and,
ultimately, the tier level of data validation required for spectfic sample results to achieve the project
Data Quality Objectives. The EPA Site Managers receive copies of Data Validation Reports and Tier
I Validation Cover Letters The OEME QA Unit also receives copies of all Data Validation Reports
and Tier I Validation Cover Letters for use in the Data Validation Oversight/Methods Review
Program
7.3 CLP National Program Office
The CLP is administered by the EPA National Program Office (NPO) under the Office of Emergency
and Remedial Response (OERR), located in Washington, D.C. The NPO is primarily responsible
for the overall management of the CLP in terms of program objectives. The NPO is also responsible
for developing arid administrating CLP contracts. CL? analytical contracts include Statements of
Work for the organic and inorganic analyses of single-phase aqueous or soil/sediment samples. The
NPO CLP short sheets and the Region I Statement of Work (SOW) short sheets for selected past and
present CL? contracts are included in Attachment F
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The NPO is also responsible for formulating and implementing policy and budget; developing and
administrating CLP analytical and support services contracts which include a contract responsible for
sample scheduling and coordination; coordinating the production and dissemination of Superfund
Performance Evaluation Samples; developing and reviewing analytical protocols; and directing CLP
quality assurance in accordance with overall OER.R quality assurance activities and directives.
7.3 1 NPO Sample Scheduling and Coordination Contract ( [ CLASS], formerly Sample
Management Office)
The contractor-operated sample scheduling office provides management, operation and
administrative support to the CLP under the direction of the NPO The primary objective
of this NPO contract is to maintain optimal use of program analytical resources The
contractor supports the NPO in sample scheduling and tracking and performs Contract
Compliance Screening (0 help ensure proper and timely payment of CLP laboratories.
7 3.2 NPO Quality Assurance Technical Support Contract (QATS)
The QATS contract provides quality assurance (QA) support to the CLP under the direction
of the NPO. QATS performs the following functions: preparing performance evaluation
(PE) samples for CLP pre-award and post-award laboratory performance evaluations;
evaluating pre-award and post-award PE sample data; performing QA audits on CLP-
generated data including mass spectrometer data tapes; and assisting in the evaluation and
development of CLP analytical protocols.
7 4 Potentially Responsible Parties (Non Fund-lead)
Potentially Responsible Parties (PRPs) as defined by CERCLA, Section 107, include 1) the current
owners or operators of the facility, 2) any person who at the time of disposal of any hazardous
substance owned or operated the facility at which the hazardous substances were disposed of; 3) any
person who by contract, agreement or otherwise arranged for disposal or treatment, or otherwise
arranged with a transporter for transport for disposal or treatment, of hazardous substances; or 4) any
person who accepts or accepted any hazardous substances for transport to disposal or treatment
facilities or sites from which there is a release or a threatened release “Persons” are defined by the
statute as individuals, commercial entities, corporations, partnerships, associations, joint ventures and
governments.
PRPs that have entered into an agreement with EPA-NE to bear the cost of site investigations and
cleanup or have been unilaterally ordered to implement site cleanups when there is an imminent and
substantial endangerment presented by the site, must use an independent party to validate their data.
All data must be validated in accordance with the most recent revision of the Re2lon I. EPA-NE Data
Validation Functional Guidelines for Evaluarin Environmental Analyses . Any deviations and/or
modifications to these Functional Guidelines must be documented in the QAPJP and/or SAP and must
be approved by EPA prior to sampling
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7.5 Other Federal Agencies (Non Fund-lead)
When a Federal Agency other than EPA owns a Federal Facility designated as a Superfund site, then
as mandated by Section 120 of CERCLA, that Federal Agency is designated the lead Agency for that
Federal Facility Site. That Federal Agency is responsible for validating its own data in accordance
with the most recent revision of the Region 1. EPA-NE Data Validation Functional Guidelines for
Evaluating Environmental Analyses . Any deviations and/or modifications to these Functional
Guidelines must be documented in the QAPjP and/or SAP and must be approved by EPA prior to
sampling
7 6 Other Federal Agencies (Fund-lead)
Other Federal Agencies may enter into Interagency Agreements with EPA-NE to work on Fund-lead
sites. Under an Interagency Agreement, the Federal Agency, i.e., Army Corp of Engineers, may
use the CLP to analyze samples. Alternatively, it may choose to use a non-CLP laboratory to
generate data for EPA. In either case, the Federal Agency should obtain a complete laboratory data
package, in accordance with requirements and/or specifications described in Attachment G so that the
data may be validated in accordance with the most recent revision of the Region I. EPA-NE Data
Validation Functional Guidelines for Evaluating Environmental Analyses . Any deviations and/or
modifications to these Functional Guidelines must be documented in the QAPjP andlor SAP and must
be approved by EPA prior to sampling.
Federal Agencies that utilize CLP for sample analysis must submit quarterly CLP sample projections
to the EPA RSCC. Completed DQO Summary Forms for each sampling event must accompany the
quarterly projections. To reserve sample slots, other Federal Agencies must follow the procedures
outlined in Section 91.3.1.
All CLP Data Validation Reports should be sent to the EPA-NE RSCC who then forwards them to
the EPA-NE CLP-TPO for purposes of contract administration. Non-CLP Data Validation Reports
should not be sent to the EPA-NE RSCC. Rather, non-CLP Data Validation Reports (including DQO
Summary Forms) andlor Final Project Reports should be forwarded to the EPA Site Manager
7 7 States (State-lead/Fund-lead)
New England States may enter into Cooperative Agreements with EPA-NE to work on Fund-lead
sites within their State. Under a Cooperative Agreement, a State may use the CL? to analyze
samples. Alternatively, it may choose to use a non-CLP laboratory such as their own State laboratory
to generate data for EPA. In either case, the State should obtain a complete laboratory data package
in accordance with requirements and/or specifications described in Attachment G so that the data may
be validated in accordance with the most recent revision of the Region I. EPA-NE Data Validation
Functional Guidelines for Evaluating Environmental Analyses . Any deviations andlor modifications
to these Functional Guidelines must be documented in the QAPjP and/or SAP and must be approved
by EPA prior to sampling.
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States that utilize CLP for sample analysis must submit quarterly CLP sample projections to the EPA
RSCC. Completed DQO Summary Forms for each sampling event must accompany the quarterly
projections To reserve sample slots, States must follow the procedures outlined in Section 9.1.3.1
All CLP Data Validation Reports should be sent to the EPA-NE RSCC who then forwards them to
the EPA-NE CLP-TPO for purposes of contract administration. Non-CLP Data Validation Reports
should not be sent to the EPA-NE RSCC. Rather. non-CLP Data Validation Reports (including DQO
Summary Forms) and/or Final Project Reports should be forwarded to the EPA Site Manager.
7 8 EPA Field Sampling Contractors (Fund-lead and PRP/Federal Facility Oversight)
EPA Field Sampling Contractors work under the direction of EPA Site Managers and are primarily
involved in Fund-lead site work and PRP/Federal Facility oversight. Samples collected by EPA Field
Sampling Contractors may be analyzed through the CLP, by the OEME laboratory or through an
EPA-NE analytical contract. Alternatively, the EPA Field Sampling Contractor may be directed by
EPA to procure their own analytical services.
7.8. 1 EPA Field Sampling Contractor Lead Chemist
This section details the responsibilities of the EPA Field Sampling Contractor’s Lead Chemist
working on Fund-lead or oversight activities for EPA-NE However, many of the activities,
roles, responsibilities and qua.lifications discussed below are applicable to non Fund-lead work
performed by a PRP or Federal Facility as well as to Fund-lead work perfonned by another
Federal Agency (i.e., ACOE) or a State.
7 8.1.1 Project Scoping
The Lead Chemist is a key participant in project scoping meetings where project Data Quality
Objectives (DQOs), plans, schedules, sampling techniques, analytical methodologies and data
validation criteria including validation tiers are discussed and agreed upon by the end users
of the data. The Lead Chemist should ensure that all agreed upon DQOs, plans, schedules,
sampling procedures, and analytical methodologies are incorporated into an EPA-approved
QAPjP andlor SAP prior to field sampling.
During the scoping meeting, the Lead Chemist must identify the CLP and non-CLP analytical
methods that are needed to generate data that achieve project DQOs. If CLP methods are
used, then the QAPJP and/or SAP must specify the validation tier, document chat the most
recent revision of the Region I, EPA-NE Data Validation Functional Guidelines for
Evaluating Environmental Analyses will be used without modification to validate the data,
and must be approved by EPA-NE prior to sampling. If non-CLP methods are used and
modified validation criteria are necessary to fully evaluate the data, then the QAPJP and/or
SAP must document the modified validation criteria and provide justification for the
modification. If modified validation criteria are not documented in the EPA-approved QAPjP
and/or SAP prior to sampling, then an amendment to the QAPJP and/or SAP should be
submitted and approved prior to the use of modified validation criteria.
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The Lead Chemist should ensure that the appropriate data validators receive copies of the
completed DQO Summary Forms. The DQO Summary Forms will identify the project
DQOs, PE samples and validation tier. The Lead Chemist should also ensure that the field
sampling noes for the sampling event are provided to the data validator for inclusion in the
Tier I Validation Cover Letter or Data Validation Report for historical purposes
7 8.1.2 Procuring Non-CLP Analytical Services
When required by EPA, the Lead Chemist is responsible for developing technical
specifications for non-CLP analyses that may require modified validation criteria. They are
also responsible for providing technical guidance to subcontracted laboratories to ensure that
fully documented, technically valid, legally defensible and usable data are delivered to EPA
To this end, it is recommended that the Region I Laboratory Pre-Oualification Standard
Operating Procedure from the Region I ARCS Delivery of Analytical Services Pilot Program.
Final Report. Volume II Appendices , 15 March 1994, (Attachment Q), be followed when
procuring non-CLP analytical services (Attachment Q). It is also recommended that the
Region I Laboratory Audit Standard Operating Procedure , from the Region I ARCS Delivery
of Analytical Services Pilot Program. Final Report. Volume II. Appendices , 15 March 1994,
(Attachment Q) be followed to audit laboratories performing non-CLP analyses, as well as
to resolve technical problems and monitor corrective actions implemented by those
laboratories.
7.8.1.3 Performance Evaluation Program
The Lead Chemist is responsible for requesting and maintaining an appropriate inventory of
PE samples and for obtaining all pertinent information regarding their identification and
content in accordance with the EPA Re2ion I Performance Evaluation Pro2ram Guidance ,
July 1996, Revision (Attachment H) or most recent revision. The Lead Chemist must ensure
that a single blind PE sample is included, whenever available, with every sample delivery
group sent to a laboratory for each matrix, analytical parameter, and concentration level
Upon receipt of the laboratory data package, the Lead Chemist is responsible for submitting
to the EPA PE Chemist a copy of the tabulated PE sample results for scoring for those PE
samples provided by EPA.
The PES Score Reports for EPA-provided PE samples and PE results for PE samples
procured from commercial vendors must be evaluated with the laboratory data package during
data validation If only a Tier I validation is performed, the PES Score Reports for EPA-
provided PE samples and PE results for PE samples procured from commercial vendors are
evaluated in addition to performing the Completeness Evidence Audit.
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7.8 1.4 Tracking Data Package Delivery
If a CLP data package is late, then the Lead Chemist is responsible for alerting the EPA
RSCC. If the EPA RSCC is unable to resolve late data delivery within 2 weeks, the RSCC
will contact the CLP-TPO to expedite problem resolution.
If data are late from a non-CLP laboratory subcontracted by an EPA Field Sampling
Contractor, then the Lead Chemist should contact the laboratory to ascertain the problem and
confirm a delivery date. Similarly, if data are late from the Contractor’s own internal
laboratory, then the Lead Chemist should contact the laboratory to ascertain the problem and
confirm a delivery date. In both cases, the Lead Chemist is responsible for expediting late
data.
7.8 1.5 Data Validation
The Lead Chemist is responsible for providing a copy of the project DQO Summary Form,
the field sampling notes, the technical specifications for non-CLP analyses, the PES Score
Reports and/or the QC acceptance ranges for commercial PE samples, and any Telephone
Logs/Communication Forms generated prior to data validation to the data validacor.
The Lead Chemist is responsible for reviewing and approving all Data Validation Memoranda
written by corporate and subcontracted data validators. The Lead Chemist is responsible for
all statements that their validators make in the Data Validation Memorandum concerning the
final data assessments including the limitations and potential uses of validated data.
The Lead Chemist, as a designated Regional CLP representative, is responsible for contacting
the laboratory to obtain necessary data resubmissions for non-compliant CLP data. They
must adhere to the EPA-NE policy for contacting the laboratory, must document in
Telephone Logs/Cotnmumcaion Forms all requests for data resubmissions and time frames,
and must transmit copies of the Telephone Logs/Communication Forms to appropriate
locations. Refer to the procedures in Section 9 1, The Regional/Laboratory Communication
Network.
The Lead Chemist ensures that a Data Validation Report or a Tier I Validation Cover Letter
is delivered to the EPA Site Manager within 21 days of the receipt of a data package from
the laboratory or in accordance with the pre-approved site schedule Expected delays in the
delivery of the validation reports must be reported to the EPA Site Manager.
The Lead Chemist ensures that Fund-lead and PRP/Federal Facility oversight CLP and non-
CL? Data Validation Reports (Tiers II and Ill) and Tier I Validation Cover Letters are
correctly distributed within EPA-NE and to other Regions See Section 13 0 for the list of
recipients and cc:rect distribution
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7 8. 1.6 Reduced Payment/Data Rejection Recommendations
It is the responsibility of the EPA Field Sampling Contractor’s Lead Chemist to ensure that
all contractual defects and unresolved deliverable deficiencies are noted in the Data Validation
Memorandum and on the ORDA/IRDA Form.
Any CLP or EPA-generated non-CLP data that are deemed to be contractually non-compliant
(based on laboratory analytical technical specification) g unusable in making site decisions
should be recommended for rejection, returned to the laboratory and payment denied In this
case, sample results are reported as “rejected” to the EPA Site Manager in the Data
Validation Report. If only one analytical fraction is rejected, then only the data for that
fraction should be returned to the laboratory and the remaining fractions should be validated
in accordance with the guidance provided in Parts II - IV.
Any CLP or EPA-generated non-CLP data that are deemed to be contractually non-compliant
and of reduced worth to the Region in terms of making site decisions should be recommended
for reduced payment. In this case, sample results should be qualified in accordance with the
guidance provided in Parts II-IV of this document.
78.161 CLPData
The Lead Chemist is responsible for notifying the EPA Data Validation Chemist when CLP
data are contractually non-compliant and unusable, in accordance with EPA-NE Standard
Operating Procedures for Submitting Data for Reduced Payment/Data Rejection , September
1991 (Attachment I) or most recent revision and in accordance with the Federal Acquisition
Regulation (FAR). The Lead Chemist is responsible for providing to the EPA Data
Validation Chemist a letter describing the contractual non-compliances and providing
supporting documentation within the time frame specified in the SOP mentioned above.
7 8 1 6.2 EPA-Generated Non-CLP Data (i.e., DAS Data)
The Lead Chemist is responsible for documenting contractual non-compliances, determining
if they affect the potential usability of the data, and ensuring that EPA does not pay for
unusable, non-compliant EPA-generated non-CLP data
7 8.1.7 Data Validation Oversight and Implementation of Corrective Action
The Lead Chermst is responsible for responding to all requests for data validation oversight
by the Region. The Lead Chemist reviews the “EPA-NE-generated Data Validation
Oversight/Methods Review Memoranda” and directs the implementation of appropriate
corrective actions. Subsequently, the Lead Chemist monitors the implementation and is
responsible for the continued effectiveness of all corrective actions.
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78.1.8 Qualifications of the Lead Chemist
The Lead Chemist should have a B.S. degree in chemistry or a related physical science and
be a professionally trained analytical chemist with at least eight to ten years of combined
inorgamc and organic analytical experience which includes familiarity with GC/MS and !CP
instrumentation. The Lead Chemist should have extensive knowledge of CLP methods,
deliverables, and program operation as well as extensive knowledge of all other EPA
program analytical methodologies, i.e., RCRA SW 846 methods, Drinking Water Program
500 series methods, ambient air and stack testing, etc , to enable them to recommend the
appropriate methods and modifications for those methods for achieving project DQOs
The Lead Chemist should have extensive knowledge of the most recent EPA-NE validation
requirements, as specified in this document. The Lead Chemist must be technically able to
identify the need to modify validation criteria when non-CLP analyses are performed and
must be able to incorporate and document the modified validation criteria into an EPA-
approved QAPjP and/or SAP.
7 8 2 Data Validator
This section specifically details the responsibilities of the EPA Field Sampling Contractor’s
data validator performing validation on data generated for Fund-lead sites or EPA oversight
activities. However, many of the activities, roles, responsibilities and qualifications discussed
below are applicable to non Fund-lead work performed by a PRP or Federal Facility as well
as to Fund-lead work performed by another Federal Agency (i.e., ACOE) or a State.
7 8 2.1 Data Validation
Data validators must assess the analytical deficiencies and contractual non-compliances of a
data package in accordance with the most recent revision of the Region 1. EPA-NE Data
Validation Functional Guidelines for Evaluating Environmental Analyses They are
responsible for using modified validation criteria when required by an EPA-approved QAPjP
andlor SAP.
The data validator is responsible for obtaining resubmirtals for non-compliant data from the
laboratory In the CLP system, only designated regional communication representatives may
contact a CLP Laboratory (usually the Lead Chemist), therefore the data validator must
contact the laboratory through their designated CLP communication representative or
alternate
The validator reviews the Data Quality Objectives for the project as documented in the
QAPjP or SAP and DQO Summary Form and determines if the degree of ‘measurement
error” associated with the data potentially compromises data usability The driving force for
data validation is that contractually compliant data are not always technically usable for
making site decisions and that contractually non-compliant data are sometimes very usable
Only the end user can determine actual usability of the data.
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The data validator must notify the Lead Chemist immediately if significant contractual
deficiencies warrant recommendation for data rejection or reduced payment.
The data validator is responsible for using the appropriate DQO Summary Form and should
contact the Lead Chemist if this document has not been provided.
The data validator must contact field samplers whenever necessary to obtain information to
assess “sampling error’. All communications must be documented in a Telephone
Log/Commumcacion Form and included in the Data Validation Report. If a copy of the field
sampling notes was not provided, then the data validator should contact the Lead Chemist to
obtain the notes.
The data validator must have the technical specifications for non-CLP analyses and any
additional data quality criteria specified in the QAPjP or SAP in order to validate non-CLP
data. If the technical specifications for non-CLP analyses and additional data quality criteria
were not provided, then the data validator should contact the Lead Chemist to obtain the
applicable technical specifications and data quality criteria.
The data validator must obtain the PES Score Reports for CLP and non-CLP analyses in
order to validate the sample data. If PES Score Reports were not provided, then the data
validator should contact the Lead Chemist to obtain the applicable PES Score Reports. If
commercial PE samples were used, then the data validator should obtain the vendor’s QC
acceptance limits from the Lead Chemist in order to evaluate the PE sample results
The data validator must obtain any Telephone Logs/Communication Forms generated prior
to data validation for CLP and non-CLP analyses in order to validate sample data. If any
Telephone Logs/Communication Forms generated prior to data validation for CLP or non-
CLP analyses were not provided, then the data validator should contact the Lead Chemist to
obtain any applicable Telephone Logs/Communication Forms generated prior to data
validation.
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The data validator generates a Tier I Validation Cover Letter with the following attachments
in the order specified below: (Refer to Section 10 for complete description of Tier I
Validation Cover Letter)
Cover Letter
2 Attachments
a CADRE-generated Data Summary Table of Unvalidated Data (not
required if CADRE Review not performed)
b. Data Validation Worksheet XI-Accuracy Check and EPA PE Score
Reports and/or non-EPA PES results with Vendor PES QC
Acceptance Limits
c. Support Documentation
i. Copy of non-CLP analytical method, e g , DAS methods,
modified EPA methods
ii. Copies of Telephone Logs/Communication Forms for.
• RSCC communications
• Requests for laboratory data resubmissioris/
clarifications
• Communications with samplers resolving sampling
problems
• Communications with TPO/Lead Chemist to report
contractually-deficient data for rejectionlreduced
payment
• Communications with EPA Site Manager concerning
possible data rejection
• EPA Site Manager authorization for alternate DV
tier
in. Copies of data supporting recommendations for reduced
payment resulting from CSF Audit and/or PE sample result
evaluation
iv. Original data to support recommendations for data
rejection/non-payment resulting from CSF Audit and/or PE
sample result evaluation
v. Copies of field sampling notes and/or field report supplied
by field sampler
vi. Copies of EPA-approved amendments to QAPjP and/or SAP
describing modified criteria to be used for validating site
data
d CSF Completeness Evidence Audit
e DQO Summary Form
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The data validator generates a Data Validation Report, applicable to Data Validation Tiers
LI and LII, that consists of the following components in the order specified below: (Refer to
Section 11 for a description of each of the Data Validation Report components).
1. Organic Regional Data Assessment/Inorganic Regional Data Assessment
(ORDA/IRDA) Form
2. Data Validation Memorandum
a. Narrative
b. Table I-Qualifier Recommendation Summary Table
c. Table lI-Overall Evaluation of Data
d Table 111-Tentatively Identified Compounds
e. Data Summary Tables
3. Standard Data Validation Worksheets
a. Manual
b. Automated Data Review Reports (i.e., CADRE)
4 Support Documentation
a. Copy of non-CLP analytical method, e.g , DAS methods, modified
EPA methods
b. Copies of EPA PES Score Reports and/or non-EPA PES results with
Vendor PES QC Acceptance Limits
c. Copies of Telephone Logs/Communication Forms for:
• RSCC communications
• Requests for laboratory data resubrnissions/clarifications
• Communications with samplers resolving sampling problems
• Communications with TPO/Lead Chemist to report
contractually-deficient data for rejection/reduced payment
• Communications with EPA Site Manager concerrung possible
data rejection
• EPA Site Manager authorization for alternate DV tier
d Copies of data supporting recommendations for reduced payment
resulting from CSF Audit and/or PE sample result evaluation
e. Original data to support recommendations for data rejection/non-
payment identified from Tier II or Tier Ill data validation
f. Copies of field sampling notes and/or field report supplied by field
sampler
g. Copies of EPA-approved amendments to QAPjP andlor SAP
describing modified criteria to be used for validating site data
5 CSF Completeness Evidence Audit
6 DQO Summary Form
The data validator is responsible for implemerning all corrective actions required by the
contractor Lead Chemist in response to EPA-NE data validation oversight findings
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7 8 2.2 Qualifications of the Data Validator
7.8 2.2. 1 Senior Validator
The senior data validator should have a B.S. or B A. degree in chemistry or a related
physical science and be a trained analytical chemist specializing in a particular discipline such
as GC pesticides, CC/MS organics, or ICP metals. The validator should have at least five
years of related analytical/instrumentation experience working with laboratory instrumentation
and analyzing multi-media environmental samples (soil, water, oil, waste, fly ash, biological
tissue and air). Data validation experience cannot be substituted for any of the five years
required laboratory experience
The senior validator should have extensive knowledge of the most recent EPA-NE validation
requirements as specified in this document. The validator must also be capable of applying
modified validation criteria when required by the EPA-approved QAPjP and/or SAP.
All Data Validation Reports must undergo internal peer review by the organization
performing the validation. A senior validator must perform secondary review of all Data
Validation Reports prepared by junior validators. If a senior validator prepares a Data
Validation Report, then a different senior validator or other qualified senior chemist must
peer review that Report
7.8.2.2 2 Junior Validator
The junior validator should have a B.S. or B.A. degree in chemistry or a related physical
science and be a trained analytical chemist specializing in a particular discipline such as GC
pesticides, GCIMS organics, or ICP metals. The validator should have at least two years of
related analytical/instrumentation experience working with laboratory instrumentation and
analyzing multi-media environmental samples (soil, water, oil, waste, fly ash, biological
tissue and air). Data validation experience may be substituted for some of the two years of
required laboratory experience However, the junior validator must have at least six months
of instrumentation experience in the areas described above.
The junior validator should have extensive knowledge of the most recent EPA-NE validation
requirements as specified in this document. The validator must also be capable of applying
modified validation criteria when required by the EPA-approved QAPjP and/or SAP
8.0 INFORMATION REVIEWED DURING THE DATA VALIDATION PROCESS
Figures 1, 2 and 3 illustrate the normal flow of the data validation process Sources of information
are noted. as well as communication channels and key decision points in the validation process To
evaluate data quality and the extent of ‘measurement error’, the following items must be incorporated
into the review of sample data. project scoping information documented in the EPA-approved SAP
and/or QAPjP, analytical results presented in the laboratory data package, field sampling information.
Contract Compliance Screening results; and Performance Evaluation Sample results.
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8.1 Project Scoping [ nformation
811 Objective
The QAPjP andlor SAP is a planning document that provides project history and background
data and documents the project DQOs and sample custody procedures, evidenciary
requirements, analytical methods, laboratory QAIQC, laboratory documentation and
deliverables, and data validation criteria and validation tier to be used for the project. These
items should be agreed upon by all end users in the initial pl2nning phase of the project.
8 1.2 Requirements
The DQOs should be fully discussed and documented in the EPA-approved QAPjP and/or
SAP and identified in abbreviated format in a DQO Summary Form. A copy of the SAP
and/or QAPjP should be available to the validator and should include: the data validation
criteria to be used (refer to Figure 4), reference to the Tier level of validation to be
performed, modified validation criteria to be used (if any) or alternate validation criteria, i.e
USATHAMA and split sample comparability criteria and decision trees to be used in
assessing split sample analyses. Project documents should detail the exact number of
samples, types of samples (field and QC), PE samples, sample matrices, sample
locations/descriptions and knowledge of any positive detects from prior site sampling efforts.
Background information on the site is essential to identifying potential usability issues. The
EPA Site Manager or Field Sampling Contractor Site Manager are the best sources for
additional site information.
8. 13 Evaluation
a. The validator should ascertain from the EPA-approved QAPJP, SAP and/or DQO
Summary Form which validation criteria were selected by the end users The
validator should ascertain whether the validation criteria contained in the Region I.
EPA-NE Data Validation Functional Guidelines for Evaluating Environmental
Analyses are to be used without modification to validate site data, or whether
modified EPA-NE validation criteria are to be utilized. Also, the validator must
ascertain from the project planning documents if alternate validation criteria, i e
USATHAMA are to be used for data validation.
b. If the Region I, EPA-NE Data Validation Functional Guidelines for Evaluatiiig
Environmental Analyses were selected as the validation criteria by the end user, then
the data validator should ascertain from the EPA-approved QAPjP, SAP and/or DQO
Summary Form, the validation tier that are to be used to evaluate the project data.
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c. The validator should determine if the correct analytical method as cited in the EPA-
approved SAP, QAPjP, and/or DQO Summary Form was used for analysis and if
required detection/quantitation limits were achieved.
d. The valjdator should be familiar with the project DQOs, as summarized on the DQO
Summary Form, in order to identify potential usability issues for the end users
e Comparability criteria for split sampling should be presented in the EPA-approved
QAPJP and/or SAP. Split sampling analyses are performed for PRP/Federal Facility
oversight using standardized EPA (full protocol) methods. Field screening
confirmatory analyses are also performed using standardized EPA methods. The %
Difference Criteria between data sets should be based on the following standard
equations to ensure consistency in presenting and assessing split data. Note:
Comparability criteria should be based on historical data generated for the site and
should take into account associated field precision. Homogenous matrices may allow
for lower % Difference Criteria while heterogeneous matrices may necessitate higher
% Difference Criteria to be set. A discussion and justification for selection of
comparability critena should be included in the EPA-approved QAPjP and/or SAP
Split Sampling Analyses
Equation 3: % Difference (Split Sampling) = C 1 C 2 x 100
C: + C 2
2
= Concentration Determined by EPA Oversight Analysis
C = Concentration Determined by PRP, Federal Facility, or State Analysis
Note that this equation assumes that values generated by EPA and those values
generated by equivalent methods used by the PRP (or other entitles) are equally
accurate While this may not always be true, the equation serves to standardize
reporting conventions and to promote data comparability. Note that this equation
retains the sign of the difference, thus absolute numbers are not used
Confirmatory Analyses
Equation 4: % Difference (Confirmatory Analysis) = C 2 G 2 x 100
C 1 = Concentration Determined by Full Protocol Confirmatory Analysis
C 2 = Concentration Determined by Field Screening Analysis
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Note that this equation assumes that values generated by the full protocol
confirmatory method are more accurate than those generated by field screening
methods. While this may not always be true, the equation serves to standardize
reporting conventions and to promote data Comparability. Note that this equation
retains the sign of the difference, thus absol’iie numbers are not used.
8 1 4 Action
a. If no validation tier or an inappropriate validation tier has been referenced in the
DQO Summary Form, then the validator should contact the Lead Chemist who will
obtain clarification/direction from the EPA Site Manager. The validator and/or Lead
Chemist should document this call in a Telephone Log. The validacor should note
in the first paragraph of the Data Validation Memorandum if, in the validator’s
opinion, the validation Tier selected during project scoping does not meet the project
DQOs.
b. i. If the EPA-approved QAPJP and/or SAP does not cite specific validation
criteria, then the validator must validate site data according to the most
recent revision of the Region I, EPA-NE Data Validation Functional
Guidelines for Evaluating Environmental Analyses . The validator should
note in the first paragraph of the Data Validation Memorandum that the data
has been validated in accordance with the most recent revision of the Region
I, EPA-NE Data Validation Functional Guidelines for Evaluating
Environmental Analyses .
ii. If modified or alternate validation criteria have been described in an EPA-
approved QAPjP and/or SAP, then the validator should note these modified
or alternate validation criteria in the first paragraph of the Data Validation
Memorandum and copies of the relevant QAPjP or SAP pages should be
attached to the Memorandum as supporting documentation.
iii. Alternatively, if the validator determines that modified or alternate validation
criteria are necessary to validate the site data in order to support project
DQOs and/or the use of non-CLP methods and those criteria have not been
included in the EPA-approved site QAPJP/SAP, then an amendment to the
QAPjP or SAP must be submitted to EPA and approved prior to validation.
The amendment should be noted in the first paragraph of the Data Validation
Memorandum and a copy attached to the Memorandum as supporting
documentation.
c. If the data are contractually compliant but unusable because the wrong analytical
method was selected and/or utilized, then this should be noted in the Data Validation
Memorandum and an alternative method should be identified for future site work.
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d. If the DQO Summary Form was not provided, then the validator should contact the
Lead Chemist to obtain the Form. If a DQO Summary Form was not completed
prior to the sampling event, then this should be noted in the first paragraph of the
Data Validation Memorandum.
e If split sampling criteria for oversight analyses or field screening confirmatory
criteria for confirmation analyses have not been established, then the validator should
contact the Lead Chemist who will obtain clarificationidirection from the EPA Site
Manager. The validator and/or Lead Chemist should document this call in a
Telephone Log
8 2 The Data Package
8 2 1 Objective
The CLP Complete SDG File (CSF) data package is designed to provide all necessary
documentation to verify compliance with the Statement of Work (SOW) and to permit
verification of the accuracy and defensibility of the reported results. It contains all the
original data generated for the data package.
A non-CLP data package should also provide all necessary documentation to verify
compliance with the analytical method and/or contracts/subcontracts to permit verification of
the accuracy and defensibility of the reported results. It should contain all the original data
generated for the data package.
8 2 2 Requirements
A list of the required CLP deliverables may be found in the appropriate CLP SOWs.
Required non-CLP deliverables may be found in the appropriate methods and/or
contracts/subcontracts developed for the analytical service. Most data collection activities
will require all original data and a complete case file purge See Attachment G for Training
Manual for Reviewing Laboratory Data Package Completeness , June 1994.
8 2 3 Evaluation
Procedures for the evaluation of specific deliverables are detailed in Parts II, III, and IV of
this document
8 2 4 Action
When contract-required information necessary for data validation is missing from the data
package, then the validator should arrange for the Lead Chemist to contact the laboratory to
obtain the omitted data according to the procedure referenced in Section 9 2
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Only authorized personnel that are designated Regional CLP representatives may contact CLP
laboratories. Only prime contractors may contact their subcontracted laboratories due to
privity of contract.
8 3 Field Sampling Information
8.3.1 Field QA/QC Samples
831.1 Objective
Field QA/QC samples, such as trip blanks, equipment blanks, bottle blanks, and field
duplicates enable data validators to identify some, but not all, of the “sampling error”
associated with the project. Specifically, the field QA/QC assist the data validator in
evaluating sampling conditions, techmques, field precision, and sample homogeneity.
8.3 1.2 Requirements -
All field QA/QC sample requirements should support the project DQOs and should be
documented in the EPA-approved QAPJP and/or SAP and DQO Summary Form.
At a minimum, equipment blanks and field duplicates must be included at a frequency of five
percent per analytical parameter/matrixlsampling team.
At a minimum, volatile trip blanks are required at a frequency of one per shipment cooler
At a minimum, temperature indicator blanks are required at a frequency of one per shipment
cooler and should be clearly identified as temperature indicator blanks
Bottle blanks are used to verify the cleanliness of a specific Lot Number of bottles and should
be included at the discretion of the sampling team At a minimum, bottle blank analyses
should be performed on one bottle per container type per lot. The Lot Number for the bottle
blank should be noted on the Traffic Report andlor Chain-of-Custody Form and in the field
sampling notes
831.3 Evaluation
Note that for large projects containing several sample delivery groups (SDGs) with many
field samples and inter-related QC samples, the EPA Field Sampling Contractor may assign
a Project Chemist to coordinate data collection and review. For large projects where the data
validator alone may not be able to fully assess field QA/QC compliance with the EPA-
approved QAPjP and/or SAP, the assigned Project Chemist should review all the individual
project Data Validation Reports to assess project compliance for field QA/QC requirements
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The validator should confirm that the required field QA/QC samples were provided to the
laboratory at the proper frequency.
It is recommended that the results for each bottle blank (used to verify the cleanliness of a
specific Lot Number of bottles) be evaluated prior to use of bottles from that Lot Number
for field sampling
The validator should evaluate contamination found in the equipment, trip and bottle blanks
as part of the laboratory method blank review. Similarly, field duplicate precision should be
evaluated concurrently with laboratory duplicate (MS/MSD) precision data to determine
whether precision problems were laboratory or field related.
8 3 1.4 Action
a If the field QA/QC samples were not provided to the laboratory in accordance with
the frequency specified in the EPA-approved QAPjP/SAP, then the validator should
note this deviation in the Data Validation Memorandum and the EPA Field Sampling
Contractor should initiate corrective action procedures.
b If the laboratory has not provided results for one or more of the samples that were
shipped, the validator should check the Data Package Narrative and Telephone
Logs/Communication Forms for a possible explanation (broken sample, insufficient
sample volume for reanalysis, etc.) If no explanation is found, then the validator
should contact the Lead Chemist who in turn contacts the RSCC to further investigate
and resolve CLP issues, For non-CLP samples, the validator should contact the
appropriate personnel to resolve the problems
c The field sampler must be informed immediately by the validaror, and the call
documented in a Telephone Log/Communication Form, if any of the following
problems are noted
• trip blanks, equipment blanks, bottle blanks or field duplicates are not
identified on the Traffic Report/Chain-of-Custody Form
• anomalies such as Traffic Report numbers being listed twice, etc
• high contamination in equipment, trip, or bottle blanks that is not present in
the laboratory blanks
8 3 2 Sample Descriptions
83 2 1 Objective
All sample locations should support the project DQOs and be documented in the EPA-
approved QAPjP and/or SAP
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Sample descriptions/locations/sampling dates are necessary information for preparing the Data
Summary Tables and for the evaluation of holding times. In addition, sample descriptions
are useful as supplementary information for the consideration and discussion of matrix
problems and chemical constituents identified in particular samples.
8.3 2.2 Requirements
All sample locations should be sampled and numbered in accordance with the EPA-approved
QAPjP and/or SAP.
For CLP data packages, copies of properly completed Traffic Reports (Attachment J, Form
vi) are mandatory deliverables
Copies of Chain-of-Custody Forms (Attachment J, Form v) must be included in all non-CLP
data packages and must contain the date of sampling, sample numbers, as well as the
sampling locations.
The sampler or Project Chemist should provide a copy of the field sampling notes to the Lead
Chemist or data validator to be included in the Data Validation Report. In situations where
sampling events extend over a period of weeks producing two or more SDGs and generate
numerous pages of field log book notes, the field notes should be copied only once, included
in one Data Validation Report and that Data Validation Report should be referenced by Case,
SDG, and date of Data Validation Report.
8 3.2.3 Evaluation
Again, note that for large projects containing several sample delivery groups (SDGs) with
many field samples and interrelated QC samples, the EPA Field Sampling Contractor may
assign a Project Chemist to coordinate data collection and review. For large projects where
the data validator alone may not be able to fully assess field QA/QC compliance with the
EPA-approved QAPjP and/or SAP, the assigned Project Chemist should review all the
individual project Data Validation Reports to assess project compliance for field QA/QC
requirements.
The validator should confirm from the EPA-approved QAPjP and/or SAP and DQO
Summary Form that all sample locations have been sampled and that there are sample results
for all locations.
Traffic Reports and COC Forms must be compared for consistency with respect to the
designation of quality control samples (blanks and duplicates) and the identification numbers
for field samples
The data validator is responsible for evaluating field sampling notes They are to be
included in the Data Validation Report to be used by the end user to assess data usability and
to support potential litigation
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8.3.2 4 Action
a. If sample locations are not sampled in accordance with the EPA-approved QAPjP
and/or SAP, then the validacor should note this deviation in the Data Validation
Memorandum and the EPA Field Sampling Contractor should initiate corrective
action procedures.
b. If discrepancies on the COC or Traffic Report Forms are identified, then the sampler
must be contacted for resolution. The resolution must be documented in a Telephone
Log (Attachment J, Form iii) and the Telephone Log must be included in the Data
Validation Report.
c If information is illegible (sample descriptions, locations, sampling date, etc ), then
the sampler must be contacted to provide a legible copy of this information
d. If Traffic Reports or COC Forms are missing, then the laboratory should be
contacted to obtain this required deliverable. If the laboratory caimot provide this
required deliverable, then the sampler must be contacted to provide a copy of these
documents. If the Traffic Reports or COC Forms were not properly completed
andlor signed by the laboratory personnel, then the laboratory must be contacted to
obtain a written letter detailing the deficiency. This letter should be included in the
CSF/data package as part of the site record and a copy included in the Data
Validation Report
e If the field sampling notes are not provided prior to validation, then the validator
must obtain a copy from the Lead Chemist for inclusion in the Data Validation
Report.
8 4 CLP Laboratory Contract Compliance Screening (CCS)
8 4 1 Objective
CCS provides a high volume assessment of CLP deliverables for compliance with some, but
not all, contract requirements. Its primary application is to determine payment
recommendation Because of this direct link to payment, CCS fosters a somewhat timely
resolution of contractual problems.
8 4.2 Requirements
The NPO Sample Scheduling and Coordination Contract (currently named CLASS) performs
CCS on all low/medium organic and inorganic data packages submitted through the CLP
Laboratories are required by EPA to submit all identified missing data, and resubmit or
exc lain all data identified as non-compliant during CCS To date, CCS has not been
performed on CL? dioxin data packages. Also, CCS is not performed on EPA-generated
non-CL? data.
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8.4 3 Evaluation
CCS may be used, when available, during data validation to evaluate those technical criteria
that are also contractual criteria and to determine the completeness of the data package If
available, CCS results should be previewed to determine important compliance issues. The
validator should compare the findings of CCS to the laboratory data package in the course
of data validation. An example regional CCS Report is contained in Attachment K.
8 4.4 Action
a. If the CCS information is not provided with the data package, it can be requested
through the RSCC. CCS information is not necessary in order to perform validation
because the validator assesses contractual compliance during the validation process
b If the CCS information indicates significant contractual non-compliance which
coincides with poor technical quality and potentially limits the usability of the data,
then the validacor should recommend reduced payment or rejection of data (See
Attachment I).
c. When a contract-required reanalysis or deliverable was noted as missing by CCS, the
validator should contact the laboratory to ascertain the expected delivery date.
8 5 Performance Evaluation Samples
8.5 1 Objective
The EPA-NE Performance Evaluation (PE) Program essentially serves three functions (1)
PE samples may be used in laboratory pre-award evaluations to identify a community of
technically capable labor .itories, (2) PE samples are used to evaluate laboratory performance
over a period of time, (3) PE samples are included in a sample group to provide information
on a laboratory’s ability to accurately identify and quantitate analytes of interest during the
period of sample analysis. In the third function, the PE program works in conjunction with
the Region I Tiered Validation approach.
8.5.2 Requirements
EPA-NE established a Performance Evaluation Program on July 1, 1993 A copy of the most
recent revision of the EPA Region I Performance Evaluation Program Guidance , July 1996,
Revision, may be found in Attachment H. The document describes the purpose, use, quality
assurance documentation requirements, responsibilities, and general procedures for utilization
of the EPA-NE PE Program arid includes a list of EPA-PE samples that are currently
available through the EPA-NE QA Unit and a list of commercially available PE samples
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It is recommended chat blind FE samples be included in each sample set sent to a laboratory,
whenever appropriate, to assist in evaluating analytical data quality One FE sample should
be included for each sample matrix, parameter, and concentration level for each Sample
Delivery Group (SDG) sent to a laboratory The PE samples should be counted as field
samples in the 20 sample SDG. The use of FE samples should be specified as a quality
control measure at the planning stage of each project and documented in the EPA-approved
QAPjP and/or SAP.
8 5 3 Evaluation
Upon receipt of the laboratory data package, the Lead Chemist or validator should determine
if a PE sample was included for each sample matrix, parameter, and concentration level for
each SDG sent to the laboratory. Next, the laboratory’s EPA PE sample results must be
submitted by the EPA Field Sampling Contractor performing data validation to the EPA-NE
FE Chemist for scoring. In the siwation where data validation is performed by a
subcontractor, only the prime contractor may submit PE results to EPA.
For Tier H and Tier III validations, the data validator must incorporate the EPA-PE sample
score results into the evaluation of data in accordance with Section Xl in Parts II, III and IV
of this document.
For Tier I validations, EPA-PE sample results must also be scored and evaluated in
accordance with the guidance noted above to determine whether laboratory problems exist
and whether a higher validation tier is warranted based upon analytical problems identified
by the PES.
If non-EPA (commercial) PE samples are reported in the data package, then the validator
should assess the results of the PE samples based upon the vendor’s QC acceptance limits in
accordance with Section XI in Parts II, III, and IV of this document.
8 5 4 Action
a. If FE samples were not submitted by an EPA Field Sampling Contractor in
accordance with the frequency requirements stated in the Region I policy, then the
validator should note this deficiency in the Daa Validation Memorandum. If an EPA
Field Sampling Contractor consistently fails to comply with Region I policy,
corrective action will be required
b. If PE sample results are acceptable or do not indicate major laboratory performance
problems, then the validator should complete the Tier I, II or Tier Ifl validation.
c If FE sample results indicate major laboratory performance problems and are
unacceptable and a Tier II or Tier III validation was required. then the validation
should be completed to ascertain the source of the analytical error. If the data quality
is suspect, then the data should be recommended for reduced payment or,
alternatively, rejected as unusable. returned to the laboratory and payment denied
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d. If PE sample results are unacceptable and a Tier I validation was required, then the
validator should document this in the Tier I Data Validation Cover Letter and
consider the need to upgrade the tier level to determine if the data is unusable and
should be rejected. The validacor must receive authorization from the EPA Site
Manager to upgrade the data validation tier prior to doing so. Authorization must
be documented in a Telephone Log and included in the Tier I Validation Cover
Letter, or (if the validation tier was upgraded) in the Data Validation Report.
8.6 Computer-Aided Data Review and Evaluation (CADRE) Reports
8.6. 1 Objective
CADRE is a computer program that was developed to perform automated validation of
organic and inorganic Low/Medium CLP data that have been entered into the national CLP
Analytical Results Database (CARD). The automated review criteria are based on the
USEPA CLP National Functional Guidelines for Organic Data Review , February 1994, and
the USEPA CLP National Functional Guidelines for Inorganic Data Review , February 1994.
In most cases, CADRE criteria are similar to Region I Tier II validation criteria. Where the
criteria are different, the CADRE program has been customized for EPA-NE to incorporate
EPA-NE Validation criteria. For those additional validation criteria, e.g. field duplicates,
that are not assessed by CADRE, a Guidance Document for Completing Region I Data
Validation Utilizing CADRE Data Review , February 1995 (Attachment L) is available to
assist data validation completion.
Currently, this automated validation program is available only for EPA CLP Fund-lead and
oversight use. However, in the future, computer-assisted data validation for EPA-generated
non-CLP data may be ava. able.
8 6.2 Requirements
Eventually, all EPA-NE CLP Organic and Inorganic Low/Medium SOW laboraory data
packages will be validated using CADRE. Currently, CADRE reports for CLP Organic
Low/Medium Volatile and Semivolatile analyses are provided to the EPA Field Sampling
Contractor along with the CSF/CLP laboratory data package to assist in data validation.
8 6 3 Evaluation
Tier I validation does not include the review of CADRE Reports. The validator should
include the CADRE-generated Data Summary Table of NOT VALIDATED DATA as an
attachment to the Tier I Validation Cover Letter.
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Tier II and III validations include the use of CADRE reports. Refer to the Guidance
Document For Completing Region I Data Validation Utilizing CADRE Data Review ,
February 1995, or most recent revision for guidance on data validation completion in
conjunction with CADRE review.
8.6.4 Action
Occasionally laboratory electronic deliverables are unavailable, incomplete or of such poor
quality that they cannot be used by the CADRE program. If a Low/Medium Organic or
Inorganic CLP CSF is received by the EPA Field Sampling Contractor from EPA without
a CADRE report but with a notification that manual validation is required, then the EPA
Field Sampling Contractor must perform manual validation for that CLP CSF.
If the CADRE report is incomplete, then the validator should contact the EPA DV Chemist
to obtain the complete report.
9.0 COMMUNICATION NETWORKS
9 1 The CLP-Regional Sample Control Center (RSCC) Communication Network
9.1 1 Objective
9.1 1.1 CLP
The Regional Sample Control Center (RSCC) is synonymous with the Regional Sample
Control Coordinator (RSCC) for EPA-New England. The RSCC places all regional requests
for CLP sample analyses through the NPO Sample Scheduling and Coordination Contract
(currently named CLASS). Requests for CLP analyses may be initiated by EPA Site
Managers or Field Sampling Contractors doing Fund-lead or PRPfFederal Facility oversight,
or States (or their contractors) performing Fund-lead work under Cooperative Agreements
with EPA, or other Federal Agencies (or their contractors), i e., the Army Corp of
Engineers, performing Fund-lead work under Interagency Agreements.
The RSCC tracks CLP samples originating from Region I, regardless of the organization that
collects them, in the New England Sample Tracking System (NESTS) database.
9 11.2 Non-CLP
The RSCC does not schedule non-CLP analytical services for EPA Field Sampling
Contractors, States or other Federal Agencies However, the RSCC schedules non-CLP
analytical services that are obtained directly through any of EPA-New England’s regional
environmental analytical procurements.
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The RSCC tracks all rion-CLP samples collected by EPA Field Sampling Contractors doing
Fund-lead or PRP/Federal Facility oversight work, i.e., through the DAS mechanism.
The RSCC does not track non-CL? samples collected by the States or other Federal Agencies
doing Fund-lead work under Cooperative Agreements and Interagency Agreements,
respectively
9 1 2 Requirements
9.12.1 CL?
EPA Field Sampling Contractors must submit quarterly CLP sample projections to the RSCC.
Completed DQO Summary Forms for each sampling event should accompany the quarterly
sample projections and must be submitted prior to sampling To reserve sample slots the
EPA Field Sampling Contractor must follow the procedures outlined in 9.1.3 1.
States and Federal Agencies that utilize CLP for sample analysis must also submit quarterly
CLP sample projections to the RSCC. Completed DQO Summary Forms for each sampling
event must accompany the quarterly projections. To reserve sample slots States and other
Federal Agencies must follow the procedures outlined in 9 1.3 1.
If EPA personnel will be collecting samples at a site for CLP analyses, then the Site Manager
must notify the RSCC and submit a completed DQO Summary Form by 5 00 p.m. on the
Tuesday before the scheduled sampling event.
9 1.2 2 Non-CLP
EPA Field Sampling Contractors that procure non-CLP analytical services, or use their own
corporate laboratory to analyze non-CLP samples or use the EPA regional laboratory for non-
CL? analyses must follow the sample tracking procedures referenced in 9.1.3.2. Completed
DQO Summary Forms must be submitted to the RSCC prior to the sampling event.
Ststes, other Federal Agencies, PRPs and Federal Facilities are not required to report non-
CLP sample tracking information to the EPA at this time. However, States, ocher Federal
Agencies, PRPs and Federal Facilities should maintain non-CLP sample tracking information
in their site files to assist EPA in tracking non-CLP data upon EPA’s request.
9 13 Procedure
9131 CL?
EPA Sampling Field Contractors, EPA Site Managers, States and other Federal Agencies
requiring CLP services must contact the RSCC in accordance with The Re2ional Sample
Control Center Guidance for The Contract Laboratory Pro2ram (CLTh and Deliverv of
Analytical Services (DAS Pro2ram for EPA-New England . July 1996 (Attachment P)
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9.1.3.2 Non-CLP
EPA Field Sampling Contractors that procure their own non-CLP analytical services, or
obtain non-CLP services from their corporate laboratory or from the EPA-NE regional
laboratory must report the sample tracking information to the RSCC in accordance with i]i
Re ionaI Sample Control Center Guidance for The Contract Laboratory Program (CLP) and
Delivez-v of Analytical Services (DAS) Program for EPA-New England , July 1996 (Appendix
P) and the DAS Sample Tracking and Scheduling Standard Operating Procedure , from the
Region I ARCS Delivery of Analytical Services Pilot Program, Final Report, Volume II
Appendices , 15 March 1994, (Attachment Q).
States and other Federal Agencies that procure non-CL? analytical services or obtain non-
CL? services from their organizations’ own laboratory should schedule and track samples in
accordance with their organizauons’ procedures.
9 1.4 Action
91.41 CL?
CL? analysis requests by an EPA Field Sampling Contractor, State or other Federal Agency
must be made by 5 OO p.m. the Tuesday before sampling. If a request is made later than this
time, sample analysis slots cannot be guaranteed. Also, if DQO Summary Forms are not
submitted prior to the sampling date, sample analysis slots cannot be guaranteed.
If an EPA Field Sampling Contractor consistently fails to allow for sufficient lead time in
scheduling CLP samples and/or fails to accurately project quarterly CLP analytical needs,
and/or fails to submit the associated DQO Summary Forms, corrective action will be
required.
If a State or other Federal Agency performing Fund-lead work fails to allow for sufficient
lead time in scheduling CLP samples and/or fails to submit the associated DQO Summary
Forms, corrective action will be required.
9 1 4 2 Non-CLP
If an EPA Field Sampling Contractor, performing Fund-lead work or PRP/Federal Facility
oversight, fails to provide the required non-CLP sample tracking information and/or the
associated DQO Summary Form, corrective action will be required.
If States, other Federal Agencies, PRPs or Federal Facilities fail to schedule or track non-
CLP samples correctly, corrective action should be initiated by that organization
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9 2 The Regional/Laboratory Communication Network
9.2.1 Objective
9.2.1.1 CLP
In January 1983, the CLP National Program Office established a system of direct
communication between the regions and CLP laboratories as a routine method for regional
data validation staff to obtain answers to technical questions concerning program data in the
timeliest and most direct manner possible.
9.2.1.2 Non-CLP
EPA Field Sampling Contractors, States and other Federal Agencies performing Fund-lead
work andior PRP/Federal Facility oversight should establish a direct communication system
with their contractor and/or subcontractor laboratories (as appropriate based upon privity of
contract) to ensure timely resolution of technical issues
For non Fund-lead sites, PRPs and Federal Facilities should also establish a direct
communication system with their contractor and/or subcontractor laboratories (as appropriate
based upon privity of contract) to ensure timely resolution of technical issues
9.2.2 Requirements
The requirements for the CLP system are as follows:
a. Regional contact with CLP laboratories is permissible only after laboratory data
submission.
b Que :tions involving data delivery, contractual requirements, procedural
recommendations, and other general CLP matters are to be referred to the RSCC, the
NPO Sample Scheduling and Coordination Contract (currently named CLASS), or
to program management (i.e., EPA-NE CLP-TPO) as appropriate.
c. Reanalysis requests originating from the data validator must be channeled by the EPA
Field Sampling Contractor Lead Chemist through the EPA-NE CLP-TPO or EPA
DV Chemist.
d Only authorized personnel that are designated Regional CLP representatives may
contact CLP laboratories, and they may contact only specified laboratory personnel
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To become a designated Regional CLP representative or alternate, the candidate’s name and
resume must be submitted to the CLP-TPO for review. Upon approval of the candidate, the
CLP-TPO will notify CLASS for inclusion on the Region I CLP representatives list.
Similar requirements should exist for a non-CLP communication System.
9 2.3 Procedure
923.1 CLP
a. The entire data package should be assessed to determine if any of the four Action
items listed below in Section 9 2 4 are a problem within the laboratory data package.
b A list of required data resubmissions and analytical clarifications should be faxed to
the laboratory prior to initiating the call.
c. The designated Regional CLP representative should call the laboratory, discuss each
item on the faxed list, and establish a due date for resubmissions The time frame
for resubmission should be limited to seven days.
d All conversations between the regional representatives and the CLP laboratories
should be recorded by both the laboratories and the regional representatives on the
Telephone Log or Regional/Laboratory Communication Form (Attachment J, Form
iii).
e. The original Telephone Log/Communication Form is included in the Data Validation
Report or Tier I Validation Cover Letter sent to the EPA Site Manager. One copy
of the Telephone Log/Communication Form is forwarded by the EPA Field Sampling
Contractor to each of the following.
• EPA NPO Sample Scheduling and Coordination Contract (currently named
CLASS)
• The EPA-NE CLP-TPO (their copy to be included in the Data Validation
Report or Tier I Validation Cover Letter)
• The CLP laboratory
• EPA-NE RSCC
f Resubmitted data should be marked as “additional data’ by the CLP laboratory All
resubmitted and/or omitted data should be submitted to the Region accompamed by
a revised DC-2 form.
g If data resubmissions or verbal clarifications are not received within the specified
umeframe, then the Regional CLP representative should contact the laboratory every
day for 7 days.
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h. If (he information is still no received within the additional 7 days, then the Regional
CLP representative should contact the CLP-TPO for follow-up action.
9 2 3 2 Non-CLP
a. For Fund-lead sites and PRP/Federal Facility oversight, all conversations between
EPA personnel, EPA contractors, States, or other Federal Agencies with non-CLP
laboratories should be recorded by both the non-CLP laboratories and the EPA/EPA
Contractor/State/Other Federal Agency contacts.
b. For non Fund-lead sites, all conversations between PRPs, other Federal Agencies,
or their contractors, with non-CLP laboratories should be recorded by both the non-
CL? laboratories and the PRP/Other Federal Agency/Contractor Contacts.
c Copies of the Telephone Log or Regional/Laboratory Communication Form should
be:
• Included in the Data Validation Report or Tier I Validation Cover Letter
• Sent to the laboratory
• Retained in the site file
9.2.4 Action
The four types of problems that require direct contact between the designated Regional
representatives and the laboratory for resolution of laboratory data package problems are
illustrated in Figures 2 and 3 and are described below:
a In the case of missing or illegible deliverables, the validator should contact the
laboratory through their designated Regional CLP representative to establish and
record the expected due date for the requested deliverables
b. i When a CLP contract required reanalysis, is missing, the validator should
check the CCS report, if available, to see if the problem was noted. If so,
the designated Regional CLP representative should contact the laborawry to
ascertain the expected due daw. If the problem was not noted by CCS, the
validator and/or Lead Chemist, in conjunction with the EPA Site Manager,
must decide whether initiation of a reanalysis request would provide usable
data (weighing a consideration of holding times, etc ). To initiate a CLP
reanalysis request, the validator or Lead Chemist must first contact the CLP-
TPO or EPA DV Chemist. If the TPO deems reanalysis appropriate, a
reanalysis request form will be forwarded by the TPO to the CLP-APO for
that laboratory
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ii When a non-CLP contract required reanalysis for Fund-lead and PRP/Federal
Facility Oversight work is missing, the EPA Field Sampling Contractors,
States and other Federal Agencies should contact their contractor and/or
subcontractor laboratory (as appropriate based upon privity of contract) to
ascertain the expected due date and ensure timely delivery of reanalysis
results.
iii When a non-CLP contract required reanalysis for non Fund-lead work is
missing, the PRP, other Federal Agency, or their contractors should contact
their contractor and/or subcontractor laboratory (as appropriate based upon
privity of contract) to ascertain the expected due date and ensure timely
delivery of reanalysis results.
c. Clarification of discrepancies or errors in the reported data usually requires
correction and resubmission of results by the laboratory. If the laboratory does not
agree with the error, then the validator should double check hisIher work to ensure
the accurate reporting and qualification of data If the laboratory is still found to be
in error but will not agree with the error, then the validator should use professional
judgment to qualify the data.
d In some cases, it may be necessary to have the laboratory provide certain
explanations or detail conditions of analysis that do not correspond to any of the
contract or method-required deliverables. In such cases, a verbal answer,
documented in a Telephone Log/Communication Form by the designated Regional
representative, is all that is contractually-required of the laboratory.
9 3 The CLP-TPO Communication Network
Similar to the communication networks described above, CLP-TPO communications involve contact
with CLP Administrative Project Officers, CLP Contract Officers, CLP laboratories, the NPO
contractors (CLASS and QATS) and the EPA Field Sampling Contractors’ Lead Chemists The CLP-
TPO receives numerous QA reports from the NPO. Those which relate directly and specifically to
CLP data validation will be forwarded to contractors responsible for data validation as appropriate.
Inter-regional questions or problems with CLP laboratory performance are referred to TPOs for
resolution For example, if a Region I data validator uncovers a possible contamination problem in
a CLP laboratory assigned to Region II, the problem is first referred to the Region I CLP-TPO who
then contacts the CLP-TPO in Region 11 to resolve the problem.
It is recommended that the CLP-TPO be notified of all problems and requirements for a particular
case at one time. If there is an urgent requirement, the CLP-TPO may be contacted by phone to
expedite corrective action A copy of the Data Validation Report with the ORDA/IRDA Form as a
cover page must be submitted to the CLP-TPO to provide documentation of the data validation and
to facilitate resolution of inter-regional CLP laboratory performance problems
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10.0 THE TIER I VALIDATION COVER LETFER
10 1 Objective
The Tier I Validation Cover Letter documents that the data associated with a specific sample delivery
group (SDG) were validated in accordance with the Region I Ter I Validation Guidance and justifies
the use of a Tier I validation. The letter also documents the evaluation of PE sample results that
were analyzed with the field samples, thereby providing a limited assessment of laboratory
performance. Attachment M contains an example of a Tier I Validation Cover Letter.
10.2 Components of the Tier I Validation Cover Letter
10.2.1 Cover Letter
Tier I Validation Cover Letters that are generated for CLP Fund-lead and CLP PRP/Federal
Facility oversight work, as well as EPA-generated non-CLP work, should be addressed and
sent to the following:
• Christine Clark
Regional Sample Control Center
U.S. Environmental Protection Agency
60 Westview Street
Lexington, MA 02173
cc: EPA Site Manager
• The subject heading of the Tier I Validation Cover Letter must include: the
contractor work assignment number, the case number and SDG number (in that
order), the laboratory name, the site name, the parameters evaluated, the total
number of samples per sample matrix per parameter, (parenthetically identify the
field duplicates), the sample matrix and field sample numbers analyzed for each
parameter, the parameter, matrix and sample number for each type of blank, and the
parameter, matrix, and sample number for each PE Sample. Note: Each sample
number must be listed individually. (Refer to Attachment N for example of Data
Validation Reports for exact Memorandum format to be used.)
• Only one SDG may be discussed in each Tier I Validation Cover Letter.
• Justification for Tier I validation. The validation Tier is based on project DQOs and
is determined by the end users at the time of project scoping.
• Evaluation of PE sample results and potential impact on data
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10 2 2 Attachments
10 2.2.1 Data Summary Tables - Unvalidated Data (CADRE-generated spreadsheets)
Data Summary Tables clearly marked NOT VALIDATED DATA’ should be included as
an attachment for all Low/Medium CLP Organic and Inorganic data that have undergone
CADRE review
NOTE: Data Summary Tables are not required for data that have not undergone
CADRE review.
10.2.2.2 Accuracy Check Worksheet- Data Validation Worksheet XI and PES Score
Report/Vendor PES QC Acceptance Limits
All SDGs are required to have a paraineter/matrixlconcentrauon level associated PE sample,
if one is available. The PE sample results should be evaluated based on Section XI in the
appropriate VOA/SV, PEST/PCB or Inorganic Functional Guidelines (Parts II, III and IV of
this document).
10 2.2.3 Support Documentation
10 2 2.3.1 Analytical Method for Non-CLP Methods
Copies of non-CLP methods and modifications to standard methods should be included in the
Tier I Validation Cover Letter as support documentation and identified as such.
10 2.2 3.2 Copies of Telephone Logs/Communication Forms for the following must be
included in the Tier I Validation Cover Letter:
• All communications with RSCC to track data packages and to resolve sample
scheduling, tracking, and shipment questions
• All Regional/Laboratory communications to laboratories requesting resubmittal and/or
clarification of data
• All communications with samplers to clarify sample numbers, locations, descriptions
or preservation techniques and/or to alert them to significant field contamination
• All communications with the CLP-TPO/EPA DV Chemist to report contractually-
deficient CLP data that will be recommended for data rejection or reduced payment
• All communications with the EPA Site Manager concerning possible data rejection
• All communications with the EPA Site Manager to authorize change in required data
validation tier
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10.2.2 3.3 Copies of Data Supporting Recommendations for Reduced Payment
All non-compliant data that are of limited use to the end user are deemed to be of reduced
worth by the region and should be recommended for reduced payment.
All non-compliances identified during a Tier I Validation that adversely affect data usability
should be documented by attaching tabulated laboratory forms, raw data, or validaor-
prepared tabulations to substantiate the findings and conclusions presented in the Tier I
Validation Cover Letter. For CLP data, support documentation attachments should be
numbered andlor labelled and referenced accordingly in the text of the Tier I Validation
Cover Letter. Similarly, support documentation for unusable non-CLP data should be
attached to the Tier I Validation Cover Letter and recommendation for reduced payment
noted. In addition, the validator should circle the specific items of concern located on these
attachments.
10.2.2.3.4 Original Data Supporting Recommendations for Data RejectioniZero Payment
All non-compliant original data that are unusable by the end user are deemed contractually
unacceptable to the region, and, therefore, the laboratory should not be paid. Original CLP
data should be attached to the Tier I Validation Cover Letter and sent to the CLP-TPO/EPA
DV Chemist with a cover letter recommending data rejection. Similarly, unusable non-CLP
data should be attached to the Tier I Validation Cover Letter and returned to the laboratory
for non-payment.
10.2.2.3.5 Copies of Field Sampling Notes andlor Field Report
The field sampling notes and/or field report should be provided by the field sampler to the
Lead Chemist or data validator to be included in the Tier I Validation Cover Letter as an
attachment. In situations where sampling events extend over a period of weeks producing
two or more SDGs and generate numerous pages of field log book notes, the field notes
should be copied only once, included in one Data Validation Report and that Data Validation
Report should be referenced by Case, SDG, and date of memorandum. The field sampling
notes are included to provide complete documentation of the sampling event to substantiate
site decisions made using the data and to support potential future litigation.
10 2.2 3 6 Copies of EPA-approved Amendments to QAPjP and/or SAP
Any EPA-approved amendments to the QAPJP and/or SAP that describe modified criteria
used to validate site data should be included in the Tier I Validation Cover Letter as an
attachment
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1022.4 CSF Audit
Refer to Attachment C, Region I CSF Completeness Evidence Audit Program , July 3, 1991
or most recent revision.
10 2 2.5 DQO Summary Form
Copies of DQO Summary Forms previously submitted by the EPA Field Sampling
Contractors, States and other Federal Agencies to the RSCC along with the quarterly CLP
sample slot projections must be included with the Tier I Validation Cover Letter.
Copies of DQO Summary Forms for non-CLP sampling events previously submitted by the
EPA Field Sampling Contractors to the RSCC prior to the sampling event, must be included
with the Tier I Validation Cover Letter. Copies of DQO Summary Forms for non-CLP
sampling events previously submitted by States and other Federal Agencies to the
“Authorizing Organization” prior to the sampling event, should be included with site
documents.
For proper distribution of the DQO Summary Forms refer to the DQO Surnniary Form
Instructions (Attachment J, i)
The Draft DQO Summary Form (refer to Attachment J, i) should be used until such time as
a Final version has been issued
10 3 Initiating the Tier I Validation Procedure
a Upon receipt of a data package, the data validator should ascertain the required data
validation tier from the DQO Summary Form and/or EPA-approved QAPjP and/or SAP If
a Tier I validation is required, then the validator should determine if EPA or commercial PE
samples were analyzed with the SDG If an EPA PE sample was analyzed, then the PE Form
I results should be faxed to the EPA PE Chemist for scoring. If PE samples were obtained
from a commercial vendor, then the vendor’s PES QC acceptance limits should be utilized
to evaluate PES results. If EPA or commercial PE samples were not included in the SDG,
then the validator should note this and the reason why in the Tier I Validation Cover Letter.
b The data validator should begin the Completeness Evidence Audit in accordance with the
Re2ion I CSF Completeness Evidence Audit Program , July 3, 1991 or most recent revision.
c Once the PES Score Report is received, the data validator should evaluate the PE sample
results in accordance with Section XI of Part II, III or IV of this document and complete the
Section XI-Accuracy Check Worksheet.
d The data validator should finalize the Completeness Evidence Audit.
e If PE sample results indicate acceptable laboratory performance, then the validator should
note this in the Tier I Validation Cover Letter
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f If PE results indicate poor laboratory performance, then the data validator should note the
specific laboratory performance problems and their impact on data quality. For example,
‘TCL MISSES” would indicate the possibility of false negatives, “TCL
CONTAMINANTS” would indicate the possibility of false positives, and “ACTION LOW’
and “ACTION HIGH” scores would indicate the possibility of negative and positive biases,
respectively.
g. If PE results indicate poor laboratory performance, then the data validator should contact the
EPA Site Manager to ascertain if a Tier II or Tier III validation is warranted. This call
should be documented in a Telephone Log. Only the EPA Site Manager can approve an
- upgrade in validation tier.
h. The data validator should assemble the Tier I Validation Cover Letter with the all the
required attachments as noted in Section 10.2.
11.0 THE DATA VALIDATION REPORT (Tiers II and III)
lii Objective
Data Validation Reports, generated for Tier II and Tier Ill validations, document that the data
associated with a specific sample delivery group (SDG) were validated in accordance with the Region
I Tier II and Tier III Validation Guidance, respectively The Data Validation Report documents and
discusses the rationale for any modifications to or deviations from the Region I Data Validation
Guidance specified in this guidance document
The findings of a Tier IL and III validation are distributed to users for three distinct applications (1)
to make site decisions, (2) to provide oversight of CLP and non-CLP laboratory and method
performance for contract management and payment recommendations, and (3) to provide EPA data
validation oversight of the EPA Field Sampling Contractors.
For individuals involved in site-related decisions, it is imperative that the Data Validation Report
present a clear explanation of those issues affecting the use of those data The Report must provide
the end users with an overview of analytical data quality and should also explain the qualitative
confidence and quantitative “measurement error” associated with all sample results. In addition, the
end users need Data Summary Tables that present all positive sample results, detectionlquantitation
limits, and associated qualifier codes.
On the other hand, the EPA individuals responsible for management and oversight of CLP and non-
CLP laboratory performance and method performance require a presentation of issues related to
laboratory non-compliance, poor laboratory practices that are not regulated in the contract, and any
unusual method or analytical problems For both contractual issues and problems affecting the
usability of the data in making site decisions, support documentation must be sufficient to allow EPA
to perform a full-scale review of the data validation in order to substantiate the Report’s conclusions
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Data Validanon Reports written by EPA Field Sampling Contractors are reviewed by the EPA-NE
Quality Assurance Unit in accordance with the EPA-NE Data Validation Oversight/Methods Review
Program. Data Validation Oversight Reports are provided to the EPA Site Managers and contract
Project Officers The contract Project Officer forwards the Data Validation Oversight Report to the
EPA Field Sampling Contractor and requests corrective action. The continued effectiveness of the
required corrective actions are monitored in subsequent validation oversights. Overall contractor data
validation performance is monitored for each contract performance period.
11.2 Components of the Data Validation Report
In order to meet the varied needs of many end users, a six part DATA VALIDATION REPORT
is generated. The report contains the following components in the order presented in this section.
Each component should be completed in accordance with the following guidance. Attachment N
includes two examples of Tier III Organic Data Validation Reports; a CLP Low/Medium organic soils
SDG and a DAS low concentration surface waters SDG. Attachment J includes a copy of the
following blank forms. DQO Summary Form, ORDA/IRDA Form, Telephone Log and
Regional/Laboratory Communication Form, Data Validation Worksheets, Chain-of-Custody Form,
and Traffic Report.
11.2.1 Organic/Inorganic Regional Data Assessment (ORDA/IRDA) Form
The ORDA/IRDA Form delineates issues relating to a laboratory’s contractual non-
compliance. The Form contains a checklist of items verified during validation. An
ORDA/IRDA Form should be completed for all Tier II and III validations for CLP data
validated by EPA Field Sampling Contractors, States, and other Federal Agencies for Fund-
lead and PRP/Federal Facility oversight work. An ORDA/IRDA Form should also be
completed for Tier II and III validations for non-CLP data performed by EPA Field Sampling
Contractors for Fund-lead and PRP/Federal Facility oversight work.
For CLP data, “TPO/PO Action” should only be checked when contractual defects have
resulted in reduced payment/data rejection recommendation letters to the TPO. All ‘TPO/PO
Action” items should be detailed and documented in the “Action Items” line. Documentation
supporting the “TPO/PO Action’ items should be included in the Data Validation Report
For EPA-generated non-CLP data, “TPO/PO Action” should only be checked when
contractual defects have resulted in reduced payment/data rejection actions taken by the EPA
Field Sampling Contractor. All “TPOIPO Action’ items should be detailed and documented
in the ‘Action Items” line Supporting documentation should be included in the Data
Validation Report. States, PRPs and other Federal Agencies are not required to submit
ORDA/ERDA Forms for non-CLP data, but are encouraged to monitor the contractual
performance of their contractor laboratories.
For both CL? and EPA-generated non-CL? data, refer to the back of the ORDA/IRDA Form
for instructions on completing the form
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11.2.2 Data Validation Memorandum (DVM)
11.2.2.1 Narrative
This should briefly identify the scope of the analytical effort, provide a general overview of
analytical quality, describe in detail and interpret all specific problem areas that were
identified in the worksheets . Specific problems that impact the potential usability of the data
should be emphasized. Data Validation Memoranda should be addressed and sent to the
following:
• Christine Clark
Regional Sample Control Center
U.S. Environmental Protection Agency
60 Westview Street
Lexington, MA 02173
cc: EPA Site Manager
(Refer to Section 13.0 for proper distribution of Fund-lead, PRP/Federal
Facility Oversight and EPA-generated non-CLP Data Validation Report
copies. Data Validation Reports generated by PRPs, States or other Federal
Agencies for non Fund-lead sites should be distributed in accordance with
those organizations’ requirements.)
• The subject heading of the DVM must include: the contractor work
assignment number, the case number and SDG number (in that order), the
laboratory name, the site name, the parameters evaluated, the total number
of samples per sample matrix per parameter, (parenthetically identify the
field duplicates), the sample matrix and field sample numbers analyzed for
each parameter, the parameter, matrix and sample number for each type of
blank, and the parameter, matrix, and sample number for each PE Sample
Note: Each sample number must be listed individually. (Refer to Attachment
N for example of Data Validation Reports for exact Memorandum format to
be used.)
• Only one SDG may be discussed in each Data Validation Report
• The first sentence of the first paragraph should state the validation tier used
to validate the sample data. If different tiers were used to validate different
subsets of the SDG, then this should be noted and the associated subsets and
tiers identified
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• The first paragraph must also state that the Region I. EPA-NE Data
Validation Functional Guidelines for Evaluating Environmental Analyses ,
July 1996 or most recent revision, was used to validate the data in
accordance with the EPA-approved SAP and/or QAPjP. If validation criteria
were modified to accommodate different QC criteria for non-CLP methods,
then the modified criteria should be described in the first paragraph. If the
EPA-approved SAP and/or QAPjP does not specify modified data validation
criteria and the validator determines that modified criteria are necessary to
properly evaluate the site data, then an amendment to the QAPjP arid/or SAP
describing the modified criteria must be submitted to EPA for approval prior
to data validation. A copy of the amendment must be included in the support
documentation for the Data Validation Report.
• The first paragraph must also identify the analytical methods used to analyze
site samples.
• The second paragraph must list the QC parameters (checks) that were
evaluated during validation. QC parameters that met criteria should be
asterisked (*) in the left hand margin of the parameter name. Similarly, QC
parameters that were not applicable to the analytical methods should be
indicated by an ‘N/A’ in the left hand margin of the parameter name. Note
that worksheets should not be included for QC parameters that met criteria
(except for Worksheet XH/XIll, Sample Quantitation) or were not applicable
to the analytical method. (Refer to Attachment N for examples of a Tier
11/Ill Data Validation Reports for exact memorandum format to be used
• ‘Potential Usability Issues” is the first parameter discussed in the DVM
The validator should discuss the potential impact of “measurement error’ on
data usability in terms of the project’s Data Quality Objectives. The
validator should cite the usable aspects of the data and should identify
problems as having either a major or minor impact on data usability
• The DVM should identify for each QC parameter that did not meet criteria
the affected samples, the analytical problem, and the recommended actions
• Information should be presented in tabular format whenever possible, (see
example DVMs in Attachment N) Narratives should be limited to
discussions of complex analytical problems and justifications of actions taken
based on professional judgment The information should be conveyed in
simple, concise language that an individual without an extensive background
in analytical chemistry can understand
• The DVM must clearly differentiate problems affecting the confidence
concerning the presence/absence of a compound versus those involving
quantitative error.
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• The DVM should also differentiate between sampling issues (sampling error)
and analytical issues (analytical error).
• The narrative should list or reference all changes that the validator has made
to the laboratory’s reported data, whether due to misidentiticadon, errors in
transcription or calculation.
• The last QC parameter discussed in the DVM is System Performance. This
should include an overview of interrelated and/or multiplicative analytical
problems that impact usability of the data.
• The narrative should list support documentation attachments and should
include the validator’s name and signature
11.2.2.2 Data Summary
11.2.2.2.1 Qualifier Recommendation Summary Table-Table!
The purpose of Table I is to identify all qualifier codes applied to each sample per parameter,
taking into account the multiplicative effects of various qualLfiers The vaJidator should
assess tendencies in bias.
11.2.2.2.2 Overall Evaluation of Data (Data Validation Worksheet)-Table II
The purpose of Table Ills to identify and summarize the “analytical error” associated with
the data as well the “sampling error” that was identified through validation. It also identifies
potential usability issues associated with the data for the end user.
Since sampling variability must be assessed by the end user, that column remains blank
on Table II throughout data validation.
11 2.2 2 3 Tentatively Identified Compound (TIC) Summary-Table III
Table III includes a list of TICs TICs reported by the laboratory as “UNKNOWNS” without
a compound class should not be included in the table
11 2 2.2.4 Data Summary Tables-Spreadsheet
The purpose of the Data Summary Table is to provide a simple, condensed form of the
analytical results (excluding FE sample results) for the end user, which enables a quick
evaluation and comparison of the constituents identified at the various sampling locations
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Separate tables in “Lotus 1 2 3” are required for soil and water analyses and for organics and
inorganics analyses. Additionally, separate tables are also required for volatile, semivolatile,
and pesticide/PCB analytes for the organic analyses. Other database software may be used
to generated Data Summary Tables as long as there is no deviation from the format and
content requirements exhibited in Attachment N.
The Data Summary Tables must include: case number, CLP SDG number, site name, site
location, matrix, parameter, concentration units, method-required detection/quantitation limits
(CRDLs/CRQLs), EPA Sample (Traffic Report) numbers, sample locations/descriptions,
laboratory sample numbers, all positive sample results, sample-specific and associated
qualifier codes, dilution factors, % solids for soils, dates sampled, dates extracted, and dates
analyzed. Examples of the Data Summary Tables are provided in Attachment N.
Only codes defined by this document are permitted to qualify data Should it be necessary
to include other codes, prior approval must be obtained from the EPA-NE CLP-TPO. if
approval is given, complete definitions must be supplied in the key for the Data Summary
Table. The standard data validation codes used in qualifying data in accordance with this
guidance are:
U - The analyte was analyzed for, but was not detected. The associated numerical value is
the sample quantitation limit. The sample quantitation limit accounts for sample specific
dilution factors and percent solids corrections or sample sizes that deviate from those required
by the method.
J - The associated numerical value is an estimated quantity.
R - The data are unusable (analyte may or may not be present). Resampling and reanalysis
is necessary for verification. The R replaces the numerical value or sample quantitation limit
UJ - The analyte was analyzed for, but was not detected. The sample quantitation limit is
an estimated quantity
EB, TB, BB - An analyte that was identified in an aqueous equipment blank, trip blank, or
bottle blank that was used to assess field contamination associated with soil/sediment samples
These qualifiers are to be applied to soil/sediment sample results only. (For additional
guidance refer to Blank Section V of Parts II, Il or IV)
11.2.3 Standard Data Validation Worksheets
The data validation worksheets included in this document must be utilized to perform the data
validauon. Any modification to the worksheets must be documented in the QAPjP and/or
SAP and be approved by EPA prior to sampling
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Worksheets should not be included for QC parameters that meet criteria or criteria that are
not applicable to the analytical method, except for Worksheet XII/XIII-Sample Quantitation.
However, the data validator must complete page two of the Data Validation Worksheet Cover
Page, and then sign and date the worksheet.
Copies of automated data review reports, i.e., CADRE, should be included in this section.
Any automated data review reports, such as CADRE should be incorporated into the Data
Validation Report according to the Guidance Document for Completing Region I Data
Validation Utilizing CADRE Data Review , February 1995 or most recent revision
A completed Data Validation Worksheet Cover Page must precede the other worksheets.
11.2.4 Support Documentation
11.2.4.1 Analytical Method for Non-CLP Methods
Copies of non-CLP methods and modifications to standard methods should be included in the
Data Validation Report as support documentation and identified as such.
11 2.4.2 Copies of Telephone Logs/Communication Forms for the following must be
included in the Data Validation Report:
• All CLP “Records of Communications” with the RSCC to track data packages and
to resolve sample scheduling, tracking, and shipment questions
• All Regional/Laboratory communications with laboratories requesting resubmtttal
andior clarification of data
• All communications with samplers to clarify sample numbers, locations, descriptions
or preservation techniques and/or to alert them to significant field contamination
• All communications with the CLP-TPO/EPA DV Chemist to report contractually-
deficient CLP data that will be recommended for data rejection or reduced payment
• All communications with the EPA Site Manager concerning possible data rejection
• All communications with the EPA Site Manager to authorize change in required data
validation tier.
11 2 4 3 Copies of Data Supporting Recommendations for Reduced Payment
All non-compliant data that are of limited use to the end user are deemed to be of reduced
worth by the region and should be recommended for reduced payment.
All non-compliances, identified in the Data Validation Memorandum and/or on the
ORDA/IRDA Form, that adversely affect data usability should be documented by attaching
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tabulated laboratory forms, raw data, or validator-prepared tabulations to substantiate the
findings and conclusions presented in the text. Support documentation attachments should
be numbered and/or labelled and referenced accordingly in the text of the DVM r4arracive
and on the ORDA/IRDA Form. in addition, the validator should circle the specific items of
concern located on these attachments
11 2 4.4 Original Data Supporting Recommendations for Data RejeciionlZero Payment
All non-compliant original data that are unusable by the end user are deemed contractually
unacceptable and of no value to the region, and, therefore, the laboratory should not be paid
Original CLP data should be attached to the Data Validation Report and sent to the CLP-
TPO/EPA DV Chemist with a cover letter recommending data rejection. Similarly, unusable,
non-compliant non-CLP data should be attached to the Data Validation Report and returned
to the laboratory for non-payment.
11.2.4.5 Copies of Field Sampling Notes and/or Field Report
The field sampling notes and/or field report should be provided by the field sampler to the
Lead Chemist or data validator to be incorporated in the Data Validation Report as an
attachment. In situations where sampling events extend over a period of weeks producing
two or more SDGs and generate numerous pages of field log book notes, the field notes
should be copied only once, included in one Data Validation Report and that Data Validation
Report should be referenced by Case, SDG, and date of Data Validation Report. The field
sampling notes are included to provide complete documentation of the sampling event to
substantiate site decisions made using the data and to support potential future litigation
11 2 4 6 Copies of EPA-approved Amendments to QAPjP and/or SAP
Any EPA-approved amendments to the QAPjP and/or SAP that describe modified criteria
used to validate site data should be included in the Data Validation Report as support
documentation.
11 2 5 CSF Completeness Evidence Audit
Refer to Section 10 2 2.4
11 2.6 DQO Summary Form
Refer to Section 10 2.2 5
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11.3 Initiating the Tier II and Tier Ill Data Validation Process
Once the various sources of information, as discussed in Section 8, are assembled, the data validator
should begin the Tier II or Tier III validation in accordance with steps a., b., and c. outlined in
Section 10.3 Next, the validator should review the Data Package Narrative and generate Data
Summary Tables in spreadsheet format (i.e., Lotus or other database software) according to the
following guidance.
11 3.1 Reviewing the CLP Data Package Narrative/Cover Page
Review of the Data Package Narrative n conjunction with the chain-of-custody forms, Traffic
Reports and Log In sheets (CLP Organic SDG Narrative or CLP Inorganic Cover Page)
should quickly familiarize the data validator with all QC, sample, shipment and/or analytical
problems.
The CLP Data Package (SDG) Narrative/Cover Page must:
• Justify the use of flagged edits on organic CLP quanutation lists.
• Document all instances of manual integration in organic CLP cases.
• Differentiate between initial analyses and reanalyses for CLP and state if reanalysis
is billable and why.
• List all pH determinations for VOAs
• Document SOW number or method name and version date
• Be signed by the Laboratory Manager authorizing the release of the data, and
verifying the contents of the data and deliverables.
Note: Non-CLP laboratory data packages should provide similar sample analysis information
in a narrative or cover page format..
Review the Data Package Narrative/Cover Page to determine if gross analytical and/or
shipment problems occurred.
If holding times were exceeded and resulted in qualified data, the data validator should assess
the reduced worth of the daa. For CLP data packages, the validator should submit a reduced
payment recommendation to the TPO in accordance with Attachment 0, March 7, 1995
Memorandum to Heidi Horahan, ARCS DPO re CLP-SOW OLMO3 I-New Contract
Requirements. If holding times were grossly violated, then data rejection may be warrantei
The data rejection procedures specified in Attachment I should be followed If VOA sample
pH measurements indicate that samples were not acid preserved in the field, then the
validator should contact the sampler to confirm that incorrect preservation techniques were
used and document the finding as “sampling error’ in the Data Validation Memorandum.
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If other analytical and/or sampling related problems, i.e., shipment, were noted in the Data
Package Narrative, then the validacor should describe in the DVM those problems that impact
the poenual usability of the data.
113 2 Generating Data Summary Tables
Transcribe the results from the Form Is onto the Data Summary Tables. For organic
analyses, do not transcribe the qualification codes used by the laboratory except for all “U”s
for non-detects as well as “J”s for positive detects reported below the sample-specific CRQL
For inorganic analyses, do not transcribe the qualification codes used by the laboratory except
for all “U”s for non-detects. For all inorganic positive detects that are less than or equal to
2x analyte IDLs, qualify sample results with a “J” code.
As appropriate, information will be added to or deleted from the Data Summary Tables
during the course of data validation. PES and method blank results should not be reported
on the Data Summary Tables.
Note that for CADRE validations, the Data Summary Tables are automatically generated
CADRE Data Summary Tables are provided to the EPA data validator for both validated and
unvalidateci data. For Tier I validations, Data Summary Tables with ‘NOT VALIDATED
DATA’ are included as an attachment to the Tier I Validation Cover Letter. For Tiers II and
Ill, the validator must complete the validation in accordance with the Guidance Document for
Completing Region I Data Validation Utilizing CADRE Data Review , February 1995 or
latest revision.
1133 Usage of Qualifier Codes on the Data Summary Tables
The data qualifier codes, presented in Section 11 2.2.2.4, identify the degree of confidence
concerning the presence or absence of reported compounds and identify results that are
considered to be quantitatively inaccurate. These codes have been regionally standardized
to ensure that data validators throughout the region employ the same set of simple, concise
definitions that are understandable to personnel within the various EPA offices. Therefore,
a. Only codes defined in Section 11.2.2 2.4 may be used to qualify or reject data.
Should it be necessary to include other codes, prior approval must be obtained from
the EPA-NE CLP-TPO
b. In general, only one qualifier code is used with each reported result. The following
hierarchy has been developed to ensure that only the most important code is used in
situations where more than one quality control problem is associated with an
analytical result:
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• Codes relating to identification take precedence over codes related to
quantitation. If results are rejected, replace the numerical sample result
or sample quantitation limit with an “R”. Thus, whenever a positive result
is rejected “R”, the “i’ code will not be used Also, whenever a non-
detected result is rejected “R’, the “U” or “UJ ” code will not be used
• Within each of the two categories of codes, the code that indicates a more
serious problem with the data takes precedence. In all cases, the R code
supersedes the J or EB, TB, BB codes.
• The J and the EB, TB, BB codes may be used together for soil/sediment
samples.
c. The above restriction on the general use of multiple qualifiers for a single result is
applicable only to the Data Summary Table and not to the narrative portion of the
Data Validation Memorandum. The narrative should mention all problems, major
and minor, associated with the individual sample results.
d. Parts II, III and IV of this document address the individual situations requiring the
use of particular qualifier codes. Upon completion of the data validation, the
validator should double check the Data Summary Tables for accuracy and
completeness to ensure that the appropriate qualifier codes were added according to
the requirements listed herein. The validator should also check that there are no
discrepancies between the worksheets, Data Validation Memorandum narrative, the
Qualifier Recommendation Summary Table, and the Data Summary Tables.
Once the data validation has been completed, the validaror compiles the Data Validation
Report and submits it for internal review within their organization.
12.0 INTERNAL REVIEW OF VALIDATION DOCUMENTS
12.1 Senior Validator Review
A Senior validator should review all Tier I Validation Cover Letters and Data Valida(ion
Reports to ensure the following
a All components of a Tier I Validation Cover Letter or Tier II or Tier 11.1 Data
Validation Report are included.
b Data validation has been performed in accordance with the Region I, EPA-NE Data
Validation Functional Guidelines for Evaluating Environmental Analyses and/or EPA-
approved modified or alternate validation criteria.
c The data package has been evaluated for analytical quality and contractual
compliance, and correct actions have been aken in the Data Validation Memorandum
to address specific analytical deficiencies
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PART I
d. Compound names and concentrations reported on Data Summary Tables are
consistent with Form I’s or other laboratory tabulated report forms. All
discrepancies should be justified in the Data Validation Memorandum.
e. Data qualifications identified in the worksheets are consistent with those in the Data
Validation Memorandum narrative, the Qualifier Recommendation Summary Table
and Data Summary Tables.
f. Non-compliant data that are unusable have been recommended for reduced
payment/data rejection when app! icable
g The project DQOs were used to determine if the degree of “measurement error’
associated with the data potentially compromises the data usability.
12 2 Lead Chemist Review
As a final step in this process, it is important that the Lead Chemist check all outgoing
reports for accuracy and completeness, due to the complexity of data validation and the
importance of performing an accurate final assessment of data quality. The Lead Chemist
must also review and concur with the final assessment of data quality and potential usability
issues raised by the junior and senior validators.
The Lead Chemist should ensure that all accepted data are contractually compliant and usable
The Lead Chemist must submit data rejection and reduced payment recommendation letters
whenever appropriate.
The Lead Chemist must ensure that the final Data Validation Report is correctly distributed
13.0 DISTRIBUTION OF DATA VALIDATION REPORTS AND TIER I VALIDATION
COVER LETTERS
The following distribution table is applicable to Data Validation Reports and Tier I Validation Cover
Letters generated by EPA Field Sampling Contractors for CLP and non-CLP Fund-lead and CLP
PRP/Federal Facility oversight work.
The CLP Data Validation Reports generated by States or other Federal Agencies performing Fund-
lead work under Cooperative and Interagency Agreements, respectively, should be sent to the EPA-
NE RSCC for purposes of contract administration. A copy of the CLP Data Validation Reports
and/or Final Project Reports should also be sent to the EPA Sie Manager.
Copies of non-CLP Data Validation Reports generated by States, other Federal Agencies, PRPs, or
Federal Facilities are not required to be forwarded to the EPA-NE RSCC. However, States, other
Federal Agencies, PRPs, or Federal Facilities should forward a copy of the non-CLP Data Validation
Report and/or the Final Project Report to the EPA Site Manager.
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PART I
Table of Deliverables
Document
REGIONAL RECIPIENTS
NATIONAL
RECIPIENTS
EPA-NE
Regions II-X
CLP-TPO/RSCC
(For Central Files)
EPA SITE
MANAGER
CLP-TPO
TIER IVALIDATJON
COVER LEVIER with
attachments
X
X
DATA VALIDATION
REPORT
ORDA/IRDA Form
DV Memo (including narrative,
Tables 1, II, III, and Data
Summary Tables)
Worksheets
Support Documentation
CSF Completeness Audit
DQO Summary Form
X
X
X
X
X
X
X
X
X
X
X
X
X ’ ’
X*
CSF - DATA PACKAGE
X
* CLP Data Validation Memoranda only (EPA-generated non-CLP Data Validation Memoranda
are not distributed nationally)
Note Telephone Logs/Communication Forms for the CLP Regional/Laboratory communication
program should be forwarded to the NPO Sample Scheduling and Coordination Contractor,
RSCC, CLP-TPO (their copy to be included in the Data Validation Report or the Tier
Cover Letter), and the CLP laboratory.
**All data packages/CSFs are ultimately archived in the EPA-NE Administrative Records Center
14.0 EPA DATA VALIDATION OVERSIGHT/METHODS REVIEW PROGRA M
The regional QA Unit of OEME reviews and comments upon contractor-prepared Data Validation
Reports and Tier I Validation Cover Letters. This oversight program serves a dual purpose. First,
the QA Unit evaluates the contractor’s ability to accurately perform data validation in accordance with
this regional policy. Secondly, the QA Unit assesses the use of current, new andlor modified
analytical methods in order to make needed method revisions based on scientific data. Resubmission
of Data Validation Reports may be required in cases where the required format and procedures were
not followed, or when clarifications or corrections are needed. The EPA Field Sampling Contractor
is responsible for implementing and monitoring the effectiveness of all corrective actions
recommended by EPA during oversight for validations performed by the prime contractor and any
subcontractors When critical deficiencies and/or problems have been identified during EPA
Oversight, the EPA Field Sampling Contractor may be required to prepare a separate Corrective
Action response letter to resolve those deficiencies and/or problems.
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FIGURE 1 - CLP DATA VALJDATION - ROLES & RESPONSIBILITiES
Con ac r Obb ins
EPA PE Samples From
CEME (Forrnezly ESO )
RSCC For
Sample Trackrng
L Final Pro ectV Crkplan
Con ac r Prepares
[ 3. Monl i Pro je on
Con actar Prepares
Quarterly Projections
I & DQO Summary Sheet
RSCC Schedules Slots
1 ekPnorTo
Sampling Event
NPOCont’acthr
Assgns Lab & Case
y
RSCC Provides Sample Info
To Lab Arid Con acter
Phone
Calls
I NPOConV ’actcr
[ rbill, TR#s, E
V
RSCC Directs CADRE
Data Packages To QA
Unit For CADRE Review
7
QA Unit Provides
CADRE Dab Packages
7
Ccnlract r’ Ships
Samplesto Lab
7
Lab Analyzes Samples
Lab Sends Data Package
To EPA RSCC
To EPA SItE Manager
( Usability Is Deteimined )
Oversight Audit __________
Report L
V
V
ToRSCC
To QA Unit
EPA Oversight
And Audit
Cone -act Project Officer L_.
[ (Contact Mar gement) 3
7 _____
Contactor Implements
[ Correctve Acton
RSCC Provides
Non-CADRE Data
Package and CCS
Ccrw’actsr Faxes EPA-PE [
Results to QA Unit
Sampler Provides
Field QA(QC. Sampling
Lo bon lrifcrmabon.
Sampling F:eid Notes,
and/or Tnp Report
Contractor* Provides
Project Site Information,
Approved QAPJP/SAP And
DQO Summary Form -Ala,
Coniacrs Lab For
Additional Information
Data Validation Report Prepared
ORDMRDA. DV Memo, Narrative,
Data Surrrrnary Tables, V\brksheets, Support
Documentation, CSF Audit And 000 Summary Form
Are Forwarded
L __i
A ‘ I
QA Unit Scores
EPA-PES Results
Ccnti’actor EPA Field Sampling Contisctor
NPO Contactor = NPO CLP Analyt l Services Suppcrt (CLASS)
-------
FIGURE 2- OVERVIEW OF THE DV PROCESS FOR CLP DATA
Cornractai Receives
Da Package
1
V.V PE5imcI.i
V .NotS.nIToI.
A NO Re , fl
c g.
F r eW Xn
R.cr.c Oua y- iVE,T r
R,... U,., b.a U
In Valicason
A
Corn ete VaIida n And
Comple DV Re ofl
ORDAIIRDA DV m lan .
&.rn y I UL
C A cA
M d 000 Fann
L St CV R,asl
V
V.,
-------
FiGURE 3- O iERVlEW OF T) - DV PROCESS FOR NON-CLP DATA GENERATED FOR EPA
nfortTIaaon
Yes
Com ete ValidaDon and
Comode OVRe rt
CRDNIPDA Dv H...n
O. TaO n I*8
t eçe1 0ooa,,,n ,e CDF , oat
Me 000 Swemarp Fcfm
Oisrt*fl DV Re i
Rua OeueOwcy. it En
Ren,w$ U,T,IeeIs •J.
Pi :at nes
In V3l atefl
I Yes _________________
- <,forma005
‘V
Contractor Receives
ta Package
F U CPA.PC SI ’u•
R.sU To oci
05 UntF S n
‘V
No tS onIToLi 5 d
Checlc Case Narrative
For Explanation &
Call Sampler To VecTfy
.àccuracy of Sample Log
Conhtactor Calls
- Documented In Phone Log -
Contractor Calls Lab
To Oetentnne Expected Delivery
Date - Call Is Docurrerited
No
V
1
VT
A
Recuest Resuteytesion
Note E’roected Delivery Dote
-------
FIGURE 4- DATA VALIDATION CRITERIA FLOW CHART FOR EPA SUPERFUND DATA
Were the EPA-NE
Functionat Gutdetines
referenced as data
validation ciitena?
I Document in lir t psiegraph
of Dv Memo thu QAPiPI’ Wee modified validation criteria
Wit not UP Pioved alternate data vatidation
2 Validate data according tO criteria e. USAIHAMA described
EPA-NE Functional Guidelines ( urapproved Q J P/SAP?
end document this in first
paragraph of Dv Memo ES
1 Document In the first paragraph of Weie the EPA NE Functional
the ON Merro that EPA-NE Guidelines modified to validate site I
Functional Guidelines validation I I
I data andlor re alternate data I
crIteria were used to validate data I
2 Document data validation Tier eve vat,dation cntena. I i USAII-4AMA, I
used to validate data L used to velldato site data?
1 Document lii I ci paragraph
of DV Memo that modified
EPA-NE criteria end/or alternati
data validation criteria were
used to validate the site data
2 Attach EPA-NE Functional
Guideline data validation
nodincations and/or alternate
data validation citerla
Were data validation criteria
documented in approved site
QAPjP/SAP or an approved
amendment to the QAPJPISAP2
Are data validation criteria
documented in unapproved
site QAPjP/SAP?
YES
Were the EPA-NE Functiona
Guidelines referenced as
data validation criteria?
I i no data vabdatton critelio
re documented In
an unapproved QAPIP/SAP
or if no site QAPJP/SAP
was written then contact
the EPA Site Manager
prior to validation
lithe validator is urrsije of the
applicability or appropriateness of ti-si
unapproved data validation criteria
then heishe should contact the EPA Site
Manager to resolve wry questions prior
to subnttlng a QAP 1 P/SAP errwodrrwrd
and prior to validating the data
Si nut QAFIP/SAP amendment
to the EPA Site Manager for approval of
modified or alternate data validation
criteria for validating site data
prior to vatidating the data
If tire vatidator is unsure of
lire appticabituly or appropriateness
of lire approved data validation
criterIa, then he/the should
contact the EPA Site Manager to
resolve any questions prior to
vatdaton
-------
PART I
References
I User’s Guide to the Contract Laboratory Program, EPA/540/P-91/002, January 1991.
2 EPA Requirements for Quality Assurance Project Plans for Environmental Data Operations,
EPA QA/R-5, August 1994, DRAFT INTERIM FINAL.
3. NEIC Policies and Procedures, EPA-330/9-78-OO1-R, May 1978, revised May 1986.
4. Data Quality Objectives Process for Superfund, EPAI54O/R-93/071, September 1993,
INTERIM FINAL.
5. Test Methods for Evaluating Solid Waste, Physical/Chemical Method (EPA Pub SW-846,
Third Edition) and updates.
6. USEPA Contract Laboratory Program Statement of Work for Inorganic Analysis, ILMO4 0,
EPAI54O/R-95/12 1.
7 USEPA Contract Laboratory Program Statement of Work for Organic Analysis, OLMO3. 1,
EPAI54O/R-941073.
8. Region I Tiered Organic and Inorganic Data Validation Guidelines, July 1, 1993, DRAFT
9 Region I CSF Completeness Evidence Audit Program, July 3, 1991.
10. Region! Laboratory Data Validation Functional Guidelines for Evaluating Organics Analyses,
2/01/88, modified 11/01/88.
11. Region I Laboratory Data Validation Functional Guidelines for Evaluating Inorganics
Analyses, 6/13/88, modified 2/89
12 Specifications and Guidance for Contaminant-Free Sample Containers - Publication 9240 0-
05A, EPA/540/R-93/05 1, December 1992.
13 Preparation of Soil Sampling Protocols Sampling Techniques and Strategies, EPA/600/R-
92/128. July 1992.
14 Guidance Document for Completing Region I Data Validation Utilizing CADRE Data
Review, February 1995.
15 USEPA Contract Laboratory Program National Functional Guidelines for Organic Data
Review, EPA/540/R-94/012. February 1994
DV MANUAL - 57 12/96
-------
PART I
16 US EPA Contract Laboratory Program National Functional Guidelines for Inorganic Data
Review, EPA/540/R-94/O [ 3, February 1994.
17 EPA Region I Performance Evaluation Program Guidance, July 1996 Revision.
18 Standard Operation Procedures for Submitting Data for Reduced Payment/Data Rejection,
September 9, 1991
19. Training Manual for Reviewing Laboratory Data Package Completeness, June 1994
DV MANUAL - 58 12/96
-------
Part I - Data Validation Manual: The Data Quality System
ATTACHMENTS
The following attachments are referenced in Part I of the Region I, EPA-NE Data Validation Functional
Guidelines for Evaluating Environmental Analyses . Guidance in some of the documents is superseded
by the more recent guidance provided in Part 1.
Attachment A “Quality Assurance for Superfund Environmental Data Collection Activities’ - Publication
9200.2-I6FS, February 1993, and “EPA Order 5360.1, Draft 1995 Quality Assurance
Order”.
Attachment B “Region I Tiered Organic and Inorganic Data Validation Guidelines’, July 1, 1993,
DRAFT
Attachment C “Region I CSF Completeness Evidence Audit Program”, July 1991.
Attachment D “Specifications and Guidance for Contaminant-Free Sample Containers” - Publication
9240.0-05 A, EPAJ54O/R-93/05 1, December 1992
Attachment E “User’s Guide to the Contract Laboratory Program”, EPA/540/P-91/002, January 1991.
Attachment F Region I Short Sheets and EPA CLP Information Sheets.
Attachment 0 ‘Training Manual for Reviewing Laboratory Data Package Completeness”, June 1994
Attachment H “EPA Region I Performance Evaluation Program Guidance”, July 1996, Revision
Attachment I “Standard Operating Procedures for Submitting Data for Reduced Payment/Data
Rejection”, September 9, 1991.
Attachment J Data Validation Report - Blank Forms
i. DQOSummaiy Form
ii. ORDA/IRDA Form
iii. Telephone Log or Regional/Laboratory Communication Form
iv. Data Validation Worksheets
v Chain-of-Custody Form
vi. Traffic Report
Attachment K Example of Contract Compliance Screening (CCS) Report
Attachment L “Guidance Document for Completing Region I Data Validation Utilizing CADRE Data
Review”, February 1995.
Attachment M Example Tier I Validation Cover Letter
Attachment N Example Tier III Data Validation Reports
Attachment 0 “March 7, 1995 Memorandum to Heidi Horahan, ARCS DPO re CLP-SOW OLMO3 1-
New Contract Requirements
Attachment P “The Regional Sample Control Center Guidance for the Contract Laboratory Program
(CLP) and Delivery of Analytical Services (DAS) Program for EPA-New England”,
Noventher 1996.
Attachment Q “Region I ARCS Delivery of Analytical Services Pilot Program, Final Report Volume
II. Appendices’, 15 March 1994
-------
Appendix A
CLP SOW OLMO3.2/Volatile Organic Analysis
Method QC criteria, Equations, and Definitions
-------
OLMO3.2/VOA
APPENDIX
The following method QC criteria, equations, and definitions apply o data generated according to the USEPA CLP
Statement of Work for Organic Analysis, Multi-Media, Multi-Concentration, OLMO3.2, Exhibit D Volatiles.
SECTION I: PRESERVATION & TECHNICAL HOLDENG TIME CRiTERIA
Refer to Region I, EPA NE Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
11, Section VOA/SV-I-B for preservation and technical holding time data validation criteria.
SECTION 11: GCIMS INSTRUMENT PERFORMANCE CHECK (TUNThIG) CRITERIA
Refer to the following method GC/MS instrument performance (tuning) QC criteria for data validation:
The analysis of the instrument performance (tuning) check solution (50 ng BFB on column) must be performed at
the beginning of each 12-hour period during which samples or standards are analyzed. The tuning check,
bromofluorobe ene (BFB), for volatile analysis must meet the ion abundance criteria given beIow
ION ABUNDANCE CRITERIA
50 8.0-400%ofm/z95
75 30.0 - 66.0% of rniz 95
95 Base Peak, 100% Relative Abundance
96 5.0 - 9.0% of m/z 95 (see note)
173 Less than 2.0% of mlz 174
174 50.0- 120 0% of mlz 95
175 4 0-90%ofmass l74
176 930- 101.0% of m/z 174
177 5 0 - 9 0% of mlz 176
Note All ion abundances must be normalized to mlz 95, the nominal base peak, even though the ion
abundance of mlz 174 may be up to 120 0% that of m/z 95.
The mass spectrum of BFB must be acquired in the following manner Three scans (the peak ape’t scan and the
scans immediately preceding and following the apex) are acquired and averaged. Background subtraction is required
and must be accomplished using a single scan no more than 20 scans prior to the elution of BFB Part of the BFB
peak must not be background subtracted
APPENDIX A - 1 DRAFT 12/96
-------
Appendix A OLMO3.2/VOA
SECTION m: [ NITIAL CALIBRATION CRITERIA
Refer to Region I, EPA-ME Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
II. Section VOA/SV-llI-B for iniual calibration data validation criteria and the following method initial calibration
QC criteria:
The initial calibration standards must be analyzed upon contract award, whenever corrective action is taken which
may change or affect the ini::al calibration criteria or if the continuing calibration acCeptance criteria have not been
met. Initial calibrations must be analyzed after the analysis of a compliant instrument performance check.
The initial calibration standards must include the target compounds listed in the Target Compound List (TCL) in
Section XIII of this Appendix, as well as the internal standards and the system monitoring compounds.
All initial calibration standards must be analyzed at the following concentration levels: 10, 20, 50, 100, 200 ug/L
(unheated for aqueous and medium level soils/heated for low level soils).
Note: The CLP SOW OLMO3.2 minimum response factor method acceptance criterion differs from the
Region I Functional Guidelines initial and continuing calibration minimum response factor validation
criterion. If data quality objectives allow for greater variability of data, then an expanded minimum response
factor validation criterion should be documented in the EPA-approved site-specific QAPJP or amendment to
the QAPJP. If response factors less than 0.05 are allowed, then the validator should ensure that there is
sufricient QC data to support the use of low response factors in sample calculations.
RELATWE RESPONSE FACTOR (RRF) - A measure of the relative mass spectral response of an analyte
compared to its’ internal standard. The RRF is calculated using the following equation:
A C.
RRF = —i- X
Where,
A, = Area of pnmaiy quanutation ion response (EICP) for the compound to be measured
A, = Area of primary quanutanon ion response (EICP) for the internal standard
C = Concentration of the internal standard
C, = Concentration of the compound to be measured
APPENDIX A - 2 DRAFF 12/96
-------
Appendi c A OLMO3.2/VOA
AVERAGE (ME.4N) RELATIVE RESPONSE FACTOR (RRF) - The average or mean RRF is determined by
the analysis of five different standard concentrations and is used in calculating compound concentrations it t samples.
The RRF is calculated using the following equation:
— RRF ,
RRF=)
2 -1
Where.
RRF, = The individual RRFs for various concentration levels
i i = The number of RRFs
PERCENT RELATIVE STANDARD DEVIATION (%RSD) - The % RSD for each comoound is a measure of
the linearity of the calibration curve. The % RSD is calculated using the following equation.
%RSD = Standard Deviation
Mean
Where,
H ( x.- ) 2
Standard Dev.iation = \j
x = Mean
n = total number of values
= each individual value used to calculate the mean
SECTION IV: CQNTIN(JI1’JG CALIBRATION CRITERIA
Refer to Re ton I EP -NE Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
II, Section VOAJSV-IV-B for continuing calibration data validation cntena ann the following method conunuing
calibration QC criteria:
The continuing calibration standard must be analyzed once every 12 hours, following the analysis of a compliant
instrument performance check and initial calibration, and prior to the analysis of fielo samoies, QC samples and
blanks.
The continuing calibration standard must include the target compounds listed in the Target Compound List (TCL)
in Section XIII of this Appendix, as well as the internal standards and the system monitoring compounds
Continuing calibration standards must be analyzed at a concentration level of 50 ug/L (unheated for aqueous and
medium level soils/heated for low level soils)
APPENDIX A - 3 DRAFI’ 12196
-------
Appendix A OLMO3.2/VOA
Note: The CLP SOW OLMO3.2 minimum response factor method acceptance criterion differs from the
Region I Functional Guidelines initial and continuing calibration minimum response factor validation
criterion. If data quality objectives allow for greater variability of data, then an expanded minimum response
factor validation criterion should be documented in the EPA-approved site-specific QAPJP or amendment to
the QA.PjP. If response factors less than 0.05 are allowed, then the validator should ensure that there is
sufficient QC data to support the use of low response factors in sample calculations.
PERCENT DIFFERENCE (%D) - The % D is used to compare the initial calibration RRF with the coruinuing
calibration RRF5O The % Difference indicates both the direction and the magnitude of the comparison, i e , the
% Difference may be either negative, positive or zero.
RRF - RRF
% Difference = C ’ x 100
RRF 2
Where,
RRF = Mean relative response factor from the most recent initial calibration meeting technical acceptance
criteria
RRFC = Relative response factor from continuing calibration standard
SECTION V: BLANK CRiTERIA
Refer to Region I Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
II. Section VOAISV-V-B for blank validation criteria and the following method QC criteria:
Method Required Blanks
Method Blank - A 5 0 niL aliquot of reagent water or purified solid matrix approximate in weight or
volume to the samples that is carried through the entire analytical process to determine
the levels of contamination associated with the processing and analysis of samples All
blanks are spiked with internal standards and surrogate compounds and blank analysis
must meet internal standard and surrogate compound criteria. The method blank must
be analyzed at least once luring every 12 hour time period on each GC/MS system used
for volatile analysis.
2 Storage Blank - Consists of two 40 tilL VOA vials filled with reagent water prepared by the laboratori
when the first samples in an SDG are received. The vials are stored, under the same
conditions, with the field samples. After all of the samples in the SDG are analyzed, a
5 0 mL aliquo of the storage blank is analyzed to determine whether contaimnation was
introduced during storage of the samples All blanks are spiked with internal standards
and surrogate compounds and blank analysis must meet internal standard and surrogate
compound criteria. A minimum of one storage blank must be analyzed per SDG after
all samples for that SDG have been analyzed.
3. instrument Blank - A 5.0 mL aliquot of reagent water that is carried through the entire analytical procedu:e
and is analyzed following highly contaminated samples containing target compounds that
exceed the initial calibration range. The instrument blanks are used to determine if
contamination is introduced by a previous sample and the level associated with the
analytical instrument. All blanks are spiked with internal standards and surrogate
compounds and blank analysis must meet internal standard and surrogate compound
crueria An instrumeru blank must be analyzed after a sample that ezceeds the
calibration range Until an instrument blank meets ihe technical acceptance critena. the
system is considered contarrunated
AYPENDIX A - 4 DRAFT 12/96
-------
Appendix A OLMO3.2/VOA
SECTION VT: SURROGATE COMPOUND CRITERIA
Refer to Region I, EPA-NE Data Validation Functional Guidelines for Evaluating Environmeital Analyses , Part
11, Section VOA/SV.VI-B for surrogate compound data validation criteria and the following method Surrogate
compound QC criteria:
The proper surrogate compounds must be quantified using correctly assigned internal standards and the correct
primary quantitation ions
10 uL of a 25 ug/mL solutton of surrogate compounds Toluene-d 1 , 4 -Bromofluorobenzene 1 , 2 -Djchloroe(hane.d
are added to 5 rnL/5 g of sample, standard, QC sample, or blank for a final concentration of 50 ug/L or 50 ug/kg.
10 uL of a 25 ug/mL solution of internal standards Chlorobenzene-d, and Bromochloromethane are added to 5 rnL/5
g of sample for a final concentration of 50 ug/L or 50 uglkg. 10 uL of a 25 ug/rnL solution of surrogate
compounds Toluene-d 3 , 4-Bromofluorobenzene. 1 .2-Dichloroethane-d 1 are added to 5 rnLs of reagent water
containing an aliquoc of the methanol medium level soil/sediment extract.
Table Aoo A.V1-1 - CHARACTERISTIC IONS FOR SURROGATE COMPOUNDS
Surrogate
Characteristic Ions
Internal Standard
Primary Quantitation Ion
Secondary
Toluene4
98
Ion(s) —
—
4 -BromofIuorobep ne
95
70, 100
174, 176
Chlorobenzene.d.
l, 2 -Dichjoroethaned 4
65
102
Chlorobenzene.d.
Bromochloromethane
The surrogate % recovery is calculated using the following equation:
Surrogate Percent Recovery = x 100%
Qd = Quantity of surrogate determined by analysis
Q , = Quantity of surrogate added to sample/blank
Table Aoo A VI-2 - SURROGATE RECOVERY LIMITS
I Method QC Criteria
Surrogate
Recovery
(Water)
Percent Recovery
Toluenie-d,
88-110
= (Soil/Sediment)
84-!38
- 3
Bromofluorobe ene
86-115 I
1 .2-Dich1oroethane.d I
76-114
APPENDIX A - 5 DRAFT 12/96
-------
Appendix A OLMO3.2/VOA
If one or more sample surrogate recovery does riot meet the acceptance criteria, the sample must be reanalyzed o
determine if the sample matrix is interfering with the surrogate recoveries. Reana1ys s is not required if the sample
is a QC sample and both the matrix spike and matrix spike duplicate surrogate recoveries failed to meet the
acceptance criteria. If the sample was r analyzed and the surrogate recovety(ies) was acceptable in the reanalysis,
then only the reanalysis should have been submitted. However, if the reanalysis also recovers the surrogate(s)
outside of the ac:epancc limits, then both analyses should have been submitted.
SECTION Yfl: INTERNAL STANDARDS CRITERIA
Refer to Re on l. EPA-NE Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
II, Section VOA/SV-VII-B for internal standard data validation criteria and the following method internal standard
QC criteria:
The correct internal standard must be used for sample compound quanutation and the correct internal standard
pnmary quantitation ion must be used for quantitation.
10 uL of a 25 ug/mL solution of internal standards Bromochioromethane, 1 ,4-Difluorobenzene, and Chlorobenzene-
d 5 are added to 5 rrtLfS g of sample, standard, QC sample, or blank for a final concentration of 50 ug/L or 50
ug/kg.
Table Anp.AVII-1 - VOLATILE INTERNAL STANDARDS WITH CORRESPONDING TARGET
COMPOUNDS AND SURROGATES ASSIGNED FOR QUANTITATTON
is Is IS
Bromochiorornethane I , 4—Difluorobenzene Chlorobenzene—d5
Ch lorornethane 1,1, 1—Trich loroethane 2—Hexanone
Bro:nomethane Carbon Tetrachionde 4—Methyl---2-—Pen tanone
Vinyl Chloride Bromodichloromethane Tetrachloroethene
Chioroethane 1 ,2—Dichloropropane 1,1 ,2,2—Tetrachloroechane
Methylene Chloride trans—I ,3—Dichloropropene Toluerie
Acetone Trichloroether ie Cblorobenzene
Carbon Disulfide Dibromochioromethane Ethylbeazene
1, 1—Dich loroethene 1,1 ,2—Trtchloroethane Srrene
1, I —Dichloroeihane Benzene Xylene (total)
1 .2—Dichloroethene(tot.) cis—1 , 3—Dichloropropene 4-Bromo fluoroben.zene (sui-r)
Chloroform Bromoform Toluene-d 8 (surr)
1 ,2—Dichloroethane
2-Butanone
I ,2-Dichloroethane-d4
(surr)
APPENDIX A - 6 DRAFT 12196
-------
Appendix A OLMO3.2/VOA
Table App A.VT1-2 - CHARACTERISTTC TONS FOR INTERNAL STANDARDS FOR VOLATILE
COMPOUNDS
Internal Standard
Characteristic Ions
Primary Quantitation Ion
Secondary Ion(s)
Bromochlorometharie
128
49, 130, 51
1,4-Difluorobenzene
114
63, 88
Chlorobenzene-d5
117
82, 119
Internal standard area counts for each of the internal standards must be within the incluswe range of -50.0% and
+ 100.0% of the response of irnernal standards in the associated daily continuing calibration standard.
The retention time of the internal standard must not vary by more than ± 30 seconds from the retention time of
the associated daily continuing calibration standard.
If one or more internal standard area count and/or retention time does not meet the acceptance criteria, then the
sample must be reanalyzed to determine if the sample matrix is interfering with the surrogate recoveries. Reanalysis
is not required if the sample iz a QC sample and both the matrix spike and matrix spike duplicate failed to meet the
internal s andard acceptance criteria. If the sample was reanalyzed and the internal standard area counts and/or
retention times were acceptable in the reanalysis, then only the reanalysis should have been submitted. However,
if the reanalysis also recovers the internal standard outside of the area count and/or retention time acceptance
criteria, then both analyses should have been submitted.
SECTION Vm: MATRIX SPIKEIMATRIX SPIKE DUPLICATE CRITERIA
Refer to Re2:ori 1. EPA-NE Data Validation Functional Guidelines for Eva1uatin Environmental Anajvses . Part
II. Section VOA/SV-VIII-B for MS/MSD data validation criteria and the following method MS/MSD QC criteria:
Tne MS/MSD spike compounds listed below are spiked at 10 uL in a 25 ug/mL. solution into the 5 mL or 5 g
sample for a final concentranon of 50 ug/L or 50 ug/kg.
A matrix spike and mauix spike duplicate must be performed for each group of samples of a similar matrix for each
SDG, or each matrix withtn an SDG or each group of samples of a similar concentration level (soils only) whicnever
is most frequent. The following advisory matrix spike compound recoveries and RPDs are listed below.
APPENDIX A - 7 DRAFT 12/96
-------
Appendix A OLMO3.2/VOA
Table App.A.VflJ-L - MATRIX SPIKE RECOVERY AND RELATIVE PERCENT DIFFERENCE LIMITS
Compound
Method QC Criteria
Water
Soil/Sediment
% Recovery
RPD**_J
% Recovery
I_RPD
1.1-Dich loroethene
61-145
14
59-172
22
Trichloroethene
71-120
14
62-137
24
Benzene
76-127
11
66-142
21
Toluene
76-125
13
59-139
21
Chlorobenzene
75-130
13
60-133
21
*The MS/MSD % recovery is calculated using the following equation:
Matrix Spike Recovery = SSR-SR x 100
Where,
SSR = Spiked Sample Result
SR = Sample Result
SA = Spike Added
The MS/MSD relative percent difference (RPD) is calculated using the following equation-
Relative Percent DifferenCe =
IMSR - MSDRI
x 100
1/2 (MSR + MSDR)
Where
MSR = Matrix Spike Recovery
MSDR = Man-ix Spike Duplicate Recovery
Note: The vertical bars in the formula indicate the absolme value of the difference, hence RPD is always positive.
SECTION IX: FIELD DUPLICATE CRITERIA
Refer to Reaton I EPA-NE Data Validation Functional Guidelines for E’,aluaung Environmental Analyses . Part
II, Section VOA/SV-IX-B for field duplicate data validation criteria.
APPENDIX A - S
DRAFT 12/96
-------
Appendix A OLMO3.2/VOA
SECTION X: SENSITIVITY CHECK CRITERIA
Refer to Region 1. EPA-NE Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
II. Section VOA/SV-X.B for sensitivity check data validauori criteria.
SECTION X i: PE SAMPLES- ACCURACY CHECK CRITERIA
Refer to Region I EPA-NE Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
II. Section VOA/SV-Xl-B for accuracy check data validation criteria.
SECTION XII: TARGET COMJ’O(JND IDENTIFICATION CRITERIA
Refer to Re21-’n I EPk-NE Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
H, Section VOA/SV-XH-B for target compound identification data validation criteria.
APPENDIX A -9 DRAFF 12/96
-------
Appciidi A
OL1 1fl3.2IVOA
SEC1’ION XIII: C(Th I POIJNI) QUANTII’ATION AND R EPORTEI) QUANTITATION LIMITS CRITERIA
Refer to R gion I. EPA-NE Data Validation Functional Guidelines for Evaluating Environmental Analyses , Pan II, Section VOA/SV.XllI-R for compound
pI inl Hal ion and reported qiianl utation I mitt dal4 validation criteria and the following method quant italton QC criteria.
Volatile larget compounds must be quantiialed using the internal standard method with the internal standards assigned in Appendix A, Section VII. The daily
RRF5() must be used for sample quantilalion. The sample target compounds must be quantilied using the following primary quantitation ions and must be
reported to mIte CRQI.s listed below
IilL!c Ilrt A Xl)I-l - TARGET COME OUND LIST (TCL). PRIMARY QUANTITATION AND SECONDARY IONS. AND CONTRACT REqUIRED
QUANTITATION LIMITS (CRQLs FOR OI.M03.l SOW VOLATILE ORGANIC COMPOUNDS
Quantitation Limits
Vo lati les CAS Number
52
96
64
66
49, 51,86
58
78
61,98
65.83,85, 98, 100
61,98
85
64,100,98
57
99, 117, 119
119, 121
85
65, 114
77
Water
Low
Soil
Med.
Soil
On
Column
ug/L
ug/Kg
ug/Kg
(ng)
Characteristic Ions
Primary Secondary
Chioromethane
74—87—3
10
10
1200 (50)
so
Bromomethane
74—83—9
10
10
1200 (50)
94
V]nyl Chloride
75—01—4
10
10
1200 (50)
62
CimloroeLkamie
75—00—3
10
10
1200 (50)
64
Metitylene Chloride
75—09—2
10
10
1200 (50)
84
Acetone
67—64—1
10
10
1200
(50)
43
Carbon Disulfide
75—15—0
10
10
1200
(50)
76
],i—Dichloroeihene
75—35—4
10
10
1200
(50)
96
],1—Dich loroethane
75—34—3
10
10
1200
(50)
63
1,2—Dichioroethene (total)
540—59—0
10
10
1200
(50)
96
Ch1oro orm
67—66—3
10
10
1200
(50)
83
1,2—Dichioroethane
107—06—2
10
10
1200
(50)
62
2—Butanone
78—93—3
10
10
1200
(50)
43*
1,1,1—Trichioroethane
71—55—6
10
10
1200
(so)
97
Carbon Tetrachioride
56—23—5
10
10
1200 (50)
117
l3roinodichloromethane
75—27—4
10
10
1200 (50)
83
1 ,2—Dichioropropane
78—87—5
10
10
1200 (50)
63
cis—1,3—DiclilorOpropefle
30061—01—5
10
10
1200 (50)
75
- m/z 43 is used for quantitatlon of 2-Butanone, but m/z 72 must be present for positive identification.
APPENDIX A - 10
DRAFT 12/96
-------
AppelilluX A
01M03.2/VOA
T ! r’i A XIiI-I - T ! FTJ MPOIJND_l IST ffCI.). PRIMARY OIJANTITATION AND SECONDARY IONS. AND CONTRACT REOIJIRED
OIJANI ITATION liMITS (CROLs) FOR OLMO3 I SOW VOLATII.I ORGANIC COMPOuNDS (CONT )
Quantitation Limits
Volat iles
CAS Number
Low
Med.
On
Characteristic
Ions
Water
ug/L
Soil
ug/Kg
Soil
ug/Kg
Column
(ng)
Primary
Secondary
Trichloroethene
79—01—6
10
]0
1200
(50)
130
95,97,132
DibroinochloroineLhane
124—48—1
10
10
1200
(50)
129
208,206
1,1,2—Trichioroethane
79—00—5
10
10
1200
(so)
97
83,85,99,132,134
Benzene
71—43—2
10
10
1200
(50)
78
trans—l,3—Dichloropropene
10061—02—6
10
10
1200
(50)
75
77
Brornoform
75—25—2
10
10
1200
(50)
173
171,175,250,252,254,256
4—Methyl—2—pentanone
108—10—1
10
10
1200
(50)
43
58,100
2—llexanone
591—78—6
10
10
1200
(50)
43
58,57,100
Tetrachioroethene
127—18—4
10
10
1200
(50)
164
129,131,166
Tolu ne
108—88—3
10
10
1200
(50)
91
92
1,i,2 .2—Tetrach loroethau
Ch lorobenzene
79—34—5
108—90—7
10
10
10
10
1200
1200
(50)
(50)
83
112
85,131,131,166
114
Ethy lbenzene
1OL) -41—4
10
10
1200
(50)
106
91
SLyrene
Xy1eiie (Total)
100—42—5
1330—20—7
10
10
10
10
1200
1200
(50)
(50)
104
106
78,103
91
AI’PI’NDIX A — II
DRAFT 12/96
-------
Appendix A OLMO3.2/VOA
SAMPLE CONCENTRATIOrI - The amount of analyte present in a sample is calculated using the RRF5O of the
continuing calibration standard in the following equations.
Sample concentration for water:
IL - ( AX) (IS) (Df )
ug - (A . ) (RRF) (V 0 )
Sample concentration for low level soil/sediment:
(A, ) (IS)
ug/Kg (Dry weight basis) = (A) (RRF) ( V ) (D)
Sample concentration for medium level soil/sediment:
( Ar) (IS) (Va) (1000) (Df )
ug/Kg (Dry weight basis) = A ) (RRF) (Va) (We) (D)
Where,
A = Area of the pnm.ary quanutation ion response (EICP) for the compound to be measured
= Area of the primary quantitation ion response (EICP) for the specific internal standard
IS = Amount of internal standard added in nanograms (ng)
RRF = Relative Response Factor from the (Ambient temperature purge for water and medium level
soil/sediment and heated purge for low level soil/sediment) calibration standard
V 0 = Volume of water purged in milliliters (niL)
Df = Dilution Factor The dilution factor for analysis of water samples for volaules by this method is
defined as the ratio of the number of milliliters (mL) of water purged (i.e., V 0 above) to the
number of rnL of the original water sample used for purging. If no dilution is performed , Df= 1.
The dilution factor for analysis of soil/sediment samples for volatiles by the medium level method
is defined as follows:
uL most conc e’ctract used to make dilution + uL clean solvent
uL most conc. extract used to make dilution
= Wetzht of the sample added to the purge tube in grams (g)
D = 100 - % Moisture
100
V = Total volume of the methanol extract in milliliters (mL)
V 0 = Volume of aliquoc of the methanol extract in riucroliters (uL) added to reageru water for purg ln2
= Weight of soil/sediment extracted in grams (g)
APPENDIX I - 12 DRAFT 12/96
-------
Appendix A OLMO3.2/VOA
CRQL CALCULATIONS
Water:
( V )
Adjusted CRQL = Contract CROL x x (Df)
QI
‘Where,
V 0 and Df are defined in the sample concentration equauon above
V = Contract sample volume (5 mL)
Soil/Sediment-Low:
Adjusted CRQL = Contract CRQL x (W)
Where,
W 1 and D are defined in the sample concentration equation above
W 1 Contract sample weight (5 g)
Soil/Sediment-Med.
Adjusted RQL = Contract RQL x (Vt) (Vp) (Di )
(W 5 ) (Va) (1/) (D)
Where,
V 1 , Df, W 1 , V 1 , and D are defined in the sample concentration equation above
W = Contract sample weight (4 g)
V 7 = Contract soil aliquot volume from soil methanol extract (100 uL)
= Coniract soil methanol extract volume (10,000 uL)
APPENDIX A - 13 DRAFT 12/96
-------
Appendix A OLMO3.2/VOA
SECTION XIV: TENTATIVELY IDENTIFIED COMPOUND CRITERIA
Refer to Region I. EPA-NE Data Validation Funczional Guidelines for Evaluaung Environmental Analyses , Part
II, Section VOA/SV-XIV-B for tentatively identified compound (TIC) dzua validation criteria and the following
method TIC QC criteria:
The validator is required to report up to 30 TICs in the Data Validation Memorandum.
TENTATIVELY IDENTIFIED COMPOUND CONCENTRATION The estimated concentration for non-taraet
compounds tentatively identified shall be determined by the irnernal standard method using the following equations
Sample concentration for water:
(A. ) (IS) (Dt)
ucz/L=
(A ) (RRF) (V 0 )
Sample concentration for low level soil/sediment:
(Ar) (IS)
ug/Kg = (A ) (RRF) (h’ 5 ) (D)
Sample concentration for medium level soil/sediment:
- — ( Ar) (IS) (Vs) (1000) (Df )
ug/Kg - (&S ) (RRF 1 (Vs) (W) (D)
Where,
= Area of the primary quantitation ion response (EICP) for the non-target compound to be measured
A 1 = Area of the primary quanutanon ion response (EICP) for the specific internal standard
IS = Amount of internal standard added in nanogranis (ng)
RRF = Retauve Response Factor assumed to be I
V, = Volume of water purged in milliliters (niL)
Df = Dilution Factor - The dilution factor for analysis of water samples for volatiles by this method is
defined as the ratio of the number of milliliters (mL) of water purged (i.e., V 0 above) to the
number of niL of the original water sample used for purging. If no dilution is performed , Df= 1
The dilution factor for analysis of soil/sediment samples for volatiles by the medium level method
is defined as follows:
uL most conc extract used to make dilution + uL clean solvent
uL most conc. e’ cract used to make dilution
W 1 = Weight of sample added to the purge rube in grams (g)
D = 100 - % Moisture
100
V , = Total volume of the methanol extract in milliliters (mL)
= Volume of altauot of the methanol extract in microliters (uL added to reagent water for pur tng
W 1 = Weight of soil/sediment extracted in grams (g)
APPENDIX A - 14 DRAFT 12/96
-------
Appendix A OLMO3.2/VOA
SECTION XV: SEMIVOLATILE CLEANUP CRITERIA
Nor applicable to volatile analysis.
SECTION XVI; SYSTEM PERFORMANCE CRITERIA
Refer to Region I. EPA-NE Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
II. Section VOA/SV-XV [ -B for system performance data validation cnceria
SECTION XVth OVERALL ASSESSMENT CRITERIA
Refer to Re on I EPA-NE Data Validation Functional Guidelines for EvaJuatin Environmental Analyses , Parr
II. Section VOAISV-XVII-B for overall assessment data validation critena.
APPENDfX A - 15 DRAFT 12196
-------
Appendix B
CLP SOW OLMO3.2/Semivolatile Organic Analysis
Method QC criteria, Equations, and Definitions
-------
OLMO3.2ISV
APPENDC B
The following method QC criteria, equations, and definitions appLy to data generated according to the USEPA CLP
Statement of Work for Organic Analysis, Multi- dedia, Multi-Concentration, OLMO3.2, Exhibit D
Semivolatiles.
SECTION I: PRESERVATION & TECHNICAL HOLDING TIME CRITERIA
Refer to Re2ion 1. EP - E Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
II, Section VOA/SV-I-B for preservation and technical holding time data validation critena.
SECTION II: GCIMS INSTRUMENT PERFORMANCE CHECK (TUNING) CRITERIA
Refer to the fo lowtng method GCIMS instrument performance (tunmg) QC criteria for data validation:
The analysis of the instrument performance (tuning) check solution (50 ng DFTPP on column) must be performed
at the beginning of each 12-hour period during which samples or standards are analyzed. The tuning check,
decafluorotriphenylphosphine (DFTPP). for semivolatile analysis must meet the ion abundance criteria given below
EON ABUNDANCE CRITERIA
51 30.0- 80.0% of m/z 198
68 Less than 2.0% of mlz 69
69 Present
70 Less than 2.0% of mlz 69
127 25.0-750% of mhz 198
197 Less than 1 0% of mlz 198
198 Base Peak, 100% Relative Abundance (see note)
199 5 0 - 9 0% of mlz 198
275 10 0 - 30.0% of miz 198
365 Greater than 0.75% of m/z 198
441 Present, but less than miz 443
442 40.0- 110.0% of mhz 198
443 15.0-240%ofmJz442
Note All ion abundances must be normalized to mlz 198, the nominal base peak, even thouah the on
abundances of mu 442 may be up to 110% that of mhz 198.
The mass spectrum of DFT?P must be acquired in the following manner Three scans (the peak acex scan and the
scans immediately preceding and following the apex) are acquired and averaged Background subtraction is
required. anc must be accompiished using a single scan no more than 20 scans prior to the elution of DFTPP Part
of the DFTP9 peak must not be background subtracted.
APPENDIX B - I DRAFT ’ 12/96
-------
Appendix B OLMO3.2/SV
SECTION m: INITIAL CALIBRATION CRITERIA
Refer to Re on I. EPA- IE Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
II. Section VOAJSV.IIIB for initial calibration data validation criteria and the following method initial calibration
QC crneiia:
The initial calibration standards must be analyzed upon contract award, whenever corrective action is taken which
may change or affect the initial calibration criteria or if the continuing acceptance criteria have not been met. Iniual
calibrations must be analyzed after the anaiysis of a compliant instrument performance check.
The initial cztibration standards must include the target compounds listed in the Target Compound List (TCL) in
Section XIII of this Appendix, as well as the internal standards and the system monitoring compounds.
2 uL of the initial calibration standard must be injected and all initial calibration compounds and system monitoring
compounds must be analyzed at the following concentration levels; 10, 20, 40, 60, 80 ng/uL. However, the
following eight compounds only require a four point calibration and are injected at concentrution levels of 50, 80,
120, and 160 og/uL: 2 ,4-dinurophenol, 2 ,4,5-inchiorophenol, 2 -nicroaniline, 3 -nltroaniljne, 4 -nitroanjlme, 4-
nhtrophenol 4 . 6 -dinitro-2methylphenol and pentachlorophenof since detection at less than 50 rig per injection is
difficult.
Note: The CLP SOW OLMO3.2 minimum response factor method acceptance cntenon differs from the
Region I Functional Guidelines initial and continuing calibration minimum response factor validation
criterion, If data quality objectives allow for grenter variability of data, then an e.’ panded minimum response
factor validation criterion should be documented in the EPA-approved site-specific QAPJP or amendment to
the QAPjP. If response factors less than 0.05 are allowed, then the validator should ensure that there is
surncient QC data to support the use of low response factors in sample calculations.
RELATIVE RESPONSE FACTOR (RRF) - A measure of the relative mass spectral response of an analyte
compared to its’ internal standard. The RRF is calculated using the following equation’
A. C.
RRF = —. - x —f
A 25 C
Where,
A, Area of primary quantitanon ion response (EICP) for the compound to be measured
A, = Area of primary quantitation ion response (EICP) for the internal standard
= Amount of the internal standard injected (ng)
= Amount of the compound to be measured injected (ng)
APPENDIX B - 2 DRAFT 12/96
-------
Appendix B OLMO3.2ISV
AVERAGE (MEAN) RELATIVE RESPONSE FACTOR (RRI) - The average or mean RRF is determined by
the analysis of five different standard concentrations and is used in calculating a compound concentration in samples.
The RRF is calculated using the following equation:
RRF
RRF=>2
.1’l
Where,
RRF, = The individual RRFs for various concentration levels
n = The number of RRFs
PERCENT RELATIVE STANDARD DEVIATION (%RSD) - The % RSD for each compound is a measure of
the linearity of the calibration curve. The % RSD is calculated using the following equation:
%RSD = Standa:d Deviation 100
Mean
Where,
In i _ \2
Standard Deviation = _______
Ni i
x = Mean
o = total number of values
= each individual value used to calculate the mean
SECTION IV: CONTTh1UING CALIBRATION CRITERIA
Refer to Re2ion I EPA-NE Data Validation Functional Guidelines for Evaluating Environmental Anai’ ses , Part
II. Section VOA/SV-Iv -B for continuing calibration data validation criteria and the following method continuing
calibration QC criteria.
The continuing calibration standard must be analyzed once even 12 hours, fotlowing the analysis of a compliant
instrument performance check and initial calibranon, and pnor to the analysis of field samples, QC samples and
blanks
The continuing calibration standard must include the target compounds listed in the Target Compound List (TCL)
in Section XIII of this Appendix, as well as the internal standards and the system monitoring compounds.
Continuing calibrations must be analyzed at a concentration level of 50 ng/2 uL except for the following eight
compounds which are analyzed at a concentration level of 100 ng/2 uL 2.4-dinirophenol, 2,4,5-inchlorophenol,
2-nitroani1in 3-nitroaniline, 4-nitroaniline, 4-aitropnenol, 4,6-dinitro--methy(phencl and oentachlorophenol since
detection at less than 50 ng per injection is difficuit
APPENDIX B - 3 DRAFT 12/96
-------
Appendix B OLMO3.2/SV
Note: The CLP SOW OLMO3.2 minimum response factor method acceptance criterion differs from the
Region I Functional Guidelines initial and continuing calibration minimum response factor validation
criterion. If data quality objectives allow for greater variability of data, then an expanded minimum response
factor validation criterion should be documented in the EPA-approved site-specific QAPJP or amendment to
the QAPJP. If response factors less than 0.05 are allowed, then the validator should ensure that there is
sufficient QC data to support the use of low response factors in sample calculations.
PERCENT DIFFERENCE (%D) - The % D is used to compare the initial calibrauonRRF with the continuing
calibration RRF5O. The % Difference indicates both the direction and the magnitude of the comparison, i.e , the
% Difference may be either negative, positive or zero.
RRF - RRF
% D. fference = ____ x 100
RRF
Where,
RRF = Mean relative response factor from the most recent initial calibration meeting technical acceptance
criteria
RRFC = Relative response factor from continuing calibration standard
SECTION V: BLANK CRITERIA
Refer to Region 1, EPk-NE Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
II, Section VOA/SV-V-B for blank data validation criteria and the following method QC criteria:
Method Reauired Blank
Method Blank . A volume of reagent water or purified solid matnx approximate in weight or volume to the
samples which is carried through the entire analytical process to determine the levels of
contamination associated with the processing and analysis of the samples. All blanks are spiked
with internal standards and surrogate compounds and blank analysis must meet internal standard
and surrogate compound criteria. Method blank extraction and analysis must be performed once
per each SDG, or each 20 samples in an SDG. or whenever samples are extracted by the same
procedure, whichever is most frequent, and analyzed on each GCIMS system used to analyze
associated samples.
SECTION VI: SURROGATE COl ’v [ POUNI) CRITERIA
Refer to Re ion I. EPk-NE Data Validauon Functional Guidelines for Evaluating Environmental Analyses , Part
II, Section VOA/SV-V1.B for surrogate compound data validation criteria and the following method surrogate
compound QC criteria
The proper surrogate compounds must be quantified using correctly assigned internal standards and the correct
primary quantitation ions
APPENDIX B - 4 DRAFt’ 12196
-------
Appendix B OLMO3.2/SV
Surrogate compounds Nitrobenzerie-d , 2 -FluorobipheflYl , Terphenyl-d 14 , and l,2-Dichlorobenzene-d, (advisory) are
added to all samples, standards, QC samples, and blanks at a concentration of 100 ug/mL and surrogate compounds
Phenol-d , 2-Fluorophenol, 2,4,6-Tribromopheflol. and 2-Chlorophenol-d (advisory) are added to all samples,
standards, QC samples, and blanks at a concentration of 150 ug/mL.
Table App B VT-I - CHARACTERISTIC TONS FOR SURROGATE COMPCCNDS
Surrogate
Characteristic Ions
Internal Standard
Primary
Quantitation Ion
Secondary Ion(s)
Nitrobenzene-d 5
82
128, 54
NaphthaIene-d
2-Fluorobiphenyl
172
171
Acenaphthene-d 0
Terphenyl-d,.
244
122, 212
Chrysene-d 1
Phenol-d,
99
42, 71
1.4-Dichlorcoerizene.d
2-F uorophenol
112
64
1,4-Dichlorobeazene-d
2,4 ,6-Tribromophenol
330
332, 141
Phenanthrene-d. 0
2-Chlorophenol-d ,
(Reccvery limits advisory)
132
68, 134
1 , i Dich1orobeazene d,
1 ,2-Dichlorobenzene-d 4
(Recovery limits advisory)
152
115, 150
1 ,4-Dtchlorobenzene-d,
The % surrogate recovery is calculated using the following equation:
Surrogate Percent Recovery = - x 100%
Qd = Quant y of surrogate determined by analysis
Q = Quantity of surrogate added to sample/blank
APPENDIX B - 5 DRAFT 12/96
-------
Appendix B OLMO3.2JSV
Table Ant, B VI-2 - SURROGATE RECOVERY LIMITS
Surrogate
Method QC Criteria
Percent Recovery
(Water)
Percent Recovery
(Soil/Sediment)
Nitrobenzene-d (B/N)
35-114
23-120
2-Fluorobiphenvi (BIN)
43-116
30-1 15
Terphenvl-d, 4 (B/N)
33-141
18-137
Phenol-d, (Acid)
10-110
24-113
2-Fluorophenol (Acm)
21-110
25-121
2,4 ,6-Tribromophenol (Acid)
10-123
19-122
2-Ch1oropheno1-d (Acid)
33-110
(advisory)
20-130
(advisory)
1 ,2-Dichlorobenzene4 (B/N)
16110
(advisory)
20130
(advisory)
If iwo or more acid or base neutral surrogate compounds fail to meet their recovery acceptance criteria, the
laboratory should check calculations, sample preparation logs, the surrogate compound spiking solutions, and the
instrument operation. If sample surrogate recoveries do riot meet the acceptance criteria, as a result of the above
mentioned problems or other unknown problems, the sample should be re-extracted and reanalyzed to determine
if the sample matrix is interfering with the surrogate recoveries. Re-extraction and reanalysis are not required if
the sample is a QC sample and both the matrix spike and matrix spike duplicate surrogate recoveries failed to meet
the acceptance criteria. Reanalysis is required if the failed surrogate recoveries are the result of instrument
malfunction. If the sample was re-extracted and reanalyzed and the surrogate recoveries were acceptable in the
reanalysis, then only the reanalysis shouid have been submitted However, if the re-extracted/reanalyzed sampie
also recovers the surrogates outside of the acceptance limits, then both analyses should have been submitted
APPENDIX B - 6 DRAFT 12/96
-------
Ap 1 I I OIrsl O3i
SEC’flON ‘Il: INTERNAl. STANDARDS CRITERIA
Rekr to Region I. FPA-N di lulation Functional ( ii,ilel,nes for Evahi ing Environmental An ily cs , Part II, Section VOA/SV-VlI-F for internal standard
d ,uta v.ilutl,itiui, crucu ia intI the following method interlidl standard QC criteria.
The correct internal standard and the correct internal sIdn(lar(l primary quantitatton ion must be used for sample compound quantitation
The internal standard compounds listed below are added into all samples, standards, QC samples, and blanks at a concentration of 40 ngI2 LIL.
TahIA VII-1 - SEMIV()I.ATILE INTF.RNAI. STANDARDS WITh CORRESPONDING TARGET COMPOUNDS AND SURROGATES
ASSIGNED FOR QUANTITATION
IS IS IS IS IS IS
I . — D!c r ka c.ne—lI4 hil!;Ikuc—d8 Acenaphthene—d 10 Phenanthrene—d hO Chrysene— I 12 Perylene—d 12
Phenol Nit robenzene I lexachiorocyclo— 4,6—Dinitro-—2— Pyrene Di—n——octy l-
bis(2—Ch luiocthy l) Isophorone pentadiene methylphenol B uuy lhenzy l- philialate
ether 2—N utro 1 iheno l 2,4 ,6—Trichloro— N—nitroso-di— plithalate Benzo(b)fluor—
2—Clilorophenol 2 ,4—E)m methyl— phenol phenylamine 3 ,3 ’—Dicluloro— anthene
I ,3—Diclulorohcn,epie phenol 24 .5—Tricliloro— 4—Bromophenyl henzudine Benzo(k)fluor-.——
I ,4—Dtchlorohenzcmic l)iS(2—ChlOr O— phenol phenoletluer Benzo(a)— anthene
I ,2—Dichlorohenzene ethoxy)rnetl mane 2—Chloronaphthalene I lexachloro— anthracene Benzo(a)pyrene
2—Methyl phenol 2 .-i —Dichloro— 2—N itroanui tue benzene bms(2—ethy l- Indeno( I ,2 ,3—cd)-
2,2’ -oxyhis- phenol Dtmethylphthalate Pentachioro— hexy l)phtha late pyrene
(I -Cliloroprop ine) I ,2 .4—Trtchloro— Acenaplii liy lene phenol Chrysene Dibenz(a ,h)-
4—ft Ictliylplucnul bcnzene 3—Nitroanmlmne Phenanthrene Terphenyl—d 14 anthracene
N—Nit roso— Di— n— Napluthalene Acenaphthene Carbazole (sutrr) Benzo(g .h,i)-
propylamune 4—Cluloroaiiilm uie 2,4—Dmnitrophenol Anthracene perylene
I lcxacluloroethianc I Iexacliloro— 4—Nitrophenol Di—n—h imtyl—
2—I l 1101 O l ici it) I hi it ad ie tie I)i henzo hi ran p1 it Ii al ate
(sn ii) ‘l—Clm loro—3— 2 .4—Dinitromnluene Fitiorantlienc
l 1 hiemiol—d S (siirr) mcthylp lmcnol 2 .6—Dinitromoluene 2,4 ,6-Truhroino—
2-Clmloro 1 dicno l- iI .4 2—Mctliyliiap!i— [ )ueihylphthualaue phenol (surr)
(sit ii I lialene ‘I—Cu lomoplieiiyl
I .2 — I) ic Ii Ii rol teui zenc—d -I N it rohcnze ne—d5 l)Iieny let I uer
(suit) (suirr) Fluorene
4—Nitroaniline
2—Pluorobipluenyl
(siirr)
(stirm ) = sitrrogalc coni 1 moiund
APPENDIX II - 7 DRAFT 12/96
-------
Appendix B OLMO3.2/SV
Table App B Vll-2 - CHARACTERISTIC IONS FOR INTERNAL STANDARDS FOR SEMIVOLATILE
COMPOUNDS
Internal Standard
Characteristic Ions
I
Primary Quantitacion Ion
J Secondary Ion
1 ,4-Dichlorobenzene-d,
152
115
Naphtha lerie-d 3
136
68
Acenaphthene-d 10
164
162, 160
Phenanthrene-d 10
188
94, 80
Chrysene-d 1 .
240
120, 236
Perylene-d!,
264
260, 265
Internal standard area counts for each of the internal standards must be within the inclusive range of -50 0% and
+ 100 0% of the response of internal standards in the associated daily continuing calibration standard
The retention ume of the internal standard must not vary by more than ± 30 seconds from the retention time of
the associated daily continuing calibration standard.
If one or more internal standard area count and/or retention time does not meet the acceptance criteria, then the
sample must be reanalyzed to determine if the sample matrix is interfering with the surrogate recoveries. Reanalysis
is not required if the sample is a QC sample and both the matrix spike and matrix spike duplicate failed to meet the
internal standard acceptance criteria. If the sample was reanalyzed and the internal standard area counts and/or
retention times were acceptable in the reanalysis, then only the reanalysis should have been submitted. However,
if the reanalysis also recovers the internal standard outside of the area count and/or retention time acceptance
criteria, then both analyses should have been submitted.
A1’PENDL B - S DRAFT 12/96
-------
Appendix B
OLMO3.2/SV
SECTION Viii: MATRIX SPIKE! MATRIX SPIKE DUPLICATE CRITERIA
Refer to Region 1. EP -NE Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
II, Section VOA/SV-VIII-B for MS/MSD data validation criteria and the following method MS/MSD QC criteria:
A matrix spike and matrix spike duplicate must be extracted and analyzed for each group of samples of a similar
matrix for each SDG, or each matrix within an SDG or each group of samples of a similar concernratton level.
The following advisory matrix spike compound recoveries and RPDs are listed below:
MS/MSD base neutral compounds 1 ,4-dichloroberizene. N-nitroso-di-n-propylainine, 1 ,2,4-rrichlorobenzene.
acenaphtherie, 2,4-dinitrocoluene, and pyrene are spiked a a concentration of [ 00 ug/mL and MS/MSD acid
compounds phenol, 2-chlorophenol, 4-chloro-3-methylphenol, 4-rutrophenol. and peruachioropheriol are spiked at
a concentration of 150 ug/mL.
Table Aoo B.VIll-1 - MATRIX SPIKE RECOVERY AND RELATIVE PPD XTT DIFFERENCE LIMITS
Compound
Method QC Criteria
Water
I Soil/Sediment
7o Recovery __]__RPD.’
% Recovery
RPD
Phenol
12-110
42
26-90
35
2-Chlorophenol
27-123
40
25-102
50
1,4-D icbjorobenzenc
36-97
28
28-104
27
N -Nitroso di rt propy1amine
41-116
38
4 1-126
38
1.2.4-Trichlorobenzene
39-98
28
38-107
23
4 -ChIoro-3-me ivlphenol
—
23-97
42
26!03
33
Acenaphthene
46-1 18
31
31-137
19
4-Nitrophenol
10-80 J
50
11-114
50
2 , 4 -D’nicrocoluene
24-96
—
38
28 39
47
Pencachlorophenol
9-103
50
17109
47
P’irene
26-127
31
35142
36
APPENDIX B - 9
DRAFT 12/96
-------
Appendix B OLMO3.2/SV
t The MSIMSD % recovery is calculaed using the following equation:
Matrix Spike Recovery = SSR-S2 ? x 100
Where.
SSR = Spiked Sample ResuU
SR = Sample Result
SA = Spike Added
l*The MS/MSD relative percent difference (RPD) is calculated using the following equattoir
Relative Percent Difference = l/ M S MS R ) x 100
Where,
MSR = Matrix Spike Recovery
MSDR = Matrix Spike Duplicate Recovery
Note The vertical bars in the formula indicate the absolute value of the difference, hence the RPD is always
positive.
SECTION LX: FIFLD DUPLICATE CRITERIA
Refer to Re2ion 1 EPA-NE 1 )ara Validation Functional Guidelines for Evaluatine Environmental Analyses , Part
II. Section VOA/SV-LX-B for field aupticate data validation cnteria.
SECTION X: SENSITWITY CHECK CRITERIA
Refer to Re2ion I EPA-NE Data Validation Functional Guidelines for Eva1uaun Environmental Analyses , Part
II, Section VOA/SV.X-B for sensitivity check data validation criteria.
SECTION XI: PE SAMPLES - ACCURACY CHECK CRITERIA
Refer to Re2Ior. I EP -NE Data Validation Functional Guidetines for Evaluatina Environmental Aralvses , Part
II, Section VOA,SV-XI-B for accuracy check data validation criteria.
SECTION X II: TARGET COMPOUND IDENTIFICATION CRITERIA
Refer to Re2Ion I EP -NE Data Validation Functional Guidelines for Evaluatin! Environmental Analyses , Part
II. Section VOA,SV-XII-B for target compouna identiiicauon data valiuauon criteria
APPENDIX B - 10 DRAFI’ 12/96
-------
App
OLl I03.2
SECTION XIII: COM POUND QI IANTITATION AND REPORTEE) QUANTITATION LIMITS CRITERIA
Refer to Rcginn 1, F NL P iIa Y !! ll p Fiincti p [ cj !j jines for Ev Jp pjJ fl.i p!iI Afl Jy . Part II, Section VOA/SV-XIII-B for compound
(III.ItitiiaIi uI and reported (jiiJnhlidlu)n limit data valitl .itioii .i iteria and the following method qtiariiit tion QC criteria:
Semivolat tie target compoiiiids must he qlianhlcate(I using the internal standard method with the internal standards assigned in Appendix B, Section VII. The
LiiIy RRF5O nuist be IIsC(I br sample qii.InhItation. The sample target compounds must be quantitied using the following primary quamitation tons and must
he reportc(I to the CRQLs Iisie(l below:
I L k vnJ XIII-I - TARGET CON’IPOIJND LIST (TCL). CONTRACT REQuIRED QIJANTITATION LIMITS (CROLs). PRIMARY
QIJANTITATION IONS. AND SECONDARY IONS FOR OLMO3 I SOW SEMIVOLATILE ORGANIC COMPOUNDS
Quantitation Limits
Characteristic Ions
Primary Secondary
Semivolatiles
CAS Number
Co lurnn
(ng)
Low
Med
Water
Soil
Soil
ug/L
us/Kg
ug/Kg
Phenol
108—95—2
10
330
10000
(20)
94
65,66
bis(2—Cbloroethyl) ether
]1l—44—4
10
330
10000
(20)
93
63,95
2—Chiorophenol
95—57—8
10
330
10000
(20)
128
64,130
1 ,3—Dichlorobenzene
541—73—1
10
330
10000
(20)
146
148,113
1,4—D chlorobenzene
106—46—7
10
330
10000
(20)
146
148,113
i ,2—Dich)orobenzerue
2—Methylphenol
95—50—1
95—48—7
10
10
330
330
10000
10000
(20)
(20)
146
108
148,113
107
2,2’ -oxybis
(i-Ch loropropane )tt
4—Metluylphenol
108—60—1
106—44—5
10
10
330
330
10000
10000
(20)
(20)
45
108
77,79
107
N—Nit roso—d i—n -
propy)anu ine
621—64—7
10
330
10000
(20)
70
42,101,130
llexach loroethane
67—72—1
10
330
]0000
(20)
117
201,199
Nitrobenzene
98—95—3
10
330
10000
(20)
77
123,65
Isophorone
2—Nitroplienol
78—59—1
88—75—5
10
10
330
330
10000
10000
(20)
(20)
82
139
95,138
65,109
2 ,4—F)imerhy]phenol.
105—67—9
10
330
10000
(20)
107
121,122
his (2—Chloroethoxy)
methane
111—91—1
10
330
10000
(20)
93
95,123
2 ,.I—r)ic liloropheno l
120—83—2
10
330
10000
(20)
162
164,98
],2 ,4—Tric l ulorobenzefle
120—82—1
10
330
10000
(20)
180
182,145
Napht;ha lene
91—20—3
10
330
10000
(20)
128
129,127
4—Chloroaniline
106—47—8
10
330
10000
(20)
127
129
ilexachlorobutdd]ene
87—68—3
10
330
10000
(20)
225
223,227
U Previously known by the name bis(2-Chloroisopropyl) ether
APPENDIX II - II
DRAVF 12/96
-------
Appe.ulix U
OLMO3.2ISV
- TARGET CO IINDI.IST (TCL). CONTRACT REQUIRED QIJANTITATION IJMa CROLs) PRIMARY
QIJANTITATION IONS. AND SECONDARY IONS FOR OI.MO3 I SOW SEMIVOLATILE ORGANIC COMPOUNDS (CONT )
Qttaiuitation Limits
Water
Soil
Soil Column
Senuvolatiles
CAS Number
ug/L
ug/Kg
ug/Kg
(ng)
Characteristic
Primary
Ions
Secondary
4—Chloro—3—methylpheno l
59—50—7
10
330
10000
(20)
107
2—Methylnaphtha lene
91—57—6
10
330
10000
(20)
142
144,142
l lexac hlorocyclopentadiene
77—47—4
10
330
10000
(20)
141
2,4 ,6—Trichlorophenol
88—06—.
10
330
10000
(20)
237
196
235,272
2,4,5—Trichiorophenol
95—95—4
25
830
25000 (50)
196
198,200
2—Chloronaphthalene
91—58—7
10
330
10000 (20)
162
198,200
2—Nitroaniline
88—74—4
25
830
25000 (50)
164,127
Dimethylphthalate
131—11—3
10
330
10000 (20)
65
163
92,138
Acenaphthylene
208—96—8
10
330
10000 (20)
152
194,164
2,6—Dinitrotoluene
606—20—2
10
330
10000 (20)
165
151,153
3—Nitroaniline
99—09—2
25
830
25000 (50)
89, 121
Acenaphthene
83—32—9
10
330
10000 (20)
153
108,92
2.4—Dinitrophenol
51—28—5
25
830
25000 (so)
152,154
4—Nitrophenol
100—02—7
25
830
25000 (50)
184
63 154
I)ibenzofiiran
132—64—9
10
330
10000 (20)
139,65
2,4—Dinitrotoluene
121—14—2
10
330
10000
(20)
168
165
139
Diethy lphthalate 84—66—2
4—Chlorophenyl—phenylether 7005—72—3
Fluorene 86—73—7
10
10
10
330
330
330
10000
10000
10000
(20)
(20)
(20)
149
204
166
63,182
177,150
206,141
4—Nitroan 1ine
100—01—6
25
830
25000
(50)
165,167
4 ,6—Dinitro—2—rnethy]phenol
534—52—1
25
830
25000
(50)
138
198
92 108
N—nxlroso-di-pheny lam ine
86—30—6
10
330
10000
(20)
182,77
4—Bromophenyl—phenylether
101—55—3
10
330
10000
(20)
169
168,167
Ilexachioroberizene
118—74—1
10
330
10000
(20)
250,141
Pentachiorophenol
87—86—5
25
830
25000
(50)
284
142,149
Plienanthrene
85—01—8
10
330
10000
(20)
264,268
Anthracene
120—12—7
10
330
10000
(20)
179,176
Carbazole
86-74-8
10
330
10000
(20)
167
179,176
Dx—n—buty lphtha late
84—74—2
10
330
10000
(20)
149
166,139
Fluoranthene
206—44—0
10
330
10000
(20)
150,104
Pyrene
I3uty lbenzylphthalate
129—00—0
85—68—7
10
10
330
330
10000
10000
(20)
(20)
202
101,100
ioi,ioo
APPEI ’ - 12
DRAVF
-------
Apiwmlix II
OLM O3.2/SV
T.thle App B Xlll-1 - Th! JI T COM! QL!NI) I 1ST (TCL). CONTRACT REQUIRED OIJANTITATION LiMiT JCRQLs). PRIMARY
QIJANTITATION IONS. AND SECONDARY IONS EOI ()LMOI I SOW SEMIVOLATILE ORGANIC COMPOUNDS (CONT )
Qtianticatiou Limits
Low
Med
Semivolatiles
CAS Number
Water
ugIL
Soil
ug/Kg
Soil
ug/Kg
Column
(ng)
Characteristic Ions
Primary Secondary
3 ,3’—Dichlorobenzidifle
Benzo(a)anthracene
Chrysene
bis(2- LLhylhexyl)phthalate
Di—n—octylphtha1ar
Benzo(h)t luoranthene
Benzo(k)f]uoranthene
Benzo(a)pyrene
Indeno(1,2,3—cd)pyrene
Dibenz(a ,h)anthracene
i3enzo(g ,h ,i)perylene
91—94—1
56—55—3
218—01—9
117—81—7
117—84—0
205—99—2
207—08—9
50—32—8
193—39—5
53—70—3
l91--24—2
10
10
10
10
10
10
10
10
10
10
10
330
330
330
330
330
330
330
330
330
330
330
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
10000
(20)
(20)
(20)
(20)
(20)
(20)
(20)
(20)
(20)
(20)
(20)
252
228
228
149
149
252
252
252
276
278
276
254,126
229,226
226,229
167,279
- -
253,125
253,125
253,125
138,227
139,279
138,277
APPENI)IX II — 13
DRAVF 12/96
-------
Appendix fl OLMO3.2/SY
SAMPLE CONCENTRATION - the amount of analyte present in a sample is calculated using RRF5O of the
COntinuing calibrauori standard in the following equations:
Sample concentration for water:
( A ) (IS) (VC) (DE) (GPO
ug/L = (A 1 ) (RRF) (V 1 ) (V 0 ) -
Sample concentration for low and medium level soil/sediment:
( Ar) (IS) (Va) (Df) (GPC )
ug/icg (Dry weight basis) = (A 19 ) (RRF) (V 2 ) (h’ 3 ) (D)
Where,
A 4 = Area of the pnmary quantitation ion response (EICP) for the compound to be measured
A 4 = Area of the primary quanurauon ion response (EICP) for the specific nterna1 standard
[ S = Amount of internal standard added in nanogranis (ng)
RRF = Relative Response Factor from the most recent continuing caiibrazzon standard
Df = Dilution Factor - The dilution factor for analysis of water and soil/sediment samples for
sernivolatiles by this method is defined as follows:
uL most conc, extract used to make dilution + uL clean solvent
uL most conc. extract used to make dilution
If rio dilution is performed, Df = I.
= Weight of sample extracted in grams (g)
D = 1 00 - % Moisture
100
V 1 = Volume of the concentrated extract in microliters (uL)
V 0 = Volume of water extracted in milliliters (tnL)
V = Volume of extract injected in microliters (uL)
GPC = GPC factor (If no GPC is performed, GPC = 1; if GPC is performed, then GPC = 2.0)
CRQL CALCULATIONS
Water
(V H V..) (V)
Adjusted CRQL = ContractcRQLx
V . / V 2
Where,
V, V 0 , V arid Cf are defined in the sample concentration equation above
V 4 = Contract sample volume (1000 mL
V = Contract injection volume (2 uL)
= Contract concentrated extract vclume (1000 tiE. if GPC is not performed, 500 uL if GPC was
performed).
APPENDIX B -14 DRAFT 12/96
-------
Appendix B OLMO3.2/SV
CRQL CALCULATIONS
Soil/Sediment:
( W) (V) (V) (Df )
Adjusted CRQL = Contract CRQL X ((w) (D)
Where.
V 1 , Df. W 1 , V and D are defined in the sample concentration equation above
W = Contract sample weight (30 g for low level and I g for medium level soil/sediment samples).
V , = Contract injection volume (2 uL)
V = Contract concentrated extract volume (1000 uL if GPC is not performed. 500 uL if GPC wa.s
performed).
SECTION X IV: TENTATIVELY IDENTIFIED COMPOUND CRITERIA
Refer to Region I, EPA- 1E Data Validation Functional Guidelines for Evaluating Envirorimemal Analyses , Part
El, Section VOA/SV-XIv.B for tentatively identified compound (TIC) data validation criteria and the following
method TIC QC criteria:
The validator is required to report up to 30 TICs in the Data Validation Memorandum.
TENTATWELY !DENTJNI D COMPOUND CONCENTLtTION - the estimated concemrauon for non-target
compounds tentatively identified shall be determined by the internal standard method using the following equations:
Sample concentration for water:
- ( Ar) (IS) (Va) (Df) (GPC )
ug/L - (A 5 ) (RRF) (V 1 ) (V 0 )
Sample concentration for low and medium level soil/sediment
- ( AX) (IS) (Va) (Df) (GPC )
ug/Kg - (A. 5 ) (RRF) (V 2 ) (W 5 ) (D)
Where,
= Area of the characteristic ion (EICP) for the non-target compound to be measured
= Area of the characteristic ion (EICP) for the specific internal standard
IS = Amount of internal standard added in nanograms (ng)
RRF = Relative Response Factor is assumed to be 1
Df = Dilution Factor - The dilution factor for analysis of water and soil/sediment samples for
senuvolatiles by this method is defined as follows:
uL most conc. extract used to make dilution + uL clean solvent
uL most conc. extract used to make dilution
If no dilution is performed. Df = I.
W 1 = Wetght of sample extracted in grams (g)
D = 100 - % Moisture
100
V 1 = Volume of the concentrated extract in rmcroliters (uL)
V 0 = Volume of water extracted in milliliters (rnL)
V = Volume of extract injected in nucroliters (uL)
GPC = GPC factor (If no GPC is performed, GPC = 1; if GPC is performed, then GPC = 2 0)
-------
Appendix B 01M03.2ISV
SECTION XV ; SEMIVOLATILE CLEANUP CRITERIA
Refer to Region I. EPA-NE Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
II. Section VOA/SV-XV-B for setnivolattle data validation criteria and the following method semivolaule cleanup
QC criteria:
G PC
lniual GPC calibration consists of analyzing the GPC calibration solution to establish the correct CollectS ’ and
Dump tune periods and a GPC blank to ensure that the system is free of contaminants.
I. The GPC Calibration Solution contains the following analyces in tnethvlene chloride at the
specifled concentrations:
corn oil - 25 0 mg/rnL perylene - 0.02 mg/niL
bis-(2-ethylhexyl)phthalate - 0.5 mg/niL sulfur (optional) - 0.08 mg/niL
rnethoxychlcr - 0.2 mg/niL
2. The GPC blank consists of methylerie chloride.
The GPC must be recalibrated every 7 days with the GPC Calibration Solution followed by a methylene chloride
GPC blank.
Table App B XVI-l - INITIAL AND CONTINUING GPC CALIBRATION CRITERIA
Peak
Resolution
Corn Oil and phthalate peaks must exhibit > 85% reso’ution.
Phthalate and methoxychlor peaks must exhibit > 85% resolution.
Methoxychior and perylene peaks must exhibit > 85% resolution.
Perylene and sulfur peaks (if sulfur was added) must not be samrated
and must exhibit >90% baseline resolution.
Peak Shape
Peaks must be observed and should be symmetrical for all compounds
in the calibration solution.
Retention
Time
The retention times must not vary more than ± 5.0% between
calibrations.
Blanks
A GPC blank must be analyzed after each initial GPC calibration.
Target analytes cannot be present at greater than the CRQL for any
argez analyte except phthalate esters, which must be < 5x CRQL.
SECTION XVI: SYSTEM PERFORMANCE CRITERIA
Refer to Reaton 1 EP 4E Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
II. Section VOA1SV-XVI-B for system performance data validation criteria.
SECTION XVI I: OVERALL ASSESSMENT CRiTERIA
Refer ic Re2Ion I EPA -NE Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
II. Section VOAJSV-XVII-B for overall assessment data validation criteria
APPENDIX B -16 DRAFT 12196
-------
Appendix C
CLP SOW OLCO2. 1/Low Concentration Volatile Organic Analysis
Method QC criteria, Equations, and Definitions
-------
OLCO2.1/VOA
APPENDIX C
The following method QC criter:a. equations, and definitions apply to data generated according to the USEPA CLP
Statement of Work for Organic Analysis, Low Concentration Water, OLCO2.1, Exhibit D Volatjles
Note: MS/MSD are not applicable. MS/MSDs are not required for work under this SOW.
Capillary GC columns are mandatury Packed columns cannot be used.
SECTION I: PRESERVATION & TECHNICAL HOLDING TIME CRITERIA
Refer to Region I EPA-NE Data Validation Functional Guidelines for Evaluating Environme-tal nalvses , Part
II, Section VOA/SV.I-B for preservation and technical holding time data validation crueria.
SECTION II: GCIMS INSTRUMENT PERFORMANCE CHECK (TUNING) CRITERIA
Refer to the following method GC/MS instrument performance (tuning) QC cnteria for data validation
The analysis of the instrument performance (tuning) check solution (50 ng BFB on column) must be performed at
the beginning of each 12-hour period during which samples or standards are analyzed. The tuning check,
bromofluorobe ene (BFB), for volatile analysis must meet the ion abundance crueria given below:
inL ION ABUNDANCE CRITERIA
50 8.0-40.0%ofmJz95
75 30.0 - 66.0% of rnlz 95
95 Base Peak, 100% Relative Abundance
96 5.0 - 9 0% of rnlz 95 (see note)
173 Less than 2.0% of mlz 174
174 50.0 - 120.0% of m/z 95
175 4.0-9 0%ofmass l74
176 93 0 - 101.0% of mlz 174
177 5.0 - 9.0% of mlz 176
NoteS All ion abundances must be normalized to mlz 95, the nominal base peak. even thou n the ion
abundance of mlz 174 may be up to 120% that of m/z 95.
The mass spectrum of BFB must be acquired in the following maimer Three scans (the peak apex scan and the
scans immediately preceding and following the apex) are acquired and averaged. Background subtracuon is
required, and must be accomplished using a single scan no more than 20 scans prior to the elutiori of BFB Part
of the BFB peak must not be background subtracted
APPENDIX C - 1 DRAFr 12/96
-------
Appendix C OLCO2.1/VOA
SECTION UI: INfI1AL CALIBRATION CRITERIA
Refer to Region I. EPA- 4E Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
[ I, Section VOA/SV-III-B for initial calibration data validation criteria and the following method initial calibration
QC criteria:
The initial calibration standards must be analyzed upon contract award, whenever corrective action is taken which
may change or affect the initial calibration criteria or if the continuing calibration acceptance criteria have not been
met. Initial calibrations must be analyzed after the analysis of a compliant instrument performance check.
The initial calibration standards must include the target compounds listed in the Target Compound List (TCL) in
Section XIII of this Appendix, as well as the internal standards and the system monitoring compound.
All initial calibration standards must be analyzed a the following concentration levels; 1.0, 2.0, 5 0, 10, and 25
ug/L except for the ketones which are analyzed at 5.0, 10, 25, 50, and 125 ug/L.
RELATIVE RESPONSE FACTOR (RRF) - A measure of the relative mass spectral response of an analvte
compared to its internal standard. The RRF is calculated using the following equation:
A. C
4115
Where,
A,, = Area of pnmary quantitation ion response (EICP) for the compound to be measured
A,, = Area of primary quantitation ion response (EICP) for the internal standard
C,, = Concentration of the internal standard
C. = Concentration of the compound to be measured
AVERAGE (MEAN) RELATIVE RESPONSE FACTOR (RRF) - The average or mean RRF is determined by
the analysis of five different standard concentrations and is used in calculating a compound concentration in
samples The RRF is calculated using the following equation.
RR
1 1
Where,
RRF, = The individual RRFs for various concentration levels
n = The number of RRFs
APPENDIX C - 2 DRAFT 12/96
-------
Appendix C OLCO2.1/VOA
PERCENT RELATIVE STANDARD DEVIATION (%RSD) - The % RSD for each compound is a measure of
the linearity of the calibration curve. The % RSD is calculated using the following equation:
%RSD = Standard Deviation
Mean
Where,
fn ( _ )2
Standard Deviation = I
N (n—i)
x = Mean
a = total number of values
x, = each individual value used to calculate the mean
SECTION IV; CONTINUING CALIBRATION CRITERIA
Refer to Recion I EPA-NE Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
II, Section VOAISV-IV.B for continuing calibrauon data validation criteria and the following method continuing
calibration QC criteria:
The continuing calibration standard must be analyzed once every 12 hours, following the analysis of a compliant
instrument performance check and initial calibration, and prior to the analysis of field samples, QC samples and
blanks.
The continuing calibration standard must include the target compounds listed in the Target Compound List (TCL)
in Section XIII of this Appendix, as well as the internal standards and the system monitoring compound
Continuing calibrations must be analyzed at a final concentran n of 5 ug/L for non-ketone compounds and at a final
concentration 25 ug/L for the ketones.
Note: The low concentration method % Difference for continuing calibration differs from the Region I
Functional Guidelines continuing calibration % Difference criteria (± 25.0 %). The low concentration method
requires that the continuing calibration % Difference for most target compounds and surrogates be less than
or equal to ± 30.0%. The following compounds do not have a minimum % D requirement but must meet
a minimum RRF criterion of 0.010: carbon disulfide, chloroethane, chloromethane, cis-1,2-dichloroethene,
trans-l,2-dichloroethene, 1,2-dichioropropane, and methytene chloride. Furthermore, OLCO2.1 does not
specify RRF or % D criteria for the following compounds: acetone, 2-butanone, 1,2-dibromo-3-
chloropropane, 2-hexanone, 4-methyl-2-pentanone, and 1,2, -l-trichlorobenzene. (If data quality objectives allow
for greater variability of data, then expanded %D and minimum response factor criteria should be documented ri
the EPA-approved site-specific QAPjP or amendment to the QAPjP If response factors less than 0 05 are ailowed.
then the validator should ensure that there is sufficient QC data to support the use of low RFs in sample calcutations
APPENDIX C - 3 DRAFT 12/96
-------
Appendix C OLCO2.1/VOA
PERCENT DIFFERENCE (%D) - The % D is used to compare the initial calibration mean RRF with the
continuing calibration RRF5. The % Difference indicates both the direction and the magnuude of the comparison,
i e., the % Difference may be either negative, positive or zero.
RRF - RRF
% Difference = c 100
RRFZ
Where,
RRF, = Mean relative response factor from the most recent initial calibration meeting technical
acceptance criteria
RRFC = Relative response factor from continuing calibration standard
SECTION V: BLANK CRITERIA
Refer to Re iori I, EPA-NE Data Validation Functional Guidelines for Eva1uatin Environmental Analyses , Part
II, Section VOA/SV.V.B for blank data validation criteria and the following method QC criteria.
Method Reauired Blanks
1. Method Blank - A 25.0 mL aliquot of reagent water that is carried through the entire analytical process
to determine the levels of contamination associated with the processing and analysis of
samples. All blanks are spiked with internal standards and surrogate compounds and
blank analysis must meet internal standard and surrogate compound criteria. The method
blank must be analyzed at least once during every 12 hour time period on each GC/MS
system used for volatile analysis.
2 Storage Blank - Consists of two 40 ml VOA vials filled with reagent water prepared by the laboratory
when the first samples in the SDG are received. The vials are stored, under the same
conditions, with the field samples. After all the samples in the SDG are analyzed, a 25 0
mL aliquot of the storage blank is analyzed to determine whether contamination was
introduced during storage of the samples. All blanks are spiked with internal standards
and surrogate compounds and blank analysis must meet internal standard and surrogate
compound criteria. A miaimum of one storage blank must be analyzed per SDG after
all samples for that SDG have been analyzed.
3. Instrument Blank - A 25.0 ml aiiquot of reagent water that is carried through the entire analytical procedure
and is analyzed following highly contaminated samples containing target compounds that
exceed the initial calibration range. The instrument blanks are used to determine if
contamination is introduced from a previous sample and the level associated with the
analytical instrument. All blanks are spiked with internal standards and surrogate
compounds and blank analysis must meet internal standard and surrogate compound
criteria. Instrument blanks are analyzed after a samplefdilution which contains a target
compound at a concentration greater than 25 ug/L (ketones 125 ug’L) or a non-target
compound at a concentration greater than 100 ugiL or saturated ions from a compound
(e’ccluding peaks in the solvent front).
APPENDIX C - 4 DRAFF 12/96
-------
Appendix C OLCO2.1/VOA
SECTION VI: SURROGATE COMPOUND CRITERIA
Refer to Region I . EPA-NE Data Validation Functional Guidelines for EvaJuatin Environmental Analyses , Part
I I, Section VOAJSV-VI-B for surrogate compound data validation criteria and the following method surrogate
compound QC criteria:
The proper surrogate compounds must be quantified using the correctly assigned internal stanuards and the correct
primary quantitation ions
The surrogate compound, 4-Brornofluorobenzene , is added to all samples, standards. QC samples, and blanks for
a final concentration of 5 ug/L
Table Apo D Vt-I - CHARACTERISTIC TONS FOR SURROGATE COMPOUNDS
Surrogate
Characteristic Ions
Primary Quantitation Ion Secondary Ion(s) I Internal Standard ]
4 -Brorriouluorobenzene [ 174 95, 176 I , 4 -Difluorobenzene I
The surrogate % recovery is calculated using the following equation:
Surrogate Percent Recovery x 100%
Qd = Quantity of surrogate determined by analysis
Q. = Quantity of surrogate added to sample/blank
Table Aoo D VT-2 - SURROGATE RECOVERY LIMITS
Surrogate
Method QC Criteria
—
Percent Recovery
(Water)
4-Bromofluorobeazene
80-120
Sample reanalysis is required for samples that do nct meet the surrogate recovery acceptance criteria
AJ’PENDIX C - 5
DRAFT 12/96
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Appendix C OLCO2.l/VOA
SECTION VII: INTERNAL STANDARDS CRITERIA
Refer to Region I, EPA-NE Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
II, Section VOA/S V-VU-B for internal standard data validation criteria and the following method internal standard
QC cnceria:
The correct internal standard must be used for sample compound quantication and the correct internal standard
primary quarnitauon ion must be used for quantitation.
The internal standards Bromochloromethane, 1 ,4-Difluorobenzene, and Chlorobenzene4 are added to all samples,
standards, QC samples, and blanks for a final concentration of 5.0 ug/L.
Table App D Vu-I - LOW CONCENTRATION VOLATILE INTERNAL STANDARDS WITH
CORRESPONDING TARGET COMPOUNDS AND SURROGATES ASSIGNED FOR OUANTITATION
IS IS Is
I . 4-Difluorobenzene Chlorobenzene-dc I . 4-Dichlorobenzene-d .
Acetone Benzene Bromoform
Bromochiorornechane Bromodichioromethane I ,2-Dibromo-3-chloropropane
Brornornechane Carbon tetrachloride I,2-Dichlorobenzene
2-Butanone Chlorobenzene I ,3-Dichlorobenzene
Carbon disul tide Dibromochloromethane I ,4-Dich lorobenzene
Chloroechane I ,2-Dibromoethane I ,2.4-Trichlorobenzene
Chloroform 1,2-Dichloropropane
Chloromethane cis- I ,3-Dichloropropene
1,1 -Dichloroechane trans-I ,3.Dichloropropene
I .2-Dichloroethane Ethylbenzene
1, 1-Dichioroechene 2-}-Iexanone
cis- I ,2-Dichloroecherie 4-Methyl-2-pentanone
trans-l,2-Dtch loroechene Styrene
Methvlene chloride 1,1 ,2,2-Tetrachloroethane
Vinyl chloride Tetrachloroethene
Toluerie
1,1,1 -Trichloroethane
4-Bromofluorobenzene 1,1 ,2.Trichloroethane
(surr) Trichloroethene
Xylenes (total)
APPENDIX C - 6 DRAFT 12/96
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Appendix C OLCO2.l/VOA
Table Ann D VII-2 - CHARACTERISTIC IONS FOR INTFRNAL STANflARnc FOR LOW
CONCENTRATION VOLATILE COMPOUNDS
Internal Standard
Characteristic Ions
Primary Quantitation Ion
Secondary Ion(s)
I,4-Ditluorobenzene
114
63. 38
I,4-Dichlorobenzene-d4
152
115, 50
Chlorobenzene-d S
117
82, 119
Internal standard area counts for each of the internal standards must be within the inclusive range of ± 40% of the
respouse of internal standards in the associated daily continuing calibration standard.
The retention time of the internal standard must not vary by more than ± 20 seconds from the retention time of
the associated daily continuing calibration standard.
Sample reanalysis is required for samples that do not meet the internal standard acceptance criteria
SECTION VU]: MATRIX SP [ KEIMATRIX SPIKE DUPLICATE CRiTERIA
The Low Concentration method does not require MS/MSD analysis therefore, no method-specific criteria are
available for MS/MSD. Refer to Region I. EPA-NE Data Validation Functional Guide:ines for Evaluating
Environmental knalvses , Pai-t 11, Section VOA/SV-VllI-B for MS/MSD validation criteria if MS/MSD analyses are
performed
SECTION IX: FIELD DUPLICATE CRITERIA
Refer to Re2ion I EPA-NE Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
11. Section VOA/SV -LX-B for field duplicate data validation criteria.
SECTION X: SENSiTIVITY CHECK CRITERIA
Refer to Re2ion I EP -NE Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
II, Section VOA/SV-X-B for sensitivity check data validation criteria.
APPENDIX C - 7 DRAFT 12/96
-------
Appendix C OLCO2.1/VOA
SECTION X1: PE SAMPLES - ACCURACY CHECK CRITERIA
Refer to Regton 1. EPA-NE Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
II, Section VOAJS V-XE-B for accuracy check data validation criteria and the following method accuracy check QC
criteria:
The LCS is a method-required irnerrial laboratory quality control sample that must be preDared, analyzed and
reported once per SDG. It must be prepared and analyzed concurrently with the samples in the SDG using the same
instrumentation as the samples.
Compound
Final Concentration
ug/L
Method Required
QC % Recovery Limits
Vinyl chloride
5,0
60 - 140
1.2- Dichloroethane
5.0
50 - 140
Carbon tetrachloride
5.0
60. 140
1,2-Dichloroprocane
5.0
60 - 140
Trichloroethene
5.0
60 - 140
1,1.2-Tnchloroethane
5.0
60 - 140
Benzene
5.0
60. 140
cis-1,3-Dichloropropene
5.0
60- 140
Bromoforrn
5.0
60 - 140
Tetrach loroethene
5.0
60 140
1,2-Dibromoethane
5.0
60 - 140
1 ,4-Dtchlorobenzene
5.0
60 - 140
SECTION XII: TARGET COMPOUND IDENTIFICATION CRITERIA
Refer to Region 1, EPA-’IE Data Validation Funcnonr Guidelines for Evaluating Environmental Analyses , Part
11. Section VOAJSV-XII-B for target compound identification data validation criteria.
APPENDIX C - S DRAFt 12/96
-------
Appendix C OLCO2.1/VOA
ECTION XIII: COMPOUND QUANTITATION AND REPORTED QUAI 4TITATION LIMITS CRITERIA
er to Region 1. EPA-NE Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part II, Section VOA/sv.
XllI-B for compound quancicacion and reported quanutauon limit data validation criteria and the following method quancitation QC criteria:
Volatile target compounds must be quancicaced using the internal standard method with the internal standards
assigned in Appendix A, Section VII. The daily RRF5 must be used for saniple quancicacion. The sample target
compounds must be quantified using the following primary quantitation ions and must be reported to the CRQLs listed below.
Table Aop D XIII-) - TARGET COMPOUND LIST (TCLL PRIMARY OUANTITATIONI AND SECONDARY TUNIS AND
CONTRACT REQUIRED OUANTITATION LIMITS (CRQLs FOR OLCO2 0 SOW VOLATILE ORGANIC COMPOUNDS
Quantitation Limits
Low On Characteris c Ions
Water Column Primary Secondary
Volatales CAS Number ugiL (ng)
Chloromethane 74—87—3 1 (25) 50 52
Brcmcchlorometh e 74-97-5 1 (25) 128 49,130
1,2-Dlbromoechane 106-93-4 1 (25) 107 109,188
Bromcmethane 74—83—9 1 (25) 94 96
V.nyl Chloride 75—01—4 1 (25) 62 64
Chicroethane 75—00—3 1 (25) 64 66
Methylene Chloride 75—09—2 2 (50) 84 86,49
Acetone 67—64—]. 5 (125) 43 58
Carhon Disulfide 75—15—0 1 (25) 76 78
l,1—Dichloroethene 75—35—4 1 (25) 96 61,63
l,l—D ich loroethane 75—34—3 1 (25) 63 65,83
.C1Si, 2 —Dlch loroethene 156—59—2 1 (25) 96 61,98
ans-1,2-D1ch1oroethene 156-60-5 1 (25) 96 61,99
1c oform 67—66—3 1 (25) 83 85
, 2 —..ich lorcethane 107—06—2 1 (25) 62 98
2—Bucanone 78—93—3 5 (12S) 43 72
l,l.l—Trichlcroethane 71—55—6 1 (25) 97 99,61
Carnon Tetrachioride 56—23—5 1 (26) 117 119
Brcmcdlch lorome.-hane 75—27—4 1 (25) 83 85,127
l, 2 —Dichloroprcca n 78—87—5 1 (25) 63 112
cis—:, 3 —Dlchloroproperie 10061—01—5 1 (25) 75 77
Tric 1orcethene 79—01—6 1 (25) 95 130,132
Di rc ioch1orcmethane 124—48—1 1 (25) 129 127
1, ., 2 —Trichj.oroe hane 79—00—5 1 (25) 97 83,85,99,132,134
Benzene 71—43—2 1 (25) 78 - -
10061—02—6 1 (25) 75 77
Bromoform 75—25—2 1 (25) 173 175,254
4 — .lethvl—2—pentanone 108—10—1 5 (125) 43 58,100
2—Hexarione 591—78—6 5 (125) 43 58,57,100
Tetrachloroethene 127—18—4 1 (25) 166 168,129
Toluene 108—88—3 1 (26) 91 92
l ,l. 2 , 2 —Tetrachloroethane 79—34—5 1 (25) 83 121,85
l 2 , 4 -Trich lorobenzene 120-82-1 1 (25) 180 182,145
l , 2 -D lch lorcbenzene 9 5- 50-1 1 (25) 146 111,148
l,]-Cicnlorobenzene 541-73-1 1 (25) 146 :11,148
l,4-Dlchlorobenzene 106-46-7 1 (5) 146 ::1,148
Ch lorcbenzene 108—90—7 1 (5 112 77,114
Ethyibenzene 100—41—4 1 (25, 91 106
St- irene 100—42—S 1 (25) 104 78
Xvlenes (Tctai) 1330—20—7 1 (25) 106 91
l. 2 -D1 romo-3-ch1croprcpane 96-12-8 1 (25) 75 155,157
rn/z 43 is used fcr uan::tat:cn of 2-Butancr.e, but m/z 72 must ce present for posit:7e
ric:f:cat:on.
APPENDIX C - 9 DRAFT 12/96
-------
Appendix C OLCO2.l/VOA
SAMPLE COtiCENTRATION - The amount of analyte present in a sample is calculated using the RRF5 of the
concrnuing calibration standard in the following equanon:
Sample concentration for water:
(AX) (IS) (Df)
ug/L = (A 25 ) (RRF) (V 0 )
Where,
A 3 = Area of the pnmary quantitatiori ion response (EICP) for the compound o be measured
A 3 = Area of the primary quantitation ion response (EICP) for the specific internal standard
IS = Amount of internal standard added in nanograms (ng)
RRF = The Relative Response Factor from the most recent continuing calibration standard
V 0 = Total volume of water purged in milliliters (mL)
Df = Dilution Factor- The dilution factor for analysis of water samples for volatiles by this method is
defined as the ratio of the number of milliliters (mL) of water purged (i.e., V 0 above) to the
number of rnL of the onginal water sample used for purging. If no dilution is performed, Df= 1.
CRQL CALCULATIONS
Water:
( V )
Adjustth CRQL = Contract CRQL x x WE)
‘ 0
Where,
V 0 and Df are defined in the sample concentration equation above
V , = Contract sample volume (5 to 25 mL)
APPENDIX C - 10 DRAFI’ 12/96
-------
Appendix C OLCO2.1IVOA
SECTION XIV: TENTATIVELY IDENTIk LED COMPOITrfl) CRiTERIA
Refer to Region I, EPA-’IE Data Validation Functional Guidelines for Evaluating Environrnernaj Analyses , Part
II, Section VOA/SV-XIV-B for tentauvely identified compound (TIC) data validation criteria and the following
method TIC QC criteria:
The validacor is required to report up to 30 TICs in the Data Validation Memorandum.
TENTATIVELY WEN1’WIED COMPOUND CONCENTRATION - the estimated concentration for non-target
compounds tentatively identified shall be determined by the internal standard method using the following equations.
Sample concentration for water:
— ( Ar) (IS) (Dt )
ug, - (& ) (RRF) (VJ
Where,
A 2 = Area of the primary quanticauon ion response (EICP) for the non-target compound to be measured
A 0 = Area of the primary quanutation ion response (EICP) for the specific internal standard
IS = Amourn of internal standard added in nanograrns (ng)
RRF = Relative Response Factor assumed to be 1
V 0 = Total volume of water purged in milliliters (niL)
Df = Dilution Factor - The dilution factor for analysis of water samples for volatiles by this method is
defined as the ratio of the number of milliliters (mL) of water purged (i e., V 0 above) to the
number of niL of the original water sample used for purging. If no dilution is performed Df= 1
SECTION XV: SEMJVOLATrJ E CLEANUP CRITERIA
Not applicable o low concentration volatile analysis.
SECTION XVI: SYSTEM PERFORMANCE CRITERIA
Refer to Region I EPA-NE Data Valicacien Functional Guidelines for Evaluating Environmental Analyses , Part
11, Section VOA,SV-XVl -B for system performance data validation criteria.
SECTION XVII: OVERALL ASSESSMENT CRITERIA
Refe: to Region I EP - 4F Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
II. Section VOA/SV-XVII B for overall assessment data validation criteria.
APPENDIX C - 11 DRAFT 12/96
-------
Appendix D
CLP SOW OLCO2. 1/Low Concentration Semivolatile Organic Analysis
Method QC criteria, Equations, and Definitions
-------
OLCO2. 1/SV
APPENDIX D
The following method QC criteria, equations, and definitions apply to data generated according to the USEPA CLP
Statement of Work for Organic Analysis, Low Concentration Water, OLCO2. 1, Exhibit D Semivolatiles.
Noe MS/MSD are not applicable. MS/MSDs are not required for work under this SOW.
Capillazy GC columns are mandatory. Packed columns cannot be used.
SECTION I: PRESERVATION & TECHNICAL HOLDING TIME CRiTERIA
Refer to Region I EPA-NE Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
II. Section VOA/SV-I-B for preservation and technical holding time data validation criteria.
SECTION II: GCIMS INSTRUMENT PERFORMANCE CHECK (TUNiNG) CRITERIA
Refer to the following method CC/MS instrument performance (tuning) QC criteria for data validation:
The analysis of the instrument performance (tuning) check solution (50 ng DFTPP on column) must be performed
at the beginning of each 12-hour period during which samples or standards are analyzed. The tuning check,
decafluorotriphenylphosphme (DFTPP), for sernivolanle analysis must meet the ion abundance cnter a given beIow
ir iL ION ABUNDANCE CRITERIA
51 30.0- 80.0% of rnlz 198
68 Less than 2.0% of miz 69
69 Present
70 Less than 2.0% of mlz 69
127 25.0 - 75 0% of m/z 198
197 Less than 1.0% of mlz 198
198 Base Peak, 100% Relative Abundance (see note)
199 5.0-90%ofrr iiz l98
275 10.0 - 30 0% of mlz 198
365 Greater than 0.75% of wlz 198
441 Present, b’ less than mlz 443
442 40.0- 110.0% of rniz 198
443 15.0 - 24 0% of mlz 4.42
Note All ion abundances must be normalized to miz 198, the nominal base peak, even though the ion abundances
of miz 442 may be up to 110% that of rnlz 198
The mass spectrum of DFTPP must be acquired in the following manner. Three scans (the peak ape’t scan and the
scans immediately preceding and following the apex) are acquired and averaged. Backgrounit subtraction is required
anc must be accomplished using a single scan no more than 20 scans prior to the eluuon or DFTPP Part of the
DFTPP peak must not be background subtracted
.. PPENDLX D - 1 DRAFT 12/96
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Appendix D OLCO2.l/SV
SECTION III: INITIAL CALIBRATION CRITERIA
Refer to Region I EP - 4E Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
I I. Section VOA1SV-III-B for initial calibration data validation criteria and the following method initial calibration
QC criteria:
The initial calibration standards must be analyzed upon contract award, whenever corrective action IS taken which
may change or affect the initial calibration criteria or if the continuing calibration acceptance criena have not been
met. Initial calibrations must be analyzed after the analysis of a compliant instrument performance check.
The initial calibration standards must include the target compounds listed in the Target Compound List (TCL) in
Section XIII of this Appendix, as well as the internal standards and the system monitoring compounds.
1 uL volume of the initial calibration standard must be injected and all initial calibration standards must be analyzed
a the following concentration levels; 5.0, 10, 20, 50, and 80 ngiuL except for eight target compounds and one
surrogate compound. Compounds 2,4-dinitrophenol. 2.4 ,5-trichlorophenol, 2-niroaniline, 3-nnroaniline, 4-
nitroaniline, 4-mcrophenol, 4-6-dinitro-2-methvlphenol, pentachiorophenol, and 2 ,4 ,6-cribrornophenol(surr.) must
be analyzed at 20, 50, 80, 10, and 120 ng/uL.
RELATIVE RESPONSE FACTOR (RRF) - A measure of the relative mass spectral response of an analyte
compared to its internal standard. The RRF is calculated using the following equation:
A C
RRF=-- -x-
L.X
Where,
A, = Area of primary quantitation ion response (EICP) for the compound to be measured
A, = Area of primary quancication ion response (EICP) for the internal standard
C,, = Concentration of the internal standard
C, = Concentration of the compound to be measured
AVERAGE (MEA.N) RELATIVE RESPONSE FACTOR (RRF) - The average or mean RRF is determined by
the analysis of five different standard concentrations and is used in calculating a compound concentration in samples.
The RRF is calculated using the following equation:
‘ RR’
n
Where,
RRF = The individual RRFs for various concentration levels
n = The number of RRFs
APPENDIX D - 2 DRAFT 12/96
-------
Appendix D OLCO2.L/SV
PERCENT RELATIVE STANDARD DEVIATION (%RSD) - The % RSD for each compound is a measure of
the linearity of the calibration curve. The % RSD is calculated using the following equanoir
%RSD = Standard Deviation
Mean
Where,
[ n ( x _ ) :
Standard Deviation = 1
N (n—i)
x = Mean
a total number of values
= each individual value used to calculate the mean
SECTION IV: CONTINIJING CALIBRATION CRITERIA
Refer to Re2ion 1. EPA-NE Data Validation Functional Guidelines for Evaiuatin Environmental Analyses Part
II, Section VOA/SV lV.B for continuing calibration data validation cnteria and the following method continuing
calibration QC critena:
The continuing calibrac on standard must be analyzed once every 12 hours, following the analysis of a compliant
instrument performance check and initial calibration, and pnor to the an lysis of field samples, QC samples and
blanks.
The continuing calibration standard must include the target compounds listed in the Target Compound List (TCL)
in Section XIII of this Appendix, as well as the internal standards and the system monitonng compounds
Continuing calibration standards must be analyzed at a final concentration of 20 ug/L for the majontv of the
compounds and 80 ug/L for the eight compounds specified in the initial calibration section
Note: The Low Concentration method % Difference QC criteria for continuing calibration differs somewhat
from the Region I Functional Guidelines continuing calibrati % Difference criteria. The Low Concentration
method requires that the continuing calibration % Differ :e be less than or equal to ±30.0% for two
corn pounds. 2 -nitrophenol and 2,4,-dimethvlphenol; whereas ie Functional Guidelines requires qualification
of all data associated with a continuing calibration with % Difference greater than ± 25.0%. Refer to CLP
SOW OLCO2.I for those compounds that do not have % D requirements. If data quality objectives allow for
greater variability of data, then expanded % D validation criteria should be documented in the site-specific QAPJP
or amendment to the QAPJP.
APPENDIX D - 3 DRAFT 12,’96
-------
Appendix D OLCO2.1/SV
PERCENT DIFFERENCE (%D) - The D is used to compare the intual calibranon mean RRF with the
continuing calibration RRF. The % Difference indicates both the direction and the magnitude of the comparison,
i.e.. the % Difference may be either negative, positive or zero.
RRF - RRF
% Difference = C 1 x 100
RRF 1
Where,
RRFi = Mean relative response factor from the most recent initial calibration meeting technical
acceptance criteria
RRFc = Relative response factor from continuing calibration standard
SECTION V: BLANK CRITERIA
Refer to Region 1, EPA-NE Data Validation Functional Guidelines for Evaluating Environmernal Analyses , Part
II, Section VOA/SV-V-B for blank data validation criteria and the following method QC criteria:
Method Required Blank
Method Blank - A volume of reagent water approximate in volume to the samples which is camed through the
entire analytical process to determine the levels of contamination associated with the processing
and analysis of the samples. All blanks are spiked with internal standard and surrogate
compounds and blank analysis must meet internal standard and surrogate compound criteria. A
method blank must be extracted at least once for every SDG, for each 20 samples in an SDG, and
whenever samples are extracted. Each method blank must be analyzed on each GCIMS used to
analyzed the samples prepared with the method blank.
SECTION VI: SU1 ROGATE COMPOUND CRITERIA
Refer to Reg!on I EPA-NE Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
II, Section VOA/SV-VI-B for surrogate compound data validation criteria and the following method surrogate
compound QC criteria:
Surrogate compounds must be quantified using the correctly assigned internal standards and the correct primary
quantitauon ions.
Surrogate compounds Nicrobenzene-d 5 , 2-Fluorobiphenyl. Terphenyl-d 1 , Phenol-d 5 , and 2-Fluorophenol are added
o all sarnoles, standards, QC samples. and blanks at a concentration of 40 ug/mL and surrogate compound 2,4,6-
Tribromophenol is added to all samples. standards. QC samples, and blanks at a concentration of 120 ug’mL
APPENDIX D - 4 DRAFT 12/96
-------
Appendix D OLCO2.I/SV
Table App E VT-I - CHARACTERISTIC IONS FOR SURROGATE COMPOUNDS
Surrogate
Characteristic Ions
Internal Standard
Primary Quantitation Ion
Secondary Ion(s)
N itrobenzene-d 5
82
128, 54
Na hthaIene-d
2-Fluorobiphenyl
172
171
Acenaphthene-d 10
Terphen ’l-d 14
244
122, 212
Ch iysene-d.,
Phenol-d ,
99
42, 71
1,4-Dich1orobenzene-d
2-Fluorophenol
112
64
1 ,4-Dichlorobenzene.d 4
2.4,6-Thbromopheno l
330
332. 141
Phenanthrene-d 10
The surrogate % recovery is calculated using the folloving equation:
Surrogate Percent Recovery = - x 100%
Q 4 = Quantity of surrogate determined by analysis
= Quantity of surrogate added to sample/blank
Table APO E V!-2 - SURROGATE RECOVERY LIMITS
Surrogate
Method QC Criteria
Percent Recovery
(Water)
Nitrobenzene-d,
40-110
2-Fluorobiphenvl
30-110
Terphenvl-d 4
20-140
Phenot-d 5
15-1 15
2-Fluorophenol
— 2.4,6-Tribromoohenol
15-110
15-130
If the surrogate acceptance criteria are not met, the laboratory should check calculat:cns, surrogate standard
sotutions, and instrument performance. If the failed criteria are the result of instrument malfunction, only sample
reanalysis is required to meet surrogate acceptance criteria. Sample re-extracuonlreanalvsis is required for samples
that do not meet the surrogate recovery acceptance cnteria, as a result of the incorrect surrogate standard solutions
or awi other unknown problem.
APPENDIX D - 5 DRAFT 12/96
-------
Ap 1 iidix OLCO2.l/SV
SECTION VII: INTERNAL STANDARDS CRITERIA
Refer to ji g! !LL..EPA-NE Data idation Fii cionat_c,u Ii or Evalu lug Environmental Analyses , Part II, Section VOA/SV-VII-B for internal standard
41. 11.1 v.ilid .tt ion criteria and the following inetliotl uiHeri I. l stantl .uid QC cnlerua.
The correct iniernal standard must be used for sample compound quantification and the correct internal standard primary quamitation ion must be used for
I .111111 al IOU
The internal standard compounds liste(l below are inlected into all samples, standards, QC samples, and blanks at a concentration of 20 ng/uL.
App E VII-l - LOW CONCENTRATION SEMIVOLATILE INTERNAL STANDARDS WITh CORRESPONDING TARGET COMPOUNDS AND
SURROGATES ASSIGNED FOR QIJANTITATION
IS IS IS IS IS is
I A — Dichloi-oheniene—d4 j j Ihaknc—d8 Acenaphihene—d 10 Phenanthrene—.d 10 Chrysene—.d 12 Perv1ene— d 12
Phenol Nitrobenzene Ilexachiorocyclo— 4,6—Dinitro—2— Pyrene Di—n---octyl-
bis(2—Chloroeihyl) Isophorone pentadiene methyiphenol Butylbenzy l- phtha laie
ether 2—Nitroplienol 2,4 ,6—Trichloro— N—niiroso-d,— pluhalate flenzo(b)fluior—
2—Chiorophenol 2 ,4—Dimethyl— phenol phenylamine 3,3’—DichIor — anihene
2-Meihyiphenol phenol 2,4 .5—Tric hioro— 4—Bromophenyl benzidine Benzo(k)fluor—
2.2-oxyh ts- bis(2—Chloro— phenol pheutoletlier Benzo(a)— anihene
(I -Chloropropane) ethoxy)methane 2—Chloronaphthalene I lexachioro— anthracene Benzo(a)pyrene
4—Mei liylphenot 2 ,4—Ducliloro— 2—Ni troaniline benzene bis(2— .ethyl- Indeno(l .2 3—cd)-
N-N umroso-I)u-n- phenol Dimeihylphilialate Peniachloro— hexyl)phihalate pyrene
propylamine Naphtlialene Acenaphihylene phenol Chrysene Dibenz(a h)-
I lexachioroethane 4-Chioroaniline 3—Nitroaniline Phenanthrene Terphenyl—d 14 anthracene
2-Fluorophenol Ilexachloro— Acenaplitliene Amliracene (surr) I3enzo(g,Ii i)-
(sun) btiiadiene 2 ,4—Dmiiroplienol Di-n-butyl- perylene
Pl uenol-tl5 4—Chloro——3— 4—Nitrophenol pluhalate
(surr) meihyiplienol Dibenzofuran Flimoranthene
2-Mei liylnaph- 2 .4—Dinitrotoluene 2.4 .6-Tribromo.
ih .ulcne 2 .6—Dinitrotoluene phenol (surr)
Nun abet u tene—d5 I) mci hy I phiha late
(surr) -1—Clilorophenyl-
plienyleilier
Ft imorene
4—Nit roan i line
2—I ’luorohiphenyl
(surr)
(sun) = sun agate compound
APPITh ‘ D - 6 DRAFT
-------
Appendix D OLCO2.1/SV
Table App E.VTI-2 - CHARACTERISTIC IONS FOR INTERNAL STANDARDS FOR LOW
CONCENTRATION’ SEMIVOLATILE COMPOUNDS
Internal Standard
Characteristic Ions
Primary Quantitation Ion
Secondary Ion(s)
1,4-Dichloroben.zene-d 1
152
115
Naphtha1ene-d
136
68
Acenaphthene-d 0
164
162. 160
Phenanthrene-d!Q
188
94, 80
Chrysene-d 1
240
120, 236
Perylene-d 1 ,
264
260, 265
Internal standard area counts for each of the internal standards must be within the inclusive range of - 50% and +
100% of the response of internal standards in the associated daily continuing calibration standard.
The retention time of the internal standard must not vary by more than ± 20 seconds from the retention time of
the associated daily continuing calibration standard
If the internal standard acceptance criteria are not met, the laboratory should check calculations, internal standard
solutions, and instrument performance. If the failed criteria are the result of instrument malfunction, only sample
reanalysis is required to meet surrogate acceptance criteria. Sample reanalysis is required for samples that do not
meet the internal standard acceptance criteria, as a result of the incorrect internal standard solutions or any other
unknown problem.
SECTION s /rn: MATRIX SPIKEIMATRIX SPIKE DUPLICATE CRITERIA
The Low Concentration method does not require MSIMSD analysis therefore, no method-specific criteria are
available for MS/MSD Refer to Region I EPA- IE Data Validation Functional Guidelines for Evaluating
Environmental Analyses , Part II, Section VOAISV-VIII-B for MS/MSD validation criteria, if MSIMSD analyses
are perfo—ned.
SECTION IX: FIELD DUPLICATE CRITERIA
Refer to Reeton I EPA-NE Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
II. Section VOA/SV-IX-B for field duplicate data validation criteria
SECTION X: SENSITIVITY CHECK CRITERIA
Refer to Rea’ori I EP -NE Data Validation Functional Guidelines for Evaluating Environmental Anaivses , Part
II. Section VOAISV-X-B for sensitivity check data validation criteria
APPENDIX D -7 DRAFT 12/96
-------
Appendix D OLCO2J/Sv
SECTION X I: PE SAMPLES - ACCURACY CHECK CRITERIA
Refer to Region 1, EPA-”4E Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
11. Section VOA/SV-XI-B for accuracy check data validation criteria.
The LCS is a method required internal laboratory quality control sample that must be prepared, analyzed and
reported once per SDG. ft must be prepared and analyzed concurrently with the samples in the SDG using the same
instrumernation as the samples.
Compound
Final Concentration
ug/L
Method Required QC %
Recovery Limits
Phenol
40.0
40- 120
2-Chlorophenol
40 0
50 - 110
4-Cb.loroaniline
40.0
10 - 120
2,4,6-Trichlorophenol
40.0
40 - 120
bis(2-Chioroethvl)ether
20.0
50 - 110
N-Nitroso-di-n-propylarmne
20.0
30 - 110
Hexach loroethane
20.0
20 - 110
Isophorone
20.0
50 - 110
Naphthalene
20.0
30 - 110
2,4-Dinitrocoluene
20.0
30 - 120
Diethylphthalate
20 0
50- 120
N-Nicrosodiphenylarmne
20 0
30 - 110
Hexachiorobenzene
20.0
40 - 120
Benzo(a)pyrene
20.0
50 - 120
SECTION Xfl: TARGET COMPOUND IDENTIFICATION CRITERIA
Refer to Re2Ion 1. EPA-NE Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part
II, Section VOAJSV-XII.B for target compound identification data validation criteria.
APPENDIX D - S DRAFr 12/96
-------
Appendix D OLCO2.1ISV
SECTION XIII: COMPOUND QEJANTITATION AND REPORTED QUANTITATION LIMIT CRITERIA
Refer to Region 1, EPA.NE Data Validation Functional Guidelines for Evaluaung Environmental Analyses , Part
II. Section VOA/SV-XIlI-B for compound quancitatton and reported quanutation limit data validation criteria and
the following method quantitation QC criteria:
Sernivolaule target compounds must be quarnuated using the internal standard method with the irne—ial standards
assigned in Apoendix E, Section VII. The daily RRF2O must be used for sample quantitation. The sample target
compounds must be quantified using the following primary quanticauon ions and must be reported to the CRQLs
listed below
Aoo E XII!-l - TARGET COMPOUND LIST (TCL’I . CONTRACT REQUIRED OUANTITATION LIMITS
LCROLs’i PRIMARY QUANTITATEON EONS. AND SECONDARY IONS FOR OLCO2 0 sow
SEMIVOLATILE ORGANIC COMPOUNDS
Quancitation Limits
Water Characteristic Ions
Semivolaules CAS Number ug/L Primary Secondary
Phenol 108—95—2 5 94 65, 66
bist .2—Chloroethyl) ether 111 14 1 5 93 63, 95
2—Chioropheriol 95—57—8 128 64, 130
2—Methytphenol 95—18—7 5 108 107
2,2’-oxybis
(l-Chloropropane)# 108—60—1 5 45 77. 79
4—Methyiphenol 106—44——5 5 108 107
N—Nitroso—di—n-
propylamine 621—64--—7 5 70 42, 101, 130
Hexachloroethane 67—72—1 5 117 201, 199
Nicrobenzene 98—95—3 5 77 123, 65
Isophorone 78—59——I 5 82 95, 138
2—Nurophenol 88—75—5 5 139 65. 109
2 .4—Dimethvlpbeno l 105—67—9 5 107 121, 122
bts(2—Chloroethoxv)
methane 111—91—1 5 93 95. 123
2,4—Dichiorophenol 120—83—2 5 162 164. 98
Naphthalene 91—20——3 5 128 129. 127
4—Chloroani line 106—47—8 5 127 129
Hexachlorobutadiene 87—68—3 5 225 223, 227
4 —Chloro—-3—methy!phenol 59—50—7 5 107 144, 142
2 —Methylnaphthalene 91—57——6 5 142 141
I-Ieuchlorocvc lopentadiene 777 237 235 272
2 . 4 ,&—Trichloropheno l 88—06—2 5 196 198, 200
2,4,5—Tnchloropheriol 9595_...4 20 196 198, 200
2—Chloronaph na1ene 91—58—7 5 162 164, 127
2—Nitroaniline 88—74—•-4 20 65 92, 138
Dtme:hv lphrhaiae 131—11—3 5 163 194. 164
Acenaohthvlene 208—96—8 5 152 151, 153
2 .6—Dinitroto luene 606—20--—2 5 165 89, 121
3—Nicroantline 99—09—2 20 138 108, 92
Ac napnthene 83—32—9 5 153 152, 154
2,4—Dinitrophenol 51—23—5 20 184 63. 15
# Previously known by the name bis(2-Chloroisoproovl) ether
APPENDIX D - 9 DRAFT 12/96
-------
Appendix D OLCO2.1/SV
ADD E.XIII-1 - TARGET COMPOUND LEST ( TCL). CONTRACT REQUIRED OUANTITATION LIMITS
( CROLs), PRIMARY QUANTITATTON IONS. AND SECONDARY TONS FOR OLCO2. SOW
SEMIVOLATTLE ORGANIC COMPOUNDS (CONT )
Quantitation LImitS
Water Characteristic Ions
Semivo auIes CAS Number ug/L Primary Secondary
4—Nitrophenol 100—02—7 20 109 139, 65
Dibenzofuran 132—64--—9 5 168 139
2,4—Dinitrocoluene 121—142 5 165 63, 182
Diethy lphthalae 84—66——2 5 149 177, 150
4—Chloropheny l — —pheny lether 7005—72—3 5 204 206, 141
Fluorene 86-73—7 5 166 165, 167
4—Nicroanflmne 100—01---6 20 138 92, 108
4 .6.—Dinicro—2—methy lpheno l 534—52—1 20 198 182, 77
N—nicrosodmpheny lamine 86—30—--6 5 169 168, 167
4—Bromophenyl—phenylether 101—55—3 5 248 250, 141
Hexachlorobenzene 118—74-—i 5 284 142. 249
Pencachiorophenol 87—86——S 20 266 264, 268
Phenanthrene 85—01—8 5 178 179, 176
Anthracene 120—12—7 5 178 179, 176
Di—ri--—bucylphtha late 84—74—-2 5 149 150, 104
Fluoranchene 206 14—0 5 202 101. 100
Pyrerie 129—00-—0 5 202 101, 100
Bucy lbenzy lphthaiace 85—68-7 5 149 91, 206
3,3’—Dich lorobenzidine 91—94——I 5 252 254, 126
Benzo(a)anchracerie 56-553 5 228 229, 226
Chrvsene 218—01—9 5 228 226, 229
bis(2—EthyIhe’ y1)phtha1ace 117-81—7 5 149 167, 279
Di—n——octylphiha lace 1 17—84——0 5 149
Ben.zo(b)fluoranthene 205—99—2 5 252 253, 125
Be izo(k)fluoranthene 207-08—9 5 252 253, 125
Ber .zo(a)pyrene 50—32—--8 5 252 253. 125
Indeno(1,2,3 .—cd)p rene 193—39—5 5 276 138, 227
Dmbenz(a,h)anthracene 53—70—3 5 273 139, 279
Benzo(g,h .i)perylene 191—24——2 5 276 138, 277
AJ’PEND [ X D - 10 DRAY!’ 12/96
-------
Appendix D OLCO2. 1ISV
SAMPLE CONCENTRATION - The amount of analyte present in a sample is Calculated using the RRF2O of the
continuing calibration standard in the following equation:
Sample concentration for water:
- ‘ X ) (IS) (Va) (Df )
ug/L - (As) (RRF) (V 0 ) (V.)
Where,
A = Area of the primary quancitacion ion response (EICP) for the compound to be measured
A = Area of the pnmary quantitacion ion response (EICP) for the specific internal standard
IS = Amount of wcernal standard added in nanograms (ng)
RRF = The Relative Response Factor from the most recent continuing calibrauon Standard
Df = Dilution Factor - The dilution factor for analysis of water samples for semivolatijes by this method
is defined as follows:
uL most conc extract used to make dilution + uL clean solvent
uL most conc. extract used to make dilution
If no dilution is performed, D I 1.
V 1 = Volume of the concentrated final extract in microliters (uL)
V 0 = Volume of water extracted in milliliters (rnL)
V Volume of extract injected in microliters (uL)
CRQL CALCULATIONS
Water.
Adjusted CROL = Contract C’RQL (Va) (Vp) (Df )
(TI 0 ) (TIe) (V,)
Where
V 1 , V 0 , V and Df are defined in the sample Concentration equation above
V Contract sample volume (1000 rnL)
V , = Contract injection volume (I uL)
V = Contract concentrated extract volume (1000 uL)
APPENDIX D- 11 DRAFr 12/96
-------
Appendi’ D OLCO2. IJSV
SECTION XIV: TENTATIVELY IDENTIFIED COPI’LPOUND CRITERIA
Refer to Region I, EPA-RE Data Validation Functional Guidelines for Evaluating Environinentaj Analyses , Part
II. Section VOA/SV-XIV-B for tentatively identified compound (TIC) data validation criteria and the following
method TIC QC criteria:
The validator is required to report up to 30 TICs in the Data Validation Memorandum.
TENTATIVELY 1DENTLH1 D COMPOUND CONCENTRATION - the estimated concentration for non-target
compounds tentatively identified shall be determined by the internal standard method using the following equauons:
Sample concentration for water:
- ( As) (IS) (Va) (DE )
ug/L - (A:g) (RRF) (V 0 ) (Vi)
Where,
A = Area of the primary quantitacion ion response (EICP) for the non-target compound to be measured
A, = Asea of the primary quanhitacion ion response (E [ CP) for the specific internal standard
IS = Amount of internal standard added in nanograms (ng)
RRF = Relative Response Factor of 1 (one) is assumed
Df = Dilution Factor - The dilution factor for analysis of water samples for senaivolatiles by this method
is defined as follows:
uL most conc. extract used to make dilution + uL clean solvent
uL most conc. extract used to make dilution
If no dilution is pci-formed, Df = 1.1
V 1 = Volume of the concentrated final extract in nucroliters (uL)
V 0 = Volume of water extracted in milliliters (mL)
V = Volume of extract injected in microliters (uL)
SECTION XV: SEMIVOLATILE CLEANUP CR ITERIA
Not applicable to low concentration sernivoiatile analysis.
SECTION XVI: SYSTEM PERFORMANCE CRITERIA
Refer to Re ion I, EPA-NE Data Validauori Functional Guidelines for Evaluating Environmental Majvses Part
Ii, Section VOAISV-XVI-B for system performance data validation criteria
SECTION XVII: OVERALL ASSESSMENT
Refer to Re2ion I EpA .NE Data Validation Functional Guidelines for Eva1uatin Environmental Analyses , Part
II. Section VOA/SV-XVII-B for overall assessment data validation criteria.
APPENDIX D - 12 DRAFI 12/96
-------
Appendix E
VOA/SV Functional Guidelines Action Tables
Note: This appendix is a compilation of the data validation actions that appear in tabular format
in Part II - VOLATILE/SE VH VOLATILE Data Validation Functional Guidelines. Other actions
that are presented in tabular format are not Contained in this appendix and the validator must
refer to Part II to obtain the complete set of actions.
-------
VOAJSV ACTION TABLES
APPENDIX E
Table VOAJSV-I-l:
QUALIFICATION OF VOLATILE ANALYTES BASED ON
PRESERVATION & TECHNICAL HOLDING TIMES
PRESERVATION
TECHNICAL H
OLDING TTMES 1]
Matrix
Rei’n Sc
Light
Protected
Acid
Preserved
7
Days
7 < HT 14
Lays
14 < HT 23
Days
> 28 Dav
AQ
No
Yes or No
I - detects
R-non-deieczs
J - detect.s
R•non-detects
I - detects
R -non-detects
I - detects
R-non-detecLs
AQ
Yes
Yes
A
A
3 detects
I detects
UJ- ’ion-detects
R-non-detects
Aromaucs
Aromatics
I - detects
3 detects
AQ
Yes
No
A
R-non -detects
R-non-detects
I - detects
Nori-aroenatics
Nori-aromatics
R-non - ietects
A - detects
I - detects
A-non-detects
UI-non-detects
S/S
No
N/A
I- detects
R-non-deteczs
I - detects
R-non-detects
—
I - detects
R-non-de ects
I - detects
R-non-detccts
S/S
Yes
N/A
A
A
—
J - detects
I detects
UI-non - etects
R-non-dete:a
Table VOA/SV-I-2:
QUALIFICATION OF SEM1VOLATTLE ANALYTES BASED ON
PRESERVATION & TECHNiCAL HOLDING TiMES
PRESERVATION
TECHNICAL HOLDING TIMES
Matrix
Refng & Ligh
Protected
Extracted
andior
Extracted
and/or
If Extraction HT > 28 days
and/or
Analyzed
Within H T
Analyzed
Outside H.T
Analytical HT > 60 days
J - detects
J - detects
AQ and S/S
Yes
A
UJ - non-detects
R - non-detects
AQ and S/S
No
J - detects
J - detects
J - detects
UJ non-detects
UJ - non-detects
R - non-detects
Note AQ = Aqueous, S/S = Soil/Sediment
For other matrices, the validator should estimate (J) positive detects and use professional judgment
to qualify or reject non-detects when Region I preservation and/or technical holding time criteria are not met.
For VOA aqueous saino es containing excessive headspace (bubbles greater than 2 mm in diameter), J-detects, R-non-deteCts
APPENDIX E - 1 DRAFT 12/96
-------
APPENDIX E VOA/SV ACTION TABY
Table VOA/SV4II- 1
QUALIFICATION OF VOA/SV A.NALYTES BASED ON THE rNITIAL CALIBRATION
Sample Results
QC Criterion
0.05
%RSD 30.0%
Situation 1
RRF <0 05
%RSD 30.0%
Situation 2**
RRF 0.05
%RSD >30.0%
Situation 3
RRF < 0.05
%RSD > 30 0%
Detects
A
J
J
j
Non-detects
A
R f
W
R
See Table VOA/SV-llI-2 for additional guidance.
Table VOA/SV-!Il-2:
EXPANDED INITIAL CALIBRATION VOA/SV ANALYTE OUALWICATIONS
Sample Results
Elimination of
Elimination of
Elimination of
High or Low
Calibration
High
Calibration
Low
Calibration
Points
Points
Points
%RSD > 30.0%
% fl 30.0%
%RSD 30.0%
RRF 0.05 —
RRF 0.05
Detects
J
A: On linear
A: On linear
portion of curve
portion of
curve
On high end of
curve outside
J: On low end of
linear portion
curve outside
linear portion
Non-detects
UJ
A
UJ
Table VOA/SV-IV- 1:
QUALIFICATION F VOA/SV AiNALYI’ES BASED ON THE CONTINUING CALIBRATION
Sample Results
QC Criteria
RRF 0.05
%D ± 25.0%
Situation 1
RRF <005
%D ± 25.0%
Situation 2
RRF 0.05
%D> ± 25.0%
Situation 3
RRF <005
%D> ± 25.0%
Detects
A
J
J I
Non-Detects
A
R
UJ R
APPENDIX E - 2 DRAfl’ 12/ .
-------
APPENDC( E
Table VOA/SV-VI.. 1:
VOA/SV ACTION TABLES
QUALIFICATION OF VOLATILE/SEMIVOLATrLE ANALY ES BASED ON
SURROGATE COMPOUND RECOVERIES
Surrogate Compound Recovery
Sample
ResUlts
one or more
swrogates < 10%
one VOA. two B/N or wo
acid surrogates
10% %Rec < LL
all VOA, one BIN or
one acid surrogate
LL %Rec [ IL
one VOA, two B/N or
two acid surrogates
> tjL
Dccects I
1
i
A
j
Non- ie ects
R
U I
A
A
LL - Lower Limit of method QC acceptance criteria
UL - Upper Limit of method QC acceptance criteria
Table VOA/SV-VIJ-j:
QUALIFICATION OF VOA/SV AINALYTES BASED ON INTERNAL STANDARD AREA COUNTS
Internal Standard Area Counts
Sample
Results
Area Counts <20%
of associated
calibration std. area
20% Area Counts < LL
LL Area Counts [ IL
Area Counts > UI .
Detects
5
1
A
I
Nori-dctects R UI A A
LL - Lower Limit of method QC acceptance criteria based on associated calibration standard area
UL - Upper Limit of method QC acceptance criteria based on associated calibration standard area
Table VOA/SV-VIII- I:
QUAL]FIC TION OF ORGANIC ANALYTFS IN THE UNSPIKED FTELD SAMPLE
BASED ON MATRIX SPIKE RECOVERIES AND RPDSa*
Sample Resiijts
Recovery < 10%
10% Recovery <
Lower QC Limit
Lower QC Limit
Recovery
Upper QC Limit
Recovery>
Upper QC
Limit
RPD > QC Limit
Detects
No —I t ects I
J
R
I
UI
A
A
I
A (
J
UI
Note that qualification and rejection generally are limited to the spiking compounds, however, the validator
may use professional jud2merlt to qualify or rejec: jj positive detects or non-detec:s n the unspiked samDle
if the majority of spike compound recoveries and/or RPDs are outsiae the method QC acceptance criteria.
APPENDIX E - 3
DRAF1’ 12/96
-------
APPENDLX E VOA/SV ACTION TAB!
Table VOA/SV-VIfl-2.
QUALIFICATION OF ORG %NIC ANALYTES IN THE UNSPEKED FIELD SAMPLE
BASED ON MS. MSD. AND UNSPIKED SAMPLE %RSD
Sample Results
%R.SD 50%’
%RSD> 50%’
Two out o(threesample
results reported as non detects
Detects
A
J
Professional Judgment
Non-detects
A
Professional Judgmc:xt
Professional Judgment
* If a non-detected result is reported for a compound in one of the samples in the MS. MSD or unspiked
sample set, then the validacor should use the sample quan(itatiori limit vaiue for that compound to calculate
the %RSD.
Table VOA/SV.IX- 1
QUALIFICATION OF ORGANIC ANALYTES IN FIELD DUPLICATES.
SITUATION 1: POSITIVE DETECTS IN BOTH FIELD DUPLICATES
Relative
Percent
Difference
Aqueous> 30%
Non-Aqueous > 50%
Aqueous > 30%
Non-Aqueous > 50%
Aqueous > 30
Non-Aqueous > 50%
Sample Results
Both duplicate sample
cones 2XQL
QL both duplicate samples
cones. <2XQL
One sample conc. 2 X QL
QL Othersam&econc. <2XQL
Detects
J
Professional Judgment
Professional Judgment
Non-detec ts
NA
NA
NA
* QL = Sample Quantitation Limit
NoeS Qualification refers to field duplicate sample results only. Professional judgment may be utilized to apply
field duplicate actions to all samples of the same matrix.
Table VOA/SV.IX-2:
QUALIFICATION OF ORGANIC ANALYTES IN FIELD DUPLICATES -
SITUATION 2: POSITIVE DETECT IN ONLY ONE FIELD DUPLICATE *
&aueous and Noo-4queous
Sample Resujts
One Sample Conc. = ND (or value reported as
less than the QL)
QL Other Sample Cone. < 2 X QL
One sample cone. = ND (or value
reported as Tess than the QL)
Other sample conc. 2 X QL
Detects
Professional Judgment
I
Non-detects
Professional Judgment
w
QL = Sample Quantitation Limit
RPD should not be evaluated for these duoticate pairs
Note Qualification refers to field duplicate sample results only. Professional judgment may be utilized to aopiv
fieid duplicate actions to all samples of the same matrix.
APPENDIX E - 4 DRAFI’ 12/96
-------
APPENDIX E VOA/SV ACTION TABLES
Table VOAJSV -X-l:
OVALIFTCATION OF ORGANIC ANALYTES BASED ON MDL STUDY RESULTS
Sample Results
Mean % Recovery
%Rec < 10%
10% %Rec < 30%
80% %Rec 120%
] Rec> 120%
Detcccs
I
Professional Judgmenc’
A
Judgment’
Non-Detects
R
Professional Judgment’
A
A
Sample Results
Detects (
%
RSD
1
>25% J 25%
Professional Judgment”
A I
son-detects I
Professional Judgment”
A
* Taking into consideration LFB results.
Taking into consideration initial calibration %RSDs.
Table VQA1Sv-X -2:
)UALIFICATION OF ORGANIC ANALYTES BASED ON LFB* RECOVERIES WHERE:
ONE-HALF OF LFB COl 4POUNDS OUTSIDE UPPER OR LOWER ACCEPTANCE LIMITS
Sam nle
Results
%Recovery
%Rec < 10%
10% %Rec <60%
60% %Rec 140%
%Rec> 140%
Detects
J
J I
A I
.r
Non-detects
R
UJ
A I
A
* LFB = Lanoratory fortified blank spiked with several or all of the method target compounds at or below
the quantiation limit.
Table VOA/Sv.X.3•
UALrF1CATION OF ORGANIC ANALYrES BASED ON LFB* RECOVERIES WHERE:
ONE-HALF OF LFB COI\III’OUNDS OUTSIDE UPPER OR LOWER ACCEPTANCE LIMTTS**
Sample Results
%Recu ry
%Rec < 10%
10% %Rec <60%
60% %Rec 140% I %R :> 140%
AllDetec is I
j
J
A
J
All Non-detects
R
UJ
A
A
—
* LFB = Laboratory fortified blank spiked with several or all of the method target compounds at or below
the quanutauon limit.
Professional judgment should be used when a combination of low recoveries and high recoveries are
obtained
APPENDIX E - 5 DRAFf 12/96
-------
APPENDIX E
VOA/SV ACTION TABI
Table VOA/SV-XI- 1:
OUALIFICATION OF INDIVIDUAL ORGANIC ANALYTES BASED ON LCS RECOVERIES WHERE :
ONE-HALF OF LCS COMPOUNDS OUTSIDE UPPER OR LOWER ACCEPTANCE LIMITS
Sample Results
% Recovery
%Rec < 10%
10% %Rec IlL
Detects
J
J
A
j
Non-detects
R
UJ
A
A
- Lower Limit of method QC acceptance criteria
- Upper Limit of method QC accepance criteria
Table V/SV-XI-2:
QUALIFICATION OF ORGANIC ANALYTES BASED ON LCS RECOVERIES WHERE:
> ONE-HALF OF LCS COMPOUNDS OUTSIDE UPPER OR LOWER ACCEPTANCE LTh, [ ITS*
Sample Results
% Recovery
%Rec < 10%
10% %Rec UL
AilDetects
J
J
A
J
All Non-detects
R
TJJ
A
A
* Professional judgment should be used when a combination of low recoveries and high recoveries are
obiamed.
- Lower Limit of method QC acceptance criteria
- Upper Limit of method QC acceptance criteria
Table VOA/SV-XI-3
QUAUFICATION OF INDIVIDUAL ORGANIC ANALYTES BASED ON PES RESULTS WHERE:
ONE-HALF OF PES COMPOUNDS OUTSIDE UPPER OR LOWER ACCEPTANCE LIMITS
Sample Results
•Single Blind
‘Double Blind
PES < Lower Limit
‘Action Low”
‘Single Blind
‘Double Blind
PES “Within Warning Limits”
“Warning Highi Warning Low”
•Single Blind
‘Double Blind
PES > Upper Limit
“Action High”
Detects
J
A
J
Non-Detects
R
A
A
LL
UL
LL
UL
APPENDIX E - 6
DRAFT 12/96
-------
APPENDIX E
VOAISV ACTION TABLES
Table VOAISV-XI-4.
QUALIFICATION OF ORGANIC ANALYTES BASED ON PES RESULTS WHERE :
> ONE-HALF OF PES COMPOUNDS OUTSIDE UPPER OR LOWER ACCEPTANCE LIMITS
Table VOA/SV-XIII-l.
QUALIFICATION OF VOLATTILE/SEMIVOLATILE ORGANIC ANALYrES BASED ON
SAMPLE PERCENT SOLIDS
Sample Result H Solids > 30’
10% % Solids 30%
% Solids < 10%
Detects
A
J
R
Non-detects
A
R
R
Table SV-XV-i.
QUALIFICATION OF SEMIVOLATILE ANALYTES BASED ON
GPC CALIBRATION OC LITY CONTROL
I________________
Criteria
Action
Peak
Resolution
As per method QC acceptance criteria.
Professional Jud rnent
Peak
Shape
Peak shapes must be symmetrical.
Professional Judgment
Retention
Time Shift
Retention time shifts beween GPC calibrauon
checks must not exceed ± 5%.
Professional Judgment
GPC Instrument
Blank
Target analvtes must be < QL and surrogate
compound recoveries and IS area counts and/or
RTs (if added) must meet method QC accepunce
criteria. (Note CLP SOW OLMO3 2 does not
require the addition of surrogate compounds to the
G?C instrument blank)
Refer to Section V for Blank
Actions
* Professional judgment should be used when a combination of low recoveries and high recoveries are
obtained.
APPENDIX E - 7
DRAFT 12/96
-------
APPENDIX E VOA/SV ACTION TABI
Table VOA/SV.XJ -2:
QUALIFICATION OF SEMIVOLATTLE ANALYTES BASED ON GPC CLEANUP QUALITY CONTROL
WHERE: ONE-HALF OF GPC CALIBRATION CHECK COMPOUNDS OUTSIDE UPPER OR
LOWER ACCEPTANCE LIMITS
SampleResults
% Recovery
%Rec < 10%
109 %RecUL
Detects
Non-detects I
[
A
J
R
U I
A
A
LL - Lower Limit of method QC acceptance criteria
UL - Upper Limit of method QC acceptance criteria
Table V/SV-XI-3.
QUALIFICATION OF SEMIVOLATILE ANALYTES BASED ON GPC CLEANUP QUALITY CONTROL
WHERE: > ONE-HALF OF GPC CALIBRATION CHECK COMPOUNDS OUTSIDE UPPER OR
LOWER ACCEPTANCE LIMITS
Sample Results
% Recovery
%Rec < 10%
10% %Rec UI.
AilDetects
J
I
A
All 4on-detects
R
UJ
A
A
Note: Professional judgment should be used when a combination of low recoveries and high recoveries are
obtained.
LL Lower Linuc of method QC acceptance criteria
UL - Upper Limit of method QC acceptance criteria
APPENDIX E - S DRAfl’ 12/96
-------
APPENDIX E
VOA/SV ACTION TABLES
Table SV-XV-4:
QUALIFICATION OF SEMIVOLATILE ANALYTES BASED ON SILICA GEL
CLEANUP pUALrrY CONTROL WHERE: ONE HALF OF SILICA GEL CHECK SOLUTION
COMPOUNDS OUTSIDE UPPER OR LOWER ACCEPTANCE CRITERIA
Sample Results
% Recovery
%Rec < 10% 10% %Rec LL LL %Rec UL
J J A
R UJ A
Target anaiytes must be < QL and surrogate compound
%Rec > UL
Detects
j
A
Non-detects
Silica Gel Column
Refer to Section
Blank
recoveries and IS area counts and/or RTs (if added) must meet
method QC acceptance criteria.
V for Blank
Actions
Note. Professional judgment should be used in applying the guidance above to quaiify or reject sample data.
- Lower Limit of method QC acceptance criteria.
- Upper Limit of method QC acceptance criteria.
Table V/SV-XI-5:
QUALIFICATION OF SEMTVOLATILE ANALYTES BASED ON SILICA GEL CLEANUP OUAL1TY
CONTROL WHERE: > O -E-HALF OF SILICA GEL CHECK SOLUTION COMPOUNDS OUTSIDE
UPPER OR LOWER ACCEVFAANCE LIMiTS
Sample Results
% Recovery
‘ o. ec < 10% 10% %Rec UL
AilDetects
J
J
A
J
All Non-detects
P.
Ui
A A
Note: Professional judgment should be used when a combination of low recoveries and high recoveries are
obtained
- Lower Limit of method QC acceptance cnteria
- Upper Limit of method QC accernance criteria
LL
UL
LL
UL
APPENDIX E - 9
DRAFT 12/96
-------
Attachment A
“Quality Assurance for Superfund Environmental Data Collection Activities” -
Publication 9200.2-16FS, February 1993
and
“EPA Order 5360.1, Draft 1995 Quality Assurance Order”
-------
Many Supei-fund decisions (both Fund-financed and enforcement) require the collection and evaluation of site-specific
environmental data. Major activities associated with acquiring these data include planning, sample collection and analysis, and
data quality assessment. EPA policy requires the development and implementation of quality asswance (QA) programs to ensure
that these activities generate data of known quality. The overall goal of a QA program is to measure and minimize systematic
sources of error and to monitor conditions of sampling, storage and transport.
The Office of Emergency and Remedial Response (OERR) developed this fact sheet to promote a common understanding of
Superfund QA requirements for site-specific environmental data collection activities. The fact sheet focuses on the preparation
and implementation of sampling and analysis plans (SAPs). Requirements for planning and design, sampling, analysis, quality
control (QC), and data assessment are discussed. The process described is consistent with the integrated site assessment and
accelerated response objectives of the Superfund Accelerated Cleanup Model (SACM). Conforming to these requirements will
help ensure that site managers generate data of known quality.
INTRODUCTION
This fact sheet provides Superflmd program participants with an
overview of Superfund QA requirements for data collection
activities. The information is pertinent to all Superfund site
managers, including remedial project managers (RPMs), site
assessment managers (SAM ), and on-scene coordinators
(OSCs). ‘The information also applies to Agency contractors,
states, and potentially responsible parties (PRPs) and their
contractors,
The ct sheet addresses three primary areas: (1) the mandatory
QA requirements specified in Agency policy documents; (2) QA
management for Superfund; and (3) the process for developing
SAPs for Superfund activities. The relationship between these
primary areas is depicted in Exhibit 1. References are
identified after each primary section to provide additional
information on discussion topics. These reference materials
contain guidance on the appropriate quality control (QC)
considerations site managers should include as part of the QA
program.
AGENCY QA POLICY
EPA Order 5360.1 establishes mandatory QA
requirements for Agency environme,ual data collection
activities The National Oil and Hazardous Substances
Pollution Contingency Plan (NC?) mandates specific
Superfund QA requirements.
EPA Order 5360.1 and the NC? collectively define Superfund
QA policy for environmental data collection. Both documents
emphasize two requirements. The first is that Superfund
environmental data must be of known quality. The quality of
data is known when all components associated with its
derivation are thoroughly documented and the documentation
has been reviewed by a qualified reviewer. Second, QA plans
are required to attain the first objective. These may be based
on generic or site-specific procedures depending on project
requirements. This section summarizes the QA requirements
contained in each document,
EPA Order 5360.1, entitled., Policy and Program Requirements
to Implement the Mandatory Quality Assurance Program ,
descrbes two major EPA requirements relaxed to
environmental data collection activities. The first is
panicipaxion by all EPA organizations in a central QA
program. The goal of the QA program is to ensure the
generation of data of known quality. Basic Agency QA
implementation requirements are summarized in Exhibit 2.
The cond major requirement is the development of’ QA
project plans for all environmental data collection activities.
These plans specif y data quality goals acceptable to data users,
and they assign responsibility for achieving these goals.
The NC? establishes the specific requirements used in the
Superfund program to comply with EPA’s overall QA policy.
The NC? requires sue managers to develop SAPs for the
following Superfund hazardous substance response activities:
United States
Environmental Protection
Agency
EPA
Office of
Solid Waste and
Emergency Response
Publication 920 0.2-1 6FS
February 1993
Quality Assurance for
Superfund Environmental Data
Collection,. Activities
Office of Emergency and Remedial Response
5203G
Quick Reference Fact Sheet
-------
EXHIBIT I SUPERFIJND QA OVERVIEW
I Remedial site inspections
Removal site evaluations
Remedial investigation/feasibility studies
plans document the process for obtaining data of
nt quality and quantity to satisfy data users’ needs. The
further states that the SAP shall include a field sampling
plan (FSP) and a QA project plan (QAPP). The FSP defines
the number of samples, sample type (mairiz), sampling location,
and required analyses. The QAPP describes the policy,
organization. functional activities, and data quality objectives
(DQOs) that site managers need to establish and document prior
to performing any site-specific work. The SAP is a single
document with two separable components - the FSP and QAPP
- allowing for separate submissions consistent with Regional
guidance.
REFERENCE BOX I
QA MANAGEMENT FOR
SUPERFUND ACT! VITIES
OER.R. Regional Offices, and contractors parucipaze in
Superfund QA manageme u activities.
To conform to the requirements specified in Order 5360.1 and
the NC?, Superfund follows a well-defined management
structure operated by the Office of Solid Waste and Emergency
Response (OSWER). Within OSWER. OERR establishes and
oversees QA procedures, performed in support of Superfund
data collection activities. Regions perform most data collection
activities and implement the associated QA program. Regions
achieve QA goals by using qualified personnel and well-
defined procedures (including the development of DQOs) and
performing or requiring the performance of precise data
collection and accurate interpretation of data results.
OERR Quality Assurance Program
The OERR QA program applies to all Superfund site-specific
data coLlection activities. This program has been developed to
establish national consistency in the implementation of the
Superfund QA program. Agency and Superfund policy is set
forth in the OERR Quality Management Plan to provide site
managers with information on program requirements for
generating data of known quality.
AGENCY GA POLiCY
EPA Order 5360.1
NCP
GA MANAGEMENT
OERR GA Program
Regional GA Programs
Contractor GA Programs
.
SITE-SPECIFIC CA -
- --
Sampling & Analysis
Plan (SAP) Development
- FSP
• QAPP
I I
Pro lect Sampling
Oblectives Design
Sampling Sample
Execution Analysis
Assessment
of
Data Quality
i
‘1
Environmental Protection Agency (EPA). 1984. EPA
Order 53601 - Policy and Program Requirements to
Imolernent the Mandatory Quaiity Assurance
Program Ott ce at Research and Development
Enwonmental Protection Agency (EPA). 1988 Natonal
Oil arid Nazaidous Substances Po ! ueon Contingency
Plan (NCP ) 40 CFR 300
2
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QA REQUIREMENTS
lmplemenbton of QA proced ms for all conbacts
involving eavironmen J data coliecbon activibes as
specified in applimble Agency rogulabans. sisbcontracts.
and subagroomerits
Conduct audits on a sdiedulecf basis
Deve opment and adoption of tothnic 1 guidelines tar
assessing data quality
• Establishment of achievable data quality limits for
methods cited in regulations
• Implementat ion of a corrective action program
• Provisions for appropnate tialning as required for all
levels of QA management
Regional Administrators are responsible for implementing EPA
Order 5360.1 and for tailoring the OERR QA program to
Region-specific operations. Regional Quality Management
Plans contain Region-specific policies, procedures, and
organizational structures necessary for generating data of known
ality.
. ontractor Quality Assurance Programs
Each Superfund contractor performing data collection activities
must also establish a QA program to generate data of known
quality and to meet other Agency policies. Specific
requirements for contractor QA programs are defined in the
OERR and Regional Quality Management Plans.
The contractor QA program must be documented through a
Quality Management Plan that describes the corporate QA
policies and general requirements for all environmental data
collection activities. In addition, the contractor must develop
project-specific QA plans and SAPs that are presented for
review and approval as delineated in each Region’s Quality
Management Plan.
Superfund Quality Assurance Program Assessment
EPA Headquarters and the Regions continually monitor the
effectiveness of the Superfund QA program through the use of
management and technical systems reviews. EPA Regional and
Headquarters stiff review the perfomiance of each contractor to
ensure conformance to technical and contractual requirements.
- -
Management Plan.
Exhibit 3 presents a brief description of the systems reviews.
These reviews assist OERR and Regional QA staff in assessing
the implementation and adequacy of Superfund QA at the
program and proSect management levels. Project reviews, a
type of management systems review, evaluate the integral
components associated with data collection activities. The
results of these reviews assist site managers and other data
users to verify the quality of sampling and analytical
operations.
EXHIBIT 3- SYSTEMS REVIEWS
Superfund Evidentiary Concerns
The National Enforcement Investigations Center (NEIC) is
responsible for providing a range of technical, investigative,
and litigation expertise for the Agency’s enforcement cases.
NEIC is granted statutory authority under CERCLA for
inspecting, record-keeping, and compiling confidential
information. Applicable NEIC evidendary requirements for
site-specific field activities must be included in the project
SAP.
NEIC has prepared guidance pertaining to evidenciary
requirements for Superflmd in the NEIC Policies and
Procedures Manual . Examples of evidenciary requirements
include:
Sample identification
Chain-of-custody procedures
• Sample receiving procedures
• Sample cracking procedures
• Document control procedures
u Standard operating procedures
• Preparation and annual update of a Quality Management
Plan
• Development of QA project plans tot all maior contracts
involving environmental measuiemonts
•
U
Regional Quality Assurance Programs
Management Systems Reviews assess the effectiveness of
the implementalon of the approved QA program. Those
reviews consider linkages across organizational lines and can
be used to discern areas requiring improved guidance.
Technical Systems Reviews assess project OC activities and
environmental data collection systems Areas typically
examined dunng this review include: sampling/measurement
systems; equipmentllacitity maintenance records; and control
Audits of Data Quality address whether or not sufficient
information exists for data sets to support data quality
assessment This type of audt may also be used to deten-nino
if the organization collecting or using the data pei ormed a data
quality assessment
Performance Evatuation Reviews evaluate the laboratory
and/or field analytical personners performance and the
ins umentation or analytical systems used.
3
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Additional information on evidentiary policies for the Contract
Laboratory Program (CL?) can be found in Exhibit F of the
rrent CL? Statements of Worla Exhibit F describes the
ain-of-custody, document control, and related standard
operanng procedures for the CLP. Individual laboratories are
expected to incorporate Agency evidenciary requirements in
their own standing procedures.
REFERENCE BOX 2
Envtronmen J Protection Agency (EPA) 1985 Interim Policy
and Guidance for Management Systems Audes of
National Program Offices . Quality Assurance
Management Staff (QAMS).
Environmentoi Protection Agency (EPA) 1987 Guidelines
and Specifications ‘or Prepanng Quality Assurance
Procram Ptans (QAPP5) and Quality Assurance Annual
Report and Worlplans (QAARWs) for EPA National
Program Oflicas and the Office of Research and
Development fORD ) Quality Assurance Management
Staff EPAQNG•2.
Environmental Protection Agency (EPA). 1992. QUal !Y
Assurance Management Plan for the Office of
Emergency and Remedial Response
Environmentoi Protection Agency (EPA). 1980 Guidelines
arid Specifications for Prapanng Quality Assurance
Proqrarn Plans , QAMS-004/80. QAMS is currendy
developing an update to this guidance entitled, Guidance
for Preoannq, Reviewing, and Iniolementing Quality
Assurance Management Plans , EPAQA1G—2.
SAMPLING AND ANALYSIS PLAN
DEVELOPMENT
Sampling and analysis plaits are site-specific
documents that contain sampling objectives, strategies,
and the appropriate QA procedures necessary to meet
project objectives. SAPs should incorporate or build
upon generic plans and standard operating
procedures, when available. Major activities
associated with the development of the plans are
presented in Exhibit 4.
The effective and efficient development and implementation of
SAPs is essential to obtaining data of sufficient quantity and
quality to support program decisions. As defined in the NC?,
SAPs consist of two integral components, the FSP and the
QAPP. Exhibit 5 presents the minimum requirements for each
componenL When preparing SAPs, care should be taken to
streamline the process and avoid duplication between the two
components. Also SAPs should incorporate or reference
generic plans and Regional standard operating procedures, as
ppropr ate.
The SAP should describe each project objective in detail.
Usually this is done by describing the specific decisions to be
made with the data and involving the decision maker from the
beginning. The plan should describe how each data value will
be used to make a decision. It should include a description of
the monitoring network, the location of each place samples will
be collected, the sampling frequency, the types of analyses for
each sample, the target precision at the concentration of
interest and the rationale for the design. All factors that will
influence the eventual decision should, to the extent practical,
be evaluated and specified at the beginning of the process.
The plan should balance the need for an appropriate level of
QA (commensurate with project needs) with timeliness and
cost considerations. Finally, the plan should include the
organization’s functional activities and the names of all key
people. The remaining sections of this document discuss the
SAP development process, from definition of the project
objectives to generation and evaluation of the environmental
data.
Project Objectives
Project and data quality objectives must be developed
to assist in assuring the generation of useable data.
The first stage in developing the SAP is to determine overall
project objectives and DQOs. Project objectives define the
type and extent of investigations required at a given site.
DQOs specify the level of uncertainty that site managers are
willing to accept in results or decisions derived from
environmental data. Site managers should develop project
objectives and DQOs in accordance with data useability
requirements for project activities. For example, the technical
requirements for scoring a site using the Hazard Ranking
System (HRS) may be less stringent than those required for a
risk assessment.
Because DQOs are developed before the data are collected, this
process can improve the efficiency of data gathering by
defining the number and type of samples and level of QA.
Since these factors are determined based on project need,
DQOs assist in streamlining the process and ensuring cost
effectiveness.
Exhibit 6 illustrates the DQO process as it is defined in
Guidance for Data Useability in Site Assessment . Additional
references on the DQO process can be found in Reference Box
3.
Once these objectives have been defined, the site manager
must identify the procedures required to achieve these
objectives and the acceprnble degree of uncertainty. Chemists,
geologists, biologists, ecologists, risk assessors, computer
modelers, statisticians, QA staff, and Regional Counsel should
be invited to participate in this process, as appropriate.
4
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EXHIBET 4- SAMPLING AND ANALYSIS PLAN DEVELOPMENT
Sampling Design
Effecnve sampling designs are dependent upon project
and data qualirj objectives It is important 10 crvoid
collecting more samples than required go support
project decisions.
During sampling design, site managers develop project
objectives into specific operational parameters. The design
identifies the number, type, and location of samples. Effective
sampling designs result in the generation of data that meet the
project objectives and DQOs. The sampling design should also
generate data that are representative of the conditions ax the site
within resource limitations.
Examples of the types of site-specific factors that should be
considered when designing a sampling plan include: site
accessibility, climate, potential hazards, media of concern, and
site heterogeneity. Information that cart be used to support the
design often includes site maps, geological information, disposal
records, and histoncal data. Standard Operating Procedures
(SOPs) for the most common sampling techniques and field
procedures should be used consistent with Regional guidance.
Sampling designs may be statistical, judgmental, or a
combination of both. Statistical sampling designs entail
selecting sampling locations using a probability based scheme.
Judgmental sampling designs focus the sampling Location
specifically in the area of concern. I-IRS scoring is an example
of when high bias is acceptable. therefore, the use of non-
statistical or judgmental sampling is appropriate. To determine
which design is appropriate, practical trade-offs between
response time, analytical costs, number of samples, sampling
costs, and level of uncertainty should be weighed by the site
manager. A combination of statistical and judgmental
sampling can often be used to maximize available resources,
but a statistician should be consulted.
Because site conditions may change, sampling designs should
be flexible enough to allow for modifications during sampling
execution. However, deviations from the original design
should be approved in advance by the site manager.
Field analyses can also be an important component of the
overall sampling design. These analyses can be used to
provide threshold indications of contamination and may be
helpful in revising and refining the sampling strategy.
Analytical field methods also can be useful in directing
sampling into areas of greatest contamination or “hot spots.”
7 SME\
çD AQU )
SAMPUNG & ANALYSIS
PLAN
DEVELOPMENT
5
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Field Sampling Plan: Specifies field activities
necessary to obtain envIronmental data and contains
the following elements:
Representative samples are collected through the use’
of well-defined sampling practices. - -
EXHIBIT S - SAMPLrNG AND ANALYSIS PLAN
COMPONEN1’S
samples are collected in conjunction with environmental
samples and are evaluated to establish baseline values for the
contaminants of concern. These samples are collected at or
near the hazardous waste site in areas not influenced by site
contamination. Background samples should be collected at
EXHIBIT 6 - THE DQO PROCESS
• Site background
• Sampling objectives and rationale
• Sampling matnx/locanon/frequency
• Sample identlficanortldocumentation
• Sampling equipment/procedures/decontaniinationf
disposal
• Sample handling/packaging/analysis
Quality Assurance Project Plan: Desaibes the
policy. organization, arid DQOs for decision-making
purposes. Key elements include:
• Project description
• Project organizatlon/responsibilifjes
• QA objectives for measurement
• Sampling procedures and DC
• Sample custody
• Calibration procedures
• Analytical procedures with detection
linvts/quarititacion limits
• Data reductonlvalidation and reporting
• Internal quality control
• Performance and systems reviews
• Preventive maintenance
• Data assessment procedures -
• Corrective actions
• CA reports
STEPS IN THE DQO PROCESS
State Problem - Describe the problem, possible
resolutions, and data collection constraints.
Identify Problem • State the question that will be
answered using environmental data.
Identify Input Affecting Decision - List the variables to
be measured arid other information needed to make the
deasion. Ust procedures for assessing the precision
arid accuracy of the data at the concentration of interest.
Specify Domain Of Decision - Specify the locations of
concern within the site arid describe the ditferent
pathways.
Develop Logic Statement Develop a quantitative
statement defining how the data will be summarized and
used to answer each question.
Establish Constraints On Uncertainty • Define the
procedures for deternuning total uncertainty in the data,
and develop data acceptance critena.
Optimize Design For Obtaining Data - Develop a
practical design for the study that is expected to produce
the necessary data.
Finally, field analytical methods should be used to accelerate
the site assessment process and reduce costs when their use is
consistent with site conditions (e.g. contaminants, media) and
the l)QO’s established for the site.
Sampling Execution
Sampling execution involves the collection and documentation
of samples identified by site managers during the sampling
design phase. The goal of sampling execution is to collect
- samples representative of site conditions to fulfill project
requirements and DQQs.
In order to collect representative samples, the number, location,
sampling methods, equipment, and containers must be
appropriate for the sample matrix and the contaminants of
concern. Collection procedures should not alter the matrix
sampled. En addition, samples should be preserved in a manner
that minimizes potential chemical and biological degradation.
managers are responsible for identifying background and
C samples dunn g the sampling design stage. Background
approximately the same time and under the same conditions as
the test samples, and they should be collected for each matrix.
QC samples assist in assessing the data quality. Field QC
samples are collected on-site in conjunction with environmental
samples and are used to gather information on the precision
and bias of the sampling process. Types of field QC samples
include double-blind samples (e.g., field evaluation samples,
field matrix spikes, and field duplicates), single-blind samples
(e.g., trip blanks, rinsate blanks), and non-blind samples (e.g.,
laboratory control samples as used in the CLP).
The precise composition and frequency of QC samples is
dependent on the objectives for the sampling event and existing
Regional guidelines. All field QC samples should be stored.
transported, and analyzed using the same procedures used for
site samples.
Site managers should assess sampling execution by evaluating
the data from field QC samples and observing field activities.
Field duplicate sample results can provide useful QC
information. However, this field assessment will not provide
6
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real time data on the precision of the sampling event since it is
assessed dunng the data review.
On-site observations of field activities are conducted to verify
that the SAP is being followed. The SAP should specify areas
where flexibility in procedures and/or criteria may be acceptable
and should specify procedures for documenting these changes.
Field documentation is critical to a successful QA program.
The field log book should be legally defensible and all entries
should be complete and accurate enough to permit
reconstruction of field activities.
Sample Analysis
Contract Laboratory Program (CLP) or non-CL?
analytical services may be procured in support of
Supetfund activities. Laboratories which can
demonstrate a successful history of independent audits
should be selected for use
Project DQOs and analytical factors dictate the selection of
analytical methods. The analytical method and associated QC
should provide data of known quality for the contaminants of
concern. Data users should consider the following factors when
selecting analytical methods:
• Quantitacion limit
• Detectable constituents
• Qualitative confidence
• Method precision and bias
• Turnaround time
I Analytical cost
Once the site manager has evaluated these factors, analytical
services may be procured through eitherCLP or non-CLP
services. The site manager or other data user is responsible for
planning, monitoring, and assessing the quality of data
regardless of the analytical service procured.
The CL? is a national program of commercial laboratories
under contract to EPA that provides routine or specialized
analytical services. Routine analytical services WAS) use a
limited number of standardized methods and are designed to
generate consistent results. Specialized analytical services
(SAS) provide non-standardized analyses or faster turnaround
tune and require the data user to specify the necessary
analytical methods and QC requirements. The CL? adheres to
specific data acceptance criteria that result in data of known and
documented quality. However, it cannot be assumed that CL?
data achieve the DQO requirements established for the project.
Data quality assessment is still required.
Analytical services procured outside of the CL? are
characterized as non-CL?. These can be provided by
laboratories that participate in the CL?, use CLP methods,
enernte CLP-type data packages, or by laboratories that ha e
,never participated in a national analytical program. It is
recommended that non-CL? laboratories be audited to assure
the validity and defensibility of any data generated.
Non-CLP data are generated by laboratories whose proficiency
in the methods of interest may or may not be known. Itis the
responsibility of the data generator and user to select the
method and data acceptance criteria that will verify method
and laboratory performance.
Two categories of non-CL? services are available: fixed
laboratory and field analyses. Fiaed laboratory analyses are
performed by commercial laboratories selected by the data
user. Field analyses are commonly performed in mobile
laboratories or with fleldable or portable analytical instruments.
In addition to quick turnaround and lower cost, field analyses
can: (I) focus sampling efforts: (2) provide qualitative
information; (3) provide quantitative results when
supplemented by confirmatory samples sent to a fixed
laboratory and (4) potentially satisfy project needs.
Analytical QC is comprised of a planned system of routine
activities for obtaining prescribed standards of performance.
QC frequency, type, and acceptance criteria should correlate
with the study objectives. The type, frequency, sequence, and
control criteria for analytical QC samples are predetermined for
CL? RAS. Site managers specify the control criteria for both
CL? SAS and non-CL? analyses.
Assessment of Data Quality
Site managers and other data users assess data qualizy
to determine if the data are consistent with project
objectives and are appropriate for supporting a specific
decision.
Steps in assessing data quality may include data review,
uncertainty determination, and data useability assessment.
Benefits data users can obtain from proper assessment of data
quality include: (1) establishment of data useabilicy; (2)
determination of sufficient data quantity; and (3) improvement
of future data collection efforts by identifying major sources of
error in the data.
Data ReviewfValidation: The first step in assessing data
quality is data review, also known as data validation. Data
review/validation is the technical examination of environmental
data and the associated QC data to determine the limitations of
the data. During this process, the reviewer applies analytical
criteria to determine if analyses were performed under
controlled conditions and whether or not the data should be
qualified. Because data review/validation criteria are based on
the methods used to generate the data, the results of a data
review/validation are frequently independent of the intended
use of the data. The data review/validation process establishes
the quality of the data. Data review must be consistent with
the project DQOs and QAPP.
7
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CL? data review is performed by technical personnel who have
been trained by Regional staff or follow Agency guidance. The
data package is reviewed using EPA ’s functional guidelines for
evaluating organic and inorganic laboratory data (see Reference
Box 3) and Regional SOPs that comprise standardized
procedures and criteria based on the associated analytical
methods. Non-CLP data are reviewed based on available’
information including the sample maxriz and analytical method
used and in accordance with the procedures and criteria
specified in the DQOs. Data validation procedures must avoid
conflict of interest problems.
Determination of Total Uncertainty: Each step of the data
acquisition process has an inherent uncertainty associated with
it. The uncertainty acceptance level depends on the purpose for
which the data are being collected. Total error is comprised of
two types of erroc sampling variability and measurement error.
Sampling variability is the variation between true sample values
and is a function of the spatial variation in the pollutant
concentrations. Measurement error represents the difference
between the true sample value and the reported value.
Examples of these types of errors are provided in Exhibit 7.
Factors that can influence sampling and measurement errors
include:
• Instrument capabilities
• Variability (media, spatial, temporal, operational)
• Incorrect sample collection coordinates
• Improper decontamination procedures
• Improper sample preservation
• Inadequate storage procedures
• Inappropriate sample preparation analysis
• Exceeded holding times
EXHIBIT 7. TOTAL ERROR COMPONENTS
Site managers and other data users should establish procedures
for estimating total uncertainty and data acceptance criteria
during the DQO development stage. EPA currently is
developing procedures for determining total error for soil
analyses. The Environmental Monitoring Systems Laboratory
in Las Vegas (EMSL1LV) has developed a guidance, A
Rationale for the Assessment of Errors in the Sampling of Soils ,
to serve this purpose.
Data Useability Assessment ’ After the data have been
reviewed and the total uncertainty estimated, the data must be
examined in the context of the DQOs to determine whether
they are valid for their intended use.
Site managers or other data users assess data useability by
evaluating the sampling and analytical performance against the
quality indicators specified in the DQOs. Quality indicators
consist of quantitative Statistics and qualitative descriptors and
are used to interpret the degree of acceptability of data to the
user. ‘The data quality indicators are:
• Bias/Accuracy
• Precision
ii Comparability
ii Completeness
ii Representaxiveness
Site managers may be required to implement corrective action
in the event the system fails to achieve the established
performance criteria.
EPA has established a Data Useability Workgroup to develop
national guidance for minunum data quality requirements to
increase the useability of environmental data in support of
Superfund. Within this workgroup, the risk assessment
subgroup has developed minimum requirements for risk
assessments (see Guidance for Data Useabilitv in Risk
Assessment: Final) . The site assessment subgroup has
developed similar guidance for site assessments.
Automated Computer Systems
Automated computer systems are
supporting data collection acnvities.
useful tools in
Several automated computer
systems are being developed that
can assist site managers in
performing various aspects of
data collection, including
developing SAPs, developing
and evaluating sampling ___________________
strategies, and performing
automated data review. This
section describes some of the systems that are in the prototype
stage of development. Because these systems have not been
finalized, their current useability cannot be guaranteed. Exhibit
8 provides EPA contacts for further information on each of
these systems.
Sampling and Analysfs Plan Developmenr The Quality
Assurance Sampling PLan for Emergency Response (QASPER)
was created to automate the development of a site-specific
SAP for the Removal program. The system is implemented
u3ing WordPerfect software. QASPER includes step-by-step
procedures for developing a SAP, from development of DQOs
Sampling variability is a function of the spatial vanation
ri pollutant concentrations. For example, landfills may
have “hot spots” with non-representative concentrations.
Measurement error, which has components from both
sampling and analysis, is estimated using the results of
QC samples. For example, sample results may be biased
low due to the holding time being exceeded.
8
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through data validation. The system significantly expedites the i XHhIiti - ( Ui WUi1 K SYSII .M ‘..ur iALi
SAP development process.
ASSESS: Jet ! Van Es, Exposure Assessment Division,
Development and Evaluation of Sampling Strategier Several USEPA EMSL/LV, (702) 798.2367.
automated systems have been produced to develop ind evaluate
sampling strategies. Each automated system has specific data 9ADRE John Nocenno, Quality Assurance
DMsion, USEPA EMSL/LV, (702) 798-2110.
requirements and is based on specific sire assumptions.
OQO Expert System: John Warren, USEPA Quality
The DQO Expert System was developed by the Quality Assurance Management Staff, (202) 260-9454.
Assurance Management Staff (QAMS). It is a training system
that assists in planning environmental investigations based On eDATA: William Coaldey, USEPA ‘Envlronmentai
the DQO process. The four systems that follow were developed Response Team, (908) 906-6921.
by EMSL/LV. The Environmental Sampling Expert System
(ESES) assists in planning sample collection. It includes ESES: Jeff Van Es, Exposure Assessment Division.
USEPA EMSLJ1..V, (702) 790-2367.
models that address statistical design, QC, sampling procedures,
sample handling, budget, and documentation. The current GEO-EAS: Evan Englurid, Exposure Assessment
system addresses metal contaminants in a soil matrix. Division, USEPA EMSL/LV, (702) 798-2248.
Expanded application of this system is under development. The -
Geostausticai Environmental Assessment Software (GEO-EAS) QASPER: William Coaldey. USEPA Environmental
is a coLlection of software tools for two-dimensional Response Team, (908) 906-6921.
geostatistical analysis of spatially distributed data points.
SCOUT: Jet! Van Ee, Exposure Assessment Division.
Programs include file management. contour mapping. VanognUTi USEPA EMSLILV, (702) 798-2367.
analysis, and biging. SCOUT Multivariate Statistical Analysis
Package is a collection of staustical programs that accept GEO-
EAS files for multivariate analysis. The Assessment of Errors
in Sampling of Soils (ASSESS) system estimates measurement
error variance components. It presents scatter plots of QC data
and error plots to assist in determining the appropriate number
of QC samples required.
Automated Data Review: Automated data evaluation systems
have been developed to reduce the resources . and the amount of
rime reqwred to review data. The Computer-Aided Data
Review and Evaluation (CADRE) system developed by
EMSL/LV is an automated evaluation system that assists in the
review of CL? organic RAS data. CADRE evaluates data
quality according to the QC criteria defined in the EPA’s
funcuonal guidelines for evaluating inorganic and organic data.
The system is being modified to accept manual entry of other
data sets and to accept user-defIned criteria to meet specific
information needs.
The Electronic Data Transfer and Validation System (eDATA)
developed by the Removal program assists in rapid evaluation
of data in emergency responses This system may be applicable
for both CL? and non-CL? data. The system combines DQOs,
pre-established site specifications, QC criteria, and sample
coLlection data with laboratory results to determine useability.
This software consisrs of three separate and distinct modules
that reflect the needs of the sire manager, the laboratory, and
the data validator, In using eDATA, the sire manager specifies
the DQOs associated with any given batch of samples. the
choice of the pre-established QA/QC criteria, and the limits for
volatile, semivolatile, PCB and pesticide, and metal constituents.
The site manager can also create sets of user-defined criteria to
meet prc’ect-specific needs.
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REFERENCE BOX 3
knerican Pubic Health Association. 1985 Standard Methods Environmental Protection Agency (EPA). 1991. CIP Analytical
for the Exam atfon of Water and Wastewater . Amencan Results_Database (CARD) Quick Reference Fact Sheet
Public Health Association, 16th Edition. 1985. OffIce of Emergency and Remedial Response.
Environmental Protection Agency (EPA). 1986 Teal Methods for Environmental Protection Agency (EPA). 1991. CLP
Evaluating_Solid Waste (SW-846) PhysicaUCherrucal Methoos Statement of Work For Inorganics Analysis . Document
Third Edition. Office of Sdd Waste. . Number ILMO2 0 (or most recent update).
Environmental Protec on Agency (EPA). 1987. A Compendium of Environmental Protection Agency (EPA). 1991. CIP
Superfund Field Operations Methoth . Office of Emergency and Statement of Work for Organics Analysis . Document
Remedial Response. EPN54OIP-87i001. Number OLMO1.1 (or most recent update).
Environmental Protection Agency (EPA). 1987. Data Quality Environmental Protection Agency (EPA). 1991. Compendium
Ob ectives for Remedial Response Mtvides Development of EAT Ground Water Samoling Procedures . Emergency
Process EPN54OaG.87/003. Response Division Office of Emergency and Remedial
Response EPAJS4O/P-91/007.
Environmental Protection Agency (EPA). 1987. Data Quality
Objectives for Remedial Response Activities ExarnoleScenano Environmental Protection Agency (EPA). 1991. Compendium
RL/FS Activities at a Site with Contaminated Soil and Ground of EAT Soil Samptrig and Surface Geophysics
Water Office of Emergency and Remedial Response Procedures Emergency Response Division Office of
EPAi 54O -87,VO4. Emergency and Remedial Response. EPAIS4O/P.9L006
Environmental Protection Agency (EPA) 1988 Field Screening Environmental Protection Agency (EPA). 1991. Compendium
MethodsCatalog OfficeofEmergencyandRemedialResponse of ERT Surface Water and Sedunent Sarnaling
EPNS4O/2-88/005 Procedures Emergency Response Division Office of
Emergency and Remedial Response EPA/540/P-91i005
Environmental Protection Agency (EPA) 1988 Ground Water
Modeling An Overview and Status Reooii EPA/600P2-89/028 Environmental Protection Agency (EPA). 1991 Compendium
of ERT Waste Sampling Procedures Emergency
Environmental Protection Agency (EPA). 1988 Laboratory Data Response Division Office of Emergency and Remediai
Validation Functional Guidetnes for Evaluating Inorgarilca Response EPNS4O/P-91/008
Analysis Office of Emergency and Remedial Response.
Environmental Protection Agency (EPA). 1991 Management
Environmental Protection Agency (EPA). 1988 Laboratory Data of Investigation-Derived Wastes Dunrig Site Insoections
Validation Functional Guidelines for Evaluating Organics EPA/540I -91dO09, May 1991.
Analysis Office of Emergency and Remedial Response.
Environmental Protection Agency (EPA) 1991. Practical
Environmental Protection Agency (EPA). 1989. Deterrrvning So Guide for Groundwater Samoling EPA 600i2-85/104,
Response Action Levels Based on Potential Contaminant September 1985.
Migration to Ground Water A Compendium of Examples
EPk54Oi2-89iV57. Environmental Protection Agency (EPA) 1991
Reoresentative Samoling Guidance Vol I Soil
Environmental Protection Agency (EPA) 1989. Guidance on OSWER Directive 9360.4-10.
Aapl ,ng the Data Quality Obiectives Process for Ambient Air
Monitonng Around Superfund Sites (Stages 1 and 2) . OffIce of Environmental Protection Agency (EPA). 1991. Samolers
Air Quality and Planning and tandards. EPA/450/489/015 Guide to the Contract Laboratory Program . Office of
Emergency and Remedial Response. EPAI54OIP-
Environmental Protection Agency (EPA). 1989 Quality Assurance 90/006
Tedinical Information BuRetin , Vol. 1. No.2, 11/13/89.
Environmental ProtectionAgency(EPA). 1989.SeilSameling Quality Environmental Protection Agency (EPA). 1991. Users
Assurance Use(s Guide . Environmental Monitoang Systenis Guide to the Contract Laboratory Program . Hazamcus
Laboratory. Us Vegas, NV. EPA/600/8-891046. Site Evaluation Division Office of Emergency and
Remedial Response. EPN540/P-91/ 02.
Environmental Protection Agency (EPA). 1989. Suoerfund Ground
Water IssueS Grourd Water Samptng for Metals Environmental Protection Agency ( EPA). 1992. Guidance
Office of Research and Development. EPN54O/4-89d001. for Data Useability in Risk Assessment Final Office
of Emergency and Remedial Response. Part A
Environmental Protection Agency (EPA). 1990 QNQC Guidance for 9285.7 .09A. Part B (radionudides). 9285.7-09B
Remedial Activities EPA 5401G.901004
Environmental Protection Agency (EPA). 1992 Precaration
Environmental Protection Agency (EPA). 1990 A Ra onale for the of Soil San,oling Protocol Samoling Techniaues and
Assessment of Errors in the Samoling of Soils Office of Strategies EPA 600/R 92J128
Research and Development. EPAIGOO/4-901013.
I0
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GLOSSARY
Assessment . the evaluation process used to measure the
performance or effectiveness of a system and its elements.
Assessment is an all-inclusive term used to denote any of
the following audit. performance evaluation, management
systems review, peer review, inspection or surveillance
Audit - a planned and documented investigative evaluation
of an item or process to determine the adequacy and
effectiveness as well as compliance with established
procedures, instructions, drawings, QAPPs, andlor other
applicable documents
Data Quality Objectives (OQOs) a statement of the
precise data, the manner in which such data may be
combined, and the acceptable uncertainty in those data in
order to resolve an environmental problem or condition
This may also include the criteria or specifications needed
to design a study that resolves the question or decision
addressed by the OQO process
Data Quality Objectives Process - a Total Quality
Management (TQM) tool developed by the U S
Environmental Protection Agency to facilitate the planning
of environmental data collection activities The DQO
process asks planners to focus their planning efforts by
specifying the use of the data (the decision), the decision
cntena, and their tolerance to accept an incorrect decision
based on the data The products of the DQO process are
the DOOs
Data Useability - the process of ensunng or determining
whether the quality of the data produced meets the
intended use ot the data
Detectable Constituent - a target anatyte that can be
determined to be different from zero by a single
measurement at a stated level of probability.
Management Systems Review (MSR) the qualitative
assessment of a data collection operation and/or
organization(s) to establish whether the prevailing quality
management structure, policies, practices, and procedures
are adequate for ensunng that the type and quality of data
needed are obtained
Performance Evaluation (PE) - a type of audit in which
the quantitative data generated in a measurement system
are obtained independently and compared with routinely
obtained data to evaluate the proficiency of an analyst or
laboratory.
Quality -the sum of features and properses/charactanstics
of a process, item, or service that bears on its ability to
meet the stated needs and expectations of the user.
Quality Assurance (QA) an integrated system of
management activities involving planning, implementation,
assessment, reporting, and quality improvement to ensure
that a process, item, or service is of the type and quality
needed and expected by the customer
QualIty Assurance Project Plan (QAPP) - a formal
document describing in comprehensive detail the necessary
CA, CC, and other technical activities that must be
implemented to ensure that the results of the work
performed will satisfy the stated performance cntena
Quality Control (CC) . the overall system of technical
activities that measure the a butes and performance of a
process, item, or service against defined standards to venfy
that they meet the stated requirements established by the
customer.
Quality Management Plan (OMP) - a formal document that
desenbes the quality system in terms of the organizational
structure, functionai responsibilities of management and
staff, lines of authority, and required interlaces for those
planning, implementing, and assessing all activities
conducted.
Quantitation Limit - the maximum or minimum level or
quantity of a target vanable that can be quantified with the
certainty required by the data user
Sampling and Analysis Plan (SAP) - a, formal document
that provides a process for obtaining data of sufficient
quality and quantity to satisfy data needs A sampling and
analysis plan consists of two parts
(a) The field sampling plan, which descnbes the
number, type, arid location of samples and the types of
analyses, and
(b) The qualify assurance prolect plan, which
describes policy, organization, and functional activities
and the data quality objectives and measures
necessary to achieve adequate data for use in planning
and documenting the response action.
Technical Review . a documented cntical review of work
that has been performed within the state of the art. The
review is accomplished by one or more qualified reviewers
who are independent of those who performed the work, but
are collectively equivalent in technical expertise to those
who performed the onginal work. The review is art in-depth
analysis and evaluation of documents, activities, material,
data, or items that require technical verification or validation
for applicability, correcthoss, adequacy, completeness, and
assurance that established requirements are satisfied
Technical Systems Audit (TSA) - a thorough, systematic.
on-site, qualitative audit of facilities, equipment, personnel,
training, procedures, record keeping, data validation, data
management. and reporting aspects of a system
Validation - an activity that demonstrates or confirms that
a process, item, data set, or service satisfies the
requirements defined by the user.
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iJ v’2 -
Sr .
— — UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
_____ WASHINGTON, D.C 20460
., / RECEIVED
AUG 14 1995 AUG 151995
OFFiCE OF THE REGIC
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The proposed Order is an important step to ensuring that EPA
programs collect and manage environmental data at quality levels
commensurate with regulatory and policy needs. Your
participation in the process of developing this Order is
essential. Please direct your comments to Nancy Wentworth,
Director, Quality Assurance Division at (202) 260-5763 by
September 18, 199.5.
Attachments
cc (w/attachments) : Nancy Wentworth, QAD (8201)
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COMPARISON OF PRINCIPAL DIFFERENCES
EPA ORDER 5360.1 (1984)
VS.
PROPOSED 1995 ORDER
1995 ORDER SECTION DIFFERENCE FROM 1984 ORDER
1. PURPOSE
Reaffirms policy established by 1984 Order. Refers to
“quality system ” as encompassing quality assurance (QA) and
quality control (QC) activities. Replaces Order 5360.1 in
its entirety.
2. BACKGROUND
References the 1984 Order. Indicates that purpose of the
new Order is to accommodate changes in Agency needs since
1984.
3. QUALITY SYSTEM IMPLEMENTATION
a. GOALS AND POLICY
Reaffirms primary goal of quality system is to provide
results from environmental programs that are of the type and
quality needed and expected for their intended use. Cites
0MB Circular A-119, Federal Participation in the Development
and Use of Voluntary Standards as the authority for invoking
the American National Standard ANSI/ASQC E4-1994,
Specifications and Guidelines for Quality Systems for
Environmental Data Collection and Environmental Technology
Programs , as the basis for the EPA quality system.
Incorporates policy that design, construction, and operation
of environmental technology must include effective QA/QC to
assure that performance of the technology meets
expectations. Identifies the EPA Quality Manual for
Environmental Programs as containing the specifications and
guidelines for implementing the Order.
b. QUALITY SYSTEM REQUIREMENTS
Defines explicitly the requirements for Agency-wide quality
systems that are to be established by all Agency components.
Particular emphasis is placed on the quality assurance
management function which must have the necessary
independence and authority to provide effective QA/QC
oversight. Requirements for quality management plans (QMP)
are defined, including the 5-year life span for approved
QMPs. Adds requirements for systematic planning for
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environmental data operations and for implementation of the
quality system in all extramural agreements funded by EPA.
Provides specifics on QA Project Plans (QAPP) for
circumstances requiring immediate action. Provides
requirements for basic training in quality management and
QA/QC concepts and practices. Identifies availability of
requirements documents and guidance documents for use in
implementing the quality system.
c. SCOPE AND FIELD OF APPLICATION
Explicitly defines applicability to extramural agreements,
including contracts, grants, and cooperative agreements, as
well as to responses to EPA regulations (e.g., permit
applications and consent agreements). Extends applicability
of quality system to “secondary data” (i.e., data collected
from other sources not by EPA or its representatives), to
environmental data pertaining to occupational safety and
health and to medical testing for substance abuse.
4. SPECIFIC RESPONSIBILITIES
a. AA/ORD
Reaffirms the role and responsibilities of the AA/ORD,
particularly in regard to the Senior Quality Management
Official delegation. Drops responsibilities pertaining to
technical activities such as “establish achievable data
quality limits...” which were not practical responsibilities
at the AA level.
b. NPO AA’s
Reaffirms the roles and responsibilities of National Program
Office Assistant Administrators for quality management.
Adds specific responsibilities to QMPs, annual reporting
requirements, and assessments. Provides requirement for A A-
level QA representatives.
c. REGIONAL ADMINISTRATORS
Reaffirms the roles and responsibilities of Regional
Administrators for quality management. Adds specific
responsibilities to QMPs, annual reporting requirements,
assessments, and interfaces with State and Indian Tribe
programs.
d. AA/OARN
Reaffirms the roles and responsibilities of the Assistant
Administrator for Administration and resources Management
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for quality management. Adds specific responsibilities to
QMPs and annual reporting requirements.
5. GENERAL RESPONSIBILITIES OF MANAGEMENT AND STAFF
New section . Provides general responsibilities for the QA
personnel and for Agency managers and staff.
a. QUALITY MANAGEMENT PERSONNEL
Defines general responsibilities for QA managers, officers,
coordinators, etc. Specifically includes QMP development,
liaison to QAD, reviews of QMPs and QAPPs, training, and
oversight.
b. AGENCY MANAGERS AND STAFF
Defines general responsibilities for all Agency managers and
staff personnel relative to quality management. Explicitly
applies to both intramural and extramural programs.
6. DEFINITIONS
Definitions have been added or revised where appropriate.
The definitions apply to terms used in the Order and were
taken from Annex A in ANSI/ASQC E4-l994.
7. REFERENCES
References were added that were specific to this Order.
8. ADDITIONAL REFERENCES
Specific references to the Quality Manual were made.
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DRAFT
POLICY AND PROGRAM REQUIREMENTS
TO IMPLEMENT THE MANDATORY QUALITY SYSTEM
1. PtJRPOSE . The purpose of this Order is to re-affirm the policy
defined by EPA Order 5360.1, April 1984, (Ref. 1) and to expand
that policy to accommodate the current needs of the Agency. This
Order replaces Order 5360.1 in its entirety.
2. BACKGROUND . Agency policy established by EPA Order 5360.1
requires participation in a centrally managed Quality System by all
EPA organizational units supporting environmental programs and by
organizations performing work in behalf of EPA through extramural
agreements. This Order re-affirms that policy and establishes new
policy and program requirements for mandatory quality systems for
the conduct of quality management, including quality assurance (QA)
and quality control (QC), for all environmental programs performed
by or for this Agency.
The Agency Quality System embraces many functions including:
establishing QA policy and guidelines for the development of
organization and project-specific quality plans; establishing
criteria and guidelines for assessing data quality; providing an
information focal point on QA/QC “tools” and new QA/QC
developments; performing management and technical assessments to
ascertain effectiveness of QA/QC implementation; and identifying
and developing QA training programs.
3. QUALITY SYSTEM IMPLEMENTATION .
a. GOALS AND POLICY. The primary goal of the EPA Quality
System is to ensure that all environmental programs produce
results, including environmental data, that are of the type and
quality needed and expected for their intended use. It is EPA
policy that a mandatory, Agency-wide Quality System be implemented
and maintained in order to assure that Agency decisions are
supported by environmental data of adequate quality and usability,
and that such data are appropriately documented and defensible.
Decisions by management rest on the quality of environmental data;
therefore, program managers shall be responsible for: (1)
specifying the quality of the data required from environmental
programs and (2) providing sufficient resources to assure that an
adequate level of QA/QC is performed. Similarly, it is EPA policy
that the design, construction, and operation of environmental
technology applied to emission/effluent control, waste remediation,
and pollution abatement be supported by an effective level of QA/QC
to assure that performance of the technology meets expectations.
In order to provide a basis for the planning, implementation, and
assessment of the EPA Quality System, an American National Standard
is invoked under the authority of Office of Management and Budget
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D.P%AFT
(0MB) Circular A-119, Federal Participation in the Development and
Use of Voluntary Standards, (Ref. 2) . It is EPA policy that all
environmental programs performed by or for EPA shall be supported
by individual organization quality systems that comply fully with
the American National Standard ANSI/ASQC E4, Specifications and
Guidelines for Quality Systems for Environmental Data Collection
and Environmental Technology Programs, (Ref. 3) incorporated herein
by reference, including all additions and supplements. This
standard addresses:
(1) Management Systems,
(2) Collection, Evaluation, arid Use of Environmental
Data, and
(3) Design, Construction, and Operation of Environmental
Technology.
ANSI/ASQC E4 is a national consensus standard authorized by the
American National Standards Institute (ANSI) and developed by the
American Society for Quality Control (ASQC).
Specifications and guidelines for implementing the requirements of
ANSI/ASQC E4 and this Order are contained in the EPA Quality Manual
for Environmental Programs (Ref. 4), hereafter referred to as the
Quality Manual.
b. QUALITY SYSTEM REQUIREMENTS. All EPA Headquarters
Offices, National Program Offices, Regions, Office of Research and
Development (ORD) Centers, Laboratories, and Offices and components
thereof, shall implement the specifications contained in the
Quality Manual in order to establish and maintain a quality system
encompassing QA/QC support to all applicable programs defined by
this Order. Each organization’s quality system shall demonstrate
conformance to the minimum specifications of ANSI/ASQC E4 and the
following:
(1) A quality assurance manager (QAM) function,
independent of direct environmental data generation, model
development, or technology development responsibility, that reports
to the senior accountable manager of the organization and that has
sufficient authority to assure independent oversight of the
implementation of the quality system in the environmental programs
of the organization. The senior accountable manager refers to the
individual responsible for the particular EPA organization or
accountable unit.
(2) Documentation of the organization’s quality system
in an approved Quality Management Plan (QMP). QMP approval shall
be valid for up to five years. QMPs shall be revised or replaced
within the five-year approval period following mission changes or
reorganizations requiring OARM approval.
(3) Sufficient resources to implement the quality system
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defined in the approved QMP. DRAFT
(4) Assessments of the effectiveness of the quality
system at least annually.
(5) Compliance with annual quality system reporting
requirements for Quality Assurance Annual Reports and Work Plans
(QAARWPs), as given in the Quality Manual.
(6) Use of a systematic planning approach to develop
acceptance or performance criteria for all environmental data
collection and environmental technology design, construction, and
operation.
(7) Approved Quality Assurance Project Plans (QAPPs) for
all projects and tasks involving environmental data with review and
concurrence having been made by the EPA QAM (or authorized
representative). QAPPs shall be reviewed and approved prior to any
data gathering work or use, except under circumstances requiring
immediate action to protect human health and the environment or
operations conducted under police powers.
(8) Acceptance criteria for the usability of
environmental data produced by models, compiled from information
systems and data bases, or obtained from the literature.
(10) Implementation of EPA Quality System requirements in
all contracts (including applicable work assignments, delivery
orders, and technical directives), assistance agreements, and
interagency agreements involving environmental programs.
(11) Provisions for training appropriate management,
technical, and administrative staff in basic concepts and practices
in quality management and QA/QC responsibilities and requirements.
Specific quality system requirements for EPA organizations are
defined in the Quality Manual. Specific quality system
requirements for non-EPA organizations (i.e., extramural agreement
holders, regulated entities, etc.) are defined in EPA regulations
and instructions for satisfying these requirements are documented
in Requirements Documents (designated QA/R-xx). Additional non-
mandatory guidance is provided in EPA Guidance Documents
(designated QA/G-xx).
c. SCOPE AND FIELD OF APPLICATION. In addition to
enviror mental programs conducted by EPA organizations, EPA Quality
System requirements defined by this Order shall apply to:
(1) Contractors under direct contract to EPA under the
authority of 48 CFR Chapter 15, Part 1546 (Ref. 5);
(2) Non-government recipients of financial assistance
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I ‘ . ‘• i
i
(e.g., Grants and Cooperative Agreements) under the authority of 40
CFR Chapter 1, Part 30 (Ref. 6);
(3) State and local governments receiving financial
assistance under the authority of 40 CFR Chapter 1, Part 31 (Ref.
7);
(4) Other Government Agencies receiving assistance from
EPA through interagency agreements;
(5) Environmental data submittals to EPA as part of
permit applications, self-monitoring under operating permits, and
consent agreements and orders, as required by EPA regulations;
(6) Environmental data collected from other sources
(e.g., literature, industry survey), compiled from computerized
data bases and information systems, and produced from computerized
or mathematical models of environmental processes and conditions,
which are sometimes called “secondary data”;
(7) Environmental data pertaining to the occupational
health and safety of personnel in EPA facilities (e.g., indoor air
quality measurements) and in the field (e.g., chemical dosimetry,
radiation dosimetry); and
(8) The collection and use of medical testing data from
Government and non-Government personnel in EPA facilities for
determination of substance abuse.
Organizations that provide objective evidence (such as a QMP,
quality manual, or audit report acceptable to EPA) of complying
fully with the specifications of ANSI/ASQC E4 are in compliance
with this Order.
4. SPECIFIC RESPONSIBILITIES . Under Delegation of Authority-I-
41, “Mandatory Quality Assurance Program” (Ref. 8), the Office of
Research and Development (ORD) is the focal point in the Agency for
quality assurance policy and ORD is responsible for developing QA
requirements and overseeing Agency-wide implementation of the
Quality System. The Assistant Administrator for Research and
Development (AA/ORD) is designated as the Agency Senior Management
Official for Quality Management. The Quality Assurance Division -
(QAD), a part of the National Center for Environmental Research and
Quality Assurance, and led by a Director, is designated by the
AA/ORD to serve as the central management authority for this
program and to assist the AA/ORD in Agency-wide matters pertaining
to quality management.
a. ASSISTANT ADMINISTRATOR FOR RESEARCH AND DEVELOPMENT.
The AA/ORD shall:
(1) Serve as the Agency Senior Quality Management
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,‘_, !-.;-‘
&il
Off icial for environmental programs conducted by EPA.
(2) Establish Agency policies and procedures for
planning, implementing, and assessing the effectiveness of the
mandatory, Agency-wide Quality System.
(3) Provide detailed requirements and guidance for
complying with this Order in the form of a Quality Manual and
general requirements and guidance documents.
(4) Review and approve QMPs from Agency components
conducting environmental programs for implementation for up to five
years.
(5) Perform periodic management assessments of all EPA
organizational units conducting environmental programs to determine
the effectiveness of their mandatory quality systems.
(6) Ensure that all ORD components and programs comply
fully with the EPA Quality System requirements, including the
preparation of QMPs and timely submissions of Quality Assurance
Annual Reports and Work Plans (QAARWPs), and that they have
adequate resources to accomplish their quality objectives.
(7) Ensure that all ORD-funded environmental programs
implemented by organizations outside EPA comply fully with the
requirements of this Order.
b. NATIONAL PROGRAM OFFICE ASSISTANT ADMINISTRATORS.
National Program Office (NPO) Assistant Administrators and Managers
shall:
(1) Ensure that all NPO components and programs under
their purview comply fully with the requirements of this Order,
including the preparation of QMPs and the timely submission of
annual reports (QAARWPs).
(2) Ensure that quality management is an identified
activity with associated resources adequate to accomplish its
program goals.
(3) Ensure that all applicable environmental programs
implemented by organizations outside EPA for the NPOs comply fully
with the requirements of this Order.
(4) Ensure that the parts of National Programs
implemented by the Regions or delegated to State, local, and Tribal
governments accord adequate priority to QA/QC, budget adequate
resources for QA/QC, and have sufficient oversight and guidance to
achieve effective QA/QC implementation.
(5) Ensure that all proposed and final regulations
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o: i I i
include appropriate QA/QC requirements for all environmental data
to be collected under the regulation.
(6) Perform periodic management assessments of NPO
organizational units conducting environmental programs to determine
the effectiveness of their mandatory quality systems.
(7) Ensure that quality management and QA/QC training
are provided to NPO management and staff.
(8) Designate QA Representatives on quality management
and QAIQC to advise and assist the AA in the planning, implementa
tion, and assessment of the quality systems for organizations under
the AA’s responsibility.
c. REGIONAL ADMINISTPATORS. Regional Administrators shall:
(1) Ensure that all Regional components and programs
comply fully with the requirements of this Order and the
specifications of the Quality Manual, including the preparation of
a QMP for the Region and the timely submission of annual reports
(QAARWPs).
(2) Ensure that quality management is an identified
activity with associated resources adequate to accomplish its
program goals.
(3) Ensure that all applicable environmental programs
delegated to State, local, and Tribal governments or performed by
organizations outside EPA pursuant to EPA mandates comply fully
with the requirements of this Order, including all organizations
receiving assistance under the Consolidated Environmental Program
Grant and State/EPA Agreement (SEA) process.
(4) Ensure that quality management and QA/QC training
are provided to Regional management and staff.
(5) Ensure that Federal agencies and State, local and
Tribal governments performing environmental data collection for EPA
have sufficient quality management and QA/QC training in order to
perform the work successfully.
(6) Perform periodic management assessments of Regional
organizational units conducting environmental programs to determine
the effectiveness of their mandatory quality systems.
e. ASSISTANT ADMINISTRATOR FOR ADMINISTRATION AND RESOURCES
MANAGEMENT.
The Assistant Administrator for Administration and Resources
Management (AP /OARN) shall:
(1) Ensure that all Administrative components and
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J3 J i—
programs comply fully with the requirements of this Order,
including the preparation of a QMPs for applicable OARM
organizations and the timely submission of annual reporting
requirements (QAARWPs).
(2) Ensure that quality management is an identified
activity with adequate resources to accomplish its quality goals.
(3) Establish, implement, and maintain a mechanism for
addressing quality system resource needs in the Agency’s planning
and budgeting cycle.
(4) Ensure that all Agency acquisition requirements or
mechanisms comply fully with the requirements of this Order.
5. GENERAL RESPONSIBILITIES OF MANAGEMENT AND STAFF .
a. QUALITY MANAGEMENT PERSONNEL. Quality management
personnel refers to individuals within the organization who are
assigned quality management duties as defined in the organization’s
QMP. These personnel include the Quality Assurance Manager who is
the designated individual within the organization responsible for
advising senior managers on issues pertaining to quality in
environmental programs and for implementing specific lead quality
management responsibilities. In some organizations, quality
management functions may be delegated to other qualified persons by
senior management. (Other titles for these functions include QA
Officer and QA Coordinator.) Specific duties and responsibilities
of all quality management personnel shall be documented in the
organization’s QMP. Specific responsibilities may include:
(1) facilitating QMP development and approval by the
organization and preparing updates to the approved QMPs within the
five-year approval period;
(2) representing the organization to QAD and other
groups on matters pertaining to quality management and QA/QC;
(3) providing expert assistance to the staff in the
organization on QA/QC policies, requirements, and procedures
applicable to procurement and technical activities;
(4) reviewing and approving QMPs and QAPPs submitted by
holders of extramural agreements;
(5) identifying QA/QC training needs for the
organization; and
(6) providing oversight of QA/QC implementation in the
environmental programs conducted by the organization.
b. AGENCY MANAGERS AND STAFF. Management shall:
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(1) Ensure that quality management is an identified
activity with associated resources adequate to accomplish its
program quality goals.
(2) Ensure that all subordinate organizational
components and programs are fully compliant with the requirements
of this Order.
(3) Ensure that all applicable environmental programs
for which management is responsible and which are performed by
outside organizations for EPA comply fully with the requirements of
this Order.
Staff shall:
(1) Ensure that all applicable intramural programs and
activities comply fully with the requirements of this Order.
(2) Ensure that all applicable extramural environmental
programs for which the staff member is responsible comply fully
with the requirements of this Order.
6. DEFINITIONS . The following terms have special meanings in
relation to this Order.
a. activity - an all-inclusive term describing a specific
set of operations or related tasks to be performed, either serially
or in parallel (e.g., research and development, field sampling,
analytical operations, equipment fabrication), that in total result
in a product or service.
b. assessment - the evaluation process used to measure the
performance or effectiveness of a system and its elements. As used
here, assessment is an all-inclusive term used to denote any of the
following: audit, performance evaluation, management systems
review, peer review, inspection, or surveillance.
c. consensus standard -. a standard established by a group
representing a cross section of a particular industry or trade, or
a part thereof.
d. contractor - any organization or individual that
contracts to furnish services or items or perform work.
e. environmental data - any measurements or information that
describe environmental processes or conditions, or the performance
of environmental technology. For EPA, environmental data include
information collected directly from measurements, produced from
models, and compiled from other sources such as data bases or the
literature, and used for decision-making purposes.
f. environmental programs - activities involving the
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q .1
3- eI- -. _ a
environment, including but not limited to: characterization of
environmental processes and conditions; environmental monitoring;
environmental research and development; laboratory operations on
environmental samples; and the design, construction, and operation
of environmental technologies.
g. environmental technology - an all-inclusive term used to
describe pollution control devices and systems, waste treatment
processes and storage facilities, and site rernediation technologies
and their components that may be utilized to remove pollutants or
contaminants from or prevent them from entering the environment.
Examples include wet scrubbers (air), soil washing (soil),
granulated activated carbon unit (water), and filtration (air,
water) . Usually, this term will apply to hardware-based systems;
however, i will also apply to methods or techniques used for
pollution prevention, pollutant reduction, or containment of
contamination to prevent further movement of the contaminants, such
as capping, solidification or vitrification, and biological
treatment.
h. guideline - a suggested practice that is non-mandatory in
programs intended to comply with a standard.
i. management - those individuals directly responsible and
accountable for planning, implementing, and assessing work.
j. management system - a structured non-technical system
describing the policies, objectives, principles, organizational
authority, responsibilities, accountability, and implementation
plan of an organization for conducting work and producing items and
services.
k. management systems review (MSR) - the qualitative
assessment of a data collection operation and/or organization(s) to
establish whether the prevailing quality management structure,
policies, practices, and procedures are adequate for ensuring that
the type and quality of data needed are obtained.
1. organization - a company, corporation, firm, enterprise,
or institution, or part thereof, whether incorporated or not,
public or private, that has its own functions and administration.
m. process - a set of interrelated resources and activities
which transforms inputs into outputs. Examples of processes
include analysis, design, data collection, operation, fabrication,
and calculation.
n. project - an organized set of activities within a
program.
0. quality - the totality of features and characteristics of
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a product or service that bear on its ability to meet the stated or
implied needs and expectations of the user.
p. quality assurance (QA) - an integrated system of
management activities involving planning, implementation,
assessment, reporting, and quality improvement to ensure that a
process, item, •or service is of the type and quality needed and
expected by the client.
q. quality assurance project plan (QAPP) - a formal
document describing in comprehensive detail the necessary QA, QC,
and other technical activities that must be implemented to ensure
that the results of the work performed will satisfy the stated
performance criteria.
r. quality control (QC) - the overall system of technical
activities that measures the attributes and performance of a
process, item, or service against defined standards to verify that
they meet the stated requirements established by the customer;
operational techniques and activities that are used to fulfill
requirements for quality.
s. quality management - that aspect of the overall
management system of the organization that determines and
implements the quality policy. Quality management includes
strategic planning, allocation of resources, and other systematic
activities (e.g., planning, implementation, and assessment)
pertaining to the quality system.
t. quality management plan (QMP) - a formal document that
describes the quality system in terms of the organizational
structure, functional responsibilities of management and staff,
lines of authority, and required interfaces for those planning,
implementing, and assessing all activities conducted.
u. quality system - a structured and documented management
system describing the policies, objectives, principles,
organizational authority, responsibilities, accountability, and
implementation plan of an organization for ensuring quality in its
work processes, products (items), and services. The quality system
provides the framework for planning, implementing, and assessing
work performed by the organization and for carrying out required QA
and QC.
v. shall - denotes a requirement that is mandatory whenever
the criterion for conformance with the specification requires hat
.there be no deviation. This does not prohibit the use of
alternative approaches or methods for implementing the
specification so long as the requirement is fulfilled.
w. user - when used in the context of environmental
programs, an organization, group, or individual that utilizes the
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C
results or products from environmental programs. A user may also
be the client for whom the results or products were collected or
created.
x. work - the process of performing a defined task or
activity (e.g., research and development, field sampling,
analytical operations, equipment fabrication) . -
7. REFERENCES -
a. EPA Order 5360.1, Policy and Progra.rn Requirements to
Implement the Mandatory Quality Assurance Program, April 1984.
b. Circular A-119, Federal Participation in the Development
and Use of Voluntary Standards, Office of Management and Budget,
1994.
c. ANSI/ASQC E4-1994, Specifications and Guidelines for
Quality Systems for Environmental Data Collection and Environmental
Technology Programs, American National Standard, January 1995.
d. EPA Quality Manual for Environmental Programs, 1995.
e. 48 CFR Chapter 15, Subpart 1546.2, “Contract Qualit y
Requirements.”
f. 40 CFR Chapter 1, Part 30, “General Regulation for
Assistance Programs for Other Than State and Local Governments.”
g. 40 CFR Chapter 1, Part 31, “Uniform Administrative
Requirements for Grants and Cooperative Agreement to State and
Local Governments.”
h. Delegation cf Authority 1-41, “Mandatory Quality
Assurance Program,” U.S. Environmental Protection Agency,
Washington,. DC, April 1981.
8. ADDITIONAL REFERENCES
This Order will be amplified by a detailed Agency Quality Manual
for planning, implementation, and assessment of the Quality System
and by requirements and guidance documents.
David J. O’Connor
Director
Office of Human Resources
and Organizational Services
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UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
A WASHINGTON. 0 C. 20460
APR 17 1984
O IC( OY
YNC AOMSHI$TAAYON
MflIOR JM
SUBJECr: EPA Order 5360.1, “Policy and ?rc r n Require nts to
Impl tient the Quality Assurance Progr ”
EI t1: Alvin L. Aim C 2 L . Zrc_ ..
puty iministrator
TO: Pddressees
One of my major goals is to ensure that all decisions by EPA can be
supported by a sound data base. ? 1 n irr ortant step toward achieving this
objective is to require that quality assurance becat e an integral part of
all data collection activities. ( iality assurance is the total integrated
prcqr for assuring the reliability of envirorrnental n asure nts and
consists of multiple steps undertaken to ensure that all acquired data
are suitable for the user’ s intended purpose. T of the major steps are:
the user must first specify the quality of data he needs; then the degree
of quality control necessary to assure that the resultant data satisfies his
specifications rm.zst be determined. Central to this process is assuring that
the data is of known quality. The quality of data is kr n when all CCTT-
nents associated with its derivation are thoroughly docunented, such
docunentation being verifiable and defensible.
In order to establish quality assurance solidly in all data collection
activities, the important step of issuing this order on quality assurance
is being taken. The Liçl rentation àf the el nents in this order will
require dedication and hard work by the Quality Assurance Management and
Special Studies Staff, by quality assurance officers throughout the Açency,
and by senior management. This order identifies the goals, objectives, and
general responsibilities of each pr rain area. Ib carry out the order,
specific policy and technical guidance materials need to be prepared. I
will be following that pr ress.
The attached order reflects my cam itment to the Psgency’ s QA proran
and to the prai otion of good science in all EPA rtcnitoring and measurement
activities. Therefore, I exect that each of you work cooperatively to
ensure that the appropriate level of quality assurance is embedded in all
data collection undertaken by or for the P ency.
Attachnent
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&EPA TRANSMITTAL’
CL& IFICAT10N NO.:
AP?ROVAL. DATE:
5360.1
4 / 3/84
AOORE EE
EPA ORDER 5360.1 —- POLICY AND PROGRAM REQUIREMENTS TO
IMPLEMENT THE MANDATORY QUALITY
ASSURAWCI PROGRAM
1. PURPOSE . This transmittal provides a new EPA Order 5360.1,
Policy and Program Requirements to Implement the Mandatory
Quality Assurance Program.
2. EXPL.ANATION . This Order establishes policy and program
require nents for the conduct of quality assurance (QA) for all.
environmentally related measurements performed by or for this
Agency.
3. SUPERSESSION . None
3. FILING INSTRUCTIONS . File the attached in a three ring
binder. Post receipt of Transmittal on Checklist in front of
the binder.
ORIGINATOR:
M gement and ganization Division
Office of Research and Development
EPA Foq,,i 1316-12 (Mi . 2) REPLACES EPA FORMS 1315.IA AND THE PR(V$O EO’T’ON )F 1315.13.
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EPA ORDER 5360.1
APR 3 84
LICY AND PRX AM RE JIB 4 S
TO IMPLE> ’ZT ThE MANDP TOR? QUALITY ASSURANCE P RAM
1. PURPSE . This Order establishes policy and pr r requir rents for the
conduct of quality assurance (QA) for all envirorri ntally related asurer ents
performed by or for this Agency.
2. BAO(G UND . gency policy requires participation in a centrally managed
QA prng r m by all EPA organizational units supporting envirorrr ntal ly related
measur nents. Under Delegation of Authority 1—41, Mandatory Quality Assurance
Prngr n” (dated 4/1/81), the Office of search and Develop ent CORD) is the
focal point in the P gency for quality assurance policy and is responsible for
developi ng OA requirements and overseeing gencywide iriçlernentation of the QA
progr . ORD established the ality Assurance Manag ent and Special Studies
Staff (QAMSS) to serve as the central manag nt authority for this program.
The OAMSS activities involve the develop ent of policies and procedures; co-
ordination for and direction of the in 1ementation of the agency QA prora ;
and review, evaluation, and audit of progran activities involving envirocr ntal
rr nitorLng and other types of data generation.
The ency QA program embraces many functions including: establishing QA policy
and guidelines for deve1op nt of progran and project operational plans; establishing
criteria and guidelines for assessing data quality; serving as a OA information focal
point; auditing to ascertain effectiveness of QA inçlementation; and identifying and
developing OA training projr ns.
3. GQ .LS AND POLICY . The primary goal of the QA progran is to ensure that
all enviroc nta1ly related measurenerits supported by the EPA produce data of
kn n quality. The quality of data is ki m when all car onents associated
with its derivation are thorcnr hly docunertted, such doci.inentation being verif i—
able and defensible. It shall be the policy of all EPA organizational units to
ensure that data representing enviror enta1ly related measurenents are of kn n
quality. Decisions by management rest on the quality of envirorinental data;
therefore, progran managers shall be responsible for: 1) specifying the quality
of the data required fran enviror ntal1y related measurements and 2) providing
sufficient resources to assure that an adequate level of QP. is performed.
All routine or planned projects or tasks involving envircrr ntally related
measurements shall be undertaken with an adequate QP project plan that specifies
data quality goals acceptable to the data user and assigns responsibility for
achieving these goals.
In discharging its responsibility for iu leT nting the ? 1 ency-mandated ia1ity
Assurance Program, the ORD/ONISS will strive for consensus by su nitting for
review proposed policies and procedures to affected progran offices and regions.
sponsibility for adjudication of unresolved issues, with respect to the above
and QAMSS conducted audits, will be at the 1 st level of authority consistent
with the scope of the issues. The CW 5 will refer issues which remain Un-
resolved at I r levels of authority to the MIORD for decision, after COfl-
sultation with the appropriate AA or RA.
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5360.1
APR 31984
The foll ing activities are basic to the inpl ntat ion of the O program:
a. Preparation and annual çdate of a QPi program plan based on guidelines
stab1ished by ON’tSS.
b. ve1oprent of a Q project plan for all projects and tasks involving
enviroru entafly related asur nt5 in accordance with guidelines established
by MSS.
c. Assuring thplerentatiOfl of for all contracts and financial assistance
involving envircc nta1ly related rreasureiT ntS, as specified in a çlicab1e EPA
regulations, including s contracts and subagre nts.
d. Conducting audits (systan, performance evaluations, data quality, bench,
etc.) on a scheduled basis of organizational units and projects Involving environ-
n ntally related asur nts.
e. C ve1cçing and adopting technical guidelines for estimating data quality
in terms of precision (variability) 9 bias (accuracy), represent.ativeneSs,
ca pleteness and ccxr arability , as appropriate, and incorporating data quality
requir nents in all projects and tasks involving environir entally related
u asurefnentS.
f. Establishing achievable data quality limits for xi thods cited in
regulations based on results of metha s evaluations arising fran the ri ti ds
standardization process, e.g., ASIM Standard D2777—77.
g. Lip1 nentation of corrective actions, based on audit results, and for
incorporating this process into the manage nt accountability system.
h. Provision for appropriate training based on perceived needs, for all
levels of managerT nt, to assure that O responsibilities and requiren nts are
understocxi at every stage of project inp1e ntaticn.
4. R FCt SIBILITIES .
a. In conformity with the oversight responsibility for the mandatory
program, the M/C D shall:
(1) Establish P ency policies and procedures for inç1a nting the
mandatory OPi program.
(2) Provide guidance for determining precision 9 bias, representatiVeneSs
catpleteness, and axtparability of data.
(3) Review Q Program Plans fran agency ccxçonents involved in
envircnn ntally related n asure nts.
(4) Conduct O audits of all organizational units s.çporting environ—
n ntally related asu nts based on established audit criteria and procedures.
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EPA 5360:1
3 re ..
(5) Reco nd corrective acticris, based on a .xi1 t results, for incl ion
in the manageTent aCoDlrttability syste!U.
(6) Establish achievable data quality lUnits for iTethais provided by ORD
for citation in regulations, based c i i r sults of rr thcds evaluations arising fran
the neth s standardization process, e.g. AS D1 Standard D2777—77, to help pro)ect
officers define data quality goals.
(7) Serve as the ency QP information focal point.
‘(8) velcp generic training prcçran , based on perceived needs, for all
levels of manage nt to assure that Qk responsibilities and requirerents are
Lxlderstccd at every stage of project ixTplerentation.
(9) Ensure that all ORD investigations involving data collection are
covered by an acceptable O plan with resources adequate to accci!plish program
objectives.
(10) Ensure that deficiencies highlighted In review of ORD program plans
or in audits of ORD ca çonents are appropriately addressed.
b. In accordance with policies and procedures established by WORD,
National Program Managers shall:
(1) Ensure that is an identifiable activity with associated resources
adequate to accc riylish program goals in the develoçxTent and execution of all pro-
jects and tasks, both intramural and extramural, involving envirorirentally related
rteasurerrents.
(2) Ensure that appropriate QP criteria are included in operating guidance.
(3) Establish data quality acceptance criteria for all projects and tasks
conducted by the program office.
(4) Ensure that an adequate degree of auditing is perforired to determine
ca!pliance with requirerrents.
(5) Ensure that deficiencies highlighted in audits are apprcpriately
addressed.
(6) Ensure that all projects and tasks involving environirentally related
treasurerrents are covered by an acceptable QA project plan and that the plan is
inçle T ented.
(7) Identify program—specific QA training needs and provide for the
required training.
c. In accordance with policies and procedures established by M/ORD, gional
ninistrators shall:
—3—
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EPA ORC 5360.1
-R 3i 2:;
(1) sure that OPi is an adent if ia le activity with associated resources
adequate to ac . llsh progran and regional goals in the aeve1oçir nt and execution
of all pro)eCtS and tasks thvolving envirc irnenta1ly related rreasurerrents, th
intr tural and extramural.
(2) Ensure that CA guidelines are specified for estin ting data quality
in ter is of precision 1 bias, representativeness. ca p1eteness and carparability.
for all environuentally related rreasuren nts which rr et the operating guidance
established by the program offices.
(3) Establish data quality acceptance criteria for all projects and tasks
initiated by the Region.
(4) Ensure that all projects and tasks involving envirocurentally
related rteasurerrents are covered by an acceptable CA pro)ect plan and that the
plan is iirçlerrented.
(5) Ensure that an adequate degree of auditing is perfor ted to deterr e
coapliance with CA requir nts.
(6) Ensure that deficiencies highlighted in audits are corrected
expeditiously.
(7) Identify program—specific CA training needs and provide for the
required CA training.
d. The AA for P ninistration shall establish a rrechani n for incorporating
CA in the Agency’s planning and budgeting cycle.
5. tEFINITICt S . The following terrr have special n anings in relation to this
Order.
(a) Dzct ntation . The use of doc entary evidence; a written record
furnishing inforn tion that a procedure has been perforrred. When applied to
enviror tentally related neasuren’ents it includes all calculations related to
sai!çling design; all steps in the chain of custody, where appropriate; and
all notes and raw data generated in the salTpling, analysis, or data validation
process.
(b) C fensible . The ability to withstand any reasonable challenge related
to veracity or truthfulness.
Cc) Environ enta1ly Related Measu ient . Any laboratory or field data
gat hering activity or investigation involving the determination of chemical,
physical, or biological factors related to the enviror nt.
The following are representative exazTples of enviror Tentally related
ueasurer nts. t ta collection or investigation of chemical, physical. or biO
logical factors for determination of:
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EPA 5360.1
.. 3i; ,,
(1) pollutant concentrations fran sources, in the ax ient envjrc nt,
or pollutant transport and fate;
(2) response of organist to pollutants;
(3) the effects of pollutants on hut n health and on the enviror nt;
(4) risk/benefit analysis;
(5) envirc i ntal or eccr iic thpact.
(6) the enviroarental iitçact of cultural and natural processes;
(7) pollutant levels, exposure levels, etc., used In !To:ieling.
Cd) Organizational Unit . My a ninistrative entity (national proram
office, regional office, C D or IC la ratory) which engages In envirorii ntal1y
related iteasureitents.
(e) Project . An organized i dertaking or specified .u it of investigation
involving env iror ental1y related asurie nts.
(f) C*iality Assurance . The total integrated .prograrrt for assuring the
reliability of rrcnltoring and xreasurerr nt data.
(g) Verifiable . The ability to prove or substantiate any claim or result
related to the doct.z nted record.
6. AtOITI 4AL REFERE CE . This Order will be azrplified by a detailed irrçleTen—
tation plan.
I iard 4. Messner
Assistant Aáninistrator
Office of A ninistrat ion and Resources Manag reflt
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Attachment B
‘Region I Tiered Organic and Inorganic Data Validation Guidelines”,
July 1, 1993, DRAFT
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DRAFT
REGION I
TIERED ORGANIC M INORGANIC DATA VALIDATION GUIDELINES
JULY 1., 1993
fl TRODUCTI ON
Historically, Region I has required that analytical data for
Superfund sites undergo full validation according to the Region I
Laboratory Data Validation Functional Guidelines documents.
Full validation, however, does not always meet the Data Quality
Objectives (DQOS) for each site activity, and it can contribute
to high costs and missed deadlines. To address this problem,
Region I ’s Environmental Services Division (ESD) has created a
tiered approach to data validation which accomplishes the
following:
o enables data users to select the level of validation
necessary to meet their CQOs
o saves time and money
o promotes consistent evaluation of data quality between
Superfund sites
Three tiers have been established and are described in the next
section. Tier III is equivalent to the full validation currently
performed in Region I, and includes the procedures performed
under Tiers I and II.
TIERED PPROACK TO DATA VALIDATION
The inorganic and organic data validation process can be broken
down into three distinct levels: Tier I, Tier II, and Tier III.
Tier I : A completeness evidence audit is performed to
ensure that all laboratory data and documentation are
present. Completeness evidence audits are performed in
accordance with procedures contained in the Region I CSF
Completeness Evidence Audit Proqra!n , dated 7/3/91. (This
document is the currently used procedure as referenced in
the memorandum titled suRegion I CSF Completeness Evidence
Audit Program t ’ from the Region I CLP-TPO5 to Region I
Contractors, dated 7/7/91.)
Tier II : A Tier I completeness evidence audit is performed,
and, in addition, the results of all Quality Control (QC)
1
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DRAFT
checks and procedures are evaluated and used to assess and
qualify sample results. Tier II data validation is
performed primarily from information contained on the
tabulated data reporting forms. It has been estimated by
ESD that Tier II validation takes 50% of the time required
to perform a Tier III validation.
Tier III : A full data validation is performed. Tier III
includes Tier I and Tier II procedures plus an in-depth
examination of all raw data to check for technical,
calculation, analyte identification/analy-te quantitatjon,
and transcription errors. Tier III data validation is
performed in accordance with the Region I CSF Completeness
Evidence Audit Program and the Region I Laboratory Data
Validation Functional Guidelines.
At a minimum, all data should be carried through Tiers I or II .
Tier I is mandatory, regardless of the immediate intended use of
the data, to ensure that all laboratory documents have been
obtained for future data validation, potential litigation. ar.dlor
to defend site decisions. Validation recTuirernents must always be
documented in an approved OAPP prior to sampling . Several
examples of when a Tier I or Tier II validation may suffice to
meet DQOs are as follows:
o Design run data which are collected during a
treatability study. Data used to support the final
design parameters, however, should undergo Tier III
validation.
o Long—term monitoring data which have only “minimal
changes” in constituent concentrations from the
previous round. The magnitude of these allowable
changes, as well as the procedures to be followed if
QAPJP requirements are not met, must be documented in
an approved QAPJP prior to sampling. (If QAP 3 P
requirements are not met, a Tier II or Tier III
validation should be performed.)
o EPA oversight split data which “compare well” with PRP
data. The comparison criteria, as well as procedures
to be followed if QAPJP requirements are not met, must
be documented in an approved QAPJP prior to sampling.
(If QAPJP requirements are not met, a Tier II or Tier
III validation should be performed.)
Full validation (Tier III) can always be performed at a later
date as long as Tiers I or II have been initially completed. The
entire data package (Tier III) or just individual parameters,
matrices, sample locations, and/or risk compounds (partial Tier
III) could then be specified for full validation. If a si bset of
2
-------
DRAFT
the entire data package was targeted for full validation, then a
Tier II validation would be performed on the entire data package
(if it hadn’t already) and a partial Tier III validation would be
performed for individual parameters, etc. (whatever was to
comprise the subset validation). The first paraqrapFi of the data
validation memorandum must explicitly document the level of
validation performed, i.e. Tier II plus partial Tier III
validation for benzene, Tier II plus partial Tier III validation
for sample location MW—lOO, Tier II plus partial Tier III
validation for volatile organics, etc.
In certain circumstances, full validation (Tier III) may be
deemed necessary from the start of a project. Several examples
of when full validation is needed are as follows:
o Only one set of data for a particular sample location,
type and/or parameter is available and a decision of
whether to remediate will be based on this sample. An
example of this is background data.
o The data will be used to define a critical site
boundary.
o The data will be used to determine compliance with
clean—up goals.
TIER II DATA VALIDATION PROCEDURE
To perform a Tier II data validation, a Tier I review is
completed and the results of all QC checks and procedures are
evaluated and used to assess and qualify sample results. During
a Tier II review, the raw data for field samples and QC checks
are not evaluated (with a few exceptions, i.e. pH check for
volatile organics, metals, and cyanide to verify proper sample
preservation). The goal is to validate data using information
contained mainly on the tabulated data reporting forms and chain—
of-custody (CCC) forms. Tier II assumes that all results are
reported by the laboratory and that al]. reported results are
correct .
Prior to performing a Tier II validation, conduct the Tier I
completeness evidence audit according to the requirements
contained in the Region I CSF Completeness Evidence Audit
Program, dated 7/3/91, and request the missing deliverables from
the laboratory. Begin the Tier II validation while waiting for
any missing deliverables.
To perform a Tier II inorganic validation, the reviewer must
have all data reporting forms for field sample and QC sample
results (Forms I through XIV), as well as the CCC forms in the
data package. Validation is performed according to requirements
3
-------
DRAFT
contained in the attached table (Attachment I) and in conjunction
with the Region I Laboratory Data Validation Functional
Guidelines for Evaluating Inorganics Analyses, dated 6/13/88
(modified 2/89). This guidance is also applicable to inorganic
analyses performed in accordance with the ILMO1.O, ILMO2.O, and
ILMO3.O versions of the U.S. EPA CLP Statement of Work (SOW).
Tier II reporting and deliverable requirements are the same as
those for full validation (Tier III); only the actual validation
procedures contained in Section 3 of the Region I Functional
Guidelines have been modified to minimize examination of the raw
data and to eliminate the recalculation of results.
To perform a Tier II organic validation, the reviewer must have
all data reporting forms for field sample and QC sample results
(Forms I through X), as well as the CCC forms in the data
package. Validation is performed according to guidance contained
in the attached table (Attachment II) and in conjunction with the
Region I Laboratory Data Validation Functional Guidelines for
Evaluating Organics Analyses, dated 2/1/88 (modified 11/1/88).
This guidance is also applicable to organics analyses performed
in accordance with the OLNO1.O SOW, even though the 11/1/88
Region I Functional Guidelines document has not yet been modified
to accomodate pesticide/PCB method changes contained in the
OLMO1.O SOW. Tier II reporting and deliverable requirements for
data validation are the same as for full validation (Tier III);
only the actual validation procedures contained in Sections 3 and
4 of the Region I Functional Guidelines have been modified to
minimize examination of the raw data and to eliminate the
recalculation of results.
The results for each QC parameter, specified in Attachments I and
II, must be evaluated using the data reporting forms provided by
the laboratory. The data provided on the forms are not verified
with the raw data. Information contained on the forms should be
used to verify that QC samples were analyzed with the correct
analytes at the proper frequency and concentration, that the QC
limits were met, and required corrective actions were taken. The
QC parameters of System Performance and Compound Identification
for the volatile and semivolatile fractions are not evaluated
during the Tier II review as it would require that a substantial
review of the raw data be performed.
As a result of the Tier II evaluation, the field sample results
may be accepted, qualified as estimated, or rejected.
circumstances where the entire data tacka e or data for multiple
samples must be re-jected or will be significantly gualif led based
upon the Tier II results, the reviewer must first consider the
impact of re-jected results and/or discrepant information on the
data needs of the specific prolect. If the data are critical to
the ro1ect needs, then examination of the raw data is strongly
recommended to prevent faulty site decjsjons based on technical,.
transcription, and/or calculation errors. The EPA Remedial
4
-------
DRAFT
Prolect Manager (RPM) or Site Assessment Manager (SAfl) must be
contacted to approve a partial or complete Tier III valjdat ,on
prior to its j itjatiofl . If the RPM or SAM decides that no
further validation is warranted based on the objectives of the
sampling event and the nature of the data qualification, then the
reviewer should document this decision in the first arpqraph of
the data validation (DV) memorandum. The nature of the data
problem, the extent of data qualification, and the level of
validation performed must also be documented in the DV
memorandum. It is expected that raw data review might be
required more frequently for pesticide/PCB data, since
identification and quantitation of pesticides and PCBs is based
solely on gas chromatography data with no mass spectral
confirmation/quantitatiOn.
The attached tables, Attachment I (Tier II Inorganic Data
Validation) and Attachment II (Tier II Organic Data Validation),
consist of four columns which identify the specific QC criteria
to be checked, the laboratory reporting form(s) to review, the
specific sections of the Region I Functional Guidelines to
follow, and the adjustments needed for the specific sections of
the Region I Functional Guidelines to perform a Tier II
validation.
5
-------
ATTACHMENT I
TIER II INORGANIC DATA VALIDATION
-------
TIER II INORGANIC DATA VALIDATION
DRAFT
I of 3
QC CRIrERIA
DATA RL ORT1NO FORMS TO REVIEW
APPUCABLE SECTIONS IN FUNCTIONAL
f luiD EL INES+
Data Complehlle3a
• Complete SDO File (CSF)
I. Original Simple Data Package
Including Cover Page, Form, I through
XIV, DC-i, DC-2, raw d i i.
2. Original ahipping and receiving
document.
3. All original lab record, of sample
iranafcr, preparation and an.alyaia, as
well a. telephone contact log..
• I • p. 21
• Perfonn a Tier I complclenc.. cvidcncc audit
according to pruccdurcain the Pcgion CSF
C mpIctcne ., Evidence Audit Program, dated July
3, 1991, to enwee that all laboratory data and
documergation are pre .cnt. Reque g .a 1g g
dclivenble, front the laboratory following
appropriate procedure..
holding Thnri
• Forms I, XIII, XIV
• Chalo-of -CuuiodyITr iflic Report
• Simple DigcstionlDiatillatlon Log a
• II. A through D. pp. 21-22
• Examine Cha ln-o(-Cua*odyfTraflic Report Forms to
determine if sample. were properly preacrvcd In the
field.
S To verify sample ph upon laboratory receipt,
review sample digcatio 0 log, ia thu Information Is
not included
the forms.
Calibrat loa
• Forms UA. 1W, XIV
• Ill. A through B. pp. 22-23
C.l-3, pp. 23-24
C i and 6, p. 24
C.8anJ9,p.24
D.I .3. pp. 24-25
I) 5.8. pp. 25-26
on
• Calibration correlation coefficient. for AA, hg, and
CN arc not reviewed aince thu Information is out
Included on the forms.
1
.
BL n& s
• Forms I. HI, X, XII !, XIV
• hain-oiCus*ody/Traflic Report
S IV. A through D, pp. 26.28
.
• Review d.ta reporting form, only. Do not verify
with raw data.
ICP Interfereoee Cbeck Sample
• Forms!. IV, X, XI, XIV
• V. A through B. p. 28
C.! and 2. p. 28
C.4, p. 29
D, pp. 29-31
S Review data reporting forms only. Do not verify
with raw dali.
• Paragraph C.4: For evidence of rceulia with an
ab.oluto value >2xlDL (or those anslylc. which
arc not present In the ICS A solui ion, evaluate
Form IV. Do not check the
SEE NOTE ON PAGE 3 OF 3.
+ft lON I LABORATORY DATA VALIDATION FUNCTIONAL GUIDEI.INES FOR EVAlUATING INORGANICS ANALYSES. 6113188, MODIFIED 2/89
-------
DRAFT
TIER II INORGANILpATA VALIDATION
CRITERIA DATA REPORTIHO FORMS TO REVIEW
S
APPLICABLE SECTIONS IN FUNCTIONAL
GU IDELINES+
COMMENTS
Sample A alytIi S Forms VA. VB, XIII
• Chain-of-Cuaiodytrnarnc Report
S VI. A through B. pp. 31-32
C I. p. 32
C 3-5, p. 32
D, pp. 32-33
S Review data reporting funns only. Do not vcnIy with raw
data.
5 Review Chain-of-Custodytrraflic Report Forms to venfy
that s.anpks Idcniificd a. field blanki arc not u.c4 (or
spiked umple aiuiysi..
Sample Analyali • Fonns VI. XIII
• cli.in-or-CuMody!rrarnc Report
• VII. A through U, p. 33
CI, p.33
C 3 and 4. p. 34
D. p. 34
• Review data reporting form, only. Do not vcr fy with raw
data.
5 Review Chain-of.CuModyfTraflic Report Forms to verify
that samples Identificd a. field blanka arc not u&cd (or
duplicate samplo analysis.
Duplicatci S Form Is
• Chain-of Custody /Traffic Report
S VIII. A through D. pp. 34-35
• No change (mm current proccdurca.
Sample An9JysIs S Forms VII, Xlii
• IX. A through B, p. 35
C.I, p. 35
C.3. p. 36
D, p.36
• Review data reporting forms only. Do not verify with raw
data.
Absorption Analysis S Forms I, VIII. XIII, XIV
S X. A through B, p. 37
C.I and 2, p. 37
C.4. p. 37
D, pp. 37-38
• Review data reporting forms only. Do not verify with raw
data.
5 Review Form Ta (or the prca.encdabacncc of ‘M (laga
indicatIng the failing/psuing o(the duplicate injc 9 .ioo
prcciaion criteria (or Acid .amplea.
• Do not verify post-digestion spike recoveries rcpoiud on
Form XIV with the raw data.
• To verify that the Furnace Atomic Absorption Analyiis
Scheme was followed, cvslusta Form XIV (or spike
recoveries not withIn 85-115%, InItial and rcan.alysc., and
dilution (actors. In addition to Form XIV, evaluate Form I
(or sample concentrations to verify that an MSA analysis
WI’ not rci uired (or any result quanlitaled directly from the
calibration curve and (or which apike recovenea were not
within IS-I 15%.
Dilution Analysis • Forms IX, X, XIV
S XI. A through B. pp. 38-39
CI, p. 39
C 3. p. 39
I), p. 39
5 Review data reporting forms only. Do not verify with raw
data.
• Paragraph C 3: For vidcnce of negative Interference.
evaluate Form IX. Do not check the raw data.
SEE NOTE ON PACE 3 0F3.
+HECION I LABORATORY 1)ATA VALIDATION I1JNCTIONAI. GUIDEI.INES FOR EVALUATING INORGANICS ANALYSES, 611318$, MODIFIED 2/89
-------
‘._.I... a
TIER II INO WANIC DATA VALIDATION 3 o(3
QC CRfTERIA
DATA REPORTING FORMS TO REVIEW
‘
,APPLICABLE SECTIONS IN FUNCTIONAL
GUIDELINaS+
c ) ij.ii pcrs
I Farina . . viii .
• Xii. A throu&i D, pp 39-40
• Paragraph C 3: To venly that lampic weighia.
voiume,• and dilution. are takc iIUo account when
reporting sample qu ntoatIoo limit.. cvatuatc Form.
I. X Xfll. and XIV.
S aupie Reault Vedfkatloa
.
• Form. I, XII, X 111 XIV
• XIII. A through B, pp. 40-41
C.3, p. 41
D . p. 41
• RevIew data rcpoatng form. only. Do no venfy
4ij raw data.
• For any rciaiit repoated on Form I (or which the
sample result Ii greater thin the linear range (or
IC? (Farm XI I) and greater thau the calibrated
range (or non-IC? parameters (Form XIV), ‘verify
that the result was repoded from a diluted sample
analysis (Form XIV) and that iii. diluted aamplo
result (.11. wIthin the rcqecIIvc range.. DilutIon
and preparation factors are found on Form. X I II
andXIV. Donoecbeekthcrswdga
Overall A.u smeiit of Dala (era Ca ..
I XIV., p. 42
• Umit to the sccdona cvatuated during Tier U
review.
NOTEt IN CIRCUMSTANCES WhERE TIlE ENTIRE DATA PACKAGE OR DATA FOR MULTIPLE SAMPLES MUST BE REJECTED OR WILL BE SIGNIFICANTLY QUALIFIED BASED UPON TIlE TIER
II RESULTS. TIlE REVIEWER MUST FIRST CONSIDER TIlE IMPACT OF REJECTED RESULTS AND/OR DISCREPANT INFORMATION ON TIlE DATA NEEDS OF THE SPECIFIC PROJECT. IF TIlE
DATA ARE CRITICAL TO TilE PROJECT NEEDS 1 THEN EXAMINATION OF TIlE RAW DATA IS STRONGLY RECOMMENDED TO PREVENT FAULTY SITE DECISIONS BASED ON TEChNICAL,
TRANSCRIPTION, ANDIOR CALCULATION ERRORS. TIlE EPA MEMKI)IAL PROJECT MANAGER (RPM) OR SITE ASSESSMENT MANAGER (SAM) MUST BE CONTACTED TO AP?ROVE A PARTIAL.
OR COMI ’I.ETE TIER III VALIDATION PRIOR TO ITS INITIATION.
+KECION I LABORATORY DATA VALIDATION FUNCTIONAL GUIDELINES FOR EVALUATING INORGANICS ANALYSES, 6113/88. MODIFIED 2/89
-------
ATTACHMENT II
TI II ORGANIC DATA VALIDATION
-------
TIER II ORGANIC DATA VALIDATION
DRAFT
QC CRfl RIA
DATA REPORTINCI FORMS TO k VIEW APPLICA LU SECTIONS IN FUNCTIONAL
I OIJIDELINES+ I
c -
‘
Data Coinpiedroet
• Complete SDCJ File (CSF)
I. Original Sample Data Package
including Cover Page, Forms I through
X DC-I, DC-2, isv dat.
2. Otigln.sl shipping and receiving
document.
3. All original lab record. of sample
transfer, prcpsratlon and analyiis, a.
well as telephone contact logs.
• Perform a Tier I compleicnes. evidence audit
according to procedures In the çgjon I CS 1
ComnleKnci . Evidence Audit Prnaram. dated July
3, 1991. to ensure thai all laboratory d iii and
documentation are prcacnt. Request missing
deliverables from lbs laboratory following
appropriate procedures.
holding llmai
VOA & SVOA
S Form I.
• ChaIn of Custody! Traffic Repoit
S SDQ N.mtlv.
• I. A through D, pp. 21-22
5 ExamIne Cb.lnef-cu.todytrraflic Rcpojl Forms to
determine if sample. were properly preserved In the
field.
• To verity sample p11 upon Laboratory receipt,
review the SDO Nareativo as this information Is — I
included on the (onna.
S . A through D, p 48
PcstJPCB
GC!MS Timing
VOA & SVOA
S Form Vs
• U. A through B, pp. 22-23
C.3.s and c, p.23
1), pp. 24-26
• RevIew data tepoiting forms oniy. Do not verity
wIth raw dali and do not recalculate rcportçd
value..
Calibr,doa
VOA & SVOA
S Forms IV, VI, VII
• III. A through B, pp. 26-27
C.l a.2, p. 27
C.l.b.2, p.28
C.2.s.l, p. 28
C.2.b.2 , p. 29
D, pp. 29.30
• Review dais repoitleg forma only. Do not verity
with raw data. Do not recalculate %RSD, RRF or
%D value..
• Review Form IV to dctermlno the sample.
auocisicd with each calibration.
Instnam t Faformance!Calibratloia
PcstJpCO
S Forms VI, VII, VIII, IX
. II. A. p. 49
B 1-4, pp. 49-51
C through D, pp. 51-54
• Ill. A through B. pp. 54-55
C.l.c and a, pp. 55-56
C.2, p. 56
D, p. 56
• Review data reporting forms only. Do not verify
with raw dat. and do not recalculate reported
value..
SEE NOTE ON PACE 3 0F3.
+REGION I LABORATORY DATA VALIDATION FUNCTIONAL GUIDEI.INES FOR EVALUATING ORGANICS ANALYSES, 211188, MODIfiED 1 111188
I of 3
-------
SEE NOTE ON PAGE 3 OF 3.
+REGION I LABORATORY DATA VALIDATION FUNCTIONAL GUIDELINES FOR EVALUATING ORGANICS ANALYSES, 2!I/8 8, MODIFIED 1111188
TIER II ORQA i’
A VALIDATION
- 2 o(3
DRAIf
QC CRITERIA DAJ A REPORTING FORMS TO REVIEW
II -
APPLICABLE SECTiONS IN FUNCTIONAL
GUIDELINE.S+
COMMENTS
BLiwk.s
VOA&.SVOA
• Forms I, IV
S Cliaino(Cua*odylTraflic Report
S IV. A through B, p. 30
C2. pp. 30-31
1), pp.31-33
5 Rcvicw data reporting (arms only. Do not verify with raw
data.
Pcs tJPCB
• IV. A through B. p. 57
Cl and 3, p. 57
1), pp. 57-59
Surrogate Recovery
VOA & SVOA
• Form II .
• V. A through B, pp. 33-34
C.2 i-c, p.34
C.3.i-c, p. 34
0. pp. 34-35
S Review da t . reporting forms only. Do not venfy with raw
dais.
.
S V A through B, p. 59
pp. 59- 60
PciIJPCB
Matrix Spike & Matrix Spike Dup&ste
VGA & SVGA
S Forms I, III
S VI. A through B. pp. 35.36
C.I and 3, p.36 .
0, pp. 36.37
S Review diii reporting forms only. Do not verify with raw
dati.
Pcat/PCB
• VI. A through B, p. 60
C.I and 3, pp. 60 -6 1
U, p.61
FIeld Duplicates
VOA & SVGA
S Form Ia
• Cbain of Custody! Traffic Report
• VII. A through 0, pp. 37-38
• No change from curre procedure..
S VII. A through 0, pp. 61-62
Pcs*JPCB
Iotein . .I Sgandarda I’erforwanc.
VOA & SVGA
• Form VIII.
5 VIII. A through B, p. 38
C .2 and 3, p. 38
0, pp. 38-39
5 Review data reporting forms only. Do not verify with raw
data.
Compound IdentIfication
VOA & SVGA
—
• Not cvaluaied during Thr U review.
PcatJPCS
S Forms I, X
S VIII. A, B, pp. 62, 63
C, 0, pp. 63, 64
• Review dais rcporting (aims only. Pu not verify with raw
dat..
-------
DRAFT
TIER II ORUANIC DATA VALIDATION
CRT ERJA DATA REPORTING FORMS TO REVIEW
APPLICABLE SECTIONS IN FUNCTIONAL
GUIDEL INES+
‘
& Reported • Form Ii
UmIt . S SDQ Nsmiivc
SVGA
X. C.4. p. 41
0, p. 41
• Only reported qusniiisiion limits can be evaluaicd
during a Tier II review.
• Review the SDO Narrative to identify a J explain
soy anomalics on the Form Is. Qualify data
accordingly.
• Review dat . reporting fonna only. Do Dot verity
with raw dais.
IX. C.2. p. 64
0, pp. 64-65
Coezipotind. • Fomi I.
SVGA
—
• Verily th.t target compounds arc not reported as
TIC. in another fraculon.
Performance —
SVGA
—
.
• Not evaluated during Tier U review.
of Data for a Cia. 1
I
LImit to the sections evaluated during Tier II
review.
NOTEt IN CIRCUMSTANCES WhERE TIlE ENTIRE DATA PACKAGE OR DATA FOR MULTIPLE SAMPLES MUST BE REJECTED OR WILL BE SIGNIFICANTLY QUALIFIED BASED UPON TIlE TIER
II RESULTS, TIlE REVIEWER MUST F1RS CONSIDER TIlE IMPACT OF REJECTED RESULTS AND/OR DISCREPANT INFORMATION ON TIlE DATA NEEDS OF TIlE SPECIFIC PROJECT. IF TIlE
DATA ARE CRITICAL TO TIlE PROJECT NEEDS, THEN EXAI 1INATION OF TIlE RAW DATA IS STRONGLY RECOMMENDED TO PREVENT FAULTY SITE DECISIONS BASED ON TEChNICAL,
TRANSCRIPTION, AND/OR CALCULATION ERRORS. TIlE EPA REMEDIAL PROJECT MANAGER (RPM) OR SITE ASSESSMENT MANAGER (SAM) MUST BE CONTACTED TO APPROVE A PARTIAL
OR COMPLETE TIER III VALIDATION PRIOR TO ITS INITIATION.
+REGION I LABORATORY DATA VALIDATION FUNCTIONAL GUIDELINES FOR EVALUATING ORGANICS ANALYSES, 211/88, MODIFIED 1111188
-------
Attachment C
“Region I CSF Completeness Evidence Audit Program”, July 1991
-------
U.S. ENVIRONXEN AL PROTECTION AGENCY
REGION I
60 WESTVIEW STREET, LEXINGTON HA 02173
MEHORM Dffl1
DATE: August 7, 1991
SUBJ: Region I CSF Completeness Evidence Audit Program
PROM: Noira N. Latai1le’’
Deborah A. Szaro
Region I CLP TPOs
TO: Lead Chemists
Region I Contractors
ThRU: Heidi Horahan
ARCs DPO
The attached Region I CSF Completeness Evidence Audit
Proaram/July 3, 1991 replaces the currently used procedure described by
CEAT—Techiaw in EPA Regional CSF Completeness Evidence Audit Guidelines .
in using the Region I CSF CEAP on the next CSF you receive. Note
t the forms supplied by CEAT-Techlaw during the Complete SDG File
aining seminar held on February 20, 1991 will no longer be utilized.
These are replaced by the EPA Region I Complete SDG Pile
Receipt/Transfer Form and the DC-2 Forms.
To assist you in implementing this new CSF Program, we have set
up a CSF Hotline number, (617) 229—2050, at the RegionI Weston/ESAT
office. Primary contact is Pam Rose and secondary contact is Kate
Schweitzer. All questions received by ESAT will be documented with
telephone conversation logs. Questions requiring clarification will be
forwarded by ESAT to the TPOs and/or NEIC. You will receive an answer
to your question within 24 hours be informed that the question is
being researched by the TPO/NEIC and that clarification will be provided
as soon as possible. In an effort to save the Lead Chemists’ time and
reduce the number of repeated questions, a copy of questions and answers
received from all Lead Chemists will be provided to each Lead Chemist in
a monthly report. Please take the time to read the monthly reports.
Please note the following:
o All CSF data must have the Region I CSF Completeness
Evidence Audit performed even if those data are not to be validated at
this time.
o Only Lead Chemists may call the CSF Hotline please identify
.irse1f when you call.
-------
o The Hotline is to be used to resolve technical/legal
questions and specific audit questions after you have read and become
familiar with the Region I CSF CEAP. The ESAT contacts will not walk
you through an audit.
I If you are repeatedly unable to reach either the primary or
condary ESAT contact at the CSF Hotline, call either Deborah Szaro or
Noira Lataille at (617) 860—4312.
cc: Carol Wood, QAO
Scott Clifford, ESAT DPO
-------
REGION I CSF COM LETE1 SS
EVIDENCE AUDIT PROGRMI
July 3, 1991
-------
ThBLE OF CON’PEW S
Section Page
1.0 INTRODUCTION 1
2.0 CONPONENTSOFTHECSF .............. 1
3.0 THE CSF TRACKING PROCEDURE 2
3.1 TrackingOverview 2
3.2 CSF Tracking Procedure . 3
3.3 Laboratory Resubmittal Tracking 4
3.4 Data Validation Oversight 5
4.0 THE CSF AUDIT PERFORMANCE PROCEDURE 5
4.1 CSFAuditoverview . . . . . . . . 5
4.2 Inorganic Completeness Evidence Audit . . . . 5
4.3 organic Completeness Evidence Audit 9
5.0 POTENTIAL PROBLEMS WITH THE CSF AUDIT PROCESS . . 12
5.1 Guidelines for Contacting the Laboratory . . 13
5.2 Guidelines for Not Contacting the
Laboratory 13
6.0 COMPLETION OF EVIDENCE AUDIT AND DISTRIBUTION OF
A IT . . . . . . . . . . . . . . . . . 15
-------
1.0 INTRODUCTION
Evidence audits are conducted to ensure that laboratory
documentation and data will be admissible in potential
litigation. Prior to the implementation of the OLMO1.0
Organic and ILMO1.0 Inorganic Statements of Work, evidence
audits for all Routine Analytical Services case files were
performed by CEAT-Techiaw. However, under the ILMO1.0 and
OLMO1.0 Inorganic and Organic Statements of Work,
laboratories must now develop Complete Sample Delivery Group
Files (CSFs). The CSFs consist of the original Sample Data
Package and a].]. related documentation. Laboratories
operating under the new contracts will submit the CSFs
directly to the regions, who will now be responsible for
conducting the evidence audits. This process allows the EPA
to quickly monitor the quality of the laboratory
documentation.
To easily integrate the evidence audit into the
validation procedure, the Region I Quality Assurance Office
has developed the Region I CSF Completeness Evidence Audit
Program . The program addresses two fundamental areas of
responsibility necessary to ensure the admissibility of
laboratory-generated documentation and analytical data as
evidence. First, the integrity of the CSF must be
maintained during all transfers. Second, the completeness of
the CSF documentation must be assured through the evidence
audit process.
The Region I CSF Completeness Evidence Audit Proaram
replaces the procedure described by CEAT—Techiaw in EPA
Regional CSF Completeness Evidence Audit Guidelines . None of
the forms supplied by CEAT-Techiaw at the Complete SDG File
Training seminar held on February 20, 1991 will be necessary
to complete the Region I CSF Completeness Evidence Audit or
to perform the CSF tracking procedures.
A flowchart outlining the Region I CSF Completeness
Evidence Audit Pro ram is included in Attachment I.
2.0 COMPONENTS OF THE CSF
The CSF consists of the original Sample Data Package and
all related documentation. The laboratory is required to
assemble the CSF and submit it directly to the Region (as
specified in Exhibit B, Section II, B—22 of OLMO1.0 and
Exhibit B, Section II,B—13 of ILMO1.0). The laboratory
submits a Complete SDG File (CSF) Inventory Sheet, DC-2 Form,
(inorganic pages 1-2, organic pages 1—4), which indexes all
1—1—03—01 1
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documents submitted in the CSF. In addition to the original
Sample Data Package, the CSF consists of the following
original documents:
• A completed, signed, and dated Complete SDG File
(CSF) Inventory Sheet, DC-2 Form;
• All original shipping documents including the EPA
chain of custody records, airbills, EPA traffic
reports, and sample tags sealed in plastic bags;
• All original receiving documents, including the
sample log—in sheet (DC—i Form), and other
receiving forms or copies of receiving logbooks;
• All original laboratory records, not already
submitted in the Sample Data Package, concerning
internal laboratory sample transfer/tracking,
preparation and analysis;
• All other original SDG—specific documents in the
laboratory’s possession including telephone
contact logs, copies of personal logbook pages,
and hand written case—specific notes.
3.0 THE CSF TRACKING PROCEDURE
3.1. Tracking Overview
To comply with evidence requirements, signed and dated
custody seals must be affixed to the CSF whenever it is
transferred. The CSF is considered transferred whenever it
changes location upon shipment or hand—delivery. This occurs
when the CSF is shipped from the laboratory to the Regional
Sample Control Center (RSCC), from the RSCC to the Prime
Contractor, from the Prime Contractor to the Data Validation
Subcontractor, from the Data Validation Subcontractor to the
Prime Contractor, whenever the CSF is requested f or oversight
by the Region I EPA Quality Assurance Office, or any other
time the CSF must change custody.
Data Validation Subcontractors will not be responsible
for conducting evidence audits; however, they must be
informed of and adhere to the Region I CSF Completeness
Evidence Audit Program , CSF Tracking Procedures. The Prime
Contractors are responsible for ensuring that all Data
Validation Subcontractors are properly trained in the
procedures outlined in the tracking procedure.
1— 1—03—01 2
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The CSF Tracking Procedure is initiated when the CSF is
received at the RSCC by the SampleControl Coordinator (SCC).
The 5CC will initiate the CSP Receipt/Transfer Porn, which
will remain with the CSF through every transfer. The purpose
of the CSF Receipt/Transfer Form is to document the presence
and condition of custody seals, which must be affixed to the
data package in
compliance with evidence audit requirements during all
transfers. Examples of blank and completed cs
Receipt/Transfer Forms are included in Attachment hA and
IIB.
3.2 CSF Tracking Procedure
The CSF is received at the RSCC from the laboratory
under custody seal. The SCC initiates a CSP Receipt/Transfer
Porn, which will remain with the CSF with every transfer. For
each transfer, the following protocol for CSF tracking and
completion of the CSP Receipt/Transfer Form must be followed:
1. Inspect the unopened CSF shipment. Determine if
custody seals are present or absent. If present,
determine if custody seals are intact or broken.
2. Open the CSF shipment and complete the CSF
Receipt/Transfer Form. The case number, SDG
number, and data package number will be completed
by the SCC.
• Receipt Date - Enter the date that the
cont actor/validator received the CSF;
• Received By — Enter the name and initials of
the contractor/validator who has opened the
CSF, and list the affiliation, i.e. RSCC,
Weston/ESAT, NTJS/ARCS, Dynatnac, EPA, etc.;
• CSP Activity - List the CSF activity. For
example, the 5CC will list the activity as
“CSF Receipt”. The contractor/validator will
list the activity as “validation”,
“resubmittals”, “data validation oversight”
or , C5F storage”;
• Custody Seals - Indicate whether the custody
seals were present and intact;
1—1—03—01 3
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• Released - If the CSF must be transferred to
a new location, identify which organization
the package will be released to and the date
of release, i.e. shipment date or hand—
delivery date.
3.3 Laboratory Resubmittal Tracking
All laboratory resubmittals requested during the
evidence audit and/or data validation must be shipped under
custody seal. The Prime Contractor Lead Chemist is the only
one authorized to request and receive resubmittals. The Data
Validation Subcontractor cannot request or receive
resubmittals. The laboratory may send resubmittals to either
the RSCC or the Prime Contractor.
If the laboratory sends resubmittals to the RSCC, a new
CSF Receipt/Transfer Form will be initiated by the SCC. The
resubmittals and new CS? Receipt/Transfer Form will be
shipped to the Prime Contractor Lead Chemist as stated in
section 3.2. The Prime Contractor will complete the
appropriate section of the new CSF Receipt/Transfer Form and
will indicate the “CSF Activity” as “Resubmittals”. The Prime
Contractor will then forward the resubmittals to the Data
Validation Subcontractor under custody seal.
However, if the laboratory sends resubmittals directly
to the Prime Contractor, a new CS? Receipt/Transfer Form will
be initiated by the Prime Contractor. The Prime Contractor
will complete the appropriate section of the new CS?
Receipt/Transfer Form and will indicate the “CSF Activity” as
“Resubmittals”. The Prime Contractor will then forward the
resubmittals to the Data Validation Subcontractor under
custody seal.
If the Prime Contractor receives resubmittals from both
the laboratory and the RSCC, the Prime Contractor must verify
that the resubmjttals received from the RSCC are identical to
those received directly from the laboratory. The Prime
Contractor may then discard and recycle the set of
resubmittals received from the RSCC. If the two sets of
resubmittals are not identical, the Prime Contractor must
contact the laboratory to determine which set of resubmitta].s
is correct.
Upon receipt of the resubmittals, the Data Validation
Subcontractor will complete the appropriate section of the
new CS? Receipt/Transfer Porn. Under “Released”, the Data
1—1—03—01 4
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Validation Subcontractor should indicate “Included with CSF”.
All CSP Receipt/Transfer Forms and laboratory resubmittals
must be kept with the CSF.
3.4 Data Validation oversight
If the QA Office requests a CSF for data validation
oversight, the Prime Contractor must complete the appropriate
sections of the CSF Receipt/Transfer Form and ship the CSF
under custody seal to the EPA. When the data validation
oversight is complete, the EPA will complete the appropriate
sections of the CSF Receipt/Transfer Form and ship the CS
under custody seal to the Prime Contractor.
4.0 THE CSF AUDIT PERFORMANCE PROCEDURE
4.1 CSF Audit Overview
The purpose of the evidence audit is to determine
completeness of the CSF as shipped from the laboratory. The
auditor must verify that all documents are present as stated
by the laboratory on the DC-2 Form and that jJ pages in the
CSF are accounted for on the DC-2 Form. All evidentiary
documents must be clearly identified with the case number and
SDG number, and must be signed and dated where required. The
accuracy of the Sample Data Package submitted as part of the
CSF is determined during the normal data validation procedure
and is not part of the evidentiary audit.
The CSF Audit Performance Procedure outlines the
protocol that Prime Contractors must follow to complete the
evidence audit. The evidence audit must be completed by
Prime Contractors only. Data Validation Subcontractors
performing data validation will not be responsible for
conducting the evidence audit, although they will be required
to adhere to all CSF tracking procedures. The Prime
Contractor will perform the evidence audit by reviewing the
DC-2 Form, which is submitted by the laboratory as part of
the CSF. Examples of blank organic and inorganic DC-2 Forms
are included in Attachment lilA. Examples of laboratory—
completed organic and inorganic DC-2 Forms are included in
Attachment IIIB. Examples of laboratory—completed and Prime
Contractor-completed organic and inorganic DC-2 Forms are
included in Attachment IIIC.
4.2 Inorganic Completeness Evidence Audit
The following describes the Region I guidelines for
1—1—03—01 5
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conducting completeness evidence audits of inorganic CSFs.
The CSF will be shipped to the Pri,me Contractor Lead Chemist
by the RSCC. A CSP Receipt! Transfer Porn, initiated by the
SCC, will be shipped with the CSF.
The Prime Contractor Auditor/Validator will perform the
evidence audit using a photocopy of each completed and signed
DC-2 Porn which is submitted by the laboratory as part of the
CSF or which is submitted with resubmitted documents. The
Prime Contractor Auditor/Validator must riot Write on the
original DC-2 Porn, which will remain with the CSF,
unmodified.
When resubinittals are requested, the Prime Contractor
Auditor/Validator should request that the laboratory number
the resubmitted pages so that they may be appended to the end
of the CSF. Pages should not be inserted into the CSF, and
original pages in the CSF should not be replaced by
resubmitted pages.
When the laboratory resubmittals are received, photocopy
the new DC-2 Form and perform the evidence audit for the
resubmitted sections only. The Prime Contractor
Auditor/Validator must riot write on the original DC-2 Form,
which will remain with the CSF, unmodified.
The Prime Contractor Auditor/Validator must generate
telephone communication logs whenever the laboratory is
contacted for resubmittals or clarification.
Complete the evidence audit according to the following
protocol:
1. Inspect the package for custody seals and follow
the protocol outlined in the CSF Tracking
Procedure. After completing the appropriate
sections of the CSP Receipt/Transfer Form, proceed
with the evidence audit.
2. Locate the CSF Inventory Sheet, DC-2 Form,
submitted by the laboratory. Make one photocopy
of this DC-2 Form to perform the evidence audit.
At the top of the first page, label the photocopy
“Evidence Audit Photocopy”. The original DC-2
Form submitted by the laboratory must remain with
the CSF, unmodified.
If the DC-2 Form is not included with the CSF,
contact the laboratory for submittal and complete
1—1—03—Cl 6
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a telephone communication log. Resubmittal of
just the DC-2 Form isnot required to be under
custody seal. Proceed with the evidence audit
after the DC-2 Form has been submitted by the
laboratory and photocopied by the Prime Contractor
Auditor/Validator.
3. Review the documents in the CSF. Compare the
document page numbers to the page numbers listed
on the DC-2 Form. Ensure that all documents are
accounted for and legible. If extra pages were
included with the CSF but were not listed on the
DC-2 Form, or if page numbers listed on the DC-2
Form were incorrect, request that a corrected DC-2
Form be submitted. Complete a telephone
communication log.
4. For items 1-27 on the DC-2 Form, if the
information is accurate and legible, place a check
in the EPA column for those items.
If any pages are missing, inaccurate, or
illegible, do not put a check in the EPA column.
Request resubmittal of the pages from the
laboratory and complete a telephone communication
log.
5. For item 28, check whether the traffic report is
present. If no, leave EPA column blank, request
resubmittal of the pages from the laboratory and
complete a telephone communication log.
Check whether the traffic report was signed and.
dated. If yes, place a check in the EPA column.
If no, leave EPA column blank and indicate the
non-compliance directly next to item 28 on the DC-
2 Form. Do not request a laboratory resubmittal
of the traffic report if it was present but not
signed or dated.
6. Proceed to item 29. Check whether airbills, chain
of custody records, sample tags, sample log—in
sheets (DC-i Form and/or lab form), and the SDG
cover sheet are present. If no, leave EPA column
blank, request resubmitta].s from the laboratory,
and complete a telephone communication log.
Check whether the airbills, chain of custody
records and SDG cover sheets were signed and
1—1—03—01 7
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dated. If yes, place a check in the EPA col
If no, leave EPA column blank and indicate the
non—compliance directly next to item 29 on the DC-
2 Form. Do not request laboratory resubmittals of
these documents if they were present but not
signed and dated.
Check whether the sample log—in sheet! DC-i Form
are complete and accurate. If yes, place a check
in the EPA column. If no, leave EPA column blank
and indicate the non—compliance directly next to
item 29 on the DC-2 Form. Do not request
laboratory resubmittals of these documents if they
were present but not complete or accurate.
7. Items 30, 31, and 32 concern laboratory
documentation including miscellaneous
shipping/receiving records, telephone logs,
internal laboratory sample transfer/ tracking
sheets, and sample preparation and analysis
records. Confirm that EPA sample numbers, SDG
numbers, and Case numbers are correctly referenced
to this particular Case and SDG on all documents
submitted by the laboratory. If yes, place a
check in the EPA columns. If no, leave EPA
columns blank, request that the laborat-
resubmit the correct documents and completd
telephone communication log.
8. If there are documents listed in item 33, confirm
that EPA sample numbers, SDG numbers, and Case
numbers are correctly referenced to this
particular Case and SDG on all documents submitted
by the laboratory. If yes, place a check in the
EPA columns. If no, leave EPA columns blank,
request that the laboratory resubmit the correct
documents, and complete a telephone communication
log.
9. The evidence auditor should sign the “Audited by”
section at the bottom of each photoco ied DC-2
Form. The evidence auditor’s printed name, title,
and date should also be completed. In addition,
the evidence auditor should indicate their company
name/contract below the “Printed Name/Title” line.
10. Since resubmittals may be requested during
validation, hold all DC-2 Forms until the data
validation is complete before proceeding with the
1—1—03—01 8
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distribution of the forms.
11. When requested resubmittals and new DC-2 Form are
received from the laboratory, make a photocopy of
the new DC-2 Form. At the top of the first page,
label the photocopy “Evidence Audit Photocopy”.
The original DC-2 Form submitted by the laboratory
must remain with the CSF, uninodif led. Perform the
evidence audit for the resubmitted sections on the
photocopy of the new DC—2 Form. The column on the
photocopied DC-2 Form for the original data
package, which was left blank during the evidence
audit pending resubmittals, remains blank.
4.3 organic Completeness Evidence Audit
The following describes the Region I guidelines for
conducting completeness evidence audits of organic CSFs. The
CSF will be shipped to the Prime Contractor Lead Chemist by
the RSCC. A CSF Receipt/ Transfer Form, initiated by the
SCC, wi].]. be shipped with the CSF.
The Prime Contractor Auditor/Validator will perform the
evidence audit using a photccopv of each completed and signed
DC-2 Form which is submitted by the laboratory as part of the
CSF or which is submitted with resubmitted documents. The
Prime Contractor Auditor/Va] .idator must not write on the
original EC-2 Form which will remain unmodified with the CSF.
When resubinittals are requested, the Prime Contractor
Auditor! Validator should request the laboratory to number the
resubmitted pages so that they may be appended to the end of
the CSF. Pages should not be inserted into the CSF and
original pages in the CSF should not be replaced by
resubmitted pages.
When the laboratory resubmjtta].s are received, photocopy
the new DC-2 Form and perform the evidence audit for the
resubmitted sections only. The Prime Contractor
Auditor/Validator must not write on the original DC-2 Form
which will remain with the CSF, unmodified.
The Prime Contractor Auditor/Validator must generate
telephone communication logs whenever the laboratory is
contacted for resubinittals or clarification.
1—1—03—01 9
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Complete the evidence audit according to the following
protocol: -
1. Inspect the package for custody seals and follow
the protocol outlined in the CSF Tracking
Procedure. After completing the appropriate
sections of the CSF Receipt/Transfer Porn, proceed
with the evidence audit.
2. Locate the CSF Inventory Sheet, DC-2 Porn,
submitted by the laboratory. Xake one photocopy
of this DC-2 Porn to perform the evidence audit.
At the top of the first page, label the photocopy
“Evidence Audit Photocopy”. The original DC-2
Form submitted by the laboratory must remain with
the CSF, unmodified.
If the DC-2 Porn is not included with the CSF,
contact the laboratory for submittal and complete
a telephone communication log. Resubmittal of
just the DC-2 Porn is not required to be under
custody seal. Proceed with the evidence audit
after the DC-2 Porn has been submitted by the
laboratory and photocopied by the Prime Contractor
Auditor/Validator.
3. Review the documents in the CSF. Compare the
document numbers to the page numbers listed on the
DC—2 Form. Ensure that all documents are
accounted for and legible.
If extra pages were included with the CSF but were
not listed on the DC-2 Form, or if page numbers
listed on the DC-2 Form were incorrect, request
that a corrected DC-2 Porn be submitted. Complete
a telephone communication log.
4. For items 2, 4, 5, and 6 on the DC—2 Form, if the
information is accurate and legible, place a check
in the EPA column for those items.
If any pages are missing, inaccurate, or
illegible, do not check off the EPA column.
Request resubmittals from the laboratory and
complete a telephone communication log.
5. For item 3, check whether the traffic report is
present. If no, leave EPA column blank, request
resubmittal of the form, and complete a telephone
communication log.
1—1—03—01 10
-------
Check whether the traffic report was signed and
dated. If yes, place a check in the EPA column.
If no, leave the EPA cclumn blank and indicate the
non-compliance directly next to item 3 on the DC-2
Form. Do not request a laboratory resubmittal of
the traffic report if it was present but not
signed or dated.
6. Item 7 concerns laboratory documentation including
internal laboratory sample transfer/tracking
sheets, sample preparation and analysis logbook
pages, screening records, and all instrument
output, including strip charts from screening
activities. Confirm that EPA sample numbers, SDG
numbers, and Case numbers are correctly referenced
to this particular Case and SDG on all documents
submitted by the laboratory. If yes, place a
check in the EPA columns. If no, leave the EPA
column blank, request that the laboratory resubmit
the correct documents, and complete a telephone
communication log.
7. Proceed to item 8. Check whether airbills, chain
of custody records, sample tags, sample log-in
sheets (DC-i Form and/or lab form), the SDG cover
sheet, and miscellaneous shipping/receiving
records are present. If no, leave the EPA column
blank, request resubmittais from the laboratory,
and complete a telephone communication log.
Check whether the airbills, chain of custody
records and SDG cover sheets were signed and
dated. If yes, place a check in the EPA column.
If no, leave EPA column blank and indicate the
non-compliance directly next to item 8 on the DC-2
Form. Do not request laboratory resubmittals of
these documents if they were present but not
signed and dated.
Check whether the sample log-in sheet/DC-i Form
are complete and accurate. If yes, place a check
in the EPA column. If no, leave EPA column blank
arid indicate the non-compliance directly next to
item 8 on the DC-2 Form. Do not request
laboratory resubmittals of these documents if they
were present but not complete or accurate.
8. Item 9 lists all internal laboratory sample
transfer records and tracking sheets. Confirm
1—1—03—01 ii
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that EPA sample numbers, SDG numbers, and Case
numbers are correctly referenced by the
laboratory. If yes, place a check in the EPA
columns. If no, leave EPA columns blank, request
resubmittals from the laboratory, and complete a
telephone communication log.
9. If there are documents listed in item 10, confirm
that EPA sample numbers, SDG numbers, and Case
numbers are correctly referenced to this
particular Case and SDG on all documents submitted
by the laboratory. If yes, place a check in the
EPA columns. If no, leave EPA columns blank,
request resubmittals from the laboratory, and
complete a telephone communication log.
10. The evidence auditor should sign the ‘ t Audited by”
section at the bottom of each photocopied DC-2
Form. The evidence auditor’s printed name, title,
and date should also be completed. In addition,
the evidence auditor should indicate their company
name/contract below the “Printed Name/Title” line.
11. Since resubmittals may be requested during
validation, hold all DC—2 Forms until the data
validation is complete before proceeding with the
distribution of the forms.
12. When requested resubmittals and new DC—2 Form are
received from the laboratory, make a photocopy of
the new DC-2 Form. At the top of the first page,
label the photocopy “Evidence Audit Photocopy”.
The original DC-2 Form submitted by the laboratory
must remain with the CSF, unmodified. Perform the
evidence audit for the resubmitted sections on the
photocopy of the new DC-2 Form. The column on the
photocopied DC-2 Form for the original data
package, which was left blank during the evidence
audit pending resubmittals, remains blank.
5.0 POTENTIAL PROBLEMS WITH THE CSF AUDIT PROCESS
The following is a list of guidelines to aid the auditor
in determining the appropriate action to take when a CSF or
DC-2 deviates from the required format. Examples of
situations which would and would not require contacting the
laboratory for resubmittals are also included.
1—1—03—01 12
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5.1 Guidelines for contacting the Laboratory
The laboratory must be contacted for any problem that
affects the completeness or accuracy of the CSF. For
example:
• If the CSF contains pages identified with only a
laboratory identifier, such as a LIMS project
number, the laboratory must be contacted. All
pages of the CSF must reference the CLP Case
Number and SDG to maintain data completeness. Any
pages with only a laboratory or LIMS project
number must be resubmitted.
• If the laboratory mistakenly indicates “Not
Applicable” for an item and it is obvious that the
item is applicable, i.e. the document is present
in the CSF, the laboratory must be contacted. For
example, if the laboratory mistakenly indicates
that the airbills are “NA”, then the laboratory
must be contacted and the revised DC-2 Form must
be resubmitted to indicate the exact page number
of the airbills.
• If the DC-2 Form used by the laboratory does not
itemize all pages present in the CSF, the
laboratory must be contacted. The laboratory may
use their own version of the DC-2 Form as long as
all items/pages are listed. If the DC—2 Form does
not accurately reflect the contents of the CSF,
then the laboratory must resubmit the DC-2 Form.
• If the laboratory submits photocopied
documentation instead of original documentation,
and if the location of the originals is not noted
on each photocopy, then the laboratory must be
contacted. The entire CSF must be submitted with
all original documentation, or the location of the
originals must be noted on each photocopy.
For example, sample tags and air bills must be
original documentation. Sample preparation logs
and standard preparation logs, which are usually
in bound logbooks, may be photocopies.
5.2 Guidelines for JjQ Contacting the Laboratory
The laboratory does not need to be contacted if problems
1—1—03—01 13
-------
do not affect the completeness or accuracy of the CSF. For
example: -
• If the laboratory uses a different DC-2 Form than
the one included in the Region I program (i.e.
individual items on the DC-2 Form have slightly
different headers than those on the CLP forms),
the laboratory does not need to be contacted. As
long as all documents are accurately
inventoried on the laboratory DC-2 Form and the
DC-2 Form accurately reflects the contents of the
CSF,then the
laboratory does not need to be contacted.
• If the Traffic Report includes the Chain of
Custody form, as is the case with the new Traffic
Reports, the laboratory does not need to be
contacted. The laboratory may list them
individually. The duplication of page numbers is
inevitable.
• If the laboratory has inserted resubmitted pages
into the CSF, the laboratory does not need to be
contacted. The laboratory has the option to add
the req uested resubmittals in an addendum, insert
additional pages in the package and renumber the
pages or resubmit the page with the original page
number.
• If other inconsistencies are found on the DC—2
Form, but the integrity of the package is not
affected, then complete the audit and note the
deficiency. For example, some laboratories may
not check each item individually on the DC-2 Form,
but may instead draw a continuous arrow down the
column to indicate that all items were checked.
If, however, an item that is not applicable to the
case is indicated as present by the continuous
arrow, note the inconsistency on the DC-2 Form.
• If the laboratory listed both the original and
photocopied pages of the shipping documents on the
DC-2 Form, the laboratory does not need to be
contacted. The laboratory may have listed the
photocopied documents under the “Traffic Report”
and “EPA Shipping/Receiving Documents” sections
and the original documents under “Other Records”.
As long as the original documentation is included
with the CSF, it is not necessary for the
1—1—03—0]. 14
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laboratory to resubmit the DC-2 Form with the
original documents listed under the “Traffic
Report” and “EPA Shipping/Receiving Documents”
sections.
6.0 COMPLETION OF EVIDENCE AUDIT AND DISTRIBUTION OF AUDIT
FORNS
The audit is complete after data validation has been
performed and when all DC-2 Forms have been received and
audited. Even if data validation is performed by a Data
Validation Subcontractor, the Prime Contractor is still
responsible for obtaining any resubmittals required by the
validation and new DC-2 Forms following the protocol outlined
above for CSF tracking and auditing.
The photocopied DC-2 Forms completed by the evidence
auditor, the original laboratory-submitted DC-2 Form, and the
CSF Receipt/Transfer Form should remain with the CSF. The
evidence auditor should make a copy of all DC-2 Forms that
were previously photocopied and completed during the audit
procedure. These copies, along with copies of the telephone
communication logs, should be sent to:
Contract Evidence Audit Team (CEAT-TechLaw)
12600 West Colfax Avenue
Suite C-310
Lakewood, Colorado 80215
Attn: Kern Luka, Project Leader
When the validation and evidence audit procedures are
completed, the CSF remains with the Prime Contractor until
contract expiration or until further use of the CSF is
required by Region I.
1—1—03—01 15
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Attachment I
Flowchart of Region I CSF Audit Program
-------
CSF Tracking
Procedure
Ship CSF to FISCC underl
custody seal. I
Receive CSF, check custody seal,
lnttlate CSF Receipt/Transfer Form,
transfer CSF under custody seal.
1
4
REGION I CSF AUDIT PROGRAM
- — @ ! Laborator
- 6 tegional Sample Cont N
Center (RSCC)
(validation)
(EPAQA Offic ’\
\ . (ESD) )
(dub Contractor \ _____
(Sub) )
CSF Evidence
Audit Procedure
I
Compile CSF documents, generate
Form DC-2.
Ship CSF under custody seal
Generate new DC-2 for resubmitlais,
ship to Pnme under Custody Seal.
Perform evidence audit using
Photocopied Form OC-2.
Receive validation resubrnjttajs,
perform audit of new documents with
photocopy of new Form DC-2.
Compile auditor-completed
Form DC-2s and send copy of
each to Techiaw.
I
Ship entire CSF to Prime wh ]
data va datlon completed . j
Receive CSF, check custody seals,
complete CSF Receipt/Transfer Form.
Perform evidence audit and data
validation.
If applicable, transfer CSF under
custody seal to Sub or ESD.
Receive CSF from Sub or ESD.
check custody seal and complete
CSF Receipt/Transfer Form.
Maintain final custody of CSF until
coniract expiration.
(Prime)
(oversight)
I
Receive CSF, check custody seals,
complete CSF Receipt/Transfer Form.
Complete validation oversight.
Transfer CSF under custody seal .
Receive CSF, check custody seals,
complete CSF Receipt/Transfer Form.
Complete validation.
Transfer CSF under custody seal.
-------
Attachment - hA
Blank CSF Receipt/Transfer Form
-------
EPA REGION I
COMPLETE SDG FILE
RECEIPT/TRANBFER FORM
Case #: SDG: Data Package #:
Receipt
Date
Received by:
Name mit. Affiliation
CSF
Activity
Custody Seals:
Present / Intact
(On Receipt)
Y N Y N
Y N ‘IN
Released:
To Date
Y N
‘IN
Y N
‘I N
‘IN
‘IN
‘IN
‘IN
‘IN
Y N
Y N
‘I N
‘IN
‘IN
‘IN
Y N
‘I N
‘IN
Y N
Y N
‘IN
‘IN
-------
Attachment IIB
Co p1eted CSF Receipt/Transfer Form
-------
EPA u GION I
COMPLETE FILE
RECEIPT/TRANEJFER FORM
Case #: %2 ’L’ SDG: AM I Data Package #: OO O 4
.‘
Received by:
Custody Seals:
Released:
Receipt
CSF
Present / Intact
Date
- i
Name mit. Affiliation
- r rr -L CC Q i$ #r
ActivIty
(On
u
Receipt!
‘
To Date
i s J &C I *‘
I
2
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M ’
I
‘erc c 5
Yjt wsi4
ç j
LC
‘
‘- -
A L
- cc
J \kEZ
E A
k l , zcS
t r —
c4 4(*
P t icLg .
CD N
C ) N
N
N
N
V N
V N
IN
V N
IN
V N
V N
I”
a) N
N
(? ) N
IN
V N
IN
IN
IN
IN
Y N
I ) ‘.‘S
EP
IJ- S1 4
-J “I s
jz-? j 3
1
1I!!frI i
I
-------
EPA REGION I
COMPLETE BD 1 FILE
RECEIPT/TRANSFER FORI4
case I: ? SDG: -1- l Data Package F:
Received by:
Custody Seals:
Released:
Receipt
Date
Name mit. Affiliation
CSF
ActivIty
Present / Intact
(On Receipt)
To Date
-74 zc4 q I
I
e w 49
tJ a j
c
ci 9 s
N
N
N
( ) H
A) J
L
- Z4 I
2 lz 3h
2 t2
L i t 9
LS
CL L
y J s
uJ
:
1
-------
Attachment -lilA
Blank Organic and Inorganic DC-2 Forms
-------
— R rn. .cc Iz .s c r z czr) v O
__ - __ __
LI.3OP3. jci ‘ .. -— ciTz/r” : : “. - -r’
;. _ - — •. -y • ... —, •
- - -—- -.
___ -
- - - — .. ‘* - .‘ - _.- -
— - - — — —., — •M
ZO. ._ -- - -- • £ - LtZ 1a0.w — ’ ----‘ . - ‘ -. - .— ..
— - .• - . . —. .. . . .. •- . .• .- .•. -. -. .
ALl. da L’rw .r £ tba u Lsta - L t.l-S bS 0X 4 1 si ____
(1 ’ ‘‘ * , T 1 = I)
1. I*x torr ‘at (7 C-2) (0 t r” ’tr )
2. 5 C& .m E& .tii .
3. ? i. f .c
4. Yplptilsi Data
a. QC i ’-y
£ 1z qat$ Psr . t Mcov.ry * axy (7o L )
xsfv s up1.icata a”- - i-y (7a In V )
Xat d E.ank L mazy (7 ZY J
1r±q and (ass :at (7cr V V )
b. Lanpla Data
?. ).as tt* (1 rm
sntatLvs .y Zdsn ifi.d c pI I dI (7cm I V -TC)
R:anatr cad tati.l. ion c r=atoçr1a (XIC) g= SIP
7c sach .a=plas
&i upectri s.nd of bachqd .a bt. &ctsd
gas. z *c a of ta. ut c pauzda tdanti i.d
1Q 1 1 •p.ctra of a .2 rspcztad * vit t r*s b4St
lthrary tatc as
c. gt&nd&d3 Data (3 1 I.stx a)
it &1 C4 L *tLon Data (7Gm VT V )
1Ca and Q an Papo ts for att Zta dz da
ntin thq Ca. thr*tion (7cm V I I )
RICa and Q35 ap rta for a. i Ztazdaxd.s
Intsrz’a.l Ztindazd )zsa a=ary (7c VITTI V )
d. .av QC Data
Zn
alank Data
X&triz *piks Data
Mt iz Zplk D ip2.ioata Data
I. Data
a. QC 5*Xy
i -cgatu Ps aJit Zacavszy f ax7 (1Or II *7)
X$/XSD I’ ’ (Torm II SV)
M.t ,Od hank t .1-y (7o: I v *7)
t i and Zass C L atS n (7 7 IV)
—
_ -
-------
7 :1 ( ?Q
T1
. ‘“ _.__._.,_. . .. —
r — .-. .. - L u. ‘ : - -
ORG IIC :C L! G? E 4 CS?) XI1VZ T -
.sz ZO.’ ’ 7 T
- ?- - . - .-— —-. h.. ‘•
I —
5. S ivclzti.2.aa Data (cc td)
b. Za. pi.. Dat* -
. PU t* (7c XV)
?t tztL .l.y Zd. tLfL.d (ram I ZV- IC)
Pacc ztz t t taj Lc chr arrw (ZX ) f Dr ____
Yar .a h supl.z
aw sp.ct a and backqzv d ..nbtra tad s i
of ?=. cp u .
(ta. .p.ctza of s with 3 beat lLbr& y
GPC (U GPC zf r..4)
C. Standizd.z Data (Al. IDzt ts)
InitLal Calthratjcn Data (7o VI XV)
Z Ca and Q an fc aU ita.Ddsd.s
tin inq Calibraticn ( 7or VII IV)
*Cz and Quan .apcx z f all. ztazdaxd.t
Intarz.&i. tanda d )raa Si ry (T V 1 1 13 XV )
!ntar .a.l St ard Asa 1’ ’try (Yoz VII XV)
d. Xai QC Data
31*nk Data
X&t $pl.ka Data
)(atxix £pika D p2icats Data
. P,vttcid. .
a. QC $t iiry
Surroqat. Psroant Rac vsry airy (7Dr’ II Pest)
)U/XSD D ipljcata X ’ T ( 7o U Peat)
(sth 4 31a k Z ity (7o IT Pest)
b. Sa.p1. Data
T. Org. i 3.nalysia at$ fbmet
(7cm I Peat) *
r atogra i (Pri y cD1 )
r atograsa fr s.ccnd OC oolt f1r 4 i
CC Intagrat icu r.pcrt or data ayst pri t t aM
ca1ibra jcm pl.ota
Xa.zmLt work Ihsta
tY tacsi fr GPC (if 4 ,1 t)
br ps . L’Ldaa/pez. ce fizsd by CC/ Id, coptse
of raw spectra and copies of backq oond-eubtracta4 rae .
sp. tra of target c nn4s (.aples & standards)
-------
-r ORGANIC LZ S G 7111- . (CS7) KvrJ RI
— --. .—‘—.. ,. _ . .—II .= _ .i ____ --— — .- 3 — i;i) ..-,
- - -
t 1 .c .‘.:. G a _ — - ___________
. • -‘
6. P.vtiridas (co 4)
C. St z zrdi D t*
PutLcidaa Z ai atio Sta. dazd.s I axy
(7cr VTII. P*iti$)
Prti i4.a Zvz1t &t n Standards S y
(7or V111, Pest4)
PstiCLds/P Standards * sxy (Tom . Peat ) —
P.rti ida/P dant.tfL aticn ( Yox Z, Peat )
Standard ch atoqa.ms and data wywt
i a U &tandards
7cr pssttCid.s/P s ccnfi’L.d by GC/XS, c piss Cf
a ctra for .tz.nd.szts es4
4. Mw QC &ta
31.ank ata
katrix Zpl.ka ata
Xztriz Spik. D pii ata D&ta
7. XLseeLIa. ao s Vats
Crig( t pr.ps.r&ticn and I yais lcra or pia.s of
prapaxation and a iIysia logbook pages
Int.r J.L sa. pl. s.nd ss. pla sx act transfer ( “—of —
c itody rec s
5c:, 4 ” rcords
11.1 £ strsnt oot t, ine1t2d4i q strip ehaza i
scr.. ”(”g activities (describe or list)
5.
Arbi1 ls Q1o. of shi zrs
ain—of— zstody Pac da
ss pI. Tags
Serpi. Log n Sheet (Lab & C )
Cc?sr Sheet
KLsc. 3an.aqs $bipLng/Mceivi g M da
(d.acribs list)
. Tvter a1 Lab$am,1. franafsr acordz e d?raek! 1b. .
(dsscrib. or list)
-------
.:‘:.• OR JLIC 7U1 ( Ty.. v oRT
c _ - T
r e q . G
10. Otbsr cardi (d.Ic LbS ar list)
?s3.tT” . Lcq
cc p .t.d b 7 r
(= L&b)
kziditad byt
(IPA)
(Siç&: Xs)
(S .&t X*)
ts Ja s/TitLs)
(D&t*)
11. 2 LI#Lit1 1
—
(?ri ..d s/it1..)
-------
• I OR 7 2 IC C ( LZT! SDG TILZ . CS?) I V TOKT. biiz L-.-:: .
- -- --; .-( ‘___
L2O i - - - - i2.I/$ t — -.
•.r.. _.,.. .
b. . - —
C $Z • :‘ s _______ . a i _ _ - #_
— —— — S — —, . • — •- — •E -i—-— — 4 ‘4 —‘ — —
A. . C1 $ tI Ga. j .v&zi a cp.L.te G jJm uat bs e:içt’ . 1 4 u t.$ w mxs
possth a. (PZ7XJ .V L IBI?), ZC G Ifl )
1. X nv.ntc .ry 5b ..t (Pc DC.- } (Do t
2. C vs lags
3. I rç& ic ). a.1yuii Dati £h..st (IC ) ____ ____
4. I iti&1 a d C :i q C.a1Lbxatic V.riiig* t (P z .
Paz )
S. Sti. da. d f 1 (7er , P&Xt ) ____ ____ _____ ____
. 31 ’ (?0r I) ____ _____ _____
7. I :.rf.rsne. c .ck Sap1s (Tcr ZV) ____ ____ _____ ____
3. Spiki Sa. pis R.eavsxy (70xm V, ?axt i.) ____ ____ _____
I. Post Dices: Spik.. Saxpts P.seov.ry (Tcx V. Pax )) ____ ____
2.0. D pii a:.a (7ox V)
2.3. 14 LW7 C to1 £& p1. (7c VU) ____ ____ _____ _____
12. 8ta a .d 4ditL P.as a1tt (T: VIU) ____ ____
33. 1 .r1&2 DL1ut s (7c U) ____ ____
24. Dat.c io Liits, Q a.x sIiy (70z 2) ____ ____
2.5. 1z ts .1s s t c ic 7acto i, Ar n *i.37 (7oz x l .
Part 2.)
26. I:tar.1s s t C rs tic 7actci, Ai x aUy (7or ,
Pa .zt2) ___ ___ ___ —
17. L .n.a. a qsu Quaxu.rly (Tor’a xl i) ____ ____ ____ —
U. Prap.xatio Loq (7ø ZI) ____ ____
11. .x a.1ysis Løq (?0r2 217) ____ ____
20. I .aw Data ____ ____
22.. fla s .x Zaw ata ____ ____
22. P ir ac AP Pay Data ____ ____
23. K.re xy Paw Data ____ ____
24. CyLnid. Paw Data ____ —
25. Percent Zotid.s Ca1c 1ztiona
-------
- : xwic c i V OBI
r t .._____ ______ ___________-‘
_____ ______-. —
PA
26. CLztLL1Ltic Logi (Cya. 4.s
27. iqa.tio Logs _____
28. i fi P rt
29 • ZPA Sh.t q/PacsL th;
z i1 s (Xc. Cf S . -wflt* _ )
“&th..of a.tcdy P.ac z .i
$a. pis ?zqs
Ss ’p1s Loq—1 $b..t (LI. & P C-.2.)
30. iz 1. lLttSCUI ;/P...csiYth; Paearda
(lirt &ll Ldi Ld si racorda)
Ta1sphc . Logs ____ ____ _____
31. Inttr a1 I.a. Sapl. !:a. .a *x Me rdz a d z !il 8 eT.S
(d.ic: .b. or 1 izt)
32. I t.r &1 cr1çL&2 Sa.p s Prep&ratic s..md ).a1ysiz Pacoxda
(d.scri . or .izt)
Pr.pazatico rsc.a _____________________________________ ____ ____ ______
Anai.ysi. r*cor a ________________________________________ ____ ____ ______
33. Ot sr aecrdz (ducrLb. er .Lzt)
34. c .nuz
C cp1st.d bp ___________________________ __________________________________
C Li. ) ($i &t xa) (?rtht.d I.5S/TitL*)
oditsd byt _______________________ ____________________________
(Zfl) (SLç at xs) (Printd Za ./ Lt1) ( Lta)
-------
Attachment -IIIB
Laboratory-Completed Organic and Inorganic DC-2 Forms
-------
-. . -• —OR ? IC. IZ EDG ( )
1A1 I rivr - - t M -— TT/r” r Th i
o42 1 ’ 1Dc t. o ‘— -- •- - • - .S
‘ - .— -.• ‘ -.
1.1..1. ‘ anta J *z £ t * c .apia a & f a .t - I
Si4 1 . zj ZX k i x 2 ‘ 1 I 1
a. C S’T
£ qzta Parc ut Zac v.zy t&ry (? r II ) ____ ____
XS/’XSD D pLicata St 7 ( ____ ____
Xathød E &Ak t m&x7 (7Qz X V V ) _____
and U s a Ca.1Lbrzti (7am V V )
b. S* J. Data
T. .*I Lt3 (lcr= X V )
szr.iti iXy Ide t .fi.d nd a (Yarm I
ac -. ctsd tc a.3 i c atogrzma (2XC i
•apl..
I c r . i sa=p az
Paw a *c a a d of back
ua s cta ef ta.rqu; cpc ndz £ds tifiM
(au . ctrz ci tU :sp tsd ? s it t . Last
lib.raxy — ______
c. Ztznd&rda Data (311 I at-r-.%p)
Initial C’ ation Data (?c VI V ) _____
PICa an4 Q s Zapartz i c r *1.1. Standards ____ ____ _____
ccntin t q Ca1L ratic (7cm VII ) ____ ____
PICa and Qua Papcrts far aU Standards _____ ______
nt.=&t Ztsnlazd 3rsa & &ey (lDrm v: a V ) ____ ____
d . Paw QC Data
4 a ivt 1atL1SI Dita
a. QC s axy
S ats IazQant *aca’*ry S ( T U XV) U L
)UJ’XSD t axy ficra II XV) 1O - .
.thod 21 ’ *1 ax3P (7o IT XV ) t
and Zasu Ca1thx atin ( Io v avj
1. I Y -4; rr tqst (?crm D .2) (Do t ‘ “‘ .r )
2.
3. z.ffic
4. Vo1ptj1ss ta
a
S
-7
1t i
“4
*72
I1& Data
Xatrix Ipiks Data
Xatrix Ipiks Dupliests Data
I . .-
4 i 2 .
( .
1 11 I’
I
141
2.10
7.2.L
-------
* —. — .! . • •.. . ‘ .
OBGIIIIC .C3 LZ : v u x
- _—__.___1.. . -:
— . • . . ‘=: —‘ p- : ’r . — t J •
- i i . _____4D .u•• O7 1 t ’ ___________
—. - —.. ‘...—.— .. ..-..•—...• ..——.— —. . .. —rf -
5 . S iv 1atil.a Data (c td)
b. S& 4.s Data ____
.aI .tZ (Te X &V)
*tiPs y da tUied a , (Tc z Z zv-ri:;
*acc zt t.d t ta. j chr .at w (ZX ) 2 *te
i cr sac l imz
Pay s *ctra a 4 aek d btract.4 I1•
. ç*ctra of c a
)Caa. epecta af D’z with 3 but lLbra’y *L’’ 5.
GPC c atoqrz .a (U 1C pe t a.d)
C. Stzz azds Data (AU In*t r zu)
ZzitLz.1 brztLc Data (icra VT LV) _____
a. d Qu.a.n 7a pcrtz fcr aU su . daxds
tth thq Ca1thra4 (7oz VIZ LV) ____
PXCa s.n Quan P..pcz-z i c r a.1.1 sta daxda
ttrna.1. St dazd Asa *‘ iiy (7cm vil.Ia LV) ____
t.r&3. St ’trd Asa L !!rJtry (7cm VZIZC XV) ____
d. Az QC Data
81 Data. ____
)(.&tri Spika Data ____
Kit ix Spike D ipUc&ta Data ____
‘a
4. QC Zax7
Sur qats Psic t P.lCc?s!7 V” ’7 (7Or IZ Peat)
X$/KSD Duplicate $ ‘ ry (i lIT Peat) ____
Xsthcd 3l nk Lw 1 y (7 Ty ) )
b. Sample Data
! R.s ita — crçanjC .DL3.7zta Data i it
( Taz* I Peat )
at r a (Pr ary l p
rmat raam fr seooM OC col ofLt-
cc T t.gr&ti r.p .xt or data syzt prictoat *
caithrz n plots
Xan &L rk Shasta
V tracee Zx dPC (if aI (1 b1a)
Par p.st(i4s/P s co fi m.d by QC/XI, copia.
of raw spectra a d copies of back roa d..e btra.ctad mm
sp.ct z of tsx.t ce da (s1mp .as & staMerts)
2 (
‘ !03
‘ Is?—
91L
4 ” ,
‘ 4
I .-
—a
*16
5iL L
i I i .a ..
7 ¶
a
a
a
•
— —
-------
—‘ORC BIC C I DG J7XX CS?) 4 E Z!
• • - —‘.-‘ - ‘‘ -. “
__
6. P *Wti L *I ( t )
C. Sta s.rda C&ta
Psstt td.a a ati Sta. d&x * t &rT
(Tcr= V III . ?*it.1)
Pa i 4as rva.t a’ St&rda. Z $ a y
(7 m V I II . Pst.3) ___
P.ttiCidi/P Sta dar .s *axy ( Tax ? sIt ) ____
P.sti ida/P Id ti i zti n ( T ra Z, Pst ) ____
St ‘ 4 ‘ d c .r ztCqzma - d.tts • prit t
f all. at.andard.s
Pør ,ti. i/pc a ca i d by cctXS. c=pi*Z Cf
sp.cts i ita irdi ____ ____ _____
d. av cc
E4V.k ata ____
Xat x Spi a ita
Katx .x spi . p2iata Data ____ _____
7. XL 1Iz .
Oriqia.L .paxatic a d ‘ ysU ics c cc piai ef
apazzti and u atys .a qt’ pLq.I
I taraJ. ia=pL. a. d amp .. .xt a t a sf.z ‘-ot—
C’ st y r.c s ____ _____
Scr.. .t q r. .s ____ _____
111 inzt .nt tpQt, £C 4 ’ rtzi C L 1 i
a. ttvLtiu (dsIc .be er List)
r p j tur(-
JJzbiUa (Xo. of s i tz j _ 1
t [ ..ofcugtody P.. rda _____
aampL. ?aqs
Ssrpts Log-Is Sb.ut (Las & D .3
: C Taz Shst ____ ____
KLsc.i1ana a itppthq/ ac.Lvi g dz
(dasezibs _ — - List)
I ta z t tj $a t. raaf v* ds snd sb.S .
(4.sc ibs c List)
JA
( ,00
L. 3 ( ,‘4t —
4-, ,
‘N ’
I-
__ ; :;Aô u ’
a. m ! j IP.se.i,the Dc _ - ta
C
C
—
S
a-
•7 X1 _
1 ’7*
• ___
, M•
T12. .
—
-------
- oi cxiac
;
—
P2= _
10. ‘dasert
____ _______ 1-,s
.1. c ... 1 41JLzs
c px.t.d bit
( Lab)
Itad byr
(ZPA)
U (1 iç ir.1 r.)
(Pril.d Xa /Tit1a)
a
a
( ta)
($Lç &tt xa)
(? Ld a ./ Lt *)
-------
• I OR6A1 IC C L!TX S G 7ILZ CS?) I V Y ii r : :
• • • , - . . —
• ____
TX) C’ 3 . - po . —
=snts a vusa i t a cpLste S G at criç it 4 u .nzs w *rs —
pc.athl.. Z7 r X IT , Z
1. ,sntc-y Sh..t (7cm DC—2) ( o t h. .r ) —
2. c r.r Pvjs
3. I o ;iz.tc ) a1ysts ata £h st (7 )
4. I iti.a.1 a g C ti j q C. 1thxati Vsz ig&t ” (7= 1,
2% 2 1
i ’ )J. a_ : 7o 12 PLz 2 2 7 .3 . ‘ ‘ .
Z1z . (7Cm 12:) _ 41
7. Tutirfirsne ack St p1s (?e ZV) ____ ____ _____
a. SpLka Sa p1a R. o sxy (7c V, Pu’ 1) toO i.’c ____
p ,t Lçes: spika S4 .a R& v.z7 (7 x V 7a 2)) ( t _ “.
30. ip i atss (7or V) _ 7 . llIc _
U. L&borzt ry C tr 1 £& $s (Tc= VTZ) I C . q _____
32. Stan & d ddLtL J.asuits (lcz V 3 4 1 IOL
33. 5sr i1 L1i ti s (7 Z) I 2. IO _____
14. I it .nt 0 t* i Li.itz, Quartaziy (7 Z) UO _ j .
33. I I tara1& snt ce r 7&ct a, sJ.3y (1cr Z.
t (. %UL
U. I IntsraJ t C sctL 7Aetza ail •
P 1x2) ___ ___ ___
17. I ’ LS. ...r ?.$- q.a &Z ’Z T (TC ) 1St %70
3*. ?rspirat . Log (7o ) ti t %c —
1 . ) &1yaia Log (7cm XIT %L%l _____
20. .aw.0&ta t i ___ ___
21. 71a . Raw IO, 2Jb _____
22. 7 xae. M Mv Data 21L 214
- 1.rc y Mv 0&t& ____
Cyanid. Mv Data 2.’$O _
2*. p.rc t solids C&ic latj” 2.41 2.S ‘
, g C4
-------
I ORG C LZTZ SDG PItI (CS?) V TORI
- — — • 2 ? ‘ — —,-
__ 3 . LZ3’r . _____ oi.-a I-V#t—---- ____
7 ‘
26. Løqi (CyiiiA s O 1y) z l ZSL _____
27. Lg.stio L a ____ _____
2 . st ic Pa r 1 Z 1 _____
29 • IPA Z ç q/ .csivi q ‘ ‘ ts
A ’ (Xo. cf s i ts L 2 1- _____
l”—ot.. .iIt T ‘° ‘ _____ _____ ______
rzq. Z ,( ; ic — -
Zap1. Loq.7 (Z.&b & ?c C ) 3)( % ) ____ —
c O ?ar Sh.t —
3C. Liac aflanso z Sh -/Rhe.iu-thq A.e .a
(1 YL tz$ . x*ea)
s1apb a Loql —
31. L& £a.pis :wgsr acords a.od s. kL q S a.ta
(dssci . or hat)
fJA - —
32. I tar &L OLçi a.1 S&p . P:a r& a. ) &1y*ia &. rda
(dss r bs or h Zt)
Pr.ptratLo r.c .a ____________________________ ?O 2 ____
.n&lyzis r*cor a ______________________________ - -‘
33. Otha 1.c rts (d.icJ. us or Liz)
34. It3Z
Cco$st.d byr ___________________ Swr’-.i ,.
( 1 P L$ ) (J (iLçr.1 z.) (Pzth d Xams/Tit.%a)
byi ____________________________ ________________
(Ziç at r$) (PriAtad Jaa./LthS) ( )
-------
Attachment -IIIC
Laboratory and Contractor—Co p1eted
Organic and Inorganic DC—2 Forts
-------
V je JJc . M T P
• : • • - -a xIC L!TZ .r z .: c )1 VE TO :S
-
L. J RA. S -__
• - .,
-. p . ” • .z .a. - ..
V
•
-
LU ts in t. s cI piaT a £ ti-1& St cri ‘ a’- .
saib A. 3, SZCT II 1’ 3 3)
Th
I v ter Thwt (7am DC—2) (Do t r ’)
C.Ls.. j& -ti’,,
ra-flLc - t
VQlVtil,. Diti
t. C 3t 1?7
Suz cq&ta Psr *ut Paeoisry t az7 (7O X I )
XS/MSD D ipU..c t. (70Z ii: VO )
Xsthod 3lLflk (7o I V )
a d (us ca..tthrati n (70x V VW )
b. Zapls at&
. Ras Lti — (7o I VC3 )
?sntztiisly de tLf Led po nda (7cr I VC .—T )
a n.truc ad tota.1 Lo c st ra. S (1IC) f •
Per .w. ILe p1ss
P.&w spectra and of back nd .ubtr&C .d
nile i ctra of t&r;sr cpa mdI £denttfl.4
(ass spectra of aU rsx rtsd ?T3 vit t r.s b.it
library t.at as
a
-7
•0
L _ • l
__ ‘ I
- - -
iLl
( ( .2 -
t 0
c. tandaxdz ata p.12. zt.r .”ts)
InitLLL C Lbati ata (7e VI V )
P1s and Q an Zaporta fer afl Sta 4ixdS
Le inq Ca1Lb ratLe (7cm VII )
RICe and Quan .ports for aU Sta. dard.s
Internal Standard area (7Cm VIlIl 1V )
%ILS 3 _
I L
V
1H
V 41
4. Raw QC &ta
* 7 5
*1a. k ata
XatL *pi .a v&ta •
t&trix Spika D pii ats ita
(41
21 C
4L
V-
Z_ —
‘ ..._....
—
5.
tyoIatt1. Dita
a. QC £t Vy
$ rreqst. Paxcsnt z*co ezy 11 aXT (bra X i
XZ/ 4S Z ary (70r3 III IT)
)(.thod hank £ rlry (7ora XV L V)
D i g and Kate calibration (7 V IV)
UL
a 1sL
I
“—
‘
-_-
—
-
“—
—
—
0
.9
2.
3.
4.
-------
___ /
.
- - /
g .. b
I v-
___ —
I I
i 2I
b. $apls Data
T Za.ultZ Oriz.nic a1yzia Data Sbst
(Torn X Pst )
x at r*U (Pr 7 cairn)
z atoqrw S r .ecc i4 OC coirn Lr rttin
CC Int.grztian rspozt a: data .yst printout aM
crVt’ plots
XLn &3 Wa:k ab..rs
VT tracas fr GPC (if &ti )
7ar p.atiridas/1C!* eonS ir.d by GCIJ(2, ccpi.a
of raw spectra and coptea of baekro ind-subtxaet.d we
sp.ctra of tazst cc Ms (sample. & .tandazts)
V
— F
/
/
,
— ,— , - — - —
4 - - .. - . : —- — — - - ,
- CR tC CQ EDG !IL! LCS ) p -
5. ZamitoL&tUs. Data (contd)
b. Zazp1a Data
?. Pavolts (Tarn! SV)
?ai taii s1y identified C ivJrI iL 4 1 (Tarn Z tv -T iC)
ct tct&i ion cbr atagrsR. (ZC) i
tar •ach s’ pi.z
aw S Ct Z a.i d back ..ubtrwnd w
s-p.ctra of ?. cc a
X is. s*ctra of ?C’s with 3 bstt library
CPC ctr atogram.s (if cPC perfar..d)
C. Zt* dazde Data (J.1 Inztr sntz)
initial. Calibration Data (Tarn vi ZV) ____
R iCa and Q an R.pcrtz far all ztanda.rd.s
tinuinq Calibration (Tarn V i : SV) ____
RICe and Qua.n R.partl far aU at*xidardz
IntS tJi . Standard A 5I t 7 (7orn Vi:I3 IV) ____
Znt.r al. 5ta ard Aei Sflffr 7 (Tarn Vi:IC IV) ____
d. Paw QC Data
3lank Data ____
)(atrix S ika Data ____
)Utrix £pi) a D pl.icata Data ____
a. QC 2 ’7
$ 1rraqatS Paresat Paccvsry s tiara!! Peat)
R3/XSD Duplicate t1 iy ( Tarn i:2 Pelt) ____
Xsthod Slank Sty (Torn !V Peat) ____
‘ -17 3
4:!
4 -fl
4c’ ,
-------
;. ;- -- •- ORG IC• LZ ZDG JILl ‘( Ce?) L v L K! :
— .. .- . .. . . ....._—.—• • .j ••—. .‘ ..
•• ;_ • :- -“ (‘
__ a . I s u; a -
,_J) . .— — ‘. .. . . . - .—r--— •.
- _
£. P.wti idss (cO t4)
C. ztz. 4arda Data
Ps Lc 4.s tva1 ati *tznd.ixd.$ $ aX7
(7or V’It. ?*st4)
Prt1j fi* tv*i &’ sta dazda g ’-y
(Y v Z • ?*it.3) ___
P*iticLda/P Sta 4ud* nary (70 U. Psit) tD1 __
PrtiCLds/P fl Id* i *t ( 7c za Z, ? st) IL c, tc
Zti krd chr at ra 2 a d data .71t iDt t
for a3.i at& 4*z a
7cr ps.ttCidisi/PCZS by GC/Xi, cop Sa c
ap.c ra fcr iu .& d* usd
d. P. 1w QC Data
I1i ata ( ,51 _ =
Matrix Ipiks Data C 5 &
Matrix Ipik . D pUeata Data. . - , 1 ____
7. jp. I1a .oQI Data
iqi ’ prap4X*tiC a d u tysia fca cx ccpia.s cf
rsp.x*tic5 a d &! klyPiS 1cgb k pigt.
Itar aJ aa pLa a. d aapis .xrzct ta af.r -et. ’
cutc4y ___ I )1 _____
ç raoQrd .$ _ ,cYL. - t _____
).U inatrant tpot, ic1 4 - - rtrip c -u ir
a t.niflg &cti iti.i (d.$ ribs cx List)
ç lj.LJ 1
. m r .qLntI
J.itbUJ (M c. ct ahtcsta j ) -
a oi- sto y P ds
I 1 apis aqs ____ _____ -
Sa pi . Lø9- fl Zbast (Lab & D ) ____ .. .. -
ZLac.1 .l* .D .R z tppt / .c.Lvi q ?a da
(dascrib list)
—
7 ____________________________ — : —
tab a vte ? * .f ax *. ordt * d ?ac i Sb .vtl•
(d..cribs cx list)
-------
r. _____ — ...z .. .-- —‘ _____
• .. * —
trr
10.
3.1. c _ .4JIt3$
—
c p1st.d byt
it.d byz
(tL *t z)
tY O - AAfl\
)1& A AJ 1
\J
O\S c I Ou i -
(PL tad Za /Ttt .*)
f c\ ) k ’
- (,rit.d Y* ITit a)
k)u 12Ls
‘ zhlci
(Data)
(Dit.)
-------
Eui tr
• - -GP iZIC S G •P dZ ( )
r - - — - -- -z:,j
Z 10 4 1 .
- • ‘• -
I. d r ts £n t. a Lu ca — - iJa t bs oriq ‘ ‘
css 4 . ( A zwa t1i 1 ? a SZ X X V 1
1. I — t rT !b (7c VC 2) (Do t “ sr )
2. s Cz. . jy
3. ? rzffie •
4. YolatU.i rita
a. QC *‘ y
t qat. Psrc.ftt Raccv.xy $ az (Pc TX ___
x IxzD D pLicat. (?O X l i V )
Xat od Z1a.o. Si1.7 (7o IV VC&) ___
and Xi , . Ca1L atton (? V VD )
b. £apl. Data ____ ____ _____
. Ms its - (7 r I V ) _____
Iot&ti? .Ly dintiiiad ccp zda (7cr 1 _____
*acanatr cad totaL L o t ch- atogra.o. . (2X ) icr
1 1mp h
7cr s&c .a plaz
&w specta and of baok 4-.iabtracta4
us sp.c z of taqst cpct nds idintifiad
(us sp.cra of a1 rapcxd TC’a with thr.s bait
1L *y La-has
c. Standa.d* Data ( .U Ina n. .ntm)
T LtLa1. C Lbrat Lot Data (7cm VT V ) ____
l z sod Quan apcrts icr aLl Standsxd.s ____
Cottthoioq Calibration (?o Vii VOl.)
RiCa and Q za. Z.poxta for all Standards ____
itt.roal Standard Ir is S .ry (7o ‘ Qi a V )
d. Mv QC Data
an _
hank Data
Xat ix 1pi a Vats __
) at ix Ipika DupUe-sta Data ____
S. ieo1atil Vita
a. C i aXy
lurrogate Pircent 2aeaw ry tu az, (7O Ti l v) ____
X /fl3D $.nIry (7cra lii IV) ___________
.thcd Shank I...y (Pc. TV IV ) ____
? 1 -nq and Za*s CalLbratSot ( 7Dm ‘V IV) ____ —
-------
— - • p. è - - :- -
OE i zi :c z yii z CS?) : I v ’z uz . T C t4) ±
- •. — - - -— — ..
.—. ‘ .‘ a. — a..J t• • .• s , — —
— * _____ - _‘-Iv .(_: —_
t z .$’l3 1 -s “ -‘.v ‘ -‘ -—--—- s. . e
- — —• - - -..‘: — -
A
S. Z ivo *ti .,1s* Dat.i (c td)
b. Z1p1. ata
U. Za. t* (7 XV)
a tatii 1y dantifL.d O-4 ( 7z z* X sV TIC)
tøt& L ehr &tozaa (*XC) i r
i1 pt . _____ —
ar a*c B *T 1.:
P&v s*ct a 4 bsckr ...ubtract.4 U•
ipscxa ci . —
Xii. .p..c a o ‘a .tb 3 b.et i t.braxy &‘ s. —
GPC chat. çrz .u (LZ P psr m.4)
C. £t*. szda *ta (All I zt r.z)
Xflitial C&1thrz:i &ta (7o fl XV)
RX Z a.M Qu*n Reperts i cr aU. ata d.sxda
i L q Caii ratLcn ( Toa VTT XV)
ZX .z a d Q .ai icr aLt sta daxda
Z taza1. Sta .daxd )zsa 1 a y (7cr vzuz IV )
I taru&1. St -’4&rd zaa S ’y (Tom VI C XV)
4. Mv QC ata
81 ’k atz
XatrLx Zpt.ks &ta
)(it x $pLka DupUc&ts ata
a. QC 2 =azy
Iizrr gats Psrrsut P.seevaiy S .’y (Ycz !I P1st)
xzhis Dupticat. 1’ITy ( 7cr : Psit)
Xatbo 31ti k S” y (?or XV Psat)
a. Iaxrpis at*
. Xai ,tta Or ‘-‘ 1yvia &ta Ibast
(7cm Z Past )
c ztcqrz a (?iary t )
.r .itøguaa fr s 4 ac cc cc V 4 e
GC ntsqrstic rspczt cr ay,t. prizt.cat aM
cstthat inn p1 ta
X&n *1 wcrk sha.t
VV tac.s ir a e (L i aY*ilabls)
7cr p sti td../,c . cc ZLr .d by GCflCZ, ccpi.a
Cf raw sp.ctra azd ccpLaa ef backqrc d . t arts4 a.I
.pscta Cf taxç.t cc 4s & sta.Marda)
-------
c LZ SDG JIt i(CS?) ‘ .UVZJ Tth’IX . ? (C t ) ’
- . . .,- —— ..u s- . . . . ——. .,.-——— •• ..“
—. p - • ---— -
so.tZ3’4 — - ao: “— u; -
- —__._t .._ . . . i... . _—- —
6. Pswticidaa (ct.d)
C. tt& darts ©4tz
Ps.tLCid.r t ti n Sta di .S $ AZ7
(Ycx v i : : , Pltd4)
Prtic 4a. I a1 at1e n Zta daxda I y
(7c Vi: . P.lt.’2) ___
P.stici4./P 1tsnd*r * 1&ty ( 7e , Ps*t )
Psrti ’ -/P U tiiC*tt ( T * X 2’*t )
StszA. d c &toq zu aed data sy t prim
i &1i. aun .azda —
7 psvtt idaa/P Z cc i 4 b GCJ’ . capi** C
ap.c a at& .&ztI a.4
4. Zav cc :ata
3 a.nk ata
X&t .z Zpik. &ta
Xat ix Zp k pU.c*ta Data
7.. X.1 e.11i . v *t*
Oriqi 1 r.parati sed 1ysi, iara or coL** 0 g
p.para ic aed itysii 1og oek paqsi —
T. tsr L . sa pLa and aa .. sxwact ta.nz ar (‘—of..
c stedy r.c. rga
13.1 iza an strip c & u ir
scrt.ni q tivitiss (dsa .bS or 2. .Lat)
_____________ —
$. i j /pacejyt V -’]ta
x LL1s (Xe. c i ahi sta )
n..of— astody Pa4s ____ — ____
Z.ar$a aqs
*ampls LoQ ’ .i Rast (Las & D 1)
— : C v*r Ihast
Xisc.ilan.ooi $1ippinq/c.ivi 4 Zscorda
(dascribs or 1.Lit)
tS L3 .ab 5a 1s ?rznsf.-r sed ?e i !b .
(daa .bs or list)
-------
ORG XC .co IZST . ( 7) V O ! b Ofl’ .
- r
• ••.••.• ‘ .... 4 1k—-— . . _ .j—’-• -ft--—_- ••
r ? L z ao ’ W u o .. - g
-
.O. Oth. P.e t 1 (d.scths G List) -
T*1s 1 tPt t _____ ______
_ _ —
3 . w- t I
cc t.t.d bit -. 3 t Y% _____
(=. La.b) i?.at r.) (Px 4.r tad X ./ it. a) D&t* )
_____________ C PI 2 Z
(1PM U (st zt ra) rri t s=./it3.*)
-------
t E ,44b s r ? OT C.
i o ic CL S G TILE (CS?) - I ZV TO ZT
- -. -; ..— . . .. C ‘i .4 .y ‘
3 T A It J L/$
— . .. .. . .. . . . ..,. “gvwr. . 1 —- -
• . — . ,. ,, v
. . t2 i! a
—-— , — . . . .
. 2 j- ‘- : - -:
go ants 4sJ .iv*ra tz a C pAat. & G gU st s cr .g &k 4 * w sxs —
po.sth a. ( ZmV ZI3I E, &Z t 1 C 2 )
-
1. I v. t ry £h..t (7c DC-2 ) ( o at
2. c vsx Ps s
3. I r;x . ic a. t3.ysLs ata £hnst (? )
4. ItitL.u . a. 4 C tii i rati V.ZifL& - (7O .
. . ) ZL 2.
S. . £tai d&d f . r 2 (7or 1. Put 2) Z
. I::) “7 1 #
7e I Intsrfsre .cs aek Sa.p .s (7cr V) E4 ‘ .‘
S. ZpL .a Sa.=pls ZseoYezy (7cr V, Part 2) ( O (m .. “
. Post Diçes ipL &s Swpl.s Rsccvszy (7 V, P3Xt 2)) ( (cIA
10. pU a:as (7 r V I) lb
2.1. La er&t y Cc Sa.mp s (7 x VII) I
1.2. Sta s.rd ddLtiøt a.u1ts (7cr VIII) I IOL “
13. S.rial Di1 tt z .
24. I tr .nt tsts ti t Li.itz. QUrtSZ2y I) 1 O j .
1.5. I Ti t..1 s t c ,c ic 7acecxz, A LL2.7 (7c ,
(. IUL “
: I tareXs * t C r.ci t 7actos, a. t]1y (7cr ,
Put 2) . i
37. ‘ LL ia. 7.i ti Q aaXtPZ.ty (?Cr XII) 1S t 110
3.2. P.pazzt t L q (7oz XI) 1 •’ I — —
1 . J a2ys a F Loq (?cr3 7’) ‘L
20. X Ray Data
21. T1a . .X Raw Data t (1 —
22. r aes A . Raw Data 21t 2r4 —_
23. (.rc y Paw Data 7 .r2.
24. Cyartid. paw Data z’4o —
25. Percant ScUd.s Ca c atj 2.41 2.SO
e-24
-------
Th ORGJ C L Z EDGPIT (CS?) RI C t
g8 G
—
P1= -
—=
26. :istillati Logs (Cyft”44ea 1y) 2.sl tS4 _____
27. DLges:io Logs 2 Z _____
2$. 3i Lc Za r 2- 1 2 1 ____ =
2 ZP1 Ibipp q/P..csLvL q
2ix t’ ( X c. of s i -’ta • ____ _____
IJ.fl 3*t T .se s r o 4 ____ ____
ta=pLs Taqs ___ ____
S& p1s Lcq4 Sha.t (Li & ?c C-1) ____
5 vtr 1 .s. _____
3 . acsi1&i. a £h ;/PacsiYL a; M .s
?i aU. rs cz Z)
Ts1sph @. Logs ! I L’3 ____
31. tss1 L tap s : zisz P.accrds a.zd T .rki q Z s.ta
(d•. . s or Lilt)
— __ ___ —
a
32. tirit C?igi s.1 Ga.=pls P:tpsrattc: *. d 3naLysLs *a ds
(dsac ri s or Lilt)
rtp&r&ti rac rai ____________________________________
&Lysiz rtccrti _____________________________________
33. Othsr Paeords (d.scrib. or List)
31. s taz
c t .t.d bys 4 2 AA 1 v J i Li - J3i
2 L& ) (J ( t zt ra) (Pri t u4 X&a./Tit.tS) ( a)
.L 3ditad by, ____________ cM4 1 AL cIC- ___
(t(g st .rs) 1Pri t.d(Xlas/it1s) — (D $)
-------
i i DEZX.E ,#Ut Zr DHørO C44
I OR ANIC C XPLZTZ .S G ? Z CS?) V TORT..
• • - . .. •.. .. - .:.. . ..: a •Z- .
__ __ __
- . . . -
‘ . ..A. .‘ —#‘.#••._ .-‘ —
CAU . O. 12 c11k-sD . k C i’-IDc . O T ______ ____
• —— — • —— — — — -. __ ,. _ - _ . ___ .—-— .1 . ———— • - , n- _ . _ -
________ _______
A.LL .oc sn;s aaA. .viza £ t a c p st. £DG iJ* tu*t S C L L , WA*a
çcaEbl.. (P Z7 X 3T 2 3Z 6 TI C J UCT I )
1. I .rr .ry Sh.. (?c DC-2) ( D c t ‘)
. c sr *ve
3. I crgs . .i: ) i1ysLs Dati *h..t (7 )
4. itL&t a d C :th q C ibrati Vsri2i zt 4 (IarZ
?ax 1)
S. Z. Ztand&rd i a d I (1c TI. Paz: )
. 21 (7er 11:)
7. I tar sr.n a ack Za pLs (?cz TV)
S. zpika s,=g. R.cavery (?a V 1 ar 1)
. Pest DLç.it Spiki Sap1. RacOrsry (7cz V. PZX 2))
10. D xp1i a:.s (7or VT)
1. . I o atc y Ct 1 & 1a (7c VII)
12. Stu da. ) ddttic P.aat tz (1cm vz )
3. I Earlal DL1i ti J •(7cr II)
14. I .str stt Ditiei Z.L itz, Q ars1y (7Q Z)
Ii ttra1wsr t C c..Lc . 7aet rs, A LL3.7 (7 r .
Part )
Thtar,t.e ant C rr*ci t Pietari ) ai1 y (7or .
Part )
37. I LLn.az Mng.v Q a.z:s 7 (7az )
33. Px.paratiet Log (70z5 II)
3$. na1yuia un L (7o ZT)
0. Zav Dat&
21. 7lara A3 Mw
22. 7 xta . J M v ata
23. K.rrtzy Paw Lta
24. C ’t.nida Mv et&
25. Psr *1 t Solids C-1e latiti
fl - _
—
a
-------
__________ _______ - ‘‘: _ :.—--;
- :- o c xic .C LZ s nix ‘ csr : w RI SE z
-• ‘ . ‘ ‘ - “
‘ ‘ Z - - r: GI * . C
• ••.• • : ‘— •‘
L L
. iztL11 tic. L qs (Cys!Ii4 l .2y) —
7. Diq.atLc Lcqs —
23. ai i Papor _____
2 . Xfl Shipp q/ .c.ivizq Doe ’ ts
Mz m. (Xo. ci sS.L ta —
‘i.1 .-ot.O.zst 4y Raccrda —
Sipls aqs —
Zap .s L q-I gh..t (La.b 7 C- ) —
c *.r 1 *st —
3. a *fl&zs u ;/ .scsiv g ?ac rda
(hit a L1 f?u4iyi &3. rac rdi)
a1ap e a L i
3 . ttaz a.1 .th Sip1. :z a ar *cords a 4 zckinq S .su
(des er list)
a
32. I t.r a1. C i;i a..t £& p1s P:e?s.&tic a.d ) *1ysis Rae rda
(dss x . c lilt)
r.pa.xa:Lan rsc da _________________________________ ____ ____ _____
Ui .yuis rUCQL4Z ________________________________________ ____ _____ ______
33. Othtr Meerdi (d•.ezi . er list)
34. s tzs
C p1st.d i __________ _
( .P LI ) flgrn xs) (Pxt t*d sa./1t.t$) (atS)
udit.d by __ 4’ I i t L4 ___
(SLg st ) - tPriLtsd aa,I Lt3.a ) (MU)
-------
Attachment D
“Specifications and Guidance for Contaminant-Free Sample Containers” -
Publication 9240.O-05A, EPA/540/R-93/051, December 1992
-------
C
United States Office of Publication 9240.O-05A
Environmental Protection Solid Waste and EPA54O/R-93/051
Agency Emergency Response PB93-963316
Washington, DC 20460 December 1992
Superfund
EPA Specifications and
Guidance for
Contaminant-Free
Sample Containers
-------
OSWER Directive # 9240.O-05A
December 1992
SPECIFICATIONS AND GUIDANCE
FOR
CONTAMINANT-FREE SAMPLE CONTAINERS
Office of Emergency and Remedial Response
Office of Solid Waste and Emergency Response
U.S. Environmental Protection Agency
Washington, DC 20460
-------
NOTICE
This guidance manual does not constitute a rulemaking by the Agency. The policies set forth in this Directive
are intended solely as guidance. They are not intended, nor can they be relied upon, to create any substantive
or procedural rights enforceable by any party in litigation with the United States. EPA officials may decide to
follow the guidance provided m this Directive, or may take action that is at variance with the guidance, policies,
and procedures in this Directive, on the basis of an analysis of specific circumstances. The Agency also
reserves the right to change this Directive at any time without public notice. Mention of trade names or
commercial products does not constitute endorsement or recommendation for use.
Additional copies of this document can be obtained from:
National Technical information Service (NTIS)
U.S. Department of Commerce
5285 Port Royal Road
Springfield, VA 22161
(703)487-4650
ii
-------
TABLE OF CONTENTS
SECTION TITLE PAGE
I. INTRODUCTION 1
II. SAMPLE CONTAINER AND
COMPONENT MATERIAL SPECIFICATIONS 4
III. SAMPLE CONTAINER PREPARATION
AND CLEANING PROCEDURES 14
IV. SAMPLE CONTAINER QUALITY ASSURANCE
AND QUALITY CONTROL REQUIREMENTS 17
Ill
-------
SECTION 1
INTRODUCTION
In August 1989, the Environmental Protection Agency’s (EPA) Office of Emergency and Remedial
Response (OERR) decentralized Superfund’s Sample Container Repository program (OSWER Directive
#9240.0-05). In conjunction with the decentralization of Superfund’s bottle program, OERR issued
specifications and guidance for preparing contaminant-free sample containers to assist the Regions in
obtaining appropriate sample containers from commercially available suppliers.
The December 1992 version of Specifications and Guidance for Contaminant-Free Sample
Containers” revises the specifications and provides a single source of standardized specifications and
guidance on appropriate cleaning procedures for preparing contaminant-free sample containers that meet
all Contract Laboratory Program (CLP) detection/quantitation limits, including those for low
concentration analyses.’ Although the specifications and guidance procedures contained in this document
are based on CLP low concentration requirements, they also are suitable for use in other analytical
programs.
Specifications and guidance for preparing contaminant-free sample containers are provided in the
sections that follow and are intended to describe one approach for obtaining cleaned, contaminant-free
sample containers for use by groups performing sample collection activities under Superfund and other
hazardous waste programs. Although other cleaning procedures may be used, sample containers must
meet the criteria specified in Section 11. In certain instances, the user of the sample containers may
require exact adherence to the cleaning procedures and/or quality control analysis described in this
document. In other instances, the user may require additional or different cleaning procedures and/or
quality control analysis of the sample containers. The specific needs of the bottle user will determine the
requirements for the cleaning and quality control analysis of the sample containers as long as the
minimum criteria are met. It is the responsibility of the bottle user to define the sample container
preparation, cleaning, and quality control requirements.
The document has been extensively reviewed and revised since the August 1989 iteration, and
important enhancements have been incorporated, including:
• Removing references to the color of the closures;
• Allowing the use of polypropylene closures as an alternative to phenolic closures;
• Referencing CLP Low Concentration Organics and Inorganics Statements of Work for the
analysis of calibration verification solutions and blanks;
• Including cleaning and quality control procedures for fluoride and nitrate/nitrite;
• Removing the hexane rinse from the cleaning procedure for container types A, E, F, G, H, J,
and K (semivolatile organics, pesticides, metals, cyanide, and fluoride in soils and water);
Because this document does not address the procurement of contaminant-free sample conlainers, the
title was changed from “Specifications and Guidance for Obtaining Contaminant-Free Sample Containers”
to ‘Specifications and Guidance for Contaminant-Free Sample Containers.”
I
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• Adding the recommendation that the bottle vendor establish and submit a Quality Assurance
Plan (QAP);
• Changing the QA/OC documentation requirements so that copies of the raw data from the
analyses of the QC containers are available upon request and not automatically sent co the
bottle purchaser;
• Changing the permanent lot number assignment to a nine-digit number from an eight-digit
number, where the extra digit represents the analysis parameter;
• Adding Chemical Abstract Services (CAS) registry number for the inorganic analytes in
Table 1; and
• Recommending an annual demonstration of the bottle vendor’s ability to meet detection
limits and establish reproducibility of the cleaning techniques.
OERR and the EPA Regions decided to use the most stringent CLP requirements available to set
the specifications for obtaining contaminant-free sample containers. As a result, the CL? Inorganics and
Organics Low Concentration Statement of Work (SOW) requirements were selected as the basis for these
specifications. Major factors in this decision included the desire to have a set of bottle cleaning
specifications that met or exceeded all analytical requirements and the related need to avoid potential
misuse of cleaned bottles (e.g., using a container cleaned by a multi-concentration procedure for a low
concentration sample). OERR will reevaluate this decision if the low concentration requirements are
deemed to be too stringent.
Most environmental sampling and analytical applications offer numerous opportunities for sample
contamination. For this reason, contamination is a common source of error in environmental
measurements. The sample container itself represents one such source of sample contamination. Hence,
it is vital that sample containers used within the Superfund program meet strict specifications established
to minimize contamination which could affect subsequent analytical determinations. Superfund sampling
and analysis activities require all component materials (caps, liners, septa, packaging materials, etc.)
provided by the bottle preparer to meet the criteria limits of the bottle specifications listed within Section
II.
Section III provides guidance on cleaning procedures for preparing contaminant-free sample
containers that meet the specifications contained in Section II. The procedures provided in this section
are intended to provide sample containers that meet all current CL? Low Concentration Inorganics and
Organics detection/quantitation levels.
in selecting cleaning procedures for sample containers, it is important to consider all of the
parameters of interest. Although a given cleaning procedure may be effective for one parameter or type of
analysis, it may be ineffective for another. When multiple determinations are performed on a single
sample or on a subsample from a single container, a cleaning procedure may actually be a source of
contamination for some analyte.s while minimizing contamination in others. It should be the responsibility
of the bottle supplier to verify that the cleaning procedures actually used satisfy the quality control
requirements set forth in Section IV.
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Two aspects of quality assurance (i.e., quality control and quality assessment) must be applied to
sample containers as well as to the analytical measurements. Quality control includes the application of
good laboratory practices and standard operating procedures especially designed for the cleaning of sample
containers. The cleaning operation should be based on protocols especially designed for specific
contaminant problems. Strict adherence to these cleaning protocols is imperative. Quality assessment of
the cleaning process depends largely on monitoring for adherence to the respective protocols. Because of
their critical role in the quality assessment of the cleaning operation, protocols must be carefully designed
and followed. Guidance is provided in Section IV on design and implementation of quality assurance and
quality control protocols.
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SECTION II
SAMPLE CONTAINER AND COMPONENT MATERIAL SPECIFICATIONS
This Section identifies sample containers commonly used in the Superfunci program and provides
specifications for contaminant-free sample containers for each bottle type.
A. CONTAINER MATERIAL
A variety of factors affect the choice of containers and cap material. These include resistance to
breakage, size, weight, interferences with analytes of interest, cost, and availability.
Container types A through L (Figure 1, pages 6-7) are designated as the type of sample containers
that have been used successfully in the past. Kimax or Pyrex brand borosilicate glass is inert to most
materials and is recommended where glass containers are used (i.e., pesticides and other organics).
Conventional polyethylene is recommended when plastic is acceptable because of its lower cost and lower
adsorption of metal ions. The specific sampling situation will determine the use of plastic or glass.
While the sample containers shown in Figure 1 are utilized primarily for Superfund samplingS
activities, they also may be used for sampling activities under other programs, such as the Resource
Conservation and Recovery Act (RCRA).
B. MAXIMUM CONTAMINANT LEVEL SPECIFICATIONS FOR SAMPLE CONTAINERS
The CLP, through a series of technical caucuses, has established inorganic Contract Required
Detection Limits (CRDL) and organic Contract Required Quantitation Limits (CRQL) which represent
the minimum quantities needed to support the hazardous substance identification and monitoring
requirements necessary for remedial and other actions at hazardous waste sites.
For inorganic sample containers, the CRDLs listed in Table 1, page 8, are the specifications for
maximum trace metal contamination. Concentration at or above these limits on any parameter should
preclude these containers from use in collecting inorganic samples.
The CROL specifications for organic sample containers are listed in Table 2, pages 9-13. When
the CRQL in Table 2 is multiplied by the appropriate factor listed below, the resulting value then
represents the maximum concentration allowed for particular sample containers based on organic CLP
sample sizes for routine analyses.
Container type Multiple of CRQL
A 1.0
B 0.5
D 10.0
E 8.0
F 4.0
0 2 0
H 0.5
.1 0.5
K
4
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The philosophy used for determining the maximum permissible amount of contamination in a
sample container was to consider the number of aliquots of sample that are available in the coniaine and
assume that the contamination present would be uniformly distributed in all of the aliquots. This
assumption, and the assumption that there should be no more than one-half the CROL contributed by the
container, resulted in the establishment of contamination limits by container type. For example, the
volume of container type D is sufficient to allow 20 volatile determinations. Therefore, ii 10 times the
CROL of contaminant is present in the cleaned bottle, each aliquot tested will contain one-half of the
CRQL of contaminant due to the contribution from the bottle.
C. GROSS CONTAMINATION
Gross contamination is defined as greater than two hundred times the acceptable concentration
values in Tables I or 2 (multiplied by the appropriate factor), unless the cleaning procedure is successful
in reducing the amount of contamination to within specifications. If this is not achieved, the grossly
contaminated materials should be discarded and replaced to prevent cross contamination with other
batches of containers. The bottle preparer should inspect all materials to ensure conformance with the
required specifications.
5
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FIGURE 1
SAMPLE CONTAINER
SPECIFICATIONS
Container
Type Specifications
A Container : 80-oz amber glass, ring handle
bottle/jug, 38-mm neck finish.
Closure : polypropylene or phenolic cap,
38-430 size; 0.015-in Teflon liner.
Total Weight : 2.45 lbs.
B Container : 40-mL glass vial, 24-mm neck finish.
Closure : polypropylene or phenolic, open-top,
screw cap, 15-cm opening, 24-400 size.
Septum : 24-mm disc of 0.005-in Teflon
bonded to 0.120-in silicon for total thickness
of 0.125-in.
Total Weight : 0.72 oz.
C Container : 1-L high-density polyethylene,
cylinder-round bottle, 28-mm neck finish.
Closure : polyethylene cap, ribbed, 28-4 10 size;
F217 polyethylene liner.
Total Weight : 1.89 oz.
D Container : 120-mL wide mouth, glass vial,
48-mm neck finish.
Closure : polypropylene cap, 48-400 size;
0.015-in Teflon liner.
Total Weight : 4.41 oz.
E Container : 16-oz tall, wide mouth,
straight-sided, flint glass jar,
63-mm neck finish.
Closure : polypropylene or phenolic cap,
63-400 size; 0.015-in Teflon liner.
Total Weight : 9.95 OZ.
F Container : 8-oz short, wide mouth,
straight-sided, flint glass jar,
70-mm neck finish.
Closure : polypropylene or phenolic cap,
70-400 size; 0.015-in Teflon liner.
Total Weight : 7.55 oz.
6
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FIGURE 1
SAMPLE CONTAINER
SPECIFICATIONS
(Continued)
Container
Type Specifications
G Container : 4-oz tall, wide mouth,
straight-sided, flint glass jar,
48-mm neck finish.
Closure : polypropylene or phenolic cap,
48-400 size; 0.015-in Teflon liner.
Total Weight : 4.70 oz.
H Container : I-L amber, Boston round, glass
bottle, 33-mm pour-out neck finish.
Closure : polypropylene or phenolic cap,
33-430 size; 0.015-in Teflon liner.
Total Weight : 1.11 lbs.
J Container : 32-oz tall, wide mouth,
straight-sided, flint glass jar,
89-mm neck finish.
Closure : polypropylene or phenolic cap,
89-400 size; 0.015-in Teflon liner.
Toial Weight : 1.06 lbs.
K Container : 4-L amber glass, ring handle
bottle/jug, 38-mm neck finish.
Closure : polypropylene or phenolic cap,
38-430 size; 0.015-in Teflon liner.
Total Weight : 2.88 lbs.
L Container : 500-mL high-density polyethylene,
cylinder-round bottle, 28-mm neck finish.
Closure : polypropylene cap, ribbed, 28-410 size;
F217 polyethylene liner.
Total Weight : 1.20 oz.
7
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TABLE 1
INORGANIC ANALYrE
SPECIFICATIONS
Analyte CAS Number CRDL’ Qzg/L)
1. Aluminum 7429 .90-5 100
2. Antimony 7440-36.1) 5
3. Arsenic 7440-38-2 2
4. Barium 7440-39-3 20
5. Beryllium 7440-41.7
6. Cadmium 7440-43-9 1
7. Calcium 7440-70-2 500
8. Chromium 7440-47-3 10
9. Cobalt 7440-48-4 10
10. Copper 7440-50-8 10
11. Iron 7439-89-6 500
12. Lead 7439-92-1 2
13. Magnesium 7439-95-4 500
14. Manganese 7439-96-5 10
15. Mercury 7439-97-6 0.2
16. Nickel 7440-02-0 20
17. Potassium 7440-09-7 750
18. Selenium 7782-49-2 3
19. Silver 7440-22-4 10
20. Sodium 7440-23-5 500
21. Thallium 7440-28-0 10
22. Vanadium 7440-62-2 10
23. Zinc 7440-66-6 20
24. Cyanide 57-12-5 10
25. Fluoride 16984-48-8 200
26. NitratefNitrite 1-005 100
CRDLS are based on the CLP Inorgani Low Concentration SOW
8
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TABLE 2
ORGANIC COMPOUND
SPECIFICATIONS
Volatiles CAS Number CRQL 1 (pgfL)
1. Chloromethane 74-87-3 1
2. Bromomethane 74-83-9 1
3. Vinyl Chloride 75-01-4 1
4. Cttloroethane 75-00.3 I
5. Methylene Chloride 75-09-2 2
6. Acetone 67-64-1 5
7. Carbon Disulfide 7545-0 1
8. 1,1-Dichloroethene 75-35-4 1
9. 1,1-Dichloroethane 75-34-3 1
10. C s-I ,2-Dichloroethene 156-59-4 1
11. trans-1,2-Dichloroethene 156 .60-5 1
12. Chloroform 67.66-3 1
13. 1,2-Dichloroethane 107-06-2 1
14. 2-Butanone 78-93-3 5
15. Bromochloromethane 74 -97-5 1
16. 1,1,1-Trichloroethane 71-55 -6 1
17. Carbon Tetrachloride 56-23-5 1
18. Bromodichloromethane 75-27-4 1
19. L,2-Dichloropropane 78-87-5 1
20. cis-1 ,3-Dichloropropene 10061-01-5 1
21. TriChloroethene 79-01-6 1
22. Dibromochloromethane 124-48-1 1
23. 1,1,2-Trichloroethane 79-00-5 1
24. Benzene 71-43-2 1
25. trans- 1,3-Dichloropropene 10061-02-6 1
26. Bromoform 75-25-2 1
27. 4-Methyl-2-pentanone 108-10-1 5
28. 2-Hexanone 591-78-6 5
29. Tetrachloroethene 127-18-4 1
30. 1,1 ,2,2-Tetrachloroethane 79-34-5 1
1 CRQLs are based on the CLP Organk Low Concentration SOW
9
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TABLE 2 (cont.)
ORGANIC COMPOUND
SPECIFICATIONS
Volatiles
CAS Number
CRQL’ ( 1 zgfL)
31.
1,2.Dibromoethane
106-93-4
1
32.
Toluene
108-88-3
1
33.
Chlorobenzene
108-90 .7
1
34.
Ethylbenzene
100-414
1
35.
Styrene
100-42-5
1
36.
Xylenes (total)
1330-20-7
1
37.
1 ,3-Dichlorobenzene
541-73-i
I
38.
1,4-Dichlorobenzene
106-46-7
1
39.
1,2-Dichlorobenzene
95-50-1
1
40.
1 ,2.Dibromo-3-chloropropane
96-12-8
1
CRQLS are based on the CLP Organks Low Concentration SOW
10
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TABLE 2 (conl)
ORGANIC COMPOUND
SPECIFICATIONS
Semivolatiles CAS Number CRQL 1 (pgfL)
I. Phenol 108-95-2 5
2. bis-(2.Chlorethyl)ether 111-44-4 5
3. 2-Chlorophenol 95-57-8 5
4. 2-Methy lphenol 95-48-7 5
5 2,2’-oxybis-( I-Chloropropane) 108-60-1 5
6. 4.Me lhylphenol 106-44-5 5
7. N -Niroso-di-n-dipropylamine 621-64-7 5
8. Hexach loroethane 67-72.1 5
9. Nitrobenzene 98-95-3 5
10. Isophorone 78-59-1 5
11. 2-Nitrophenol 88-75-5 5
12. 2,4-Dimethylphenol 105-67-9 5
13. bis-(2-Chloroethoxy)methane 111-91.1 5
14. 2,4-Dichlorophenol 120-83-2 5
15. 1 ,2,4-Trichlorobenzene 120-82-1 5
16. Naphthalene 91-20-3 5
17. 4-Chloroaniline 106-47-8 5
18 Hexach lorobutadiene 87-68-3 5
19. 4-Chloro-3-methylphenol 59-50-7 5
20. 2-Methylnaptithalene 91-57-6 5
21. Hexachlorocyclopentadiene 77-47-4 5
22. 2,4,6-Trichlorophenol 88-06-2 5
23. 2,4,5-Trichlorophenol 95 -95-4 20
24. 2-Chloronaphthalene 91-58-7 5
25. 2-Nitroaniline 88-74-4 20
26. Dimethylphihalate 131-11-3 5
27. Acenaphthylene 208-96-8 5
28. 2,6-Dinitrotoluene 606-20-2 5
29. 3-Nitroaniline 99-09-2 20
30. Acenaphthene 83-32-9 5
CRQLs are based on the CLP Organics Low Concentration SOW
11
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TABLE 2 (cont.)
ORGANIC COMPOUND
SPECIFICATIONS
Semivolatiles CAS Number CRQL’ ( 1 g/L)
31. 2,4-Dinitrophenol 51-28-5 20
32. 4-Nitrophenol 100-02.7 20
33. Dibenzofuran 132-64-9 5
34. 2,4-Dinnrotoluene 121-14-2 5
35. Diethylphthalate 84-66-2 5
36. 4-Ch!orophenyl-phenylether 7005-72-3 5
37. Fluorene 86-73-7 5
38. 4-Nitroaniline 100-01-6 20
39. 4,6-Dinitro-2-methylphenol 534-52-1 20
40. N-Nitrosodiphenylamine 86-30-6 5
41. 4-Bromophenyl-phenylether 101.55-3 5
42. Hexachlorobenzene 118.74-1 5
43. Pentachlorophenol 87-86-5 20
44. Phenanthrene 85-01-8 5
45. Anthracene 120-12-7 5
46. Di-n-butylphthalate 84-74-2 5
47. Fluoranthene 206-44-0 5
4 S Pyrene 129-00-0 5
49. Butylbenzylphthalate 85-68-7 5
50. 3,3’-Dichlorobenzidine 91-94-1 5
51. Benzfajanthracene 56-55-3 5
52. Chyrsene 218-01-9 5
53. bis-(2-Ethylhexyl)phthalate 117-81-7 5
54. Di-n-octylphthalate 117-84-0 5
55. Benzo [ bltluoranthene 205-99-2 5
56. Benzo [ klfluoranthene 207-08-9 5
57. Benzolalpyrene 50-32-8 5
58. Indeno( I ,2,3.cd)pyrene 193-39-5 5
59. Dibenz [ a,hlanthracene 53-70-3 5
60. Benzo(g,h,i pety1ene 191-24-2 5
‘CRQLS are based on the CLP Organics Low Concentration SOW
12
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TABLE 2 (cont.)
ORGANIC COMPOUND
SPECIFICATIONS
Pesticides/PCBs CAS Number CRQL’ (pg/L)
1. a lpha -Bi-IC 319-84.6 0.01
2. beta-BHC 319-85-7 0.01
3. deRa-BHC 319-86-8 0.01
4. gamma-BHC (Lindane) 58-89-9 0.01
5. Heptachlor 76.44-8 0.01
6. AIdrin 309-00-2 0.01
7. Heptachlor epoxide 1024-57-3 0.01
8. Endosulfan 1 959-98-8 0.01
9. Dte ldrin 60-57-1 0.02
10. 4,4’-DDE 72-55-9 0.02
11. Endrin 72-20.8 0.02
12. Endosulfan II 33213-65-9 0.02
13. 4,4’-DDD 72-54-8 0.02
14. Endosulfan sulfaLe 1031-07-8 0.02
15. 4,4’-DDT 50-29-3 0.02
16. Methoxychlor 72-43-5 0.10
17. Endrin ketone 53494-70-5 0.02
18 Endnn aldehyde 7421 -36.3 0.02
19 aipha-Ch lordane 5103-71.9 0.01
20. garnma-Chlordane 5103-74-2 0.01
21. Toxaphene 8001-35-2 1.0
22. Aroclor-1016 12674-11-2 0.20
23. Aroclor-1221 11104-28-2 0.20
24. Aroclor-1232 11141-16-5 0.40
25. Aroclor-1242 53469-21.9 0.20
26. Aroclor-1248 12672-29-6 0.20
27. Aroclor-1254 11097-69-1 0.20
28. Aroclor-1260 11096-82-5 0.20
CROLs are based on the CLI’ Organics Low Concentration SOW
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SECI ION III
SAMPLE CONTAINER PREPARATION AND CLEANING PROCEDURES
This Section is provided as guidance for the preparation of sample containers that meet the
contaminant-free specifications contained in Section II. There are various procedures for cleaning sample
containers depending upon the analyses to be performed on the sample. The following cleaning
procedures are modeled after those specified for the Superfund Sample Container Repository program.
Other suitable cleaning procedures exist and may be used as long as the sample containers meet the
criteria established in Section II. In some instances, the specific needs of the bottle user may dictate exact
adherence to the sample container preparation and cleaning procedures that follow, while in other
instances, modifications may be required. It is the responsibility of the bottle user to define the sample
container preparation, cleaning, and quality control requirements.
A. Cleaning Procedure for Container Types: A. E, F, 0, H, .T, and K
1. Sample Type: Semivolatile Organics, Pesticides, MetaLs, Cyanide, and Fluoride in Soils and Water.
a. Wash glass bottles, Teflon liners, and caps with hot tap water using laboratory grade
nonphosphate detergent.
b. Rinse three times with copious amounts of tap water to remove detergent.
c. Rinse with 1:1 nitric acid (reagent grade HNO 3 , diluted with ASTM Type I deionized water).
d. Rinse three times with ASTM Type I organic free water.
e. Oven dry bottles, liners, and caps at 105-125°C for one hour.
f. Allow bottles, liners, and caps to cool to room temperature in an enclosed contaminant-free
environment.
g. Rinse bottles with pesticide grade methylene chloride (or other suitable solvents specified by
the bottle user) using 20 mL for 1 /2-gallon containers; 10 mL for 32-oz and 16-oz containers;
and 5 mL for 8-oz and 4-oz containers.
h. Oven dry bottles, liners, and caps at 105-125°C for one hour.
i. Allow bottles, liners, and caps to cool to room temperature in an enclosed contaminant-free
environment.
j. Place liners in lids and cap containers.
k. Label each container with the lot number and pack in a case.
I. Label exterior of each case with the lot number.
m. Store in a contaminant-free area.
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2. Sample Type: Nitrate/Nitrite in Soils and Water.
a. Substitute reagent grade sulfuric acid (H 2 S0 4 ) for nitric acid in step A.l.c.
b. Follow all other steps in the cleaning procedure described in part A.l above.
B. Cleaning Procedure for Container Types: B, D
Sample Type: Purgeable (Volatile) Organics in Soils and Water.
a. Wash glass vials, Teflon-backed sepia, Teflon liners, and caps in hot water using laboratory
grade nonphosphate detergent.
b. Rinse three times with copious amounts of tap water to remove detergent.
c. Rinse three times with ASTM Type I organic-free water.
d. Oven dry vials, caps, sepia, and liners at 105-125C for one hour.
e. Allow vials, caps, sepia, and liners to cool to room temperature in an enclosed contaminant-
free environment.
f. Seal 40-mL vials with sepia (Teflon side down) and cap.
g. Place liners in lids and cap 120-mL vials.
h. Label each vial with the lot number and pack in a case.
I. Label exterior of each case with the lot number.
j. Store in a contaminant-free area.
C. Cleaning Procedure for Container Types: C, L
Sample Type: Metals, Cyanide, and fluoride in Soils and Water.
a. Wash polyethylene bottles and caps in hot tap water using laboratory-grade nonphosphate
detergent.
b. Rinse three times with copious amounts of tap water to remove detergent.
c. Rinse with 1:1 nitric acid (reagent grade HNO 3 , diluted with ASTM Type I deionized water).
d. Rinse three times with ASTM 1 ’pe I deioniied water.
e. Invert and air dry in a contaminant-free environment.
f. Cap bottles.
g. Label each container with the lot number and pack in a case.
15
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h. Label exterior of each case with the lot number.
i. Store in a contaminant-free area.
2. Sample Type: Nitrate/Nitrite in Soils and Water.
a. Substitute reagent grade sulfuric acid (H 2 S0 4 ) for nitric acid in step C.1.c.
b. Follow all other steps in the cleaning procedure described in part C.1 above.
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SECTION IV
SAMPLE CONTAINER QUALITY ASSURANCE AND QUALITY CONTROL REQUIREMENTS
A. Quality Assurance
The objectives of this Section are to: (1) present procedures for evaluating quality assurance (QA)
information to ensure that specifications identified in Section II have been met, and (2) discuss techniques
(or the quality control (QC) analysis of sample containers to be used in conjunction with the cleaning
procedures contained in Section III.
The bottle vendor should establish a Quality Assurance Plan (QAP) with the objective of
providing sound analytical chemical measurements, production procedures, and tracking systems. The
QAP should incorporate procedures for the inspection of incoming raw materials; preparation, cleaning,
and labeling of container lots; quality control analyses of cleaned container lots; document control,
including all documentation required for analysis, packing, shipping, and tracking of container lots; any
necessary corrective actions; and any quality assessment measures implemented by management to ensure
acceptable performance. The QAP should be available and provided to the bottle purchaser upon request.
Major QAJQC activities should include the inspection of all incoming materials, QC analysis of
cleaned lots of containers, and monitoring of the container storage area. Complete documentation of all
QC inspection results (acknowledging acceptance or rejection) should be kept as part of the permanent
bottle preparation files. QAIQC records (e.g., preparation/QC logs, analytical data, data tapes, storage log)
also should be stored in a central location within the facility.
Documentation indicating that the container lot has passed all QA/QC requirements should be
provided by the bottle vendor to the bottle purchaser with each container lot. Documentation should
include a signed and dated cover statement affirming that all QA/QC criteria were met. Copies of raw
data from applicable analyses of the QC containers, laboratory standards, check samples, and blanks should
be available and provided upon request. Original documentation should be retained for at least 10 years.
Minimum documentation that should be available, if applicable, for each lot of containers includes:
• A statement that NSample container lot _____ meets or exceeds all QA/QC criteria
established in ‘Specifications and Guidance for Contaminant-Free Sample Containers; ’
• Reconstructed Ion Chromatographs (RICs) from volatile and semivolatile organics
determinations, including calibration verification standards, check samples, and blanks;
• GC chromatographs from pesticides determinations, including calibration verification
standards, check samples, and blanks;
• ICP, hydride-IC?, or ICP-MS instrument readouts from metals determinations, including
calibration verification standards, check samples, and blanks;
• AA raw data sheets and instrument readouts from metals determinations, including
calibration verification standards, check samples, and blanks; and
• Cyanide, fluoride, and nitrate/nitrite raw data sheets and instrument readouts from these
determinations, including calibration verification standards, check samples, and blanks.
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Prior to the first shipment of containers, and at least annually thereafter, the batik vendor should
demonstrate its ability to meet the CRDLS and CRQLs, and establish the reproducibility of the clcaning
techniques for each bottle type. The ability to meet the CRDLs and CRQLS is accomplished through the
determination of instrument detection limits (IDLs). The bottle vendor should use the procedures in the
current CL? Low Concentration Inorganics and Organics SOWs to determine IDLs. IDLs should be
below the CRDLs or CRQLs. To establish the reproducibility for each bottle type, the bottle vendor
should randomly pick seven containers from a cleaned lot and analyze as described in the Quality Control
Analysis part of this Section. Parameter concentrations should be at or below the CRDL or CRQL for
each bottle type. Documentation from these analyses should be available and provided upon request.
I. Incoming Materials Inspection:
A representative item from each case of containers should be checked for conformance with
specifications provided in Section II. Any deviation should be considered unacceptable. A log of
incoming shipments should be maintained to identi1 ’ material type, purchase order number, and delivery
date The date of incoming inspection and acceptance or rejection of the material should also be recorded
on this log.
2. Quality Control Inspection of Cleaned Lots of Containers:
Following container cleaning and labeling, containers should be randomly selected from each
container lot to be used for QC purposes. The two categories of QC containers should be as follows:
a. Analysis QC Containers:
One perccnt of the total number of containers in each lot should be designated as the analysis QC
container(s). For lots of less than 100 containers, one container should be designated as the
analysis QC container. The sample container preparer should analyze the analysis QC
container(s) to check for contamination prior to releasing the associated container lot for
shipment. The QC analyses procedures specified in the Quality Control Analysis part of this
Section for determining the presence of semivolatile and volatile organics, pesticides, metals,
cyanide, fluoride, and nitrate/nitrite should be utilized.
For each analysis QC container(s), an appropriate QC number should be assigned that cross-
references the QC container to the related lot of containers. For example, the QC number could
be a seven-digit number sequentially assigned to each lot that has undergone QC analysis. Under
this numbering scheme, the first alphabetical character would be the container type letter from
Figure 1, the next four digits would be assigned sequentially in numerical order starting with
“0001” for the first lot to undergo QC analyses, the sixth character would indicate the number of
QC container for the lot, (e.g., “1’ for the first QC container in the lot, U2U for the second, etc.)
and the last character would be either a “C” to indicate clearance or an “R” to indicate rejection.
If the representative analysis QC container(s) passes QC inspection, the related lot of containers
should be released, and the appropriate QC number should be entered in the preparationlQC log
to indicate clearance of the lot for shipment.
If the analysis QC container(s) are found to be contaminated per the specified QC analysis
procedures, the appropriate QC rejection number should be assigned and entered in the
preparationJQC log. Any container labels should be removed and the entire lot returned for
reprocessing under a new lot number. Excessive QC rejection for a particular container type
should be noted for future reference.
18
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A laboratory standard, check sample, and a blank should be run with each QC analysis. A
calibration verification standard should be analyzed once every 12 hours. All QC analysis results
should be kept in chronological order by QC report number in a central QC file. The QC
numbers assigned should be documented in the preparation/QC log, indicating acceptance or
rejection and date of analysis.
A container lot should not be released for shipment prior to QC analysis and clearance. Once the
containers have passed QC inspection, the containers should be stored in a contaminant-free area
until packaging and shipment.
b. Storage QC Containers:
One QC container per lot should be designated as the storage QC container. The storage QC
container should be separated from the lot after cleaning and labeling and should be stored in a
designated contaminant-ftee area for one year. The date the container is placed in the storage
area should be recorded in the storage QC container log.
If contamination of the particular container lot comes into question at any time following
shipment, the storage QC container should be removed from the storage area and analyzed using
the QC analysis procedures for that container type (see Quality Control Analysis, this Section).
Upon removal, containers should be logged out of the storage area.
The designated storage area should be monitored continuously for volatile contaminants in the
following manner. A precleaned, 40-mL vial that has passed a QC inspection should be filled with
ASTM Type I organic-free water and be placed in the storage area. This vial should be changed at
one-week intervals. The removed vial should be subjected to analysis for volatile organics as
described in the Quality Control Analysis part of this Section. Any peaks indicate contamination
Identif ’ contaminants, if present, and include the results in a report to all clients who purchased
bottles from the affected lot(s).
B. Quality Control Analysis
The types of QC analyses correlate with the types of containers being analyzed and their future
use in sample collection. The QC analyses are intended for the determination of:
• Semivolatile organics and pesticides;
• Volatile organics;
• Metals;
• Cyanide;
• fluoride; and
• Nitrate/Nitrite.
QC analyses should be performed according to the container type and related sample type and
utilize the specific method(s) described below.
19
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Determination of Semivolatile Organics and Pesticides:
Container Types: A, E, F, G, H, J, and K
a. Sample Preparation:
• Add 60 mL of pesticide.grade methylene chloride to the container and shake for two
minutes.
- Transfer the solvent to a Kuderna-Danish (KD) apparatus equipped with a three-ball
Snyder column. Concentrate to less than 10 mL on a steam bath. Split the solvent into
two 5 mL fractions for semivolatile and pesticide determinations.
• Add 50 mL of pesticide-grade hexane (for pesticide determinations only) to the KD
apparatus by slowly pouring down through the Snyder column. Concentrate to less than
10 mL to effect solvent replacement of hexane for methylene chloride.
- Concentrate the solvent to I mL using a micro-Snyder column.
- Prepare a solvent blank by adding 60 mL of the rinse solvent used in step of the
cleaning procedure for container types A, E, F, G, H, J, and K (Section III page 14)
directly to a K]) apparatus, and proceed as above.
b. Semivolatile Organics Sample Analysis:
- Instrument calibration should be performed as described in the most recent CLP Low
Concentration Organics SOW with the following exceptions:
(1) If problems are encountered meeting the %RSD criteria on the initial calibration
for semivolatiles, the high concentration point should be deleted and a four-point
calibration used.
(2) The low concentration standard should be used for the continuing calibration
standard for semivolatile analyses.
(3) The percent difference window should be widened to ± 30 percent for all
compounds.
- Inject 1 L of solvent into a gas chromatograph/mass spectrometer (GCIMS).
- Calibration verification standards should be analyzed as described in the most recent
CLP Low Concefltration Organics SOW.
- Blanks should be run as described in the most recent CLP Low Concentration Organics
SOW.
- If compounds other than those listed in Table 2 are found in the container blank that
are not in the solvent blank at a peak height or peak area greater than 20 percent of the
nearest internal standard, the containers should be rejected (See Section II, Table 2 for
compound specifications).
- Identify and quantitate any contaminant(s) that cause rejection of a container lot.
20
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- A standard mixture of the nine semivolatile organic compounds listed in Table 3 (rage
26) with concentrations in the 5-20 ppb range should be analyzed to ensure that
sensitivities are achieved chat will meet contract required quantitation limits. This
standard should be prepared from a different source from the calibration standards.
c. Pesticides Sample Analysis:
• Instrument calibration should be performed as described in the most recent CLP Low
Concentration Organics SOW.
• Inject 1 L of solvent into a gas ctiromatograph (GC) equipped with an electron capture
detector (ECD).
- Calibration verification standards should be analyzed as described in the most recent
CLP Low Concentration Organics SOW.
• Blanks should be run as described in the most recent CLP Low Concentration Organics
Sow.
- If compound peaks other than those listed in Table 2 are at a peak height or peak area
greater than 5 percent of the peak height or peak area of tetra chloro-m-xylene, the
containers should be rejected (See Section II, Table 2).
- Identify and quantitate any contaminant(s) that cause rejection of a container lot.
- A standard mixture of the seven pesticide compounds listed in Table 3 (page 26) with
concentrations in the 0.01 to I ppb range should be analyzed to ensure that sensitivities
are achieved that will meet contract required quantitation limits. This standard should
be prepared from a different source from the calibration standards.
2. Determination of Volatile Organics:
Container Types: B and D
a. Sample Preparation:
- Fill the container with ASTM Type I organic-free water.
- Cap the container and let stand for 4.8 hours.
b. Sample Analysis:
- Instrument calibration should be performed as described in the most recent CLP Low
Concentration Organics SOW with the following exceptions:
(1) If problems are encountered meeting the %RSD criteria on the initial calibration
for volatiles, the high concentration point should be deleted and a four-point
calibration used.
(2) The low concentration standard should be used for the continuing calibration
standard for volatile analyses.
(3) The percent difference window should be widened to ± 30 percent.
21
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Calibration verification standards should be analyzed as described in the most recent
CL? Low Concentration Organics SOW.
• Blanks should be run as described in the most recent CLP Low Concentration Organics
SOW. The blank should consist of an aliquot of the ASTM Type I water used in the
sample preparation.
- If compounds other than those listed in Table 2 are found in the container blank that
are not in the solvent blank at a peak height or peak area greater than 20 percent of the
nearest internal standard, the containers should be rejected (See Section II, Table 2 for
compound specifications).
- Identify and quantitate any contaminant(s) that cause rejection of a container lot.
A standard mixture of the five volatile organic compounds listed in Table 3 (page 26)
with concentrations in the 1-5 ppb range should be analyzed to ensure that sensitivities
are achieved that will meet contract required quantitation limits. This standard should
be prepared from a different source from the calibration standards.
3. Determination of Metals:
Container Types: A, C, E, F, G, H, J, K and L
a. Sample Preparation:
- Add 100 mL of ASTM Type I deionized water to the container, and acidify with 1.0 mL
of reagent-grade HNO 3 . Cap and shake for three to five minutes.
- Cap the container and let stand for 48 hours.
- Treat the sample as a dissolved metals sample. Analyze the undigested water using the
most recent CLP Low Concentration InorganiCs SOW.
b. Sample Analysis:
- Instruments used for the analysis of the samples should meet the contract required
detection limits in Table 1.
- The ASThI Type I deionized water should be analyzed before use on the bottles that are
designated for analysis to ensure that contaminated water is not used for rinsing the
bottles.
- Calibration verification standards should be analyzed as described in the most recent
CLP Low Concentration Inorganics SOW.
- Blanks should be analyzed as described in the most recent CLP Low Concentration
lnorganics SOW. A calibration blank is a solution made up exactly like the sample
preparation solution. The calibration blank should be less than the values contained in
Table 1.
- A set of standards in the expected working range should be analyzed with each analytical
run. The acid matrix of the standards, blank, and quality control samples should match
that of the samples.
22
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- Concentrations at or above the detection limit for each parameter (listed in Table 1)
should be cause for rejection of the lot of containers. NOTE: The sodium detection
limit for container types A, E, F, 0, H, J, and K is 5000 ig/L unless the containers will
be used for low concentration analyses, then the detection limit is 500 pgfL.
4. Determination of Cyanide:
Container Types: A, C, E, F, G, H, J, K and L
a. Sample Preparation:
- Place 250 mL of ASTM Type I deionized water in the container. Add 1.25 mL of 6N
NaOH (for container types F and 0 use 100 mL of ASTM Type I deionized water and
0.5 mL of 6N NaOl-f). Cap the container and shake vigorously for two minutes.
b. Sample Analysis:
- Analyze an aliquot as described in the most recent CLP Low Concentration Inorganics
SOW.
- The detection limit should be 10 gfL or lower.
• Calibration verification standards should be analyzed as described in the most recent
CLP Low Concentration Inorganics SOW.
- Blanks should be run as described iii the most recent CLP Low Concentration Inorganics
SOW. The calibration blank should consist of an aliquot of the ASTM Type I water
used above.
• A set of standards in the expected working range, a check sample, and blank should be
prepared exactly as the sample was prepared.
- The detection of 10 JLg/L cyanide (or greater) should be cause for rejection of the lot of
containers. NOTE: Contamination could be due to the container, the cap, or the
NaOH.
5. Determination of Fluoride:
Container Types: A, C, E, F, G, I-I, J, K and L
a. Sample Preparation:
- Place 250 mL of ASTM Type I deionized water in the container (for container types F
and 0 use 100 mL of ASTM Type I deionized water). Cap the container and shake
vigorously for two minutes.
b. Sample Analysis:
- Analyze an aliquot as described in the most recent CLP Low Concentration Inorganics
SOW.
- The detection limit should be 200 pgfL or lower.
23
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- Calibration verification standards should be analyzed as described in the most recent
CLP Low Concentration Inorganirs SOW.
- Blanks should be run as described in the most recent CLP Low Concentration Inorganics
SOW. The calibration blank should consist of an aliquot of the ASTM Type I water
used above.
- A set of standards in the expected working range, a check sample, and blank should be
prepared exactly as the sample was prepared.
- The detection of 200 g/L (or greater) of fluoride should be cause for rejection of the lot
of containers. NOTE: Contamination could be due to the container or the cap.
6. Determination of NitratefNitrite:
Container Types: A, C, E, F, G, H, J, K and L
a. Sample Preparation:
- Place 250 mL of ASTM Type I deionized water in the container (for container types F
and G use 100 mL of ASTM Type I deionizei water). Cap the container and shake
vigorously for two minutes.
b. Sample Analysis:
- Analyze an aliquot as described in the most recent CLP Low Concentration Inorganics
sow.
- The detection limit should be 100 pgfL or lower.
- Calibration verification standards should be analyzed as described in the most recent
CLP Low Concentration Inorganics SOW.
- Blanks should be run as described in the most recent CLP Low Concentration Inorganics
SOW. The calibration blank should consist of an aliquot of the ASTM Type I water
used above.
- A set of standards in the expected working range, a quality control sample, and blank
should be prepared exactly as the sample was prepared.
- The detection of 100 g/L (or greater) of nitrate/nitrite should be cause for rejection of
the lot of containers. NOTE: Contamination could be due to the container or the cap.
C. Preparation and Labeling
Sampling for environmental specimens requires that sample containers be transported to field sites
prior to sample collection. As a result, considerable time may elapse between the receipt of sample
containers and collection of the samples. Because of the large number of samples taken at any one site,
accounting for all sample containers can become extremely difficult. The following guidance on the
identification and tracking of sample containers is based on procedures that have been used successfully in
the CLP bottle program.
24
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Each shipment should be inspected to verify that the requested number of cleaned and prepared
sample containers have been supplied and meet the requirements specified in Section I I (Tables I
and 2). If any shipment fails to meet the required specifications, it should be discarded and
replaced with a supply of sample containers that meet the required criteria.
2. The sample containers should be removed and prepared in accordance with the methods
designated below.
3. A permanent nine.digit lot number should be assigned to each lot of sample containers for
identification and tracking purposes throughout the life of the containers. Figure 2 provides an
example of a lot number sequence.
FIGURE 2
LOT NUMBER SEQUENCE
95th day
r—Analysis Parameter
the year
Repository
Code
A 2 095 01
Container J
1 rpeA
Belongs to the 1st Lot
Year i washed that day
a. The first digit represents the container type in Section II (Figure 1).
b. The second digit represents the last digit of the calendar year.
c. The next three digits represents the day of the year on which the sample containers were
washed.
d. The sixth and seventh digits represent the daily lot number.
e. The cighth digit represents the analysis parameter where:
A = Semivolatile organics. pesticides, metals, cyanide, and fluoride;
B = Metals, cyanide, and fluoride;
V = Volatile organics;
S = Semivolatile organics and/or pesticides;
M = Metals;
C = Cyanide;
F = Fluoride; and
N = Nitrate/nitrite.
The final digit represents the identification of the person who prepared the lot.
25
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4. The lot number for each container should be entered, along with the date of washing, type of
container, and number of containers per lot, into the preparation/QC log book.
5. Lot numbers printed with solvent resistant ink on a nonremovable label should remain with the
corresponding containers throughout the cleaning procedure.
6. After sample container cleaning and drying, the label should be aflixed to the containers in a
permanent manner.
7. At least one face should be clearly marked, excluding the top and bottom faces, of each case of
sample containers with the assigned lot numbers.
TABLE 3
STANDARD MIX FURES OF ORGANIC COMPOUNDS TO VERIFY SENSITIVITY
Volatiles
Semivolatiles
Pesticides
Methylene Chloride
Nitrobenzene
Gamma-BHC
Acetone
4-Chioroaniline
Heptachlor
Aidrin
2.Butanone
2,6-Dinitrotoluene
Dieldrin
Trichioroethene
Toluene
Diethylphthalate
4-Bromophenyl-phenylether
Hexachlorobenzene
Pentachiorophenol
Di-n-buty lphthalate
bis(2.Ethylhexyl)phthalate
Endrin
4,4’-DDT
Aroclor 1260
26 * J• , G.P.O. :1993_341_83581056
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Attachment E
“User’s Guide to the Contract Laboratory Program”, EPA/540/P-91/002,
January 1991
-------
9240.0-0 1 D
EPAJ54O/P-9 1/002
January 1991
User’s Guide to the Contract Laboratory
Program
Office of Emergency ana Remedial Response
U.S. Environmental Protection Agency
Washington, DC 20460
P r e :r , ec ’c ’c
-------
Additional copes of this document can be obtained
from:
USEPA Sample Management Office
P.O. Box 818
, Jexandria, VA 22313
NOTICE: The policies and procedures set forth here
are intended as guidance to Agency and other
government employees. They do not constitute
rulemaking by the Agency, and may not be relied on
to create a substantive or procedural right enforceable
by any other person. The Government may take
action that is at variance with the policies and
procedures in this manual.
ii
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TABLE OF CONTENTS
FOREWORD ... vii
C}LA .P1 . I .. .. .. 1
A. CL? Objective and Orientation ... I
B. CLPStructure i
CHAY ERU . .. ..... .. -... --..——..__.--.- -
A. Organic Routine Analytical Services ......... .8
B. Inorganic Routine Analytical Services_.. .8
C. Dioxin/Furan Routine Analytical Services .8
D. Spedal Analytical Services . ._. .3
E. Analytical Methodology Improvement/Development 18
CHAPTER III ___......... . • . .. .. .19
A. Analysis Request Procedures...... — 19
B. Regional Organic/Inorganic Allocation System .23
C. Sample Documentation
D. Sample Packaging and ShipmenL....... . .25
E. Procedures forProblem Resolution .26
CH.APTER IV.......... ........ .. .._. ._ ...
A. Shipment Management Program .... .23
B. Information Services .. .. .23
C. Enforcement Support ..... ....._
D. Cost Recovery Substantiation ....... — .31
E. Contract Compliance Screening (CCS)._ .31
F. Data Review SeMces .31
CHAF V............. ...... .... ........_. .33
A. Laboratory Selection Process .33
B. Liboratory Startup Process .34
C. Laborato rv PerfOrmanc2 Evaluation..
111
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CHAPTER VI 36
A. Laboratory Quality Control Criteria
B. Analytical Data Review 39
C. Laboratory Evaluation Samples 40
D. GC/MSTapeAudits 41
E. On—Site Laboratory Evaluations 41
F. Quality Assurance and Data Trend Analysis 4.2
G. Data Management
APPENDLXA _. ... ..
APPENDIX B --.. 47
National Program Office 47
Sample Management Office 49
LTSEI’ARegio n l 50
USEPAR.egio li 51
USEPA Region LU 52
USEPA Region IV
USEPARegionV
USEPA Region VI _55
USEPA Region VU
USEPA Region ‘JU l .57
USEPA Region IX
USEPARegionX
Miscellaneous Information
Regional Sample Control Centers _... 61
Regional Technical Project Offic rs
APPENDIX C ..
Aria lvtical References
Quality Assurance References
Safety References
Samplinz Ref erer.ces
Sh.ipoing Refer nc s
IYDEX
iv
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LIST OF FIGURES
Figure 1. Relationship of CL? Principals . .2
Figure 2. Relationship of Other CL? Offices . .2
Figure 3. Routine Analytical Services 6
Figure 4. Special Analytical Services 7
Figure 5. Organic Routine Analytical Services, Multi-Media, Multi-Concentration 9
Figure 6. Organic Routine Analytical Services, Low Concentration Water 10
Figure 7. Organic Routine Analytical Services, Low Concentration Water - Volatiles Only... .11
Figure 8. Organic Routine Analytical Services, Multi-Media, High Concentration 12
Figure 9. Inorganic Routine Analytical Services, Multi-Media, Multi-Concentration 13
Figure 10. Inorganic Routine Analytical Services, Low Concentration Water 14
Figure 11. Inorganic Routine Analytical Services, Multi-Media, High Concentration 15
Figure 12. Dioxin/Furan Routine Analytical Services .. 16
Figure 13. RAS Analysis Request Procedures - User Information Required .20
Figure 13. SAS Analysis Request Procedures - User Information Required... .21
Figure 15. Sample Tag .24
Figure 16. Additional CU’ Enforcement Support.. .30
Figure 17. Cost Recovery Substantiation 17
Figure 18. Data Review Services is
Figure 19. The CL? Laboratory Selection Process 33
V
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vi
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FOREWORD
This document has been prepared by the Contract Laboratory Program (CLP) Sample Management
Office (SMO) spe fica1iy for the guidance and direction of program clients. The CLP User’s Guide is
designed to darify procedures for CLP analysis. The CL? User’s Guide acts as a reference for the
Regions and laboratory contractors to promote consistency in procedures throughout the Regions and
ensure the proper adherence to CL? requirements. This document along with the CU’ Sampler’s Guide
provides a thorough overview of the CL?.
Fifth Printing
Issued: January1991
vii
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CHAPTER I
BACKGROUND AND INTRODUCTION
A. CL? Objective and Orientation
The Contract Laboratory Program (CLP) is
made up of contractor Iaboratoiies and supports
the Environmental Protection Agency’s (EPA)
Superfund effort. It was begun under the 1980
Comprehensive Environmental Response,
Compensation, and Uabi.lity Act (CERCLA) and
continues under the 1986 Supei-fund Amendments
and Reauthorization Act (SARA). The CLP
provides a range of state—of—the—art chemical
analytical services of known quality on a high
volume, cost effective basis. The CL? is structured
to provide legally defensible analytical results
for use in supporting Agency enforcement actions.
The CL? can also meet other req iirements of the
user community. Quality assurance procedures and
documentation designed for the intended purposes
of the data are part of all program activities.
Client orientation is a key factor in the design
and application of all CU’ services and responses.
Tne CL? supplies analytical services in direct
response to requests from the EPA Regions, the
primary users of the progrant States and other
Agency programs are also part of the CL? user
community.
The CL? objective is to develop, manage and
improve its analytical programs in support of all
Superfund requirements. This is accomplished by
increasing analytical capacity and improving
analytical program requirements and related
support services.
B. CL? Sftuct-uxe
CL? services involve numerous Agency
pro r ms, ccn actors and other grouDs throughout
the country. These organizations are identified
and their role in the program described in the
foUowing sections. Figures 1 and 2, “Relationship
of CL? Prindpals,” and “Relationship of Other
CLP Offices,” illustrate the interaction of these
groups in CU’ operation. In addition, a directory
listing addresses and telephone numbers of key
program personnel is located in Appendix B.
1. Clients/Users
a. EPA Regions
The ten EPA Regions are the primary clients
of the CL?. Each Region has established a
Regional Sample Control Center (RSCC) that
sci ules all Regional G P analysis requests. The
RSCC balances Regional sampling with allocated
numbers of CL? sample analyses available each
month and prioritizes the Region’s analytical
workload when conflicts occur. RSCC personnel
coordinate closely with the Sample Management
Office (SMO) throughout Regional sampling
events, assisting in tracking sample shipments to
the laboratory and resolving arty problems that
arise. The RSCC also processes analytical
requests from state or other program users that are
located in the Region’s geographical area.
b. States
Any state undertaking initial site
investigations and entering into cooperative
agreements [ under the Resourte Conservation and
Recovery Act (RCRA)- CERCLA Cooperative
Agreements] with the Government for dean up of
local waste sites can use CL? services. States must
access CU’ analytical services through the RSCC.
Data packages are also distributed to states
through the RSCC.
c. Non—Superfluid Clie s
Program services are available to support
Non-Superfund clients. Non—Superfund analyses
and other support are provided by the CLI’
through transfer of funds from the Non—Superfurid
program. Non- Superfund clients currently include
other government agerices and EPA programs,
such as the Office of Acid Deposition, the Office
of Solid Waste, the Office of Water, and RCRA.
In this chapter...
CLP Objective and Orientation
CLP Structure
ClientsiUsers
Regional Program Support
Analytical and Support SeMces
Contractors
1
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CLP User’s Guide
FIGURE 1. RELATIONSHIP OF CLP PRINCIPALS
ap CI. aIVwI
FIGURE 2. REM 77ONSHIP OF 077-/ER CLP OFFICES
Rapcrt
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Chaptcr I — Background and Introduci-ion
2. Program Management
a. National Program Office
The CLI’ is directed by the National Program
Office (Nl’O). in EPA Headquarters Analytical
Operations Branch (AOB), Hazardous Site
Evaluation Division (HSED), Office of Solid
Waste and Emergency Response (OSWERL
located in Washington, DC. The NPO is
comprised of the AOB Branch Chief and Deputy
Branch Chief, the Analytical Methods
Implementation Section (A.MIS) Chief who also
serves as the National Program Manager, the
National Organics Program Manager and
National Inorganics Program Manager, the
Regional Operations Section Chief, the Quality
Assurance Coordinator, the Data Integrity
Specialist, the SMO Project Officer, and the ADP
Officer.
NPO responsibilities indude-
• overall management of the CL? in terms of
program objectives;
• expansion and interface with clients and
other groups;
• policy and budget formation and
implementation;
• development and administration of CL?
analytical and support services contracts;
• development and technical review of
analytical protocols;
• review of Special Analytical Services
subcontracts;
• review of CLP—generated laboratory data;
• monitoring and formal evaluation of
analytical and support contractors; and
• direction of CLP quality assurance in
coordination with overall OSWER
quality assurance activities.
The National Program Manager (NPM)
assisted by the National Organics and Inorganics
Program Managers, in addition to directing the
AMIS section staff, is responsible for the
formulation of CL? policies and direction. By
communicating with Regional and Agency
communities on a continuing basis, the NPM keeps
all parties apprised of program activities and
receives input on program effectiveness. The NPM
and Organics and Jnorganics Project Managers also
directs annual technical caucuses for the purpose
of re ortin initiatives and progress of the past
year. AMIS is also responsible for development of
sample bottle specifications and data review
guidelines for all analytical services.
The Regional Operations Chief directs a staff
responsible for the Sample Management Office
contract, the Environmental Services Assistance
Teams contracts, and the Shipment Management
contract. In addition, the Regional Operations
Section tracks the supply and demand between
CL? capacity and client needs, and provides
budget support and administration. (Note AMIS
manages this using information from ROS.)
The Quality Assurance Coordinator manages
all aspects of program quality assurance needed to
provide information to the Branch Chief and
Section Chiefs to determine if management’s QA
expectations/needs are being met. The QA
Coordinator works closely with the Office of
Research and Development’s Environmental
Monitoring Systems Laboratory in Las Vegas
(OR]) EMSL/LV) in administering and improving
the QA program. The QA Coordinator interacts
with the APOs in refining and updating
analytical method QA. The QA Coordinator also
communicates with the Regions and other program
users to resolve QA issues related to anaiytical
data. For purposes of QA procedures review and
guidance development, the QA coordinator
conducts volunteer workgroups throughout the
year.
The APOs are responsible for administrative
and technical program decisions, contract
monitoring and contractor performance evaluation.
On a daily basis, the APOs work closely with the
Regional Technical Project Officers and contract
laboratories to resolve technical issues. Tr Al’Os
also direct the continuing effort to improve
contract language and to develop analytical
methodologies. For the purposes of CL? protocol
review, method development, and QC criteria
development, the Ai’Os conduct volunteer
workgroups throughcut the year.
The Data Integrity Specialist is responsible
for implementing Good Automated Laboratory
Practices into analytical services, developing
poli to protect the Government from alleged
fraud in the laboratory community, and heading
projects-/workgroups focussing on the integrity of
Superfund analytical data.
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CLP Users Guide
b Sample Management Office
The contractor—operated SMO provides
management, operations and administrative
support to the CL?. The primary objective of SMO
is to maintain optimal use of program analytical
resources. SMO activities fall into the following
areas:
• sample scheduling and tracking
• Contract Compliance Screening;
• Special Analytical Services
subcontracting;
• laboratory invoice processing;
• maintenance of CU’ records and
management reporting;
• procurerrcnt/IFB support and statement of
work production;
• coordinating CLP meetings and
conferences; and
• NPO management, technical, and
administrative support.
SMO routinety receives Regional analytical
requests, coordinates and schedules sample
analyses, tracks sample shipment and analyses,
receives and checks data for completeness and
compliance, processes laboratory invoices, and
maintains a repository of sampling records and
program data. In response to client requests for
specialized analyses, SMO sub.contracts for
Special Analytical Services (SAS), scheduling
and tracking for SAS efforts as outlined above.
SMO maintains a comprehensive database of CL?
services, performance and utili ation in order to
generate a variety of management and user
reports.
c. Office of R swch and Dc dopmenf,
Environmental Monitoring Systems
Laboratorg/L.as Vegas (EMSL/LV)
ORD provides program QA support through
EMSL/LV. EMSL/LV assists in the following
functions:
• performing preaward and postaward on—
site laboratory evaluations;
• preparing performance evaluation (PE)
samples for preaward and postaward
laboratoriperforrnance evaluations;
• evaluating preaward and postaward PE
sample data;
• performing QA audits on CLP-genera ted
data induding mass spectrometer data
tapes; and
• assisting in the evaluation and
development of CL? analytical methods
and protocols.
EMSL/LV also operates the program’s QA
database to conduct program and laboratory trend
analyses used in developing and updating contract
quality control criteria.
d. National Enforcement Inv ffgations Center
The National Enforcement Investigations
Center (NEIC) advises the NPO in defining and
applying program enforcement requirements.
NEIC-developed sample custody procedures,
chain—of—custody records, sample tags, and
custody seals are used to maintain the integrity of
sample analyses for supporting Agency
enforcement actions. NEIC routinely perform.s
evidence audits of contract Laboratories and
generates sample profiles used in Agency
enforcement litigation. A description of the
enforcement support provided by NEIC appears in
Chapter IV, Section D.
3. Regional Program Supp t
The Regions play an integral role in prog
activities, both as the primary CL? user and a
key part of analytical program management. The
decentralization of program responsibilities to
the Regions is an effective means of directing
program operations nationwide. Extended
Regional participation in the program has and
will continue to increase the program’s
responsiveness to Superfund meqi±en ts.
a. Regional Technical Prøjert Officers
In 1984, Regional Administrators appointed a
CLI ’ Technical Project Officer (TPO) for each
Regional office. Under the guidance of the NPO,
the Regional TPO monitors the contract
laboratories located in the Region. The TPO
works closely with the APO in responding to
identified problems lit laboratory operations and
participating in on-site evaluations. The TPO is
the first line of contact for the laboratory for all
technical problem resolution and only rever 3
technical prcblems to the NPO that appear tc
have program implications.
4
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Chapki I — Background and Introduction
b. ReSior a1 Sarnp(e Control Centers (RSCC)
In 1984. each Region established an RSCC to
centralize scheduling of CL? sample analyses
within the Region. The RSCC is comprised of one
or more individuals. One individual is named as
the primary RSCC. The RSCC is responsible for
coordinating the level of Regional sampling
activities to correspond with the monthly
projected demand for analytical services. When
conflicts occur, the primary RSCC makes the final
determination of Regional analysis priorities.
The RSCC routinely places all Regional requests
for CL? analyses, coordinates with SMO during
sampling and sample shipment, and resolves any
problems concerning the samples. The RSCC also
serves as the central point of contact for questions
concerning Regional sampling efforts.
c. Regional/L.a boratory Conirnunic.ation System
In 1983, the NPO established a system by
which the Regions and contract laboratories can
communicate in the most timely and direct manner
possible. Regional communication contacts
routinely call laboratory communication contacts
to resolve technical questions conceming program
data. This communication link also bendits the
laboratory by providing direct feedback on its
data product.
4. Analytical and Support Services Contractors
a. Analytical Contract Laboratories
The CLP’s analysis contractors come from the
nationwide community of chemical analytical
laboratory facilities. To become part of the CL?,
laboratories must meet stringent requirements and
standards for equipment, personnel, laboratory
practices, and analytical and quality control
operations. Firm, fixed—price contracts are
awarded to the lowest responsive, responsible
bidders through the Government’s Invitation for
Bid (IFB) process. Before a contract Is awarded,
low priced bidders must successfully analyze
performance evaluation samples and pass a
preaward laboratory audit. After contract award,
laboratories are closely monitored to ensure
compliance with the terms and conditions of the
contract. Details of preaward and postaward
evaluations are addressed in Chapt V.
b. Shipment Management Program
The Sbipm nt Management program was
a-eated by the NPO in 1988 to provide a consistent
means of tracking the various shipping accounts
established for CL? use. The Shipment
Management contractor establishes, maintains
and monitors the shipping accounts for the
transportation of sample containers, sample
coolers, contract compliance screening results and
other items requested by the NPO. Further
information on the Shipment Management
program is provided in Q apter IV, Section B.
D
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CHAPTER II
DESCRIPTION OF ANALYTICAL SERVICES
The CL? provides routine and specialized
analytical serviees to support a variety of
Superfund sampling activities. These activities
range from those associated with the smallest
preliminary site investigation to those of large
scale, complex remedial, monitoring and
enforcement actions. In response to the inc easing
analytical demands of Regional dients, the CL?
has continually expanded its capacity for
standardized analyses through frequent contract
solicitations. On the average, the CL? provides
over 6,000 sampe analyses per month through its
routine and specialized analytical services
programs. The CLP will continue to adjust
analytical capabilities and capacity in response
to client needs.
The CU’ operates the following analytical
FIGURE 3. ROUTiNE AJVALYflCAL SERVICES
F ofs
programs:
• Organic Routine Anaiytcal Services
(RAS),
• Inorganic RAS,
• High Concentration Organics
• High Concentration Inorganics
• Organics Low Concentration (Drinking
Water)
• Inorganics Low Concentration (Drinking
Water)
• Volatile Organi Low Concentr -ation
(Drinking Water)
• Dio,dns/Furans
• Special Analytical Sex-vices (S AS).
In the future, many other analytical programs
will be induded under RAS:
• Fast Turnaround CC Saeen Organics
• Air Toxics
• Ceo technical
• Water and Soil Cnaracterization
• Mixed Waste
Laboratories operating under firm, fixed-price
contracts with the EPA provide Routine
Analytical Services to Superfund clients. Non—
Superfund thents can also access RAS programs
once special funding arrangements have been
made.
Figure 3 summarizes RAS services. For
detailed analytical information, users are
inst-x-ucted to consult the Region’s Master Copy
In this chapter
Organic Routine Analytical Services
Inorgar c Routine MalyticaJ Services
Dioxin/Furan Rouline Analytical Services
Spedal Anatytical Services
RAS Plus SAS
All SAS
Contract De very and Quahty Control
Requirements
Analytical Methodology lmprovementl
Development
Protocol Standardization and Improvement
Method Development
•
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6
-------
Chapter II — D crip!ion of AMIytical Scruic
Statements of Work under which CLI ’ RAS
laboratory contractors operate.
Routine Analytical Services apply to the
analysis of water and soil/sediment samples.
Samples for analysis should be single—phase and
homogeneous with the exception of high
concentration analysis which may be multi—
phase. Sample matrices other than water or
soil/sediment are processed through the SAS
program.
Organic and inorganic low and medium
concentration RAS contract methods are used to
analyze low to medium sample concentrations for
organic target compounds and inorganic target
an.alytes, respectively. The sampler identifies
low and medium levels of concentration in the
field to determine sample collection volume arid
packaging and shipment procedures. Low level
samples are considered to be those collected off-
site in areas where hazards are thought to be
significantly reduced by normal environmental
processes. Medium level samples, where a
compound or eleneit may comprise as much as
fifteen percent of the total sample, are most often
those collected on—site in areas of moderate
dilution by normal environmental processes. The
contract laboratory performs preliminary
characterizations to determine the appropriate
analytical protocol (low or medium) to be used.
Organic high concentration RAS contract
methods are used to analyze high concentration
samples for organic target compounds. High
concentration santp es are considered to be those
collected directly from drums, pita, ponds, lagoons
or areas where no dilution of waste is evident.
Required sample volume and container types
used for sample collection for RAS analyses are
detailed in the CLP Sampler’s Guide. Contractors
should acquire sample bottles which meet EPA
quality assurance standards. These containers
may also be utilized in SAS projects as
appropriate.
Contract delivery requirements for each RAS
program are specified in the following sections.
The contract laboratory is required to deliver all
analytical results and quality control (QC) data
for each Sample Delivery Group (SDG) in one
data package. An’SDG is defined by one of the
following. whicheve? occurs first:
each case of field samples; or
• each twenty field samples within a case;
or
• each fourteen calendar day (seven days
for low concentration inorganic) period
during which field samples in a Case are
received, beginning with the receipt of
the first sample in the SDG.
Laboratories are subject to liquidated damages
for late delivery and incentives for early delivery
of the data package.
The SAS program provides specialized
analytical services to Superfund and Non-
Superfund clients for organica, inorgarücs, dioxin
arid other compounds in a variety of matrices.
SAS services are offered to meet specific
analytical requirements which do not fall under
RAS programs and are solicited through
individual fixed-price subcontracts awarded to
qualified laboratories.
Figure 4 outlines the services available under
the CLP’s SAS programs. The client should
carefully consider the provisions of each CU’
analytical program during the planning stages of
a sampling event to determine the applicability
of theanalysis touserneeds.
FIGURE 4. SPECIAL ANAL YflCAL SERVICES
NOTE: The client is responsible for
designating [ FB method adjusthients for “RAS Plus
SAS’ requests and for supplying suitable
analytical protocols for “All SAS requests.
Additionally, the client must provide quality
assurance/quality control procedures and criteria,
and must specify data delivery schedules. AU
information must accompany the client’s request
for SAS services.
The CLP QC program for F..AS laboratory
analysis is structured to provide consistent resul
of known arid documented gualit: Sample dat. :
packages contain QC documenta on that allow
ex enenced chemist to determir.e t e cualitv
PA3 - SA$ —
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I
-------
CLP Uscr’s Guide
the data and its applicability to each sampling
activity. In addition, laboratory contracts contain
provisions for sample reanalysis if specified QC
criteria are not met by the contract laboratory.
Each CL? laboratory is also encouraged to develop
additional internal QA/QC procedures.
The minimum QC requirements of the RAS
programs consist of both an initial and ongoing
demonstration of laboratory capability to
generate acceptable -performance with the
contract methods. The contract laboratory must
demonstrate that instrument calibration criteria
have been met, that interferences from the
analytical system are under control, and that
spike and duplicate recoveries failing outside
contract acceptance windows are attributable to
sample matrix interferences and not to laboratory
analytical errors. The QC requirements for each
RAS program are provided in the following
sections.
A. Organic Routine Analytical Ser,ices
Organic Routine Analytical Services are
comprised of four analytical contracts which
allow the analysis of different media and
concentr ons. Figures 5-8 detail each of these
four analytical contracts.
B. Inorganic Routine A nalytica1
Services
Inorganic Routine Analytical Services are
comprised of three analytical contracts which
allow the analysis of different media and
concentrations. Figures 9-11 detail each of these
three analytical contacts.
C DioxinlFuzan Routine Analytical
Services
Dioxin/Furan Routine Analytical Services are
detailed in Figure 12.
D. Special Analytical Services
In addition to the standardized analyses
available under the RAS program, SMO provides
Regional clients with specialized analyses under
the SAS program. While these analytical
services are beyond the scope of RAS contract
protocols, they are consistent wtth CL? objectives.
Services provided through the SAS program
include fast turnaround analyses, verification
analyses, analyses requiring lower detection
limits than RAS methods provide, identification
and quantification of non—TCL constituents,
general waste characterizations, analysis of
nonstandard matrices and other specific analyses.
As part of the SMO contract with EPA, Viar
and Company solicits, awards and administers
SAS subcontracts. By utilizing subcontracts, SMO
can procure specialized services in a timely
manner on an as—needed basis. Due to the often
unusual nature of SAS requests, users must plan
their projects in advance to allow SMO sufficient
time to procure these services.
For each SAS request, the client provides
SMO with the necessary analytical methods,
QA/QC requirements and acceptance criteria in
writing. SMO procures SAS by subcontracting
with laboratories with RAS contracts in the
appropriate analytical program.. When RAS
laboratories cannot meet the analytical
requirement of the SAS, requests are solicited to
other laboratories which have Indicated the
ability to meet program performance
requirements. R.AS contract laboratories are
evaluated for current RAS performance before
they are considered for SAS solicitations, and are
not solicited for SAS work if deficient in this
area. Other laboratories qualify to perform
certain types of SAS work by successfully
completing performance evaluation sample
analyses or by justification of unique analytical
capability.
Once the laboratory community is determined,
SMO provides the community with the particular
requirements of the SAS. Laboratories are asked
to bid firm, fixed-price(s) for the performance of
specific types of analyses on a defined number of
samples.
A laboratory’s ability to bid for SAS work and
the prices being bid may vary depending on the
size or scope of the analytical request, data
turnaround requirements and analytical
parameters of a particular task, weekly RAS
sample loading, and laboratory operating
conditions at the time of solicitation. SMO
evaluates laboratory bids in terms of bid price and
responsiveness to the specified task. The SAS is
awarded to the lowest bidding laboratory which
responds to the dient’s analytical requirement. A
written, individual SAS subcontract agreement is
then made between the laboratory and Viar.
8
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Chapter Ii — Description of Analytical Ser iccs
FIGURE 5. ORGANIC ROUT/NE ANALYTICAL SERVICES, MULTI-MEDIA, MULTI-
CONCENTRATION
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CLP Users Guide
FIGURE 6. ORGN’JIC ROUTINE ANALYTICAL SERVICES, LOW CONCENTRATION WATER
OW Reia
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•10
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Chapter II — Description of AnalyHcal Services
FIGURE 7. ORGANIC ROUT/NE ANALYTICAL SERVICES, LOW CONCENTRATION WATER -
VOLA TILES ONLY
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i i
-------
CL? Users Guide
FIGURE 8. ORGANIC ROUTINE ANALY77CAL SERVICES, MULTi-MEDIA, HIGH CONCENTRATION
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12
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Chapter II - D cription of Analytical Seruic
FIGURE 9. INORGANiC ROUTINE ANAL Y71CAL SERWCES, MUL Ti. ‘ 4EDIA, MUL 17-
CONCENTRA TION
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13
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CLP LIser s Guide
FIGURE 10. INORGANIC ROUTiNE 41./ALYTICAL SERVICES. LOW CONCENTRATION WATER
SOW Rcjcc
ot Work
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Do Numb 11.0)1.0
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withec 7 divi of
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& L wihij 7 dayi of wiic
byAPO
14
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Clthpfcr 11 — D criptior of Analytical Ser ’ic
FIGURE 11. INORGANIC ROUTINE ANAL YI7CA! SERVICES, MULTI-MEDIA. HiGH
CONCENTRATION
SOW Rda’ ,cc
SuL L cl Woit (oi 1nol gEuc AnaAy iz
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by APO
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with x bid F a k r uhi.
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• An .aiyncal Spike S Ie Analyits (A).
-
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• M bod Dø L e ( (DL) D z .ai ee
• 1nx eJ t foi 10’ (10’).
• Hy&idc 10’ (HYI0’) QC A uJyits
15
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CLP User’s Guide
FIGURE 12. D1OXINJFURAN ROUTINE ANALYTICAL SERVICES
SOW Rda
5z n ci Woit fix Muiyui of Po ych1om i D p-DiO (PCDD) Pyc Jutn a1
D m6r ii (P F) Muh-Mcdia. MuuCon
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• Total t cd D .ii
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• 17 Epca& Z3.7,S-a th e4 PcDDiiP Fs
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•
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.
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45 days il a ruxql ci iaç c ii SDG
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R fix 365 days d i iuicc
ix z w 7 days ta ‘s
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D ipc1oe
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Fth d P S i 1e t UhL
SOPS tu y of
opa
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aa! pk d a a evth xxio(
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• baQM C( s e e SOW)
16
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Chapter II — D cription of Analytical Servic
SAS requests are separated into two basic
categones, “RAS Plus SAS” and “All SAS’. These
categories are utilized in defining client requests
and pursuant SAS solicitation and contract award.
Analytical services available through the SAS
program are desmbed below.
1. RASP1usSAS
a. Fast Turnaround
Fast turnaround requests require the
application of existing RAS analytical
parameters, methodologies and detection limits
with a shorter time(rame for performance of
analysis and/or delivery of data. Procurement for
fast turnaround SAS is dependent upon program
sample load, laboratory capacities and
laboratcry operating conditions at the time of the
request. Because of constant fluctuations of these
factors, it may not be possible to obtain fast
turnaround service on an unlimited basis. Fast
turnaround contracts are solicited only in
situations of demonstrated need and are used
primarily to support EPA emergency actions and to
meet impending litigation deadlines.
The following illustrates common “RAS Plus
SAS” fast turnaround requests. The SAS portion is
underlined:
• RAS organic target compound analysis
with data delivery in seven days .
• RAS inorganic target compound analysis
with data delivery in fourteen days .
b. Special RLquiranents in Addition to RAS
A client may need to access the standardized
RAS programs and add to the contract
requirements. The following examples illustrate
common ‘RAS Plus SAS” requests. The SA5
portion is underlined:
(1) Organic
• Orga.nics RAS TCL analysis with
additional non—target compounds .
• Pesticide target compound analysis
minor alterations or additional orocedures
(2)
applied .
Inorganic
Me ais and cyanide analyses with sr.ecial
ngr rous samole ho eriizahon
• Metals analysis at lower detection limits
than required by the RAS reqi.iirerrents .
RAS metals and cyanide analysis with
minor alterations or additional
analytical prç edure, applied .
(3) High Concentration Organic
• RAS High Concentration Analyses
• RAS analysis at lower detection limits
than required by the High Concentration
protocol .
2. AI1SAS
CLP dients frequently request types of
analyses that are not directly applicable to the
RAS program. These requests occur most often
with samples of difficult or unusual matrices and
measurements of analytical parameters not
provided through the RAS program. The SAS
program accommodates unusual analytical
requests on an A11 SAS basis. Complete
methodology and QA/QC specifications must
accompany the request. These types of analyses
indude, but are not limited to, the following:
• Volatile target compound analysis
lpw detection limits than required by
the ff3 .
• Seven TCL Aroclors analysis only (i.e., n
the entire ff3 pesticide fraction).
• Non-target compound analyses.
• RAS compound /analyte analysis by non—
RAS methods .
• Specified RAS elen ttal analysis only
(e,g., dmium, rr cuxy and selenium).
• Metals analysis by rion-RAS methods .
• Air samples (e.g., tena*, charcoal and
florisil tubes) for specific organic
analyses.
• Methods comparison/evaluation studies.
• Asbestos analysis.
• Acid deposition parameters.
• Non—Superfund analytical services of any
type.
• Geotechnical/Geophystcal tests on soil
samples.
• Radioactivity analyses.
• Leaching procedures (TCLP, EFTOX).
• Wet cherriistrv procedures.
• Physical tests.
requir rnents .
17
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CLP User’s Guide
• Bioassays.
• RCRA parameters.
• “Explosives” Analyses.
• Othersasdefinedbydient.
3. Contrad Delivery and Quality Control
Requ lreinent3
SAS contracts require delivery schedules for
sample extraction, analysis and data reporting,
and require laboratory QC procedures and
reporting of QC parameters as defined by the
client requestor. Delivezy and QC requirements as
detailed in RAS program contracts may be used as
a guide but must be specified by the client at the
time of request. The requestor must specify all
deliverables required to ensure that the
appropriate data packages are received. aients
are encouraged to maintain a high level of QC in
all analysis requests, unless there is substantial
reason for deleting certain QC requirements.
E Analytical Methodology
Improvement/Development
1. Protocol Standardization and Improvement
In order to maintain state—of—the---art
protocols and accommodate newly defined or
changed requirements of the Superfund dfort, CU’
participants are constantly refining and
improving analytical protocols. To accomplish
this, program participants submit comments and
suggestions to the NPO. The NPO reviews all
submitted information and considers
recommendations for program modification on a
periodic basis.
Since 1982, the NPO has planned technical
meetings to utilize all available resources in
updating analytical program methodologies and
data reporting requirements. Technical meetings -
such as workgroups, and caucuses — are initiated by
the NPO on a periodic basis. Participants include
the Regions, NPO, EMSL/ LV, EMSL/Cincinnati,
NEIC, SMO, contract laboratories, program
support contractors, other EPA programs, and
other government agencies, as appropriate. These
meetings are instrumental in improving CL?
protocols and ensuring that deliverables meet user
needs.
EPA personnel review the discussions of the
technical meetings and compile recommendations
for protocol changes. Following NPO approval of
recommended changes, existing laboratory
contracts are modified by the Contracting Officer
to include the recommended revisions. Whenever
possible, all laboratory contracts within an
analytical program are changed simultaneously to
maintain consistency within the prograxm NPO-
approved protocol revisions are included in any
new IFB solicitations.
2. Method Development
Developrx t of new analytical methods may
be initiated by a newly identified or redefined
Agency analysis requirement. Analytical
methods utilized in the CL? are based on
methodologies developed and approved by EPA.
The NPO, EMSL/LV, the Regions, and the
contractor community have historically
contributed to the development of new program
analytical methodologies. Methods are reviewed
by several sources and are tested prior to
implementation to the extent possible to meet
program requirements.
18
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Chapter III — Utilization of Analytxcal Scrvic
CHAPTER III
UTILIZATION OF ANALYTICAL SERVICES
The CL? provides dients with prompt access
to laboratory services through a documented
system of sample scheduling and tracking.
Individuals interested in obtaining CLP
analytical support must contact their Regional
EPA office’s RSCC. SMO coordinates the
scheduling of sample analyses through the Cl P
and tracks the progress of samples from collection
through final data production.
The RSCC is established by the EPA Regional
Administrator and is centered in each Region’s
Environmental Services Division or Waste
Management Division (see Appendix B). The
RSCC, consisting of one or more individuals,
places analytical requests. SMO is authorized to
accept analytical requests only through the
P.5CC. In addition, the RSCC is responsible for
ensuring Regional compliance with the CLP’s
projection/allocation system. The primary RSCC
determines analytical priorities for the Region
when conl1ic s occur.
SMO seeks to effectively match the
analytical needs of program clients with the
capabilities of contract laboratories. To this end,
SMO tracks current utilization, availability of
resources and laboratory performance limitations
for each program.
The success of the CL? scheduling process
depends on two factors:
• ongoing commL lnication anutg the P. 5CC,
field sampler, SMO and laboratory
personne and
• correct use of sample scheduling and
tracking documents by the P.5CC, field
sampler and laboratory personnel.
A. Analysis Request Procedures
1. RAS Inithfion Process
a. User Information Required
To initiate a RAS request, the RSCC or
Regional designee contacts the appropriate SMO
Coordinator by telephone or fax and provides a
complete description of the analytical
requirement (SMO personnel are identified in
Appendix B.) The information SMO requires to
initiate a RAS request is listed in Hgure 13.
The P.5CC or designee is responsible for
estimating the number and types of samples and
the sample shipment dates for the analytical
request. Overestimation of the number of samples
to be collected or miscalculation of shipment dates
unnecessarily ties up available laboratory
capacity and lessens program responsiveness.
Underestimation of the number and types of
samples to be collected may result in unavailable
services for any additional analyses needed.
b. Lead—time Required
By noon EST on the Wednesday of the week
prior to the scheduled start of a planned sampling
activity, the P.5CC or designee contacts SMO to
place a request for RAS services and to provide
scheduling informa on to SMO. Allowing this
lead—time makes laboratory scheduling and
resolution of sampling questions easier. It also
In this chapter
Analysis Request Procedures
RAS Initiation Process
SAS Initiation Process
Procedures for Making Changes to
Analytical Requests
Regional Organic/Inorganic Allocation
System
Sample Documentation
Sample Traffic Report
SAS Packing List
Sample Number
Sample Tag
Chain-ct-Custody Record
Sample Packaging and Shipment
Packaging Requirements
Shipping Instructions
Shipment Coordination
Procedures for Problem Resolution
Resolving Problems Concerning Sample
Shipment and Analysis
Resolving Problems Concerning Analytical
Data
19
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CLP Users Guide
allows the sampler time to prepare the required
sample documentation prior to field activity, if
appropriate. Advance scheduling is available
and should be utilized whenever necessary. Late
scheduling requests (i.e., requests received
between Wednesday noon and Friday) are
accommodated with laboratory capacity
availability. To avoid possible shortfalls,
Regions are strongly encouraged to submit all RAS
scheduling requests by Wednesday noon, where
possible.
FIGURE 13. RAS ANALYSIS REQUEST
PROCEDURES - USER INFORMA17ON
REQUIRED
c. Case Number Assig7nne t an.d L2bora forg
Scheduling
At the time of request, SMO assigns a
sequential Case number to each RAS sampling
activity for identification throughout sample
tracking and data production. A Case number
designates a group of samples collected at one site
or geographical location during a predetermined
and finite time period. The RSCC records the
Case nuinbe and uses it in re erendng that request
throughout sampling and analysis.
SMO then schedules the requested analyses
through an appropriate RAS laborator
Laboratory selection is determined by
• the types of analyses,
• numberof samples,
• contract capacity,
• sample balance among the various
laboratories, and
• laboratory loading and instrument
conditions.
Laboratory selection is also based on the
Regional Distribution of Laboratories System
developed by the NPO and desigi d to minimize
the number of laboratories produth g data for any
one Region. When possible, the nearest available
laboratory is assigned in order to minimize sample
shipping costs.
Once RAS Laboratory assignmen are made,
SMOcontacta theRSCCordesigneetoconfirmthe
field investigation plans, Identify the
laboratories to be used for the Case, and answer
any further questions regarding program
procedures or documentation. At that point, the
RSCC or designee must indicate all known or
anticipated sample scheduling changes. Any
further changes should be communicated to SM
immediately upon identification to ensure I
timely resolution of conflicts and the optini
allocation of program resources. After the initial
placement of the RAS request, the RSCC or
designee may assign a logistical contact, such as
the team leader in the sampling effort, to
coordinate with SMO in finalizing sampling
requirements, and initiating and arranging sam.ole
shipment.
d. User Knowledge of An ytic .2 1 Protocol
Each RSCC is responsible for gaining and
maintaining a working knowledge of current RAS
protocols and analy cal services. SMO prov des
each Regional TPO (listed in Appendix B) with
Master Copy notebooks of each RAS program [ FB
Statement of Work (SOW). The Master Copy
notebooks are periodically updated to re iet
program protocol changes.
The SOW represents the standard d
requirements that each individual RAS
laboratory is contractually bound to follow The
analytical SOWs contain steci c informa or. cn
Nam jidu,J .o d at.d - -
Naa e(a3,ai.od .i lekp n. Uuaiba< UI n tfr pcr nd.
NIDW. y aM UI 1W W b
SuprluM IWI J1 to a dIGIt a!ph u 4c coda).
Nu b.u aM 1xoI nt$ i W ba
Ty oIaMyi ib.d.
• 8 i tic Vc1*t i ,a (VOAg). • Lo Coc - o Watrr or
S ti,oL j GV ), O! 5aA c Coc pouM VOA.
P ddas/Modo, a. SV.P /Ag or..
• !r.crnzd Total Me .k . D oL, • Low Co on Watarfo
Mu . Cpalds. Lsior k Anaiy TouL MetaM.
• Hi4 yt & 1 Cy . Ta )‘flhro an. fluc .
Az /Toxiphe . • Low Wa fo
• JJja) Conc n Cr r nic VOA IT VOAL
M L CyatJd. p C thit-y. •
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• PpaL n,L,iajy A a I
•
• EdSiWIa i p oa •
• R LaJ • ____
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a pu.d ddaya du. b .ta w .dJ cnj. a.anjLLn 5 .ajwocoa t
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Ad
20
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Chapter III — Utilization of Analytical Servic .
• sample types suited to RAS analysis,
• compounds identified and quantified,
• analytical methods, protocols, detection
limits,
• deliverable requirement, and
• quality con ol requirements.
Program users should consult the appropriate
SOW to confirm that the RAS program is suited to
art analytical request.
2. SAS In.ithtion Process
a. User Information Requird
Analytical requirements differing from RAS
parameters are processed through the SAS
program as described in Chapter II, Section D.
Initiating a SAS request is a twc -part process.
• The RSCC or designee sends a copy of the
SAS client request, appropriate
attachments (if needed) and a copy
requested analytical method to SMO.
• The RSCC-or designee contacts the
appropriate 5M0 Regional Coordinator
by telephone and provides a complete
description of the analytical requirement.
The information SMO requires to initiate a
SAS request is listed in Figure 14.
FIGURE 14. SAS ANALYSIS REQUEST
PROCEDURES - USER INFORMATION
REQUIRED
Most SAS requests are made in writing using
the SAS client request form. In emergency
situations, the verbal request may be made prior
to a written request Following the verbal request,
the RSCC must submit a completed SAS Client
Request form to SMO. This form serves as the
wntten record to darify and confirm the dienrs
requirement for specialized analytical work.
The RSCC is responsible for estimating the
number and types of samples and the sample
shipment dates for the SAS request.
Overestimation of the number of samples to be
collected or miscalculation of shipment dates
unnecessarily ties up available laboratory
capacity lessening program responsiveness.
Underestimation of the number and types of
samples to be collected may result in unavailable
services for any additional analyses needed.
Depending on the size and extent of the
miscalculation, the entire request may have to be
resolidted and sampling plans postponed
accordingly. SAS solicitations result in binding
conhacts. If the contract has been awarded, it
may r t be possible to make changes.
b. Le .d—Lime Required
When a sampling activity has been planned,
the RSCC contacts SMO and places the specific
written request for SAS services. Because SAS
services are individually procured on a
competitive basis, a minimum lead-time of two
weeks, from receipt of the request, is required to
process a properly completed SAS request Three
to four weeks lead-time is sfrongly recommended
whenever possible. SAS solicitation will not be
started until the SAS requirements have been
completely defined by the RSCC. Modifications
to any SAS request wiU cause the entire process to
begin again. Fully defined requests initiated with
less than two weeks lead—time may not be
solid ted and awarded in time to meet the original
shipment date.
Certain types of SAS requests require a longer
lead-tune. A rninimuni lead-time of two to three
weeks is required for SAS requests which involve
distribution of protocols (see item d, below). A
minimum lead—time of four or more weeks is
recommended for large scale, analytically
complex or N on-Superfund SAS requests. Award
of Non—Superfund SAS subcontracts may only be
made after the apDroprlate funding process i
complete. The RSCC should contact SMO several
Na . 04 or t
}4eoiejj). 4 Ieiepi aw w Cs3 04 wid.
city arid a 0( bi
5i p fw u / e io a e t i %b-ftu iaX dt).
N thuazid %I 1X 04 ba
So c maJyu r u1M.ffwOpnA •OWZXl A AJ linu±i
Xh:rQlr.d de t:
M. ej &r. lx L3ic dev4iciir.. du04 tr or Lci & .ai y . U ip bk.
Da tu,woi ri4 a id d knmd.
f . r u if aDpIv r1aw.
5th uJ irçla 4J Oa Mid MLpm da
Nzozz, of mp L r’ tt
P I ,wy A t • 5 r L Sitr biv zboo
• Site - .
• E teI r i, a on • ? 4 a1Oioim5tz4y
• Rr Iid 1n paori/F siSJ1tv • F a i tyA . ..a t
Sb dy • Mooi Effort
• R !i ai •
• R iidW • Ct id Wa ?l4Utertri 5 T
• t! orce
• E m.6 y R oa ae ( viã3 • R ,c! Co on oM
• Na Png ,b L De w R Ad
• Opaibo &tidM&b •
• S t 04mruriaryAa t
Su,c ,d mn L wt with the sac pw Mid/or ate.
Othar Jor _ io wluth c af iu1u or I vaic t (Le_
an coa dd.ir due . wa iiar n.owt 5 e wpm u .
3 riwij) 04 Re o. a1 or -. r toc (or rw peob4 i r uno,i.
21
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CLP Users Guide
weeks in advance if there is a question regarding
the lead—time needed to schedule a particular
SAS request.
c. SAS Number Assignment and Laboratory
Scheduling
At the time of request, SMO assigns a
sequential SAS number to each SAS sampling
activity for identification throughout sample
tracking and data production. If SAS services are
being provided in association with RAS services,
SMO also assigns a Case number. Like the Case
identification, the SAS number designates a group
of samples collected at one site or geographical
location during a predetermined and finite time
period. The RSCC or designee records the SAS
number and Case number (if applicable) and uses
both numbers in referencing the request throughout
sampling arid analysis.
SAS laboratory selection is based on a verbal
and written solicitation process for each
individual request. This solicitation results in a
written SAS award to the lowest qualified
bidder. Once SAS laboratory assignments are
made, SMO notifies the RSCC of the laboratories
that will be performing the analyses. -
The nature of the SAS laboratory solicitation
process requires the RSCC to be as exact as
possible with all elements of a request at the time
of request. SMO understands that actual site
conditions can vary considerably from expected
conditions and necessitate changes in the sampling
plan. However, the requestor is responsible for
notifying SMO immediately of any changes to
allow sufficient time to amend the SAS contract(s)
to meet the changed needs. If an original request
is changed significantly, the original SAS
contract will be voided, and the entire analysis
effort will be resolicited. SAS resolicitation
requires additional time before sample shipment
can take place.
d. User Provided Analytical Protocol
At the time of request, the RSCC must provide
the analytical methodology and quality control
requirements to be utilized for the SAS request
before SMO can initiate a solicitation. For SAS
requests that are based on the use of amended RAS
protocols, the RSCC must speciv modifications or
additions to tl ese protocols. If such changes are
extensive, the client request preparer must submit
changes under the SAS to SMO in written form two
to three weeks in advance of scheduled sample
shipment For SAS requests which require use o’
method that is not commonly available,
RSCC must submit the method two to three wee
in advance of sample shiprr t. Additional lead—
time is required for protocol distribution and
review by solicited laboratories.
SAS requests which cite well known
analytical publications do not require additional
lead-time for distribution since laboratories have
immediate access to this information. Examples
of frequently utilized method manuals are as
follows:
• Methods for Chemical Analysis of Water
and Waste, USEPA, Current Edition, or as
specified.
• Test Methods for Evaluating Solid Waste,
Physical/Chemical Methods, SW—846,
USEPA Office of Water and Waste
Management, Current Edition, or as
specified.
• StandardMethodsfortheExaminaticn of
Water and Waste Water, APHA,
AWWAI, WPCF, Current Edition, or as
specified.
Further analytical references are supplied i”
Appendix C. The RSCC should contact SMi
several weeks in advance if there Is a questh n
to whether a particular method will require
additional lead-time for distribution.
3. Procedures for M2king Changes to Analytical
Requ&s
The RSCC or designated logistical contact
must immediately notify the appropriate SMO
Coordinator of all changes in sampling plans
before and during the sampling event and after
shipment of samples to the laboratory. Changes
in plans include changes in sample matrices,
numbers of samples, analyses requested, deter on
limits, shipping dates, postponements or
cancellations. Failure to notify SMO of such
changes can result in delay in sampling to
accommodate scheduling changes, delay in start of
analysis due to conflicts, unsuitability of a
particular sample to an analytical program. cr
analysis data inappropriate for client purpos .
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Chapter III — Utilization Analytical Seruices
B. Regional Organicflnorganic
Allocation System
The NPO has established an allocation
system to equitably apportion available
laboratory capacity to the Regions during periods
of heavy sampling activity and limited
laboratory capacity. Currently, capacity is
available for the projected sample demand;
however, when the allocation system is in effect,
all organic and inorganic RAS and “RAS Plus
SAS” Cases will be scheduled accordingly.
During the last month of each fiscal year
quarter, the NPO provides the RSCC with the
Region’s monthly allocation of organic and
inorganic sample analyses for the following
quarter. The RSCC is responsible for planning
monthly sampling activities in accordance with
the NPO allocation.
Under the scheduling/allocation system, the
RSCC requests sample analyses for all planned
Regional sampling activities for a week on the
Wednesday of the prior week and assigns a
priority, if requested by SMO, to each request.
Upon receiving the Region’s analytical requests,
SMO makes laboratory assignments for the week
and schedules received requests up to each
Region’s allocation limit. Requests in excess of the
monthly allocations will not be processed by SMO
until all Regional requests which fall within
allocations have been placed at a laboratory. At
this time, any excess laboratory capacity for the
week is determined, and the NPO prioritizes
Regional sampling requests that exceed
allocations. SMO assigns available laboratory
capacity for sampling activities as prioritized by
the NPO. For additional information concerning
the allocation sy5tem, users should contact the
SMO Regional Coordinator or Analyst for their
Region (see Appendix B).
C Sample Documentation
Each sample processed by the CL? must be
properly documented to ensure timely, correct and
complete analysis for all parameters requested,
and most importantly, to support the use of sample
data in potential enforcement actions. The CL?
documentation system provides the means to
individually identify, track and monitor each
sample from the point of collection through final
data reporting As used herein, a sample is
defined as a representative specimen collected at
a specific location of a waste site at a particular
time for a sp..dflc analysis. The term sample may
refer to field samples, duplicates, replicates,
splits, spikes or blanks that are shipped from the
field to a laboratory. Whenever questions arise,
samplers should contact SMO or the RSCC for
direction and clarification concerning the proper
completion and distribution of CL? paperwork.
1. Sample Traffic Report
RAS organic and Inorganic samples are
documented with corresponding CU’ sample
Traffic Reports (TRs), a four part carbonless form.
Each TR may document up to twenty samples
shipped to one CL? laboratory under one Case
Number and one RAS analytical program.
Samplers must complete the appropriate TRs for
every shipment of RAS samples to a CLP
laboratory. Copies of properly completed TR
forms are induded in the CL? Sample?s Guide.
TR forms must also be used when an individual
sample is to be analyzed for both RAS and SAS
parameters. A SAS Packing list must not be used
for RAS + SAS Cases. Both the Case number and
the SAS number must be entered at the top right of
the form in order to clearly Identify and frack the
sampling event. Samplers must take caution r t to
include the Case number on “AU SAS samples
taken at the same site. Additionally, the
sampler must briefly describe the SAS
requirement on each TR (e.g., VOA — 1 ppb
detection limit”).
Each TR form includes a Giain-of-Custody
Record. Information about the Giain-of--Custody
Record follows.
SMO provides TR forms to each Region
through the RSCC. The RSCC should contact
SMO two or more weeks in advance to order
additional TR forms.
2. SAS Packing List
For “All SAS samples, samplers should use
the SAS Packing List (FL), a four part carbonless
form. The PL provides space to list up to twenty
samples on one form. SAS samples are numbered
using the SAS number followed by a two digit
number beginning with 01 (e.g., 4100-E-Ol, 4100-
E-02, etc.). If the sampling activity extends over
several days and more than one PL is used, care
must be taken not to repeat sample numbers.
23
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CLP Users Guide
Regions should consult SMO to verify that the FL
is appropriate to use in their situation.
Alternatively, the samplers may also use TRs
for all SAS requests but must be careful to ensure
that RAS Case numbers do not appear on those
forms.
Each SAS FL includes a Chain-of—Custody
Record. Information regarding the Chain-of—
Custody Record follows.
SMO provides SAS PL forms to each Region
through the RSCC. The RSCC should contact
SMO two or more weeks in advance to order
additional SAS PL forms.
3. Sample Number
A unique sample number, recorded on the TR
and SAS PL, identifies each sample. Inorganic
and organicfVOA sample numbers have different
fcrmats and are not interchangeable. Strips of
adhesive labels preprinted with individual
sample numbers are provided by SMO with TR
forms. Sampleri must provide sample labels,
marked in indelible ink with the appropriate
SAS sample numbers, for use with NAil SAS”
samples.
The sampler affixes the sample label to the
corresponding contain that make up the sample
and, if appropriate, to the outside of the metal
can in which tl sample is packed (see Section D
for packaging requirements). fl top edge of the
label should be placed at the level of initial
sample volume so that any loss of volume can be
easily detected. In order to protect the labels from
the effects of water and solvent, labels are
covered with dear, waterproof tape.
4. Sample Tag
Each s.alnDle removed from a waste site and
transferred to a laboratory for analysis must be
identified by a sample tag which contains specific
sample information as defined by NEIC. Sample
tags are retained by the laboratory as physical
evidence of sample receipt and analysis. Sample
tags may be obtained through the Regional office;
in some instances, sampling contractors may be
required to provide their own sample tags. An
example sample tag is sl- wn in Figure 15.
Additionally the sample tag contains
appropriate spaces for noting that the sample has
been preserved and indicating the analytical
parameter(s) for which t ’e sample will be
analyzed. After the sample tag Is completed.
each tag is securely attached to the sample
container. Samples are then shipped under chai
of—custody procedures as described in ti
following section.
5. ChaIn—of-Custody Record
In accordance with Agency enforcement
requirements, offidal custody of samples must be
documented from the time of collection until the
time of introduction as evidence during litigation.
The Chain-of-Custody Record is not a separate
document and is Induded as part of the Sample
Traffic Reports and SAS Packing Lists.
FIGURE 15. SAMPLE TAG
A sample is considered to be in an individual’s
custody if any of the following criteria are met 1)
the samole is in your possession or it is in you
view after being in your possession; 2) it was in
your possession and then locked up or sealed to
prevent tampering; or 3) it is in a secured area.
The team member performing the sampling is
responsible for the care and custody of the
collected samples until they are dispatched
properly. In follow up, the sampling team leader
reviews all field activities to confirm that proper
custody procedures were foliowed during the field
work.
The Chain—of—Custody Record is ernoloyed a
physical evidence cf sample c’ustcdv Th
sampler completes a Chairt— f—Custcdy R crd
24
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Chapter III - Utilization of Analytical Sert’ices
accompany each cooler shipped from the field to
the laboratory. Chain—of-Custody Record forms
can be obtained through the Regional office.
The sampler records the proect number,
samplers’ signatures and the Case and/or SAS
number as header information on the Chain-of—
Custody Record. The oorrux n1y known name of the
site should not be included since CLP laboratories
may perform work for the responsible party of
that site. For each station number, the sampler
indicates date, time, whether the sample Is a
composite or grab, station location, number of
containers, analytical parameters, CU’ sample
number(s) and sample tag number(s). When
shipping the samples, the sampler signs the
bottom of the form and enters the date and time
the samples are relinquished. The sampler enters
shipper name and airbill number under the
“Remarks” section on the bottom right of the form.
The custody record is completed using
waterproof ink. Any corrections are made by
drawing a single, ball-point pen line through 1
initialing and dating the error, then entering the
correct information. Erasures or use of fluid
correction procedures are not permissible.
The original signature copy of the Chain-of—
Custody Record is enclosed in plastic (with CL?
sample documentation) and secured to the Inside
of the cooler lid. A copy of the custody record is
retained for the sampler’s files. Whenever
samples are split with a source or government
agency, a separate Chain-of-Custody Record
should be prepared for those samples to indicate
with whom the samples are being split and
sample tag serial numbers from spUta.
Shipping coolers are secured and custody seals
are placed across cooler openings. As long as
custody forms are sealed inside the sample cooler
and custody seals remain intact, commercial
carriers are not required to sign off on the custody
form.
The laboratory representative who accepts
the incoming sample shipment signs and dates the
Chain-of-Custody Record to acknowledge receipt
of the samples. Once the sample b-ansfer process
is complete, the laboratory is responsible for
maintaining internal logbooks and records that
provide a custody record throughout sample
preparation arid analysis.
D. Sample Packaging and Shipment
1. Pi&iglng Requirements
Samples processed through the CL? must be
packaged for shipment in compliance with the
most current US. Department of Transportation,
state, local, and comn dal carrier regulations.
All required government and commercial carrier
shipping papers must be filled out and shipment
classifications made according to these
regulations. (Consult Appendix C for shipping
ref e re rices
Waterproof, metal or hard plastic Ice chests
or coolers are the only acceptable type of sample
shipping container. Inside the cooler, sample
contaIx s must be endosed in dear plastic bags so
that sample tags and labels are visible. Water
and soil samples suspected to be of medium/high
concentration or soil samples suspected to contain
dioxin must be enclosed in a metal can with a
clipped or sealable lid (e.g., paint can. ,). The
outer metal can must be labeled with the number
of the sample contained inside. ContaIi s which
do not fit Into paint cans should be double ba ed.
Shipping containers should be packed with
noncombustible, absorbent packing material (e.g.,
vermiculite) surrounding the sample bottles or
metal cans containing samples to avoid breakage
during fransport. Earth or loose Ice should rever
be used to pack samples; earth is a contaminant,
and ice melts resulting in container breakage.
Water samples for low level organic analysis
and low/medium level cyanide analysis must be
cooled to 4 C with ice when shipped. Shipping
with ice is optional for soil samples for
low/medium level organic analysis or
low/medium level cyanide analysis. Ice is not
required in shipping high concentration water or
soil samples for organic analysis or for any
irtatzix/concentration samples for metals or dioxin
analysis. Ice should be in sealed plastic bags to
prevent melting ice from soaking packing material
which, when soaked, makes handling of samples
difficult in the laboratory.
Low level inorganic arid VOA water samples
require chemical preservation. Users should
consult Chapter II as well as the analytical
method and Regional requirements for
preservation techniques.
TRs, SAS PLs, Chain-of-Custody Records, and
any other sample documentation accompanying
25
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CLP User’s Guide
the shipment must be enclosed in a waterproof
plastic bag and taped to the underside of the
cooler lid. Coolers must be sealed with custody
seals in such a manner that the custody seal would
be broken if the cooler were opened.
Shipping coolers must have clearly visible
return address labels on the outside. Shipping
coolers that are labeled in this manner will be
returned to the sampler by the laboratory within
fourteen days following laboratory sample
receipt.
2. ShIpping Instructions
All samples should be shipped through a
reliable commercial carrier, such as Federal
Express, Emery, Purolator or equivalent.
Sampling offices are responsible for sample
shipping charges.
Samples for organic analysis must be shipped
for overnight delivery. If shipn t requires more
than a 24-hour period, 40 CFR sample holding
times might be exceeded, thus compromising the
integrity of the sample analysis. Samples for
inorganic RAS analysis should be held until
sampling for the Case is complete and then
shipped for two—day delivery. In the inorganic
RAS program, three days is the recommended
period for coUection of a Case of samples.
The NEIC/Denver and the ERT/Cinciranati
hazardous waste site manuals provide extensive
information on EPA—approved sample packaging
and shipment techniques. References for these
materials are provided in Appendix C. In
addition, general questions concerning sample
packaging and shipment may be directed to SMO.
To facilitate return of the coolers, shippers
should dearly mark the name and address of
return destination on the coolers. Use of stencils
and paint is highly recommended for permanent
identification.
3. Shipment Coordination
To enable SMO to track the shipment of
samples from the field to the laboratory and
ensure timely laboratory receipt of samples, the
sampler must notify SMO of all sample shipments
on the day of shipment. At that time, the
sampler should provide the following
information:
• Sarn ler name ar.d phone nuinber.
• Case number and/or SAS number of the
project. I
• Exact number(s), mathx(ces) and
concentration(s) of samples shipped.
• Laboratory ies) to which samples were
shipped.
• Carrier name and airbill number(s) for the
shipment.
• Method of shipment (e.g., overnight, two-
day).
• Date of shipment.
• Suspected contaminants associated with
the samples or site.
• Any irregularities or anticipated
problems with the samples, induding
special handling instructions, or
deviations from established sampling
procedures.
• Status of the sampling project (e.g., final
shipment update of future shipping
schedule).
Sample shipment made after 5:00 p.m. EST
should be 1led in to SMO at the start of business
the next day (8. 00 a.m. EST). SMO must be
notified by 3:00 p.m. EST Friday of sam
shipments intended for Saturday delivery. C
laboratories remain open to receive Saturday
.shipments only upon advanee noti&ation by SMO
and only when shipment information has been
provided to SMO by the sampler.
The success of sample shipment coordination
depends on the proper use and handling of the
sample tracking forms and timely, complete
communication among the RSCC, samplers, SMO
and laboratories. Any postponements,
cancellations, ch.anges in the number or type of
samples to be collected or changes in shipping
dates must be communicated to SMO immediately.
E Procedures for Problem Resolution
1. Resolving Problems Concerning Sample
Shipment and Analysis
Program laboratories notify SMO of problems
with sample receipt or during sample analysis.
SMO immediately contacts the RSCC to relay the
problem and to assist in formulating a soluncn.
SMO then contacts the laborator, involved to
communicate the recommended action and,
authorize processing of the sample(s) in quest
Timeliness is the ke to prcblern resolution s:rc
26
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Chapter III — Utilization of Analytical Services
delays could affect contractual time requirements
for sample extraction and analysis and, if
extreme, could invalidate the analysis.
Users should refer general questions regarding
sample shipment, required sample analysis,
laboratory contracts or the status of data
deliverables on a particular Case or SAS to the
appropriate SMO personnel thiough the RSCC.
Technical questions regarding contract analytical
procedures should be referred to the TPO of the
laboratory or the APO if the TPO is unavailable.
2. Resolving Problems Concerning Analytical
Data
In the CLP’s Regional/Laboratory
Communication System, authorized Regional
personnel can contact specified laboratory
personnel to resolve questions regarding the final
data package. This system may only be used after
laboratory data submission and may never be used
to initiate additional analytical work to resolve
data questions. All communications between
laboratories and Regional contacts are recorded by
each party on a Telephone Record Log.
Documented information includes Case and/or
SAS number, individuals making contact, sub ct of
the discussion and its resolution. As a follow up,
the Region and laboratory send copies of
completed telephone logs to SMO, where the logs
become a permanent part of the Case/SAS file.
Telephone Record Logs are available from SMO.
Prior to the laboratory’s submission of the
final data package, client queries regarding those
analyses or data are handled by SMO through the
RSCC. Depending on the nature of the question,
SMO will respond or will direct the dient to the
appropriate NPO official for resolution.
Comments regarding laboratory performance,
whether positive or negative, should be directed
in writing to the TPO of the laboratory with a
copy provided to the APO.
27
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The CLP provides several supplementary
services that have developed as a natural
extension of the program’s analytical services. A
description of each auxiliary service and the
procedures for accessing the service are provided
in the following sections.
A. Shipment Management Program
The Shipment Management Contractor
establishes, maintains and monitors all shipping
accounts for the transportation of CU’ materiaLs.
Currently, the Contractor coordinates accounts for
the shipment of sample containers, sample coolers
and contract compliance screening results. Other
items that are routed for CL? use may also be
addressed by this program at the request of the
NPO.
1. Sample Coolers
Field samplers package samples into coolers
for transportation to contract laboratories per the
procedures specified in Chapter 111, Section D.
Sampling contractors are responsible for dearly
marking a return address on the outside of each
cooler. Contract laboratories are required to return
each cooler to the indicated sampling office
within fourtcen days of sample receipt. The
Shipment Management Contractor is responsible
for tracking and paying for cooler shipments from
the laboratories to the sampling offices.
2. Confrad Cimtpllance Screening Results
After reviewing each data package via the
Contract Compliance Screening (CCS) process (see
Section F), SMO distributes the results to
EMSL/LV, the appropriate Region and the
appropriate laboratory. SMO also se Is a copy of
the air carrier manifest to the Shipment
Managen ent Contractor who uses the manifest to
verify and pay shipping invoices. If any problems
arise regarding the shipment of CCS results, both
SMO and the Shipment Management Contractor
should be notified immediately.
B. Information Services
1. Backlog Status Reports
SMO distributes the Laboratory Sample
Backlog Status Report and Regional Sample
Backlog Status Report. These reports show the
status of each sample until it is complete or
continues to be incomplete for a maximum of 180
days. These reports are distributed twice monthly
to all fl’Os, RSCCS and Contract Laboratories.
a. Laboratory Sample Backlog Sfafus Report
The Laboratory Sample Backlog Status
Report is available by laboratory contract.
Information is presented by laboratory contract
number and Case number. Contract type and
Regional Lab location are indicated for each
contract. SDC number; sample number; sample
suffix; data due date (DDD); data receipt date
(DRD), if applicable; number of days late, if
applicable; data complete date (DCD) and a
status message are also indicated.
The sample suffix column is used to
distingi.iishadd tionai analyses performed on an
original sample. These codes include-.
B = Blanks
M = Matrix
D = Duplicate
Q = RestedRerun
CHAPTER IV
AUXILIARY SUPPORT SERVICES
In this chapter
Shipment Management Program
Sample Coolers
Contract Compliance Screering Results
Information Services
Backlog Status Reports
Sample Status Information
General Program Information
Enforcement Support
Generation of Known Qualty Data Suitable
for Use in Enforcemerit/Uligation
Additional CLP Enforcement Support
Cost Recovery Substantiation
Contract Compliance Screening
Data Review Services
28
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Chapter IV — Auxiliary Support Sa-uices
= Replicate
= Automatic Rerun
= Laboratory Control
Sample
R
x
L
There are six sample status messages.
Samples only appear under one status message.
The status messages are as follows:
(1) Data Not Due - This message indicates
that samples have been received by the
laboratory, but the data have not been
received and are not yet due.
(2) Data Late - This message indicates that
the due date has past and data have not
yet been delivered by the laboratory. If
this message appears in the status column
for a sample, the number of days late will
appear in the days late column.
(3) In CCS Review - This message indicates
that data for a sample have been received
and the results of the Contract
Compliance Screen have not been sent to
the laboratory.
(4) In 10 Day Resolution Period —This
message will appear in the Status column
for any sample data which have been
received, screened and screening results
sent to the laboratory, but the 10 day
resolution period has not yet passed. The
resolution pesiod is 10 days from the date
the laboratory receives the screening
results. The laboratory has 10 days to
resolve any noncompliance issues,
including technical noncompliance and
incompleteness.
(5) Incomplete After C( Days -This message
will appear when data have been
received, screened and the 10 day
resolution period has passed, and the
sample data remain incomplete. The
number of days since the lab received the
initial screening results is printed in the
status column. This samole win continue
to appear on the backlog list until it
remains incomplete for 180 days.
(6) Complete — This message will appear in
the Status column for an sample made
complete since the last Backlog Statu.s
Report was generated.
b. Regional Backlog Stat’.zs Re or
The Regional Sampte Backlog Status Report
is ve.y similar to the L.abora:cr-v Report. Tne
status information is presented by Client, rather
than by laboratory. The laboratory code name
and contract type are listed for each sample
to the sample suffix column.
Both the Laboratory and Regional Sample
Backlog Status Reports include three totals at the
end of each report. The “total number of
outstanding samples” includes samples for which
data are not due, late, in 10 Day Resolution period
or are incomplete. The “total number of samples
late” indudes only those samples which do not
have an initial data receipt date. If data were
received, but were incomplete, it would not count
in this category. “Total Number of Samples
Incomplete refers to samples that either are in
the 10 Day Resolution Period or remain
incomplete after the 10 day resolution period has
2. Sample Status In.fnrrrtition
After scheduling analysis, SMO tracks
samples from shipment through data reporting
via manual and computerized fracking systems.
SMO maintains ongoing communication with the
TPOs, RSCCS and laboratories regarding sample
status and responds to inquires from concerned
parties, as appropriate.
3. General Program Iri.fonna±ion
Under the direction of CLP management, SM-
serves as the program’s information center for
incoming calls and correspondence. Program
participants and other interested parties may
request from SMO information and materials on
program services and procedures. SMO provides
this information when possible and refers callers
to the proper sources for additional information.
C Enforcement Support
1. Generation of Known Quality Data Suitable
for Use in Enforcement/Litigation.
One ma r objective of Superfund is to recover
costs incurred in the investigation and clean up oi
hazardous waste sites from responsible parties.
The process by which these parties are identified
and determined to be responsible often involves
litigation. Frequerttlv, procedures necessitate the
use of CLI ’ data generated from the analysis oi
samples -collected at a given site. The CL?
supports these and other enforcement require!m?nts
of Superfund by ensuring that CL ? analytical da
are documented and available for litiga
10
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CLP Users Guide
Through NEIC. the CL? has established detailed
procedures and documentation to ensure that
sample data meet Agency enforcement standards.
Each CL I’ analytical contract requires the
laboratory contractor to implement a
comprehensive document control system and to
employ strict chain—of—custody documentation
procedures in the receipt and handling of samples
throughout the analytical and data reporting
process. The laboratory must have the following:
• written standard op ating procedures for
receipt and log-in of samples,
• maintenance of sample secuiity after log-
in,
• tracking of samples through all steps of
preparation and analysis, and
• organization and assenibly of all sample-
related documentation on a Case—specific
basis.
At a minimum, required document control and
chain-of-custody records include
• custody records,
• sample tracking records,
• analyst logbook pages,
• bench sheets,
• chromatographic charts,
• computer printouts,
• raw data summaries,
• insfrun t logbook pages,
• correspondence and docun t inventory.
Before a laboratory is awarded a CU’ contract
and continuing periodically throughout the life of
the contract, NEIC audits each laboratory
facility to ensure compliance with chain—of—
custody and document control requirements. In
addition to facility audits, NEIC reviews
laboratory data and evidence documentation on a
regular basis.
2. Addition.al CLP Enforcement Support
Court appearances and other mandated
deadlines often do not allow sufficient time for
completion of the normal complete SDG File, data
package, and traditional file purge package
submission, review and audit process. In this
event, enforcement activities require direct CL?
support. Data package evaluation and/or
testimony from laboratory or CL? personnel may
also be needed. Through SMO, the CL? has
established procedures to coordinate and respond
to sl rt term (rn, more than 180 days) enforcement-
related requirements. These procedures are
detailed in Figure 16.
OWPE provides this CL? information along
with documentation gathered from other sources
to the Regional case development team in the full
cost recovery package.
FIGURE 16. ADO ONAL CLP ENFORCEMENT SUPPORT
Reqie
cuçh
Leai
lime
Reqie Proceö es
Re e Inlomabon
Reqiired
Docimen n Pm ded
By CLP
NPO
2
. .
• S tmt ie *cemen1-
m requ in a
e NPO.
?FO ruvieii t
de iriestie
ct re p . and xi azth
e id kei ons
9
i
t9ç ,esb EZVJId
e4 by ofo
d b ’w &ç a w ,
( 6 1Tb , ia,n7
•
. aid epcr rui
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a airç t e enfottarent
W Nit
• Cas&SASr jntec s) of
zpec5c an pIriç(s)
• Sa e Jmbe s)
• Da s) of nip e c3 on
• U ry( es) that
por*a’med e amiyas
T f 3u c(t reedad
• AIT2rçaI d e me ’
of al Uxy and
endece cxner r
retaeng b spoctfc sair.pie
of requei If
• ir s iz*rn n r&a ig
b sar e afoJy s or P ri ig
r t zciec cafly required
ur eoatry crta’ c .
• AaSIa fl VTw ç,n9 (
e-t saT ny by
zoClPpe som o
ka ,e Ra9oraJ resour s
fcr ar v caJ dau r e*’
30
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Chapter IV - Auxiliarg Supyx rt Scruic
FIGURE 17. COST RECOVERY SUBSTANTIATION
Reqie
ttroi.41
Lead
Time
Request Proceóires
eques o In oirnabon
F qir d
Doc men bon Pm’ ided
By CIP
4.6
Co rp e a Cost Re xv
(C2) chedtht
• LW a rp e d CR thed$sz
b OW?E
• OWFE a 1ec ard o
.aI4e d docjmen xn
Name and s of
•
F rc a1 Surn b Cod
Ma Iy* is
•
V ch a Car
Coil Repot
• Pcu c Senicai
Ca eSan eUd
(SAS) Coit Re ,rt
• Co .sof&&S-Páa d
c c
La
D. Cost Recovery Substantiation
The CLI’ provides documentation for prcgram
analytical costs to the EPA’s Office of Waste
Programs Enfordement (OWPE) in support of
Superfund cost recoveiy forts. These procedures
are detailed in Figure 17.
E. Contract Compliance &re ning (CCS)
SMO performs CCS on all RAS data produced
by the CLI’. Modified CCS can also be performed
on a case-by-case basis on RAS Plus SAS or MAll
SAS” data.
CCS is a stnictured review which detennines
completeness of data deliverables and compliance
of QA/QC parameters with contract
specifications. The primary objectives of CCS are
to resolve identified discrepancies in a timely
manner and to identify the liquidated damages
category for data not in compliance. Data which
meet all CCS criteria at initial receipt are
recommended for 100% payment of the amount
due. Data with CCS defects are recommended to
have some payment withheld, either
temporarily or permanently, depending on the
nature and extent of the defect identified.
CCS procedures are applied to organic,
inorganic and dioxin data. CCS results are
produced on a fast—’ urnaround basis (fiIte n days)
and identify compliance discrep.ancies by code,
criterion, fraction and sample. Results are
distributed to the relevant laboratory, Region and
EMSL /LV.
Results are accumulated in the CCS Database
in order to produce routine and requested
summaries of laboratory performance and
compliance trends.
F. Data Review Services
A full range of review services are used to
assess CL? data. Objectives of the review servicc
are:
• To determine the useability and
limitations of data given particular field
or policy assessment criteria.
• To maximize the amount of useable data
by identifying aiticai properties of data
and by resolving or proposing solutions to
analytical or quality control problems.
• To provide systematic and standardized
data quality assessn t and status
summary to determine method, laboratory
and program perforniax ce.
These review services are performed by a
number of operations:
• Review for data useability is performed
by Regional personnel and contractors.
Recomrnertded review procedures have
been standardized and organized into
functional guidelines for evaluating CL?
data. EPA Data Validation Wor grou:s
have produced specific documents for
review of organic. inorganic ar.d dicxn
analyses.
31
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CLP Llsers Guide
• Comprehensive QA review is performed
by EMSL/LV on specific data packages.
Review and assessment of some program-
wide QA results are also performed by
EMSL/LV to evaluate method and
laboratory performance and the quality of
analytical data.
• Under direction of the CLP management,
EMSL/LV and/or SMO may perform
additional data review to assess a
probleni Case or provide a second opinion
on data useability.
• Under direction of the CL I ’ management,
SMO third party data reviews may be
used to resolve disputes, espedally for
SAS cases.
All requests for SMO data review services
should be placed using the SMO Data Review
Request memorandum available from SMO.
Request procedures are detailed in Figure 18.
Copies of the request should be submitted to SMO
(Attention: Data Review Team), the SMO P0 and
the RSCC Upon authorization by the APO, SMO
schedules the review and notifies the requestor of
the date of scheduled completion. (Data review
cannot be initiated until all deliverables for the
subject Case(s) have been received from the
laboratory.)
FIGURE 18. DATA REVIEW SERVICES
Re te
ttrough
Lead
Time
Reqiest Procedires
Requestor lntcrrnaticn
Aeqiired
Doaimen bon Provided
By CLP
SMO.
2 wgor.s
Ca, I a SMO Oaa Ro ,ow
• S .C Case nur t ’
• An 1u n t ti thu
APO,
RSCC
mxT an Jm
Of th
nwrD nôJ to S C (Ann:
Dz Re uw Toani). 5
APO and the R C.
U c APO 9(OV2I. S C
t tf s the t e or ci the
thie c i v d T WtIJ1.
D ’i ,wi in be a ed
&rti a) lor
— ) lime b n
,eca from th. orVory
• S4e nine
• Anu)yx J ii )
• Nurrb
Sanç
. T po(s) o4 r w mque ed
• Ro ie .d 1a icr tv,i w
• Uw cam. and ru
. tr1end e ci d a
2 32IT r A ?FI
and su or 2r -t ii
. tatmn . P’ d for
t F z
1 2TP tT I 1 . the ia1
á ths d4a ate
xc tabie quaJd xi
Pe or or the naz
we dcc.5aed and
1Z r v icn or ci
the at a ci psdomw a we
r the r 4 b
.-
32
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CHAPTER V
LABORATORY SELECTION AND STARTUP
A. Laboratory Selection Process
From time to time, when EPA needs to replace
existing IFB contract resources where contracts are
due to expire, to increase capacity over what is
currently provided under existing contracts, or to
initiate a procurement for a new type of analysis,
EPA solicits laboratories for the CLP. This
process is summarized in Figuie 19. EPA solici
bids from interested laboratories, evaluates each
laboratory on the basis of the criteria listed
below, and awards contracts to qualified, low-
bidding laboratories.
1. Qualification Requlrtnients
a. Bid Price
The first criterion for laboratory selection is
bid price. Following bid opening, the bid prices
are reviewed and evaluated by NPO and
Contracts Management Division (CMD) offidais.
The lowest competitive bidders will be sent
performance evaluation (PE) samples at the
In this chapter
Laboratoty Selection Process
Qua fication Requirements
Bidder Respons blity
Laboratory Startup Process
APO
APOITPOISMO!Laboratory
Communication
Laboratory Performance Evaluation
Performance Evaluation Sample Analysis
On—site Laboratory Evaluation
Corrective At ion
FIGURE 19. THE CLP LABORATORY SELECTION PROCESS
( IS > ___________ I
5 ; 5 ;.•. . .. .S — .•
.5 _ ,. _ .4 . . .
:1
—. S S S S
;.‘ ( •
“S •... •;:•‘ • .
PE —. . — • —S
. — -. — ‘ . . 5’
P.s a.
,_
- • -‘ •: ‘ “ ‘ ps. vW — b P •
I l (%I .
—
t_ — . — , _
— — V
.4 .5’
33
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CLP Llsers Guide
direction of the Contracting Officer (CO).
b. Preaward Performance Evaluation Sample
Analysis
The second aiterion for laboratory selection is
acceptable preaward FE sample analysis. FE
samples are sent to laboratories at the direction of
the Co.
FE samples, distributed by EPA, are
representative of the types of field samples that
the laboratory would be routinely analyzing under
the subject procurement. The laboratory is
required to analyze PE samples according to
contract procedures set forth in the IFB and to
report PE sample data according to IFB
requirements. The turnaround time for PE sample
data submission is indicated in each IFB. Bidders’
PE sample data are evaluated by NPO and
EMSL/LV personnel for compliance with contract
requirements and accuracy of determination of
compounds at the levels known to be in the PE
samples. Analysis results are rated by a
scoresheet developed by the EPA; currently, the
acceptable performance score is seventy—five
percent.
2. Bidder Responsibility
a. Bidder—Supplied Documentation
At the time of submission of PE sample data,
bidders are required to submit documented
evidence that they have the internal procedures,
equipment and personnel in place for successful
performance of contract requirements. Required
docuirentatfon includes:
• functional descriptions and detailed
resun of key personr l;
• inventory of laboratory equipment;
• description of laboratory space; and
• written Standard Operating Procedures
(SOPs).
Submitted documentation is reviewed by NPO
and EMSL/LV personnel and is utilized by the
EPA in performance of the site evaluation. After
contract award, bidders are required to submit
revised SOl’s to the APO.
b. Laboratory Site Evaluation
NPO, TPO, CMD, EMSL/LV and NEIC
personnel participate in on—site evaluations of
laboratory facilities of bidders which scored
acceptably on the FE sample analyses and are
within the EPA-determined competitive range.
The results of the on—site evaluation are
considered in the final determination of bidr
responsibility for contract award.
B. Laboratory Startup Process
Laboratories are expected to be capable of
receiving full contract sample requirements upon
award. At award, laboratories must provide
standards in compliance with the performance
specifications supplied in the con act.
1. MO Review of First Data Packages
Initial data packages are targeted for
immediate review and evaluation by the APO,
EMSL/LV and the Region. This intensive review
focuses on any problems the laboratory may have
in applying methodologies or in reporting data.
The APO and TPO supply feedback to the
laboratory concerning the status of the data and
work with the laboratory in identifying and
remedying problems. Depending on the extent of
the problems found during the review of an initial
data package, the APO or TPO may visit the
laboratory facility and work on—site with
laboratory personnel to rectify problems.
2. APO!rPOISMO!L boratozy Communication
Telephone communication is the most wide
applied method for problem—solving an
m.3intainng efficient laboratory opera tic ns
during both the laboratory startup phase and
throughout the performance of the contract. In
general, the laboratory notifies SMO
immediately upon identification of any problem
regarding the samples. Any questions regarding
difficulties encountered in analysis should be
addressed to the TPO of the Region of sample
origin with SMO serving as a go-between to record
resolution of the issue. SMO routinely resolves
sample-related problems in coordination with the
Regional client and rthrs technical problems to
the APO or TPO, who then contacts the laboratory
to resolve the problem. The resolution and any
specific actions taken are reported to the
appropriate SMO personnel who records this
information as part of the permanent Ca.se record.
The laboratory also records the problem and
resolution in the narrative portion of the sample
data report so .hat the Region will consider this
information when evaluating and using the data.
3-4
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Chapter V — Laboratory Selection and Startup
C Laboratory Performance Evaluation
1. Performance Evaluation Sample Analysis
EPA may distribute FE samples to contract
laboratories for analysis. EMSL/LV evaluates
the laboratories’ FE sample data, and the NPC)
uses this evaluation in formally assessing
laboratory contract performance. Additionally,
EMSL/LV enters FE 5ample data into the
program’s QA and Results Database. These data
are utilized, along with other laboratory data, in
trend analyses and evaluation of contract QC
criteiia. Refer to Chapter VI, Section C for a more
detailed description of FE samples.
. On—site Laboratoxy Evaluation
Regional, NEIC and EMSL/LV personnel visit
each contract laboratory facility in order to
evaluate laboratory procedures or to identify
laboratory problems for correction. The frequency
of on—site evaluation depends, in part, upon
laboratory perforr.ance. The APO and TPO
utilize the evaluation reports which result from
these on-site visits in identifying and remedying
laboratory performance problems. Chapter V I,
Section E details the on—site laboratory
evaluation process.
3. Corrective Action
The APO and TPO, work dosely with each
laboratory to correct identified laboratory
performance problems. Depending on the scope of
the problems, the laboratory may be placed on
temporary hold and will not receive additional
samples for analysis until the problem has been
corrected.
If the laboratory’s noncompliance to contract
performance or delivery requirements continues,
the NPO may request the CO to initiate a contract
action such as a Show Cause Notice or a Cure
Notice.
A Show Cause Notice requires the Contractor,
within a ten—day period, to present any facts the
government can use to determine if the
Contractor’s failure to perform arose without any
fault or negligence on the part of the Contractor.
The Contractor must submit substantial evidence
to demonstrate that the contract should not be
terminated for default. A recovery plan is
generally included as part of the Contractor’s
response to the Show Cause Notice. NPO and
GAD officials review the Contractor’s response
and proposed recovery plan to determine whether
the Contractor has presented sufficient evidence
to demonstrate timely remedy of the
noncompliance. Following this review, if the
Contractor has presented acceptable evidence
toward recovery, the government issues a Cure
Notice to the Contractor.
A Cure Notice specifies the Government—
accepted recovery plan that the Contractor must
follow to avoid contract termination. The
recovery plan indudes actions and time schedules
for completion of each step of the recovery process,
and specifies an overall time period acceptable
for completion of recovery.
Should the Contractor not comply with the
recovery schedule, the Governmenrs next and
final step may be contract termination for default.
In addition to terminating the laboratory’s
corthact, this action affects the evaluation of the
laboratory’s responsthility for award under future
CLP solicitations.
-------
CHAPTER VI
PROGRAM QUALITY ASSURANCE
Quality assurance (QA) and quality control
(QC) are integral parts of the CL?. The quality
assurance process consists of management review
and oversight at the planning, implementation,
and completion stages of the environmenb.l data
collection activity. The QA process ensures that
data provided are of the quality required. The
quality control process includes those activities
required during data collection to produce the
data quality desired and to document the quality
of the collected data.
During the planning of an environmental data
collection program,. QA activities focus on defining
data quality criteria and designing a QC system to
measure the quality of data being generated.
During the implementation of the data coUection
effortr QA activities ensure that the QC system is
functioning effectively, and that the deuiciendes
uncovered by the QC system are corrected. After
environmental data are collected, QA activities
focus on assessing the quality of data obtained to
determine its suitability to support enforcement or
remedial decisions.
A complete QAIQC program includes internal
laboratory QC criteria that must be met to ensure
acceptable levels of performance. These
performance levels are determined by QA review.
External review of data and procedures is
accomplished by the monitoring activities of the
NPO, the Regions, SMO, NEIC and EMS LILy.
Laboratory evaluation samples, magnetic tape
audits and laboratory on-site evaluations provide
an external QA reference for CLP. A feedback 1 oop
supplies the results of the various review
functions to the contract laboratories through
direct communication with the APOs and TPOs.
The following sections describe overall QA/QC
operations and how the CLP meets the QA/QC
obective.
A. Laboratory Quality Control Criteria
1. Standard Operating Procedures
In order to obtain reliable results, adherence
to prescribed analytical methodology is
imperative. In any operation that is performed on
a repetitive basis, reproducibility is best
accomplished through the use of Standard
Operating Procedures (SOPs). As d ned by the
EPA, an SOP is a written document which
provides directions for the step-by-step execution
of an operation, analysis, or action which is
commonly accepted as the method for performing
certain routine or repetitive tasks.
SOPs prepared by the Contractor must be
functional: i.e., dear, comprehensive, up-to-date,
and suffldently detailed to permit duplication of
results by qualified analysts. All 501’s, as
presented to the Agency, must reflect activities as
they are currently performed in the laboratory. In
addition, all S Ql ’s must
• Be consistent with current EPA
regulations, guidelines, and the Cl_P
contract’s requirements.
• Be consistent with instrument
manufacturers’ s ediic instruction
manuals.
In This cha,pto,
Laboratory Qua ty Control Ciiteria
Standard Operating Procedures
Quality Assurance Plan
Analytical Standards Traceability
Requirements
Analytical Data Review
Contract Conipllance Screening
Regional Data Review
Laboratory Evaluation Samp es
GCIMS Tape Audits
On—Site Laboratory Evaluations
Quality Assurance On-Site Evaluation
Evidentiary Audil
Discussion of the On-Site Team’s Findings
Corrective Action Reports For Follow-Through
to Quality Assurance and Evident,aiy Audit
Reports
Quality Assurance and Data Trend Analysis
Data Management
36
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Chapter VI - Program Quality Msurance
• Be available to the EPA during an On-
Site Laboratory Evaluation. A complete
set of SOPs shall be bound together and
available for inspection at such
evaluations. During on-site evaluations,
laboratory personnel may be asked to
demonstrate the application of the SOPS.
• Provide for the development of
documentation that is sufficiently
complete to record the performance of all
tasks required by the protocol.
• Demonstrate the validity of data
reported by the Contractor and explain
the cause of missing or inconsistent remits.
• Describe the corrective measures and
feedback mechanisms utilized when
analytical results do not meet protocol
requirements.
• Be reviewed regularly and updated as
necessary when contract, facility, or
Contractor procedural modifications are
inade
• Be archived for future reference in
useability or evidentiary situations.
• Be available at specific work stations as
appropriate.
• Be subject to a document control procedure
which precludes the use of outdated or
inappropriate SOPs.
a. SOP FORMAT:
The format (or SOPs may vary depending upon
the kind of activity for which they are prepared,
however, at a minimum, the following sections
must be ir iuded:
• Title Page
• Scope and Application
• Definitions
• Procedures
• QCUmits
• Corrective Action Procedures, Including
Procedures for Secondary Review of
Information Being Generated
• l)ocumentation Description and Example
Fom
• Miscei1ane us Notes and Precautions
• Ref e.—ences
L i. SOPs Delivery Requirements
Within forty-five (45) days of contr2
receipt, a complete set of SOPs, relevant to tr.
contract shall be sent to the Technical Project
Officer, SMO and EMSL/LV. Also, during the
term of performance of the contract, copies of SOPs
which have been amended or new SOPs which
have been written shall be sent to the Technical
Project Officer, EMSL/LV (quality assurance
SOPs) and NEIC (evidenfiazy SOPs).
2. Quality Assurance Plan
The Contractor shall establish a quality
assurance program with the objective of providing
sound analytical chemical measurements. This
program shall incorporate the quality control
procedures, any necessazy corrective action, and
all documentation required during data collection
as well as the quality assessment measures
performed by management to ensure production of
acceptable data.
As evidence of such a program, the Contractor
shall prepare a written Quality Assurance Plan
(QAP) which describes the procedures that are
implemented to achieve the following
• Maintaining data integrity, validity, and
useability.
• Ensuring that analytical measurement
systems are maintained in an ceptable
state of stability and reproducibility.
• Detecting problems through data
assessment and establishing corrective
action procedures which keep the
analytical process reliable.
• Documenting all aspects of the
measuremett process in order to provide
data which are technically sound and
legally defensible.
The QAP must present, in specific terms, the
policies, organization, objectives, functional
guidelines, and specific QA and QC activities
designed to achieve the data quality requirements
in each contract. Where applicable, SOPs
pertaining to each element shall be induded or
referenced as part of the QAP. The QAP must be
available during on-site laboratory evaluation
and upon written request by the Administrative
Project Officer.
The following elements should be contained u
the Quality Assurance Plan.
37
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CLP LLcers Guide
A Organization and Personnel
1. QA Policy and Objectives
2. QA Management
a. Organization
b. Assignment of QC and QA
R ponsibiliti
c. Reporting Relationships
d. QA Document Contro& Pcedures
e. QA Program Assessment Procedures
3. Personnel
a. Resumes
b. Education and Experience P tinent
to this Contr t
C. Training Progress
B. Facilities and Equipment
1. Insthinientation and Backup
Alternatives
2. Maintenance Activities and Schedules
C. Docun t Control
1. Laboratory Notebook Policy
2. Samples Tracking/Custody Procedures
3. Logbook Maintenance and Archiving
Procedures
4. Case File Organization, Preparation
and Review Procedures
5. Procedures for Preparation, Approval,
Review, Revision, and Distribution of
SOPs
6. Process for Revision of Technical or
Documentation Procedures
D. Analytical Methodology
1. CalIbration Procedures and Frequency
2. Sample Preparation/Extraction
3. Sample Analysis Procedures
4. Standards Preparation Procedures
5. Decision Processes, Procedures, and
Responsibility for Initiation of
Corrective Action
E. Data Generation
1. Data Collection Procedures
2. Data Reduction Procedures
3. Data Validation Procedures
4. Data Reporting and Authorization
Procedures
F. Quality Control
1. Solvent, Reagent and Adsorbent
Check Analysis
2. Reference Material Analysis
3. Internal Quality Contiol Checks
4. Corrective Action and Determination
of QC Limit Procedures
5. Responsibility Designation
G. Quality Assurance
1. Data Quality Assurance
2. Systems/internal Audits
3. Performance/External Audits
4. Corrective Action Procedures
5. Quality Assurance Reporting
Procedu
6. Responsibility Designation
3. Analytical Standards Traceability
Re
The U.S. Environmental Protection Agency
may not supply analytical reference standards
either for direct analytical measurements or for
the purpose of traceability. All contract
laboratories may be required to prepare from neat
materials or purchase from private chemical
supply houses those standards necessary to
successfully and accurately perform the analyses
required in this protocol
a. Prep2ration of Chemical Standards from the
N t High Purity Bulk Material
A laboratory may prepare their chemical
standards from neat materials unless their
contract specifies otherwise. Commercial sources
for neat chemical standards pertaining to
compounds listed on the Target Compound List are
given in the Appendix C of the “Quality
Assurance Materials Banic Analytical Reference
Standards” Seventh Edition, January 1988.
Laboratories should obtain the highest required
purity when purchasing neat chemical standards;
standards purchased at less than 97% purity must
bedocun ited as to whyahigherpuritycould not
be obtained.
b. Pwchase of Chemical Stand. rds Alr idy in
Solution
Solutions of analytical reference standards
can be purchased by Contractors provided they
n et the following aiteria:
1. Laboratories must maintain the foilowing
documentation to verify the integrity of
the standard solutions they purchase:
a. mass spectral identification
confirmation of the neat material
b. purity conflmiation of the neat
material
c. chrornatographic and quantitative
documentation that the solution
3S
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Chapter VI - Program Qw2lity Assurance
standard was QC checked according to
the following section
2. The Contractor must purchase standards
(or which the quality is demonstrated
statistically and analytically by a
method of the suppliet’s choice.
The laboratory is responsible for the quality
of the standards employed for analyses under this
contract.
c. Requesting Standards From the EPA
Standards Repository
Under special or en gency circumstances
only, solutions of analytical reference materials
can be ordered from the US. EPA Chemical
Standards Repository, depending on availability.
The Contractor can place an order for standards
only after demonstrating that these standards are
not available (torn comn dal vendors either in
solution or as a neat material.
d. Documentation of the V ’ification and
Preparation of Chank4 Standards
It is the responsibility of each laboratory to
maintain the necessary documentation to show
that the chemical standards they have used in
the performance of CU’ analysis conform to the
requirements previously listed. Weighing
logbooks, calculations, chromatograms, mass
spectra, etc., whether produced by the laboratory
or purchased from chemical supply houses, must be
maintained by the laboratory and may be subject
to review during on-site inspection visits.
Documentation of standards preparation may be
required to be sent to EPA for verification of
contract compliance. In those cases where the
documentation is supportive of the analytical
results of data packages sent to EPA, such
documentation is to be kept on file by the
laboratories for a period of one year.
B. Analytical Data Review
Upon completion of analysis and data
reporting, the contract laboratory simultaneously
sends a copy of the complete data package to
SMO, EMSL/LV and the Regional client. Each of
these groups performs complementary aspects of
data review. SMO C review identifies
contractual discrepancies; EMSL/LV review
determines technical quality and consistency; and
Regional data review relates useability of the
data to a specific site.
1. Contract Compliance Screening
CCS is one aspect of the Government’s
contractual right of inspection of analytical data.
CCS examines the Contractor’s adherence to the
contract requirements based on the sample data
package delivered to the Agency.
CCS is performed by the Sample Managerr t
Office (SMO) under the direction of the EPA. To
assure a uniform review, a set of standardized
procedures have been developed to evaluate the
sample data package submitted by a Contractor
against the technical and completeness
requirements of the contract.
CCS results are mailed to the Contractor and
all other data recipients. The Contractor has a
period of time to correct defldencies. The
Contractor must send all corrections to the
Regional Client, and SMO.
CCS results are used in conjunction with other
information to measure overall Contractor
performance and to take appropriate actions to
correct deficiencies in performance.
2. RegIonal Data Review
Contract Laboratory data are generated to
meet the specific needs of the Regions. In order to
verify the useability of data for the intended
purpose, each Region reviews data from the
perspective of end-user, based upon functional
aspects of data quality. General guidelines for
data review have been developed jointly by the
Regions and the National Program Office. Each
Region uses these guidelines as the basis for data
evaluation. Individu al Regions may augment the
basic guideline review process with additional
review based on Region-specific or site-specific
concerns. Regional reviews, like the sites under
investigation, vary based on the nature of the
problems under investigation and the Regional
response appropriate to the specific circumstances.
Regional data reviews, relating useability of
the data to a specific site are part of the
collective assessment process. They complement
the review done at the Sample Management
Office, which is designed to identify contractual
discrepancies and the review done at EMSL/LV
which is designed to evaluate Contractor and
method performance. These individual
evaluations are integrated into a collective
review that is necessary for program and
laboratory administration and management and
39
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CLP Usci- ’s Guide
may be used to take appropriate action to correct
deficiencies in the Contractor’s performance.
C Laboratory Evaluation Samples
Although intralaboratory QC may
demonstrate Contractor and method performance
that can be tracked over time, an external
performance evaluation program is an essential
feature of a QA program. As a means of measuring
Contractor and method performance, Contractors
participate in irtterlaboratory comparison studies
conducted by the EPA. Results from the analysis
of these laboratory evaluation samples will be
used by the EPA to verify the Contractor’s
continuing ability to produce acceptable
analytical data. The results are also used to assess
the precision and accuracy of the analytical
methods for specific analytes.
Sample sets may be provided to participating
Contractors as frequently as on an SDG-by-SDG
basis as a recognizable QC sample of known
composition; as a recognizable QC sample of
unknown cz mposition or not recognizable as a QC
material. The laboratory evaluation samples
may be sent either by the Regional client or the
National Program Office, and may be used for
contract action.
Contractors are required to analyze the
samples and return the data package and all raw
data within the contract required turnaround
time.
At a minimum, the results are evaluated for
compound identification, quantification, and
sample contamination. Confidence intervals for
the quantification of target compounds are based
on reported values using population statistics.
EPA may adjust the scores on any given laboratory
evaluation sample to compensate for
unanticipated difficulties with a particular
sample. Contractors are required to use the
NIST/EPA/MSDC mass spectral library to
tentatively identify a maximum number of non-
target compounds in each fraction that are present
above a minimal response. Tentative
identification of these compounds, based on
contractually described spectral interpretation
procedures, is evaluated and integrated into the
evaluation process.
A Contractor’s results on the laboratory
evaluation samples will determine the
Contractor’s performance as follows:
1. Acceptable, No R ponse Required (Score
greater thanor equal to90percent):
Data meet most or all of the scoring
criteria. No response is required.
2. Acceptable, Response Explaining
Deficiency ies) Required (Score greater
thanor equal to 75 per tbut less than 90
percent):
Deficiencies exist in the Contractor’s
Within 14 days of receipt of notification
from EPA, the Contractor shall describe
the defid .ency(ies) and the action(s)
taken to correct the defldency(ies) in a
letter to the Administrative Project
Officer, the Technical Project Officer and
EMSL/LV.
3. Unacceptable Perfürmancc, Response
Explaining Deficiency(ies) Required
(Score less than 75 percent):
Defid es e, st in the Contractor’s
performance to the extent that the
National Program Office baa determined
that the Contractor has not demonstrated
the capability to m t the contract
Within 14 days of receipt of notification
from EPA, the Contractor shall desaibe
the dthclency(ies) and the action(s)
taken to correct the deficieixy(ies) in a
letter to the Administrative Project
Officer, the Technicsl Project Officer and
EMSL/LV.
The Contractor shall be notified by the
Administrative Project Officer or
Tedudcal Project Officer concerning the
remedy for their unacceptable
performance. A Contractor may expect,
but EPA is not limited to, the following
actions: Reduction of the num of
samples sent under the contract, suspension
of sample shipment to the Contractor, a
site visit, a full data audit, analysis of
remedial PE samples, and/or a contract
sanction, such as a Cure Notice.
Note A Contractor’s pronipt response
demonstrating that corrective actions
have been taken to ensure the Contractor’s
capability to meet contract requirements
wiU facilitate continuation of full sample
delivery.
40
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Chapter VI- Program Quality Assurance
D. CC/MS Tape Audits (Organics Only)
Periodically, EPA requests from Contractors
the CC/MS magnetic tapes corresponding to a
specific case in order to accomplish tape audits.
Generally, tape submissions and audits are
requested for the following reasons
• Program overview
• Indication of data quality problems from
EMSL/LV, SMO, or Regional data
reviews
• Support for on-site audits
• Specif 1 c Regional requests
Depending upon the rea.scn for an audit, the
tapes from a recent case, a specific case, or a
laboratory evaluation sample may be requested.
Tape audits provide a mechanism to assess
adherence to contractual requirements and to
ensure the consistency of data reported on the
hardcopy/floppy diskettes with that generated
on the CC/MS tapes. This function provides
external monitoring of Program QC requirements
and checks ad1 of the Contractor to internal
QA procedures. In addition, tape audits enable
EPA to evaluate the utility, precision, and
accuracy of the analytical methods.
The CC/MS tape shall include raw data and
quantitation reports for samples, blanks,
laboratory evaluation samples, initial
calibrations, continuing calibration, BFB and
DFTPP associated with the case requested.
Upon request of the Administrative Project
Officer or EMSL/LV, the required tapes and all
necessary documentation shall be submitted to
EPA within seven days of notification.
E. On-Site Laboratory Evaluations
At a frequency dictated by a contract
laboratory’s performance, the Administrative
Project Officer, Technical Project Officer or their
authorized representative will conduct an on-site
laboratory evaluation. On-site laboratory
evaluations are carried out to monitor the
Contractor’s ability to meet selected terms and
Conditions specified in the contract. The
evaluation process incorporates two separate
categories: Quality Assurance Evaluation, and an
Evidentiary Audit.
1. Quality Assurance On-Site Evaluation
Quality assurance evaiuators inspect thi
Contractor’s facilities to verify the adequacy and
maintenance of instrumentation the continuity of
personnel meeting experience or education
requirements, and the acceptable performance of
analytical and QC procedures. The Contractor
should expect that items to be monitored will
indude, but not be limited to the following items.
• Size and appearance of the facility
• Quantity, age, availability, sched Wed
maintenance and performance of
instrumentatjoir
• Availability, appropriateness, and
utilization of SOPs
• Staff qualifications, experience, and
personnel training programs
• Reagents, standards, and sample storage
facilities
• Standard preparation logbooks and raw
data
• Bench sheets and analytical logbook
maintenar e and review
• Review of the Contractor’s sample
analysis/data package inspection
ures
Prior to an on-site evaluation, various
documentation pertaining to performance of the
specific Contractor is integrated in a profile
package for discussion during the evaluation.
Items that may be included are previous on-site
reports, laboratory evaluation sample scores,
Regional review of data, Regional QA materials,
CC/MS tape audit reports, results of CCS, and
data trend reports.
2. Evidentiaxy Audit
Evidence auditors conduct an on-site
laboratory evaluation to determine if laboratory
policies and procedures are in place to satisfy
evidence handling requirements as stated in
Exhibit F. The evidence audit is comprised of the
following three activities
a. Procedural Audit
The procedural audit consists of resiew and
examination of actual standard operating
procedures arid accompanying documentation for
the following laboratory operations:
41
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CLP LLser’s Guide
• sample receiving,
• sample storage, sample identification,
• sample security, sample tracking (from
receipt to completion of analysis) and
• analytical project file organization and
assembly.
b. Writteu SOPs Audit
The written 501’s audit consists of review and
examination of the written SOPs to determine if
they are accurate and complete for the following
laboratory operations:
• sample receiving,
• sample storage,
• sample identification,
• sample security,
• sample tracking (from receipt to
completion of analysis) and
• analytical project file oz anization and
assembly.
c. Analytical Prefect File Evidence Audit
The analytical project file evidence audit
consists of review and examination of the
analytical project file documentation. The
auditors review the files to deterrnixie
• The accuracy of the doctm t inventory
• The completeness of the file
• The adequacy and accuracy of the
docwx tt nunib&ng sys n
• Traceability of sample activity
• Identification of activity recorded on the
dc m
• Erroc correction metbods
3. Discussion of the On-Site Team’s Findings
The quality assurance and evidentiary
auditors discuss their findings with the
Administrative P:oject Officer/Technical Project
Officer prior to debriefing the Contractor. During
the debriefing, the auditors present their findings
and recommendations for corrective actions
necessary Lu the Contractor personneL
4. Coc ctive Action Reports For Follow-
Through to Quality Assurance and
Evidentiary Audit R’eports
Following an on-site evaluation, quality
assurance and evidentiary audit reports which
discuss deficiencies found during the on-site will
be forwarded to the Contractor. The Contractor
must discuss the corrective actions taken to resolve
the defidendes discussed during the On-site visit
and discussed in the on-site reports in a letter to
the Administrative Project Officer, Technical
Project Officer, EMSL/LV (response to the quality
assurance report) and NEIC (response to the
evidentiary report) within 14 days of receipt of
the finding or within the time agreed upon
between the Administrative Project
Officer/Technical Project Officer and the
Contractor. U SOPs are required to be written or
SOPs are required to be amended, the Contractor
must provide the SOPs to the Technical Project
Officer, EMSL/LV (quality assurance/technical
SOPs) and NEIC (evidentiary SOPs) within 30
days of receipt of the finding or within the time
agreed upon between the Administrative Project
OfficerlTechnical Project Officer and the
Contractor.
If the Contractor fails to take appropriate
corrective action to resolve the deficiencies
discussed in the on-site reports, a Contractor may
expect, but the Agency is not limited to, the
-following actions: reduction of the number of
samples s t under the contract, susper sion of
sample shipment to the Contractor, a follow-up
site visit, a full data audit, analysis of remedial
FE samples and/or contract sanction, such as a
Cure 4o Lice.
F. QualityAssurance and Data Trend
Analysis
Data submitted by laboratories are subject to
review from several aspects: compliance with
contract-required QC, useability, and full data
pa&age evaluation. Problens resulting from any
of these reviews may determine the need for a
CC/MS tape audit, an on-site laboratory
evaluation and/or a remedial laboratory
evaluation sample. In addition, QC prescibed in
the methods provides information that is
continually used by the Agency to assess sample
data quality, Contractor data quality and
Program data quality via data trend analysis.
Trend analysis is accomplished by entering data
into a computerized data base. Statistical reports
that evaluate specific anomalies or disclose
trends in many areas are generated from this
database.
Program-wide statistical results are used to
rank laboratories in order to observe the relative
42
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Ch ter VI - Program Qualify Assurance
perfr mance of each Contractor using a given
protocol against its peers. The reports are also
used to identify trends within laboratories. The
results of many of these trends analyses are
induded in overall evaluation of a Contractor’s
performance, and are reviewed to determine if
corrective action or an on-site laboratory
evaluation is indicated in order to meet the
QA/QC requirements of the contract
Contractor performance over time is monitored
using these trend analysis techniques to detect
departures of Contractor output from required or
desired levels of quality control, and to provide an
early warning of Contractor QA/QC problems
which may not be apparent from the results of an
individual case.
As a further benefit to the Program, the data
base provides the information needed to establish
performance-based criteria in updated analytical
protocols, where advisory criteria has been
previously used. The vast empirical data set
produced by contract laboratories is carefully
analyzed, with the results augmenting
theoretical and research-based performance
criteria. The result is a continuously monitored set
of quality control and performance criteria
specifications of what is routinely achievable and
expected of environmental chemistry laboratories
in mass production analysis of environmental
samples. This, in turn, assists the Agency in
meeting Its objectives of obtaining data of known
and documented quality.
C. Data Management
Data management procedures are defined as
procedures specifying the acquisition or entry,
update, correction, deletion, storage and security
of computer readable data and files. These
procedures must be in written form and contain a
dear definition for all databases and files used to
geflerate or resubmit deliverables. Key areas of
concern indude: system organization (including
personnel and security), documentation operations,
traceability and quality control.
Data manually entered from hard-copy must
be reevaluated through quality control measures
and the error rates estimated. Systems should
prevent entry of incorrect or out-of-range data and
alert data entry personnel of errors. In addition,
data entry error rates must be estimated and
recorded on a monthly basis by reentering a
statistical sample of the data entered
calculating discrepancy rates by data element.
The record of changes in the form of corrections
and updates to data originally generated,
submitted, and/or resubmitted must be documented
to allow traceability of updates. Documentation
must indude the following for each change:
• Justification or rationale for the change.
• Initials of the person making the change
or changes. Data changes must be
imp’emented and reviewed by a person or
independent of the souxce generating
the deliverable.
• Change documentation must be retained
acardlng to the schedule of the original
deliverable.
• Resubmitted diskettes or other
deliv bles must be reinspected as a part
of tie laboratories’ internal inspection
pro prior to resubmission. The entire
deliverable, not just the changes, must be
mspected.
• Tie Laboratory Manager must approve
changes to originally submitted
deliverables.
• Documentationofdatachangesmaybe
requested by laboratory auditors.
Lifecyde managelrient procedures must be
applied to computer software systems developed
by thelaboratory to be used to generate and edit
contract deliverables. Such systems must be
thoroughly tested and documented prior to
utilization..
• A software test and acceptance plan
induding test requirements, test results
and aeceptance criteria must be
developed, followed, and available in
written form..
• Sys n changes must not be made directly
to production sys is generating
ddiv bles. Changes must be made first
to a development system and tested prior
to implementation.
• Each version of the production system wi
be given an identification number, date ci
installation, date of last operation and
archived.
• System and op ations documeitstion
must be develoced and maintained for
43
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CLP Us&s Guide
each system. Doctur ntation must include • Systent operation .ind naintenance
a users manual and an operations and including documentation and training.
maintenance manual. • Database integrity, including data entry.
Individual(s) responsible for the following data updating and quality control.
functions must be identified: • Data and system security, backup and
archiving.
44
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APPENDIX A
LIST OF ACRONYMS
AA Atomic Absorption
AMIS Analytical Methods Implementation Sections
AOB Analytical Operations Branch
APO Administrative Project Officer
AR Authorized Requestor
B/N/A Base, Neutral, Acid Extractable Compounds
CCS Contract Compliance Sceerung
CEAT Contractor Evidence Audit Team
CERCLA Comprehensive Environmental Response, Compensation and U ability Act
CL? Contract Laboratory Program
CMD Contracts Man.agexr nt Division
CO Contracting Officer
CR Cost Recovery
CRQL Contract Required Quantitation Limit
DCD Data Complete Date
DDD Data Due Dat2
DR Delivery Request
DRD Data Receipt Date
EMSL Environmental Monitoring Systems Laboratory
EPA Environmental Protection Agency
ERT Environmental Response Team
ESAT Environmental Services Assistance Teams
FIT Field Investigation Team
FR Federal Register
FSCC Fused Sii Capillary Column
GC/EC Gas Chromatography/Electron Capture
CC/MS Gas Chromatography/Mass Spectrometry
HRGC High Resolution Gas Chromatography
HRMS High Resolution Mass Spectrometry
HSED Hazardous Site Evaluation Division
ICY/MS Inductively Coupled Plasma/Mass Spectrometry
45
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CLP User’s Guide
IDL 1ns -ument Detection Limit
IFB Invitation (or Bid
LCS Laboratory Control Sample
NEIC National Enforcement Investigations Center
NIST National Institute for Standards and Technology
NPM National Program Manager
NPO National Program Office
ORD Office of Research and Development
OSWER Office of Solid Waste and Emergency Response
OWPE Office of Waste Programs Enforcement
FE Performance Evaluation
PEST Pesticides
FL Packing List
QA Quality Assurance
QAP Quality Assurance Plan
QC Quality Control
QTM Quick Turnaround Method
RAS Rautine Analytical Services
REM Remedial Action Team
ROS Regional Operations Section
RSCC Regional Sample Control Center
SARA Supethind Amendments and Reauthorization Act
SAS Special Analytical Services
SDG Sample Delivery Group
SICP Selected Ion Current Profile
SIM Selected Ion Monitoring
SMO Sample Management Office
SOP Standard Operating Procedure
SOW Statement of Work
SV Semivo latjle
TAT Technical Assistance Team
TCL Target Comcound List
TIC T ntative1v Identified Compound
TPO Technical Pro}ect Officer
TR Traffic Report
VOA Volatle Organics Analysis
46
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APPENDIX B
CLP DIRECTORY
National Program Office
USEPA Analytical Operations Branch (OS-230)
401 M Street, SW
Room M-2624
Washington. DC 20460
202/382-7906 FrS 382-7906
Hans Cruinp-Weisner, Branch Odd
202/382-7906 P15 382-7906
Joan Fiske Deputy Branch Odd
202/382-3115 P15382-3115
Howard Fribush, CLP Project Offl
202/382-2239 P15 382- 9
Karen Bankert, G2 Pro t Officer
202/382-7942 F S 382-7942
Angelo Carasea, National Organic Program Manager, CLP Project Officer
202/382-7911 FIS 382-7911
Michael Huxd, National Inorganic Program Manager CL? Project Officer
202/382-7908 FiS 382-7906
Russell, McCal1igt r, CLP Project Officer
202/382-7908 FIS 382-7908
Lynn Beasley, Regional Operations Section, Acting Cnief
202/475-8607 FF5 475-8607
Patricia WiI hire, SMO Project Officer
202/382-7943 FTS 382-7943
David Eng, AD? Officer
202/382-4619 FTS 382-4619
Jim Baron, QAC
Oiuck Sands, Data Integrity Specialist
USEPA Contracts Management Divisi a (MD-33)
Alexander Drive
Research Triangle Park, NC 27111
Janet Simmons, Contract Officer, Acting Procuren t Branch Chief
919/5414081 FTS 629—4081
Marian Bernd, Contract Officer
202/382-0532 FF5 3.82-0532
Vira Burnett, Contract Officer
919/541-3045 FTS 629-3045
Larry Presnell, Contract Officer
919/541-3166 FTS 629-3166
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CLP User’s Guide
USEPA Environmental Monitoring Systems Laboratozy (EMSULV)
944 East Harmon Avenue
Las Vegas, NV 89108
Mailing Address:
P.O. Box 93478
Las Vegas, NW 89193-3478
Data To:
EMSL/LV Executive Center
944 East Harmon Ave.
Las Vegas,NV 89119
Atth: Data Audit Staff
USEPA National Enforcement Investigations Center (NEIC)
Denver Federal Center 53, E-2
P.O. Box 25227
Denve CO 80V5
3O3/ 6-511l F S 776-5111
USEPA Environmental Monitoring Systems Laboratory ( {SIiCh1dnn2+il
26 W. Martin Luther King Dr.
Cincinnati, OH 45268
4S
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Appci dix B - CL? OtTcrLory
Sample Management Office
Mailing Address:
USEPA Contract Laboratory Program
Sample Management Office
P.O. Box 818
Alexandria, VA 22313
703/557-2490 FTS 557-2490
Street Address:
Viar and Company, Inc.
300. N. Lee Street
Alexandria, VA 22314
7 133/684-5678
Sample Min ement O fize Regional Coordinatori and Analy s
_____ Coordinator Analyst
Region I Vikki Denslow Tern Shaughnessy
Region II Bret Elderd Diane Cutler
Region ifi E!e or McL n Diane Cutler
Region 1V Torn Sigler Tern Staughnessy
Region V Loren Minnich - SAS
Blake Henke - RAS Tern Sbaughnessy
Region VI E r McLean Tern Sbaughnessy
Region VII David Mack Diane Cutler
Region Vffl Monica McNeil Diane Cutler
Region IX Susan Grove Diane Cutler
RegionX David Mack Tern Shaughnessy
49
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CLI’ User .c Guide
USEPA Region I
USEFA Region I, W?vfD
J.F. Kennedy Federal Bldg
(HPC-CAN7)
Boston, MA 022Q3
(617) 573-5707 ETS 833-1707
USEPA Region I, ESD
60 Westview Street
Lexington, MA 2173
(617) 860-4300
FrS 828-6300
‘Nancy Barmakian F S 883-1797 ARCS Project Officer
Michael Hurd F l ’S 382-7908 CLI’ Adminisfraffr’c Project Officer
Deb Szaro, Moira Latailie 617/860-1312 CLI’ Technical Project Officer
David Tordoff 617/860-4362 ERCS Deputy Project Officer
‘Don Smith FF5 833-1648 FIT Regional Project Officer
Nancy Smith FF5 833-1697 NPL Coordinator
Leonard Wallace 617/860-4694 Regional R ponse Team Coordinator
‘Heidi EllIs 6171573 .5798 RegIonal Sample Control Coordinator
‘Nancy Barm.akian FF5 883-1797 REM Project Officer
John Carlson 617/860-4300 TAT Deputy Project Officer
‘Rick Leighton Ff5 883-1654 TES Project Officer, CERCLA
‘Kathy Castagna FF5 333-i609 TES Pro iect Offlcer RCRA
50
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Appendix B - CLP Direcioiy
IJSEPA Region II
USEPA Region II
26 Federal Plaza
M W York,, NY 10278
(212) 264-2525
FTS 264-2525
USEPA Region II, ESD
Woodbridge Avenue
Building 209
Edison ,, NJ 08837
(201) 321-6754
FrS 340-6754
‘Shaheer Alvi PTS 264-2221 ARCS Project Officer
Angelo Carasea FTS 382-7911 CLP Adnrini trat ’e Projei Officer
Lisa Gatton FF5 340-6676 CLP Tedinical Project Officer
Michael Polito Fl ’S 340-6652 ER(3 Deputy Project Officer
Amy Brothu Fl’S 906-6802 FIT REgional Project Officer
‘Ben Conetta - Fl’S 264-66% NPL Coordinator
Richard Salkie FTS 340-6657 Regional R ponse Team Coordinator
Philip Guarrala Fl’S 340-6997 RegIonal Sample Conb ol Coordinator
Shaheer Alvi Fl’S 264-2221 REM Project Offl
Michael Poll to Fl’S 340-6652 TAT Deputy Project Offi
‘Cathy Moyik Fl’S 264-8123 TES Project Officer, CERCLA
‘Derval Thon as Fl’S 264-1829 TES Project Officer, RCRA
51
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CLP User’s Guide
USEFA Region III
‘USEPA Region Ill,
Superfund Branch
841 Chestnut Street
Philadelphia, PA 19107
(215) 597-0992
FTh 597-0992
USEPA Region Ill, CRL
839 Bestgate Road
Annapolis, MD 21401
(301)266-9180
‘Fran Burns F1 597-4750 AR Project Officer
‘Roy Schrock FIS 597-0913 AR Project Officer
Angelo Carasea FTS 382-7911 CL I ’ Administrative Project Officer
S tevie Wiiding }TS 266-9180 CL I’ Technical Project Officer
‘Steve Jarvela FIS 597-7915 ER Deputy Project Officer
‘Bob VanFossen FIS 597-3152 ER(3 Deputy Project Officer
‘Tony Dappafor Fl ’S 597-3153 FIT Regional Project Officer
‘Margaret Jennis FTh 597-34i7 NPL Coocdinator
Dennis Carney Fl ’S 597-0992 Regional R ponse Teaz Coordinator
Coileen Walling 30 1J266-9180 Regional Sanaple Con ol Coordinator
BW Hagel F S 597-3435 REM Project Officer
‘Bob VanFossen FTS 597-3152 TAT Deputy Project Officer
‘Elaine Speiwak Fl’S 597-8183 TES Pro t Officer, CERCLA
‘Jeff Barnett FL’S 597-6688 TES Pro t Officer, RCRA
52
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Appendix B - CLP Dire ory
USEPA Region IV
USEPA Region IV
Superfund Branch
345 Courtland Street., N.E.
Atlanta, GA 30365
(404) 347-4727
Fl ’S 257-4727
USEPA Region IV, ESD (ASB)
Analytical Support Branch
College Station Road
Athens, GA 30613
(404) 546-3111
F S 250-3111
Doug Thompson FIS 257-2234 ARCS Project Officer
Howard Fri bush FF5 382-2239 CLP A4ministrative Projeci Offic.rr
Torn Bennett F l ’S 250-3112 CU’ Technical Project Officer
•Fred Stroud Fl’S 257-3931 ERCS Deputy Project Officer
Narindar Kurnar FIS 257-5065 FIT Regional Project Officer
Deborah Vaughn-Wright Fl’S 257-5065 NPL Coordinator
Doug Lair Fl’S 257-3931 Regional Rc ponse Team Coordinator
Bill Bokey Fl’S 353- O Regional Sample Conb ol Coordinatrr
Ken Meyer Fl’S 257-2234 REM Project Offi
Carol Monell Fl’S 257-3931 TAT Deputy Project Officer
‘Doug flxnnpson F l’S 257-2234 TES Project Officer, CERCLA
Rowena Sheffield Fl’S 257-2234 TES Project Officer, RCRA
53
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CLP User’s Guide
USEPA Region V
USEI’A Region V, ESD
536 S. aark Street
Tenth Floor, 5SCRL
Chicago, IL 60605
vrs 353-3808
USEPA Region V, WMD
230 S. Dearborn Street
12th Floor (HR-12)
Chicago, IL 60604
(312) 886-7579
FTh 886-7579
‘Susan Heston FF5 886-9553 ARCS Project Offi
‘Stephen Nathan FTS 886-54% ARCS Project Officer
CarI Norman FF5 886-5495 ARCS Project Offi
Russell McCallisfer F S 382-2239 CLP Administrative Proj t Officer
Pat Churllla FTS 353-2313 CL? TedlnIr2l Project Officer
Jackie Van Bo€se FIS 353-1908 ERCS Deputy Project Officer
Charles Brasher FF5 353-7625 ERCS Deputy Project Officer
Gail Nabasny FF5 353-1056 FIT Regional Project Officer
‘Jeanne Griffin FF5 886-3007 NFL Coordinator
‘Maiy Gade FFS 353-9773 Regional Response Team Coordinator
Jan Pels FF5 353- ’2O Regional Sample Confrol Coordina±or
Gail Nabasny FF5 353-1056 R { Project Offl
Steve Faryan FF5 353-9351 TAT Deputy Project Officer
‘Eva Howard FF5 886-7274 TES Project Officer, CERCLA
‘Lorraine Ko ik FF5 353-6431 TES Project Officer, C CLA
‘Fred Norling FF5 8364510 TES Project Officer, RCRA
>4
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Appendix B - CLP Direc org
US EPA Region VI
USEPA Region VI Laboratozy
10625 FalistoneRd
Houston ,TX 77099
(713) 983-2100
FTS 730-2100
USEPA Region V I
First Interstate Tower
1445 Ross Avenue
Dallas, TX 75202
(214) 665-6491
F l ’S 255-6491
Julie Brown Fl’S 255-6720 ARCS Project Ofñcer
Michael Hurd RS 382-7908 CLP Administrath’e Proj f Officer
‘Wililam (B.J.) Verrett FTS 730-2139 CLP Ter-hni ’1 Project Officer
Chris Petersert Fl ’S 255-2270 ERCS Deputy Project Officer
Ed Sierra F l’S 255-6491 FiT Regional Project Officer
Jana Harvill Fl’S 255-6740 NPL Coordinator
Charles Gazda Fl ’S 255-2270 Regional Response Team Coordinator
Jim Mu]iirts Fl’S 255-2270 Regional Response Team Coordinator
Myra Perez Fl’S 526-9425 Regiocal S ple Coutrol Coordln.a±zx
Eve Boss Fl’S 255-6720 REM Project Officer
Chris Petersen Fl’S 255-2270 TAT Deputy Project Officer
Karen Witten Fl’S 255-6720 TES Project Officer, C CLk
Rena McCuxg Fl’S 255-6780 TES Project Officer, RCRA
55
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Appcndix B - CLP E> c cr
USEPA Region VIII
USEPA Region VIII
999 18th Street, Suite 500
Denver, CO 80202-2405
FF5 330-1720
(303) 293-1720
‘Denver Federal Center
Building 5
WI Entrar e, 2nd Floor
Denver, CO 80 5
FF5 776-5064
(303) 236-5073
Montana EPA Office
301 South Park
P.O. Drawer 10096
Helena, ? ff 59626
FF5 585-5414
(406) 4-49-5414
Craig Hargreave FF5 330-1187 ARCS Project Officer
Jeff M.ashburn FTS 330-7156 ARCS Project Offl
Ru.ssdfl McCallister FT$ 382-7908 CLP Mmin straHve Proj t Officer
Steve Ca]lio FF5 330-7511 CLP TedutIcalProje Officer
Mika Zimmerman FrS564-7081 ERCS Deputy Project Officer
Gerald Snyder FF5 330-7504 FIT Regional Project Officer
Paul Arell FF5 330-7398 NPL Coordinathr
John Giedt FIS 330-7142 Regional Response Team Coordinator
Floyd Nichols FiS 330-7167 Regional Response Team Coordinator
Tanuxty 1Cm&. F l ’S 330-7507 Regiorul Sample Ccnirol Coordinabx
Greg Hargreaves FTS 330-1187 REM Project Ofi3
ru n Knoy FF5 330-7162 TAT Deputy Project Officer
Sam Marqu Fl’S 330-7151 TES Proect Officer, aRCLA
RoUand Leth FF5 564-1516 TES Project Officer, R( SA
57
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CLP User’s Guide
USEPA Region LX
USEPA Region IX, OPM, P.3-2
1235 Mission Street
San Francisco, CA 94103
Fl-S 556-6458
(415) 556-6458
FAX (415) 556-6874
Laboratory
USEPA Region IX
944 East Harn n Avenue
Las Vegas, NV 89119
Peter Rubenstein Fl-S 454-0307 ARCS Project Officer
Karen Bankert t TS 382-7942 CLP Mminisfrat ve Project Officer
Kent Kitchingmaxt Fl-S 556-5033 CL? Technical Project Officer
Chris Weden Fl-S 454-8132 ERCS Deputy Project Officer
Douglas Fra.zer Fl-s 454-7305 FIT Regional Project Officer
Lisa Nelson Fl-s 454-7701 NPL Cooi dinator
Kathleen Shii1 min Fl-S 454-7745 Regional R ponse Team Coordinator
RobbyHedeen 415/744- 1244 Region Sample Control Coordinathr
Rob Stern Fl-S 454-7406 REM Project Officer
William Lewis Fl-S 454-7464 TAT Deputy Project Officer
Judy Walker Fl-S 454-0748 TES Project Officer, CERCLA
Lucy )vflenar Fl-S 454-8386 TES Project Officer, RCRA
58
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Appendix B — CLP Directory
US EPA Region X
USEPA Region X, ESD
1200 Sixth Avenue
M/SES-095
Seattle, WA 98101
FTS 399-1200
(206) 442-1200
Laboratory
‘USEPA Region X
P.O. Box 549
Manchester, WA 98353
FTS 399-0370
(206) 442-0370
Joanne LaBaw FF5 399-2594 ARCS Project Officer
Howard Fri bush FTS 382-2237 CLP Administrative Project Officer
‘Gerald Muth FF5 399-0370 CU’ Technical Project Officer
Jeff Webb FTS 399-1196 ERCS Deputy Project Officer
William Longston FTS 399-11% ERCS Deputy Project Officer
John Osborn FTS 399-0837 FIT Regional Project Officer
David Bennett FTS 399-2103 NPL Coordinator
James Everts FT 399-1196 Regional R ponse Team Coordinator
Carolyn Wilson FTS 399-1632 Regional Sample Control Coordinator
Joanne LaBaw FF5 399-2594 REM Project Officer
Carl Kitz FTS 399-1196 TAT Deputy Project Officer
Mike Slater FFS 399-0455 TES Project Officer, CERCLA
Shirley Towns Fl ’S 399-2586 TES Project Officer, RCRA
59
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CLP User’s Guide
Miscellaneous Information
Cooler Returns
T. Head and Company
950 Herndon Parkway
Suite 230
Herndon, VA 22070
703/473-3886
E T Edison
USEPA Environmental Response Branch
GSA Raritan Depot
Woodbridge Avenue
Edison, NJ 08837
PTS 340-6649, 6689, 6743
60
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App ’ndLx B - CLP Directory
Regional Sample Control Centers
Regional Sample Control
Address Coordinator Phone Nun ber
USEPA Region I, WMD Heidi Ellis 617/573-5798
J.F. Kennedy Federal Bldg. FTS 833-1798
Boston, MA 02203
USEPA Region II, ESD Philip Guarraia 201/321-6997
Woodbridge Ave. Bldg. 209 FTS 340-6997
Edison 1 NJ 06837
USEPA Region In, CRL Colleen Walling 301/266-9180
839 Bestgate Rd.
Annapolis, MD 21401
USEPA Region IV, ESD Bill Bokey 404/546-3300
Env. Compliance Branch Fl ’S 250-3300
College Station Road
Athens, GA 30613
USEPA Region V,ESD Jan Peis 312/353-2720
536 S. Clark St. FFS 353-2720
Tenth Floor, CRL
a dcago, IL 60605
USEPA Region VI Myra Perez 713/953-3425
Monterey Park P1. Bldg. C Fl ’S 526-9425
6606 Hornwood Dr.
Houston,. 1 ( 77074
USEPA Region VII, ESD Nicole Roblez 913/236-3881
25 Funston Rd. FTS 757-3881
Kansa.s City, KS 66115
USEPA Region VIII Tammy Kozak 303/294-7507
999-18th St. Fl’S 330-7507
12th Floor
Denver, CO 80202
USEPA Region IX ,, OPM Ro’obie Hedeen 415/744-1244
215 Fremont St.
San Frandsco, CA 94105
USEPA Region X. ESD Carolyn Wilson 2C /4424632
1200 Sixth Ave. E/S 095 FTS 3994632
Seattle, WA 98101
61
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CLP Users Guide
Regional Technical Project Officers
Region! Deb Szaro, Moira Lataille 617/860-4312
Region U Lisa Gatton FTS 340-6676
Region Ill Stevie Wilding FIS 266-9180
Region IV Torn Bennett FIS 250-3112
Region V Pat Qturilla F S 353-2313
Region VI William (B.J.) Verrett F S 730-2139
i egion VI I Larry Marchin FIS 757-3881
Region VU! Steve CalIio Fl ’S 330-7511
Region D( Kent Kitchingrnan Fl’S 556-5033
Region X Gerald Muth FTS 399-0370
62
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APPENDIX C
REFERENCES
NOTE: The references in this appendix are supplied for general information purposes and do not
necessarily represent methods or procedures utilized in the CLI’.
Analytical References
American Public Health Association, American Water Works Association, Water Pollution Control
Federation. Standard Methods for E mination of Water and Wastewater. 14th ed. rev. 1975.
American Society for Testing and Materials. Annual Book of ASTM Standards. Part 31, Standard
D3223-73; 1976 (p. 343).
Bishop, J.N. Mercury in Sediments. Ontario Water Resources Comm. Toronto: 1971.
Brandenberger, H.; Bader, H. The Determination of Nanogram Levels of Mercury in Solution by a
flameless Atomic Absorption Technique. Atomic Absorption Newsletter 6:101; 1967.
Environmental Monitoring and Support Laboratory, U.S. Environmental Protection Agengy. Interim
Methods for the Sampling and Analysis of Priority Pollutants in Sediments and Fish Tissue. Cincinnati:
October 1980 (rev.).
Environmental Monitoring and Support Laboratory, U.S. Environmental Protection Agency. User’s
Guide for the Continuous flow Analyzer Automation System. Cincinnati: 1981.
Garbarino, J.R.; Taylor, H.E. An Inductively-Coupled Plasma Atomic Emission Spectrornetric
Method for Routine Water Quality Testing. Applied Spectroscopy 33:3; 1979.
Goulden, P.D.; Afghan, B.K. An Automated Method for Determining Mercury in Water. Technicon.
Adv. in Auto. Arialy. 2; 1970 (p. 317).
Hatch, W.R.; Ott, W.L Determination of Sub-Microgram Quantities of Mercury by Atomic
Absorption Spectrophotometry. Analytical Chemistry 402085; 1968.
Kopp, J.F.; Longbottom, M.C.; Lobring, LB. Cold Vapor Method for Determining Mercury. AWWA
64:20; January 1972.
Martin, T.D.; Kopp, J.F.; Ediger, RD. Determining Selenium in Water, Wastewater, Sediment and
Sludge by flameless Atomic Absorption Spectroscopy. Atomic Absorption Newsletter 14:109; 1975.
Martin, Theodore D. Inductively Coupled Plasma-Atomic Emission Spectrometric Method of Trace
Elements Analysis of Water and Waste. Method 200.7. ModifIed by CL? Inorganic Data/Protocol
Review Committee.
Office of Solid Waste and Emergency Response, U.S. Environmental Protection Agency.
Modification (By Committee) of Method 3050. SW-846, 2nd ed. Test Methods for Evaluating Solid
Waste; July 1982.
Organochiorine Pesticides and PCBs, Method 608; 2,3,7,8-TCDD, Method 613; Purgeables
(Volatiles), Method 624; Base/Neutrals, Adds and Pesticides, Method 625; Federal Register 44(233),
December 3, 1979 (pp. 69501, 69526, 69532, 69540).
Owerbach, Daniel. The Use of Cyanogen Iodide (CNI) as a Stabilizing Agent for Silver in
Photographic Processing Effluent Sample. Photographic Technology Division, Eastman Kodak
Company. Rochester, New York.
63
-------
CLP User’s Guide
Technicon Industrial Systems. Operation Manual for Technicon Auto Analyzer IIC System.
Technical Pub. No. TA9-0460-O0. Tarrytown New York: 1980.
U.S. Environmental Protection Agency. Handbook for Analytical Quality Control in Water and
Wastewater Laboratories. USEPA -600/4-79-01 9 .
U.S. Environmental Protection Agency. Handbook for Monitoring Industrial Wastewater. USEPA
Technology Transfer; 1973.
US. Environmental Protection Agency. Methods for Chemical Analysis of Water and Wastewater.
USEPA Technology Transfer; 1974.
US. Environmental Protection Agency. Methods (Torn Chemicaj Analysis of Water and Waste.
USEPA-600/4-79-02; March 1979.
US. Environmental Protection Agency. Procedures Manual for Groundwater Monitoring at Solid
Waste Disposal Facilities. USEPA 530/SW-611; 1977.
Winefordner, J.D. Trace Analysis: Spectroscopic Methods for Elements. Chemical Analysis 46: 41-
42.
Winge, R.K.; Peterson, V.J.; Fassel, V.A. Inductively Coupled Plasma-Atomic Emmission
Spectroscopy Prominent Unes. USEPA-600/4-79-017.
Wise, RH.; Bishop, D.F.; Williams, RT.; Austerri, B.M. Gel Permeation ChromatogTaphy in the
CC/MS Analysis of Organics in Sludges. Municipal Environmental Research Laboratory, U.S.
Environmental Protection Agency. Cincinnati.
Quality Assu.rance References
American Chemical Society Committee on Environmental Improvement, and Subcommittee on
Environmental Analytical Chemistry, “Guidelines for Data Acquisition and Data Quality Evaluation
in Environmental Chemistry”, Analytical Chemistry, Volume 52, Number 14, December 1980.
Environmental Monitoring Systems Laboratory, US. Environmental Protection Agency, Analytical
Reference Standards and Supplemental Data: The Pesticides and Industrial Chemicals Repository,
EPA-600/4-84 -082, October 1954.
Environmental Protection Agency, “Guidelines Establishing Test Procedures for the Analysis of
Pollutants Under the aean Water Act; Final Rule and Interim Final Rule and Proposed Rule”, 40 CFR
Part 136, Federal Register, Vol. 49, No. 209., pp 43234-43442, October 26, 1984.
Fisk, J.F. and Manzo, S.M. “Quality Assurance/Quality Control in Organics Analysis”, Proceedings
from the Water Pollution Control Federation Meeting, May 1986.
Health Effects Research Laboratory, US. Environmental Protection Agency, Manual of Analytical
Methods for the Analysis of Pesticides in Humans and Environmental Samples, EPA-600/8-80-036, June,
1980.
Health Effects Research Laboratory, US. Environmental Protection Agency, Manual of Analytical
Quality Control for Pesticides and Related Compounds In Human and Environmental Samples-Second
Revision, EPA-600/2-8 1-059, April 1981.
Laidlaw, R I -I., “Document Control and Chain of Custody Considerations for the National Contract
Laboratory Program,” Quality Control in Remedial Site Investigations: Hazardous and Industrial
Solid Waste Testing, Fifth Volume, ASTM STI ’ 925, C.L. Perket, ed., American Society for Testing and
Materials, Philadelphia, 1986.
Moore, J.M. and Pearson, J.G. Quality Assurance Support for the Superfund Contract Laboratory
Program”, Quality Control in Remedial Site Investigation: Hazardous and Industrial Solid Waste
Testing. Fifth Volume, ASTM STP 925, CL. Perket, ed., American Society for Testing and Materials,
Philadelphia, 1986.
-------
Appendix C - References
Office of Monitoring Systems and Quality Assurance, US. Environmental Protection Agency
interim Guidelines and Specifications for Preparing Quality Assurance Project Plans”, QAMS-005/80
December 1980.
Office of Solid Waste and Emergency Response, U.S. Environmental Protection Agency, Test
Methods for Evaluating Solid Waste, Third Edition, SW-846, November 1986.
US. Environmental Protection Agency. Guidelines Establishing Test Procedures for the Analysis of
Pollutants Under the aean Water Act; Final Rule and Interim Final Rule and Proposed Rule. 40 CFR
Part 136. Federal Register 49(209); October 26, 1984 (pp. 43234—43442).
Safety References
Committee on Chemical Safety. Safety in Academic Chemistry Laboratories. American Chemical
Society Publications. 3d ed. rev. 1979.
Department of Health, Education and Welfare, Public Health Service, Center for Disease Control,
National Institute for Occupational Safety and Health. Carcinogens-Working with Carcinogens. Pub.
No. 77-206; August 1977.
Occupational Safety and Health Administration. OSHA Safety and Health Standards, General
Industry (29 CFR 1910). OSHA 2206. rev. Januaiy.1976.
Wallace, hA.; Fulkerson, W.; Shults, W.D.; Lyon, W.S. Mercury in the Environment-The Human
Element. Oak Ridge National Laboratory. ORNL/NSF-EP-1; January 1971 (p. 31).
Sampling References
Environmental Response Team, US. Environmental Protection Agency. Field Monitoring and
Analysis of Hazardous Materials. EPA Training Manual. Course No. 165.4. Cincinnati: 1980.
Huibregtse, KR.; Moser, J.H. Handbook for Sampling and Sample Preservation of Water ar
Wastewater. USEPA-600/4-76.049; 1976.
Municipal Environmental Research Laboratory, US. Environmental Protection Agency. Samplers
and Sampling Procedures for Hazardous Waste Streams. EPA-600/280-018. Cincinnati: 1980.
National Enforcement Investigations Center. Enforcement Considerations for Evaluation of
Uncontrolled Hazardous Waste Sites by Contractors. EPA Office of Enforcement Denver 1980.
Office of Solid Waste and Emergency Response, U.S. Environmental Protection Agency, Sampler’s
Guide for the Contract Laboratory Program, First Edition, , December 1990.
Olson, D.M.; Berg, E.L.; Christensen, R.; Otto, H.; Ciancia, J.; Bryant, C.; Lair, M.D.; Birch, M.;
Keffer, W.; DahI, T.; Wehrier, T. Compliance Sampling Manual. Office of Water Enforcement, EPA
Enforcement Division, Compliance Branch; 1977.
Weber, C l. Biological Field and Laboratory Methods for Measuring the Quality of Surface Waters
and Effluents. USEPA-670/4-73-OQI; 1973.
Shipping References
Federal Express Corporation, Hazardous Materials Department. Telephone: 1-800-235-5392.
U.S. Department of Transportation. A Guide to the Federal Hazardous Materials Transportation
Regulatory Program; 1983.
U.S. Department of Transpor:ation. U.S. Department of Transportation Rezulabons. 49 CF , Parta
100-199; October 1, 1978.
65
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A
AMIS 3
Aitalytical data 1-8, 17-23, 27-31, 34-43
Analytical Methodologies
Development 18
Improverr t 18
Analytical Operations Branch (see AOB)
Analytical Standards Traceability
Requirements 38
AOB3
APO 3, 4, 27, 32-36
C
Case Number 20,23
CCS 5, 28-31, 39, 41
CERCLA 1
Chain-of--custody 4,24-26,30
Chemical Standards 38, 39
LP6 -
Cients I
Non-Superfund dients 1,7
Objective and Orientation I
Structure 1,2
User comrrnmityl
Usersi
CMD 33-35
CO 33-35
Comprehensive Environxnentai Response,
Compensation, and Liability Act (see
CERCLA)
Contract Compliance Screening (see CCS)
Contract DeIiv y Requirements 7
Contract Laboratory Program (see CLP)
Contracting Officer (see CO)
Contracts Management Division (see C.MD)
Cost Recovery 29,31
INDEX
E
EMSL/LV3, 4,18, 28,31-42
Enfoiter it 30
Environmental Monitoring Systems
Laboratory in Las Vegas (see
EMSL/LV)
Environmental Services Assistance Team
(see ESAT)
EPA
Regions I
Evidentiary Audit
Analytical Project File Evidence Audit
42
Procedural Audit 41
Written SOP $ Audit 42
G
GC/MS Tape Audits 41
H
Hazardous Site Evaluation Division (see
HSED)
High Concentration RAS
1nor nic 6,16
Oi anic 6,7,12
HSED 3
tFB 33, 34
Ircrganic RAS 8
High Cor entration 6,16
Low Coi entration Drinking Water 6,
14
Multi-Media, Multi-Concentration 6, 7,
13
Invitation for Bid (see LFB)
0
Data package 1, 7, 18, 27-34, 39-41
Data reporting 18, 23, 29, 30,38,39
Data review 3,31, 32, 39, 41
Data Review Request 32
Data usability 31, 32, 37, 39, 42
Dioxin/Furan RAS 6, 8,16
L
Laboratory 1-8, 17-43
Laboratory capacity 19,20-23,33
Laboratory Evaluation Samples 40
laboratory selection 33
Laboratory Selection Process 33
Laboratory Startup 3-4
Liquidated damages 7
Low Concentra on Drinking Water RAS
Inorganic 6, 14
Oiganics 6,10
Volatile Orgarucs Only 6. 11
67
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CLP User’s Guide
National Enforcement Investigations
Center (see NEIC)
National Program Office (see NPO)
NE 4, 18,24, 26,30,34-37,42
NPM 3
NPO 3-5 , 18, 20, 23, 27,28,33-36
0
Office of Add Deposition I
Office of Solid Waste I
Office of Solid Waste and Emergency
Response (see OSWER)
Office of Waste Programs Enforcement 31
Office of Water 1
Organic R.AS 8
High Concentration 6,7, 12
Low Concentration Drinking Water 6,
10
Low Concentration Drinking Water for
Volatiles Only 6,11
Multi-Media, Multi-Concentration 6, 7,
9
OSWER 3
P
PE Samples 33,34,35
Performance Evaluation Samples (see PE
Samples)
Pmblent Resolution
Analytical data 27
APO/TPO/SMO/Laboratory
Communication 34
CuxeNotice35
First data package 34
P Iormance 35
Sample Analysis 26
Sample Shipping 26
Show Cause Notice 35
Program information 29
Program Utilization
R.AS I9
SAS 21
0
QA 3,4, 8, 17,31-43
QA Coordinator 3
QA.P 37
QC3,7,8,17, 18,31,35—43
Quality Assura nce Plan (see QAI’)
Quality Control (see QC)
A
RAS6-8,17-24,26,3l
Case Nunther 20,23
Dioxin/Furans 6,8
Initiating a RAS Request 19
Inorganic 6,8, 13, 14, 16
Laboratory selection 20
Lead-time required 19
Organic 6, 8-12, 20
Scheduling 19,20
Traffic Report 23,26
User ki owledgeo(pmtocol 20
R .A I
Regional Organic/Inorganic Allocation
Systent23
Regional Sample Control Center (see
RSCC)
Reports
Laboratory Sample Backlog Status
Report 28
Regional Sample Backlog Status
Report 22, 29
Resource Conservation and Recovery Act
(see R .A)
Routine Analytical Services (see RAS)
RSCC 1,5,19-29,32
S
Sample Delivery Group (see SDG)
Sample Management Office (see SMO)
Sample Number 24
Sample Packaging 25
Coolers 5,25-28
Sample Shipping 26
Coordination 26
Problent Resolution 26
Return of coolers 26
Sample Tag 24
SARA 1
SAS 4,6-8, 17, 18, 21-27, 31, 32
All SAS 7
Changing a SAS request 22
alent Request Form 21
Delivery requirements 18
Eligible laboratories 8
Fast turnaround 17
Initiating a SAS Request 21
Laboratory availability 8, 17
Laboratory selection 8,22
Lead—time requirements 21
Packing List 23, 26
RASpIusSAS7
SAS Number 22,23
68
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Index
ScF dullng 22
User provided analytical protocol 22
SAS Numbe 22.23
SAS Packing Ust 23, 26
Scheduling
RAS 19,20
Regional Organic/Inorganic Allocation
System 23
SAS 8, 17, 22
DG 7, 28, 30,40
Shipment Management Program 5,28
Site evaluation 34, 35, 41, 42
SMO 1,4,8,18-41
SMO Coordinator 19
SOPs 34, 36, 37, 38, 41, 42
SOW 20, 21
Special Analytical Services (see SAS)
Standard Operating Procedures (see SOPs)
Statement of Work (see SOW)
States 1
Superfund An dzri its and
Reauth)rjzatjon Act (see SARA)
T
T hnicaI Project Officer (see T1’O)
TPO 4 , 20, -29, 34-36
Traffic Report 23,26
69
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Attachment F
Region I Short Sheets and EPA CLP Information Sheets
-------
USEPA
CONTRACT LABORATORY PROGRAM
SHORT SHEETS
-------
SOW SHORT SHEET GUIDELINES
The following is a description of the categories included in the
Statement of Work (SOW) Short Sheets.
• Title: Name of the document as it appears on the cover page
of the document.
• Document Number: Number of the document as it appears on
the cover of the document. Not all SOWs have associated
document numbers. A SOW may be referenced by either the
document date or the document number, depending on which one
is applicable.
• Document Date: Date the document was initially issued
according to the cover page of the document. Not all SOWs
have associated document dates. A SOW may be referenced by
either the document date or document number, depending on
which one is applicable.
• Effective Dates: Range of dates for which the Regions can
submit samples for analysis under a particular SOW. If
contracts have not been awarded yet, then the expected award
date is listed.
• Concentration: Range of sample concentrations for which the
SOW is applicable, such as low to medium, high, or > 20
mg/kg.
• Data Turnaround: Number of days the laboratory has to
submit the complete data package after sample receipt.
• Matrices: Sample matrices for which the SOW is applicable,
such as aqueous, soil, sediment, multi—phase, etc.
• Significant Features: Information about the SOW which
distinguishes it from other SOWs. This section highlights
critical items such as holding times, concentrations, and
matrices which may be different.
• Revisions/Modifications: Revisions from the previous SOW
which may significantly affect data useability.
• Recommended Uses: Explanation of appropriate Superfund
activities for which the SOW may be utilized.
• Analytes/CRQLs: References Attachment I which lists the
parameters included in the analysis and their respective
CRQLs or CRDLS. The aqueous and soil CRQLs and CRDLS are
listed. “Notes” are provided at the bottom of each
Attachment to document deviations from the CRQLs and CRDLs
listed.
-------
AVAILABLE SHORT SHEETS
TiTLE DOCUMENT DATE SHORT SHEET
OR NUMBER REVISION NUMBER
USEPA Contract Laboratory Program 2188 1.0
Statement of Work for Organic Analysis
Multi-Media, Multi-Concentration
USEPA Contract Laboratory Program OLMO1 .0 1.0
Statement of Work for Organic Analysis
Multi-Media, Multi-Concentration
USEPA Contract Laboratory Program OLMO1.9 3.0
Statement of Work for Organic Analysis
Multi-Media, Multi-Concentration
USEPA Contract Laboratory Program OLMO2.1 2.0
Statement of Work for Organic Analysis
Multi-Media, Multi-Concentration
USEPA Contract Laboratory Program 9/88 1 0
Statement of Work for Organic Analysis
Multi-Media, High-Concentration
USEPA Contract Laboratory Program 7/88 1.0
Statement of Work for Inorganic Analysis
Multi-Media, Multi-Concentration
USEPA Contract Laboratory Program ILMO1.0 1.0
Statement of Work for Inorganic Analysis
Multi-Media, Multi-Concentration
USEPA Contract Laboratory Program ILMO2. 1 2.0
Statement of Work for Inorganic Analysis
Multi-Media, Multi-Concentration
USEPA Contract Laboratory Program ILMO3.0 2.0
Statement of Work for Inorganic Analysis
Multi-Media, Multi-Concentration
USEPA Contract Laboratory Program IHCO1.2 1.0
Statement of Work for Inorganic Analysis
Multi-Media, High-Concentration
USEPA Contract Laboratory Program DFLMO1.2 3.0
Statement of Work for Analysis
of Polychlorinated Dibenzo-p-Dioxins (PCDD)
and Polychiorinated Dibenzofurans (PCDF)
Multi-Media, Multi-Concentration
1
-------
AVAILABLE SHORT SHEETS (continued)
TITLE DOCUMENT DATE SHORT SHEET
OR NUMBER REVISION NUMBER
Superfund Analytical Methods for Low 10/92 2.0
Concentration Water for Organic Analysis
USEPA Contract Laboratory Program 6/93 2.0
Water Quality Parameters in
Multi-Concentration Water (WQP)
USEPA Contract Laboratory Program ILMO4.0 0.0
Statement of Work for Inorganic Analysis
Multi-Media, Multi-Concentration
USEPA Contract Laboratory Program OLMO3.2 0.0
Staement of Work for Organic Analysis
Multi-Media, Multi-Concentration
2
-------
1TILE: USEPA CONTRACI LABORATORY PROGRAM
STATEMENT OF WORK FOR ORGANIC ANALYSIS
MULTI-MEDIA, MULTI-CONCENTRATION
DOCUMENT NUMBER: Not Applicable
DOCUMENT DATE: February 1988
EFFECTIVE DATES: January 20, 1989 through September 10, 1991
CONCENTRATION: Low to Medium
DATA TURNAROUND: 35 Days
MATRICES: Aqueous/Soi/Sediment
SIGNIFICANT FEATURES
• The parameters include volatile, semivolatile, and pesticidelPCB compounds.
• Volatiles and seniivolatiles are analyzed by GCIMS; pesticideslPCBs are analyzed by GCIECD.
• Major Tentatively Identified Compounds (flCs) are reported for GCIMS analyses.
• Second column confirmation by GCIECD is required for all pesticidesfPCBs. PesticidesfPCBs which
are identified by GC/ECD at concentrations above 10 ngluL are confirmed by GCIMS analysis.
REVISIONSIMODWICATIONS
The 9/88 and 4/89 revisions to the 2/88 SOW do not significantly affect data useabiity.
RECOMMENDED USES
This Routine Analytical Services (RAS) method is recommended for broad spectrum analysis to
define the nature and extent of potential site contamination during SSI, LSI, and RI/FS activities. This
method is suitable when a thirty five day turnaround for results is adequate. It is recommended for
samples from known or suspected hazardous waste sites where potential contamination may be present
at significant risk levels.
* Sediment samples with high moisture content should be solicited as RAS + SAS (Special
Analytical Service) in order to achieve the CRQLs.
ANALYTES/CRQLc
The parameters included in the analysis and the Contract Required Quantitation Limits (CRQLs)
are listed in Attachment 1.
Revision 1.0
-------
ATrACHMENT I (page 1 of 3)
USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR ORGANIC ANALYSIS
MULTI-MEDIA, MULTI-CONCENTRATION
FEBRUARY, 1988
TARGET COMPOUND LIST - VOLATILES
A’
Co npound CRQL
(ug/L,ppb)
LowSoil
cRQL
(ug/ g,ppb)
•. .. 10
10
10
10
10
10
10
10
Chloride 5
5
... 10
10
5
5
5
5
5
5
5
5
5
5
5
5
10
10
S
5
Tetrachloride 5
5
10
10
S
5
Conipound
‘
•. A4üeâ ill.
• 5 ”CRQL
(u b)
Low Soil
CRQL
g g,ppb)
la-Dichioropropane
s
cia-l,3-Dichloo@ropene
5
S
Trichioroethenc.. .
5
5
Dibromochioromethane
5
5
‘1,1,2-Trichioroethane
5
5
Benzece
5
5
trans-1,3-Dicb loropropene
5
5
Bronioforni
4-Methyl-2-penranone
10
10
2-Hexanone •. ..
10
10
Tetrachioroethene
5
5
Toluene ‘. .
5
5
1,1,2,2-Tetrachloroethene
5
5
ChEoroben.zene
5
5
Ethyl Benzene
5
5
Styrene.. 5
S
Total Xylenee f.
5
5
• THE SAMPLE-SPECIFIC CRQLs FOR SOIL SAMPLES WILL BE ADIUSTED FOR PERCENT MOISTURE AND WILL BE
HIGHER THAN THOSE USTED ABOVE.
• MEDIUM LEVEL SOIL CRQL = 125 x AQUEOUS CRQL REPORTED IN UGIKG.
Revision 1.0
-------
TiTLE: USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR ORGANIC ANALYSIS
MULTI-MEDIA, MULTI-CONCENTRATION
DOCUMENT NUMBER: OLMO1.O
DOCUMENT DATE: Not Applicable
EFFECTIVE DATES: September 28, 1990 through February 1994
CONCENTRATION: Low to Medium
DATA TURNAROUND: 14 Days or 35 Days
MATRICES: Aqueous/Soil/Sedimeat -.
SIGNIFICANT FEATURES
• The parameters include volatile, semivolalile, and pesticide/PCB compounds.
• Volatiles and scmivolatilcs arc analyzed by GCIMS, pcsticidcslPCBs are analyzed by GCIECD.
• Major Tentatively Identified Compounds (TICs) are reported for GCIMS analyses.
• Second column confirmation by GCFECD is required for all pesticideslPCBs. Pesticides/PCBs which
are identified by GCIECD at concentrations above 10 ng/uL are confirmed by GCIMS analysis.
REVISIONS(MODIFICATIONS
The following is a list of the significant changes from the 2/88 SOW that arc incorporated in the
OLMO1.0 SOW:
• Selected volatile CRQLs have been raised; pesticide/PCB low soil CRQLS have been lowered; and
selected pesticidelPCB aqueous CRQLS have been changed.
• Target Compound List (TCL) changes include the elimination of vinyl acetate from the volatile TCL; the
elimination of benzyl alcohol and benzoic acid from the semivolatile TCL; the addition of carbazole to
the semivolatile TCL; and the addition of endrin aldehyde to the pesticide TCL. The semivolatile TCL
compound bis(2-chloroisopropyl)cther was renamed 2,2’-oxybis(l..chloropropane).
• A new method for analysis of pesticides/PCBs is used. Changes include the use of wide bore capillary
columns; new surrogates; and new calibration techniques.
• Pesticide/PCB quantitation is performed using both the primary and secondary columns. The lower value
is reported by the laboratofy.
The only significant change in the OLMO1.1 (December, 1990) and OLMO1.1.1 (February, 1991)
revisions to the OLMO1.0 SOW was the lowering of selected seniivolatile CRQLS. The significant changes
in the OLMO I.1 through OLMO1.7 revisions to the OLMOI.0 SOW were the lowering of selected seniivolatile
CRQLs and options for either a 14 day or 35 day data turnaround.
RECOMMENDED USES
This Routine Analytical Services (RAS) method is recommended for broad spectrum analysis to define
the nature and extent of potential site contamination during SSI, LSI, and RI/FS activities. This method is
suitable when a fourteen day or thirty five day turnaround for results is adequate. It is recommended for
samples from known or suspected hazardous wnstc sites where potential contamination may be present at
significant risk levels.
Sediment samples with high moisture content should be solicited as RAS + SAS (Special Analytical
Service) in order to achieve the CRQLS.
ANALYTES/CRQLS
The parameters included in the analysis and the Contract Required Quantitation Limits (CRQLs) are
listed in Attachment 1.
Revision 1.0
-------
ATIACHMENTI (p&ge 1 of 3)
USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR ORGANIC ANALYSIS
MULTI-MEDIA, MULTI-CONCENTRATION
OLMO1 .0
TARGET COMPOUND LIST - VOLATILES
Aqueous
“CRQL
(ug/L,ppb)
LowSoU
S _ _________
C o S.. 10 __ _
Bromomcthanc 10
VInyl Chlthidc :.• 10 ______________ ______ _______
C.b lorodbane . 10 ____________________
Methylene Chiotide 10 _____________________ __________ ___________
Ao one 10
Cazbon Dijutfide 10° ________________
1,1-Dich loi’octhcnc 10’
1,1-Dichlorodhane . . 10’
12- ch1o octhen ( tot 1) 10* _______________ _______ ________
cor oitiz. 10* ____________________ _________ __________
l,2-Dich larocth,.ne 10°
2-But s.none 10 _____________________
I,1,1-Trich lorocthane 10’
Carbon Tc rach1ondc 10’
Bromodichlororncthanc .• .. 10’
I , 2-Dichloropropanc 10’
CRQLs prcviously S ug/L &nd S uglKg in 2188 SOW.
NOTE:
• THE SAMPLE-SPECIFIC CRQLs FOR SOIL SAMPLES WILL BE ADJUSTED FOR PERCENT MOISTURE AND WILL BE
HIGHER THAN THOSE LISTED ABOVE.
• MEDIUM LEVEL SOIL CRQL = 120 x AQUEOUS CRQL REPORTED IN UG!KG.
S S:: 5;S. . .. . Ai ueoux’ 5
5 RQL
.. S< ‘ (ug/L,ppb)
LowSoil
‘CRQL. .
(ug Kg ppb)
10’
10*
10*
10°
‘SS SS.•
10’
10’
..
10°
10’
10*
10’
• 10°
10’
10
10
. 10
10
.. 10’
10’
: .. . 10°
10’
10*
10’
10’
10°
‘.
•
10’
10°
5 T 10°
10’
Revision 1.0
-------
A17ACHMENT I (page 2 of 3)
US EPA CONTRACT LkBORATORY PROGRAM
STATEMENT OF WORK FOR ORGANIC ANALYSIS
MULTI-MEDIA, MULTI-CONCENTRATION
FEBRUARY. 1988
• THE SAMPLE-SPECIFiC CRQLa FOR SOIL SAMPLES WILL BE ADJUSTED FOR PERCENT MOISTURE AND WILL BE
HIGHER THAN THOSE USTED ABOVE.
• MEDIUM LEV . SOIL CRQL 1980 x AQUEOUS CRQL REPORTED IN UGtKG.
TARGET COMPOUND UST - S flVOLATILES
Aqu us
CRQL
(ug Lppb)
Low Soil
CRQL.
(ugIlCg,ppb)
10
330
10
330
10
330
10
330
‘ 10
330
: 10
330
‘ 10
330
“ S 10
330
• 10
330
10
330
10
330
‘‘S 10
330
10
330
‘ ‘ 10
330
10
330
10
330
. 50
1600
hane 10
330
10
330
10
330
10
330
•... 10
330
10
330
10
330
10
330
10
330
10
330
50
1600
10
330
50
1600
10
330
10
330
10
330
“z uoous
Compound CRQL.
(ug/L.ppb)
wSoil
CRQL .
(ug!Kg,ppb)
50
1600
,. .. , 10
330
.. ‘. 50
1600
‘. 50
1600
10
330
10
330
‘ •. 10
dhcr 10
.. .. .. .. 10
330
330
330
. ‘ .• 50
1600
50
1600
“ ‘ 10 .
10
‘ 10
330
330
330
50
1600
10
330
.. 10
330
10
330
•.. 10
330
i
330
10
330
20
660
.... 10
330
“ 10
330
10
330
‘ ‘ ‘ 10
330
10
330
10
330
10
330
10
330
. 10
330
10
330
NOTE:
Revision 1 0
-------
USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR ORGANIC ANALYSIS
MULTI-MEDIA, MULTI-CONCENTRATION
FEBRUARY, 1988
ATTACHMENT I (page 3 of 3)
TARGET COMPOUND LIST - PESTICIDES/PCBs
Aqueo is
‘ 5 C poimd ... . .“QQL
0.05
ow&1
‘ CRQL S’
.. (u IK ,ppb)
8.0
.. 0.05
8.0
. S 0.05
8.0
) 0.05
8.0
S.• S.. 0.05
8.0
•. 0.05
8.0
0.05
8.0
I 0.05
8.0
0.10
16.0
..S 0.10
16.0
0.10
16.0
.. . .. 0.10
16.0
0.10
16.0
0.10
16.0
NOTE.
Aqueous
. CRQL.S.
: .. (ug ppb)
Low Soil
S...
( ppb)
. 0.10
16.0
0.5
80.0
.. 0.10
16.0
0.5
80.0
0.5
80.0
1.0
160.0
0.5
80.0
. . 03
80.0
.. 0.5
80.0
0.5
80.0
..,, 0.5
80.0
1.0
160.0
1.0
160.0
• THE SAMPLE-SPECIFIC CRQL.S FOR SOIL SAMPLES WILL BE ADJUSTED FOR PERCENT MOISTURE AND WILL BE
HIGHER THAN THOSE LISTED ABOVE.
• MEDIUM LEVEL SOIL CRQL = 15 x LOW LEVEL SOIL CRQL REPORTED IN UG/KG.
Revision 1.0
-------
ATTACHM T I (psjc 2 of 3)
USEPA CONTRACT LABORATORY PROGRAM
STAT T OF WORE FOR ORGANIC ANALYSIS
MUL1T.) IA. MULX1.CONC ITRAT1ON
0U40I.0
• CRQLapfcv o IySOu fLa I000ug/K 2J88SOW CRQLapaty20viILa i660uSIK1m2I88SOW
MOlt.
• ThE SA1 WL&SPECIF1C CRQLI FOR SOIL J LE WIU. BE ADJUSTED FOR P CDIT MOISTURE AND WILL BE HIGHER ThAN
ThOSE USTED ABOVE.
• ) 1UM LEVU. SOIL CRQL 1000 x AQUEOUS CRQL REPORTED IN UG/KG.
TARGET COMPOUND LIST. SEROVOI-ATh15
C.pi usd
CRQL
(i /Lppb)
‘ Sod
CRQL
( .ppb)
‘
10
330
b (2-Q3 yl) r
10
330
2 io vp&D
10
330
U4 ithIo ob€.
10
330
10
330
L2’DIcb s
330
10
330
10
330
10
330
N•N 4d mpy
10
330
10
330
•.
10
330
S
10
330
10
330
10
330
10
330
.4.fl 1n oç oi
10
330
1.2.4-Tt Jo obc ..
10
330
Nø .’f’— ——
10
330
4CWo o i1
10
330
HcTthoo d ac
10
330 -
4-Cb .3—mcthy baioI
10
330
2 .M y pb M1 c
10
330
10
330
2.4.6-Trith1o oçbcno4
10
330
2.4.STnth1o oçb o1
23’
800’
2-CbIoto p dia1ee
10
330
2-N o. j1 e
25’
800’
D yIpl ifsI.i.
10
330
Ac èthy1 r
10
330
2 .6-D ittow
10
330
3N r ai1
23’
800’
, c t
(oj/Lppb)
L Sod
.
(uiIX ppb
tO
330
25’
800’
25•
800’
- . 10
330
10
330
. ... 10
330
10
10
330
330
5 555 ?
23’
800’
23’
100’
10
330
10
330
10
330
23’
800’
:•.. 10
330
.. 10
330
.- 10
330
.. 10
330
10
330
10
330
10
330
10”
330”
.. 10
330
-: .. 10
330
10
330
10
330
10
330
10
330
.- 10
330
10
330
10
330
10
330
Revision 1.0
-------
ATI’ACHMENT I (page 3 of 3)
USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR ORGANIC ANALYSIS
MULTI-MEDIA, MULTI-CONCENTRATION
OLMOL.O
TARG COMPOUND LIST - PESTICIDES!PCBs
coui’
Compound .. CRQL ’
.5 ; (ug/Lppb)
Low Soil”,
CRQL
(ug Kg,ppb)..
T 0.05
1.7
‘ 0.05
1.7
0.05
1.7
(Lindanc) 0.05
1.7
‘‘ ::.‘ 0.05
1.7
0.05
1.7
0.05
1.7
I 0.05
1.7
0.10
3.3
0.10
3.3
.. 0.10
3.3
[ I 0.10
3.3
0.10
3.3
sulfate 0.10
3.3
Aqu us CRQLS changed from 2/88 SOW to the following:
‘. Aqueout.
Compound CRQL
‘(ugIL,ppb)’
Low Soil”
CRQL
(u 1Xgppb)’
0.10
3.3
0.5
17.0
OJO
3.3
0.10
3.3
0.05’
1.7
0.05’
1.7
“ 5.0’
1700
1.0’
33.0
“ 2.0’
67.0
- 1.0’
33.0
1.0*
33.0
1.0’
33.0
1.0
33.0
.. 1.0
33.0
* Aquccus CRQLS (ug/L) - alpha- and gamma- Cblordane from 0.5 to 0.05;
Toxaphene from 1.0 to 5.0;
Aroclorz-1016, 1232, 1242, and 1248 from 0.5 to 1.0;
Aroclor-1221 from 0.5 to 2.0.
All low soil CRQLs changed from 2/88 SOW to the following:
“Low Sod CRQLS (uglKg) -
NOTE:
alpha-BHC through Endosulfan I from 8.0 to 1.7;
Dicidrin through 4,4’-DDT and Endrin kctonc from 16.0 to 3.3;
Mcthoxychlor from 80.0 to 17.0;
alpha- and gamma-Chiordanc from 80.0 to 1.7;
Tonphcnc from 160.0 to 170.0;
Azoclor-l016, 1232, 1242, and 1248 from 80.0 to 33.0;
Aroclor-1221 from 80.0 to 67.0;
Aroclor-1254 and 1260 from 160.0 to 33.0.
Revision LO
-------
TiTLE: USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR ORGANIC ANALYSIS
MULTI-MEDIA, MULTI-CONCENTRATION
DOCUMENT NUMBER: OLMOI.9
DOCUMENT DATE: Not Applicable
EFFECTIVE DATES: July 1993 through February 1995
CONCENTRATION: Low to Medium
DATA TURNAROUND: 14 Days or 35 Days
MATRICES: Aqueous/Soil/Sediment’
SIGNIFICANT FEATURES
• The parameters include volatile, semivolatile, and pesticidelPCB compounds.
• Volatiles and semivolatiles are analyzed by GCIMS, pesticides/PCBs are analyzed by GCIECD.
• Major Tentatively Identified Compounds (TICs) are reported for GC/MS analyses.
• Second column confirmation by GCIECD is required for all pesticideslPCBs. The lower of the
two concentrations detected on both columns is reported. PesticideslPCBs which are detected at
concentrations above 10 ng/uL are confirmed by GC/MS analysis.
REVISIONSIMODIFICATIONS
The only significant revisions to the OLMO1.O SOW in the OLMO1.8 revision were changes in the format
and content of the Agency Standard diskette deliverable.
The following is a list of the significant changes from the OLMO1.8 revision that are incorporated in the
OLMO1.9 revision:
• MS/MSD analysis is not required for SDGs containing only equipment/trip blanks or PE samples.
• Specific instructions are given regarding resolution of problems with reduced sample volume and
MS/MSD sample designation.
RECOMMENDED USES
This Contract Laboratory Program (CLP) method is recommended for broad spectrum analysis
to define the nature and extent of potential site contamination during Site Investigation (SI) and Remedial
Investigation/Feasibility Study (R.I/FS) activities and to verify that Remedial Design/Remedial Action
(RDIRA) activities comply with pre-determined clean-up standards. This method is suitable when a 14
day or 35 day turnaround for results is adequate. It is recommended for samples from known or
suspected hazardous waste sites where potential contamination may be present at significant risk levels.
* This method is not applicable to soil/sediment samples with high moisture content.
ANALYTES/CRQLs
The parameters included in the analysis and the Contract Required Quantitation Limits (CRQLs)
are listed in Attachment 1.
Revision 3.0
-------
ATTACHMENT 1 (page 1 of 3)
LJSEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR ORGANIC ANALYSIS
MULTI-MEDIA, MULTI-CONCENTRATION
OLMO1.9
TARGET COMPOUND LIST - VOLATILES
Aqueot
CRQI
(ugIL,ppb)
“LowSoU 5
CRQL
(uglKg,ppb)
10
10
10
10
10
10
10
10
chloride 10
10
10
10
10
10
10
10
10
10
(total) 10
10
10
10
10
10
10
10
10
10
tctrachloridc 10
10
10
10
10
10
NOTE:
Aqueous
CRQL
(ugIL,ppb)
LOWSOU
CRQL
(nglKg,ppb)
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
• The san p1c.ipcciflc CRQL. for soil/sediment saznplca will be adjusted for pcrccnt moisWre and will be highcr than those listed above.
• Medium level sod/sediment CRQL = 120 x aqueous CRQL reported in ug/kg.
Revision 3.0
-------
ATIACHMENT I (page 2 of 3)
USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR ORGANIC ANALYSIS
MULTI-MEDIA, MULTI-CONCENTRATION
OLMOI .9
TARGET COMPOUND LIST - SEMIVOLATILES
Compound
.
Aqueous
CRQL
(ug/L,ppb)
Low Soil
CRQL.
(ug/Kg,ppb
Pha L
10
330
bis(2.chIoloethyI)dhet
10
330
2-Ch1oropbc l •. ...
10
330
1,3-Dichkuvbuizcac ..,
10
330
I,4-D1ch1ozvbcr e
10
330
1 ,2-Dichlcroba c
10
330
2-Mcthy1pbc l -
10
330
2,2 ’-orybia(l-chlo upmpeno)
10
330
4.McthyIph o1
10
330
N-Nddi-n-propy lamine
10
330
Hexachloroethane
10
330
Nitroba anc
10
330
Isophorvne
10
330
. ..2 NitxophcnoI
10
330
im hylphenoI
10
330
2 -Clilotod.hoxy)m hanc
10
330
2,4.Dich loruphcno l
10
330
12,4-Trichloxobe cnc
10
330
Napbthaiene
10
330
4-Ch lorcaniline
10
330
Hexachlorobutadiene
10
330
4 -Ch1oro-3 .m .hyIphcnoI
10
330
2-Methy lnaphthalenc
Hehloyc loptadicnc
2,4,6.Trich lorophcnol
10
330
10
330
10
330
2,4,5-Trich lorophcno l
25
800
2-Chloronsphthalene
10
330
2-Nitroanilino
25
800
Dimcthylphthal ate
10
330
Acc n aphthy lenc
10
330
2,6-Dinitroto luenc
10
330
j 3-Nitmaniline
25
800
NOTE:
Aqueous
CRQL.
(ugJL,ppb)
Low Soil
CRQL
(ugfK ,ppb)
- .. 10
330
25
800
.. .• 25
800
10
330
10
330
10
330
10
330
.. 10
330
25
800
25
800
10
330
10
330
10
330
. 25
800
10
330
.. 10
330
10
330
10
330
10
330
10
330
10
330
10
330
10
330
10
330
10
330
10
10
330
330
10
330
10
330
,2,3-ed)pyrcne 10
330
10
330
10
330
The sample-specific CRQLS for soiilscd imcnt samples will be adjusted for percent moiswrc and will be lughcr than those Listed above.
• Medium Ievci sod/sediment CRQL = 1000 x aqueous CRQL in ug/Kg.
Revision 3.0
-------
ATTACHMENT I (page 3 of 3)
USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR ORGANIC ANALYSIS
MULTI-MEDIA, MULTI-CONCENTRATION
OLMO1 .9
TARGET COMPOUND LIST - PESTICIDEIPCB
Aqueous
CRQL
(ugIL,ppb)
Low Soil..
CRQL’ 5
(ugIKg,ppb)
0.05
1.7
0.05
1.7
0.05
I.?
0.05
1.7
0.05
1.7
0.05
1.7
Epoxide 0.05
1.7
0.05
1.7
0.10
3.3
0.10
3.3
0.10
3.3
0.10
3.3
0.10
3.3
iulfatc 0.10
3.3
NOTE:
-‘ Aqueous
CRQL
(ugIL,ppb)
S 5. .
L w Soil
•. CI QL
(uglKg,ppb
)
. 0.10
3.3
0.5
17.0
0.10
3.3
0.10
3.3
0.05
1.7
0.05
1.7
5.0
170.0
1.0
33.0
2.0
67.0
1.0
33.0
1.0
33.0
1.0
33.0
1.0
33.0
1.0
33.0
• The sample-specific CRQLs for soil/sediment samples will be adjusted for percent moisture and will be higher than
those listed above.
Revision 3.0
-------
TiTLE: USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR ORGANIC ANALYSIS
MULTI-MEDIA. MULTI-CONCENTRATION
DOCUMENT NUMBER: OLMO2.1
DOCUMENT DATE: Not Applicable
EFFECTIVE DATES: No contracts have been awarded
CONCENTRATION: Low to Medium
DATA TURNAROUND: 14 Days or 35 Days
MATRICES: Aqueous/SoillSediment ’
SIGNIFICANT FEATURES
• The parameters include volatile, semivolatile, and pesticide/PCB compounds.
• Volatiles and semivolatiles are analyzed by GC/MS, pesticides/PCBs are analyzed by GCIECD.
• Major Tentatively Identified Compounds (TICs) are reported for GCJMS analyses.
• Second column confirmation by GCIECD is required for all pesticideslPCBs. The lower of the two concentrations detected on
both columns is reported. PesticideslPCBs which are detected at concentrations above 10 ng/uL are confirmed by GC/MS
analysis.
REVISIONSIMODIFICATIONS
The following is a list of the significant changes from the OLMO I.9 SOW that are incorporated in the OLMO2.0 SOW (including revision
0LM02. 1):
For volaciles analysis, if gaseous compounds 1) fail to exhibit narrow symmetrical peak shape, 2) are not separated from the
solvent front, or 3) are not resolved greater than 90% from each other, then a subambient oven controller must be used and the
initial temperature must be 10°C.
• Background subtraction must be performed utilizing a spectrum obtained no greater than 20 scans prior to the elution of BFB
or DFTPP.
• For semivolatile analysis, the final column temperature must be held for three minutes following the elution of the last
semivolatile organic target compound.
• Samples which contain alkane series in the TICs will be evaluated using the mass chromatograms of mJz 43, 57, and 71 and the
alkane series will be reported as one TIC along with a total estimated concentration.
• A multi-component pesticidelPCB standard must be analyzed within 72 hours of detecting a multi-component pesticidelPCB in
a field sample.
• The number of volatile organic TICs has been raised from 10 to 30 and the number of semivolatile organic TICs has been raised
from 20 to 30.
RECOMMENDED USES
This Contract Laboratory Program (CLP) method is recommended for broad spectrum analysis to define the nature and extent
of potential site contamination during Site Investigation (SI) and Remedial Investigation/Feasibility Study (RIIFS) activities and to verify
that Remedial Design/Remedial Action (RD/RA) activities comply with the pre-determined clean-up standards. This method is suitable
when a 14 day or 35 day turnaround for results is adequate. It is recommended for samples from known or suspected hazardous waste
sites where potential contamination may be present at significant nsk levels.
This method is not applicable to soil/sediment samples with high moisture content.
ANALYrESICRQLS
The parameters included in the analysis and the Contract Required Quancitation Limits (CRQLs) are listed in Attachment I.
Revision 2.0
-------
A1TACHMENT I (page 1 0(3)
USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR ORGANIC ANALYSIS
MULTI-MEDIA. MULTI-CONCENTRATION
OLMQ2. 1
TARG COMPOUND LIST - VOLATILES
Coznpound
Aqueous
CRQL
(ugIL,ppb)
Low Soil
CRQI 4
(ugI g,ppb)
ChIorom hane
10
10
Bromomcthane
10
10
Vinyl chloride
10
10
Oh loroethano
10
10
McthyIcn chloride
10
10
Acetone
10
10
Carbon disuliide
10
10
l,l-Dich lorocthcnc
10
10
1,1-Didiloroethanc
10
10
1,2-D chIorocthcne (total)
10
10
Chloroform
10
10
1,2-Dichiorocehane
10
10
2-Bucanonc
10
10
1 ,1,1-Triehloroethanc
10
10
Carbon tctrachloridc
10
10
Bromodich loromcthano
10
10
1,2-Dichloroptopa ne
10
10
NOTE:
AqueoiLs
CRQL
(ug/L,ppb)
Low Soil
CRQL
(ugIKg/ppb)
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
1O•
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
• The sample-specific CRQLS for soil/scdunent samples will be adjusted for pereent molacure and will be higher than those listed above.
• Medium level soil/sediment CRQL = 120 x aqueous CRQL reported in ug/lcg.
Revision 2.0
-------
ATTACHMENT I (page 2 of 3)
USEPA Cor rrRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR ORGANIC ANALYSIS
MULTI-MEDIA, MULTI-CONCENTRATION
OLMO2. I
TARGET COMPOUND LIST - SEMIVOLATILES
Compound
Aqueous
CRQL
(ug/L,ppb)
Low Soil
CRQL
(ugfKg,ppb)
Phenol
10
330
bL.(2 .chlorocthyl)dher
10
330
2-Qdoropbamo l •.
10
330
1 1 3-Dicblorobcus e nc
10
330
1,4-Dichlorobcr cne
10
330
1 .2-Dithlorobcsaezsc
10
330
2 -Mdhylp&noI
10
330
2.2’.oxybii(t-ehloropmpane)
10
330
4-M hy1pheno1
10
330
N-Niti so-&-o-propyIaininc
10
330
Hex ehIotv hane
10
330
Nitroba cnc
10
330
I pho vnc ‘‘
10
330
2-Nitrophenot
10
330
2,4-Dimcthy lpheoo l
10
330
2-Ch1orocthoxy)mcthanc
10
330
) [ chlo iophcnol
10
330
1 -Trictüoxvbc ene
10
330
Nap 1 baIene
10
330
4-Chloroanilino
Hehlorobutadienc
4-Ch loro-3-rnethy lpheno l
tO
10
tO
330
330
330
2-Methy1naphtha1er c
10
330
Hex achlorocyclopaui .diene
10
330
24,6-Triehlorophenot
10
330
2,4,5-ThchIoi ophenot
25
800
2-Chloronaphihalene
tO
330
2-Nitrvanslinc
25
800
Dimethy lphthalazc
10
330
Accnaphthylene
10
330
2.6-Dinitrocoluenc
3-Nitroanilinc
10
25
330
800
NOTE:
Compound
Aqueous
CRQL ,
(ug/L,ppb)
Low Soil
CRQL.
(uglKg,ppb)
AccnaphLhcnc
10
330
2,4 -D&nitn phcnol
25
800
4-Nkrupbcnol
25
800
Diba2ofii n
10
330
.2,4-DirütotnIuc
10
330
Diy1p ldhAht
4-Ch lorophenyl.phcny ldhe.r
F luorenc
10
330
tO
330
10
330
4-Nitroaniline
25
800
4,6-Dbutxo-2-methy tphcno l
25
800
N-Nitxosodsphenyfazninc
tO
330
4-Brorncpheny l-pbcny lcthcr
10
330
Flexc1osobcs cnc
10
330
Pcnxachlorophcno l
25
800
Phcnanthzvnc
tO
330
Anthraccnc
10
330
Carbazo lc
10
330
Di-n-butylphthalate
tO
330
Fluoranthenc
tO
330
Pyrene
10
330
Bu mylbenzylphthalnte
10
330
3,3 ’-DiehIombet id ne
Bei o(a)anthraccnc
Chryscn
10
330
10
330
10
330
bis(2-ethy1hexy1)phtha1at
10
330
D -n-ocy1phthaIatc
10
330
Bcrtzo(b)ftuoranthcnc
10
330
Bcz o(k)f1uoranthene
10
330
Bcr o(a)pyrcne
10
330
Indeno(1.2,3-cd)pyrene
tO
330
Dibei o(a,h)anthraecnc
10
330
Be i o(g,hMpcrylenc
10
330
S Thc sample-specific CRQLS for sodiscdimcnt samples will be adjusted for percent moisture and will be higher than those listed above
Medium lcvcl sod/sediment CRQL = 1000 x aqueous CRQL in ug/Kg.
Revision 2.0
-------
AUACHMENT I (page 3 of 3)
USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR ORGANIC ANALYSIS
MULTI-MEDIA, MULTI-CONCENTRATION
OLMO2.1
TARGET COMPOUND LIST - PESTICIDEIPCB
Aqueous
CRQL
(ugIL,ppb)
Soil
•. CRQL
(uglEg,ppb)’
0.05
1.7
0.05
1.7
0.05
1.7
0.05
1.7
0.05
1.7
0.05
1.7
Epoxide. ... 0.05
1.7
0.05
1.7
“ ‘ 0.10
3.3
0.10
3.3
0.10
3.3
0.10
3.3
0.10
3.3
!ulfate 0.10
3.3
NOTE:
. Aqueous
CRQL
(ug/L,ppb)
Low Soil
CRQL
(ug/Kg,ppb)
• “ 0.10
3•3
0.5
17.0
0.10
3.3
0.10
3.3
0.05
1.7
0.05
1.7
5.0
170.0
1.0
33.0
2.0
67.0
. 1.0
33.0
1.0
33.0
1.0
33.0
I 0
33.0
1.0
33.0
• The sample-specific CRQLs for soil/sediment samples will be adjusted for percent moisture and will be higher than
those listed above.
Revision 2.0
-------
TiTLE: USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR ORGANIC ANALYSIS
MULTI-MEDIA, HIGH CONCENTRATION
DOCUMENT NUMBER: Not Applicable
DOCUMENT DATE: September 1988
EFFTLC11VE DATES: June 7, 1989 through December 26, 1991
CONCENTRATION: High: Greater than 20 ppm
DATA TURNAROUND: 35 Days
MATRICES: LiquidlSolidlMulti-phase
SIGNIFICANT FEATURES
• No holding times are designated for high concentration samples.
• The analyses are suitable for highly contaminated samples (>20 mg/Kg).
• The analyses are acceptable for liquid, solid, or multiphase samples. Multi-phase samples are separated into
water miscible liquid, water irnmiccible liquid, or solid phases. Each phase is analyzed separately.
• Volatile, extractable (sernivolatiles and pesticides), and multicomponent extractable (Aroclors and Toxaphene)
compounds are included.
• Volaxiles and extractables are analyzed by GCIMS; Aroclors and Toxaphene are analyzed by GC/ECD.
• Second column confirmation by GCIECD is required for Aroclors and Toxaphene.
• Major Tentatively Identified Compounds (TICs) are reported for GC/MS analyses.
REVISIONS/MODIFICATIONS
The 1/89 and 4/89 revisions to the 9/88 SOW do not significantly affect data useability.
RECOMMENDED USES
This Routine Analytical Services (RAS) method is recommended for pre-remedial, remedial, or removal
projects where high concentrations of organic contaminants (greater than 20 mg/Kg) are suspected and a thirty
five day turnaround for results is adequate. It is recommended for samples obtained from drummed material,
waste pits or lagoons, piles of waste, tanker trucks, onsite tanks, or apparent cont min ted soil areas. The waste
material may be industrial process waste, byproducts, raw materials, intermediates and contaminnted products.
Samples may be spent oil, spent solvents, paint wastes, metal treatment wastes, and polymer formulations.
The method is suitable for solids, liquids, or multiphase samples, a phase being either water miscible
liquid, water immiscible liquid, or solid. Various methods of phase separation may be utilized depending on the
number and types of phases in a sample.
ANALYTES/CRQLs
The parameters included in the analysis and the Contract Required Quantitation Limits (CRQLs) are listed
in Attachment 1.
Revision 1.0
-------
AUACHMENT I (page 1 of 3)
USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR ORGANIC ANALYSIS
MULTI-MEDIA, HIGH CONCENTRATION
SEPTEMBER, 1988
TARGET COMPOUND LIST - VOLATILES
Compound
‘.
RQL
(mgFKg,pp i)
5.0
5.0
5.0
“
5.0
2.5
5.0
2.5
2 . 5
.
2.5
(total)
2.5
2.5
•.
2.5
5.0
.
2.5
Tetrachiori
dé
2.5
5.0
thane
2.5
NOTE:
Compound ..
:.; cR.QL
(n3gfKg,ppin)
.
2.5
cis-1,3-Dichloroprop e ne
2.5
Thchloroethene
Dirom xbloromethin
2.5
2.5
1,1,2-Trichioroethane
2.5
Benzeae 1..’
2.5
trans-i .3-Dichloropropene
2.5
‘Bromoform ‘
2.5
:.: .
5.0
2-Hexanone .•
5.0
Tetrachioroethene
2.5
1,1 ,2,2-Tetrachloroethane
2.5
Toluene
2.5
Chlorobenzene ‘ ‘
2.5
ELhy lbónzene• : .‘
2.5
Styrene’ ;
2.5
Xylene (lolal) ....
2.5
• ALL CRQLS ARE BASED ON WET WEIGHT AND APPLY TO SOLID AND LIQUID SAMPLES.
• RESULTS FOR BOTH SOLID AND LIQUID SAMPLES ARE REPORTED AS MGIKG, WET WEIGHT.
Revision 1.0
-------
USEPA CONTRACT LABORATORY PROGRAM
STA1tM NT OF WORK FOR ORGANIC ANALYSIS
MULTt-) IA. HIGH C0NC TRA11ON
SEPT 1 BER. 1911
ArFAcHMThT I (pqo 2 013)
TARGET COIQOUND LIST• EXTRACTABLE S
5 > 5-
cm!.
.—
20
...L .‘ > :
20
20
20
20
20
•:± * .
20
• S’ ” 5 - 5 -
20
.
20
‘
20
..
20
•.. .. ‘‘
20
....
20
... .... ..
20
•
20
-. ‘ - ‘- - ‘
20
.... • > .
100
20
20
20
20
20
20
20
20
20
20
100
20
100
20
NOTE&
..
‘
•pp )
20
S . SS S
20
.. ‘
100
M_ :••:..
20
100
:: .
100
20
: > . >
20
Dicthy a kfr .. ‘;.
20
20
.
20
‘
4.6.D7 - do ••; >••
100
100
Nc.od bai, s
4.Bc y1 ..
20
20
3p s>
20
20
b -aRC
20
100
f -B 1C (I1. 1w)
20
‘
20
‘
20
dba.BHC ‘ ....
20
Hcp k*Iiw
20
AMi
20
20
•
20
20
Mo oth1o obçb yI
100
Dci btpb yI
100
TrIo obçâ yI
100
• ALL CRQLa ARE BASED ON WET WEIGHT AND APPLY TO SOLID AND LIQUID SAMPLES.
• RESULTS FOR BOTh SOLID AND LIQUID SAWLES ARE R OW ED AS MOIIG. WET WEIGHT.
Revision 1.0
-------
US ’A CONflACT LAEORATORY PROGRAM
STAT fT OF RZ FOR ORGANIC ANALYSIS
MULThMEDIA. HIGH CONC ’ TRATION
ic
ATIAcHJ. 1T I (psjo 3 of 3)
TARGET COMPOUND LIST. IRACTABLE1 (CON W )
S.cRQL
( gIg4.pç )
.
100
20
‘
20
20
20
‘ ‘
20
20
100
.
100
20
20
20
- .•
100
20
. “ .
20
::‘.. -
20
• :•.‘
Sc__
( sl i.v )
E .... .
20
S •vs.;’..s <:. .
. ‘
20
20
20
S
:
40
b
20
No o4
200
...
5 5; 5
20
ac(b) r.md c @ . :
20
Bci
20
•
20
II,2.3-c4)pyr ic
20
-
20
BLyláio.. - -
20
-
...
-
..CRQE .
( Xj.pp )
‘
‘ - •
50
-
10
•
‘ -
10
•
10
-
10
•
•.::
10
10
••
10
NOTFi
• ALL CRQLJ ARE BASU) ON WET WEIGHT AND APPLY 10 SOLID AND LIQUID SAMPLES.
• RESULTS FOR BOTh SOLID AND LIQUID 3ftJb4PL s A F RflORT AS MG/KG. ViTT WEIGHT.
TARC C1 MPOUND LIST. MJLTI MPOMEW ATABI .ES
Revision 1.0
-------
‘lITLE: USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR INORGANIC ANALYSIS
MULTI-MEDIA, MULTI-CONCENTRATION
DOCUMENT NUMBER: Not Applicable
DOCUMENT DATE: July 1988
F .FFECTIVE DATES: May 23, 1989 through March 29, 1992
CONCENTRATION: Low to Medium
DATA TURNAROUND: 35 Days
MATRICES: Aqueous/Soil/Sediment *
SIGNIFICANT FEATURES
I The analyses are suitable for aqueous, soil or sediment samples at low to medium concentration levels.
REVISIONSIMODIFICATIONS
2/89 - Method for Total Cyanide (CN) Analysis by Midi Distillation Method 335.2 CLP-M was
added.
6/89 - Revisions to the 7/88 SOW do not significantly affect data useability.
RECOMMENDED USES
This Routine Analytical Services (RAS) method is recommended for broad spectrum analysis to
define the nature and extent of potential site contpmination during SSI, LSI, and RIIFS activities. This
method is suitable when a thirty five day turnaround for results is adequate. It is recommended for
samples from known or suspected hazardous waste sites where potential cont2nhirrntion may be present
at significant risk levels.
* Sediment samples with high moisture content should be solicited as RAS + SAS (Special
Analytical Service) in order to achieve the CRDLs.
ANALYTES/CRDLs
The parameters included in the analysis and the Contract Required Detection Limits (CRDLs) are
listed in Attachment 1.
Revision 1.0
-------
ATTACHMENT I (j age 1 of 1)
USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR INORGANIC ANALYSIS
MULTI-MEDIA, MULTI-CONCENTRATION
JULY, 1988
TARGET ANALYTE LIST
AQUEOUS
Analyte CRDL
(ugIL,ppb)
SO1L
RDL
(mgfKg,ppm)
200
40
60
12
10
2
Bzriurn - .•. 200
40
S
I
5
1
5000
1000
10
2
50
10
25
5
‘. 100
20
3
0.6
NOTE:
AQUEOUS
Analyte CRDL:. .. ,
(ugIL,ppb)
SOIL
.. . CRDL
( g/Kg,ppin)
5000
1000
15
3
0.2
0.1
40
8
5000
1000
S
1
. 10
2
5000
1000
.‘ 10
2
50
10
20
4
10
2
• THE SAMPLE-SPECIFIC CRDLs FOR SOIL SAMPLES WILL BE ADJUSTED FOR PERCENT MOISTURE
AND WILL BE HIGHER THAN THOSE LISTED ABOVE.
Revision 1.0
-------
TiTLE: USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR INORGANIC ANALYSIS
MULTI-MEDIA, MULTI-CONCENTRATION
DOCUMENT NUMBER: ILMO1.O
DOCUMENT DATE: Not Applicable
EFk’i CTIVE DATES: September 7, 1990 through September 26, 1993
CONCENTRATION: Low to Medium
DATA TURNAROUND: 35 Days
MATRICES: Aqueous/Soil/Sediments
SIGNIFICANT FEATURES
• The analyses are suitable for aqueous, soil or sediment samples at low to medium concentration levels.
• This Statement of Work includes the niidi distillation for cyanide analysis and the microwave digestion
for GFAA and ICP analyses. These two sample preparation procedures require less sample volume
than the traditional Statement of Work sample preparation procedures.
REVISIONSIMODIFICATIONS
None to Date
RECOMMENDED USES
This Routine Analytical Services (RAS) method is recommended for broad spectrum analysis to
define the nature and extent of potential site contamination during SSI, LSI, and RIIFS activities. This
method is suitable when a thirty five day turnaround for results is adequate. It is recommended for
samples from known or suspected hazardous waste sites where potential contamination may be present
at significant risk levels.
* Sediment samples with high moisture content should be solicited as RAS + SAS (Special
Analytical Service) in order to achieve the CRDLs.
ANALYTES/CRDLs
The parameters included in the analysis and the Contract Required Detection Limits (CRDLs) are
listed in Attachment 1.
Revision 1.0
-------
AUACHMENT I (page 1 of 1)
USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR INORGANIC ANALYSIS
MULTI-MEDIA, MULTI-CONCENTRATION
lI_MO 1.0
TARGET ANALYTE UST
Analyte
Aqueous
CRDL
(ugFL,ppb)
Soil
CRDL
(mg/Kg,ppm)
Aluminum
200
40
Antimony
60
12
Arsenic
10
2
Bazium
200
40
Beryllium
5
1
Cadmium
5
1
Calcium
5000
1000
Chxocium
10
2
Cobalt
50
10
Copper
25
5
Iron.
100
20
Lead
3
0.6
NOTE:
Analyte
Aqueous
CRDL
(ugfL,ppb)
Soil
CRDL
(mglKg,ppm)
Magn iuni
5000
1000
Manganese
15
3
Mercury ‘
0.2
0.1
Nickel
40
8
Potassium
5000
1000
Selenium
5
1
Silver
10
2
Sodium
5000
1000
Thallium
10
2
‘Vanadium
50
10
Zinc
20
4
Cyanide
10
2
• THE SAMPLE-SPECIFIC CRDL5 FOR SOIL SAMPLES WILL BE ADJUSTED FOR PERCENT MOISTURE
AND WILL BE HIGHER THAN THOSE LISTED ABOVE.
Revision 1.0
-------
1TILE: USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR INORGANIC ANALYSIS
MULTI-MEDIA, MULTI-CONCENTRATION
DOCUMENT NUMBER: ILMO2.1
DOCUMENT DATE: Not Applicable
i ii C11VE DATES: March 1993 through October 1994
CONCENTRATION: Low to Medium
DATA TURNAROUT4D: 14 Days or 35 Days
MATRICES: Aqueous/Soi/SedimenC
SIGNIFICANT FEATURES
• The analyses are suitable for aqueous, soil, or sediment samples at low to medium concentration
levels.
REYISIONSIMODWICATIONS
The following is a list of the significant changes from the ILMO1.O SOW that are incorporated in the
ILMO2.1 SOW:
• Specific analysis instructions are presented when samples are received for dissolved metals
analysis.
• Requirements for contract reports/deliverables distribution are included for 14 day turnaround
contracts.
• SOPs are now required to be distributed by the laboratories to EPA-NEIC.
• Microwave digestion for soil/sediment samples is not appropriate for quantitative recovery of
antimony.
RECOMMENDED USES
This Contract Laboratory Program (CLP) method is recommended for broad spectrum analysis
to define the nature and extent of potential site contamination during Site Investigation (SI) and Remedial
InvestigationlFeasibility Study (RJ/FS) activities and to verify that Remedial DesigniRernedial Action
(RDIRA) activities comply with pre-determined clean-up standards. This method is suitable when a 14
day or 35 day turnaround for results is adequate. It is recommended for samples from known or
suspected hazardous waste sites where potential contamination may be present at significant risk levels.
* This method is not applicable to soil/sediment samples with high moisture content.
ANALYTES/CRDL
The parameters included in the analysis and the Contract Required Detection Limits (CRDLs) are
listed in Attachment 1.
Revision 2.0
-------
AUACHMENT I
USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR INORGANIC ANALYSIS
MULTI-MEDIA, MULTI-CONCENTRATION
ILMO2.1
TARGET ANALYTE LIST
Aqueous
CRDL
(ugfL,ppb)
oi1
CRDL
(mg/Kg,ppm)
200
40
60
12
10
2
200
40
5
1
5
1
5000
1000
10
2
50
10
25
5
100
20
3
0.6
NOTE:
Aqueous
CRDL
(ugIL,ppb)
Soil
CRDL
(mg/Kg,ppm)
5000
1000
15
3
0.2
0.1
40
8
5000
1000
5
1
10
2
5000
1000
10
2
50
10
2
• The sample-specific CRDLs for soil/sediment samples will be adjusted for percent moisture and will be
higher than those listed above.
Revision 2.0
-------
TITLE: USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR INORGANIC ANALYSIS
MULTI-MEDIA, MULTI-CONCENTRATION
DOCUMENT NUMBER: ILMO3.O
DOCUMENT DATE: Not Applicable
EFFECTIVE DATES: May 1993 through March 1996
CONCENTRATION: Low to Medium
DATA TURNAROUND: 14 Days or 35 Days
MATRICES: Aqueous/Soil/Sediment’
SIGNIFICANT FEATURES
• The analyses are suitable for aqueous, soil, or sediment samples at low to medium concentration
levels.
REVISIONS1MODIFICATIONS
The following is a list of the significant changes from the ILMO2.1 SOW that are incorporated in the
ILMO3.O SOW:
• An analytical spike and an aqueous Laboratory Control Sample 0_CS) are not required when
analyzing field samples for dissolved metals.
• Terminology was added to require that sample coolers be returned to the appropriate sampling
office within 14 days following shipment receipt.
• Additional instrumentation requirements were added for greater than 500 samples per month
capacity.
• For cyanide water analysis, the LCS requirement was changed from “not required” to ‘using the
distilled ICV as the LCS”.
RECOMMENDED USES
This Contract Laboratory Program (CLP) method is recommended for broad spectrum analysis
to define the nature and extent of potential site contamination during Site Investigation (SI) and Remedial
InvestigationiFeasibility Study (RIIFS) activities and to verify that Remedial Design/Remedial Action
(RD/RA) activities comply with pre-determined clean-up standards. This method is suitable when a 14
day or 35 day turnaround for results is adequate. It is recommended for samples from known or
suspected hazardous waste sites where potential contamination may be present at significant risk levels.
* This method is not applicable to soil/sediment samples with high moisture content.
ANALYTES/CP.J)L s
The parameters included in the analysis and the Contract Required Detection Limits (CRDLs) are
listed in Attachment 1.
Revision 2.0
-------
ATFACHMENT I
USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR INORGANIC ANALYSIS
MULTI-MEDIA, MULTI-CONCENTRATION
ILMO3.O
TARGET ANALYTE LIST
Analyte
Aqueous
CRDL
(ugiL,ppb)
‘‘Soil
CRDL
(mglKg,ppm)
Aluminum
200
40
Antimony
60
12
Arsenic
10
2
Barium
200
40
Beryllium
5
1
Cadmium
5
1
Calcium
5000
1000
Chromium
10
2
Cobalt
50
10
Copper
25
5
hon
100
20
Lead
3
0.6
NOTE:
Analyte
‘
Aqueous
CRDL
(ugIL,ppb)
Soil
CRDL
(mg/Kg,ppm)
Magnesium
5000
1000
Manganese
15
3
Mercury
0.2
0.1
Nickel
40
8
Potassium
5000
1000
Selenium
5
1
Silver
10
2
Sodium
5000
1000
Thallium
10
2
Vanadium
50
10
Zinc
20
4
Cyanide
10
2
• The sample-specific CRDLs for soil/sediment samples will be adjusted for percent moisture and will be
higher than those listed above.
Revision 2.0
-------
TiTLE: USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR INORGANIC ANALYSIS
MULTI-MEDIA, HIGH CONCENTRATION
DOCUMENT NUMBER: IHCOI.2
DOCUMENT DATE: Not Applicable
Li J C’flVE DATES: May 15, 1991 through November 30, 1993
CONCENTRATION: High
DATA TURNAROUND: 35 Days
MATRICES: LiquidiSoiid/Multi-phase
SIGNIFICANT FEATURES
• The analyses are suitable for highly contaminated samples.
• The analyses are acceptable for liquid, solid, or multiphase samples. Multi-phase samples are
separated into water miscible liquid, water immi ccibIe liquid, or solid phases. Each phase is analyzed
separately.
• The analyses include conductivity and pH; potassium is not included.
REVISIONSIMODIFICATIONS
The IHCO1.1 and IHCO1.2 revisions to the IHCOI.0 SOW do not significantly affect data
useability.
RECOMMENDED USES
This Routine Analytical Services (RAS) method is recommended for pre-remedial, remedial, or
removal projects where high concentrations of inorganic contaminants are suspected and a thirty five day
turnaround for results is adequate. It is recommended for samples obtained from drummed material,
waste pits or lagoons, piles of waste, tanker trucks, onsite tanks, or apparent contaminated soil areas.
The waste material may be industrial process waste, byproducts, raw materials, intermediates and
contaminated products. Samples may be spent oil, spent solvents, paint wastes, metal treatment wastes,
and polymer formulations.
The method is suitable for solids, liquids, or multiphase samples, a phase being either water
miscible liquid, water immiscible liquid, or solid. A phase separation step is applied prior to digestion.
Each phase is analyzed and reported as a separate sample.
ANALY1’ES/CRQLs
The parameters included in the analysis and the Contract Required Quantitation Limits (CRQLs)
are listed in Attachment 1.
Revision 1.0
-------
ATI’ACHMENT I (page 1 of 1)
USEPA CONTRACF LABORATORY PROGRAM
STATEMENT OF WORK FOR INORGANIC ANALYSIS
MULTI-MEDIA, HIGH CONCENTRATION
IHC OI.2
TARGET ANALYTE LIST
Analyte
CRQ
(mgfKg,
L
ppm)
80
20
5
80
5
10
80
10
20
40
•
20
•‘
10
..
80
NOTE:
S
Analyte
(m
CRQL
gIKg, ppm)
..
10
‘
0.3
20
S
10
80
20
20
10
,
- -.
1.5
:.
NA
3.0
(pmhos/cm)
• ALL CRQLs ARE BASED ON WET WEIGHT AND APPLY TO SOLID AND LIQUID SAMPLES.
• RESULTS FOR BOTH SOLID AND LIQUID SAMPLES ARE REPORTED AS MGIKG, WET
WEIGHT.
Revision 1.0
-------
TiTLE: USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR ANALYSIS OF POLYCHLORINATED DIBENZO-p-DIOXINS (PCDD)
AND POLYCHLORINATED DLBENZOFURANS (PCD )
MULTI-MEDIA, MULTI-CONCENTRATION
DOCUMENT NUMBER: DFLMO1.2
DOCUMENT DATE: Not Applicable
EFFECTIVE DATES: May 1992 through May 1994
CONCENTRATION: Low to Medium
DATA TURNAROUND: 45 days
MATRICES: Aqueous/Soil/Fly Ash/Chemical Waste
SIGNIFICANT FEATURES
• The parameters include 2,3,7,8-substituted Tetra-, Penta-, Hexa-, Hepta-, and Octachiorinated dibenzo-p-dioxins
(PCDDs) and dibenzofurans (PCDFs).
• Total homologue concentrations are reported for a given level of chlorination (i.e. Total TCDD, Total PCDF, etc.).
• 2,3,7,8-TCDD toxic equivalence is determined using all 2,3,7,8-substituted isomers.
• The dioxins and furans are analyzed by High Resolution Gas Chromatography and Low Resolution Mass Spectrometry
(HRGCILRMS).
Second column confirmation is required if the toxic equivalence is greater than or equal to O.lppb (soil or fly ash), 7ppt
(aqueous) or 7ppb (chemical waste).
• Chemical waste includes oils, stilibottoms, oily sludge, wet fuel oil, and surface water heavily contaminated with oils.
Soil samples include sediment matrices.
REVISIONSIMODIFICATIONS
Revisions DFLMO1. 1 (September 1991) and DFLMOI.2 (April 1992) do not significantly affect data useability.
RECOMMENDED USES
This Contract Laboratory Program (CLP) method is recommended for analysis of polychiorinated dioxins and furans to
define the nature and extent of potential site contamination during Site Investigation (SI) and Remedial Investigation/Feasibility
Study (RIIFS) activities and to verify that Remedial Design/Remedial Action (RDIRA) activities comply with pre-determined
clean-up standards. This method is suitable when a forty five day turnaround for results is adequate. It is recommended for
samples from known or suspected hazardous waste sites where potential contamination may be present at significant risk levels.
This method is not applicable to soil/sediment samples with high moisture content.
ANALYTES/CRQLs
The parameters included in the analysis and the Contract Required Quantitation Limits (CRQLs) are listed in Table 1.
Revision 3.0
-------
TABLE 1
USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR ANALYSIS OF POLYCHLORINATED
DIBENZO-p-DIOXINS (PCDD) AND POLYCHLORINATED DIEENZOF(JRANS (PCDF)
MULTI-MEDIA, MULTI-CONCENTRATION
Dfl.MO1.2
TARGET COMPOUND LIST
Compound .
...
Aqueous
CRQL ....
(ng/L,ppt)
Low Soil
cRQL’
(ugIKg,ppb)
fly Ash .
.cRQLA’
(ug/Kg,ppb) .•
Ch nicaI Waste.
CRQL
(ugfKg,ppb)
TEF?
2 .3j,8 -TcDD
10
1.0
1.0
10
1.0
2,3,7,8 -TcDF
10
1.0
1.0
10
0.10
1,2,3,? 8-PecDF
25
2.5
2.5
25
0.05
1,2,3,7,8-PecoD
25
2.5
2.5
25
0.50
2 ,3 ,4,7,8-PecDF
25
2.5
2.5
25
0.50
1,2 ,3,4 ,7,8-HxcOF
25
2.5
2.5
25
0.10
1,2,3 ,6,7,8-HxcoF
25
2.5
2.5
25
0.10
1,2,3,4 ,T,8 -Hxc OO
25
2.5
2.5
25
0.10
1,2 ,3,6,7,8Kx DD .
25
2.5
2.5
25
0.10
1 ,2 ,3,7.8,cHxco O
25
2.5
2.5
25
0.10
2,3 ,4,6,7,8-HxcDF
25
2.5
2.5
25
0.10
1,2,3,7,8,c-wxcDF
25
2.5
2.5
25
0.10
1 ,2 ,3,4 ,6,7,8-HpcOF
25
2.5
2.5
25
0.01
1.2 ,3.4,6.7 ,8 -11 cDD
25
2.5
2.5
25
0.01
1 ,2,3 ,4,7,8,9-I4pCDF
25
2.5
2.5
25
O.01
ocoo
50
5.0
5.0
50
0.001
O F
50
5.0
5.0
50
0.001
—
Homologue Compounds
Number of Possible Isomers
Number of 2,3,7,8-Substituted Isomers
TOTAL TcDO
22
1
TOTAL T DF
38
1
TOTAL Pe D
14
1
TOTAL PecDF
28
2
TOTAL HxcOD
10
3
TOTAL HXcDF
16
4
TOTAL I4pcOO -
2
1
TOTAL Hp DF
4
2
OCOD
1
1
O cOF
1
1
NOTE:
A. The sample-specific CRQL.S for soil/sediment and fly ash samples will be adjusted for percent moisture and will be higher than
those listed above.
B. TEF = 2,3,7.8-TCDD Toxic Equivalence Factors (TEFs) for the PCDDs/PCDFs.
Revicinn (1
-------
TITLE: SUPERFUND ANALYTICAL METHODS FOR LOW CONCENTRATION WATER FOR ORGANICS
ANALYSIS
DOCUMENT NUMBER: Not Applicable
DOCUMENT DATE: October 1992
EFFECTIVE DATES: December 1992 through June 1994
CONCENTRATION: Low
DATA TURNAROUND: 14 Days
MATRICES: Aqueous
SIGNIFICANT FEATURES
• The parameters include volatile, seinivolatile, and pesticide PCB compounds.
• Volatiles and semivolatiles are analyzed by (3CIMS; pesticidesIPCBs are analyzed by GCIECD.
• All parameters require significantly reduced CRQLS as compared to the OLMO1.9 SOW.
• A 25mL aliquot of sample is purged for volatiles analysis.
• Analysis of a Laboratory Control Sample (LCS) for each parameter is required.
• Analysis of an MS/MSD duplicate pair is n required.
• Seinivolatile and pesticide/PCB samples must be extracted by continuous liquid-liquid extraction procedures.
REVISIONS/MODIFICATIONS
The following is a list of the significant changes from the 6/91 Low Concentration SOW:
The requirement for a diskette deliverable was removed.
• Technical acceptance criteria for the volatile LCS were established.
• Potential action against a laboratory for Performance Evaluation (PE) scores below 75% was added.
RECOMMENDED USES
This Contract Laboratory Program (CLP) method is recommended for broad spectrum analysis to define the nature
and extent of potential low level organic* contamination in water supplies during Site Investigation (SI) and Remedial
InvestigationiFeasibility Study (RJ/FS) activities and to verify that Remedial DesigniRemedial Action (RD/RA) activities
comply with pre-determined clean-up standards. This method attains lower detection limits than SOW OLMO1 .9 and can
aid in the determination of low level contamination in public drinking water supplies. The majority of samples are
expected to be from drinking water and well/ground water sources around Superfund sites. This method is suitable when
a 14 day turnaround for results is adequate.
* This method should not be used for low concentration volatile organics analyses in Region I when comparison to
the drinking water Maximum Contaminant Levels (MCLs) is required. The Region I EPA 524.2 standard
specifications should be utilized for this purpose.
ANALYFES/CRQLs
The parameters included in the analysis and the Contract Required Quantitation Limits (CRQLs) are listed in
- .ttachment 1.
Revision 2.0
-------
AUACHMENT 1 (page 1 of 3)
SUPERFUND ANALYTICAL METHODS FOR LOW CONCENTRATION
WATER FOR ORGANICS ANALYSIS
10/92
TARGET COMPOUND LIST - VOLATILES
COMPOUND
•.CRQL
(ugIL, ppb)
Q 1oromethane
I
Bromornethane
1
Vinyl chloride
1
Chloroethane
1
Methylene chloride
2
Acetone
5
Carbon disulfide
I
1,1-Dichloroethene
I
1,1-Dichloroethane
1
cis-I,2-Dich loroethene
1
trans-I ,2-Dichloroethene
1
Chloroform.
1
1,2-Dichloroethane
1
2-Butanone
5
‘Broniochioromethane
I
I,I,1-Trichloroéthane
1
Carbon tet.rachloride
1
Bromodichioromethane
I
1 ,2-Dichloropropane
1
cis-1,3-Dichloropropene
1
COMPOUND
..CRQL
(ugfL, ppb)
Trichloroethene
1
Dibroniochloromethane
1
1,1,2-Trichioroethane ..
I
Benzerie • . , ..
1
trans-I ,3-Dichloropropene
1
Bromoforni
I
4-Methyl-2-pentanone
5
2-Hexanone
5
Tetrachioroethene
I
1, 1,2,2-Tetrachioroethane
1
1,2-Dibromoethane
I
Toluene
1
Ch lorobenzene
1
Ethylbenzene
1
Styrene
1
Xylenes (Total)
I
1 ,3-Dichlorobenzene
1
I ,4-Dichlorobenzene
I
I ,2-Dichlorobeazene
I
I ,2-Dibromo-3-chloropropane
I
Revision 2.0
-------
ATI’ACHMENT I (page 2 of 3)
SUPERFUND ANALYTICAL METHODS FOR LOW CONCENTRATION
WATER FOR ORGANICS ANALYSIS
10/92
TARGET COMPOUND LIST - SEMIVOLATILES
COMPOUND
CRQL
(aWL, ppb)
Phe 1’”,
5
om hy1)di er
5
2-orcph oL
5
2.Mcthylph io1
5
2.2Y.oxybii(1-chloropropane)
5
4-Methylphenol
5
N-Nitzoeo .di.n-propy [ ftsnino
5
Hcx ch1ox hane
5
Nit obcrw.cnc
5
lsophoronc
S
2.Nitrophcnol
S
2,4-Dimcihy1phcno
5
biz-(2-Ch1o octhazy)mcthanc
5
2.4-Diehlotvpheno [
5
1,2,4-Trichlorobenzcnc
5
Naphth 1cnc
S
4-Chlomathlinc
5
Hcx chIorobuta4icnc
5
4.ChIoro-3-mcthyIpheno
5
2-Methylnaphthalcnc
5
Hexathtlorocyc!opcntadienc
5
2,4,6-Trich1or phcno1
5
2,4,S-Trichlorophcnol
20
2-Chloronaphthelenc
5
2.Nitroazulinc
20
D methy1pht h eIate
5
Accnaphthylenc
5
2,6•D&nitmtoluene
5
3-Nkroanilinc
20
Acenaphthenc
5
COMPOUND
CRQL
(ag/I ., ppb)
2.4 -Diziltrophci oL
20
4-Nitropbcnol -
20
D be üoftu n
5
2,4-DiniLn,toluene
5
Dicthyiphth 1a
5
4-Chlorophcnyl-phcnylether
S
Fluorenc -•
5
4-Nitmanilinc
20
4,6-Dinitro-2-methylphenol
20
N.Niodipcnylaniinc
5
4-BromophcnyI phcny!cthcr-
S
Hcx chLombe ene
5
Pcnt chIorophcno1
20
Phcnanthrenc
5
Anthraccoe
5
Di-n•butyiphthalazc
5
Ftuor nthcnc
5
Pyrenc
5
Bu tb y1pt th ie..
5
3,3’-DichIombc dinc
5
Bea)anLhr ccnc
5
Chiyscnc
5
bii(2-cthythcxyl)phthelaxc
5
Di .n-octytphthalatc
5
Bcnzo(b)fluoranthene
5
Benzo(k)fluorenthene
5
Bcnzo(a)pyz no
5
Indenc(1,2,3-cd)pyrenc
S
Dibenzo(a,h) nthrftccnc
5
3enzo(g .h, )pcrylenc
5
Revision 2.0
-------
ATTACHMENT I (page 3 of 3)
SUPERFUND ANALYTICAL METHODS FOR LOW CONCENTRATION
WATER FOR ORGANICS ANALYSIS
10/92
TARGET COMPOUND LIST - PESTICIDE/PCB
PARAMETER
..
CRQL
(ugfL, ppb)
alpha-BHC.
0.01
beta-BHC
0.01
delta-BHC
0.01
gamma-BHC (Lindane)
0.01
Heptachlor’ ..
0.01
Aldrin
0.01
Heptachior epoxide
0.0!
Endosulfan I •.
0.01
Dieldrin
0.02
4,4’-DDE
0.02
Endrin
0.02
Endosulfan H
0.02
4,4’-DDD
0.02
Endosulfan sulfate
0.02
AR F1E1L
CRQL
(ug , ppb)
4,4’-DDT
o.o2
Methoxychlor
0.10
Endrin ketone
0.02
Endrin aldehyde
0.02
a!pha- hIordane
o.oi
gama-ailordane
0.01
Toxaphene
1.0
Aroc lor- 1016 . ‘
0.2
,Aroclor-1221
0.4
Aroclor-1232
0.2
Aroclor- 1242
0.2
Aroclor-1248
0.2
Aroc lor-1254
02
Aroclor-1260 ..
0.2
Revision 2.0
-------
TITLE: USEPA CONTRACT LABORATORY PROGRAM
WATER QUALITY PARAMETERS (WQP) IN MULTI-CONCENTRATION WATER
DOCUMENT NUMBER: Not Applicable
DOCUMENT DATE: June 1993
EFFECTIVE DATES: July 1993 through June 1994
CONCENTRATION: Low to Medium
DATA TURNAROUND: 14 Days or 35 Days
MATRICES: Aqueous
SIGNiFICANT FEATURES
• The parameters include Alkalinity, Ammonia-Nitrogen, Total Organic Carbon (TOC), Chemical Oxygen
Demand (COD), Chloride, Nitrate/Nitrite, Total Phosphorous, Total Dissolved Solids (TDS), Total
Suspended Solids (TSS), and Sulfate.
• Ion chromatography may be used in place of conventional methods for the determination of Chloride,
Nitrate/Nitrite, Phosphorous, and Sulfate.
• The laboratory IDL for a parameter may exceed the CRDL if the sample concentrations are greater than
5xIDL.
REVISIONS/MODIFICATIONS
The following is a list of the significant changes from the 2/93 version that are incorporated in the 6/93 SOW:
• The CRDL for Total Dissolved Solids was elevated from 4,000 ug/L to 10,000 ugIL.
• The analysis procedure for Total Organic Carbon (I’OC) was changed from following a step-by-step
procedure for calibrating and standardizing the TOC analyzer to performing these functions according to
the manufacturer’s specifications.
RECOMMENDED USES
These Contract Laboratory Program (CLP) methods are intended for use only with aqueous samples.
They are recommended for analysis of selected water quality parameters to define the nature and extent of
potential site contamination during Site Investigation (SI) and Remedial lnvestigationiFeasibility Study (RI/FS)
activities and to verify that Remedial Design/Remedial Action (RD/RA) activities comply with pre-determined
clean-up standards. These methods may also be used for monitoring the wastewater treatment processes of
pretreatment plants and Publicly Owned Treatment Works (POTWs). These methods are suitable when a 14 day
or 35 day turnaround for results is adequate. They are recommended for samples from known or suspected
hazardous waste sites where potential contamination may be present at significant risk levels.
ANALYTES/CRDLs
The parameters included in the analysis and the Contract Required Detection Limits (CRDLs) are listed
in Attachment 1.
Revision 2.0
-------
ATTACHMENT 1
USEPA CONTRACT LABORATORY PROGRAM
WATER QUALITY PARAMETERS (WQP) IN MULTI-CONCENTRATION WATER
6/93
PARAMETER LIST - WATER QUALITY PARAMETERS
PARAMETER
CRDL (ugfL, ppb)
Alkalinity
2000
Ammonia-Nitrogen
1000
Total Organic Carbon (TOC)
100
ChemIcal Oxygen Demand (COD)
3000
Chloride
2000
NitratelNitrite
100
Total Phosphorous
100
Total Dissolved Solids (TDS)
10000
Total Suspended Solids (TSS)
4000
Sulfate
2000
Revision 2.0
-------
TITLE: USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR INORGANICS ANALYSIS
MULTI-MEDIA, MULTI-CONCENTRATION
DOCUMENT NUMBER: ILMO4.0
DOCUMENT DATE: Not Applicable
EFFECTIVE DATES: August 1995 through May 1999
CONCENTRATION: Low to Medium
DATA TURNAROUND: 14 Days or 35 Days
MATRICES: Aqueous/So ilJSediment ’
SIGNIFICANT FEATURES
• Analyses are suitable for aqueous, soil or sediment samples at low to medium concentration levels.
• Metals except mercury are analyzed by furnace AA, flame AA, and/or ICP-AES; mercury by cold vapor AA; and cyanide
by spectrophotometry after distillation.
RECOMMENDED USES
This Contract Laboratory Program (CLP) method is recommended for broad spectrum analysis to define the nature and
extent of potential site contamination during Site Investigation (SI) and Remedial Investigation/Feasibility Study (RIIFS)
activities and to verify that Remedial Design/Remedial Action (RDIRA) activities comply with pre-determined clean-up
standards. This method is suitable when a 14 day or 35 day turnaround for results is adequate. It is recommended for samples
from known or suspected hazardous waste sites where potential contamination may be present at significant risk levels.
* This method is not applicable to soil/sediment samples with high moisture content.
REVISIONSIMODIFICATIONS
The following is a list of significant changes from the SOW ILMO3.0 that are incorporated in the SOW ILMO4.0:
• New procedure The lab must measure the sample shipping cooler temperature at time of sample receipt using the cooler
temperature indicator bottle, if present, located in the cooler. The lab must contact CLASS if the cooler’s temperature
exceeds 10°C.
• If dissolved metals are required by the EPA Regional offices and there are no instructions on the Traffic Report, the lab
must digest the samples designated as dissolved metals.
• If elements (e.g., As, Pb, Se, TI) traditionally analyzed by GFA.A are analyzed by ICP, the spiking levels for Furnace AA
must be used (provided the ICP IDLs are CRDL).
• Additional analysis frequency requirement for IC? CRDL and ICS standards: also analyzed at a frequency of not greater
than 20 analytical samples per analysis run.
• For analytes with CRDLs 1O .tgfL, IC? ICSA results must be within ±2x CRDL of the true value; otherwise, these
analytes must be analyzed using an alternate method (e.g., GFAA) for samples analyzed since the last compliant ICSA.
• For analytes with CRDLS l0 .igfL, the ICP ICSA results must be reported from an undiluted sample analysis.
• Independent ICP Interference Check Samples: Elements As, Sb, Se, TI were added (0.1, 0.6, 0.05, and 0.1 mgfL,
respectively); Ag and Pb conc ntrat ions were lowered (0.2 and 0.05 mgfL, respectively).
• Alternate methods for catastrophic IC? failure are no longer included.
• Cyanide spiking concentration for aqueous and soil matrix spikes: 100 jigfL in the distillate (i.e., the final sample solution
prepared for analysis), regardless of the amount of sample used.
• Mercury - clarification of the CRDL standard requirement in the calibration curve for manual cold vapor AA; a linear
regression equation must be used for automated cold vapor AA analysis.
ANALYTES/CRDLS
The parameters included in the analysis and the Contract Required Detection Limits (CRDLs) are listed in Attachment 1.
Revision 0, 7/22/96
-------
ATTACHMENT I
USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR INORGANICS ANALYSIS
MULTI-MEDIA, MULTI-CONCENTRATION
ILMO4.0
TARGET ANALYTE LIST
NOTE:
Analyte
Aqueous
CRDL
(ugfL, ppb)
Soil
CRDL
(mg/kg, ppm)
Aluminum
200
40
Antimony
60
12
Arsenic
10
2
Barium
200
40
Beryllium
5
1
Cadmium
5
1
Calcium
5000
1000
Chromium
10
2
Coba [ t
50
10
Copper
25
5
Iron
100
20
Lead
3
0.6
Ana lyte
Aqueous
CRDL
(ugIL, ppb)
Soil
CRDL
(mgfkg, ppm)
Magnesium
5000
1000
Manganese
15
3
Mercury
0.2
0.1
Nickel
40
8
Potassium
5000
1000
Selenium
5
1
Silver
10
2
Sodium
5000
1000
Thallxum
10
2
Vanadium
50
10
Zinc
20
4
Cyanide
10
2.5
• The CRDLs for soils are based on the following: for all metals (except mercury) - I gram sample, 200 mL final digestate
volume, and 100% solids; for mercury - 0.2 gram sample, 100 mL final sample solution volume, 100% solids; and for
cyanide - I gram sample, 250 mL final distillate volume, 50 mL of distillate taken for manual spectrophotometric
determination, and 100% solids.
The sample-specific CRDLs for soiVsediment samples will be adjusted for percent solids and will be higher than those
listed above.
Rcvision 0, 7/22/96
-------
TITLE: USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR ORGANIC ANALYSIS
MULTI-MEDIA, MULTI-CONCENTRATION
DOCUMENT NUMBER: OLMO3.2
DOCUMENT DATE: Not Applicable
EFFECTIVE DATES: July 1994 through February 1999
CONCENTRATION: Low to Medium
DATA TURNAROUND: 14 Days or 35 Days
MATRICES: Aqueous/Soil/Sediment’
SIGNIFICANT FEATURES
• The parameters include volatile, sernivolatile, and pesticidefPCB compounds.
• Volatiles and semivolatiles are analyzed by GCIMS; pesticidesfPCBs are analyzed by GC/ECD.
• Major Tentatively Identified Compounds (TICs) are reported for GCIMS analyses.
• All pesticideIPCB analyses require second column contirmation by GCIECD. PesticidefPCB compounds are confirmed
by GCIMS if they are of sufficient concentration to be detected by GCIMS (Concentrations in the sample extract at or
above 10 ng/ .xL for pesticides, 50 n Jj.iL for Aroclors, or 125 ng.4xL for Toxaphene should enable the lab to confirm by
GC/MS analysis)
RECOMMENDED USES
This Contract Laboratory Program (CLP) method is recommended for broad spectrum analysis to define the nature and
extent of potential site contamination durmg Site Investigation (SI) and Remedial Investigation/Feasibility Study (RIJFS)
activities and to verify that Remedial Design/Remedial Action (RDTRA) activities comply with the pre-determined clean-up
standards This method is suitable when a 14 day or 35 day turnaround for results is adequate. It is recommended for
samples from known or suspected hazardous waste sites where potential contamination may be present at significant risk
levels.
* This method is not applicable to soil/sediment samples with high moisture content.
REVISIONSIMODIFICATIONS
The following is a list of significant changes from the SO\V OLMO1.9 SOW that are incorporated in the SOW OLMO3.I
(including revision OLMO3.2):
Volatiles
• Medium level soiVsedunent extract and purge solution preparation procedures were revised for the method blank,
MSIMSD, and samples.
• Minimum sample amount for low level soil/sediment analysis was lowered to 0.5 g.
• Minimum initial and continuing calibration Relative Response Factor (RRF) for 1,1,2,2-Tetrachloroethane was lowered to
0.300.
• In addition to % recovery criteria, System Monitoring Compounds are evaluated based on Relative Retention Time
(RRT) criteria.
• The concentration of Methylene Chloride in method, storage, and instrument blanks must be less than 2.5 times the
CRQL.
Semivolatiles
• Low level soil CRQLs were changed from 800 uglkg to 830 ug/kg for the following compounds: 2,4,5-Trichlorophenol,
2-Nitroaniline, 3-Nitroaniline, 2,4 Dinirrophenol, 4-Nitrophenol, 4-Nitroaniline, 4,6-Dinitro-2-methylphenol, and
Pentachlorophenol.
• The minimum RRF for initial and continuing calibrations for Acenaphthylene and Acenaphthene was changed to 0 900
• The RRT of each surrogate must be within ± 0.06 RRT units of its RRT in the continuing calibration standard. The
sample(s) must be reanalyzed if the RRT criteria are not met.
• The GPC blank must contain target compounds at less than the CRQL, except phthalate esters (less than 5 times the
Volatiles and Sernivolatiles
• GCIMS Performance Check: Back round subtraction must be performed using a single scan acquired no more than 20
scans prior to the elution of BFB (VOA) or DFTPP (SVOA).
• The number of volatile organic TICs was raised from 10 to 30; the number of semivolatile organic TICs was raised from
20 to 30. Alkanes are searched and summed separately (not included in the 30). For both fractions, the data collection
window is specified as 30 sec before the first target analyte and 3 mm after the last target analyte.
• The non-TCL library search is performed using NISTIEPAJNIH (1992 or later) and/or Wiley (1991 or later) or
equivalent.
I of 2 Revision 0, 7/22/96
-------
PesticidesIpCBs
• Packed columns must not be used for analysis.
• Initial and continuing calibration PEM Resolution Criteria are 90%; %D criteria are -25% and 25%.
• Initial calibration %RSD criteria are < 20% except for alpha-BHC and delta-BHC which are 25%
• PEMs, INDAs, INDBs and instrument blanks must meet initial calibration criteria.
• Surrogate advisory limits are 30-150%. Method blank surrogates must meet criteria.
• Detailed Sulfur Cleanup Blank preparation and QC acceptance/corrective action procedures were added.
Semivolatiles and Pesticides/PCBs
• Continuous LIL extraction procedures with and without hydrophobic membranes are provided for sample preparation.
• GPC calibration solution concentrations changed for bis(2-Ethylhexyl)phthalate (0.5 mg/mL) and Methoxychlor (0 1
mg/mL).
All Fractions
• The lab must measure the sample shipping cooler temperature at time of sample receipt using the cooler temperature
indicator bottle, if present, located in the cooler. The lab must contact CLASS if the cooler’s temperature exceeds 10°C.
• Specifications for analysis of multiphase samples are included.
• Detailed requirements were added for sample collection and preservation, standard analysis and documentation, and
corrective actions for individual standards, mixture standards, and blanks.
• The MSIMSD are analyzed and reported at the same dilution as the least dilute sample for which the original sample
results are reported
The following are significant changes from the OLMO3.0 or OLMO3 1 revision that are incorporated in the OLMO3.2
revision:
Semivolatiles Limits number of searched alkanes to 20 suspected alkane peaks of greatest apparent concentration
Alkanes are not counted as part of the 30 TICs.
• Semivolatiles Revised for clarification - if Internal Standard (IS) recoveries were outside criteria for a sample used for
the MSI?VISD, reanalysis of the sample extract is required only if IS recovery criteria were met in both the MS and
MSD.
PesticidefPCB. The pesticide GPC calibration check solution contains Endrin and Dieldrin at 0.5 ug.’rnL for a 2 mL
GPC loop; the Aroclor mixture contains Aroclor 1016 and Aroclor 1260 in methylene chloride at 0.5 u .’mL for a 2 mL
GPC loop.
All fractions Ampulated standard solution extracts in lass vials may be used until the manufacturer’s expiration date,
or 2 yrs from preparation date if no manufacturer’s expiration date is provided.
ANALYTES/CRQLs
The parameters included in the analysis and the Contract Required Quantitation Limits (CRQLs) are listed in Anachit
2 of 2 Rcv sion 0, 7/22/96
-------
Analytical Services Available Through Superfund’s Analytical Operations
Branch/Contract Laboratory Program (CLP)
e Analytical Operations Branch of the Hazardous Site Evaluation Division has 18 analytical services available to
variety of needs for Superfund decision-making. The following table shows types of analyses available,
atemertt of work and fact sheet numbers, dates, turnaround times, lower limit of required quantitation, and uses,
nitations, average costs, and monthly laboratory capacity. For additional information about a specific service.
cluding target analytes, consult the method-specific fact sheet or call your Regional Sample Control Coordinator or
.2 Technical Project Officer, or call the Analytical Operations Branch on (703) 603-8870.
nalytical Services for Superfund August 1993
Type of Anuitysi. Stats.
of wor)c No.,
Sheet Numb;r or Detel
Data
oun4
limets)
Lowei Umitof Required Ouantitaticn t
.
..
•“ S
Full Orgaruca. Volatile..
Semivolatilas. Pesticides
in Water and Soil
(OLMO 8. 9240 0-O8FS)
Low concentration
Volatile . Semivolatiles.
Pesticides in Water (SOW
Rev. 10/92. 9240.0-
1OFSI (available in SAS)
-
35 days
14 days
WATER:
Vo : 10 pg/I
S , vcJati 10-25 pg/I
P c . 0 05.0.10 pg/I. except
methoxychlor 0.5 pg/I: Aroclors 1-2
pg/I. toxaphene S pg/I
SOILS:
Vda øs: Low conc. 10 pg/Kg: medium
conc. 1.200 pg/Kg
S iivolarI : Low conc. 330-800
pg/Kg. medium conc 10.000-25,000
pg/Kg
Pes dd : 1.7-3.3 pg/Kg. except
methoxychlor 17 pg/Kg: Aroclors 33-67
pg/Kg. toxaphene 170 pg/Kg
! : To determine extent of organic. contamination;
asses potential for risk to human health and environment;
determine appropriate clean-tip action; determine when
remedial action. are complete; determine absence of
organic contaminants.
LIMITATIONS: Main survey method to determine general
organic. concentration. Use for other than low
concentration ground and drinking water samples. For
suspected high hazard samples, use high concentration
organic method.
AVE COST: $ 790 per sample (35.day; all fractions)
$1,355 per sample (14.day; all fractions)
CAPACITY: 4.300 samples per month (35-day)
700 samples per month (14.day)
14 days
WATER:
Vol ,ta o. 1 pg/I (ketones 5 pg/I)
Sb at 5-20 pg/I
P ddcs 0.01-0.02 pg 11. except
methoxychlor 0.1 pg/I: Aroclors 0 2-0.4
pg/I. toxaphene 1.0 pg/I
iJg : To determine extent of well/ground Water contam-
Inatien; assess potential for risk to human health;
determine appropriate clean-up actions; determine when
remedial actions are completed; determine absence of
organic contaminants.
LIMITATIONS: Use only for drinking/ground water type
samples when concentrations for undiluted samples are
not expected to exceed the upper limit of the calibration
curves as follows: 25 pg/I for volatile.. 80 pg/I for
samivolatiles, and 0.32 pg/I for pesticides except for
Aroclors 6.4 pg/I and toxaphene 16 pg/I.
AVE COST: $675 par sample tall fractions)
$135 per sample (VOA only)
CAPACITY: 50 samples per month (all fractions)
100 sampleu per month (VOA only)
DioxunelFurene in Water.
1 y Ash. Soul, and Waste
DFLMO1.1. 09240.0-
17FS)
45 days
WATER: 0.0 1-0 05 pg/I
FLY ASH: 1-5 pg/Kg
SOIL: 1-5 pg/Kg
WASTE 10-50 pg/Kg
To determine extent of dioxin/furan contamination.
assess potential for risk to human health and
environment: determine appropriate clean-up actions.
determine when remedial actions are complete: determine
absence of dioxin/furan contaminants.
LIMITATIONS: Use only for specified matrices. analytes.
and concentrations.
AVE COST: $635 per sample
CAPACITY: 50 cample per month
I The required quantitatuon level us a range of quantitatlon levels for enalytes In a service. See the fact sheet for analyte- and
technlque.specufic information.
-------
T ’pa el Analysis
(Statement of Wo k No..
Pact SheetNumber r
Dater
Rapid Turnaround Dioxins
in Solids. Asphalt. Water.
Air and Wipe (SOW Rev.
11/92)
40 hours
(electronic.
air)
7 days
(hardcopy)
CAPACITY : 3.600 samples per month
Quick Turnaround
Organics in Water.
Soil/Solid. Wipe
(QTM SOW Rev. 2193.
Draft Fact Sheet 7/93)
(available in SAS)
lnorgsnics. Total Metals.
Dissolved Metals.
Cyanide in Water and Soil
(ILMO3 0.9240 0 09FS)
Toxicity Characteristic
Leaching Procedure
(TCLP SOW Rev 6/93)
(available in SAS)
WATER :
PARs: 20 pg/I
Pf, ,dt 5Opg/L
A,odozz 1-2p 9 /L (toxaphene 5pgIL)
Peztiddes: 0.1 pg/L
V a es: 20 pg/I
SO ILISOLID :
PARs: 330 pg/Kg
Pf io s: 830 pg/Kg
Arodorz: 17-33 pg/Kg (toxaphene 83
pg/Kg)
Pes 1.7 pg/Kg
Va/atlas: 40 pg/Kg
WATER :
ToW metals, Di, solved metals:
3-60 pg/I (Hg 0.2 pg/LI
(Al 200 pg/LI; (Ca, K. Mg. Na 5,000
pg/LI
Cyar dc 10 pg/I
SOIL:
ToW metals. 600-10’ pg/Kg
(Hg 100 pg/Kg)
Cyea/dc. 1.000 pg/Kg
ORGANICS
Volatlas, Semnivolaties: 50 pg/L
(pentachiorophenol and 2.4,5
trichlcrophenol 125 pg/I)
Pasv es: 1 0 pg/I tg.BHC 0 5 pg/I),
(toxaphene 50 pg/LI
METALS
1 00-200 pg/I
(Pd. Hg 40-60 pg/I, Ba 4.000 pg/LI
To address organics situations requiring a quick
answer or on-site feedback; to direct sampling efforts.
monitoring well placement; selection of screen intervals.
to monitor cleanups and treatments for effectiveness
LIMITATION : Service is most effective when contamin-
ants of concern are known or suspected and can be
focused on analyte(s) or fraction(s) of concern. Use with
the full organics service.
AVE COST : $250 per fractional analysis
CAPACITY : 90 fractional analyses per day
2.160 fractional analyses per month
To determine extent of inorgartics contaminati
assess potential for risk in human health and
environment; determine appropriate dc an-up action;
determine when remedial actions are complete; determine
absence of inorganic contaminants.
LIMITATIONS Main survey method to determine general
inorganics concentration. Use for other than low
concentration ground and drinking water samples. For
suspected high hazard samples, use high concentration
inorganic method.
AVE COST . $109 per sample (35-day)
$165 per sample (14-day)
CAPACITY : 4.600 samples per month (35-day)
900 samples per month (14-day)
Determination of toxicity characteristic for disposol
of waste.
LIMITATION Quantitation limits are highly matrix-
dependent.
AVE COST . Organics $675 per sample (all frac:ions)
lnorganics: $135 per sample
CAPACITY Organics 50 samples per month
Inorganics SO samples per month
Data
Turnaround
T imete
Lower Limit of Require uantitation
Usee /LimnitetionsICo ts/Capechy
16 hours
(electronic)
SOLIDS : 0.3 pg/Kg
ASPHALT : 0.7 pg/Kg
WIPE. WATER. AIR : 1.0 ng!sample
USES: T 0 address dioxin situations requiring a quick
answer or on-site feedback; Identify critical samples for
confirmatory analyses; optimize analysis conditions for
confirmatory analyses.
LIMITATIONS : Use only for samples likely to contain low
level dioxin and when data are needed quickly
AVE COST : $166 per sample
48 hours
(electronic)
7 days
(hardcopy)
validated
data
35 days
14 days
35 days
-------
..Low Limitof R.quiröd Cu: tita4on
1urnarou d ‘ .:
PARAMETER
AlL a. S04 2.000 pg/I
TOC. Fi 7? 100 pg/I
NH3 1.000 pg/I: COD 3.000 pg/i.
TSS 4.000 pg/i.; TDS 10.000 pg/I
USES: To determine water quality; determine appropriate
clean-up actions: determine when remedial actions are
complete; determine presence or absence of water quality
parameters.
LIMITATIONS : Use when water samples contain low or
medium levels of up to 10 water quality parameters.
Quantitation limits are highly matrix-dependent.
AVE COST : $215 per sample (all parameters)
CAPACITY : 250 samples per month
UQUID, SOLID. AND MULTIPHASE :
Totdmct&fs S,000-80.000 .ug/Kg (for
Hg 300 p91kg)
Cyais dc 1.500 pg/Kg
USES: To determine extent of high level contamination;
determine drum contamination. asseec potential for risk to
human health and environment; determine appropriate
clean-up actions; determine presence or absence of high
levels of inorganic Contaminants.
LIMITATION : Use for determination of other than low or
medium Concentration inorganic contaminants.
AVE COST $95 per sample
CAPACITY : 100 samples per month
oncentration
.ics in Water -
Immiscible Liquids and
Solids (SOW Rev. 9/88
and 4/89) (available in
SAS I
LIQUIDS and SOLIDS :
Vdat es: 2.5-5.0 mg/Kg
Exüactabies 20-200 mg/Kg
A,odors 10mg/Kg
Toxapbcno 50 mg/Kg
USES: To determine extent of high level contamination;
determine drum Contamination; assess potential for risk to
human health and environment; determine appropriate
clean-up actions; determine presence or absence of high
levels of organic contaminants
LIMITATIONS . Use for determination of other than low or
medium concentration organic contaminants.
AVE COST - $650 (all fractions)
CAPACITY . Project.specific requests
Low Concentration Total
Metals. Cyanide. Total
Nitrogen, fluoride in
Water (7/92 Draft.
9240 0-1 iFS)
lavailable in SAS)
WATER :
Totdmet.als: 1-10 pg/I (Hg 0.2 pg/I)
(As. Ni. Zn 2Opg/L: Fe 100 pg/i.)
(Ca. Mg. Na 500 pg/I; K 750 pg/I)
Cyst lOpgIL
Tot Nit. 100 pg/ I
Rtaodde: 200 pg/I
USES: To determine extent of well/ground water
contamination: assess potential for ri;k in human health.
determine appropriate clean-up actions; determine when
remedial actions are complete; determine absence of
inorganic Contaminants.
LIMITATIONS . Use only for drinking/ground water type
samples when concentrations for undiluted samples are
not expected to exceed the upper limit of the calibration
curves: 200 pg/I for Hg. 200-400 pgFL for cyanide.
I mg/I for total nitrogen. 1000 mg/I for fluoride, and for
the following analytes using flame AA - 7 mg/i. for Ca.
0 5 mg/I for Mg. 2 mg/I for K, and 1 mg/I for Na For
analytec not described above, no upper calibration limit is
specified
AVE COST $215 per sample
CAPACITY : Project.specific requests
Type OFAnaIytis.. t ta.
m iitofWcrkNo, .’Fec*
Number ot Date
Multi-Concentration
Water Quality Parameters
(SOW Rev. 7/93. Draft
Fact Sheet 8/93)
(available In SAS)
14 days
¶J,s Limit oflsJCoqts /Ce acity -
High Concentration Total
Metals and Cyanide in
Liquid. Solid, and
Multiphaso Samples
(IHCO1.2. 9240 0-I 6FS)
35 days
35 days
14 days
-------
General Radiochemical
Analytical Services
Protocol in Water and Soil
(GRASP SOW Rev
6/1/92)
(available in SAS)
WATER
Cross Alpha: 3 pCi/I
GrossHeta ’ 2pCi/L
Metals: 0.05 pCi/I (for Ra. Sr.90
1 pCi/I: Cs-137 10 pCi/I; 1 1.000
pCi/I)
SOIL/SEDIMENT
Metals: 0.05 pCi/g (f or Re. Sr-90
0.1 pCi/c)
. To determine presence or absence of radioactivity;
assess potential for risk in human health and
environment; determine appropriate clean-up action;
determine when remedial actionS are complete
LIMITATION : Main survey method to determine general
radioactivity
AVE COST : S 1.300 per sample (all analylesi
CAPACITY : Project-specific requests
.‘
lyp. olAnatysic (Slate
enl of Work No., tact
Shoe; Number or Date)
Data
Turnaround
1im6fe
Lower Limit bt Required Ouanl tat*On
:
-.
Uses /LumitationtiCoete/C P C itV
••
ORGANICS:
Tenax 2-48
To determine extent of contamination; assess
Vola& s: Canister 2-5 ppbv.
potential for risk In human health and environment;
Analysis of Ambient Air
ng on column
37-183 ng/m 3
determine appropriate clean-up action; determine when
(SOW Rev. VCAAO1.0,
S m’vola , p a a :
remedial actions are complete; determine presence or
VTAAO1.0.SVAA O1.0
35 days
absence of air contamination.
and MAAO1.0. 9240 0-
INORGANICS:
1-lO9ng/m’
15FS)
Total
LIMITATIONS: fVolatiIe ) For canister, insufficient flow
( vaulable in SAS)
rates and sampling times may prevent collection of
sufficient quantity of sample, for Tenax, certain analytes
are not captured.
AVE COST $700 per sample (organics)
$375 per sample (metals)
CAPACIIYI. Project-specific requests
45 days
-------
Analytical Services Available Through Superfund’s Analytical Operations
Branch/Contract Laboratory Program (CLP)
Analytical Operations Branch of the Hazardous Site Evaluation Division has 18 analytical services available to
-eera variety of needs for Superfund decisionmaking. The following table shows types of analyses available.
atement of work and fact sheet numbers, dates, turnaround times, lower limit of required quantitation. and uses.
mitations. average costs, and monthly laboratory capacity. For additional information bout a specific service.
c!uding target analytes, consult the method-specific fact sheet or call your Regional Sample Control Coordinator or
‘LP Technical Project Officer, or call the Analytical Operations Branch on (703) 603-8870.
.Ji Organic.. Volatiles,
amIvoIetAles, Pesticide.
Water and Soil
.LMO.8, 9240.O-O8FS)
.w conc.ntratlon
Volatile.. S.mivotatlis.,
‘estictdes In Water (SOW
t.v. 10192. 9240.0-
1OFS)
Availabi. as HQ Multi-
Cient SAS
• •%
Dtta <
.)• .. , .S • SC
Tunwoun4
oR qirired O 1tstt i
C, c .4
% ‘ - .••-‘ “ . __% .
. 4 ,
WATER :
Vd .r. lOpg/L
S su .tJ 10-25 pg/I
Peztiddes: 0.05-0.10 pg/I. except
methoxychlor 0.5 pg/I; Aroclors 1-2
I pg/I. toxaphene S pg/I
SOILS :
V aiiar Low cone. 10 pg/Kg; medium
cone. 1.200 pg/Kg
Sw,ivo .tI.s Low cone. 330-800
pg/Kg; medium cone. 10.000-25.000
pg/Kg
P 1.7-3.3 pg/Kg, except
m.thoxychlor 17 pg/Kg; Arodori 33-67
pg/Kg, toxaphens 170 pg/Kg
WATER :
V !ati 1 pg/I (ketones S pg/I.)
$ ev vtI 5-20 pg/I
P 6 0.01-0.02 pg/I. except
m.thoxychlor 0.1 pg/I; Arcciors 0.2-0.4
pg/I. toxaphen. 1.0 pg/I
October 1993
C
* ‘ .V . •: •. c . :.. .<‘•4.. .. C....
USES: To determine extent of organic. contamination;
isses potontlaJ for risk to human health and environment;
determine appropnat. dean-up action: determine wh.n
remedial actions ar. complete; determine absenc. of
organic contaminants.
UMITAT1ONS : Main survey method to determin, general
organics concentration. Us. for other than low
concentration ground and drinking water samples. For
suspected high hazard samples, use high concentration
organic method.
AVE COST : 8 790 per sample (35-day. eli fractions)
8 1,355 per sample (14-day all fractions)
CAPACITY : 4.300 samples per month (35-day)
700 samples per month (14-day)
To determin, extent of weUlground wat.r contam-
ination: assess potential for risk to human health;
d.termin. appropriate dean-up actions; d.termin. when
remedial actions are completed; determine absence of
organic contaminants.
LIMITATIONS : Use only for drinking/ground water type
samples when concentrations for undiluted samples are
not expected to exceed th. upper limit of the calibration
jrvs. is follows: 25 pg/I. for volatile.. 00 pg/I for
s.mivolatllos. and 0.32 pg/I for pesticides except for
Aroclors 6.4 pg/I. and toxaphen. 16 pg/I.
AVE COST : $675 p.r sample (all fractions)
8135 per sample (VOA only)
CAPACITY : 50 samples per month (eli fractions)
100 samples per month (VOA only)
I Tb. required quantitation level I. e rang. of quanthatlon levels for enalyt.s In. service. See th. fact sheet for analyt.. end
t.chnlque-ep.cfllc Information.
..nalytical Services for Superfund
• . ••• •
T.,p Øf An Fe tStet6
‘iflt Df WQ’k No. .F,ct
aet
35 days
14 days
,vaiiable in RAS
14 days
WATER: 0.01-0.05 pg/I
USES: To determine extent of dioxin/furan contamination;
assess potential for risk to human h.alth and
FLY ASH: 1-5 pg/Kg
environment; determine appropriate clean-up action.;
ioxan ./Furans In Water.
determine when remedial actions are complete: determine
y Ash. Soil. end Waste
45 days
2!k: 1-5 pg/Kg
absence of dioxin/furan contaminants.
OFLMO1.1, 09240.0-
7FS)
WASTE: 10-50 pg/Kg
LIMITATIONS: Us. only for specified matrices. analytes,
and concentrations.
— in RAS
AVE COST: $635 per sample
CAPACITY: 50 samples per month
-------
Type ol Aneiyeie ..
fStatamont of %‘Vork No
c Shs4tNwnberor
Detel. . -, .
Data
Turnaround
T1ms (d
‘t ow.rLimii of Requi ed Quanti ation
. . . . . . . •.
.. ‘S..
Use. nitati is/Costs/Capacity ..
. .. ..ç
.. .: .. ..
Rapid Turnaround Dioxin.
in Solids. Aephalt. Water.
Air and Wipe (SOW Rev.
11/92)
Available in RAS
16 hours
(e lecironicl
40 hours
(electronic.
air)
7 days
(hardcopy)
SOUDS: 0.3 pg/Kg
ASPHALT: 0.7 pg/Kg
WIFE, WATE,:l. AIR: 1.0 nglsampla
! : To address dioxin situations requiring a quick
answer or on-sits feedback; Identify critical samples to
confirmatory analyses: optimize analysis Conditions for
COflfWmatOIy analyses.
LIMITATIONS: Use only for samples likely to contain Ic
level dioxin arid when data are needed quickly.
AVE COST: $166 per sample
CAPACITY: 3.600 samples per month
Quick Turnaround
Organic. in Water.
Soil/Solid. Wipe
CQTM SOW Rev. 2193.
Draft Fact Sheet 7/93)
Avøil ble as HQ Multi-
Client SAS
48 hou,s
(electronic)
7 days
(hardcopyl
validated
data
WATER:
PAJis 2Opg/L
enois: 50 pg!l..
A,o ...o, : 1-2pglL (toxaphene Spg/U
PesDddoJ : 0.1 pgIL
VoI.tic: 20 ig/L
SOIL/SOLID:
PA&: 330 pg/Kg
?ha,& 830 pg/Kg
Aj’odor 17.33 pg/Kg (toxaphene 83
pg / Kgl
P dd 1.7 pg/Kg
Vth ez 40 pg/Kg
USES: To address organic, situations requiring a quick
answer or on-site feedback; direct sampling efforts;
locate sampling areas; monitor the placement of wells.
select screen intervals; monitor cleanupe and treatmen
for effectiveness. Can be used to c.ritorPRP activiti.
end provide foedback at public meetings.
LIMITATION: Service is most effective when contarnin
ants of concern are known or suspected arid can be
focused on enelyte(s} or lraction(sl of concern. Use wi
the full organic. service.
AVE COST: $250 par fractional analysis
CAPACITY: 90 fractional analyses per day
2.160 fractional analyses per month
Inorganica. Total Metals.
Dissolved Metals.
Cyanide in Water and Soil
(ILMO3.O.9240 0- 09F 5)
Available in RAS
35 day.
14 days
WATER;
ToWme r. Dizsa’vedmef4s-
3.60 yg /L (Hg 0.2 pg/U
(Al 200 pg/Li: (Cs. K. Mg. Na 5.000
pg/Li
4’.,ad. lOpg/L
.Q [ i:
Tor .dm .iis- 600-10’ pg/Kg
(Hg 100 pg/Kgl
C ra,p de 1.000 pg/Kg
USES: To determine extent of inorganics contaminatior
aesess potential for risk in human health and
environment: determine appropriate clean-up action;
determine when remedial actions are complete: determ
absence of inorganic ccn amirants.
LIMITATIONS: Main survey method to determine goner
inorgenics concentration. Use for other than low
concentration ground and drinking water samples. For
suspected high hazard samples, use high concentratior
lziorganic method.
AVE COST: $109 per sample (35dayl
$165 per sample (14-day)
CAPACITY: 4.600 samples per month (35-dayl
900 samples per month (14.day
Toxicity Characteristic
Leaching Procedure
ITCLP SOW Rev. 6/93)
Available as HQ Multi-
Client SAS
35 days
ORGANICS
Senilvolath’es: 50 pg/i.
(penrachlorophenoi and 2.4.5-
lrichlorophenol 125 pg/LI
P : l.Opg/L (g-BHC 05 pg/U.
(toxephene 50 pg/I)
METALS
lOO -200pq/t.
(Pd. Hg 40-60 pgfl . Ba 4.000 pg/LI
USES: Determination of toxicity characteristic for dispi
of waste.
LiMITATiON: Quantitation limits are highly matrix-
dependent.
AVE COST: Organ.cs: $675 per sample (all fraction
Inorganics: $135 per sample
CAPACITY: Orgenica: 50 samples per month
Inorganics: 50 sample. per month
-------
‘.Iult i-Concantration
‘later Quality Parameter.
SOW R.v. 7193. Draft
pact Sheet 8/931
vailable as HO Multi-
1ient SAS
PARA METER
ALS( a. 304 2.000 pg/I
TOC ,Mt.7P lOOpgll.
NH3 1.000 pg/I; COO 3,000 pg/I
7 S4.0O0pglL TOS 10.000pg/L
To determine water quality’, determine appropriate
clean-up actions; determin, when remedial actions at.
complete: determine presenc. or absence of water quality
parameters.
LIMITATIONS : Use when water samples contain low or
medium levels of up to 10 water quality paramsters.
O.uantitation limits are highly matrix-dependent.
AVE COST : $216 per sample (all parameters)
CAPACITY : 250 samples per month
aigh Concentration Total
tetal. and Cyanide In
quid. Solid, and
tultiphase Samples
•HCO1.2. 9240.0-16FS)
vailabla in RAS
USES: To determine extent of high level contamination;
determine drum contamination: assess potential for risk to
human health and environment; determine appropriate
clean-up actions: determine presence or absence of high
levels of inorganic Contaminants.
LIMITATION : Use for determination of other than low or
medium concentration inorganic contaminants.
AVE COST : $95 per sample
CAPACITY : 100 samples per month
ncent,atiofl
in Water -
Immiscible Uquids and
Solids (SOW Rev. 9/88
and 4189)
LIQUIDS and SOLIDS :
Volad 2.5-5.0 mg/Kg
£xUasb1 20.200 mg/Kg
Afodo T 10mg/Kg
Tax p.5ear 50 mg/Kg
To determine extent of high level contamination;
determine drum contamination: assess potential for nak to
human health and environment; determine appropriate
clean-up actions: determine presenc. or absence of high
levels of organic contaminant..
LIMITATIONS : Use for determination of other than low or
medium concentration organic contaminants.
AVE COST : $650 (all fractions)
CAPACITY : Project-specific requests
.ow Concentration Total
ietals. Cyanide. Total
.trogen. fluoride in
/ater (7/92 Draft.
24O O-11FS)
,ailable as HQ Multi-
:ent SAS
WATER :
ToWmeta s 1-10 pg/I (Hg 0.2 pg/I)
(As, NI. Zn ZOpglL; F. 100 pg /I)
(Ca, Mg. Na 500 pg / I K 750 pg/I)
Cysi de 10 pg/I
Tot Mt. 100 pg/I
Ruodde 200 pg/I
USES: To determine extent of well/ground water
contamination; assess potential for risk in human health;
determine appropriate clean-up actions; determine when
remedial actions are complete; determine absence of
inorganic contaminants.
LIMITATIONS : Use only for drinking/ground water type
samples when concentrations for undiluted samples are
not expected to exceed the upper limit of the calibration
curves: 200 pg/ I for Hg. 200-400 pg/I for cyanide.
1 mg/I for total nitrogen. 1000 mg/I for fluoride, and for
the following analytee using flame AA. 7 mg/I for Ca,
0.5 mg/I for Mg, 2 mg/I for K, and 1 mg/I for Na. For
analytes not described above, no upper calibration limit is
specified.
AVE COST : $215 per sample
CAPACITY : Project.epecilic requests
‘typ. of Analysis (State..
ment,of Work Pjo., Fsc
Data
.ltunaround
Lov ritRuired Qu ’ntitatkn
14 days
Uses Limitation .ICosia/Cap’acity S S
35 days
LIQUID. SOLID, AND MULT1PHASE :
ToLd m .aSr 5,000-80.000 pg/Kg (for
Hg 300 pg/Kg)
Cv”t e . 1.500 p9/Kg
35 days
Available in SAS
14 days
-------
Analysis of Ambient Air
(SOW Rev. VCAAO1.0.
VTA.A01 .0.SVAAO1 .0
snd MAAO1.0. 9240.0-
ISFS)
U./Unteio1Cout .Capac ity .. 5
S ..
- < • . . 5;. . .. - . S ..
: To determine .xtent of contamination: ass.as
potential for risk In human health end environment;
det.rmiiw appropriate cleanup action; determine when
remedial actions are complete: d.termin. presence or
absence of air contamination.
LIMITATIONS : (Volatile.) For canister, insufficient flow
rates end sampling times may prevent collection of
sufficient quantity of sample; for Tenax. certain analytes
are not captured.
AVE COST : $700 per sample (organic.)
$375 per sample (metals)
CAPACITY : Project-specific requests
General Radiochemical
Analytical Services -
Protocol in Water and Soil
(GRASP SOW Rev.
6/11921
WATER
G, zrAIpha. 3 pCi/I
Gmzz&ta: 2 pCi/I
Mct z: 0.05 pCiIL (for Re. Sr-90
1 pCi/I. Cs-137 10 pCI/I; T 1.000
pCI/I)
SOIL/SEDIMENT
MeC : 0.05 pCllg (for Pa. Sr-90
0.1 pCilg )
USES: To determine presence or absence at radioactivity:
assess potential for risk In human health and
environment: determine appropriate clean-up action;
determine when remedial actions are complete
LIMITATION : Main survey method to determine general
radioactivity
AVE COST : $1,300 per sample (all analytes)
Type of AnalysE. (S ate.
D(flt of lark No., Fed
lumb.rQfD te
L&pv. LImi of Re uws d Quantitation
(4.’
Data
Turnai ouncI
5 llrn.taL. ‘ :
35 days
ORCANICS :
canister 2-5 ppbv Tenax 2.48
ng on column
P dd 37.183 ng/m’
INORCANICS :
TeWme.L1z 1-lO9ng/m 3
Available in SAS
45 day.
Available in SAS
CAPACITY : Project-specific requests
-------
TITLE: USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR ORGANICS ANALYSIS
LOW CONCENTRATION WATER
DOCUMENT NUMBER: OLCO2.1
DOCUMENT DATE: Not Applicable
EFFECTIVE DATES: September 1996 through September 2000
CONCENTRATION: Low
DATA TURNAROUND: 14 Days
MATRICES: Agueous*
SIGNIFICANT FEATURES
• The parameters include volatile, semivolatile, and pesticide/PCB compounds.
• Volatiles and semivolatiles are analyzed by GCIMS; pesticides/PCBs are analyzed by GC/ECD.
• All parameters have significantly reduced CRQLs as compared to SOW OLMO3.2.
• A 25 ml aliquot of sample is purged for volatiles analysis.
• Sernivolatile samples are extracted by continuous liquid-liquid extraction procedures; pesticide/PCB samples are extracted
by separalory funnel or continuous liquid-liquid extraction procedures.
• Analysis of a Laboratory Control Sample (LCS) for each parameter is required.
• Analysis of an MSIMSD duplicate pair is required.
REVISIONS!MODIFICATIONS
following is a list of the significant changes from the 10/92 Low Concentration SOW that are incorporated in SOW OLCO2. 1:
• The lab must measure the sample shipping cooler temperature at time of sample receipt using the cooler temperature
indicator blank, if present, located in the cooler. The lab must contact CLASS if the cooler’s temperature indicator
exceeds 10°C.
• The term Laboratory Evaluation Sample (LES) replaced Performance Evaluation Sample.
• Compound 1 ,2,4-Trichlorobenzene was removed from the semivolatile Target Compound List (TCL) and added to the
volatile TCL.
• The number of volatile TICs was raised from 10 to 30; the number of semivolatile TICs was raised from 20 to 30. Up
to 10 alkanes, which are not part of the 30 semivolatile TICS, are searched.
• The separatory funnel extraction method for pesticidelPCB samples was added.
• Control limits for recovery of volatile, semivolatile, and pesticide/PCB Laboratory Control Sample (LCS) compounds
were modified.
RECOMMENDED USES
This Contract Laboratory Program CLP) method is recommended for broad spectrum analysis to define the nature and
extent of potential low level orpnic contamination in water supplies during Site Investigation (SI) and Remedial Investigationl
Feasibility Study (RI/FS) activities and to verify that Remedial Design/Remedial Action (RD/RA) activities comply with pre-
determined clean-up standards. This method attains lower detection limits than SOW OLMO3.2 and can aid in the determination
of low level contamination in public drinking water supplies. The majority of samples are expected to be from drinking water
and well/ground water sources around Superfund sites. This method is suitable when a 14 day turnaround for results is adequate.
* This method may not be applicable for analysis of aqueous low concentration volatile organic samples when project DQOs
require comparison of sample results to the drinking water Maximum Contaminant Levels (MCLs).
ALYTES/CRQLs
The parameters included in the analysis and the Contract Required Quantitation Limits (CRQLs) are listed in
Attachment 1.
Revision 0, 12/04/96
-------
ATTACHMENT 1 (Page 1 of 3)
USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR ORGANICS ANALYSIS
LOW CONCENTRATION WATER
OLCO2.1
TARGET COMPOUND LIST - VOLATILES
COMPOUND
CRQL
(ugIL,_ppb)
Chioromethane
1
Bromomethane
1
Vinyl chloride
1
Chloroethane
1
Methylene chloride
2
Acetone
5
Carbon disulfide
1
1, 1-Dichloroethene
I
1,1-Dichloroethane
1
cis-1 ,2-Dichloroethene
I
trans-i ,2-Dichloroethene
1
Chloroform
I
1 ,2-Dichloroethane
1
2-Butanone
5
Bromochloromethane
1
1,1, 1-Trichloroethane
1
Carbon Tetrachloride
1
Bromodichloromethane
1
I ,2-Dichloropropane
I
cis-1 ,3-Dichloropropene
1
Trichloroethene
1
COMPOUND
CRQL
(ug/L, ppb)
Dibromochloromethane
1
1,1 ,2-Trichloroethane
1
Benzene
1
trans-i ,3-Dichloropropene
1
Bromoform
1
4-Methyl-2-pentanone
5
2-Hexanone
5
Tetrachloroethene
1
11 ,2,2-Tetrachloroethane
1
1 ,2-Dibromoethane
1
Toluene
1
Chlorobenzene
1
Ethylbenzene
1
Styrene
1
Xylenes (Total)
1
1,3-Dichlorobenzene
1
1 ,4-Dichlorobenzene
1
I ,2-Dichlorobenzene
1
I ,2-Dibromo-3-chloropropane
1
1,Z4-Trichlorobenzene
I
Revision 0, 12/04/96
-------
Al IACI-iMUU 1 (PageZOti)
USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR ORGANICS ANALYSIS
LOW CONCENTRATION WATER
OLCO2.1
TARGET COMPOUND LIST - SEMIVOLATILES
COMPOUND
‘
CRQL
(ugFL, ppb)
Phenol
5
bis(2-Qiloroethyl)ether
5
2-Chiorophenol
5
2-Methylphenol
5
2,2’-oxyb s(1-Chloropropane)
5
4-Methy1pheno
5
N.Nitroso-di-n-propylamine
5
Hexachioroethane
5
Nitrobenzene
5
Isophorone
5
2-Nitrophenol
5
2,4-Dimethylphenol
5
b s(2-Ch1oroethoxy)methane
5
2,4-Dichlorophenol
5
Naphthalene
5
4-Qiloroanilinc
5
Hexachiorobutadiene
5
4-Chloro -3-methylphenol
5
2-Methylnaphthalene
5
Hexachlorocyclopentadiene
5
2,4,6-Trichlorophenol
5
2,4,5-Trichlorophenol
20
2-Chtoronaphthatene
5
2-Nitroaniline
20
Dimethylphthalate
5
Acenaphthylene
5
2,6-Dinitrotoluene
5
3-Nitroaniline
20
Acenaphthene
5
2.4-Dinitrophenol
20
COMPOOND
CRQL
(ug/L,_ppb)
4.-Nitrophenol
20
Dibenzofuran
5
2,4-Djnitrotoluene
5
Diethylpbthalate
5
4-Chlorophenyl-phenylether
5
Fluorene
5
4-Nitroaniline
20
4,6-Dinitro-2-inethylphenol
20
N-Nitrosodiphenylamine
5
4-Bromophenyl-phenyletber
5
Hexachlorobenzene
5
Pentachiorophenol
20
Phenantlutne
5
Anthracene
5
DI-n-butylphthalate
5
Fluoranthene
5
Pyrene
5
Butylbenzylphthalate
5
3,3’-Dicblorobenzidine
5
Benzo(a)anthracene
5
Chrysene
5
bis(2-Ethylhexyl)phthalate
5
Di-n-octylphtha]ate
5
Benzo(b)fluoranthene
5
Benzo(k)fluoranthene
5
Benzo(a)pyrene
5
Indeno(l ,2,3-cd)pyrene
5
Dibenzo(a,h)anthra cene
5
Benzo(g.h,i)perylefle
5
Revision 0, 12/04/96
-------
ATTACHMENT 1 (Page 3 of 3)
USEPA CONTRACT LABORATORY PROGRAM
STATEMENT OF WORK FOR ORGANICS ANALYSIS
LOW CONCENTRATION WATER
OLCO2.1
TARGET COMPOUND LIST - PESTICIDES/PCBS
COMPOUND
CRQL
(uglL, ppb)
a1pha- HC
0.01
beta-BHC
0.01
delta-BHC
0.01
gamma-BHC (Lindane)
0.01
Heptachlor
0.01
Aldrin
0.01
Heptachior epoxide
0.01
Endosulfan I
0.01
Die ldrin
0.02
4,4’-DDE
0.02
Endrin
0.02
Endosulfan ll
0.02
4,4’-DDD
0.02
Endosulfan sulfate
0.02
COMPOUND
CRQL
(ugfL,ppb)
4,4’-DDT
0.02
Methoxychlor
0.10
Endrin ketone
0.02
Endrin aldehyde
0.02
aipha-Chlordane
0.01
gamma-Chlordane
0.01
Toxaphene
1.0
Aioclor -1016
0.20
Aroclor-1221
0.40
Aroclor-1232
0.20
Aroclor-1242
0.20
Aroclor-1248
0.20
Aroclor-1254
0.20
Aroclor-1260
0.20
Revision 0, 12/04/96
-------
Attachment G
“Training Manual for Reviewing Laboratory Data Package Completeness”,
June 1994
-------
TRAINING MANUAL FOR REVIEWING
LABORATORY DATA PACKAGE COMPLETENESS
June 1994
-------
TABLE OF CONTENTS
Page
1 . 0 INTRODUCTION . . . . . . . . . 1
2 . 0 LABORATORY DOCUMENTATION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
3.0 LABORATORYDATAPACKAGECONTENTS.......................4
3 . 1 Narrative . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
3.2 Laboratory Logbook Pages .......................... 5
3.3 Chain—of—Custody Records .......................... 6
3.4 Tabulated Su mmary Forms and Raw Data .. 6
3.4.1 Organic Tabulated Summary Forms
and Raw Data ...........•........ 7
3.4.2 Inorganic Tabulated Summary Forms
and Raw Data 16
4 . 0 ACRONYMS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
ATTACHMENTS
I ORGANIC DOCUMENT INVENTORY CHECKLIST
II INORGANIC DOCUMENT INVENTORY CHECKLIST
III EXAMPLE ORGANIC TABULATED SUMMARY FORMS
IV EXAMPLE INORGANIC TABULATED SUMMARY FORMS
V LABORATORY DOCUMENTATION AND CONTENTS CHECKLIST FOR
ORGANIC AND INORGANIC DATA
VI REGION I CSF COMPLETENESS EVIDENCE AUDIT PROGRAM, JULY 3,
1991
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Training Manual Page i. of 24
Laboratory Data Package Completeness Introduction
1.0 INTRODUCTION
When an analytical laboratory is requested/contracted by the
Client to analyze field samples, the laboratory is required to
provide adequate documentation supporting all current and future
uses of the data. Potential uses of the data may include
monitoring, modelling, risk assessment, site characterization,
support of a remedy decision, and/or confirmation of treatment.
Laboratory documentation and data may also be utilized in
potential litigation as evidence.
Data packages produced by an analytical laboratory must contain
all of the documents which were produced or used by the
laboratory for that particular analysis. Although the specific
documents required by the laboratory depends on the particular
CLP RAS SOW or Client Request/Contract, in general, the
laboratory data package must resemble as closely as possible the
data packages required by the current CLP RAS SOWs for organics
and inorganics. The tabulated summary forms provided in the SOWs
must be utilized and modified appropriately, and qualifier flags
such as those in the SOWs must be applied to the data as
appropriate. For projects other than CLP RAS SOW projects, the
data package must contain all modifications from the CLP R.AS SOWs
as specified in the Client Request/Contract.
This training manual provides procedures for reviewing laboratory
data package completeness. Section 2.0 contains the specific
laboratory documentation required in the data package, and
Section 3.0 contains the specific information which must be
provided on each document for both organic and inorganic
analyses.
The required laboratory documentation and contents described in
this manual closely resemble those required in the current CLP
RAS SOWs for organics and inorganics. The exact format of the
tabulated summary forms and specific documents required will
depend on the particular analysis method and format requested/
contracted by the Client. Sections 2.0 and 3.0 contain
comprehensive laboratory data package requirements which can be
modified according to the Client Request/Contract. A checklist
of the required laboratory documentation and contents for organic
and inorganic data are provided in Attachment V. Attachment VI
contains the RecUon I CSF Completeness Evidence Audit Pro rain
document, dated July 3, 1991.
-------
Training Xanual Page 2 of 24
Laboratory Data Package Completeness Doci .entation
2 • 0 LABORATORY DOCUKEI TATION
The laboratory data package must adhere to the following general
requirements :
• The data package must contain all original documents where
possible
• The data package must be legible,
• The data package must be clearly labeled and completed in
accordance with Client instructions
• The data package must be arranged in increasing alphanumeric
Client sample number order, or organized in a logical manner
as specified by the Client Request/Contract
• The data package must be paginated consecutively in
ascending order.
The laboratory data package documentation for both organic and
inorganic analyses consists of the following comprehensive list:
1. original sample data package including tabulated summary
forms and raw data for field samples, standards, QC samples,
and blanks (see below — sample data package)
2. A completed and signed Document Inventory Sheet used to
record the inventory of the complete laboratory data package
(see Attachments I and II for a comprehensive list of
required documents for organics and inorganics,
respectively)
3. All original shipping documents including, but not limited
to, the following documents:
a. Client Chain-of-Custody Records/Traffic Reports
b. Airbills
c. Custody Seals
d. Sample tags (if present)
4. All original receiving documents including, but not limited
to, the following documents:
a. Sample Log-In Sheet used to document the receipt and
inspection of samples and containers
b. Other receiving forms or copies of receiving ].ogbooks
c. Sample Delivery Group cover sheet identifying the
samples received for the group of samples in the data
package
5. All original laboratory records of sample transfer,
preparation, and analysis including, but not limited to, the
following documents:
a. Original preparation and analysis forms and/or copies
of preparation and analysis logbook pages
b. Internal sample arid sample extract (organics) or sample
digestate/distillate (inorganics) transfer chain—of—
custody records
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Training MAnual Page 3 of 24
Laboratory Data Package Completeness Doc entation
6. All other original project-specific documents in the
possession of the laboratory including, but not limited to,
the following documents:
a. Telephone contact logs
b. Copies of personal logbook pages
c. All handwritten project-specific notes
d. All other project-specific documents not covered by the
above.
The sample data package must include data for analysis of all
samples in that Sample Delivery Group including the following:
1. Narrative
2. Tabulated summary forms for:
a. Field sample data (in increasing Client sample
identification number)
b. Laboratory standards (in chronological order by
instrument)
c. QC samples (in chronological order by type of QC
sample)
d. Blanks (in chronological order by instrument)
3. Raw data for field samples, laboratory standards, QC
samples, and blanks (in chronological order by instrument)
4. Laboratory logbook pages for preparation and analysis of
field samples, standards, QC samples, and blanks
5. Chain-of-Custody Records
6. Other project—specific documents in the laboratory’s
possession.
In addition, for organic data each type of tabulated summary form
must be grouped by fraction (volatile, semivolatile,
pesticide/PCB). Depending on whether the data package contains
organic or inorganic analytical data, the required tabulated
forms and format for field samples, standards, QC samples, and
blanks will vary. Section 3.0 describes the specific information
required for documentation of these analyses.
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Training Manual Page 4 of 24
Laboratory Data Package Completeness Contents
3,0 LABORATORY DATA PACKAGE CONTENTS
The following sections list the information which must be
provided on each laboratory document (listed below) in the sample
data package for organic and inorganic analytical data:
1. Narrative
2. Tabulated summary forms
3. Raw data
4. Logbook pages
5. Chain—of-Custody Records.
Because of the differences in the required information between
organic and inorganic analyses on the tabulated summary forms and
raw data, these documents are discussed separately for organic
and inorganic data (Sections 3.4.1 and 3.4.2, respectively). The
narrative, logbook pages, and Chain-of-Custody Record
documentation for both organic and inorganic analyses require
similar information and are discussed together below (Sections
3.1, 3.2, and 3.3). The specific requirements resemble those of
the current CLP RAS SOWs and must be modified as appropriate to
the Client Request/Contract.
3.1 Narrative
The narrative must describe the analytical methods and exact
procedures performed by the laboratory as well as any deviations
from the methods. The laboratory must document in detail all
problems encountered with quality control, samples, shipment, and
all analytical problems encountered in processing the samples.
Problem resolution must be documented as well as any other
factors which may affect the validity of the data. The
laboratory must also discuss all unusual occurrences encountered
during the analysis of the sample set. The laboratory must
explain all data flags if not specified in the analytical method.
Additionally, for CLP RAS specific organic data the laboratory
must list the pH of each water sample submitted for volatiles
analysis. The laboratory must also list all instances of manual
integrations performed by analysts. For CLP RAS specific
inorganic data, the laboratory must indicate whether IC?
interelement corrections and background corrections were applied.
The laboratory must provide examples of calculations of both a
detected positive result and a detection/quantitatiofl limit
reported for each type of sample analysis. All equations, sample
volumes, sample weights, dilution factors, percent solids/percent
moisture, and other information required to reproduce the
laboratory results must be indicated.
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Training Kanual Page 5 of 24
Laboratory Data Package Completeness Contents
The narrative must also include the following additional items of
information:
• Laboratory name
• Client Request/Contract project number
• CL? RAS or other Client sample identification numbers cross—
referenced to the laboratory sample identification numbers.
In addition, the narrative must be signed and dated by the
laboratory manager or designee.
Communication Logs
All telephone communications between the laboratory and sampling
personnel or other parties outside the laboratory, which took
place to resolve sampling discrepancies or analytical problems
must be documented in detail on telephone communication logs.
Those telephone logs must explicitly detail the problems
discussed, the resolution agreed upon, the names and affiliations
of the communicating parties, and the date the communication took
place. All telephone logs must be appended to the narrative.
3.2 Laboratory Logbook Pages
The data package must contain the following laboratory logbook
pages. Where possible, the originals must be submitted.
• Standards preparation logs
• QC sample preparation logs
• Sample preparation/extraction/digestion logs
• Sample analysis run logs
• Personal logs
• Hand—written project-specific notes.
The logbook pages must contain the following information where
applicable:
• Laboratory name
• Client sample identification number
• Laboratory sample identification number
• Dates of preparation and analysis, and initials of
preparer/analyst
• Source of standards and QC samples
• Weights and volumes of samples and standards
• Initial and final volumes of sample prepared/purged!
extracted/digested
• Percent moisture/percent solids
• Injection/analysis volumes
• Date and time of sample injection
• Dilution factors.
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Training Manual Page 6 of 24
Laboratory Data Package Completeness Contents
3,3 Chain—of-CustodY Records
Documentation must be provided of the traceability of the Client
samples from the time the samples are released to the laboratory
and while in the laboratory’s possession. Two types of custody
records must be provided in the data package: records of external
sample transfer and custody from parties outside the laboratory,
and records of internal sample transfer and custody within the
laboratory.
On the external Chain-of--Custody Record, usually initiated by the
Client/sampler, the laboratory is responsible for providing the
following information:
• Date of sample receipt
• Signature of receiving personnel
• Condition of shipping containers and sample bottles upon
receipt
• Condition of custody seals
• Presence/absence of airbills, custody seals, Client custody
records, traffic reports, sample tags
• Problems or discrepancies with samples received or the
documentation on the Chain-of-Custody Record.
The Chain-of—Custody Record also contains other vital information
(e.g. sampling date/time, etc.) but documentation of this
information is the responsibility of the Client/sampler.
The laboratory’s internal Chain-of-Custody Records must contain
the following information:
• Laboratory name
• Client sample identification number
• Laboratory sample identification number
• Date of sample transfer and receipt
• signature of personnel transferring/receiving the sample
• Purpose of transfer/receipt, location of sample transferred.
3.4 Tabulated $u marv Forms and Raw Data
The exact format of the tabulated summary form for each field
sample, QC sample, standard, and blank will depend on the
particular analysis method requested/contracted by the Client.
The laboratory must provide certain information on all the
tabulated summary forms and raw data: laboratory name,
project/contract number, concentration units wherever numerical
values are reported, and indication of wet or dry weight for
solid matrices. The following sections list the specific
requirements for organic data and inorganic data.
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Training Wanual Page 7 of 24
Laboratory Data Package Completeness Contents — Organic
3.4.1 ORGANIC FORMS M(D RAW DATA
Information required on tabulated summary forms are presented in
the following sections for the organic data listed below:
1. Field sample results
2. Surrogate results (system monitoring compound results)
3. Matrix spike/matrix spike duplicate results
4. Method/laboratory blank results
5. Tuning results (GC/MS instrument performance check)
6. Initial calibration results (GC/MS)
7. Initial calibration results (GC)
8. continuing calibration results (GC/MS)
9. Continuing calibration results (GC)
10. Internal standard results (GC/MS)
11. GC analytical sequence
12. Pesticide cleanup results
13. Pesticide/PCB identification summary
14. Method detection limit study results
Tabulated summary forms for organic data required by the CLP RAS
SOWs are provided in Attachment III as examples.
Field Sample Results (Form 1)
comprehensive tabulated summary forms must be prepared for each
field sample analyzed by the laboratory. At a minimum, the
tabulated summary forms must contain the following information:
• Client sample identification (ID) number
• Laboratory sample ID number
• Target compound names
• Tabulated analytical results for identification (numerical
quantitation limits) and quantitation (positive hits) with
concentration units
• Any laboratory qualifier flags — laboratory qualifier flags
for each target analyte must be tabulated on a separate form
(definitions must be provided for each laboratory qualifier
flags).
For each field sample, the tabulated summary forms must also
contain the following information as appropriate to the analysis
method:
• Laboratory file ID
• Sample matrix type
• Level of analysis (low, medium)
• Percent moisture or percent solids
• GC column
• Sample weights and/or sample volumes prepared/purged!
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Training )tanual Page 8 of 24
Laboratory Data Package Completeness Contents - Organic
extracted/analyzed
• Initial and final extract and extract clean-up volumes,
injection volume
• Clean-ups performed
• Dilution factor
• Measured pH
• Dates of sample receipt, extraction, and analysis.
Surrogate Results (System Xonitorin Compound Results ) (Form 2)
Surrogate recovery data help to evaluate the efficiency of the
sample preparation and analysis procedures arid analytical system.
The tabulated surrogate results summary form must contain the
following information:
• Sample matrix
• Level of analysis (low, ned)
• GC column
• Client sample ID numbers
• Surrogate compounds added
• Percent recoveries of surrogates
• QC limits for all surrogate standards in field samples, QC
samples, and blanks
• All outliers flagged
• Total number of surrogates outside QC limits
• Indication of surrogates diluted out.
Matrix Spike/Matrix ppike Duplicate Results (Form 3)
Matrix spike and matrix spike duplicate samples are analyzed to
evaluate the effects of the sample matrix on the methods used for
analysis. The tabulated MS/MSD results summary form must contain
the following information:
• Sample matrix
• Level of analysis (low, ned)
• Client sample ID number
• Matrix spike compounds added
• True concentrations of the spikes added
• Concentrations of the spike compounds observed in the spiked
sample
• Sample concentration of each spike compound detected in the
original unspiked sample for the MS and MSD
• Percent recoveries of the spiked compounds in the MS/MSD
samples
• Relative percent differences of the spiked compounds between
the MS and MSD samples
• QC limits for all spike compounds - percent recovery and
relative percent difference
• All outliers flagged.
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Training Manual Page 9 of 24
Laboratory Data Package completeness Contents - organic
In addition to the above, the results for all target compounds in
the MS and MSD samples must be tabulated on the summary forms
used to tabulate the field sample results.
) (ethod/Laboratorv Blank Results (Form 4)
The laboratory must provide blank information to determine the
levels of contamination associated with the processing and
analysis of the samples for method blanks and, depending on the
analysis method, laboratory (instrument) blanks. The tabulated
method/laboratory blanks results form must contain the following
information:
• GC column, instrument ID
• Date and time of analysis for the blank itself
• Date of extraction -
• Matrix with which the blank is associated
• Level of analysis (low, med)
• Laboratory sample ID number
• List of Client field sample ID numbers and MS/MSD samples
associated with each blank (separate forms are used for each
blank)
• Laboratory file IDs of the samples and associated blank
• Dates/times of analysis for field samples and NS/MSD samples
which are associated with each blank.
In addition, results for each method and laboratory instrument
blank must be included on the tabulated summary forms that are
used for field sample results (Form 1).
Tuning Results (GC/MS Instrument Performance Check ) (Form 5)
For CC/MS analyses, the laboratory must perform instrument
performance checks to assure correct mass calibration, mass
resolution, and mass transmission. The.tabulated GC/MS tuning
results summary form must contain the following information:
• Instrument ID, laboratory file ID
• Date and time of injection for each tune compound analysis
(each tune on a separate form)
• Tune compound name
• Mass—to-charge ratio (m/e) for each ion
• Ion abundance criteria
• Percent relative abundances.
The form must also contain the following tabulated information
associated with each tune and in chronological order:
• Client sample ID numbers associated with that tune
• Laboratory sample ID numbers
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Training Kanual Page 3.0 of 24
Laboratory Data Package Completeness Contents - organic
• Laboratory file IDs
• Date and time of analysis for all field samples, .MS/MSD
samples, blanks, and standards associated with that tune
• All outliers flagged.
Initial Calibration Results (GC/MBt (Forms 6A—6C)
Prior to any analysis, the laboratory must initially calibrate
the GC/14S system to determine the linearity of the response. The
tabulated GC/MS initial calibration results summary form must
contain the following information:
• Instrument ID, laboratory file IDs
• Purge method
• Dates and times of standard analyses for that initial
calibration
• Target compound names
• Concentrations of the calibration standards
• Relative response factors for each target and surrogate
compound at each standard concentration
• Mean relative response factors for each target and surrogate
compound
• Percent relative standard deviations for each target and
surrogate compound
• QC limits for each initial calibration (each initial
calibration on a separate form) — minimum RRF, maximum % RSD
values
• All outliers flagged.
Initial Calibration Results (GCI (Forms 6D—6G)
Because the identification of compounds using GC is based
primarily on retention time data or pattern recognition, the
retention times and retention time windows are crucial to the
provision of valid data. Generally, the tabulated initial
calibration results summary forms for GC systems consist of
retention time and calibration factor information. The data for
pesticides, generally multi-point calibrations, and PCBs,
generally single-point calibrations, are usually provided on two
separate forms.
The following retention time information must be documented on
the initial calibration results summary form:
• Instrument ID, GC column
• Dates of analysis
• Concentration of the calibration standards
• Target compound and surrogate compound names
• Retention times for each target and surrogate compound at
each standard concentration
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Training Manual Page 11 of 24
Laboratory Data Package Completeness Contents — Organic
• Mean retention times for each target and surrogate compound
(if multi—point calibration)
• Retention time windows for each target and surrogate
compound (QC limits).
The following calibration factor information must be documented
as veil:
• Instrument ID, GC column
• Dates of analysis
• Concentrations of the calibration standards
• Target compound and surrogate compound names
• Calibration factors for each target and surrogate compound
at each standard concentration
• Mean calibration factor (for multi—point calibration) for
each target and surrogate compound -
• Percent Relative Standard Deviation for each target and
surrogate compound
• QC limits — % RSD
• All outliers flagged.
Resolution between compounds is documented with the following
information:
• Instrument ID, GC column
• Dates and times of analysis
• Laboratory sample ID
• Names of compounds for which resolution is measured
• Retention times for each of those compounds
• Percent resolution between each pair of compounds
• QC limits — % resolution
• All outliers flagged.
Continuing Calibration Results (GC/MS ) (Form 7A—7C)
The continuing calibration standards are analyzed to verify the
accuracy of the initial calibration. The tabulated continuing
calibration results form must contain the following information:
• Instrument ID, laboratory file ID
• Purge method
• Date and time of continuing calibration analysis
• Date and time of initial calibration analysis associated
with that continuing calibration
• Target compound and surrogate compound names
• Mean relative response factors from initial calibration for
each target and surrogate compound
• Relative response factors from continuing calibration for
each target and surrogate compound (each continuing
calibration on a separate form)
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Training Kanual Page 12 of 24
Laboratory Data Package Completeness Contents - Organic
• Percent differences for each compound
• QC limits for each target and surrogate compound (each
continuing calibration on a separate form) — minimum RRF,
maximum % D
• Concentrations of the continuing calibration standards
• All outliers flagged.
Continuing Calibration Results (GC ) (Forms 7D, 7E)
The tabulated continuing calibration results form must contain
the following information:
• Instrument ID, GC column
• Laboratory sample ID
• Dates and times of continuing calibration standards analysis
• Date of associated initial calibration analysis
• Target compound and surrogate compound names
• Retention time for each target and surrogate compound
• Calculated amount of standard
• Nominal amount of standard
• Relative Percent Difference for each compound
• QC control limits — RPD
• Percent breakdowns for compounds used to measure extent of
breakdown (endrin and 4,4’-DDT) and combined breakdown
• QC limits — percent breakdown.
Internal Standard Results (GC/I4S ) (Forms BA—SC)
Internal standard responses in all calibration standards, field
samples, QC samples, and blanks are crucial to the provision of
reliable analytical results because the internal standards are
used to quantitate the compounds. The tabulated internal
standard results summary forms must contain the following
information.
• Instrument ID, laboratory file ID
• GC column, purge method
• Date and time of continuing calibration standard analysis
• Client sample identification numbers
• Internal standard compound names
• Retention times and area counts of the quantitation for each
internal standard compound in the continuing calibration
standard, field samples, MS/NSD samples, and blanks
associated with that continuing calibration (separate form
for each continuing or initial calibration)
• QC limits — area counts and retention times
• All outliers flagged.
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Training Manual Page i.3 of 24
Laboratory Data Package Completeness Contents - Organic
GC Analytical Secruence (Form 8D)
The Client Request/Contract may require standards and samples to
be analyzed according to a special sequence. In this case, the
following information must be provided:
• Instrument ID, GC column
• Initial calibration dates
• List of Client sample ID numbers in that analytical sequence
(in chronological order) for all standards, field samples,
QC samples, and blanks
• Laboratory sample ID numbers
• Dates and times of analyses
• Mean surrogate retention times — from initial calibration
• Retention times of the surrogate compounds
• QC limits of the surrogates — retention times
• All outliers flagged.
Pesticide Cleanup Results (Form 9)
Tabulated summary forms may be required when cleanup procedures
are employed during the preparation of pesticide extracts for
analysis. The following information are documented for reporting
the results of the check of the Florisil cartridges used to
process samples and extracts, and to summarize the results of the
calibration of the Gel Permeation Chromatography (GPC) used to
process soil sample extracts for Pesticide/PCB analyses.
Florisil Cartridge Check Results (Form 9A):
• CC column
• Florisil cartridge lot number (each lot on a separate form)
• Date of check solution analysis
• Names of compoundsin the Florisil cartridge check solution
• Amount of spike in the check solution
• Amount of spike recovered in the check solution
• Percent recoveries
• QC limits — percent recoveries
• All outliers flagged
• Client sample ID numbers associated with that Florisil
cartridge
• Laboratory sample ID numbers associated with that Florisil
cartridge
• Dates of sample analysis.
GPC Calibration Results (Form 9B):
• GPC column
• Calibration date of GPC column
• CC columns
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Training Manual Page ii of 24
Laboratory Data Package Completeness Contents — organic
• Name of spike compounds added to GPC column
• Amount of spike added
• Amount of spike recovered
• Percent recoveries
• QC limits — % recoveries
• All outliers flagged
• Client sample ID numbers associated with the GPC column
calibration
• Laboratory sample ID numbers associated with the GPC column
calibration
• Dates of sample analyses.
Pesticide/PCB Identification Summary (Form 10)
This form summarizes the quantitations of all target
Pesticide/PCB compounds detected in each field sample, QC sample,
and blanks. If no compounds are detected in a given sample, this
form is not required.
• Instrument ID, GC columns
• Dates of analysis
• Client sample ID number (on a separate form for each sample)
• Laboratory sample ID number
• Target compound name detected
• Retention time of compound on each column
• Retention time windows
• Concentration (mean concentration for multicomponent
compounds)
• Percent difference.
Method Detection Limit Study Results
The tabulated MDL study results must contain the following
information:
• Target compound names
• Concentrations of spikes added
• Concentration detected for each MDL spike
• Standard deviation and calculated MDL for each target
compound.
The exact procedure utilized to generate the MDLs must be
documented in detail in the narrative. The equation and
associated constant values utilized to calculate the MDL for each
analysis must be documented. The column, instrument ID, trap
composition, and operating conditions must be clearly documented
in the raw data.
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Training )(anual Page 15 of 24
Laboratory Data Package Completeness Contents - Organic
Raw Data
The laboratory data package must contain raw data for all field
samples, standards, QC samples, matrix spike and matrix spike
duplicate samples, and blanks. The exact format and content of
the raw data will depend on the particular analysis method
requested/contracted. However, all instrument printouts, strip
chart recordings, chromatogramS, quantitation reports, mass
spectra, and other types of raw data generated by the laboratory
for a particular project must be provided in the data package.
Typical raw data for organic CC/MS analyses includes, but is not
limited to the following:
• Reconstructed total ion chromatogram for each sample or
sample extract, standards, QC samples, and blanks
• Instrument quantitation reports containing the following
information: laboratory sample identification number, Client
sample identification number, date and time of analysis,
retention time and/or scan number of quantitation ion with
measured area, analyte concentration, copy of area table
from data system, GC/MS instrument ID, laboratory file ID,
column, trap composition, and operating conditions
• Raw and enhanced mass spectra for all positive target
compound results in field samples; daily continuing
calibration standard reference spectra for all positive
field sample results
• Mass spectra and three library searched best-match mass
spectra for all tentatively identified compounds reported
• Instrument normalized mass listing and the mass spectrum for
each tune.
Typical raw data for organic GC analyses includes, but is not
limited to the following:
• Chromatograms for field samples, calibration standards, QC
samples, and blanks containing the following information:
Client sample identification number, laboratory sample
identification number, volume injected, date and time of
injection, GC column identification, GC instrument
identification, laboratory file ID, operating conditions,
positively identified compounds must be labeled with the
compound names either directly from the peak or on a
printout of the retention times
• Chromatograms f or both GC columns
• GC integration report or data system printout
• Manual worksheets.
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Training Manual Page 16 of 24
Laboratory Data Package completeness contents - Inorganic
3.4.2 INORGANIC FORKS Mm RAW DATA
Tabulated summary form requirements are presented in the
following sections for the inorganic data listed below:
1. Field sample results
2. Initial and continuing calibration verification results
3. Contract required detection limit standard results
4. Blank results
5 • ICP interference check sample results.
6. Matrix spike and post-digestion spike sample results
7. Duplicate sample results
8. Laboratory control sample results
9. Method of standard additions results
10. ICP serial dilution results
11. Instrument detection limits
12. ICP interelement correction factors
13. ICP linear ranges
14. Preparation log
15. Analysis run log and Furnace U QC results.
Tabulated data reporting forms for inorganic data required by the
CLP RAS SOWS are provided in Attachment IV as examples.
Field Sample Results (Form 1)
Comprehensive tabulated summary forms must be prepared for each
field sample analyzed by the laboratory. At a minimum, the
tabulated summary forms must contain the following information as
appropriate to-the analysis method:
• Sample matrix type
• Level of analysis (low, medium)
• Percent moisture or percent solids
• Date of sample receipt
• Client sample identification number
• Laboratory sample identification number
• Target analyte names
• Tabulated analytical results for identification (numerical
detection/quantitation limits) and quantitation (positive
hits) with concentration units
• Any laboratory qualifier flags — laboratory qualifier flags
for each target analyte must be tabulated on a separate form
(definitions must be provided for each laboratory qualifier
flags)
• Concentration qualifier - indication of results less than
the contract required detection limits
• Analytical method used for each analyte (usually indicated
with a symbol).
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Training Manual Page 17 of 24
Laboratory Data Package Completeness Contents - Inorganic
Information regarding sample weights, volumes, dilution factors,
and dates of digestion and analysis which are provided on the
field sample results summary forms for organic data are not
typically provided on those forms for inorganic data. Instead,
this information is provided on other tabulated forms which
follow.
Initial and Continuina Calibration Verification Results (Form 2A)
Initial and continuing calibration verification standards are
analyzed to verify and ensure the accuracy of the initial and
continuing calibrations. The tabulated initial and continuing
calibration verification results summary form must contain the
following information:
• Sources of the initial and continuing calibration
verification standards
• Target analyte names
• True values of the calibration verification standards
• concentrations found for the calibration verification
standards
• Percent recoveries
• QC limits — percent recoveries
• Analytical method used for each analyte (usually indicated
with a symbol).
The order of reporting the initial and continuing calibration
verification standards for each analyte must follow the order in
which the standards were analyzed.
Contract Rectuired Detection Limit Btandard Results (Form 2B)
Contract required detection limit (CRDL) standards are analyzed
to verify the linearity of the instrument near the contract
required detection limit. The tabulated CRDL results form must
contain the following information:
• Source of the CRDL standards
• Target analytes
• True values of the RDL standard for each analyte
• Concentrations found for each analyte
• Percent recoveries for each analyte
• QC limits (if known).
The order of reporting the CRDL standard results for each analyte
must follow the order in which they were analyzed.
plank Results (Form 3)
The tabulated blank results summary form must, in general,
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Training Xanual Page 18 of 24
Laboratory Data Package Completeness Contents — Inorganic
contain information for two types of blanks: initial and
continuing calibration blanks, or instrument blanks, and
preparation blanks. The tabulated blank results summary form
must contain the following information:
• Matrix for which the preparation blank is associated
• Concentration units of each blank type
• Target analyte names
• Initial and continuing calibration blank results
• Preparation blank results
• concentration qualifiers
• Analytical method used for each ana]yte (usually indicated
with a symbol).
The order of reporting the initial and continuing calibration
blanks and preparation blanks for each analyte must follow the
order in which they were analyzed.
ICP Interference Check Sample Results (Form 4)
ICP interference check samples are analyzed to verify
interelement and background correction factors by analyzing
target analytes in the presence of interferents. The tabulated
ICP interference check sample results forms must contain the
following information:
• ICP instrument ID number
• Source of the ICS solutions
• Target ICP analytes
• True values of each target ICP analyte in the solution
containing interferents only
• True values of each target ICP ana].yte in the solution
containing interferents and analytes
• Concentrations of target ICP analytes detected in the
solution containing interferents only
• concentrations of target ICP analytes detected in the
solution containing interferents and analytes
• Percent recoveries.
The order of reporting the interference check sample results for
each analyte must follow the crder in which they were analyzed.
Matrix Spike and post—Digestion spike Sample Results (Form 5A,
5B)
The matrix spike sample analysis provides information about the
effect of the sample matrix on the digestion and measurement
methodology. The post-digestion spike recovery is based on the
addition of a known quantity of analyte to an aliquot of digested
sample. The tabulated matrix spike and post-digestion spike
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Training Manual Page 19 of 24
Laboratory Data Package Completeness Contents - Inorganic
sample results (Forms VA and VB, respectively) must contain the
following results:
• Sample matrix
• Level of analysis (low, medium)
• Percent solids of the sample
• Client sample identification number
• Target analyte names
• concentrations of the spikes added to the sample
• Concentrations found in the spiked sample
• Concentration found in the unspiked sample
• Percent recoveries
• QC limits — percent recovery
• All outliers flagged
• Concentration qualifiers
• Analytical method used for each analyte (usually indicated
with a symbol).
Duplicate Sample Results (Form 6)
Duplicate sample analysis provide information about the
laboratory precision. The tabulated duplicate sample results
form must contain the following information:
• Sample matrix
• Level of analysis (low, medium)
• Percent solids of the original sample and duplicate sample
• Client sample identification number
• Target analyte names
• Concentration of the original sample result
• Concentration of duplicate sample result
• Relative percent difference
• QC limits
• All outliers flagged
• Concentration qualifiers
• Analytical method used for each analyte (usually indicated
with a symbol).
Laboratory Control Sample Results (Form 7)
Laboratory control sample results provide information about the
efficiency of the digestion method and accuracy of the results.
The tabulated laboratory control sample results form must contain
the following information:
• Source of the laboratory control sample
• Matrix of the LCS
• Target ana].yte names
• True concentrations
• Concentrations found
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Training Manual Page 20 of 24
Laboratory Data Package Completeness Contents - Inorganic
• Percent recoveries
• QC limits
• Concentration qualifiers.
Because a laboratory control sample should be digested for each
matrix and digestion batch, additional forms must be present as
appropriate if more than one LCS for a matrix was analyzed.
Method of Standard dditions Results (Form 8)
The method of standard additions analysis may be performed by the
laboratory to quantitate the analyte in the sample when matrix
interferences are present. The tabulated method of standard
additions results form must contain the following information:
• Client sample identification number
• Concentrations of each NSA spike added
• Absorbance detected in each NSA spike as well as the sample
itself
• Final concentration
• Correlation coefficient
• All outliers flagged.
Results for different samples for each analyte must be reported
sequentially.
ICP Serial Dilution Results (Form 9)
ICP serial dilution analyses provide information as to the extent
of the matrix effects in the sample. The tabulated ICP serial
dilution results form must contain the following information:
• Sample matrix
• Level of analysis (low, medium)
• ICP instrument ID
• Client sample identification number
• Target analyte names
• Concentrations of the undiluted sample result
• concentrations of the diluted sample result
• Percent difference
• QC limits — percent difference
• All outliers flagged
• Concentration qualifiers
• Analytical method used for each analyte (usually indicated
with a symbol).
Instrument Detection Limits (Form 10)
The tabulated instrument detection limit results form must
contain the following information:
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Training )(anual Page 21. of 24
Laboratory Data Package Completeness Contents — Inorganic
• Instrument ID numbers used for the IDL determination
• Date the IDLs were determined
• Wavelength and background used for each analyte
• Target añalyte names
• Type of background correction used (where applicable)
• Instrument detection limits
• Contract required detection limits
• Concentration units
• Analytical method used for each analyte (usually indicated
with a symbol.
ICP Interelement correction Factors (Form 11)
This form must document for each ICP instrument used for
analysis, the interelement correction factors applied by the
laboratory to obtain the reported data. The tabulated ICP
interelement correction factors form must contain the following
information:
• ICP instrument ID number
• Wavelength for each analyte used for the determination
• Date of interelement correction factor determination
• Target ICP analyte names
• Interfering analytes with which the interelement correction
factors were determined
• Interelement correction factors for each analyte.
ICP Linear Ranges (Form 12)
A linear range verification check standard must be analyzed and
reported for each target analyte as this concentration is the
upper limit of the ic linear range beyond which results should
not be reported without dilution of the sample. The tabulated
ICP linear ranges must contain the following information:
• - ICP instrument ID number
• Date of the linear range determination
• Integration time for each analyte
• Target IC? analytes
• Concentration of the upper limit of the linear range for
each analyte.
preparation Log (Form 13)
‘This form provides sample preparation information which
documented in the laboratory logbook pages. The following
information is required:
• Analytical method (each analytical method on a separate
form)
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Training Manual Page 22 of 24
Laboratory Data Package Completeness Contents - Inorganic
• Client sample ID number of all field samples, QC samples,
standards, and blanks digested/distilled
• Sample preparation date
• Sample weight
• Sample volume.
Analysis Run Log and Furnace AA OC Results (Form 14)
This form provides information as to the analytical sequence of
each analyte and any dilution factors applied. The tabulated
analysis run log summary form must provide the following
information.
• Instrument ID
• Analytical method
• Start and end dates of the analytical sequence
• client sample ID numbers in chronological order
• Dilution factors
• Time of analysis for each analytical sample and standard
• Analytes associated with the run sequence.
Furnace AA QC analysis results are also typically provided on
this form. Because of the nature of the furnace AA technique,
the Client Request/Contract may require special QC sample
analyses for quantitation of field samples. The QC samples which
may be required are the following: duplicate injections of each
analytical and field sample, and post—digestion spikes of each
field sample. For furnace AA analyses, the following additional
information are required on the Analysis Run Log Form:
• Percent relative standard deviation of duplicate injections
(outliers usually indicated with flags on the tabulated
field sample results summary form, Form 1)
• Percent recoveries of post-digestion spikes
The above information must be reported on separate forms for each
furnace AA analyte.
Raw Data
The laboratory data package must contain raw data for all field
samples, standards, QC samples, matrix spike and duplicate
samples, and blanks. The exact format and content of the raw
data will depend on the particular analysis method requested/
contracted. However, for each reported value for a particular
project, the laboratory must include all raw data used to obtain
that reported value.
Typical raw data for inorganic analyses include, but is not
limited to the following:
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Training Kanual Page 23 of 24
Laboratory Data Package Completeness Contents — Inorganic
• Instrument printouts, strip chart recordings, etc., for all
field samples, QC samples, standards, and blanks containing
the following information: laboratory sample identification
number, Client sample ID number, date and time of analysis,
absorbance/emission values, analyte concentration,
instrument ID, lab file ID, and instrument operating
conditions.
• Standard curve raw data, plotted standard curves, linear
regression equations, and correlation coefficients.
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Training Manual Page 24 of 24
Laboratory Data Package Completeness onyms
4,0 ACRONYMB
AAS Atomic Absorption Spectrometry
CCV Continuing Calibration Verification
CLP Contract Laboratory Program
CRDL Contract Required Detection Limit
CRQL Contract Required Quantitation Limit
GC Gas Chromatography
GC/MS Gas Chromatography/MaSS Spectrometry
GPC Gel Permeation Chromatography
ICP Inductively Coupled Plasma
ICS Interference Check Sample
ICV Initial Calibration Verification
ID Identification
IDL Instrument Detection Limit
LCS Laboratory Control Sample
MDL Method Detection Limit
MS Matrix Spike
MSD Matrix Spike Duplicate
MSA Method of Standard Additions
PB Preparation Blank
QC Quality Control
RAS Routine Analytical Services
RPD Relative Percent Difference
RRF Relative Response Factor
RSD Relative Standard Deviation
SOW Statement of Work
-------
ATTACHMENT I
ORGANIC DOCUMENT INVENTORY CHECKLIST
-------
ORCA.NIcS COMPLETE SDC FILE (CSF) i v rroay SHEET
LABORATORY NAME ___________________________________
CITY/STATE __________________________________________________
CASE NO. __________ SDC NO. __________ SDG NOS. TO FOLLOW __________
___________ ___________ SAS NO. ________
CONTRACT NO.
SOW NO. ____________________________________
All dnc ents delivered in the complete SDG file u.st be original documents
where possible. (IEFE n ct IBIT B, SECTION II and SECTION III .)
PACE NOs CHECK
FROM TO LAS EPA
1. Inventor’r Sbeee (Form DC-2) (Do not number) ________
2. SDG Case Narrative
3. SDC Cover S1 eet/Trpffjc Reyort
4. Vol tj1es Data
a. QC Sux mary
System Monitoring Compound Sti iry
(Form II VGA)
Matrix Spike/Matrix Spike Duplicate Su nm iry
(Form III VOA)
Method Blank Su .ary (Form IV VOA)
CC/MS Instrument Performance Check
(Form V VGA)
Internal Standard Area and RT Suary
(Form VIII VOA)
b. Sample Data
TCL Results - (Form I VGA)
Tentatively Identified Compounds
(Form I VGA-TIC)
Reconstructed total ion chromacograns (RIC)
for each sample
For each sample:
Raw spectra and background-subtracted
mass spectra of target compounds
identified
Quantitacion reports
Mass spectra of all reported TICs with three
best library matches
c. Standards Data (All Instruments)
Initial Calibration Data (Form VI VOA)
RICs and Quan Reports for all Standards
Continuing Calibration Data (Form VII VOA) ________
RICs and titatjon Reports for all Standards
d. Raw QC Data
BFB
Blank Data
Matrix Spike/Matrix Spike Duplicate Data
FORM DC-2-l
OL ’t01.7 7/c:
-------
ORCANICS COMPLETE SDC FILE (CSF) INVENTORY SHEET (Cant.)
CASE NO. SOC NO. SOC NOS. TO FOLLOW
SAL NO.
PAGE NOs C hECK
OM TO LAB EPA
5. ivo layjle Data
a. QC Sin nry
Surrogate Percent Recovery S’ ry (Form II SV) ____ ____ ________
MS/MSD Sttmr nry (Form III LV) ____ ____ _______
Method Blank Su ary (Form IV LV) ___ ___ _______
CC/MS Insts ent Performance Check
(Form V LV)
Internal Standard Area and P.T Summary
(Form VIII LV)
b. Sample Data
TCL Results (Form I SV-L, SV-2)
Tentaei’u-ely Identi.fied Compoumds (Form I SV-TIC)
Recomstrucced total ion cromatograms (RIC)
for each sample
For each sample:
Raw spectra and background- sub trac ted
ma.ss spectra of target compounds ________
Qua.ntitacion reports _________
Mass spectra of TICs with three best library matches _______
GPC chromarograms (if GPC performed) ________
c. S r rdard.s Data (All In struments)
Initial Calibration Data (Form VI SV-l, SV-2) _______
RICs and Quan Reports for an Standards _______
Continuing Calibration Data (Form VII SV-l, SV-2) _______
RICs and Quantitation Reports for all Standards _______
Semivolatj].e GPC Calibration Data-UV
detector traces
d. Raw QC Data
DFTPP
Blank Data
Matrix Spike/Matrix Spike Duplicate Data
a. QC SLtTI 1!Ilry
Surrogate Percent Recovery 5 ” ’-y (Form II PEST) ____ ____ _____ ________
MS/MSD Duplicate Su ry (Form III PEST) ____ ____ _____ _______
Method Blank S ary (Form IV PEST) ____ ____ _____ ________
FORM DC-2-2
6. Pesrtcides
CL iOl.7 7/9:
-------
ORCANICS COMPLE SDC TILE (CSF) INvEN’roay SHEET (Cont.)
I CASE NO. SDC NO. SDC SOS. TO FOLT O J
L S/IS NO.
PAGE NOs CHZC (
FROM TO LAB EPA
6. Pesti ides (cont.)
b. Sample Data
TCL Results - Organic Analysis Data Sheet
(Form I PEST) _______
Chroaatogras.s (Primaxy Col ) _________
Chroaatograms from second CC colt t confirmation ________
CC Integration report or data system printout
Manual work sheets
For pesticides/Aroclors confirmed by CC/MS. copies
of raw spectra and copies of backgro md-si ibtracted nass
spectra of target compotnids (samples & standards)
c. Standards Data
Initial Calibration of Single Component
Analytes (Form V I PEST-i and PEST-2)
Initial Calibration of Multicemponent Analyces
(Form VI PEST.3) _________
Analyte Resolution Stary (Form VI PEST-4) ________
Calibration Verification SUmmary (Form VII PEST-i) ________
Calibration Verification Summarj (Form VII PEST-2) ________
Analytical Sequence (Form VIII PEST) ________
Piorisil Cartridge Check (Form IX PEST-i) ________
Pesticide CPC Cali ration (Form IX PEST-2) ________
Pesticide Identification SummAry for Single Component
Analytes (Form X PEST-i)
Pesticide Identification St ary for Multicomponent
Analytes (Form X PEST-2)
Chromatograms and data system printouts
A printout of retention times and corresponding peak
areas or peak heights
Pesticide CPC calibration data - UV detector traces
d. Raw QC Data
Blank Data
Matrix Spike/Matrix Spike Duplicate Data
FORM DC-2-3
OL iOl.7 7/91
-------
ORGANICS CO I .Erz SDG F 2 (CST) INVENTORY SU T (Cant.)
CASE NO. SDC NO. SDC NOS. TO POLLO Z
SAS NO.
PAGE NOs CHECK
i OM TO LAB EPA
7. Nisce1lpneo i., Data
Original preparation and analysis forms or copies of
preparation and analysis logbook pages ____ ____ _____ ______
Internal sample and sample extract transfer
chain-of-custody records
Screening records
A].1 instrument output, including strip charts
from screening activities (describe or list)
8. EPA Shiv in /Recejvj Docume ts
Airbills (No. of shipments _) ____ ____ _____ ________
ain-of-Cu.stody Records
Sample Tags ____
Sample Log-In Sheet (Lab & DC1) ____ ____ _____
Miscellaneous Shipping/Receiving Records
(describe or list)
9. Internal Lab Sample Transfer Records and Trackjrj Sheets
(describe or list)
10. Othet Records (describe or list)
Telephone Cotxnicatjon Log ____ ____ _____
11. Co e ys :
oopleced by: _________________________
(CLP Lab) (Signature) (Printed Name/Title) (Date)
udited by: ________________________
(EPA) (Signature) (Printed Name/Title) (Date)
FORM DC-2-4
OL’ Ol.7 7/91
-------
-oaxzcc L :z c ZIZ •.(C ) - ttic
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Kathod I’ - k Z aXT (7o 7 ) ____
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RICa and Quan Rap s for a U Sta a ___ o y ______
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4. Raw Q a2a
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Matrix Spike V pItc-ats Data k — ______
s. F i’ ’k a 1., Vite
a. QC S aay
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Xet o4 hank S’.r (7am IT IV ) L - / _______
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3. Ziy Lat. .3.aa Data (t4)
b. £a t• Data. ____ ____ _____
?. 2aa Lta (7am X LV ) ____
Ts tattv.Ly tdanti. Ld X ____
Rasw tatal. L A ctz at3qr a (XXC f icfl
7cr •a s az
Raw sp.cts s d bac - d—. btracta4 — - .
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(ass spsctza of ‘z vtt i bsst 2.i zary aa s 7
PC c . atcqraa (U G?C ps .c c ta4) _ /
C. Stz. daxdz Data ( .1.i. I zt s)
jtja t a i Cats (7D v svj 3 I fo 7
.ZCs a. 4 R.poru i c r a U. ata .c4az z
tii q Ca1L :a ( 7Dr vr L V ) ‘ 1 3 ‘ 1 ___
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Z t*r .LL zsa L axy ( TD v ” LV) L Z3 3f ____
Ictaz &.L St ard ) a S’ 7 (7o VC LV) 4 ‘ 15/ V
4. M v QC Cats
3’ /,7.o / ____
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Katrir lptka D xp . i ta Cats ___ f70 ____ _____
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ICS/X D pH st . S’ ’y ( Tu Z Peat) I / _______
Xst Vtnk L ty (7 ZY Peat) . f1! (i Z ______
b. S’pte Cats _____
T. Jesuits — Orç.i4 Analysis Cats L t
(t Z Peat )
xoeat (Pri srT
irm s.uond OC oo& c ofL ati
ac Ct.grat rspox or data ayit prist aM
cuiL .rs 4 plots _______
y ost
CT ts u fr UC (U avaiLa Ja
7or sr4 je. 1 /p 5 co Lr ag pg
of raw u ctr and copi.. of backqrcundsu tz2 a4 rsU
spectra Of tarqst c- --- (s i.s S
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C. tta daxts Data
.tac.I1zz.eu. Data
crLq [ r t prspazztic a d -“ysia ie c pims o
raparati a ‘yiil 1og k aq s ____ ____ _____
tars .L aaapl . a. d a&p1. tra aia. . r ”tth—ot —
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gcr.. i q -
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S. m i L/ ac,Ltf. D - ,—--ta
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23.. 7Ii LAMW0U* L4 2 1b ‘
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23. X.re ry Mv Cats ____
24. CytnLds Mv CAts 2. O _______
23. PSXCSflt Solids Ca1 L&t1ona _4% 2.SJO
EPA Ra I Y C ’rn ”
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3.3. Pr.paxatio2 L (Ton xx ) Lit 1W —
13. Lnalysia Lcq (7cm T) çf I O _____
20. : 3.svOat& $ ___ ____ ______
21. 7I& .&IMVD$t& __ __ - .
22. 7urna M ZZ 2J( 2$ ______
23. X.rc uxy Pa CaM _____
24. Cyanide Mv 04t& 1 140 ____ _______
23. Psc.nt Solids 1 14I!1 1
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— • • ‘.• —
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OR NLC C LZT! C ?ILZ ( C. !) -.
3Lt ’ xc. xc.: 7 !!v / —zc.-
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(d.iczth. or list)
Prvp&r&ti n sc a __________________________ ___
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D.sc iti _______ ____ _______
33, Ot az Pacords (ds.cx .b. or list)
34
C plstad byt ____________ 4 J 2 I
(2 L&b) ( S ( SLq &*S ) prin jM/ jt a (;sz.)
nditd byt _____________ _____________
(173) (7:i ts4 xa siTitis)
EPA R. i ai CPC Ani.
-------
Attac ent I
Flcwckiart o Region I CSF Audit Prcgra
-------
CSF Tracling
Procedure
REGKJN I CSF AUDIT PROGRAM
CSF Evidence
Audit Procedure
Ship CSF to RSCC under
custody seal .
Receive CSF. check custody seai.
htUate CSf Rec4t/Trensfer Form.
bansfur CSF under custody seal.
Receive CSF. chock custody seals,
complete CSF Aecelpt/Transler Form
Perlomi avtdenco aucflt and data
valdaUon.
H appUcable, transfer C8F under
custody eee to BLb or ESI).
Receive CSF from Sub or E8 1).
check custody seal and complete
CSF FteceipllTransler Form.
Maintain final custody ol CSF until
contract expiration .
Receive CSF, check custody eeals,
corrçlelo CSF AecelpVTransfer Form.
Complole va dation.
- i Laboralory )
I
_____ f jtona1 Sample Contr I”
___ ( zime Contracto?\ ____
(Prime)
(oversight)
(va c1at ion)
1 PA QA Office ‘\
-.4 (ESt))
(Sub Contraclor’\
\ J L I
Compile CSF documents. generate
Form DC-2.
Ship CSF tinder custody seal
Generate now DC-2 for rest ibmiflals.
ship to Pnme under Custody Sea)
Perlorm evidence audit using
Photocopied Form DC -2.
Rocetvo vatidation rositbiflhttals.
perform tiuclit of now documents will
photocopy of nc w Form I)G2
Compilo at iclitorcompiututl
Form DC2s and send copy of
each to Techiaw.
Ship entire CSF to Ptirno w )’ion
data va cia1Ion cot nptoiod
Receive C8F. chock custody seals,
complete CSF Receipt/Transfer Form.
Complete valkiatlon oversight.
Transfer CSF under custody ea1 .
Transfer CSF tinder custody seal
-------
ATTACKNENT II
INORGANIC DOCUMENT INVENTORY CHECKLIST
-------
TULL I ORGANICS
COMPLETE SDG FILE (CSF)
INVENTORY SHEET
Lab Name: ___________________________ Cit’r/State:
Case No. SDG No. _____ SDC Nos. to Follow: ______ ______ ______
SAS No. Contract No. _______ SOW No.
All doctents delivered in the Complete SDG File muzt be original documents
where possible. (Reference Exhibit B, Section II D and Section III V)
__ E e Nos . (Please Check:)
From To Lab Region
1. Inventory Sheet (DC.2) (Do not number)
2. Cover Page
3. Inorganic Analysis
Data Sheet (Form I-IN)
4. Initial & Continuing Calibration
Verification (Form hA-IN)
5. CRDL Standards For AA and ICP
(Form liz-IN)
6. Blanks (Form 111-IN)
7. ICP Interference Check
Sample (Form IV-IN)
8. Spike Sample Recovery (Form VA-IN)
9. Post Digest Spike
Sample Recovery (Form ‘lB-IN)
10. Duplicates (Form VI-IN)
11. Laboratory Control Sample
(Form Vu-IN)
12. Standard Addition Results
(Form VIII-IN)
13. ICP Serial Dilutions (Form 1X-IN)
14. Instrument Detection Limits
(Form X-IN)
15. ICP Interelement Correction Factors
(Form XIA-IN)
16. ICP Interelement Correction Factors
(Form XIB-IN)
17. ICP Linear R.anges (Form XhI-IN) ____
18. Preparation Log (Form XIII-IN) ____
19. Analysis Run Log (Form XIV-IN) ____
20. ICP Raw Data
21. Furnace AA Raw Data
22. Mercury Raw Data
ILZtO2.O
Form DC-2
-------
Pate Nos . (Please Check:)
From To Lab Rezion
23. Cyanide Raw Data
24. Preparation Logs Raw Data
25. Percent Solids Deterination Log
26. Traffic Report
27. EPA Shipping/Receiving Documents
Airbill (No. of Shipments ____)
Chain-of-Custody Records
Sample Tags
Sample Log-In Sheet (Lab & DC1)
SDG Cover Sheet
28. Misc. Shipping/Receiving Records
(list all individual records)
Telephone Logs
29. . Internal Lab Sample Transfer Records &
Tracking Sheets (describe or list) ____
30. internal Original Sample Prep & Analysis Records
(describe or list)
Prep Records _________________
Analysis Records ______________
Description ___________________
31. Other Records (describe or list)
Telephone Counication Log
32. Coents:
Completed by (CLP Lab):
(Signature)
Audited by (EPA):
(Print Name & Title)
(Signature) (Print Name & Title)
(Date)
(Date)
Form DC-2 (continued)
ILMO2.0
-------
Attachment hA
B1ani CSF Receipt/Transfer Fo
-------
EPA REGION I
COMPLETE BDG FILE
RECEIRT/TRAIIBFER FORM
SDG: Data Package#:
Receipt
Date
Received by:
Maine mit. Affiliation
CSF
Activity
Custody Seals:
Present / Intact
(On Receipt)
V N V N
Released:
To Date
V N
IN
IN
V N
V N
IN
I N
V N
V N
V N
V N
V N
IN
V N
V N
I N
V N
V N
V N
V N
V N
V N
V N
V N
-------
Attach enc IIB
C p1eted CSF Receipt/Transfer Form
-------
I1?h flL GIOI1 I
COHVLET1 UDG FILE
RECEI T/TRANUPER FORH
h SDG: A.Pre Datapackage#:4c -
Received by:
Custody Seals:
Released:
Receipt
CSF
Present / Intact
Date
Name In It. AffiliatIon
ActivIty
(On R)
t n i
I&
c( (4Jas 4 Ar
Q &t I
( i ii
V i
AiiE JI1 ?CS
i
2 1
1 1L
y -
( iJc z
LZV
gc z
c..
kc: 4 c U-b-S
C
(Ii) n
(Y H
J
( ) U
a) 1
(? u
- -
t J Q ML
rn
2J .! 1J L_
2) 2
3I ’I II
‘1 ’
cui A1 1 .
f
J \AiZ
E
c j c &
Iw -
I
-------
£VJ REQION I
COHPLETI LJD FILE
RECErvT/Tn1 trnFEn FOUH
sr :
Receipt
Date
Received by:
CSF
CUstody Seals:
Present / Intact
Release d:
To Date
A )A CS iL1iL
t1a e mit. Affiliation
e c 1 I S
in “c
ji L1
Activity
tio
(C UkY \1C
(On
( N
( !
V H_
IN
V N
V H
Y N
Receipt)
( N
( ‘!
1 i
Y !‘
IN
V N
N
V N
V 11
V N
-------
ATTACHMENT III
EXAMPLE ORGANIC TABULATED SUIIMARY FORMS
-------
lÀ
EPA SAMPLE NO.
VOL 1’ILE ORGANICS ANALYSIS C TA SHEET
Lab Name: _______ - Contract:_____
Lab Code:
Case No.:
SAS No.:
SDG No.:
Matrix: (soil/water) ______
Lab Sample ID:
Sample wt/vol:
_______(g/mL) ____
Lab File ID:
Level: (low/med)
Date Received:
% Moisture: not dec.
Date Analyzed:
CC Column:
Soil Extract Volume:
ID: ______(nun)
________(u L)
Dilution Factor: _________
Soil Aliquot Volume: _____(uL)
CA.5 No.
COMPOUND
CONCENTRATION UNITS:
(ug/L or ug/Kg) _______
Q
I
I
74—87—3 Chioromethane_____
74—83—9 Brornomethane_________________ I
75—01—4 Vinyl Chloride______________ I
75—00—3 Chioroethane_________________
75—09—2 Methylene Chlor.de__________ I
67-64—1 Acetone______________________
75—15—0 Carbon DLsulflde____________
73—35—4 1,l—Dichloroethene__________
75—34—3 1,1—Dichioroetharme__________
540—59—0 1,2—Dichioroethene (total)_
67—66—3 Chloroform___________________
107—06—2 1,2—Dichioroethane__________
78—93—3 2—Butanorie___________________
71—55—6 1,1, 1—Trichioroethane_______
56—23—5 Carbon Tetrachlorjde________
75—27—4 Bromodichiorotnethane________
78—87—5 1,2—Dichioroproparie_________
10061—01—5 cis—1, 3-Dichioropropene_____
79—01—6 Trichioroethene______________
124—48—1 Dibromochiorornethane_________
79—00—5 1,1, 2—Trichlcroethane_______
7 1—43—2———----————Ber mzene ____________________
10061—02—6 trans—i, 3—Dichloroproperte_
75—25—2 Bromoforn____________________
108—10—1 4—Methyl-2—Per.tanone________
591—73—6 2—Hexanone___________________
127—18—4 Tetrachioroethene___________
79—34—5 1,1,2, 2-Tetrachloroothane_
108—88—3 Toluene______________________
108—90—7 Chlorohenzenc________________
100—41—4 Ethylbonzenc________________
100—42—5 Styrene_____________________
1330—20—7 Xyle e (totii) ____-
I
I
I
I
I
I
I I
I I
FORN I VOA
3/90
-------
13
EPA SAMPLE NO.
SEMIVOLATILE ORGANICS ANALYSIS DATA SHEET
Lab Code: Case No.: SAS NO.: SDG No.:
Matrix: (soil/water) ______ Lab Sample ID: __________
Sample wt/vol: ______(g/inL) ____ Lab File ID: __________
Level: (low’/med) _____ Date Received: _________
% Moisture: decanted: (Y/N)_ Date Extracted:_________
Concentrated Extract Volume: _______(uL) Date Analyzed: __________
Injection Volume: _____(uL) Dilution Factor: ________
CONCENTRATION UNITS:
COMPOUND (ug/L or ug/Kg) _______
108—95—2 Phenol_______________________
111—44—4 bis (2-Chloroethyl) ether_____
95—57—8 2—Chioropheno]._______________
541—73—1 1,3—Dich lorobenzene_________
106—46—7 1,4—Dich lorobenzene_________
95—50—1 1,2—Dich loroben zene_________
95—48—7 2—Methyiphenol______________
108—60—1 2,2 ‘—oxybis(l—Chloropropafle)
106—44—5 4—Methyiphenol______________
621—64-7 N-Nitroso—di-n—propy lamlfle_
67—72—1 ljexachloroethane_____________
98—95—3 Nitrobenzene________________
78—59—1 Isophorone__________________
88—75—5 2Nitrophefl o l_______________
105—67—9 2,4—Dimethy lpheno l__________
111—91—1 bis (2—Chloroethoxy)methane_
120—83—2 2,4—Dichiorophenol__________
120—82—1 1,2, 4—Trichlorobenzene______
91—20—3 Naphtha lene__________________
106—47—8 4—Chioroanilifle______________ ______________ _____
87—68—3 Hexachiorobutadiene _________ _____________ _____
59—50—7 4-Ch loro—3—methylpheflO l_____ _____________ _____
91—57—6 2-Methylrtaphtha lefle•
77—47—4 Hexach1orOCyC1Openta Lefle ______________ _____
8 8—06—2 2,4, 6—Trichiorophenol _______ ______________ _____
95—95—4 2,4,5—Trichiorophenol_______ ____________ ____
91—58—7 2—Ch loronaphthalene_________ _____________ _____
88—74—4 2—Nitroaniline ______________
131—11—3 Dimethylphtha late
208—96—8 Acenaphthy lene_______________
606—20—2 2,6—Dinitrotoluene —
99—09—2 3—Nitroaniline_______________ _____
83—32—9 Acenaphthene_________________
Lab Name:
Contract:
GPC Cleanup:
CAS NO.
(Y/N)_
pH:____
Q
—
I
I
—
—
I
I
I
I
I
I
FORM I SV-l
3/90
-------
EPA SA1’IPLE NO.
CONCENTRATION UNITS:
COMPOUND (ug/L or ug/Kg) _______
51—28—5 2,4—DinitrOphenol__________ —
100—02-7 4—NitrophenOl________________ —
132—64—9 DibenZOf uran_________________ —
121—14—2 2,4—Dinitrotoluene__________ —
84—66—2 Diethylphtha late_____________ —
7005—72—3 4_Ch loropherty l—PheflYlether_ —
86—73—7 Fluorefle_____________________ —
100—01—6 4—Nitroaflulifle_______________ —
534—52—1 4, 6—Dinitro—2—methylPfleflOl_I_
86—30—6 N—Nitrosediphenylamirle (1)_L
101—55—3 4 -Brom ophefly l—pheflyleth er_I_
118—74—1 Hexach lor obeflzerle____________ —
87—86—5 Pentachiorophenol____________ —
85—01—8 Phenanthrefle_________________ —
120—12—7 Anthracene___________________ —
86—74—8 Carbazole____________________ —
84—74—2 Dj -n-butylphtha late________
206—44—0 Fluoranthefle________________ -
129—00—0 Pyrene_______________________ -
85—68—7 Buty lbenzylphtha late
91—94—1 3,3 ‘-DichlorobeflZidifle______
56—55—3 Benzo(a)arithracefle__________ -
218—01—9 c hrysene
117—81—7 bis(2 -Ethy lheXYl)PhtXlalate_I.
117—84—0 Di-n—oCty lphthalate
205—99—2 Benzo(b)f lUoranthefle________
207—08—9 Benzo(k)f lUOrarlthefle________
50—32—8 Benzo(a)pyrefle I
193—39—5 Iriderto(1, 2,3—cd) pyrene______ I
53—70—3 Dibenz(a,h)aflthraCefle_______
191—24—2 Benzo(g,h,i)perylene I.
I
I
I
I
1C
SEMIVOLATILE ORCANICS ANALYSIS DATA SHEET
b Name:_________________________ Contract: _____
.ab Code: — • Case No.: — SAS Uc. _______ SDG No.:
atriX (soil/water) ______ Lab Sample ID: —
Sa p1e wt/v01 ______(g/mL) — Lab File ID: —
Level: (] .ow/ined) _____ Date Received:
Moisture; decanted: (Y/N)_ Date Extracted:_
Concentrated Extract Volume: _______(uL) Date Analyzed: —
Injection Volume: _____(uL) Dilution Factor:
GPC Cleanup: pH:____
CAS NO.
Q
— I
I I
I I
I I
(1) — Cannot be separated from Diphenylamine
•I I
I I
__J__I
__I
FORM I SV-2
3/90
-------
. 414.L Id.á.. £ ‘S
it)
PESTICIDE ORCANICS ANALYSIS DATA SHEET
Lab Code:
Case No.:
SAS No.: _______ SDC No.:
Matrix: (soil/water) ______
Sample wt/vol: _______(g/mL) —
% Moisture: decanted: (Y/N)_
Extraction: (SepF/Cont/Sonc)
Concentrated Extract Volume: _______(uL)
Injection Volume: _____(uL)
CAS NO.
(Y/N)_
COMPOUND
Lab Sample ID:
Lab File ID:
Date Received:
Date Extracted:__________
Date Analyzed:
Dilution Factor:
Sulfur Cleanup: (YIN) —
CONCENTRATION UNITS:
(ug/L or ug/Kg) _______
Q
319—84—6 alpha—BHC__________
319—85—7 beta—BHC___________
319—86—8 delta—BHC__________
58—89—9 gamma-BHC (Lindane)
76—44—8 Heptachlor
309—00—2 Aldrir
1024—57—3 Heptachior epoxide
959—98—8 Endosulfan I
60—57—1 Dieldrin
72—55—9 4,4’—DDE
72—20—8 Endrin
33213—65—9 Endosulfän II
72—54—8 4,4’—DDD
1031—07—8 Endosulfan su1 ate
50—29—3 4,4’—DDT____
72—43—5 Methoxychior
53494—70—5 Endrirt ketone
7421—36—3 Endrin aldehyde
5103—71—9 alpha—Chlordane
5103—74—2 gamma—Chiordane
8001—35—2 Toxaphene
12674—11—2 Aroclor— 1016
11104—28—2 Aroclor—1221
11141—16—5 Aroclor-1232
53469—21—9 Aroclor—1242
12672—29—6 Aroclor—1248
11097—69—1 Aroclor- 1254
11096—82—5 Aroclor— 1260
Lab Name:
ContraCt
GPC Cleanup:
pH:____
I I
I.
I
I
I
I
I I
I
I
I
I
I
.
I
FORM I PEST
3/90
-------
Lab Code: Case No.: ______
Matrix: (soil/water) ______
Sample wt/vol: _______(g/mL)____
Level: (low/med) _____
% Moisture: not dec.______
CC Column: ID: ______
Soil Extract Volume: _______(uL)
______ SAS 1o.: SOC No.:
Lab Sample ID: —
____ Lab File ID:
Date Received: —
Date Analyzed: —
Dilution Factor:
Soil Aliquot Volume: _____(ul..)
Lab Name:
lE
VOL1 TILE ORGANICS ANALYSIS DATA SHEET
TWTATIVELY IDENTIFIED cO ?0UNDs
ContraCt:
EPA SA1 PLE NO.
Number TICs found:
CAS NUMBER
CONCENTRATION UNITS:
(ug/L or ug/Kg) _______
COMPOUND NANE
RT
EST. CONC.
I I
IQI
I I
. 1 I
I I
1.
2.
3.
4.
5.
6.
7.
8.
9-
10.
11.
12.
13.
14.
15.
16.:
17.
18.
19.
20.
21.
22.
23.
24. -
25.
26.
27.
28.
29.
30.
. 1 I
. 1 I
.1 I
.1 I
.1 I
.1 I
. 1 I
.1 I
.1 I
.1 I
.1
:t
________________________ _________________________________________________________ _________________ ___________________________ ___________ I
_______ _________________ _____ ________ I ___ I
________ __________________ _____ ________ I ___ I
________ __________________ _____ ________ I ___ I
________ __________________ _____ ________ I ___ I
________ _________________ _____ ________ I ___ I
________ __________________ _____ ________ I ___ I
___________ I
I
I
I
I
I
I
I
I
I
I
I
I
FORM I VGA-TIC
3/90
-------
iF
SEMIVOLATILE CRGANICS AUALYSIS DATA SHEET ________________
TE::TATr:E:y I DEUTI Fl ED COM POCNDS
Matrix: (soil/water) ______
Sample vt/vol: ______(g/mL) ____
Level: (low/med) _____
% Moisture: ______ decanted: (Y/N)_
Concentrated Extract Volume: ______ (uL)
Injection Volume: _____(uL)
CONCENTRATION UNITS:
(ug/L or ug/Kg)_______
I IQI
- I ====——--—=========——========= I ======== ==== • - I ===== I
1. _______ I ________________ I _____ ________ I ___ I
2.____________ ___________________________ I ________ ____________I _____ I
3. ____________ ____________________________ I ________ _____________ I _____ I
4 . ____________________________ ________ I
5 . I ___________________________ ________ ____________
6 . ____________________________ ________ _____________
7 . _____________________________ _________
8 . _____________________________ _________
9 . ____________________________
10 . _____________________________ _________
11 . ____________________________ ________ _____________ _____
12 . ___________________________ ________ _____________
13 . _____________________________
14 . ______________________________ _________ ______________
15 . ___________________________ ________ ________ _____
16 . ___________________________ ________ _____
17 . _____________________________ _________
18 . __________________________ ________
19 . ___________________________ ________
20 . ____________________________ ________ _____
21 . ____________________________ ________ _____
22 . _____________________________ _________ _____________
23 . _____________________________ _________
24 . I ___________________________ ________ ____________ _____
25 . ____________________________
26. _____________ I _____________________________ _________ I _____
27. ____________ ____________________________ ________ I _____
28 . ___________________________ ________
29. ____________ ____________________________ ________ I _____
30. _____________ ____________________________ ________ I _____
Lab Code:
Lab Name: Contract:
EPA SAMPLE NO.
Case No.: SAS tb.:
I_
I
I
I
I
I
SDG No.:
Lab Sample ID: —
Lab File ID:
Date Received: —
Date Extracted:_
Date Analyzed: —
Dilution Factor:
GPC Cleanup:
(Y/N) —
Number TICs found:
pH:____
CAS NUMBER
COMPOUND NAME
RT
EST. CONC.
I __________________ _____ I ________
________ __ I ____
I _________ ___ ____
I __________________ _____ I ________
I __________________ _____ I ________
I __________________ _____ I _________
I I
I I
I I
I I
I I
I I
I I
I I
_______________________________________________________ E _____________________________________
_________ I ___________________ I ______
___________________________________________________________________ I
_________ I ___________________ I ______
.1 __________________________________________________________ I
FORM I SV-TIC
3/90
-------
2A
WATER VOLATILE S’!STEM MONITORING CO!IPOUND RECOVERY
Lab Name:_________________________ Contract:___________
Lab Code: . Case No.: SAS iTo.: SDG No.: _______
SMC1 SMC2 SMC3 IOTHER I I
(TOL) l(BFB)#l(DCE) _____
====== I ====== I =——--—= I I
________________________ ____________ I _____________ _____________ ____________ I_I
________________________________ I _________________ _________________ ________________ I_I
_____________________________ _______________ I _______________ _______________ _______________ I_I
____________________________ I ______________ I _______________ I _______________ _______________ I_I
____________ I _____________ I _____________ I I_I
____________________________ ______________ I _______________ I _______________ I I_I
__________________________ _____________ ______________ I ______________ I ’ I_
_____________________________ ______________ _______________ I _______________ I _______________ I_I
_________________________ I ____________ _____________ I _____________ I _____________ I_I
________________________ I ____________ _____________ I _____________ I _____________ I_I
__________________________ ______________ ______________ I ______________ I ______________ I_I
_____________________________ I _______________ I _______________ I _______________ I _______________ I_I
_____________________________ I _______________ I _______________ I _______________ I _______________ I_I
___________________________ I _____________ I ______________ I ______________ I ______________ I_I
_____________________________ _______________ I _______________ I _______________ I _______________ I_I
___________________________ _____________ I ______________ I ______________ I _____________ I_I
_____________________________ _______________ I _______________ I _______________ I _______________ I_I
_____________________________ _______________ I _______________ I _______________ I _______________ I_I
_____________________________ _______________ I _______________ I _______________ I _______________ I_I
___________________________ ______________ I ______________ I ______________ I ______________ I_I
_____________________________ I ______________ .I _______________ I _______________ I _______________ I I
_____________________________ I _______________ I _______________ I _______________ I _______________ I_I
_____________________________ ______________ .1 _______________ I _______________ I _______________
__________________________ _____________ I ______________ I. ______________ I ______________ I_I
________________________________ ________________ _________________ I _________________ I ________________ I_I
________________________________ ________________ _________________ I _________________ I ________________ I_I
________________ I I _________________ I ________________ I_I
_____________________________ ______________ I _______________ I _______________ I _______________ I_I
________ ____ I ____ I ____ I ____ I I
____I__I__I__I__:::i
QC LIMITS
SMC1 (TOL) = To luene—d3 (88—110)
SMC2 (BFB) = Bromofluorobenzene (86—115)
SMC3 (DCE) = 1,2-Dichloroethane—d4 (76—114)
Column to be used to flag recovery values
* Values outside of contract required QC limits
D System Monitoring Compound diluted out
EPA
SAMPLE NO.
01
02
03
04
05 H
O6
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
221
231
24
25
26
27
28
29
30
page — of
FORM II VOA-1
3/90
-------
28
SOIL VOLATILE SYSTEM MONITORING COMPOUND RECOVERY
Lab Name:
Lab Code:
Case No.:
Contra c .:
SAS No.:
SDG No.:
Level: (low/med) _____
02.
02
03
041
051
061
071
081
091
10
1].
12
13
14
.‘ —
16
17
18
19
20
21
22
23
24
25
26
27!
28!
29!
30!
EPA SMC1
SAMPLE NO. (TOL) #
SMC2 I SMC3 IOTHER ITOTI
(BFB) l (DCE)1 IOUTI
====== I ====== I ===== I == I
____________ I _____________ I —
_____________ I ______________ I ______________ I_I
______________ $ •I _______________ I_I
______________ I _______________ I _______________ I_I
_______________ I _______________ I_I
______________ _______________ _______________ _l
______________ _______________ I _______________ _I
______________ _______________ I _______________ _I
______________ I I_I
______________ _______________ I _______________
______________ _______________ I _______________
_______________ I _______________ _I
____________ I _____________ ____________ I_I
_____________ I ______________ _____________ I_I
_____________ I ______________ I ______________ I_I
_______________ I _______________ _______________ I_
I
I
—
—
l_
I
SMC1
SMC2
SMC3
I _______________
_______________ I_I
_______________ I—I
_______________ I_I
_______________ I_I
QC LIMITS
(84—138)
(59—113)
(70—121)
page — of
# Column to be used to flag recovery values
* Values outside of contract required QC limits
D System Monitoring Compound diluted out
I
(T0L) = Toluene—d8
(BFB) = Bromofluorobenzene
(DCE) = 1,2—Dich loroethane—d4
FORrI II VOA-2
3/90
-------
2C
WATER sE:1IVo TILE SURROGATE RECOVERY
Lab Name:
Contract:
Lab Code: _______
Case No.:
SAS No.: _______ SDG no.:
I I
I I
I I
EPA Si J S2 S3 I S4 S5 S6 I S7 S8 ITOTI
I SAMPLE NO. I(NBZ)# (FBP ) (TPH)#l(PHL) (2FP)# (TBP)#I(2CP)# (DCB) IOUTI
I ====== I ====== ———== ———— ——— I === I
_________________________ I ____________ ____________ I ____________ I _____________ _____________ ____________ I ____________ I _____________ I_I
___________________________ I _____________ I _____________ I _____________ I ______________ ______________ _____________ I ______________ I ______________ I_I
_________________________ I ____________ ____________ I ____________ I _____________ _____________ ____________ I ____________ I _____________ I_I
___________________________ I _____________ I _____________ I _____________ I ______________ ______________ I ______________ I _____________ I ______________ I_I
_________________________ ____________ ____________ I ____________ I _____________ _____________ ____________ I ____________ I _____________ I_I
_________________________ ____________ ____________ I ____________ I _____________ _____________ ____________ I ____________ I _____________ I_I
_________________________ ____________ ____________ I ____________ I _____________ I ____________ I ____________ I _____________ I_I
___________________________ _____________ I I _____________ ______________ I ______________ _____________ I _____________ I ______________ I_I
_________________________ ____________ ____________ I ____________ I _____________ ____________ I ____________ I _____________ I_I
___________________________ _____________ _____________ _____________ ______________ I ______________ ______________ I _____________ I ______________ I_I
___________________________ _____________ _____________ _____________ I ______________ I ______________ I ______________ I _____________ I ______________ I_I
___________________________ _____________ _____________ _____________ I ______________ I ______________ I ______________ I _____________ I ______________ I_I
___________________________ _____________ _____________ I _____________ I ______________ I ______________ I ______________ I _____________ I ______________ I_I
___________________________ _____________ _____________ I _____________ I ______________ I ______________ I ______________ I _____________ I ______________ I_I
___________________________ _____________ I I _____________ I ______________ I ______________ ______________ I _____________ I ______________ I_I
________________ ________ ________ I ________ I ________ I ________ ________ I ________ I ________ I_I
_________________________ ____________ ____________ I ____________ I _____________ I _____________ _____________ I ____________ I _____________ I_I
_______________________ ___________ ____________ I ___________ I ____________ I ____________ ____________ ____________ I ____________ I_I
___________________________ _____________ _____________ I _____________ I ______________ I ______________ ______________ I ______________ I ______________ I_I
_____________________________ ______________ I _______________ I _______________ I _______________ I _______________ _______________ I _______________ I _______________ I_I
___________________________ _____________ ______________ I _____________ I ______________ I ______________ I ______________ I ______________ I ______________
________ ____ ____ I ____ I ____ I I I ____ I ____ I I
___________________________ _____________ I _____________ _____________ I ______________ I ______________ I ______________ I ______________ l_ ._I
________ ____ I ____ I ____ I ____ I ____ I ____ 1 ____ I ____ I I
___________________________ _____________ ______________ I _____________ I ______________ I ______________ I ______________ I _____________ I ______________
___________________________ _____________ I ______________ I _____________ I ______________ I ______________ I ______________ I _____________ I ______________ I_I
___________________________ ______________ I ______________ I _____________ I ______________ I ______________ I ______________ I _____________ I ______________ I_I
______________________________ _______________ I _______________ I _______________ I _______________ I _______________ I _______________ I _______________ I _______________
___________________________ _____________ I ______________ I _____________ I ______________ I ______________ I ______________ I _____________ I ______________ I_I
_________________________ ____________ I _____________ I ____________ I _____________ I _____________ I ____________ I ____________ I _____________ I_I
Si (NBZ)
$2 (FEP)
S3 (TPH)
S4 (PHL)
S5 (2FP)
S6 (TBP)
S7 (2CP)
S8 (DCB)
= Nitrobenzerte-d5
= 2—Fluorobiphenyi.
= Terpheny l—d14
= Pheno l—d5
= 2—Fluorophenol
= 2,4, 6-Tribromopheno].
= 2—Chlorophenol—d4
= 1, 2—Dichlorobenzene—d4
QC LIMITS
(35—114)
(43—116)
(33—141)
(10—110)
(21—110)
(10—123)
(3 3—110)
(16—110)
page — of
Column to be used to flag recovery values
* Values outside of contract required QC limits
D Surrogate diluted out
01
02
031
041
05
061
071
081
09
10
12.
12
13
14
15
16
17
18
19
20
21
22
23
24
25 I
26
27
28
29
30
(advisory)
(advisory)
FORM II SV—1
3/90
-------
2D
SOIL SEMIVOL? TILE SURROGATE RECOVERY
Lab Name: Contract:___________
Lab Code: Case No.: SAS No.: SDG No.:
Level: (low/xned)
I EPA Si 52 j S3 j S4 I S5 S6 I S7 SB ITOTI
I SAMPLE NO. (NBZ)fl(FBP)# (TPH)#l(PHL)#I(2FP)#I(TBP)fl(2Cp) (DCB)IOUT:
— I- •l••• — --— I I I —I
0i ____________________ I __________ I __________ __________ I __________ I __________ I __________ I _ __________ I_I
02j I I I ______ I ______I ______ I _____ ______ I
031 ____________ ______ I ______ ______I ______ I ______ I ______ I ______ I I
04j ____________ ______ I ______ ______I ______ I ______ I ______ I_ I ______ I i
051 ____________ I ______ I ______ I ______ I ______I ______ I I ______ I 1
061 ____________ I ______ ______ ______I ______ I ______ I ______ I ______ I ______ I I
0•7I ______________________ I __________ ___________ ___________ I ___________ I ___________ I ___________ I ___________ I ___________ I I
081 _____________________ I __________ __________ __________ __________ I __________ I __________ I __________ I __________ I I
091 _____________________ __________ __________ I __________ __________ I __________ I __________ I __________ I __________ II
10 1 ________________________ ___________ ___________ I ___________ ____________ I ____________ I ____________ I ___________ I ____________ II
ill ___________ _____ I_____ _____ ______ ______ ______I_____ ______l I
3.2 _________________________ ____________ ____________ ____________ I _____________ _____________ I _____________ I ____________ I _____________
13 ______ I ___ ___ ___ I ___ ___ ___ ___ I ___ I_I
14 ______________ I _______ _______ _______ _______ I _______ I _______ _______ I _______ I_I
15 ____________ _____ I ______ I ______ ______I ______ V ______ ______ I ______ I ....... .j
161 ____________ _____ ______ ______ ______ I ______ I ______ ______ I ______ I_I
171 ___________ _____ _____ _____ _____I _____ I _____ _____I _____I_I
3.8 _____________________________________ I __________________ __________________ __________________ I ___________________ I __________________ I ___________________ I __________________ I __________________ I
19 ____________ I ______ ______ I ______I______ ______ I ______ I ______I ______ I
20 ____________ ______ ______ I ______I______ ______ I ______ I ______ V ______ I . . . . .I
21J ___________ _____ _____ I ______ I______ ______ I ______ I _____ ______
221 ___________ _____ _____ ______I I I ______ I _____ I I
231 ___________ _____ I _____ _____I I I ______ I _____ I ______I I
241 ______ I ______ I I ______I ______ I ______ I ______ I ______ I. . . . . . . . .. .j
25j ____________ I ______ I ______I ______ I ______I ______I ______I ______ ______ I_I
261 1 _____ I _____I _____I ______I I ______I _____ ______ I___..I
271 ________________________ I ____________ I ___________ I ____________ I . I ____________ I ___________ ____________
281 _____________________ __________ I __________ I __________ I __________ I __________ I __________ I __________ ___________ I I
29 ___________ _____ ______I ______ I ______I ______ I ______I ______ I ______ 1I
301 ____________ ______ ______ ______ I ______ I ______ I ______ I ______ I ______ I I
# Column to be used to flag recovery values
* Values outside of contract required QC limits
D Surrogate diluted out
page — of
Si (NBZ)
52 (FBP)
S3 (TPH)
54 (PHL)
S5 (2FP)
S6 (TBP)
57 (2CP)
S8 (DCB)
= Nitrobenzerie—d5
= 2—Fluorobiphenyl
Terphenyl—d14
Pheriol—dS
2-Fluoropheno].
= 2,4, 6—Tribromophenol
= 2-Chloropheno] .—d4
= 1, 2—Dichlorobenzene—d4
QC LIMITS
(23—120)
(30—115)
(18—137)
(24—113)
(25—121)
(19—122)
(20—130)
(20—130)
(advisory)
(advisory)
TORN II SV—2
3/90
-------
2E
WATER PESTICIDE SURROGATE RECOVER?
Lab Name: — Contract: ___________
Lab Code: Case No.: SAS No.: SDC No.:
CC Column(1): ________ ID: ( mm ) CC Coluinn(2): ________ ID: ____
I EPA
ISAMPLE NO.
TCX 1ITCX 2IDCB 1IDCB 2IOTHER IOTHER ITOTI
%REC #I%REC I%REC I%REC I (1) I (2) IOUTI
I ====== ====== I ====== I =——- - I I I
01 _____________________ ____________ 1 ____________ I _____________ I _____________ I ____________ I ____________ I_I
02 ___________ _______ I _______ _______ I _______ I _______ I ______ i_I
03 _____ ___ I ___ ___ I ___ I ___ I I I
O4 __________ ______ I ______ I ______ I ______ I ______ I I I
05 _______________________ I _____________ I _____________ I ______________ I ______________ I ______________ I _____________ I__I
061 __________ I ______ I ______ I ______ I ______ I ______ I ______ I I
071 __________________ I ___________ I ___________ I ___________ I ___________ I ___________ I __________ I I
081 _____________________ I ____________ I ____________ I ____________ I _____________ I _____________ I ____________ I I
091 __________ I I ______ I ______ I ______I ______I II
101 _______________________ I _____________ I _____________ I _____________ I ______________ I ______________ I _____________ II
ill __________ I ______I ______I ______I ______I ______ I ______ II
121 __________ I ______ I ______ I ______ I ______ I ______ I ______ II
131 __________ I ______ I ______ I ______ I ______I ______ I ______ I I
141 _______________________ I ______________ I ______________ I ______________ I ______________ I ______________ I _____________ I_I
151 __________________ I ___________ I ___________ I ___________ I ___________ I ___________ I __________ I I
161 _______________________ I ______________ I ______________ I ______________ I ______________ I _____________ I _____________ II
17 _________________________ I _______________ I _______________ I _______________ I _______________ I _______________ I ______________ I_.__..I
18 ___________ I _______ I _______ I _______ I _______I _______ I ______ I_I
19 ___________________________ I ________________ I ________________ I ________________ I _________________ I ________________ I ________________ I I
20 _______________________ I ______________ I ______________ I ______________ I ______________ I ______________ I _____________
2 . _________________________ I _______________ I _______________ I _______________ I _______________ I _______________ I ______________
221 _______________________ I ______________ I I ______________ I ______________ I ______________ I _____________ I_I
23 ___________ I ______ I ______ I _______ I I ______ I ______ I_I
24 _______________________ I ______________ I ______________ I ______________ I ______________ I ______________ I _____________ I_I
251 _____________________ I ____________ I _____________ I ____________ I _____________ I _____________ I ____________ I_I
261 _______________________ I ______________ I ______________ I ______________ I ______________ I ______________ I _____________ I_I
271 _______________________ I _____________ I _____________ I ______________ I ______________ I ______________ I _____________ I_I
281 _______________________ I ______________ I _____________ I ______________ I ______________ I ______________ I _____________ I_I
291 __________ I ______ I ______ I ______ I ______ I ______ I ______ I
OI ___________ I ______ I ______ I _______ I _______ I _______ I ______ I_I
TCX = Tetr ch1oro—m-xy1ene
DCB = Decachiorobiphenyl
# Column to be used to flag recovery values
* Values outside of QC limits
D Surrogate diluted out
age of
ADVISORY
QC LIMITS
(60—150)
(60—150)
FORM II PEST-i
3/90
-------
2F
SOIL PEs::cIDE SURROC tTE RECCVERY
Lab Name:_______________________ Contract:__________
La Code: Case No.: SAS No.: SDG No.:
GC Coluxnn(1): ________ ID: ( mm ) GC Column(2): ________ ID: ( mm )
TCX Tetrachloro—xn—xylene
DCB = Decachiorobiphenyl
ADVISORY
QC LIMITS
(60—150)
(60—150)
page — of
# Column to be used to flag recovery values
* Values outside of QC limits
D Surrogate diluted out
EPA ITCX 1ITCX 2 DCB 1IDCB 2 OTHER OTHER I
SANPLE NO.I%REC I%REC ‘ REC 1%REC (1) (2) OU”fl
==== I ====== I ====== =— — = I ===== — — — ————= = I
01 ___________ I ______ I ______ ______I _______ •______ ______ I
02 __________ I ______ I ______ ______ I ______ ______ I I I
03 __________ I ______ I ______ ______ ______ ______ I ______I_I
04 ______________________________ I __________________ I __________________ _________________ I ___________________ __________________ I __________________ I I
051 _________ I _____ _____ I ______ ______ I ______I I
06 __________ ______ ______ ______ _______ ______ I 1 1
07 __________ ______ ______ I ______ _______ ______ t ______I_I
081 __________ _____ ______ ______ I ______ I I
09 __________ ______ ______ I ______ ______ I ______I I
10 __________ ______ ______ ______ ______I ______I I
lit_________ _____ _____ _____ ______ ______I ______I t
121 _____ _____ _____ ______ _____I _____ II
131 _________ _____ _____ _____ ______ ______ I ______ I I
141 _________ _____ ______ _____ ______ ______ I ______ I I
151 __________ ______ ______ ______ ______ ______ I ______ I I
16 ___________ ______ ______ ______ _______ _______ i _______ 1 1
17 __________ ______ ______ ______ I _______ ______I ______
18 ___________ _______ _______ _______ I _______ I _______ I _______ I_I
19 _____ ___ ___ ___ ___ ___ ___ i
20 ___________ I ______ ______ ______ _______ I _______ I _______ I I
21 ___________ I ______ ______ ______ _______ I _______ I _______ II
22 ___________ I ______ ______ ______ _______ I _______ _______
231 __________ ______ I ______ I ______ I _______ I ______ I ______ I I
24 ________ _____ I _____ I _____ I _____ 1 _____ I _____ I_I
25 ______________________ _____________ ______________ I ______________ I I ______________ I _____________ I_I
26 ___________ ______ _______ I I _______ I _______ I _______I_I
271 _______________________ ______________ I ______________ I _____________ I ______________ I ______________ I ______________ I_I
281 _______________________ I ______________ I ______________ I I ______________ I ______________ I _____________ I_I
291 __________ I ______ I ______ I ______ I ______ I ______ I ______ I_I
301 _______________________ I ______________ I ______________ I _____________ I ______________ I ______________ I _____________ I_I
•I
-1
FOR 1 II PE T—2
3/90
-------
3A
WATER v0LAT::z flATRIX SPI1
-------
35
SOIL VOL.\TILE MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECO1ERY
Matrix Spike - EPA Sample No.:
COMPOUND
1, l— ich1oroethene I
Trichioroethene________
Benzene_________________
Toluene________________
Cri lorobenzene__________
MSD I
% I QCLIMITS
R.EC # RPD fl RPD I REC.
===========— I ——I——- I
______ I ______ I 22 159—1721
______ I ______ I 24 162—1371
______ I ______ I 21 166—1421
______ ______ I 21 159—1391
______ I ______ I 21 160—1331
____ I ____ I ____ I ____ I
# Column to be used to flag recovery and RPD values with an asterisk
* Values outside of QC limits
RPD:______ out of ______ outside limits
Spike Recovery:______ out of ______ outside limits
CO ENTS:
Lab Name: __________________
Lab Code: Case No.:
Contract: ____________
SAS 1o. _______ SDG No.:
— Leve l:(1ow/med) ____
SAMPLE I MS
I CONCENTRATION I CONCENTRATION
I (ug/Kg) ! (ug/Kg)
COMPOUND
SPIKE
ADDED
1,1—Dichioroethene_____ I _________
Trichioroethefle________ _________
Benzerie________________ _________
Toluene I _________
Chioroberizene I _________
IMS
I
I REC
I.
QC. I
LIMITS I
REC. I
59—1721
62—137 I
66—1421
59—139 I
60—133 I
TSPIK.E MSD
I ADDED ICONCENTRATI0N
I (ug/Kg) I (ug/Kg)
I ====== == I
FORM III VOA—2
3/90
-------
WATER SEMIVOLATILE MATRIX SPIKE/M.ATRIX SPIKE DUPLICATE RECOVERY
Lab Name:
Contract:
Lab Code:
Case No.: ______
SAS No.:
SDG No.:
Matrix Spike — EPA Sa p1e No.:
COMPOUND
Phenol I _________
2—Chiorophenol I _________
1, 4—Dichlorobenzene I _________
N—Nitroso—di-n—prop. (1) I _________
1,2, 4—Trichj.orobenzenel __________
4 —Chloro—3 —methy].phenol __________
Acenaphthe e____________
4—Nitrophenol__________
2, 4—Dinitrotoluene_____
Pentachiorophenol I.
Pyrene I.
QC LIMITS I
RPD ; RPD I REC. I
______ I 42 112—1101
______ I 40 127—1231
______ I 28 j36— 97j
______ 38 141—1161
______ 28 139— 981
______ 42 12]— 9 l
______ I 31 146—1181
_____ I 50 110— 801
______ I 38 124— 961
______ I 50 I 9—1031
______ I 31 126—1271
____ I ____ I ____ I
(1) N-Mitroso—di-n-propylamine
Column to be used to flag recovery and RPD values with
* Values outside of QC limits
RPD:______ out of ______ outside limits
Spike Recovery:______ out of ______ outside limits
CO! 1ENTS:
an asterisk
COMPOUND
S PIKE
ADDED
(ug/L)
S AN P LE
CONCENTRATION
(ug/L)
MS
CONCENTRATION I
(ug/L)
MS
REC
Phenol_________________ _________
2—Chloropheno l __________I
1, 4—Dichlorobenzene I __________
N—Nitroso—di—n-prop. (1) _________
1,2, 4—Trichlorobenzene_
4—Chloro—3—methylphenol I __________I
Acenaphthene I __________
4—Nitrophenol I _________I
2,4—Dinitrotoluene I _________
Pentachloropheno l______ __________
Pyrene
____________________________________________________________________ I
I I
I :
I
I
I
I
I
I
I QC. I
ILIMITSI
gi REc. I
I 12—1101
.127—123 I
36— 97!
41—1161
P39— 981
23— 9 I
46—1181
10— 801
24— 961
I 9—103 I
:126—1271
_I ______________
SPIKE
ADDED
(ug/L)
MS D
CONCENTRATION
(ug/L)
MsD
REC
____ ______ ___ I ___
______ ________ ____ I ____ I
______ ________ ____ I ____ I
FORM III SV—1
3/90
-------
3D
SOIL SEMIVOL.ATILZ MATRIX SPIKE/MAT X SPIKE DUPLICATE RECOVERY
Lab Name:_______________________
Lab Code: . Case No.: ______
Matrix Spike — EPA Sample No.: _____
Con trac:: ____________
SAS No.: _______ SDG No.:
Level: (low/med) ____
SPIKE
ADDED
(ug/Kg)
==
Phenol__________________ _________
2—Chiorophenol I_________
1, 4—Dichlorobenzene I __________
N—Nitroso—di—n—prop. (1) I_________
1,2, 4—Trichlorobenzene l__________
4 —Chloro-3—methylphenol _________
Acenaphthene___________
4 —Nitrophenol___________ __________
2, 4—Dinitrotoluene_____ _________
Pentachiorephenol______ _________
Pyrene__________________
(1) N—Nitroso—di—n—propylamifle
QC. I
LIMITS I
REC. I
26— 90$
25—102!
28—104 I
______ $4 1—126 I
_______ I 38—1071
_______ I 26—103
______ I 3 1—137
_______ I 11—114
______ $28— 89
______ 117—109
______ 135—142 I
____ I ____
: Column to be used to flag recovery and RPD values with
* Values outside of QC limits
RPD:______ out of ______ outside limits
Spike Recovery;______ out of ______ outside limits
CO? cENTS: _____
an asterisk
COMPOUND
SAMPLE
CONCENTRATION
(ug/Kg)
II
I
MS
CONCENTRATION
(ug/Kg)
MS
REC #
COMPOUND
SPIKE
ADDED
(ug/Kg)
MS D
CONCENTRATION
(ug/Kg)
MS D
REC
RPD
Phenol I
35
50
I 27
I 38
23
33
19
50
I 4
I 47 I
36
2—ChlorophenoJ. I
1,4—Dich lorobenzene I
N—Nitroso—di—n—prop.(1)I
l,2,4—Trich lorobenzene l
4—Chloro—3—methylphenol l
Acenaphthene
4—Mitrophenol__________
2,4—Dinitrotoluene_____
Pentachiorophenol______
Pyrerie_________________
I
I
I
I
QC LIMITS I
RPD R.EC.
$26— 901
25—102
28—104
141—1261
I 38—1071
26—1031
3 1—137 I
11—114 I
28— 891
17—1091
35—142 I
FORM III SV—2
3/90
-------
3E
WATER PEZT:C:DE MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
- Lab Name:_________
Lab Code: ________
Case No.:
Contract:
SAS No.:
SDG No.:
Matrix Spike — EPA Sa p1e No.:
I SPIKE I SANPLE I Z 15 I
I ADDED ICONCENTPATIONICONCE} TRATIOU
M.
%
I
I
QC. I
LIMITS I
COMPOUND
——
gamma—BHC
I
I
I (ug/L) (ug/L) I (ug/L)
=___-_ --_ I ======_=————
(Lindarte) I
Heptachlor_____________
REC
#1 P lC. I
I
56123
40—1311
40—1201
52—1261
56—1211
I38— 127I
I I
Aidrin_________________
Die ldrin_______________ I
Endrin________________ I
4,4’—DDT_______________ I
I
I
Column to be used to
QC LIMITS
RPD I PlC. I
I - =1
15 156—1231
20 140—1311
22 140—1201
18 152—126 I
21 156—1211
27 138—1271
____ I ____ I
flag recovery and RPD values with an asterisk
* Values outside of QC limits
RPD:______ out of ______ outside limits
Spike Recovery:______ out of ______ outside limits
CO ENTS:
COMPOUND
I SPIKE
I ADDED
I (ug/L)
I NSD
I CONCEN’IRATION
(ug/L)
ga a—BHC (Liridane)
Heptachior__________
Aidrin_____________
Dieldrin___________
Endriri_____________
4,4 ‘—DDT
MS 0
PlC
RPD
.1
FORM III PEST—i
3/90
-------
3F
SOIL PESTICIDE MATRIX spIKE/UATRI:•: SPIKE DUPLICATE RECOVERY
Lab Name:
Contract:
Lab Code:
Case No.: ______
SAS ?Io.:
SDG No.:
Matrix Spike - EPA Sample No.:
SPIKE SAMPLE MS I MS I QC.
I ADDED CONCENTRATIONCONCENTRATIONj % ILINITSI
I (ug/Kg) (ug/Kg) I (ug/Kg) I REC U REC. I
I ======== ======————=== I ============ I ——— I ====== I
____ I _________ _____________ _____________I ______ 146—1271
_________ _____________ I I ______ 135—1301
I _________ I _____________ _____________ I ______ 134—1321
I _________ I _____________ _____________ ______ 131—1341
__________ I ______________ ______________ ______ 142—1391
_________ _____________ ______________ ______ 123—1341
______________________ I ________________________________ ________________________________ ______________ I _______________ I
COMPOUND
gamnla—EHC (Lindane) ____I _________
Meptachior_____________ _________
Xl dr in_________________ _________
Dieldrin_______________ _________
Endrin__________________ _________
4,4 ‘—DOT________________ __________
QC LIMITS
RPD I REC.
_____________ I— —I
50 f46? l27I
31 135—1301
43 134—1321
38 131—1341
45 142—1391
50 23—134j
Colu mn to be used to flag recovery and RPD values with an asterisk
* Values outside of QC limits
RPD:______ out of ______ outside limits
Spike Recovery:______ out of ______ outside limits
C0 ENTS:
COMPOtJND
ga1 ia—BMC (Lindane) ____
Heptachior_____________
Al dr in________________
Dieldrin_______________
Endrin__________________
4 ,4’—DDT_______________
I.—
I SPIKE
ADDED
(ug/Kg)
MS D
CONCENTRATION
(ug/Kg)
N SD
?
PEC U
RPD #
,1 I
_______________ I _______________ I
____ I ____ I
____ I ____ I
I ____ I I
____ I ____ I ____ I
FOR.M III PEST-2
3/90
-------
EPA SAMPLE NO.
Lab Name:
Lab Code:
4A
VOLXILE METHOD BLANK SU 1ARY
ContraCt:
Case No.: SAS No.:
I __________ I
_______ SDG No.:
Lab File ID:
Lab Sample ID:
Date Analyzed:
Time Analyzed:
GC Column: _________ ID: ______ (mm)
Heated Purge: (Y/N) —
Instrument ID: __________
THIS METHOD BLANK APPLIES TO THE FOLLOWING SAMPLES, MS AND MSD:
CO ENTS:
EPA
SAMPLE NO.
LAB
SAMPLE ID
LAB
FILE ID
I TIME
ANAL?ZED
I
I
I
I
I
Oil
021
031
041
051
061
071
081
091
1OI
lii
121
131
14 I
151
161
171
181
191
20
211
221
231
241
251
261
271
281
291
301
I
I
I I
I I
I I
I
I
I
I
.
I
.
: I
I I
I I
I I
I I
I I
page — of
FORM IV VOA
3/90
-------
EPA SAMPLE NO.
Lab Name:
Lab Code:
Lab File ID:
Instrument ID:
4B
SENIVOLATILE METHOD BLANK SUMMARY
CoritraCt
Case No.: SAS Io.:
Matrix: (soil/water) ______
Level: (low/med)
SDG No.:
Lab Sample ID;
Date E ctracted:
Date Analyzed:
Time Analyzed:
THIS METHOD BLANK APPLIES TO THE FOLLOWING SAMPLES, MS AND MSD:
COMMENTS:
Oil
021
03$
04 I
O5
06
07
O8
09
10
11
l2
13
14
151
16
17
18
19
20$
21
22
23
24
25
26
271
281
291
301
_____________________________ I
____I
_I ________________________ I
_l ________________________ I
I
I
I
I
I
I
EPA
. LAB
LAB
I
DATE
SAMPLE NO.
———--——
SAMPLE ID
—--—=========
FILE ID I ANALYZED
==———————
I_______
____ I ___
________________________________________________________________ I
______ ____ I
_____ I ____ I
_________ I ______ I
________________________________________________________________ I ____________________________________________
page — of
FORM IV SV
3/90
-------
4C
EPA SAMPLE NO.
Lab Name:
Lab Code: __________________
Lab Sample ID:
Matrix: (soil/water) ______
Sulfur Cleanup: (Y/N) —
Date Analyzed (1)
Time Analyzed (1)
Instrument ID (1)
CC Column (1): _________
THIS
PESTICIDE I!ETHOD BLANK SUt 1ARY
I
I
I
I
I
I
EPA I LAB
SAMPLE NO. SAMPLE ID
DATE
I
DATE
ANALYZED
1IANALYZED 2
Contract:___________
Case No.: SAS No.: SDC No.:
Lab File ID:
Extraction: (SepF/Cont/Sonc)
Date Extracted:
Date Analyzed (2):
Time Analyzed (2):
Instrument ID (2):
ID: (mm) CC Column (2): ID:
METHOD BLANK APPLIES TO TiLE FOLLOWING SAMPLES, MS AND MSD:
I
I ============ —
Oil
021 I
03 I I
041 I I
05 I I
06 I
07 I
08 I
09
10 I
11
121 I
13 I
141 I
151 I
161 I I I
171 I
181 I I I
19 I I 1
201 I I I I
21
22 I I
23 1
24 I
25 I I
26
(mm)
=-
I
CO ENTS:
page — of
FOfl!I IV PEST
3/90
-------
5A
Lab Name:
Lab Code:
La.b File ID:
Instrument ID:
GC Column:
Contract:
SAS No.: ______ SDG No.:
BFB Injection Date:
BFB Injection Time:
Heated Purge: (Y/N)
I m/e I
I 50
I 75 I
95
f 96
I 173 I
174
1 175 I
I 176 I
177 I
01
02
03
04
05
06
07
08
09
10
1].
12
13
141
16 I
17J
181
19
20
211
221
VOLATILE ORGANIC INSTRUMENT PERFORMANCE CHICK
BROMOFLUOROBENZENE (BFB)
Case No.:
ID:
( mm )
ION ABUNDANCE CRITERIA
% RELATIVE
ABUNDANCE
8.0 — 40.0% of mass 95
30.0 — 66.0% of mass 95
Base peak, 100% relative abundance__________________
5.0 — 9.0% of mass 95
Less than 2.0% of mass 174
50.0 — 120.0% of mass 95 I
4 .O —9.0%ofma 5s174________________ C
93.0 — 101.0% of mass 174 C
5.0 — 9.0% of mass 176 C
•
)1
)].I
)1
1—Value is % mass 174 2—Value is % mass 176
THIS CHECK APPLIES TO THE FOLLOWING SAMPLES, MS, MSD, BLANKS, AND STANDARDS:
I EPA TINE •(
I 3AMPLE NO. I______________ ANALYZED I
I
LAB
SAMPLE
ID
LAB
FILE ID
DATE
ANALYZED
—— —
—
— I
I
I
I—
I
I
I
l
I
I
I
I
—
—
I
I
I
I
I
I
—
—
I
—
—{
of
page
FORN V VOA
3/90
-------
5B
SEMIVOLATILE ORGANIC INSTRUMENT PERFORMANCE CHECK
DECAFLUOROTRIPHENYLPHOSPHINE (DFTPP)
Lab Name:
Contract:
Lab Code:
Case No.:
SAS No.:
_______ SDG No.:
Lab File ID:
D PP Injection Date:
ION ABUNDANCE CRIT IA
— 80.0% of mass 3.98
than 2.0% of mass 69
69 relative abundance
than 2.0% of mass 69
— 75.0% of mass 198
than 1.0% of mass 1.98
Peak, 100% relative abundance
5.0 to 9.0% of mass 198
10.0 — 30.0% of mass 198
Greater than 0.75% of mass 198_
Present, but less than mass 443
40.0 — 110.0% of mass 198
15.0 — 24.0% of mass 442
T2IS CHECX APPLIES TO THE FOLLOWING SAMPLES, MS, MSD, BLAmCS, AND STANDARDS:
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
221_
page — of
EPA
LAB
LAB
DATE
TIME
SAMPLE NO.
SAMPLE ID
FILE ID.
ANALYZED
ANALYZED
:
I ______ I ______ I
I ______ ______ I
I ______ I _______ I
______ I _______ I
I ________________ I. I
I —
I.nstrument ID: DFIPP Injection Time:
30.0
Less
Mass
Less
25.0
Less
Base
I a/e
1 51
68
69
I 70
1 127
197
1 198
199
1 275
365
I 441
1 442
I 443
% RELATIVE
ABUNDANCE
__________________________ I ______ (
___________________________ ______ C
1—Value is % mass 69 2—Value is % mass 442
)2
FORM V SV
3/90
-------
6A
VOLATILE ORGANICS INITIAL CALIBRATION DATA
Lab Name:_______________________ Contract:___________
Lab Code: Case No.: LAS No.: SDC No.: _______
In.strument ID: ________ Calibration Date(s):_________
Heated Purge: (Y/N) — Calibration Times: __________
CC Column: _________ ID: ( mm )
ILAB FILE ID: RRF1O = RRF2O ____________ I
(RRF5O ____________ RRF 100=____________ RRF200=____________
I I I_ %I
1 O UND I RRF1O I P.RF2O RRFSO RRF100 RRF200 I RRF RSD I
.— -------I----- - - - - - - -H- - -I--
Iciloromethane I I______ I ______ ______I I I
IBra omethane * i _____i _____ _____ _____ _____ ____*
IVinyl Chloride *______ ______ ______ ______i______ ______ *
I loroethane______________ _____I _____I _____ _____I I I I
INethylene Chloride I I I ______ ______I I I I
jAcetone ______I ______i ______ ______ ______ ______ _____
Icarbon Disulfide___________ ______ I ______ I _____I I_____
ji,1—Dichloroethene * I I ______ ______I I I *
11, 1—Dichioroethane * I I ______I ______I I *
Il.2—Dichloroethene (total) I I______ I______ ______I _____I I I
ICh.loroform * I ______ I ______I ______I _____I I *
Jl,2—Dich.loroethane * I______ I ______ ______I ______I I *
j2—Butanone_________________ ______ ______ I ______I ______I ______ I______
Il,l,l—Trich. loroethane * I_____ ______I ______I_____ _____ _____
Icarbon Tetrach].oride * I______ ______I ______I ______ ______ _____*
IBromodichioromethane * I ______ ______I ______I______ ______I _____*
Il,2—Dichloropropane I _____ I ______ ______I ______I ______I 1 _____
Icis—] .,3—Dichloropropene * I ______ ______I 1 ______I I _____*
ITrichioroetherie * I ______ ______I ______I ______I I *
I Dibromochioromethane *______ ______I ______I ______I ______I______ _____*
11,1,2—Trichioroethane *______ I ______I ______I ______I ______I ______ _____*
IBenzene *______ I ______ I ______ I ______ I ______ I ______ _____*
ttrans —1,3 —D ichloroproperle_*______ I ______ I ______I ______I ______I______ _____*
IBromofor m *_____ I I ______I I ______I______ _____*
I4-Methyl—2—Pentanone I ______ I ______ I I ______I ______ _____ I
j2—Hexanone________________ I _____ I I ______I _____I _____I _____ I
ITetrachioroethene * I ______ I ______I ______I I______ _____*
J.l.l,2,2 —Tetrachloroethane_*______ I ______ I ______ I ______I ______I ______ _____*
IToluene *_______ I _______ I _______ I _______ I _______ I _______ ______*
jCilorobenzene * I _____I _____I _____I I I - *
IEthylbenzene * I ______I ______I ______ ______I I *
IStyrene * I ______I ______I ______I ______ ______ _____*
! Xylene (tota 1 ) *______ I ______ I ______I ______ I ______I I _____*
I - - -. ———========== I ====== I === = I —= I ———== I ==== I I I
IToluene—d8__________________ ______ ______ I ______I ______I ______I I _____I
IBromof luoroberizene *______ I ______ I ______I ______I ______I ______ I _____*
Il,2—Dlch loroethane—d4_______ I ______ ____ I _____I ______I ______I ______ I _____I
I __________________________________________ I _________ _I _________ I _________ I •I _________ I ________ I
* Compounds with required minimum RRF and maximum %RSD values.
All other compounds muzt meet a minimum RRF of 0.010.
FORU VI vo 3/90
-------
GB
SENIVOLATILE ORGANICS INITIAL CM..IBRATION DATA
Lab Name:_________________________ Conz act: ___________
Lab Code: Case No.: SAS No.: SDG No.:
Instrument ID: calibration Date(s):_____
Calibration Times:
IL .B FILE ID: RRF2O = RRF5O
IRR.F80 _____________ RRF12O — RRF16O=
I I
I I I
I
%I
I COMPOUND IRRF2O
RRF5O IRRF3O IRRF12OIRRF16OI
RRF I RSD I
-- —=— — I ====== ==== I ====== I ==== I —
IPhenol *______ I I I
lbis(2—Chloroethyl)ether_____ I
2—Ch].orophenol *______ I_______ I I
I1,3—Dichlorobenzene * I I
I -
I
I
I ===== I
I
I
I
I
jl4—Dich lorobenzene * I I
I
I1,2—Dichlorobenzene *______ I I
l2—Methylphenol *
I I
I I
12,2’—oxybis(l—Chloropropane)I
4—Methylphenol *______ I
IN_Nitr o di_n_propylam ine_*______ I I
IHexachioroetharie * I I
jNitrobenzene * I
l lsephorone * I I I
12—Nitrophenol *______ I I
I2,4—Dimethylphenol *______ I
Ibiz(2—Ch1oroethoxy)met iane *______ I I I
(2,4—Dichiorophenol *______ I
Il,2,4—Trichloroberizene *______ I I
INaphthalene *______ I
14—Chloroanjline I I I I
IHexachiorobutad iene I I
I4—Chloro—3—methylphenol * I
I2—Methylnaphthalene * I I
IHexachlorocyclopentadiene_I I
l2,4,6—Trich lorophenol *______ I I I I
I2,4,5—Trich loropheno]. * I I I
12—Chloronaphthalene *______ I I I
l2—Nitroaniline_____________ I
I Dimethylphthalate I I I
IAcenaphthylene * I
12,6—Dinitrotoluene *______ I
I3—Nitroaniline_____________ I I
IAcenaphthene a______
l2,4—Dinitropheno l I______ I I
I4—Nitrophenol I I I
IDibenzofuran *______ I I I
12,4—Dinitrotoluene *______ I
I I. I I I I
* Compounds with required minimum RRF and maximum %RSD values.
All, other compounds must meet a minimum RRF of 0.010.
I
I
I
I
I
I
I
I
I
I
•
I *
I
I
I
I
I
I
I
I
I
I
I
I
I
I I
FORM VI SV—l 3/90
-------
6C
S (IVOLATILz ORGANICS INITIAL CALIBRATION DATA
Lab Name:________________________ Contract:__________
Lab Code: _______ Case No.: SAS No.: ______ SDG No.:
Instrument ID: _________ Calibration Date(s):__________
Calibration Times: _________
LAB FILE ID: RRP2O — RRF5O
RRF8O —_____________ RRP 12O— RBP 16O —___________
CCMPOCND RRF2O RR.F50 R.F80 RRF12O RRF16O RR.F RSD
Diethylphthalate____________ ____________________ ______ ______ ______ _____
4 —Chloropbenyl-phenylether_*______ ______ ______ ______ ______ ______ _____*
Fluorene * *
4 —Nitroanjljne_______________ ______ ______ ______ ______ ______
4, 6-Dinitro—2-methylpX eno1 ______ ______ ______ ______ ______ ______ _____
N-Nitrosod.iphenylamine (l)_ ______ ______ ______ ______ ______ ______ _____
4 -Bromoplienyl-phenylether * ______ ______ ______ _____*
Mexachlorobenzene * *
Pentachlorophenol * ______ ______ ______ *
Phenanthrene * *
Anthracene * *
Carbazole____________________ ______ ______ ______ ______ ______ ______ _____ I
Di—n—butylpbthalate_________ ______ ______ ______ ______ ______ ______ _____
Fluoranthene *
Pyrene * *
Butylbenzylphthalate________ ______ _____
3,3’ —Dichlorobe.rtzjdjne______ ______ _____
Benzo (a) anthracene *
Chrysene * *
bis (2-Ethyihexyl) phthalate_ ______ ______ _____
Di—n—octylphthalate_________ ______ ______ _____
Benzo(b)fluoranthene * *
Benzo(k)fluoranthene a *
Benzo(a)pyrene a *
Indeno(1,2,3—cd)pyrene *______ ______ _____*
Dibenz(a,h)anthracene - a *
Eenzo(g,h,i)pery lene a *
Nitrobenzene—d.5 I ______ ______ ______ _____*
2—Fluorobipheny]. a______ _____*
Terpheny l—d 14 * ______ ______ _____*
Phenol—dS a______ ______ _______ *
2—Fluoropheno]. * *
2,4 ,6—Tribromophenol I_____ ______ ______ ______ _____I
2—Chlorophenol—d4 a______ ______ *
l,2—Dichlorobenzene—d4 *______ ______ *
______________ I ___ ___ ___ ___ ___ ___ ___ I
(1) Cannot be separated from Diphenylamine
* Compounds with required minimum RRF and maximum %RSD values
All other compounds must meet a minimum BPS of 0.010.
FORN VI SV—2 3/90
-------
60
PESTICIDE INITIAL cALIBRXrION OF SINGLE COMPONENT AN1 LYTES
b Name: _________________________ Contract: ___________
Lab Code: Case No.: SAS No.: SDG No.: _______
Instrument ID: _________ Level (x low): low mid ____ high ____
GC Column: __________ ID: ( mm ) Date(s) Analyzed: _______ ________
epoxi.de_
I__________
RT OF STANDARDS I MEAN I RT WINDOW
COMPOUND LOW I MID I HIGH I RT I FROM I TO I
— I — I — I ===== I ======
alpha—BHC___________ ______ ______ ______I ______I ______I ______ I
beta—BHC____________ ______ ______ ______I ______I I ______I
delta—B c___________ ______ ______ ______ I ______I I ______
gamxna—BHC (Lindane) ______ ______I ______I ______I ______I I
Heptachlor__________ ______ ______ ______I ______I ______I I
Aldrin_______________ ______ ______ _______I _______I ______ I_______
Heptachior ______ ______ ______I ______I ______I I
Endosulfan ________I______ I ______I _______ I ______I ______ I ______
Dieldrin_____________ I ______ ______I _______ I _______I ______I ______I
44’—DDE___________ I ______ ______I ______ I ______ I ______ I ______ I
Endrin________________ I _______ _______I _______ I _______ I _______ I _______ I
Endosulfan II I______ ______I ______I ______I I I
4,4’—DDD________________ I ________ I ________ I ________ I ________ I ________ I ________ I
Endosulfan sulfate I ______I ______I ______I ______I ______I______ I
4.4’—DD’r___________________ I _________ _________ I __________ I __________ I _________ I _________
Methoxych] .or I______ ______I _______I ______I ______I______
Endrin ketone I______ ______I I ______I ______I______ I
Endrin aldehyde I I I ______I ______I ______I ______ I
alpha—Ch lordane I I I ______I ______I ______I ______ I
gamma—Chiordane I I ______I ______I ______I ______I ______
l————I======l======l
Tetrachloro—m—xylene l I I I ______I _____I______ I
Decachlorobjpheny ll I ______ ______I ______I ______ ______
_____________ I ____ I ____ I ____ I ____ I ____ I ____ I
* Surrogate retention times are measured from Standard Mix A analyses.
Retention time windows are ± 0.05 minutes for all compounds that elute
before Heptachior epoxide, ±0.07 minutes for all other compounds,
except ±0.10 minutes for Decachiorobiphenyl. -
FORM VI PEST—I
3/90
-------
6E
PESTICIDE INITIAL CALIBRATION OF SINGLE COMPONENT ANALYTES
ab :lame:
Contract:
Lab Code:
_______ Case No.:
SAS No.:
SOC No.:
Level (x low): low _____ mid — high _____
( mm ) Date(s) Analyzed:
Surrogate calibration factors are measured from Standard Mix A analyses.
.RSD must be less than or equal 20.0 % for all compounds except the
.;urrogates, where %RSD must be less than or equal to 30.0%. Up to
tio target compounds, but not surrogates, may have %RSD greater than
20.0% but less than or equal to 30.0%.
Instrument ID:
CC Column:
ID:
COM POUND
MEAN ! %RSD
I
=========== I ===•===
j I
I
I
I CALIBRATION FACTORS
I LOW I MID HIGH
======= ==._.=___.._= I I — — — I
alpha—BHC___________ __________ __________I __________
beta—BHC __________ I __________I __________
delta—BHC___________ __________ I __________
gamma—BHC (Lindaneji I I __________
Heptachior___________ I I I ___________
Aidrin I I I __________
Heptachj.or epoxl.de l__________ __________I __________
Endosulfan I________ I __________I __________I __________
Dieldrin____________ I __________I __________
4,4’—DDE____________ I _________ I _________
Endrin_______________ __________I.__________
Endosulfari II _________ __________ I.
4,4’—DDD____________ __________ __________ I,
Endosulfan sulfate __________ __________
4,4’—DDT_____________ I __________ __________ I.
Nethoxychior_______ I _________ _________ I.
Endrin ketone_______ I __________ __________ ___________
E drin aldehyde_____ __________ __________ __________
aloha—Chiordane_____ __________ I __________I ___________
gamma—chiordane I
=——— —-——--== I
— —
Tetrachloro—m—xylene I
I
Decach lorobjpheny l l__________
==— ——I -
_______ I _______ I
_______ I _______ I ____ I
_______ I ________ I ____
===========
_______ I _______ I ____
_______ I ____
_______ I ________ I ____
FOt M VI PEST-2
-------
6F
PESTICIDE 11!TAL C LIBRATIOU OF I1ULTCO PONENT ANALYTES
Lab Name:
Lab Code:
Instrument ID:
GC Column:
Case No.:
ID:
( mm )
Contra ct:•
SAS No.:
Date(s) Analyzed:
ANOUNTI I
(ng) IPEAKI RT I
I ====== I
*1 I _______
*2 I _______ I
*3 _______
41 ____
________ _5_I ______I
_________ *1 I _______
*2 I _______
1*31 ____I
141 ____
______I
I *1 _______I
*2 I _______ I
*3 _______
41 ____I
________ I *1 I _______
I *2 _______
*3 _______
4 _________
5
4
SDG No.:
CALIBRATION I
FACTOR I
______________________________________ I
,i I
.
I
I
____ I ____
_________________________________ I ________________________________
________ 1*11 _______ I ______ I
I *2 I _______ I _______
*3 ________ _______ I
141 ____ I ____
________ _______ I ______ ______
_________ I l I _______ I _______ I ______
I I ________ I _______ I _______
*3 ________ _______ I _______
I I ____ I ____ I ____
_____ I ____ I ____ I ____
_____ I ____ I ____ I ____
I ____ I I ____
I ____ I ____ I ____
I ____ I ____ I ____
_____ I ____ I ____ I ____
_____ I I ____ ____
I ____ I ____ I ____
I ____ I ____ ____
141 ____ ___ I ___
151 ____ I ___ ___
____ __ I ___ I ___ I ___
Aroclor 1254 I ________
I I
______________ I _____ I
Aroclor 1260 ________
I _____________ I _____ —
COMPOUND
Toxaphene
RT WINDO 4
FROM TO
—
—I
I Aroclor 1016
I Aroclor 1221
I Aroclor 1232
I Aroclor 1242
I Aroclor 1246
______________________________ __________________________________________________________ I
______________________________ ___________________________________________________________ I
______________________________ ___________________________________________________________ I
______________________________ ___________________________________________________________ I
______________________________ ___________________________________________________________ I
_______________________________________ __________________________________________________________________________ I
___________ 5
*3
4
___________ 5
_________ I *1
I I *2
I I
*3
* Denotes rcquired peaks
FORN VI PEST-3
3/90
-------
PESTICIDE ANi L’LTE RESOLUTION SUMMARY
Lab Name:
Lab Code:
Case No.:
Contract:
SAS Ho.:
_______ SDC No.:
CC Column (1): _________ ID: (mm)
EPA Sample No. (Standard 1.): _________
Date Analyzed (1):
Instrument ID (1): ________
Lab Sample ID (1): ___________
Time Analyzed (1): _______
01
02
03
041
05
06
07
08
09 I
I
I IRESOLUTIONI
I
ANALYTE I RT I (%)
—= =—==————————————=————————=== I — I
I I
I
I
I
I I
I I
I I
I I
I
I
CC Column (2): _________ ID:
EPA Sample No. (Standard 2):
Date Analyzed (2): ____________
( mm )
Instrument ID (2):
Lab Sample ID (2):
Time Analyzed (2):
01
02
03
04
05
06
07
08
09
I
IRESOLUTION
I
ANALYTE I RT I (%) I
— — I =====
I I
I
I
I
I
I
I
Resolution of two adjacent peaks must be calculated as a percentage of the
height of the smaller peak, and must be greater the- - r equal to 60.0%.
FORtI VI PEST—4
3/90
-------
7A
VOLa\TILE CONTINUING CALIBRAT:Ou CHECK
Lab Name:________________________ Contract:__________
Lab Code: Case No.: SAS No.: SDG No.: _______
Instrument ID: Calibration Date: Time:
Lab File ID: ____________ Thit. Calib. Date(s): _________
Heated Purge: (YIN) — mit. Calib. Times:
GC Column: _________ ID: ( mm )
1 I IMINI MAXI
I COMPOUND. RRF jRRF5O I RRF I D %D I
I ====== —— I
IChioro methane______________ _____ _____ I _____ I
IBromomethane_______________ ______ ______ 0.1001 ______ 125.01
1Vinyl Chloride______________ ______ ______ 0.100 125.01
1 Chioroethane_________________ ______I I
IMethylene Chlor .de_________ ______ ______ I ______I I
lAcetone____________________ ______ ______I I ______I I
JCarbon Disulfide___________ ______ ______I ______I I
I1,1—Dichloroethene_________ ______ ______ 0.100 ______ 125.01
I1,1—Dichloroet :-e_________ ______ ______ 0.200 ______ 125.01
Il,2—Dichloroet e (total)_ ______ ______ I ______ I I
Ichioroform__________________ ______ I ______ 0.2001 125.01
11,2—Dichioroetriane_________ ______ ______ 0.1001 ______ 125.01
12—Butanone I _____ I _____ I _____I I
I1,1,1 —Tricnioroetr ane I ______ I ______ 0.1001 ______ 125.01
ICarbon Tetrachioride I ______ ______ 0.100 1 125.01
IBromodichioromethane________ I ______ I ______ 10.2001 125.01
11 ,2—Dichioroproparie________ I ______ I ______I I ______ I I
Icis—l,3—Dich].oropropene I ______ I 10.2001 ______ 125.01
ITrichioroethene____________ I ______ 10.3001 ______ 125.01
IDibromochioromethane I ______ 10.1001 125.01
1.1,1,2—Trichioroethane I ______ ______ 10.1001 125.01
lBenzene______________________ I ______ ______,!O.500I ______ 125.01
Itrans—1,3—D ch1cropropene ______ I ______ 10.1001 ______ 125.OI
lBroinoform____________________ ______ I ______ 10.1001 ______ I25.OI
14—Methyl—2—Pentanone________ ______ I ______ I I
J2—Hexarione_________________ ______ I ______I
ITetrach1oroet1 ene__________ ______ _____ 0.2001 125.01
I].,1,2,2—Tetrachloroethane ______ ______ 10.5001 125.01
IToluene_____________________ ______ ______ 10.4001 ______ 125.01
ICh lorobenzene______________ - ______ ______ 0.5001 ______ 125.01
IEthylbenzene________________ ______ 0.1001 ______ 125.01
IStyrene_____________________ ______ ______ 0.3001 ______ 125.01
IXylene (total) ______________I ______ I 0.300 1 125.01
I === I === I I I
jToluene—d3___________________ I ______I ______I _____ I ______I ____I
IBromof luorobenzene_________ I ______I ______ 10.2001 125.01
11,2—Dichloroethane—d4_______ I ______I._____ I _____I ______ I ____I
__________________ I ____ I ____ I ___ I ____ I ___
All other compounds muzt meet a min].I:lum RRF of 0.010.
I
FORM VII VOA
3/90
-------
70
SEMIVOLATILE CONTINUING CALIORATION C EC1(
Jamc: _________________________ Contract: ___________
.ab Code: Case No.: SAS No.: SOC No.:
:nstru ent ID: __________ Calibration Date:__________ Tirne:_
b File ID: ___________ mit. Calib. Date(s):__________ —
mit. Calib. Times: ___________ —
I I MIN I I MAXI
I COMPOUND RRF IRRFSO RRF I %D I %D I
I = == — —= =——— — I I I I I
IPhenol_____________________ ______I 10.8001 125.01
jbis(2—Chloroethyl)ether_____ ______I 10.7001 125.01
12—Chiorophenol_____________ ______I 10.8001 ______ 125.01
I1,3—Dichlorobenzene________ _____I _____ 10.6001 _____ 125.01
I1,4—Dichlorobenzene________ ______I ______ 0.5001 125.01
I1,2—Dichlorobenzene I ______I ______ 0.4001 125.01
12-Methyiphenol_____________ ______I ______ 0.7001 125.01
12,2’—oxybis( l—Chloropropane) _____I_____ I _____I I
4—Methylpheno1______________ ______I 10.6001 125.01
I N—Nitroso—di—n—propylaml.ne_ ______ ______I 0.5001 ______ 125.0 I
IHexachioroethane___________ _____ 10.3001 125.01
INitrobenzene_______________ ______ 10.2001 125.01
l lsophorone_________________ ______ 10.4001 125.01
12—Mitrophenol I ______ 10.1001 ______ 125.01
12,4—Dimethyiphenol I ______I 10.2001 ______ 125.01
Ibis(2—Ch loroethoxy)methane_l _____I 10.3001 125.01
j2,4—Dichlorophenol I ______I______ 10.2001 125.01
Il,2,4—Trich lorobenzene I ______I ______ 10.2001 125.01
jNaphthalene I ______I 10.7001 125.01
I4-Chloroani ll.ne I _____I ______ I I ______ I
IHexachiorobutadiene I _____I I I _____I I
14-Ch loro—3—methylphenol I ______I 10.2001 125.01
12-Methy lnaphtha].ene I _____I 10.4001 125.01
IHexachlorocyc lopentadiene_l _____I I I ______I
12,4,6—Trichiorophenol I _____I 10.2001 125.01
12,4,5—Trichiorophenol I I 10.2001 _____ 125.01
12-Chloronaphthalene I I ______ 0•800l 125.01
12—Nitroaniline I ______I ______I I ______ I
IDimethylphtha late I _____ ______I I ______I
IAcenaphthy lene_____________ I _____ I 11.3001 125.01
126—Dinitrotoluene I I 10.2001 125.01
3-Nitroani1ine_____________ ______I ______I I ______I
(Acenaphtherte_______________ _____I 10.8001 125.01
12 .4-Dinitrophenol__________ I _____ I ______I I ______I
!4-Nitrophenol_____________ I I ______I I _____I
I oibenzofuran_______________ I ______ I 10.8001 125.01
2 ,4—Dinjtrotoluene_________ I _____ I ______ 10.2001 125.01
I _____ ___________ I ____ I ____ I ___ I ____ I ___ I
All other compour ds must mcet a minimum RRF of 0.010.
FOI M VII SV-]. 3/90
-------
7C
SEMIVOLATILE CONTINUING CALIBR/ TIC? CHECK
•b ! arne:__________________________ Contract: ___________
b Code: • Case No.: SAS No.: _______ SDG No.:
:nstrument ID: __________ Calibration Date: Time:
.ab File ID: ______________ mit. Calib. Date(s):___________
mit. Calib. Times:
I I_ I IMINI IMAXI
I COMPOUND RRF IRRF50 I RRF I %D I %D I
I =====————- = — — ====== I I ===== I I === I
IDiethy lphtha late___________ _____I I I _____I I
j4—Chlorophenyl—phenylether_ ______I ______ 10.4001 ______ 125.01
IFluorene____________________ ______ I ______ 10.9001 ______ 125.01
J4—Nitroanilirie_____________ ______I ______I I ______I I
14,6—Dinitro—2—methylphenol_I ______I ______ I I ______ I
IN—Nitrosodiphenylamine (1)_I ______I I I ______I
14—Bromophenyl—phenylether_l _____I 10.1001 125.01
IHexach lorobenzene I _____I 10.1001 125.01
IPentachiorophenol I_____ _____ 0.0501 125.01
IPhenanthrene _____ ______ 0.7001 ______ 25.01
lAnthracene_________________ ______I______ 0.7001 ______ 25.01
ICarbazole__________________ ______I______ I ______
lDi—n—butylphtha late I I______ I _____ I
jFluoranthene______________ _____I _____ 0.6001 _____ 25.01
IPyrene______________________ ______ I ______ 10.6001 ______ 125.01
lfluty lbenzylphthalate_______ _____I I I _____I
l3, ’—Dichlorobenzidine_____ ______ I ______I I _____ I
IBenzo(a)anthracene I _____ I 10.8001 125.01
IChrysene____________________ I ______ I ______ 10.7001 ______ 125.01
Ibis(2—Ethylhexyl)phthalate_l ______I ______I I ______I I
lDi—n—octylphtha late I _____I I I _____I
IBenzo(b)fluoranthene I ______I 10.7001 125.01
IBenzo(k)f luoranthene I _____I 10.7001 125.01
lBenzo(a)pyrene______________ I ______ I ______ 10.7001 125.01
lInder o(1,2.,3—cd)pyrene I ______I ______ 10.5001 125.01
Dibenz(a,h)anthracene I ______I ______ 10.4001 125.01
Benzo(g,h,i)pery lene I ______I ______ 10.5001 ______I25.Of
—— ——======= ======== = = I
INitrobenzene—d5 I I ______ 10.2001 125.01
12—Fluorobiphenyl I ______I ______ 10.7001 125.01
jTerphenyl—d14_______________ I ______ I ______ 10.5001 ______ 125.01
lPhenol—d5___________________ I ______ I ______ 10.3001 ______ 125.01
12—Fluorophenol______________ I ______ I ______ 10.6001 ______ 125.01
12 .4,6—Tribromophenol I ______ I I I _____I I
I2—Chlorophenol—d4___________ I ______ I ______ 10.8001 ______ 125.01
I1,2—Dich lorobenzene—d4_____ I _____ I ______ 10.4001 125.01
___________________ I ____ I ____ I ___ I ____ I ___
(1) Cannot be separated from Dlphenylam.1.ne
All other compounds must meet a minimum RRF of 0.010.
FOflM V II SV—2
-------
7D
PEST:cIDE CALIBRATIOU VERIFIC TIOU SUMMARY
Lab Name:________________________ Contract: __________
Lab Code: Case No.: SAS No.: SDG No.:
CC Column: — ID: ____ (mm) mit. C ilib. Date(s):
EPA Sample No. (PIBLK): _________ Date Analyzed :
Lab Sample ID (PIBL}C):___________ Time Analyzed :
EPA Sample No. (PEM): __________ Date Analyzed :
Lab Sample ID (PEM):__________ Time Analyzed
PE.H I I RT WINDOW I CALC MOM I I
I COMPOUND I RT I FROM I TO I AMOUNT AMOUNT I RPD I
I ________________________ I I _________ I I (ng) ( ng ) I ________
I === I ==== I I — - I — I
I aipha—BEc__________________ I ______ I _______ I _______ I -_I _________I ______ I
Ibeta—BHC I ___I I ___ _____I _____I ___ I
I gamma—BHC (Lindane) _______I ______I ______ I ______ ________ I ________ I _____ I
lEndrin____________ I ____ I ____ I ____ I _____ I _____I ___ I
I -4,4’—DDT___________________ ______ I ______ I ______ I ________ I ________ I _____ I
Methoxycrilor I ______ I ______ ______ I ________I ________I _____I
I _________________ I ____ I ____ I ____ I _____ I _____ I ___ I
4,4’—DDT % breakdc rn (1): _______ Endrin % breakdown (1): _______
Combined % breakdown (1):
QC LIMITS:
RPD of amounts in PEM must be less than or equal to 25.0%
4,4’—DDT brc3kdown must be less than or equal to 20.0%
Endrin breakdown must be less than or equal to 20.0%
Combined breakdown must be less than or equal to 30.0%
F0 :: VII PEST—i 3/90
-------
7E
PESTICIDE CALIBRATION VERIFICATION SU tARY
Lab Name: ________________________ Contract:_
Lab Code: Case No.: 5hZ No.: SDG No.:
GC Column: _________ ID: ( mm ) mit. Calib. Date(s):_______ _______
EPA Sample No. (PIBLK): _________ Date Analyzed
Lab Sample ID (PIBLK): __________ Time Analyzed
EPA Sample No. (INDA): ________ Date Analyzed
Lab Sample ID (INDA): ____________ Time Analyzed __________
INDIVIDUAL NIX A RT WINDOW CALC MOM
COMPOUND RT FROM TO AMOUNT AMOUNT RPD
(ng) (ng)
_______ _______ ==
gamma—BHC (Lindane) _______
Heptachior_________________ ______ ______ ______ _________ ________ _____
Endosulfan I______________ ______ ______ ______ ________ ________
Dieldrin___________________ ______ ______ ______ _________ ________
Endrin_____________________ ______ ______ ______ _________ ________ _____
4 ,4 ‘—DDD_________________ ______ ______ ______ ________ ________ _____
4,4’—DDT________________ _____ _____ _____ _______ _______ ____
Methoxychior______________ ______ ______ ______ ________ ________ _____
Tetrachloro-m-xylene______
Decachiorob iphenyl________
EPA Sample No. (INDB): Date Analyzed ________
Lab Sample ID (INDB): __________ Time Analyzed :_____ —
INDIVIDUAL MIX B RT WINDOW CALC MOM
COMPOUND RT FROM TO AMOUNT AMOUNT RPD
- (ng) (ng)
beta—BHC -
delta—BHC ________ ________ _____
Aidrin____________________ ________ ________ _____
Heptachior epoxide________ _________ ________ _____
4,4 ‘—DDE_________________ _____ ______ ________ _____
Endosulfan II ______ ______ ______ _________ ________ _____
Endosulfan sulfate________ ________ ________
Endrin ketone_____________ ______ ______ ______ ________ ________ _____
Endrin aldehyde___________ ______ ________ ________ _____
aipha—Chiordane___________ ______ ________ ________ _____
gamina—Chlordane___________ ______ _________ ________ _____
Tetrachloro-m—xylene______
Decachlorobiphenyl________ ________ _____
QC LIMITS: RPD of amounts in the Individual Mixes must be less than
or equal to 25.0%.
FORM VII PEST-2 /90
-------
8A
VOLATILE nrrERNAL STANDARD AREA AND RT StJ1 ARY
Lab Name:
Lab Code: - Case No.: ______
Lab File ID (Standard): ____________
Instrument ID:
CC Column:
ID:
Contract:
SAS No.: ______ SDG No.: _______
— Date Analyzed:___________
•Time Analyzed:
AREA UPPER LIMIT = +100% of internal standard area
AREA LOWER LIMIT = — 50% of internal standard area
RT UPPER LIMIT = +0.50 minutes of internal standard RT
RT LOWER LIMIT = —0.50 minutes of internal standard RT
: Column used to flag values outside QC limits with an asterisk.
* Values outside of QC limits.
( mm ) Heated Purge: (Y/N) —
IS1 (BEN) = Bromochloromethane
1S2 (DFB) = 1,4—Difluorobenzene
153 (CBZ) = Chlorobenzene—d5
page _..of —
FORM VIII VOA
3/90
-------
88
SEMIVOLATILE INTERNAL STA-UDA.RD AREA AND RT SUMMARY
Lab Name:
Contract:
Lab Code:
________ Case No.:
SAS No.: _______
SDG No.:
Lab File ID (Standard):
Date Analyzed:
Instrument ID:
Time Analyzed:
1S1(DCB)
AREA #
12 HO YR STD
UPPER LIMIT
LOWER
LIMIT
RT •
1S3 (ANT)
AREA
AREA UPPER LIMIT = +100% of internal standard area
AREA LOWER LIMIT = — 50% of internal standard area
RT UPPER LIMIT = +0.50 minutes of internal standard RT
RT LOWER LIMIT = —0.50 minutes of internal standard RT
Column used to flag internal standard area values with an- asterisk.
* Values outside of QC limits.
page of
4
“a.
1S2 (NPT)
EPA SAMPLE
NO.
RT
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
IS1 (DCB) = 1,4—Dich].orobeylzene—d4
1S2 (NPT) = Naphthalene—d8
153 (ANT) = Acenaphthene—d lO
FOP.Z1 VIII SV-] .
3/90
-------
page — of
8C
SEMIVOL TILE INTERNAL STANDARD AREA AND RT SU 1ARY
Contrac:: - ________
SAS Uo.: SOC No.:
Date Analyzed:
Time Analyzed:
I 1S4(PHN)
I AREA
I =====—- -—=
12 HOUR STD
UPPER LIMIT
LOWER LIMIT
RT I
====== I
.1
IS5(C Y) I
AREA
RT
156 (PRY)
AREA
EPA SAMPLE I
NO.
RT iLl
Lab Name:
Lab Code: . Case No.:
Lab File ID (Standard): _____
Instrument ID: ___________
. 1 ___________ _______________
Oil _____________ __________
021 ____________ __________
031 ___________ _________
04 I ___________
05 1 ____________ __________
06 _____________ ___________
07 ____________ __________
08 ______________ ___________
09 ____________ __________
10 ______________ ___________
l1 ____________ __________
12 _____________ ___________
13 ______________ ___________
14 ______________ ___________
15 ______________ ____________
161 ____________ __________
171 ____________ __________
181 ____________ __________
19 ______________ ____________
20 ______________ ___________
21 ______________ ___________
22 ____________
I ===== —
======—
I
—I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
I
—
I
I
I
I. I
I
I
.
l_
I
I
I
I
I I
I I
I I
I
I I
I I
I I
I I
I I
I
I I
I I
I I
I
I
I
I
I
1S4 (PHN) = Phcnanthrenc-d lO
155 (CRY) = Chrysene—d12
156 (PRY) = Perylene—d12
AREA UPPER LIMIT = +100% of internal standard area
AREA LOWER LIMIT = — 50% of internal standard area
RT UPPER LIMIT = +0.50 r inute of intern 1 standard RT
RT LOWER LIMIT = —0.50 minutes o internal standard RT
Column used t flag irt rnal 5tandard area va)ues t:ith an asterisk.
* Values outside of QC li itZ.
ror rt VIII
3/90
-------
SD
PESTICIDE ANALYTICAL SEQUENCE
Z:.: Uame:
Contract:
.ib Code:
Case No.:
SAS No.:
SOC No.:
C C 1utnn:
ID: ____(nm) mit. Calib. Date(s):_______ -—
Instrument ID:
Oh
02
03
04
05
06
07
08
09
10
11
12
13
14
151
161
17
18j
191
201
211
221
23 I
24 I
25
26]
27]
281
29
301
311
321
EPA I
SAMPLE NO. I
— I
TCX = Tetrach loro-m-xylene
DCB = Decachiorobiphenyl
Column used to flag retention
* Valucs outside of OC limits.
QC LIMITS
(± 0.05 MINUTES)
(± 0.10 MINUTES)
______ I ______ I
_____ I _____ I
_____ I _____ I
_____ I I
_____ I _____ I
_____ ______ I
_____ I ______
_____ I _____
_____ _____ I
_____ I _____
_____ I _____ I
_____ _____ I
___________________________________________ I
__________________________________________ ___________________________________________ I
_________________________________________ ___________________________________________ I
__________________________________________ ___________________________________________ I
__________________________________________ ___________________________________________ I
_____ ______ I
________ ________ I
_____ I ______ I
_____ I ______ I
__________________________________________ ___________________________________________ I
_____ I ______ I
_____ ______ I
time values with an asterrsk.
THE ANALYTICAL SEQUENCE OF PERFORMANCE EVALUATION MIXTURES, BLANKS,
SAMPLES, AND STANDARDS IS GIVEN BELOW:
MEAN SURROGATE RT FROM INITIAL CALIBRATION
TCX: ______ DCB: ______
LAB
SAMPLE ID
DATE
ANALYZED
‘I
TINE
ANAL? Z ED
=========
TCX I DCS I
RT :i RT !
I ======== I
I
I—
I
I I
— of
ror i VIII PEST
3/90
-------
9A
PESTICIDE FLORISIL CARTRIDGE CHECK
:.. b 1ame: _________________________ Contract:___________
L .3b Code: Case No.: SAS No.: SDG Mo.:
Florisil Cartridge Lot Number: — Date of Analysis: ____
ZC Column(1): ________ ID: ( mm ) CC Column(2): ________ ____
I SPIKE
ADDED
COMPOUND (ng)
-
a lpha-BMC_________________ _________ _________ ______
gamma-BMC (Liridane)______ ________ ________ ______
Heptach lor_______________ _________I _________ ______
Endosulfan I_____________ ________ _________ ______
Die ldrin__________________ _________ I _________ ______
Endrin_____________________ _________I _________
4,4’—DDD__________________ _________ I _________
4,4’—DDT_______________ •1 ________
Methoxychior______________ I I _________ ______
Tetrachloro-rn—xylene I I _________ ______
Decachiorobiphenyl I I _________ ______
_________________ I ______ I ______ ____ _____
Column to be used to flag recovery with an asterisk.
* Values outside of QC limits.
THIS CARTRIDGE LOT APPLIES TO THE FOLLOWING SAMPLES, BLANKS, MS , AND MSD:
ID: — (mm)
SPIKE I
RECOVERED % I QC I
(ng) IREC # LIMITS I
==——== I ====== ===——— I
__________ I _______ I 80—120 I
___________ I _______ I 80—120 I
___________ _______ 80—120 I
___________ I _______ I 80—120 I
I _______ I 80—120 I
__________ I I 80—120 I
I I 80—120 I
___________ I 80—120 I
___________ _______ I 80—120 I
__________ I _______ I 80—120 I
___________ _______ I 80—120 I
______ I ____ I _____ I
EPA I LAB I DATE
I SAMPLE No. SAMPLE ID IANALYZED
I
1
DATE I
ANALYZED 2
==—-I
- -
-—-=1=
—
I
I
I
I
I
I
.
I
I
—I___
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18J
191
201
2l
22J
2)1
I
I
I
I
I
I I
I
I
I I —
I
— of
.1
I _I
FORM IX PEST—I
3/90
-------
PESTICIDE GPC CALIBRATIC
Lab Name:
Lab Code:
GPC Column:
GC Column(1):
________ Case No.:
ID:
____ Contract:
______ SAS No.:
_______ SDG No.:
Calibration Date:
( mm ) CC Colurnn(2): —
_____ ( mm)
I.
COMPOUND
______ I ______
___________________________________________________________________________ I. ___________________________________ I _________________________________
Oh
02j
03 I
04 I
051
061
071
081
091
10 I
ill
121
13
14 I
15 1
16 I
17 I
18
19
20
211
221
23 I
241
251
261
_________ I _____
gamma—BHC (Lindane) _______
Heptachior________________
Aidrin
Dieldrj.n I
Endrin
4,4 ‘-DDT
SPIKE I SPIKE I I QC.
ADDED IRECOVEREDI % ILIMITS
(ng) I (ng) I REC fl REC.
========= I ========= I ====== I
_________ _________ ______ 180—110
__________ _________ I ______ 180—110
_________ _________ I ______ 180—110
_________ _________ I ______ 180—110
_________ _________ I ______ 180—1101
_________ I ______ 180—1101
I _____________ I _____________ I
Column to be used to flag recovery values with an asterisk
* Values outside of QC limits
THIS CPC CALIBRATION APPLIES TO THE FOLLOWING SAMPLES, BLANKS, MS A.ND MED:
EPA I LAB I DATE I DATE I
SAMPLE NO. I SAMPLE ID ANALYZED 1IANALYZED 21
= ======= I ============= I ========== =====—— —— I
‘
I
I I
I
I
I
I
I
I
I
I
!
I
I
I
I
I
I
I
I I
I I
I I
I I
I
page — of
FO! IZ PE T-2
3/90
-------
EPA S? PLE NO.
1OA
r’ESTICIDE IDENTIFICATION SUUMARY
FOR SI :cLE COMPONENT ANAL?TES
__________________________ Contr c : ___________
________ Case No.: — SAS No.: _______ SDG No.:
___________ Date(s) Analyzed: ________
___________ Instrument ID (2): _____
_________ ID: ( mm ) GC Column(2): _________
I I I P.T WINDOW
ICOLI RT I FROM TO
I ===I ====== I ====== I
I I I I
Ill ____ I ____ I ____
I I I
121 ____I ____ ____
I I I I
I I I I
Ill ____ I ____ I ____
I I I
121 ____ ____ ____
I I I I I’
I I I I I
Ill ____ I ____ I ____ I
I I I I I•
121 ____ I ____ I ____ I ________
I I I I
I I I
Ill ____ I ____ I ____ I ________
I I I I
121 ____ I ____ I ____ ________
I I I I
I I I I
I ]. I ____________ I _____________ I ____________
I I I I I
I 2 I ______I _______ I _______ I .
I I I I I
I I I I I
Ill ____ I ____ I ____ I
I I I I I
121 ____ I ____ ____
I. I I
I I I I
Ill ____ I ____ I ____
I I I
121 ____J ____ ____ ________
I I I
I I
Ii I ____ ____ _________
12 ____ ____ _________
Lab Name:
Lab Code: ________
Lab Sample ID
Instrument ID (1):
CC Column(1): ________
I
I
I
I
I
I
ANALYTE
ID:
( mm )
CONCENTRATION
I _______________________________
I ________________________________
page — of
I i
I I
I I
I I
I I
I I
I I
FOR;1 X PEST-i
3/90
-------
lOB
EPA SAMPLE NO.
Lab Code:
Lab Sample ID
Instrument ID (1):
PESTICIDE IDENTIFICATIC! SW H ARY
FOR MULTICOMPONCNT AI’!Ai..YTS
Case No.:
SAS No.:
SDG No.:
Date(s) Analyzed:
Instrument ID (2):
At least 3 peako are required for jdentj jcatjon of inulticomponent analytes
page — of
Lab Name:
Contract: ___________
CC Columri(j.):
( nm) CC Column(2): __________ ID: _____ (mn)
ID:
======—===
I
I I RT WINDOW I I MEAN
I
I
ANALYTE
PEAK I RT I FROM I TO I CONCENTRATION CONCENTRATION
%D
,
— = ==— I ==—— I ===I =====
1 I I
I 21 I I I
I 31 I I I
COL(JNN1 141 I
I I
I I I I
I 1 I I I
I 21 I I
I 31 I I I
COLTJMN2 141 I I I
151 I I I
1= I ====== I ! = = —========
Ill I I I I
121 I I I I I
131 I I I I
COLUMN 1 141 I I I I
151 I I I I I
I I I I I I
Ill I I I I I
121 I I I I
131 I I I I I
COLTJMN2 141 I I I I
151 I I I
==== I ====== I I ===== I ============= I == ==-==———
Ii•I I I I I I
121 I I
131 I I I
141 I I I
151 I I
I I I I I
I ii I I
I 2 I I
I 31 I I
141 I I I I I
151 I I I I I
I I I I I I I
I COLUMN
1
I COLUMN
2
1•O M x PE T—
3/90
-------
Attachment l i lA
Blank Organic and Inorganic DC-2 For
-------
—QRG IC. CO PLETZ .SDG 11 12 -. C ) •
-
- - •. .. — ••) — t.. ¼• - :‘ w -. -: i -
L 3OMT I - ‘ -. - : - - 4 • - ‘ - ç1T!IS” -:
-
DG T0 ______
— ________ —
•.•b - A
•• _,— .. - — • - • , . .
, e t5. . •r — w-. •..— • . -.“-‘ —I- • ,-lP-.i
LL docu sntz d.iLy x LA pi a iLL. mist oriq -. 1
.sLb1.. (RZZ x -ii T 3, SZC X I 1 A aZCTX XXI I)
YP’ (
.. II1v tOt? Sb t (7or DC’2) (Do t nt I .r )
2. $DC Ca.aa
i. ? r*ffte pF
4. Vo a j1q Dat-a
a. QC St? 7
S ircqats Perc. t Racavsry I axy (1oz L ) ________
)CSIXSD Duplicats Bt ” -’7 (70r III VC&)
X.thod 3 ank s ary (7oz 17 VC&) _______
Tt ” 4 -’ g end Kaas Calibration (70 V V ) _______
b. Sanpls Data
T. Rasulta — (Tom X VO&)
sntati .ly Identified Cc po .nda (7oz I VO&—TZC) _____ _______
R.ccn.t Ct 5d total. ion c atcgraa (RIC) iar
s apl
Tor sacs sampl .s
Raw sp.ctra and of backgrcd-fobt !act .d
aai .p.ctra of target c ndz idsntLfid
Mass spectra of aLL rs rtd IC ’i with three Mat
lLh.r&rT
c. Standarts Data (AU Inatr I)
Initial CaU.hratie ’ Data (7o Vt V ) _______
RICa and Q ien Rapezts for aLL Sta.ndarda ________
Continting C 14hratLo (7cm VI I ) _______
RICa and Q ian Reports for aLL Standards ________
InternaL Standard rea 5” ’y (7o v a.a ) _______
d. Raw QC Data
an ___
Zlank Data _______
Matrix $pike Data ________
Matrix SpiAa Duplicate Data ________
a. QC 3t1w 1 7
Surrogate Percent Racavexy S a.ry (T U IV)
/n.sn S” ’-’7 (Tcrm III IV)
Method Blank $tiw 4 7 (7o IV IV)
?ui li g and Kiss Calibration (70 V IV )
EPA Rcgionai CZF CompIcxo csz Atz hmo t 2
Eyid Audil G idcth
5• two1atiIe Oats
Page 1 of 4
-------
..‘ L R%S ZT CcL
- - DG L, ’iO 7 rJr j ___________
— / —__-_——‘a_. — - - -;-;-- _ •
PAaz I
1
3. Data (cozztd)
b Sa pL. Data
T ResuLts (7cra X tV)
? tattvsIy IdeutUi.d c pour4a (7c Z ST-T ic)
Recooatauct.d tcta.t ion c v a gzaa ( XC) i c r . a —
a apLs
7cr iac $lN 1SZ
Raw spectra and backiroun4 subtr*z ad ap
spectra of T Cpounds
(au spectra of Tic ’s with 3 best library eatc
CPC c atcgraaa (U CPC perfc —. .l )
C. 5t&r4& s Data (All Inltx ta
Initial Calibration Data (7cr vi LV)
ca and Q nn Reports for all stan.daxda
Continuing Calibration (Yor v i : SVJ
RICa and Qu*n Reports for sit standards
Thtaxn&j Standard Ares 8t? .rI4ry (70r VIlIS I V )
Internal St 4&r4 Arsa B ’ - y (Tcxm VI C IV)
4. Raw QC Data
hank Data
Matrix Spike Data
Matrix Spike D plicats Data
5. P e,tjc j4 .
a. QC S ary
Surrogate Percent Recovery “ -y (7or i: Pest)
MS/MZD Duplinate sw . iiry (7oz X i : Pest)
Metbod hlank S iry (POrm IV Pest)
b. Saple Data
i’ . Reaulti — Organic Matysis Data Sheet
(TeEm I Pest)
ro atograss (Primary l )
x atogvaaa ir second CC col fL=ation
CC Integration report or data syst print a
calibration plots
Manual i erk sheets _______
DV traces i GPO (if available)
7cr pesticides/PORe coui1x by GC/xs, copies
of- raw spectra and copies of bac rc d_ acted ase
spectra of target nda (samples & standaxds)
EPA Regicnii CZF Coi ezatc 2
Evida c AuduGuidehi cs Pige 2 of 4
-------
- S ORGANIC - IOMPLETZ EDG JIL J( Ce?) iV OR!. S M1{T (Contd) I --
f — t G SD 3 OS. TO p??1 — ‘ •.- 4
- - - -
P3
T 4 ?Ø — —
6. Pesticides (Co td)
C. Stad&rds Data
Pesticides v&Luatio Standard.s S” ’7
(70 VIII , Pest —i)
Pesticides rvalw -4 !tand.ards S” -.’7
(7o VIII, Psst 2) ________
Pesticid./P Sta d,rdz S zry (7o , Pest) _______
P.sticida/P Ide t12icar4 n (7cm X. Pest) ________
Standard chr ttoqra a a.@d data syt int t
for all standards
Per pssticidas/PCZs contix .d by GC/XS, copies of
spectra for standards ..d
d. Mv QC Data
31an.k Data
Xatrix Spike Data
_____Jtatrix Spike D zpU.c ate at.a
7. Lsce1Ianeo ig Data
Orig 1 -’ a1 prparation and an.lysis fors or copies of
preparation and analysis logbook page.
Internal. sample and s& pla extract tra.naf sr .in—of—
ctstody .c rds
Sorsning records
All instrt.nt oQtp t, ioclgd4 strip charts fr
screening activities (d.ecr .bs or list) _______
e. * pp Receirtha Dcc — s
kirbtlls (110. of shi nta I
atn of — ust dy R.da
Sa.pl. Tag.
Sample Log—Zn Sbat (Lab &
0 Ccvsx S .st
X.Lsc.llan.ous EhLpping/Rec.iyinq *a d.s
(describ, or list)
. Tnter .tl Lab Sample ?ransfer Re -ds aDd ?s 4, Sh..ta
(d.scrib. or list)
EPA Rq ana1 CZF CompIczo s A hm 2
Evid AudLGuidd 5 es Page3of4
-------
ORCA IC CO L EDG T 1 Z ( fl fliW TOR! :-:.: -
I : -
- z X 7 ’ G O_?0L -. ‘ . . ;
—••- - - - - —
10. P cordi (d.scrib. ar list)
T1qth ne C ,, iMeati L
fi
c pl.t. by:
(2 Lab)
AT cit.d by:
cm)
( ata)
EPA Rcg anaI CSF Coc&aicu
Ev ” Audit Guide1 c
A”n t 2
(Signaturs)
(5iq &tur)
(Print.4 Xa ./TLt1e)
( &ta)
(Pri ts4 Ka s/TLt1a)
Page 4 of 4
-------
• •. :: I ORG? 2(IC COWPLZTX SDG ZILZ C i V OR s zT; . •‘
— -•,--—,‘ . q ,. —.4 -
LOT i j - ‘- CII JS ‘ •
— — t -
czIQ.-—Ir” gDo £DG O3 .
L ‘• • I . F —
• - A i rn c— - ‘ -
TRACT ROe’ •
- •‘ ‘ ‘ .• -. - — - • -
J.U docu.nta d.iiv.rsO in t e co pJ..t. SDG iLa ast be a: qina , 4Qcu nta vbsre
possible. (RZ7 Z I3IT 3, £Z TIC2( II C AND £3CT011 III
7R — - -
1. Inventory Sheet (7or DC 2) (Do not ni b.r) _____ _______
2. Cover Peg. ____ ____
3. Inorganic Analysis Data Sheet (T 1) ____ ____ _____
4. Initial. and continuing Calibration V.rificetion (?c II .
Part 1) ___
5. L Standard i cr AX and I (7or II. Part 2) ____ ____
6. !la (7ez III )
7. Intari.r.nce .ck Sa.npl. (7cr V) ____ ____
8. Spike Ga.npl. P.covery (7or V, Part 1) ____ ____
9. Post Digest SpLIce Sarpl. Recovery (?o 7, Part 2)) ____ ____ _____ _______
i D. Dixplicatss (7or VI) ____
1. Laboratory Control. Saople (7c VII) ____ ____ _____
—‘ . Standard Addition Results (Ya VIII) ____ ____
I Serial. Dilutions (Tor IX) ____ ____
.4. Instrunent Detection Lifflits Quarterly (7o I) ____ ____ _____
15. I Thter.l.oent Correction 7actorz, Annua.Uy (7or ,
Part 1)
IS. I Tht.r.l. ant Correction 7actors, Annually (To ,
Part 2)
17. LLn.ax Ranges Quarterly (Tor ) ____ ____
is. Preparation Log (lcr TTII ) ____
19. AnaLysis Run Log (7oz XT)
20. I Raw Data
21. 71a e AX Raw Data
22. 7u.rnacs U Raw Data
23. Xercuxy Raw Data
24. Cyanide Raw Dat
25. Percent Solids Calculationg
EPA Region 1 CSF Comple&azcis Arr thm 1
Evidowe AudiL Gwdth Pigs 1 of 2
-------
I ORG 4 RIC CC LZTZ SDG PILZ (CS?) -
— —— —.. — ‘ -‘ — — — .- — . —— ., __ —. — — ——— —. • — *d
____‘ DC 0. S G XOS. —..
, , ,. ,. ——- —. . : — , ,•
‘ 2 L_2
26. DLstil1ati zi L . (Cya id.s O iy) ____ _____ ________
27. DLg.stio Loqs ____ _____ ________
28. Traliic Bapart ____ ____ _____ ________
29. ZPA Shipping/Bacaivitq oc szta
LrbiUs (Ito. of shir4nta ) ________
c ain—oi—czIt T Mcorda _________
ta pl. Tsqi ________
Sa pl. Loq—I S •st (L & 7o C—l) ________
SDG C v.r Shast ________
30 • Miac.lla.ncaiaa Sb.tppix q/R.csi ing R.c xda
(iist all. Lndi’rid a.L records)
.l.ph ns LØqs ____ ____ _______
33. I t.r al Lab ft pL. T:s s.r Pacords ard ackthg Sb..ts
(d.scribs or list)
32. Iz tarnal 0riqi a.l Ssmpi. Preps.ratLo ar4 A a.l.3sia Records
(d.scri s or list)
Prsp&ration records ___________________________________ ____ ____ _____ _______
.nalysis records ______________________________________ ____ ____ _____ _______
Description __________________________________________ ____ ____ _____ _______
33. Other Records (describ, or list)
34. “.ntag
Co pl.t.d byt __________________________ _______________________________ ________
( ..P Lab) (Siç1at xs) (P:i t.d 2 a ./Titls) (Data)
1 ud.Lt.d byt ________________________ _____________________________ ________
( 12 k) (Siq &t re) (Printed Xa ./TLt s) (Data)
7 M 4 DC-2-.2
EPA Regional CSF Coz ’ ” Atza±in t 1
Evid Aiali& Page 2 of 2
-------
Attacb ent IIIB
Laboratory—Completed Organic and Inorgan .c DC-2 Forms
-------
Attach ent IIIC
Laboratory and Ccfltractor-Ccmpleted
Orqanic and Inorganic DC-2 Forms
-------
•
8v Da.ic . Au -r
- -. S G Z 1 ( )
i IrP S,ESh1 fl 4Fit?b %. -
___
1 ’ Wi4 -uDa . o ‘ v - - • ____
__ - .:
1 j s ____ ____ •-•
s*ib1a. ( s w .& - 1, £ tI . 7 2 Z)
fl (T DC4 ) ( o t ‘ sr ) ___
I C31 iY 1 ____ _____
? re.ffic —. it ____ ____ ,
c1zti1.i _ Dtta ____ ____ , - ________
a. QC S” ’7 /
Sux cqat. Ps c t 2acov y S axy ( 7w 1 ___ 9 V ______
xl/xso P -4t• ‘ -7 ( T X VC&) 10 ___ / ______
Zat cd I” S ary (7 ZY V ) ___ ____ •1
aDA .SS C L &t1 7fl (7 V V ) n V ______
b. £ ‘t ls ata ___ /
. Zanits - ( T X
Thntativs .y dant i.ad G-.4 . (7o X T ) ____ _______
.acc sw cr.ad t.ota. Lc c r at oqrsma (MC) gcr
icr •ac asas
*ay .psccra aDA of b4ckd-s trzcr /
we . psLza of tzrq.t Lds i. L.d _____ ________
(ass spectra of LU r. rt4 TC1 it tsr.. .at
.Lbruy a e
c.. St.aDAard.s at& (311 1 zt a)
aLt(•’ t &4 4,cl ( T T / ç j(3 V /
Cz aDA Q *s ta for .11 St&DAarda , c 4 1 ( iZ “
C ct4 i q C rv 4 n (7o T i : ) 3 O - ‘ P
Cs and Q u4 *apozta for tU t O V ______
Intszna.L StII!1 4 1rd Jx.a S axy (? I I .(, / _______
4. av Q 52a
Zn i1 2c9 /
31.1 na _ ta 2-to 22 O _______
atriz Spike Data 2.2 -) ________
Xatriz Spike D pLLcata Dita ___ ______
it (v 1ptil DIta -
a. QC S exy
S 4ats Pt .ant Iaco .xy (y gyj Z4 21 O ‘ vl _
s/xsD S”- ry (7am Z j I ___ ____ ______
st od hank S” ’ ty (7cz* IT IV ) L I t “ -f ‘ ‘
and aus Ca1ibra th , ( 7 V IV) ____ _____ ( 1
-------
‘ : : ‘: ‘• - -‘ -ORG XIC. c LE! ‘EDG ZIZ (C ) £l1 .
zz .7 - , -
aoJA ‘ T ;‘ ( 7ffr— — -
—. . - .. ‘ . 4 -. . . ____
S “ — •Na
o 4. !D . -
• .1 — .. • • - - ‘• — -• - - - ---& . — • —
AU. 4 tZ Ga.LLT*r £ t a UpLSCa £ ____
osath1 . i P
P3
—
1. Th- -.. tCrr b t (7 DC4) (Do t _______
2. ff C i i . Fa .ti
2. ? fLcP-w .t ______
4. Yplatils.Data _______
a. QC S axy
£ a .c qata P. caat Racc?sxy *mxy (7 U _______
CStXZD Dupticata S ’- ’7 (7ø U ________
Xst o4 E91 t a . y (7 ZY &) ________
? ‘ q . 4 (a z. Ca.librattaii (7o V ) ______
b. Zi 1 ata ____ ____ _____ _______
. aault* — (T0 ____ _______
antatiwsiy Id$ ? t iId C— y (7 —TIC) ____ _______
Racofl*tr Ctad tot&L i c x atogras (22C) Lar a
. pL .
7cr sseh .aapla$
Raw .p.ct* a 4 c backq d...ubtractad
we ap.ct* ei t*xqst c da LA. 4 4
Xaaa spectra of a U reported TICa wits t x.e beat
U Z&r7
c. Staz &rd.s at& (RU I ztr .a)
IAit ’-I it f a t n ata (7 V i )
R.tCz ttd Q an M ts for aU. Sta 4arda ________
c=i=izq C it r*tio (7s VU ________
RICa azd Quan Raporta for au. Sta dixda ________
Iztar a Sta d&d irsa S axy (T VIUa ) ________
d. ZawQCD4&
m ___
$ta ________
X*triz Spike ata ____
Xat Spike Duplicate Data ____
S. ii ,1ati1ea Va
a. QC S=mXT
g gata P i t acavszy 1 ax] (?o U IV)
j fltj St 17 (7 Ui IV)
Xt od Ili k (7o iT IV) —
ar 1!l q a 4 X ii i CalLb. attha ( Tom V IV)
-------
- - . ._..—‘.‘--‘.. . _ Z :- ,
oR’ ’ r çp tS C. i 4 Cs!) Ci ) 1:
-= -
* ?U .as ata ( c u )
b. Ca a . ___
3az Lts ( 7 I XV)
?s zttiiLy Zda t .Ltad a ( Tu I
t aj L c r azo na (UC g= —
7 sacs 1a,
av sp.c s 4 b-* i
. ps ta c . ________
Xasa s m it zp ci s b. t L r xy w
GPC (U CC cai-
C .. £ti 4.iz aa (Ai2. aat )
I .tPtaj. f i n ata ( Z TI XV)
! TCI L 4 Qua .ap rta £ &U. a — t a
azi 4 i tnq e21 1 * 4i ( 7 VII XV)
Cz 4 Q’Qa Japcxu g £2.2. s ’ 4 ’ s
“ trna1 £t3 dad Aria *‘-y ( Tc ‘ Whiz X V )
I tar a .L Ztla4jd Aa* * mry v c XV)
4• 7d QC
Xa ri Spurn M
-tr .x Sptka D zp2i ats Mt&
a.
Soqata Putt ac ,s y ( 7o P.a )
1UI3 ptfrna a axy ( l u . . z ) sat )
Zitbod 21a k 1 uy (7 17
&j 3
- - -
‘-‘
/
L Z
gj
b. z 1a MU çj 5
2U J.tZ Vtflie £ <I t$ Mta
(7 P ) . S -.
( -,
ft i.,A OC co*
GC T .gtaPthn rs cr data ays p aM
c’ 4 m1.x* ;1 *
wzt a s
W s a tr c (j avajja
7 psati 4aa/p c1 iL s4 by pt
cf raw s a aed c3pLaa e
• a c tazqst C 4S (c 1a. ata a a )
V
I-
•1
V
___ V
L/57 q.o
‘ I ‘ ire’
4 ff
£,P ’ P0
5 T
V
- -
V
-/
=
V
V
‘I-
X- - 44
-------
;.? : ?.ORGA21IC LE DG .7 Z - CS?) .z Rz (C r4)C -
— — — ‘ . — — . — — — ._..: — ... . .aa ‘- -w’ ‘ — —— —
- - . - ___
. t2 M GJmr- P P FI4 -
m;*t —
6. Puttcid.a ( td)
d. 7aw QC 4tL
1p- 1 at ____ ____ _______
Matrix Zpika Data ____ ____ _______
J(Ltrix Spik p Lcata Lt& ___ __ ____
iqir’ ’ pi za i Lad IysLa ccpiaa c
pr.pizattCfl tad -. yt .a 1oqb k pmqss ____ ____ ______
I tar &L ii 1i Lad $ipL SXtX&Ct tza air ‘
c itad ’ r1c 3fl1S ____ ____ ____ _______
s .. iaq ueor4a ____ ____ _____
1.1 i ztr .nt ixcL 4 (i strip cb.arta £r
.cr..a.L q tctLvitisu (da. ib. cx 3.Lat)
a. m .ta
A1r L1 (1G. 0 g ab.t ta j _ ) ____ ____ _____ _______
a 4 i _ ogu. at 4y . da — no. rc çy e4 ____ ____ _____ _______
Zupi.. a $ ____ ____ _____ _______
S 1a_£oqi Zn 1 s.t (Lab a ) ____ ____ _____ _______
C v Z S St _ _ __ ___
KLac.11afl$ $ 1 ippt qI aCSLI D4 ? s -c .4a
(d.crtbe Li lt )
tJt ’ __ ___ ___ _____
. y t.r i.1 Lab Si cle Tr* *fsr ec* d* *a (
c. Stz. 4Lrda C t
psstiid.a t ta St*adi.rda S axy
(70 V IX. PIt 1.)
P.stieidas lt..ttaticn
(7 Nit—2)
Ps.tieid./P StiM&rdl * AX7 ( 7Gm . Psit )
p.r i w ./p :dsctW.c*ti ( 7 X.
StLadazd chx qrama Lad data ,ywt i t
sJ.i. ,taada.rda
Tar ps i1.m/ l c ±i .’4 by QC1 U. capi.a c .
.p.ctra far ata. dirda .d
b IL
ls-
o L
( D C
7..
—
c, /
c —
—
C:’
E
—
_ 7I
c.-r - _
—
___ ___ a —
__ __ —
) c at.
7
qh.Lj
..—
—
-,. p
1
, ‘
7I
‘.—
-,- 2.
a.—
-i-,’.a
-)7Y
•
—,
— —
— — —
—
-------
- ORGIIiIC cCXPL :S 7ILZ ( 7 V iTcR! Co
ao i4_ s JO A30 --L .?. ØJ —
___ —
.10.
u. c.. 1 at1s
_ ‘-7
c p1.t.4 t __________________ I UU J . !
( 2 L&b) ,J (Pr .nt.d 1I I?LtLa) (Data)
Iwlitid byt ____________ 1’ I /
m) ‘ (Pr1. Ia Fa # t.La )
AJu 2L
EPA Ra p ii
-------
.-...
! OR IC C LKT SDG 7 Z 4 CS!) - I V IT ZT C j )
• , , - 4/. ’.’ 44 . - . i.
—= t 3
S. S iva1&ti1as ata (t4)
b. ZapL. Data
T . Zaa ts ( T SV)
Iflt*ti?.1y Zd ti L.4 ( TOm I SV—TC)
R.constr ct total. ion ch.r atoqrza. (JX) for
For •sc
zv sp.ctza a d b*ckqr d—f .btractad Wa
sp.ctra og r ________
x i i i .psc xa of ?1C5 vith best ii .tuy .sv’. .. _______
CPC c x at z a (if GPC psx ctam4) ________
c. Standa.rda Cita (All. I .zW nta)
I iti& c .atia Cata (7c V I SV)
RXCZ a d Q aL apoxu for all sta . daxda
cotti inq C’libraticn ( toxa VI SV)
XICS i d Q in aporr.a i c r .1.1. ara dax a
I ntar=a.L Stii 1ard Area S””iry (7o vIL’- IV )
ntsznaL St 4 4rd rea S ’j 7c V IT)
d. QC ata
—
31 ata
X.atrii Spike ata
Matrix Spike D pLicat. at&
a. QC S aX7
Suxr qata Pacaat Zacc sry *aXy (Tare X I Peat) _______
Ms/)cs D pLtczt . 1”’7 ( Tore U Feat) ________
Xsthod I1 S azy (Tore XV Peat) _______
a. Ss.pl* V4 ____
. Xea 1ta — Orv ’ Analysis eats sa.at
(Tare I Psat )
r st (Primary 1 t )
r atcqr i second GC eo& confirsti
GC t.qrstLa* report or data, syst rinto t aM
c’tb-rst plots ________
Xaal. work absets
UT t acs fr GFC (if aTtilibi.) _______
7cr pssticidia/PC51 confiz d by GCI’XI. copies
of raw spictra aM capt.. of backqro d-.tctad We
spoct. a of t*rqst c po nda (samplss st ’1arda )
-------
-- GRGA2 IC cC a LX ..SDG .‘(C YLzcLORZ Ccntd)-
-
6. Psgticidas (cc t4)
c. Zt& darts Data
Ps.ttcjdas Za.t a j n 1t& d&rda S 1Lr7
(7o VZ . P.st—a)
Pastifidis t tW!I- .I t2fl 5
(7o VT .Z . PsIt.2) ______
P.st4 4 r4./P 1ta daxda SI axy (To , Pest ) ______
Pesticida/P Id a Zica t (7o Z, Pelt ) _____
S ’ in 4 &rd chr atoqrzaa aM data syvts. i t
icr iii. ata d&rda
7cr sstic.14sa/P a ca i .4 by GC/ U, ccpl.ss c i
ap.cxa icr st& dazd.s ad
d. Raw QC Data
31a .k Data
Xatrix Spike Data
Matrix Spike D zpUcats at.a
7. - Xiseet1a &x i Data
Oriq ’ .I ptpsxatic lad ‘ ysis icra or pis. ci
ep&a t n mad 41ysLI L ock pages
ntsr a.3. sa pi. and sma pi. sztra.ct tzanaisr .tn-oi..
c Itady
r. ds __
1l1 Lnstrsnt tb t . i 4”7 strip c arta ir
. s.nixq etiwittss (da ib. or ilat) ________
S. 1 hjv L /Rc.Lyi n D .e! .IAt1
Mzbifls (1 o. ci ab.tp.-is
in—oi— zstcdy Raooxdz
Zaapia mqs
Zasp2.. Lcq4n Sh.st (Lab LD 3 _______
C az Sbmst
1(isesilan.ou.s Sktppthq/Rac.irinq Records
(d.scribs or list)
. Tctsxn l Lth Sample azd fleata
(d.scr . or lilt)
I
-------
- ORGANIC CQ LZU S T 1 .( 7J ‘I ___
. - - •.•. — - ••. . % —‘,. — -
T, 0 __
7 4 - -
.O. Qt .r ! r z (deicr L1.st)
pLst.d byi 1th’V ‘)Lt k cMT14 I
(2 L ) (Pr4. tad J4 /Tit1a)
i t .d byt \Ait’ $1) _______________ _____
( ) J (SLnar. .r.) ( ?rt 1 F /itJ. )
EPA P9 n 1 CP C4’ p . — 2 4 .‘f
-------
r ’ OTOCop’
- -.•. I OR ANIC CO LZ’Z SDG 7 1 11 CS7) INV RT . .. -
• • —. •. _ — • — . - . f% •. . . s. 1 .. .__..
.. ——-—_ — — — .. — i. •
tty ____ __o ._ o __________
•- --‘- . ;_ __ •_. . ._,. Ar,>, .._,... _..
(CT . 5 * 2f -/ r (ef o -• -
LL . c snts ai vs.rsa £n tAl C pL•t. £bG 1 La tus be e: .qi.n& , oc tg WA*CS
possible. (P27 1 : a: z : ; szc i
. flYs t y th.st (?o DC.4) ( o ct 11’1aI Pur )
3. vsr Page
3. Inorqa ic A a1ysLs ta Sheet (7 )
1. ThitLa1 a . d C. tiinq CalLbratic V i ic atj (Taza fl,
7ax 1) __
1. L Sta.ndm.d f z M &nd (7or X:. Pa.r 2) 2 . -
4. (7cr 111) _ 47 _ —
7. Intar a:snc. eck S*=pls (?c XV) ____ .
Spi a Sa pl. *seavezy (7o V, Put ) 4Q ___ ____ _______
. Post Lqest SpL a Sa pls acovary (7a V, Part 2)) ( c ( o — _______
10. iiplicatea (7o V I) : 7e) — 7 c _ _ _
4 !ab ratcty C Atrol Sa pls (7am V ) — j — ________
-_. St&nds.zd ?4dLtic *as tta (7o VZZ) £ j j j _ •_____ ________
1.3.- CPS.rja.i. Dthatia (Toz ) Iol .. ____ ______
14. I .itru .nt .t.cti tlita , C *ztsrLy (7o Z) RQ _______
3$ I tsr.la snt 7 _____
Part i) % 3( jj
14. I Int.r.l .nt C rrectic tactcrs, Ann s33 7 (7or
Paxt2) L’4 J$ U
17. LL .er ?a q. Q arteriy (7oz ) S i — —
1$. Pr.paratic Log (7o X I3 ii t 1W — — ________
11. 1 a1y.Ls P Log (Tom J l 1 i __ •
20. : av vats . t L 14 “ •
1. flae LA Zaw vats 14 ____ —
3. 7uz ace U tv 21L 2.th
13. X.rc ry av vats 2 .2 a a:
21. Cyanide Zav vats 1:1: : 2. 4O —
5. Percent SoiLd.a C* .tc latjc g 2 Sô
EPA Rqicnal CF Cc rn
Evk .AudU G ’ P xs oil
-------
C J ZhI Ix ’
T2 q L : :
r p rs:t n zs 1 . .Ja
M. Lyet. *a t ‘ 111 —
‘.M)
33. Othir Paco da (dsu tbs _ - - 3Lit)
34. c.— u$
Tpl byi
(2 Lab)
itad byi
c i
i/lA 4 4 1
5c n ak C wM
I - .
(Pr2. 4 H / t i-s)
1u ’ )#?Lci
,4tjaI
7 kkI
( 1
Til r
2 . L q. (Cyi.ni4a .Ly)
27. Lqsst .c Løq.
22. ziiLc Ja ’t
2 . X71 Sb.tpi q/Pa sLvi q ‘ ta
1ti {!1 . (14. af sb.t a P
‘i1n—i oiztXy Mo a rtø 4
& a aqs
ZazpL. Laq .Z Zb .t (Lab & T ©C4)
1C C tb..t
3 . XiicsLl&naoua Zbipi q/ .eai.i q Zae da
yj e, 1
a1ap a Løqi
is: zs ___
2. t ___ ____
___ 2. 1 ____
3t7
31. 4tsx a L Lab Zwp3.. z a sr lacorti .. 4 ?zzcki q 2bssta
(ds.ibs
32. Z tsz a L Cri;i ud $.=pLs Pr p&ra 4- ’ &M ____
(d.a s ar L .gt)
-------
o Toc Ev oe c )Drr
• -: INORGANIC C ’ ’LZ X SCG 7IL (CS?) I VIX y 5 •• . - -
• . d.. . i L •1 _, •
L OR - f2 —
•. •••.. #—. • • •- -• •;; ;__ .
. . t22 ’1 s os. o . i— -
•* SS( -• • — .• . ••i.. .... — •, — —
-
.LLL øocu snta d• vszs £ tJ . c pL•ta S G J.2.a £ aat Or qtn* w aze
• i.. ( 27I . ( L 1I? 3, SZ 2( :: a JC SZ
—
. cT. tGry th..t (7oa DC—2) (Do cat n b..r) _____ ________
. avsr Paq ____ ____ ____
. I org cic Analyit. Data Sha.t (7 I) ____ ____ _____ ________
4. IflitL Ii &nd C ti Lnq C.&1LbratL VszUieatinn (70r* 1.
Part 1) ____ ____
3. DI. Sta1 da.rd f JJ. &r d (?or ZI, Part 2) ____ ________
. J1 1 a (7Cm Lt3 ____
7. IAta: e:scc* ek Sap s (Yor IV) ____
1. Spika Sa=X. aecv*xy (Tor 7, Part 1) ____ _____
. Pare DLqeat SpLka Capts acar.ry (Tcr v, 2)) ____ ____ ____ _______
DupU.catas (7ar VZ) ____ ____
ti.boratary Cact t Si pLs (Ta V1) ____ ____ _____
.2. Standard 34dLttcn aiulti (Te ____ ____ _____ ________
3. Z.riai. DL1uti z (Term Z) ____ ____ _____
.4. InSt S t Dst.eLe .Lmits, Quartsz .y (7o Z) ____ ____ _____ ________
X Tntsra a snt C rcticn 71etars, Acnca.L2.y (Tarm xx.
Part i) j . “
IfltIra1S s t Ca aCtiCU 7actazz, A a11y (7 r xx.
Part 2) ____ ____ ____
7. LLc.a.r Pa.nqi Q artsr1y (Term xx ___ ____ ____ _______
Z. Pr.p&ratto Log (Term X ) ____ ____ _____ ________
3. *naly.ii Log (Term xxYJ ____ ____ _____ ________
: *av Data
: . fla U Zaw Data
. 7urtaca U M v Data
:3. X.rc zy *1w Data
:i. C a.nids Paw Data
‘i-, Psrc.nt Solids Ca.3c latioca
.1 ( V (eq..q.,1.i .
-------
Th ORG NIC S !!J 7II1J Z d) - - -
s .1Z3 ” T ’ 10. ____ S __________ , ç;4...
—
____ L1.Z ! T I
35. DLzttlliti L qs (esi t ’i .Ly)
27. i;sitic L qa
28. &.t ic M rt
2 . zPa zbL pLr q/7..c.LvL q D ’ ta
1SzbLfl ( . cf shLiut* ____ ____ _______
ti.n—of—C.iIt y *ao ø.I _____ _____ _________
$i pLs Taqs
SwpL. L q.-Za 5 ..t (L1.b & 7 C.’4.) ____ ____ ________
s c v*r s .st ____ _____ _________
30. Xiac.U& .cua £hippi g/Rac.i?i q Me da
(li*t all i iYLdual riccrda)
i,tsp aa Loqs
i. tsXT a1 a.b 5*p1. i sftr a ts a. 4 ?ic*1nq s ta
(d.acrib. cr liat)
_______________________________________________________________ a
32. tar al. ciqi -’ S pls P*paratt & d “slyaLi *a dz
(d.seribs ar List)
pr.p&r*tic rtc .I ___________________________________ ____ ____ _____ _______
ua.Lysis ___________________________________ ____ ____ _____ _______
33. Othsz ae rdi (d.scri S or list)
34 rr
p e - I bW a L.
ccplst.d byt .) ( WA I” \ J ñrs t.- Thi c - . -- 1’ i ‘ I
( .P Lab) ttLc &t S) (Printed aasITLtL) (a )
1 ditad byt _______ \ t ç . oi c ____
Li (sLr aLu:s) . ts4 JI S/TLt $)
EPA R ii P Crijip .a i . . .
•_,
-------
ATTACHMENT IV
EXAMPLE INORGANIC TABULATED SUMMARY FORMS
-------
U.S. EPA — CLP
Lab Name:
1
INORGANIC ANALYSIS DATA SHEET
Contract:
EPA SAMPLE NO.
Lab Code:
Case No.:
SAS No.:
SDG No.:
Matrix (soil/water): ______ Lab Sample ID:
Level (low/med): Date Received:
% Solids:
Concentration Units (ug/L or mg/kg dry weight): _____
Color After:
Clarity After:
Artifacts:
Comments:
I
I
I
I
I
I
CAS No.
N
CI Q
_I ______________
_I _________________
_I _______________
—I _________________
I_I _______________
—I ___________________
74 29—90—5
7440—36—0
7440—38—2
744 0—3 9—3
7440—41—7
744 0—4 3—9
744 0—7 0—2
7440—47—3
744 0—48—4
744 0—50—8
7439—89—6
7439—92—1
7439—95—4
7439—96—5
7439—97—6
I7440—02—0
17440—09—7
I7782—49—2
7440—22—4
17440—23—5
7440—28—0
7440—62—2
7440—66—6
I Arialyte Concentration’
Aluminum_I
Antimony_
Arsenic
Barium
Beryl 1 ium
Cadmium
Calcium
Chromium
Cobalt
Copper_i
Iron I
Lead_____
Magnesium
Manganese
Mercury_
Nickel
Potassium I
Seleniu m_
Silver
Sodium
mall ium_
Vanadium_
Zinc_____
Cyanide_
Color Before:
_I _______________
_I ______________
_______________ I_I
_____________ I_I
_______________ I_I
— Texture:
Clarity Before:
FORM I — IN
ILMO2 . 0
-------
£.ra’% —
2A
INITIAL AND CONTINUING CALIBRATION VERIFICATION
Lab Name:
Contract:
Lab Code: ______
Case No.:
LAS No.:
SDG No.:
Initial Calibration Source:
Continuing Calibration Source:
Concentration Units: ug,’L
I I
I Initial Calibration i
IAnalYte True Found %R(l) I True
I _____ I ____ _____ ___ I ____
IAlum nu m_I ________I _________ I ______ I ________
IAntimony_I _______I ________I _____I _______
IArsenic_I _______I ________I I _______
IBarium_I _______I ________I I _______
IBerylliumI _______ I I _____ I
ICadmium_I _______I ________ I _____ I _______
ICa lcium_I _______ I ________I _____ I _______
‘Chromiu m_I _______I ________I _____I _______
.Cobalt_I _______ I ________I _____ I _______
ICopper_I _______I ________I _____I _______
l lron_____ I _______ I ________ _____ I _______
ILead____ I I I I ______
IMag nesiu mi _______ I ________ I _____ I _______
Manganese I I I _____I _______
mercury_I I ________I I _______
INickel_I I ________ I _____I _______
IPotasslumI I ________ I _____I _______
Iselenium_l _______I ________I_____ _______
ISilver_I_______ I I _____ _______
lSodium_l I ________ I I
tThallium_I_______ I I_____ I I
IVanadiumI I I I I
IZinc I _______ I ________ I I
ICyanide_I ______I_______ _____I I
I ______ I ____ I _____ I ___ I ____
I I
Continuing Calibration II
Found %R(l) Found %R(1) I i M
___________________ ____________ ___________________ I I_I
____________________ _____________ I _____________________ I Il_I
____________________ _____________ I _____________________ I I I_I
____________________ _____________ I _____________________ I Il_I
_____________ I I I I_I
_____________ I _____________________ I I I_......I
____________________ I _____________ I I Il_I
___________________ I I ___________________ I ____________ I I_I
___________________ I I ___________________ I ____________ Il_I
_________________ I I __________________ I ___________ I I_I
___________ I I I _______ II.
_________________ I I I I I.
___________________ I ____________ I ___________________ I ____________ I
___________________ I ____________ I ___________________ I ____________ I I_
___________________ I ____________ I ___________________ I ____________ I I_
___________________ I ____________ I ___________________ I ____________ I I_
_________________ I ___________ I __________________ I ___________ I I_
_________________ I ___________ I __________________ I ___________ I
________________ I __________ I ________________ I __________ I I_’
_________________ I ___________ I __________________ I ___________ I I_
I ___________ I __________________ I ___________ I I_
___________________ I ____________ I I ____________ I I._.......
___________________ I I I ____________ I I_I
________________ I __________ I _________________ I ___________ Il_I
_________________ I ___________ I __________________ I ___________ Il_I
_______________ I _________ I ________________ I __________ I I_
(1) Control Limits: Mercury 80—120; Other Metals 90—110; Cyanide 85—115
TORN II (PART 1) - IN
ILMO2.O
____________________________________________ I ____________________________
_____________________________________ I _______________________
_____________________________________ I _______________________
I ___
-------
U.S. EPA — CLP
2B
CRDL STANDARD FOR AA AND IC?
Lab Name:
Contract:
Lab Code:
Case No.:
SAS No.:
SDG No.:
AA CRDL Standard Source:
ICP RDL Standard Source:
Concentration Units: ug,’L
I I
I I CRDL Standard for A.A
I I
lAnalyte j True Found
I ______ I ____ ______ ___
I Aluminum! _______ __________ ______
I Antimony_I_______ __________ _____
I Arsenic _______ __________ ______
Barium _______ _________ _____
Beryl1ium __________ _____
I Cadmium! _______ _________ _____
1 Calcium I _______ __________ ______
IChromium_I ______I _________ _____
I Cobalt _______ __________ ______
1 Copper_i _______ _________ _____
Iron_____ _______ _________
Lead_____ _______I __________I ______
iMagnesium I _______I __________ I _____
lXanganese _______I _________
INercury_I I________
lNickel_I I _________
IPotassiu mi I _________
ISelenium_I _______I _________ I
ISilver__j I
ISodium_I I _________
IThallium_I I __________
lVanadium_I I _________
IZinc____ ______ I _________
I _____ I ____ I ______
CRDL Standard for ICP I
Initial Final I
Found Found %R I
I _____ I ______ I ___ I ______ I ___ I
_____ I ______ I ___ I ______ I ___ I
_____ I ______ I I ______ I ___ I
_____ I I ___ I ______ ___ I
__ ___ __ I ___ __
I ____ I ____ ___ _____ ___
I _____ I ______ I ___ ______ I ___
I _____ I ______ I ___ ______ ___
I _____ I ______ I ___ I ______ ___
I ____ I _____ I ___ ______ I ___ I
I ____ I _____ ___ _____ I ___
I _____ I ______ ___ ______ I ___ I
I _____ I ______ ___ I ______ I ___ I
I _________________ I _____________________ I_ I _____________________ I ____________ I
I ____ I _____ I ___ I ______ I ___ I
____ I _____ I ___ I ______ I ___
____ I _____ I ___ I ______ I ___
I I I ___ I ______ I I
_________________ I _____________________ I_ I I ____________ I
_____ ______ I ___ I I ___ I
_____ I ______ I ___ I ______ I ___ I
_____ I ______ I ___ I ______ I ___ I
_____ I ______ I ___ I ______ I ___ I
FORM II (PART 2) — IN
ILMO2 .0
True
____________________________________________ I _________________________
__________________________________________________________________ I _____________________________________
_____________________________________________________ I ______________________________
-------
U.S. EPA - CL?
3
BLANKS
Lab Name:
Lab Code:
Case No.:
Contract:
SAS No.: _____
SDG No.:
Preparation Blank Matrix (soil/water): ______
Preparation Blank Concentration Units (ug/L or mg/kg): _____
I Initial
I Calib.
Blank
lAnalyte (ug/L) C
IAlu inU _ _________i=i
IAntimony_ _________I_I
IArzenic........I _________ I_I
IBar1u m_I _________ LI
IBerYll1 _________
I Cad. iim_
I Calcium_
I Chromium_ __________
Coba1t_ _________
Copper_i_________
Iron_____ _________
Lead_____ __________
Macnes iu __________
Manganese I __________
I Mer ry I __________
NicJ el_ _________
Potassium __________
ISeleni1 _I _________
I Silver_I __________
ISodi _I_________
I Thallium_I_________
IVanadiu _ _________
I Zinc_____ _________
I Cyan .de_ __________
Prepa-
ration
Blank
I I
I CI
_I
I I —
I _I
I _I
I _I
I I_I
I —I
I
I
....I
—
I
=1
I
I
I
I
I
—
I I_I
I_I I — I
I_I I
Continuing
Calibraticn
I
Blank
1 C
(ug/L)
2 C 3
I
Cj
I I
I I
IMI
I—I
I_I
I_I
I_I
I — —
— I_I
I_I — I_I
I .._I — I_I
I I_.. — I_I
— I_I
— — I_I
—‘ I_I
— I_ I_I
— — I_I
I—
— I_I
— I_ I_I
I_ — I_I
I I_I —.
— I_I I_I —
I — I — I_I —
— I — I_I I —
I_ I_I I_
— I_I I_I
I_I I_I I_I
I_I I_I I_I
I_ I_I
I_I I_I I_I I_I
I_I I_I I_I I_I
I_I I_I I_I I_I
I
I
I
FORI( III - IN
II . C
-------
U.S. EPA - CL?
4
IC? INTERFERENCE
CHECK SAMPLE
Lab Name:
Lab Code:
IC? ID Number:
Case No.:
Contract: ___________
LAS No.:
ICS Source:
SDG No.:
Concentration Units: ug/L
True
Sal.
AD
Aluminu I _I________
Antimony! _____I________
Arsenjcf ______ I________
Barium ______
Beryllium! ______
Cadmium!_____ ________
Calcium! ______ _________
Chromium!______ ________
Cobalt! ______ ________
Copper ______ I _________
Iron_____
Lead_____ ______
Magi esium ______ I ________
Manganese ______ _________
Mercury!_____ _______
Nickel ______
Potassium ______
Selenium — I _________
Silver ______
Sodium _I___
Thallium ______I _________
Vanadium —
Zinc I_ _L_ —
Initial Found
Sal. Sol.
A AS
____ ____ I __
__________________ I _________________ I _
_____ I _____ I ___
_____ I _____ ___
_____ I _____ I ___
Final Found I
Sol. Sol. I
A AD %R I
FORM IV - IN
ILMC2 .0
lAnalyte I
Sal.
A
II
I I
II
___I L __I___
______ I ______ ___ I ______ I ______ I ____
_____ I _____ ___ I _____ _____ I ___
_____ I ___ I _____ _____ ___
______ I ______ ___ I ______ I ______ I ____
_____ I _____ ___ _____ I _____ ___
_____ I _____ ___ _____ I _____ I ___
_____ I _____ ___ _____ I _____ I ___
__________________ I _________________ ___________ ____ I __________________ I ___________
_____ I _____ ___ _____ _____ I ___
_____ I _____ ___ _____ _____ I ___
__I__ _ -I__ __
_____ I ____
_____ ___ I
_____ I ___ I
_____ I I
______ I ____ I
_____ I ___ I
_____ I ___ I
_____ I ___ I
-------
U.S. EPA — CL?
5A EPA SANPLE NO.
SPIKE SP14PLE RECOVER?
_____ SDG No.:
Level (low/med):
Concentration Units (ug/L or mg/kg dry weight): —
1 I
I control I
I Limit I Spiked Sample
I %R I Result (SSR)
I _____ ____ I _________
lAlunum.... _______I. I _________
Antimony — I .
Arsenic_ I.
Barium_I _______I. _______
Beryllium I
Cad.mium_ _______
ICalcium_
ICliromium_I
Cobalt ________
Copper_ ________
lIron I ______I. _______
Lead_____ _______
MagneS1Ufl _______I
MangafleSe _______I
Mercury_I
Nickel_ ._I
IPot ss iumI _______ I
Selenium_I
Silver_I
Sodium_I I
Thallium_I
jVanadium_I _______ I
IZinc I I
Icyanide_I _______
I _____ I ____
Comments:
Lab Name: ______
Lab Code: —
Matrix (soil/water)
% Solids for sample:
_______ Contract: __________
case No.: ____ SAS No.: _____
lAnalYte
CI
Sample
Result (SR)
Q
N
I I
I I
I Spike I
CI Added (SA)I %R
_I _________________________ I ___________________
I_I _______________________ I _________________
I_I _____________________
_________________________ I ___________________ I
C l.
I I
I_I
I_I
(—I
I I
. 1
LL_J
I_I _
I_I_I
I_I_I
I_I_I
,I _I _I
.1 .....t_l
. 1 _I_
•I_I —
I I
— I
—I.
—I ,
I_I
I I
I I
I—I
I __________________ I_I_
FORN V (PART 1) - 11
IL .0
-------
U.S. EPA - CLP
Lab Name:
5B
POST DIGEST SPII SAMPLE RECOVERY
EPA SAMPLE NO.
I I
I I
‘I I
Lab Code:
Case No.:
SAS No.:
SDG No.:
Matrix (soil/water): ______
Concentration Units: ug/L
Level (low/med): ______
I Analyte
IAlu ninum_l.
I Antimony_I.
IArsenic_l
I Barium_I
I Beryllium
I Cadmium I
I Calcium I
I Chromium I
I Cobalt_i
I Copper_I
Iron____
I Lead_____
Magnesium
Manganese
Merc’.lry_
INickel_
I Potassium
Selenium
Silver
S odium
Thallium_
Vanadium
Zinc_____
ICyanide_I
C
—I
I_I
I—
I—
I—
—I
_I
I_I
. 1_I
. 1_I
. 1_I
_I
I_I
Comments:
Contract:
I I
Control I
I Limit I Spiked Sample
I %R I Result (SSR)
I I
Sample
Result (SR)
_________________________________ _I _________________________
________________________________________ —I ______________________________
__________________ _________________________________________ —I ____________________________________
__________________ _________________________________________ —I ____________________________________
_________________ _____________________________________ I_I _________________________________
_I I I I
I I I
Spike I I I
C Added (SA)I %R IQI N I
________________________ ___________________ I_I_I
I ________________________ ___________________ I_I_I
I I _________________________ ___________________ I_I_I
. 1 I_I_I
I I _____________________ I ________________ I_I_I
I _____________________ I ________________
_________________________ I ___________________ I_I_I
I_I _____________________ ________________ I_I_I
I_I ___________________ _______________ I_I_I
I_I _____________________ ________________ I_I
l_I _______________________ _________________ I_ —
I_I _______________________ . _________________ _ —
I....I _______________________ I _________________ _ —
_______________________ I _________________ _ —
I_I _______________________ I _________________ _ —
I_I _________________________ I ___________________ _ —
I_I _______________________ I _________________ _ —
-I____ ___-I-
— ______________________ _________________ I_I_
— ________________________ I ___________________ _I_
_______________________ _________________ _I_
— _________________________ ___________________ _I_I
FORM V (PART 2) -
ILMO2 .0
-------
U.S. EPA — CLP
EPA 5AMPL NO.
Lab Code:
Case No.:
SAS No.:
SDG No.:
Matrix (soil/water): _______
% Solids for Sample:
Level (low/med): ______
% Solids for Duplicate:
Concentration Units (ug/L or mg/kg dry weight): _____
Control I
lAnalyte I Limit I
_____ I _____ I
Aluminum ________ I
kntimonyl ________ I
Arsenic I ________ I
Barium I ________ I
Beryllium I _________ I
Cadmium 1
Calcium I _________
Chromium I _________
ICobalti ________ I
Copper_ I _________
Iron_____ _________
Lead_____ _________
Magnesium _________
Manganese __________ I
Mercury ________
Nickel _________
Potassium _________
Selenium _________
Silver _________
Sodium _________
Thallium ________
Vanadium ________
Zinc_ - ________ I
Cyanide ________
I ______ I _____
I I
II
Dupl:c..:e (D) C
.
I —
—
I
I
I
I—I
I_
I
,_
I
I_
I
I_
I
. —
I I
I I
Lab Name:
6
DUPLI CATES
Contract:
Sample (S) C
RPD
I
I
I I
I
I_I
I I
I
Q M
_I
_I —
— .
_I _I
— _I
— _I
—.
_I —
—I—I
_I _I
_I _I
_I _I
_I _I
FORM VI - IN
-------
U.S. EPA - CL?
7
LABORATORY CONTROL S? J1PLE
Lab Name: _________________________ Contract:
Lab Code: •Case No.: SAS No.: _____ SDG No.:
Solid LCS Source: _____________
cueous LCS Source:
I I I
I I Aqueous (ug/L) I
lArialyte True Found %R I True
I ______ I ____ _____ ___ I _____ _____ — _____ _____ ___
lAluminum_I _______ I _________ I ______ I ________I ________ I_ ________ _________
IAntimony.j _______I________ I _____ I ________I _______ ________ ________
IArsenic_I _______ I _________ I ______ I ________I ________ C ________
IBarium l ______ I ________ I _____ I _______ I _______ _______ ________
IBery] .liuml ______I ________ I _____ I _______ I _______I _______ ________
ICadmium_I _______ I ________ I _____ I ________ I ________ ________
lCalcium_I ______I ________ I _____ _______ I _______ _______
IChromium_I _______ I________ I _____ I I _______ I ________
ICobalt_I ______ I _______ I _____ I _______ I _______ I
Copper ______I _______ I _____ I _______I —
llron____ ______ I _______ I _____ _______ — _______ ________
ILead_____ ______I_______ I _____ _______ _______ _______ ________
Magnesium _______ ________ _____ ________ ________ ________ ________
I Manganese _______ _________ ______ _________ ________ ________ _________
IMercury_ ______ I_______ _____ _______I _______ _______ ________
INickel_ ______I_______ _____ _______ _______I _______ _______
IPotass iu m ______ ________ _____ _______ _______ _______ ________
ISelenium_ ______ _______ _____ I _______I _______ _______ ________
ISilver_ ______I________ _____ _______ _______ ________
Sodium_ ______ ________ _______ _______ _______ ________
jThalliu m_ _______ I _____ I I ________
IVanadium_ _______ I________ _____ ________I _______ ________
Izinc_____ ______ I ________ _____ ________ I _______ _______ ________
ICyan ide_I I________ _____ _______I_______ _______ ________
I _____ I ____ I _____ ___ I _____ I _____ _____ _____
FORM VII — IN II..M02.O
Solid (mg/kg)
Pound C Limits
_____ I ______ ___ I
I _____ ___
I _____ I ___ I
I I ____ I
I _____ I _____ ___
____________________ I _____________________ _____________
— _____ I _____ I ___
— _____ I ______ I ___
— _____ I _____ ___ I
____________________ I ______________________ _____________ I
— _____ I _____ ___ I
_I __________________ I ____________________ ____________ I
_I ____________________ I _____________________ _____________ I
_I __________________ I ____________________ ____________ I
_I ____________________ I _____________________ _____________ I
_I __________________ I ____________ I
_I ____________________ I _____________ I
_I ____________________ I _____________________ _____________ I
_I __________________ I ____________________ I ____________ I
_I ____________________ I _____________________ I _____________ I
-------
U.S. EPA — CL?
8
STANDARD ADDITION RESULTS
Lab Name:
Contract:
Lab Code:
Case No.:
SAS No.:
SDG No.:
Concentration Units: ug,’L
I I I
I EPA I
ISa p1e I 0 ADD 3. ADD
I No. lAnI ABS
I ________________ I_I___._ — _______________ ____________
I __________________ I_I _____________ I ________________ I _____________
I ________________ I_I I _______________ I ____________
I ________________ _I ____________ I _______________ I ____________
_________________ _____________ I ________________ I _____________
__ _ I_
________________ ____________ I _______________ I ____________
____ ___ I ____ ___
____ I ___ ____ I ___
___ __I___ __
___H __
____________________ I — ______________
__________________ I_I _____________
____________________ I_I ______________
I ________________ _I ____________
I __________________ _I _____________
I ____________________ _I ______________
I __________________ _I _____________
I ____ — ___
I _______________ ___________
I _______________ ___________
I ____ — ___
I ________________________________ _______________________
FORN VIII - IN
3 ADD I Final
CON ABS I Conc. r Q
____________ I _________________ I _______________ _I
_____________ I __________________ ________________ I_..._I
_____________ I __________________ ________________ I_I
_______________ _____________ I __________________ ________________ I_I
_______________ ! __________________ ________________
_______________ _____________ __________________ ________________ I_I
_______________ _____________ ________________ I_I
_______________ _____________ __________________ _________________ I_I
_______________ _____________ __________________ ________________ I_I
_______________ _____________ __________________ ________________ I —
____________________ __________________ i_i
__________________ ________________ I_I
_________________ _______________ I_I
_________________ _______________ I_I
_________________ _______________ I_I
_________________ I _______________ I_I
I ________________ I ______________
________________ I ______________
_______________ I_I
________________ I— .—’
____________________ __________________ I—,
_________________ I _______________ I_I
I I_I
__________________ ________________ I—I
__________________ ________________ I. .—.’
__________________ ________________ I.....’
__________________ I ________________ I_I
__________________ ________________ I—I
______________________ ____________________ I
IL 0
CON ABS
2 ADD
CON ABS
______________________________ I ___________________________________
___ I ____
___ ____ ___ ____ I I ____
___ ____ I ___ I ____ I ___ I ____
___ ____ ___ I ____ ___ ____ I
___ ____ ___ I ____ ___ ____ I
___ ____ ___ I ____ I ___ I ____ I
___ ____ I ___ ____ I ___ I ____ I
____ I ____ I ___ ____ I ___ I _____
___ I ____ I ___ ____ I ___ I _____
___ ____ ___ I ____ I ___ ____
____ ___ I ____ I ___ _____
____ ___ I ____ ___ _____
____ ____ ____ I ____ ____ I _____
___ I ___ I ____ ___ I ____
___ ____ I ___ I ____ ___ I ____
___ I ____ I ___ I ____ ___ I ____
___ I ____ ___ I ____ ___
___ I ____ I ___ I ___ ____
___ I ____ ___ ____ ___ ____
___ I ____ ___ I ____
___ I ____ ___ I ___ I _____
___ I ____ I ___ I ____ I ___ _____
___ I ____ I ___ I ____ I
___ I ____ I ___ I ____ I ___ I ____
___ I ____ I ___ I ____ I ___ I ____
____ I ____ I ___ I ____ I ___ I _____
___ I ____ I ___ I ____ I ___ I _____
-------
U.S. EPA - CLP
9
CP SERIAL DILUTIOUS
_____________ Contract: —
Case No.: SAS No.:
EPA SAMPLE NO.
SDG No.:
Concentration Units: ug,’L
Level (low/med):
Ana lyte
I I
I Alu i.num I
I Ant i ony I
Arsenic_ I
Bariu I
Beryllium
Cadmium
Cal ciu
Chromium
ICobalti
I Copper I
l lron_____ I
ILead____
IMagnesiu I
I }!anganese
I Mercury
I Nickel
I Potassjun I
I Selenjum
I Silver
I Sodiu
IThallium
Vanadju
I Zinc_____
Serial
Dilution
Result (5)
Differ-
ence
C
. 1_._ ___________________
. 1... ___________________
‘I—I
.I—I ___________________
I I ________
I ________________________________
I I ____________
.11 __________________
I _____________
I I _____________
I I _____________
II _____________
II _____________
I
I
I
—.
I
I
..—I
I—
I—
—I
—.I
I
I —
Lab Name:
Lab Code:
atrjx (soil/water): _______
llnitial SamDle
I Result (I)
C
QM
—I—
_I_I
—I—i
—I—I
I_I
—I—I
I_I_I
FORM IX - IN
ILMO2.O
-------
U.S. EPA - CL?
2.0
INSTRZ]NZNT DET CTI0N LI) ITS (QUARTERIX)
Lab Name: _________________________ Contract: _____
Lab Code: Case No.: ____ SAS No.: SDG No.:
IC? I Number: _____________ Date:
flame AA ID Number:
Furnace AA ID Number: _____________
I I I I II
Wave—I
lenqt Back- I DL ( IDL
Analyte I (nm) (ground I (ug/L) ! (ug/L) M
________ ______ I _____ ______ I ______ I
jA1u iinu_m I 200 ! ________
lAntimony_ I 60 ______ —
(Arsenic_ ______ _____ 10 —
(Barium _______ ______ 200 I
jBery].li _______ _____I 5 ______
ICadmium_ ( I______ s I ______ —
(Calcium_f _______ ______ 5000 _______ —
(Chromium_f _______ ______ I 10 _______
ICobalt_ (_______ ______I 50 ______ —
(Copper_I_______ ______I 25 I______
Iron______ ________ _______ ( 100 ________
Lead___ ____ ___I 3! I_I
Magnesiumf _______ ______I 5000 I _______
Manganese _______ ______I 15 I I_I
iMercury_ ( ________ _______ f 0.2 I ________ I_I
Nickel.___ ________ _______ 40 I _______
Potass .um ( _______ ______f 5000 _______ —
Selenium_f _______ ______I 5 _______
Silver I ________ ______I 10 _______ _I
Sodium___ _______ ______ 5000 I _______
Thallium_f _______I ______ 10 I_______ _f
Vanadium_ ( _______I______ 50 I_______
Zinc______ I ________ 1 _______ I 20 ________
I ___________________ I _______________ I _____________ I ______________ ______________ I_I
Comments:
FORM X - IN Ii. wr. 0
-------
U.S. EPA - CLP
hA
I CP INTEREL NT CORRECTION FACTORS (ANNUALLY)
Lab Name: _________________________ Contract __________
Lab Code: Case No.: ____ SAS No.: — SDG No.:
ICP ID Number: ____________ Date:
I I
Wave— I
lençth
lAnalyte (nn)
I Aluminu
Antimony_ _______ __________ __________
I Arsenic_ _______ ___________
I Barium _______ __________ __________
I Beryllju ________
I Cad ju _______ ___________
ICalcium_I I _________ _________ _________
I Chrc ju ______ __________
ICcba lt_I______ _________ _________ _________
opper_j_______ __________ __________ _________
i lron____ I ______ _________ _________
ILe ad I — . ________ ________ ___ ____
IMagnesi .u _I __________ __________ _________
Manganese _______ ___________ ___________
IMerciiry_ ______I
Nickel_ _______I
IPotassiu ______
ISeleniunt_ ______
ISilver I __________ __________ _________
SodiU I _______I __________ __________ _________
IThal lium_I _______I __________ __________ _________
IVanadi =_I ______I __________ __________ _________
12m b I ______ I __________ __________ _________
I _____________________ I ________________ _________________________ ________________________ ______________________
Coents:
Al
Intere].e e.nt Correc jon Factors for:
Ca Fe Mg
— _______ I
I
—
I
—
I
I
—
FORM XI (PART 1) - IN
ILMOZ.O
-------
13.5. EPA - CL?
ICP INTERELZ NT CORRECTION FACTO 5 (A UALLY)
Lab Name: ________________________ Contract: _________
Lab Code: _____ Case No.: ____ SAS No.: SDG No.:
IC? ID Number: ____________ Date:
I I I
I Wave— I
I length
Analyte (nm)
A..lum.Lnum_ I_______
Antimony_ I_______
Arsenic I
Barium_I _______
Beryllium ________
Cadmium_I _______
Calciumf _______ ___________ ___________ __________ __________
C rcmiu m_l _______ ___________ ___________ __________ __________
Cobalt ________ ___________ ___________ __________ ___________
Copper_ _______ ___________ ___________ __________ __________ _______
Iron I_______ __________ __________ __________ __________ ______
Lead_____ _______ __________ __________ _________ __________ ______
Magnesium I _______ ___________ ___________ __________ __________
Manganese I________ ___________ ___________ __________ ___________
Nercury_ ______ _________ _________ ________ ________
Nickel I_______ ___________ ___________ __________ __________
PotazsI I_______ ___________ ___________ __________ __________
Selenium_f_______ __________ __________ __________ __________
Silver I_______ __________ __________ __________ __________
I Sodium_I_______ __________ __________ _________ __________
I Thallium_I _______ ___________ ___________ __________ __________
I Vanadium_j______ _________ _________ _________ _________
Izinc I______ _________ _________ ________ ________
I _____ I ____ ______ ______ ______ ______
Interelement Correction Factors for:
I I I
I I I
I I I
I I
I I
I I
I I
I I
I I
Comments:
FORN XI (PART 2) - IN
IL
-------
L .S. EPA - CLP
12
ICP LI 1tAR RANGES (QUARTERLY)
Lab Name: _________________________ Contract:
La.b Code: Case No.: ____ SAS No.: SDG No.:
ICP ID Num.ber: — Date:
IA-tum inum_ _______I
Antimony_I I
Arsenic_I I
Barium I _________I
Berylli I ________I
ICadmium_ I ________I
lCalcium_I ________I
Cbzomium I I
ICobalt_I ________I.
ICopper_I ________I
lIron I _______I
ILead I _______I
Magnes iumf ________I
Manganese I ________I
Ixercury_ _______I
Nickel_ ________I
Potassium _________I
ISelenium_ ________
I Silver_ ________
I Scdium_ _________
I Thallium_ _________
Vanadium_I_______
Zinc I ________
Arialyte
Comments:
I
—
Integ. I
Time
Concentration
(Sec.)
(ug/L)
M
—I
I_
I—
I—
I_
FORM XII - I X
ILMO2 .0
-------
U.S. EPA - CP
13
PRZPARATION LCG
Lab Name:
Contract:
Lab Code:
Case No.:
_____ SAS No.: _____
SDG No.:
Method:
I
EPA
I
I
I
I
Sample
Preparation ( Weight volume
I
No
•
Date I (gram) f (mL)
I
I I
I I
I I
I I
I
I I
.
I
I
I
I
I
I
I
I
I I
—
FOB XIII - IN
-------
t.S. EPA - CLP
14
ANALYSIS RUN LOG
Lab Name:
Contract:
Lab Code:
Case No.:
______ SAS No.:
SOC No.:
Instr,iment ID Number:
Method:
Start Date:
End Date:
I Analytes
I EPA __________ ___________________ _________
Sample 0/F Time % R AISIAIBIBICICIC 1CICIFIPIMIMIHINIK SIAINITIV ZI
No. ILIBISIAIEID AIRIOIUIEIBIGINIGIII EIGIAILI N
I ________________ I ________________ ________ _______________ I_I_I_I_I_l_I_I_I_I_..I.__I_I_I.__I_I_._I_ _I_I_ _I_ —
I _________________ I _________________ _________ ________________ _I..... — _I_I_ _I_I_I_I_I_I_I_I_I_I._. _I_I_
I _______________ I _______________ I ________ I ______________ _I_ — _I_I_ _I._.I_I_I_I_I_I_I_I_I.... _I_I_I_I_I_
I _______________ I _______________ I ________ I ______________ _I I_.I_I_I_I_I_ I_I_I_I_I_I_._I_l_I_I_
I ________________ I ________________ I ________ I _______________ _‘_ — — _I.....I_ ..._I_I_I_I_I_I_I_I_I_I_I_ ...I..... _I_I_
I ________________ I ________________ I ________ I _______________ _I._.I_ — _I_._I.._ _I_I_I_I_I_...I__I_I_I_I_I_I_ — —
I _______________ I _______________ I ________ I ______________ _I....I I_I_I_I_I_I_I_I_I_I_I_I_I_ —
_______________ I _______________ I ________ I I_I_I I_I_I_I_I_I..._I_I_I_I_I_I.....I_I... — —
I I ________________ I ________ I I_I_I_ _I_I_I_I_I_I_I.._I_I_I_I_I_I_II_ — _I_I_
________________ I ________________ I I _______________ I_I_ _I_ _I_I_ ._...I_I_I_I_I_I.....I....I_I_I I
_______________ ______________ I ________ ______________ I_..._! ?_I_ — _I_I_I_I_I_I I
________________ _______________ ‘ ________ _______________ I_i I_..I_I_ — — _I_I I_I
________________ _______________ I ________ _______________ I_I ,_I_I_ — — _I_I_ — _I_I_._l_ ......l_I
______________ ______________ I _______ I _____________ _I I_I.._ —
_______________ I ______________ ________ I ______________ _I I I..._I_I_I_... _I......
_______________ I ______________ ________ I ______________ _I._.I
_______________ I ______________ I ________ ______________ _I I_I_ _I_..I_I___ _t_I_ ....I_
____________ I ___________ ______ ___________ _!_I I_I _I__I_I__I_I
_______________ _______________ ________ I ______________ I_I_....I I_I_..I._.I._..I_I I
_________________ _________________ _________ ________________ I_I I_I_I....I_I
________________ ________________ ________ _______________ I_I_ _I_....I_._ . ....I._._I_I_.....I_I_I I_ —
I _________________ _________________ _________ ________________ I_I_I_I_ _I_I.....t_I_I_I_I_ _t_I_ _I_ ..._I_
I _________________ I _________________ I _________ I ________________ I.__I_t_I_.. __I_I_I_I_I_I._.I_ _I_I_... _I_ _I_
I I I 1 LJ_I_I_ _I_U...I.I_I_L._I...L _I_I
I I I _________ I ________________ I_._I__.I_I_I_I_I_I_I_I_I_..._I__I_I__I_ _I_I —
_________________ I _________________ I _________ I ________________ I_I_I_I__.I_I_I_I_..I_ _I_I_I_ _I_ _I_ — — —
_________________ I _________________ I _________ I ________________ I!_I_I......I_I_I_I.....I_ _I_I.....I._. _I..... I_ _I —
_________________ I _________________ I _________ I ________________ I_I_I_..I_I_I_I_I__I.... — ...I_I_ _I_I_ _I_
_____I I I I_I_I_I_I_ 2_LL. - _I_ _I_LL _L. - =1
________________ I ________________ I ________ I _______________ I_I_I_I_I — _I....II II_ _I_I_ ......I_I_I.._.,T
_________________ I _________________ I I ________________ t_I_I_I_I_.. — _I_I_I_._I_I_I_I_I__.I....I_I_I I
_________________ _________________ I I ________________ I_I_I.__I_I_ — _I_I_I_I_..I_...I_I_I_I.....I_ _I_I
________________ _______________ I ________ I _______________ I_III_I_I II!I...I_I_I......I.....I_I......_ .__.I
I ________________ I ________________ I ________ I _______________ I_!I.,.I..._I_I _I_I_..i_II_I_II_ItI_I_
FOB XIV - IN
I _I_I
_I _;
_I
—I
— I_I_I — I
_.I_I —
— ....I —.
— _I ...._I
— _... I _‘ —
— _I —
— _I —
_I _I_ _
_I _I — — ,
— — — —
IL O2.O
-------
ATTAChMENT V
LABORATORY DOCUMENTATION AND CONTENTS CHECI(LIST
FOR ORGANIC AND INORGANIC DATA
-------
LABORATORY DATA PACKAGE COMPLETENESS
• DOCUI4ENTATION CHECKLIST
COMPLETE LABORATORY DATA PACKAGE D0CUMENrATI0N
iecluding tabulated wmmaq forms and raw data for field satxçlca, gandarda. QC un lcs.
and blanks (s o s bclow- sançl. data pscksgs)
2. A cocrçleted and signed Docums lnveinot7 Sheet used to record the inveotosy of the co kte laboratory data package
3. All onginal shipping documcots including, but not limited to, the following crnn . :
a. Clicot in-of-Cuatody Records/Traffic Reporu
b. Aitbllha
c. Cugody Scala
d. Saaçle tags (if preseot)
4. All onginal receiving docu a including, but not limited to, the following docume a:
a. Saaçle Log-b Sheet used to docurneot the receipt end inipecuoc ot ucspks and cor ainers
b. Other receiving forms or copies of receiving logbooks
c. Sample Delivery Group cover sheet identifying the uncles received for the group of samples in the data package
S. All original laboratory recordi of ua le trinafer. preparation. and analysis incloding. but not limited to, the following
documcnu:
a. Original preparation a d analysis (anna and/or copies of prcparauon and analysis logbook pages
b. Internal sample and sample c nct (orginics) or sample digc*atc/ .il.t. (inorganica) transfer chain-of-cu ody
6. All othc original project-specific documents in the possession of the laboratory including, but not limited to. the following
documents:
a.
b.
C.
d.
Telephoos contact logs
Copies of personal logbook pages
All handwritten project-specific noses
All other pro ect-spectflc documents not covered by the above
SAMPLE DATA PACKAGE DOCUMENTATION
1. Narrative
2. Tabulated 1mmary forms for
• Field sample data (in increasing Client sample iden fication mambcr)
• lAboratory Randarda (in chrooological order by instrument)
• QC samples (in chronological ordct by type of QC sample)
• Blanks (in chronological ordct by instrument)
3. Raw dats (c c field samples, laboratory standard.., QC samples, and blanks (in chronological order by instrument)
4. Lsborsso.y logbook pages for preparation and analysis of field samples, standards, QC samples, and blanks
5. .ain-of.Custody Racorda
6. Other project-specific documents in the laboratory’s possession
For orgasic data each type of isbulatad .tmmaly form nv1st be grouped by fraction (volatile. aemvolatilc. pesticidc/PCB). Depending
on whether the dax* package cou s ins organic cc inorganic analyucal data, the required tabulated forms and format for Geld samples.
standard.., QC samples, and blanks will vary.
1
-------
LABOBATORY DATA PACKAGE COMPLETENESS
DOCUMENTATION CHECKLIST
S
ORGANIC TABULATED SUMMARY FORMS
I. Field uncle multi
2. Sunogste multi (iytcin uiocztonng compound multi)
3. Micnx spikeJmatr x çikc dupliutn multi
4. Mcthod/1abo atorY blank multi
5. Tuning multi (GCIMS in rumei pci{orTUe cbec )
6. Iniual calibrution re lta (GC/MS)
7. Initial calibration taniiti (GC)
8. Cor. n iing calibration multi (GC/MS)
9. Condoning calibration re&alti (CC)
10. Ii crna1 ‘ d multi (GC/MS)
II. CC analytical .cquc c
12. Pe cide cicamip multi
13. Pc acidc/PC3 idend6c.stioo Immary
14. Method detection limit udy rewlLi
INORGANIC TABULATED SUMMARY FORMS
1. Field u nç lo rcvdt.i
2. Initial and coetioning calibration vcn caUOQ multi
3. Coeti act required dcwctioa limit .n Ia’d multi
4.
5. ICP iixcc(erencc C CCk umple multi
6. Matnz apikc and pom-digc*ioc iikc umplc re ilti
7. DupLicate uncle multi
S. Labontoey cotitol uncle multi
9. Method of mnd.rd addition. re ihi
10. ICP aerial dilution rcndti
11. In *vnxec detection limiti
1 . ICP Li ern1cmc correction factors
13. IC? liorazrangcs
14. Preparation log
15. Analyn. log and Fiuoace AA QC multi
2
-------
LABORATORY DATA PACKAGE COMPLETENESS
CONTENTS - GENERAL CHECKLIST
DOCtJM 4TATION CONT ITS
NARRATIVE • Laboratory name
• Clici Raquc /CooLract pro oct number
• CL? RAS or other Clicec sançle idenuflcanon numbers crose4eferenced to the
laboratory sa Ie idcndflcatioa numbers
• Aniiynca-l methods and e Ct procedures perfoe by the laboratory
• Any deviations from the methods
• All problems ciicow crod with quality coerrol. sample.. shipmeec. and all analytical
problems c countcrcd in processing th. samples
• Problem resolution mu be documeered U wall u any other factors which may affect
the validity of the data
• All occun occa encowsered duneg the analysis of the sample set
• Explananon of all data flAgs if çectflod in the analytical method
• For CL? RAS M,cciflc organic data. pH of each water sample eibmiucd for volatile.
analysis, hat of all ins .r, . f mi iiJ j cgrauoes performed
• For CL? RAS specific inorganic data - whether IC? iiwelemeor corroctions and
backgivuød corrections were applied
• Example. of calculations of both a detected ponuve remb and a dctecuoo/quantitatioo
limit reported (or each typo of sample analysis including all equations. sample volun s,
sample weights. dilution (actors, pcrcc Wpczccat mounire. and other information
required to reproduce the Laboratory tenths mea be indicated
• Signed and dated by the laboratoq manager
• All telephone communications appended to narianve ______
LABORATORY LOGBOOK Logbook documet atioc:
PAGES S Standwfs preparation loga
• QCaamploprcparatioeihogs
• Sample prepant ioo/exiraction/digcaioo logs
• Sample analysis run logs
• Peruonaflogs
• Hand-written project-specific notes
Logbook pages coeteeca (where applicable):
• Labor wcy name
• C1ie sample idcotificaticn number
• Laboratory sample sdcati& -thoti manther
• Discs of preparation and analysis, and i sala of preparerlanslya
• Source of gandarda and QC uncles
• Weights and volumes of samples and andarda
• burial and final volumes of uncle preparedlpurgodi
cxv actcdldige i sed
• P rces* motaure/pcrvcor solids
• 1c ecto&analysia volumes
• Dais and time of uncle injection
• IDihilon factors
CHA OF-CUSTODY External ath-of-Cuatody Record:
RECORDS • Dais of sample receipt
• Signantre of teceiving personnel
• Cn d .w n of shipping containers and sample beck. upon receiPt
• Condition of cuatody seals
• Prc. .. . ,ce/sbscacc of aiibills, cugody scala. Client cuatody records, treftic reports.
sample lags
• Problems or discrcpancica with urrçka received or the documentation on the aio -o(-
Cuatody Record
Internal ain.o(-Cuatody Records:
• Laboratory name
• Client sample identification number
• Laboratory sample idcntrficaiion number
• Date of sample transfer and receipt
• Signanue of personnel inna(evrtnglreccsving the sample
• Purpose of triasfcrireccipt., location of sample izana(cued
3
-------
LABORATORY DATA PACKAGE COMPLETENESS
CONTENTS - ORGANIC TABULATED SUMMARY FORMS
oocu m r cowr rrs
FT D SAMPL.E RESULTS • Clicac ua lo I4C lfi cEhOQ (ID) in mbcr
• Labontesy aansple ID ber
• Tar coasp aod na a
• Tabulated analytkal t tZta for ide 6-’ ..’it ( t ncal qua ztaz oo Iiinica) and
q ’ .i ”on (positive bite) with co e rsi on it s
• Any liboraloty qualaGcr flags - Iabonaosy çuliScr flag. (or each %ar u aoalytc mu
be tabulated oo a separate fonn ( dcffIi! — ‘ - be provided for each laboratoty
ç aliGcr flags).
• LaborIws7filoED
• Sa Ie maltu type
• L.evcl of analysis (low, iediuin)
• Pcrce “- “e or pcrcc aolids
• GCcoluma
• Seespla weight. a d1or uncle voluine* prepasedlpurged/
cxzeacted/ analyzcd
• Ini t ial and final extract and extract clcan- volumes, inject oo volume
• Cleanups performed
• Ddutioo factor
• Mea, redpH
• Date, of ian,lo recczpe. extraction. and analysis
SURROGATE RESULTS
• Sançk ina&nx
• Level of analysis
• GC column
• Clici* aample ED number.
• Surrogate conspounds added
• Perceu recoveries of wrrogszcs
• QC limits for sU si rrogate e andards in Geld uirçlcs. QC un lea, and blanks
• All outliers flagged
• Tote! member of siurogatca outside QC Ilnies
• l’ ’(jou of mrrogatcs diluted out
MATRDC SPIKE/MATRIX
SPIKE DUPLICATE
RESULTS
• Siuspl. matrix
S Level of analysis
CUci aa çle ED member
• Matrix spike coaspoundsedded
• Tn co eatrations of the spikes added
• Comeextraboos of the apik. coospounds cbac*v.d in the spiked sanclo
• Sa le coocextra*too of each spike co — 4 ’cted in the osigmal un .piked sample
forthe MS end MSD
• Peicu* recoveries of h. spiked compounds in the MS/MSD uiiçks
• Relative pcrceat diffcteeces of the spiked omp usia between the MS and MSD
‘a—
• QC limits foe all spike compounds- perc recovety and relative pcrcci* differcece
• AU outliers flagged
In addition to the above, the resiulis (or all target coa oundain the MS and MSD uncle. muat
be tabulated oe the summary forms used to tabulate the field sample results.
4
-------
LABORATORY DATA PACKAGE COMPLETENESS
CONTENTS - ORGANIC TABULATED SUXMARY FORNS
DOCUMENT II
METHOD/LABORATORY
BLANK RESULTS
• OC col”mn. innnimcna ID
Dii i and lime of analyiu for the bLink gacIf
• Daze of cmacuoa
• Matrix with which the blank i i u.ociated
• .cvdo(anilyiis
• Laboratory ian le ED mnthet
• Lit of Cliee field sample ID oumberu and MSIMSD samples uaociaie4 with each
blank (separate forms are used for each blank)
• Liborazory file ID. of the samples and associated blank
• Dazcslunxa of analysis for field samples and MS/MSD samples which are associated
with each blank
In addition, reniks for each method and laboratory ioitsizme blank it be ixluded on the
tabulated forms that are used for the Geld sample rentha.
TUNI]4G RESULTS (GC/MS
INSTRUMENT
P FORMANCE CHEC)Q
• Initrument ED. laboratory file ED
I Daze and lime of injection for each tine compound analysis (each tine on a separate
form)
• Tune compound name
• Mw-wchaxgo ratio (in/c) for each ion
• Ion abundance criteria
• Pcrccnt relative abund.n cs
The form met also contain the following tabulated information wociated with each tine and in
— oedw
• Client simple ID mimbcrs u.ociated with that tine
• Laboratory sample ID ouaibas
• Labo rs zoayflheID.
• Date and time of analysis for all field samples, MSIMSD sample*, blanks, and
itandeeda wociatcd with that tine
I All outliers flagged
INTrEAL CALIBRATION
RESULTS (GC/MS)
• I zment ID, laboratory file ID.
• Purge method
• Discs and limes of “ d analyses for that inkial calibration
• Target compound names
• Concentrations of the calibtazioc itandards
• Relative rc onas factors for each targit and suvegise compound at each mnda,d
cooce
• Mean relative response factors (or each target and ssrivgazc compound
• P .ezi relative atandsed deviations (or each target and sirrogita compound
• QC limits for each initial calibrtuoa (each initial ca! t*ticn on a separate form) -
mi, . zin R2.F. niaz imem%RSD value.
• All outliers flagged
5
-------
LABOPATORI DATA PACKAGE COMPLETENESS
CONTENTS - ORGANIC TABULATED SUMMARY FORMS
DOCtTh4 1T CONT 4TS
u rrrIAL CAliBRATION Re etion time informanoa:
RESULTS (GC) S Io swDc ID, GC column
• Dazes of analysis
• Coaccaztsuoa of the calibrazioc aaduds
• Target compound and s ncpze compound eames
• Pl.4#f nn tim.s foe each target and . rzogazs compound ac each azandard cor cnLtatzo0
• Mean rv*eet oa times foe each target and a rogize compound (if muhi-potet
• Rr ’ lime windows foe each target and . rmgaze compound (QC limits)
Calibisuon cw infoemazioc
• In vmeet ID, GC c’ ” ”
• Dates of analysis
• Cooecets Uoes of the calibrsuoa gandaida
• Target compound and irmgate compound aames
• Calibration facton for each target and narrogale compound at each izandard
co cetraZa0a
• Mean calibration actoe (foe multi-point calibrthoa) for each target and nartogate
• Percent Relative Standard Deviation for each target .nd narrogite compound
• QCUmi as-%RSD
• Ali oualiers flagged
Resohitioc in(ormstioo
• lnaznament ID. GC column
• Da les and times of analysis
• Laborazozy aançlc ID
• Names of compounds foe which is measared
• R.eteesion limos for each of those cccçounda
• Percent resohnioc between each pair of coeçounda
• QClis.%roso luz i o n
• All outliers ifigged _________
CONTI} 1W4G • Inaziument ID. laboestozy file ID
CALIBRATION RESULTS • Purge method
(GC/MS) • Date and tim. of coetiajing calibration analysis
• Daze and time of initial calibration analysis aamciazed wub that coiiiaaing calibraitoc
• Target compound and surrogate compound names
• Mesa relative rmpoaae factors from initial calibration for each target and surrogate
• Relative rmpcose factors from c uig calibraume for each target and surrogate
compound (each c’ ”g calibration on a sqtsxau. fooc)
• P.. ,. .at differences foe each compound
• QC limits foe each target and sunvpze compound (each coeeiiein g calibration on a
separate foret) - minimum RU. insim % D
• Conccesrazioca of lbs contiating calibration esndssds
• Uiersllagged _______________
6
-------
LABORATORY DATA PACKAGE COMPLETENESS
CONTENTS - ORGANIC TABULATED SUMMARY FORMS
I DOCiflA r
CONTINUING
CALIBRATION RESULTS
(GC)
In sume ID, GC column
• Laboratory uncle ID
Dates and times of co’ ’ing calibration andazda analysis
• Date of aaaocisicd initial calibration analysis
• Target coccotiad and siurmgaxe coa owxi oa
• R.eieauon time (or each target and siinvgaie coacound
• Calculated amouai of gsndagd
• Nccn inac*ouaiotsw ld ard
• Relative Percem DitTcre c for each coacound
• QC control limits - RPD
• Percent brtakdowna (or conipounda used to asiirc c cnt of breakdown (codrin and
4,4’-DDT) and combined breakdown
• QC limita - pcrccntbrcakdown
INTERNAL STANDARD
RESULTS (GC/MS)
• In umcnt ID. uboratary file ID
• GC colu . purge hod
• Date and Limo of cors.r.nrtg calibration gandard analysis
• Client uimple idci i&atioa aambcra
• Internal compound names
• Rete vla times and azea counts of tho ç ’’ ’ ’ for each internal andard compound
in the con ’r-’ng calibration .i hrd. field MS/MSD umplcz, and blanks
a.uociatcd with that c n mrng calibration (separate form for each Gof f IIng or tazual
calibration)
• QC limits- area counts and rctcntioU times
• All outliers flagged
CC ANALYTICAL
SEQIJ€NCE
• Inmrnmont ID, OC column
• Initial calibration dazes
• Lint of Client sample ID ounthcrs in that l cal .cquemc (in chronological order)
for all gandarda, field aaiiçka, QC uncles. and blanks
• Laboratory sample ID azmbcrs
• Dazea and times ofanalyacs
• Mean wrevpi. e ’ ”a ti - from initial calibration
• P ’ times of the surrogate compounds
• QC limuta of the surrogates- rrteiii n times
• All ouilien flagged
7
-------
LABORATORY DATA PACKAGE COMPLETENESS
CONTENTS - ORGANIC TABULATED SUI4MARY FORMS
DOCUMENT
CONTENTS
CLEANI.JP
Floiiad Caetridg. cck Rn Zti:
OC coin
• F lorinl cartridge lot ountbcr (each lot cca seçarato form)
• Date o(cbcck i&ii i .nacaiysü
• Nan a of cooçouoda in the Rorisil cartridge check iolut oc
• Amouci of çike in the check moluzioc
• Amouci of ipike recovered to the check
• Pcrccot recoveries
• QCIimi*s.petceotrccoveries
• All oudicea øagged
• CILcot ianç . ID numbers associated with tha t form! cartridge
• Labocstes ’ san le ID number, uaocistcd with tha t Floriail cartridge
• Dazes of uu lc inalyci
GPC Calibranco R ths:
• GPCc* mn
• Calibrauoc data of GPC column
• GC cclu s
• Name of spike coaspouzids added to GPC column
• Amouoto(ipike added
• Am ci of spike recovered
• Perceot recoveries
• QC limits - % recoveries
• All outlices üagged
• Cileot u !e ID ountheri associated with tha GPC column calibration
• Laboncoty uncle ID munbcr , wociiicd with thc GPC column calibration
• Dates of ia o k analyses
0 In rirmcot ID, GC columns
• Dazes o(a n aly s
• Clicci wxsplc ID mnzther (oni aeparste form for each uncle)
• Labonaixy WxclC ID number
• Targra coazspciual namo dctcc&ed
• Retention time of compound on each colume
• p.t. .i;n Itme windows
• Coecs acioa (mnan concentration for nsih ccmpooct1 compounds)
• Perceot difference
DETECTION
RESULTS
S Target compound names
0 Concentrations of spikes added
• Concentration detected (or each MDL ipike
• Standard deviation and calculated MDL for each target compound
The cxace prvc.dzuv utdicod to gcacnzc the MDLa mo* be documented in detail in the narrative.
The ocuaocc and associated cocgant values u*alimd to ulaie the MDL for each analysts me*
be Tba coluom, inMnuncci CD, trip compoesion. and operating conditions muse Sc
clearly docui,w .d in the raw data.
8
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LABORATORY DATA PACKAGE COMPLETENESS
CONTENTS - ORGANIC RAW DATA
DOCUM CT
co r
RAW DATA The laboraicey data package mug coatain raw data ,r all field unçlu. aedards. QC uu lcs.
matrix spike a d matrix spike deqilicate ssesplcs, and b lanks. The exact format and cocicnt of the
raw data will depend on the paiticular analysu method requc*ed/co ractcd. However. ill
imeii pn m4* atrip chart recording., chometograma. q. ”” ’n repoeti. aiau epectra,
and other type. of raw data gcixritcd by the laboniory foci pamcWar project mu be providcd
in the data package.
Typical raw data for organic GC(MS analyses includes, but is limited to the foUowing:
• RncOonNctcd total ion cb logrun for each as lc or uc lc e ract, nandards.
QC aan le ., and bLuiks
• n*rumcat quantitatioo report. coni ng the following information: tsbocacoq sanqile
idciiiflcazioa number, Clscg sanqile number, laboratory file ED. dale and
time o(analy .u, rei’ ctkn line .ndloc scan number of q ’ ’ .on on with mcaiured
area, analyse coocerenuoc, c y of area sable from data sy em. GC/MS n ricmem
ED. laboratory file ID, column, trep coaipoáioa. and operating cond eiom
• Raw and cthaoccd maci speeu (or all positive target ccixçcund t anaka in field
sansples daily co unng calibration gandud reference qi r* for all poaiuvo field
sample tanaka
• Mau specua and three Library searched be -maich mass qiccus for all tentatively
idc 6cd compounds repotsed
• Lnatsvmeat normalized mu. lining and the mass spectrum for each nina.
Typical raw data for organic GC analyses includes. but is limbed So the following:
• zomatograuia for acid aamplca, callbrinoe macduds, QC samples, and blank.
co iithig the following fl(O(, I1M1R ’ Clicat mplc ideiiiflcatioc number, volume
iniocled. date arid time of injection, CC column .i .nn. CC inmriimcse
ideimcflcauoo, pontively ideetafled compound. ms* be labeled with the compowid
on either directly from the peak or on $ fliiOut of the rrteiiaoo times
• Qxvmitogram. for bosh CC C” 1 ’J”
• CC iz*egrauon report or data sydem pri osm
• Manual worbhccta
9
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LABORATORY DATA PACKAGE COMPLETENESS
CONTENTS - INORGANIC TABULATED SUMMARY FOPMS
p --
DocljMEWr CON1
• Sauç lo ma tr tx type
• Level of anaJyaü (lOW. medium)
• Perccet u. &rO orpcrcet aolidi
• Date of uzeple receipt
• CUcet itieplo idenufication number
• borsto 7 uu Ie ide tflcauoo tmbcr
• Target analyts names
• Tabulated anal iical rcwtl&a for de3i& hoe ( t flCiJ Li m its)
q. ,tHl ott (pedtivo hits) with coo c raUon units
• Any aboratot7 qualifier flags - aboratory qualifier ftiga for each target analyte mu
be tabulated on a separate form (dcf1ni1 on. t* be provided for each laboratory
qualifier flags)
• Cooceetntioa qusilfiers ( tM cazing rendts less than the CRDL)
• Analytical method used for each analyt. (uacally iial•. r d with a iyu oQ
FIELD SAMPLE RESULTS
(rrIAL AND CONTINUDIG
CAL IBRATION
VERIFICATION RESULTS
• Sources of the initial and co. ’ .ng ca ration ye cation ataedaids
• Target inalyte names
S True values of the calibration verification ataedazda
• Cooceetnuocs found for the calibration vcaflcauoa standards
• Pcrcc recoveries
• QC limits- pcrccet recoveries
• Analytical method used for each analytc (unraliy with i symbol)
The order of reporting the initial and conthiIiiflg calibration ycriGc tio standard.. for each analyte
nw* follow the order in which the standards wets analyzed.
CONTRACT REQUiRED
DETECTION LUi(TF
STANDARD RESULTS
• Source of the CR L standards
• Target analytes
• True values of the CRDL ‘-.-d for each anslyte
• Coacenirstions found for each analyte
• Perceni recoveries for each analyte
• QClimits(itkaown)
The order of reporting the CRDL •‘ -“d rcwlts for cacb snalyto follow the order in which
they were analyzed.
BLANK RESULTS
• Matrix for which the prcparation blank is wocraied
• Coaceatratioa units for each blank type
• Target analytc names
• Initial and cocstiaiing calibration blank tenths
• Preparation blank remits
• Cooccetration qualifiers
• Anilytical used for each analyts (umally ‘ 4 with a symbol)
The order of reporting th. initial and co.u.nwng calibration blanks and preparation blanks for each
anslyte nasni folios’ the order in which they were analyzed.
IC? IN 9LFER2 CE CHECK
SAMPLE RESULTS
S I C ? instzu ID onmber
S Source of the ICS .ol” ’n.
• Target IC? analytes
• True values of each target IC? ansl 1a in the solution cu d u i ig inicrfereus only
• True values of each target IC? snalyte in the solution co ”g ustcrferrnis and
analytes
• Coecenirszsons of larger IC? anaiytes detected in the co .g inserfeeceta
only
• Cw-. taiiocs of target IC? analytes detected in the lnl. t o co’ ’g inicrfercnts
and analytes
• Percent recoveries
The order of reporting the inrerfercuec chock aarrçle re,.ilts for each analyte aa’* follow the
order in which they were analyzed.
10
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t. ABORATORY DATA PACKAGE COMPLETENESS
CONTENTS — INORGANIC TABULATED SUMMARY FORMS
DOCUM (T JL .
MATR.DC SPflCE AND POST-
DIGESTION SPIKE SAMPLE
RESULTS
• Sanspic me nx
S Level of snalys&s (low, medium)
• precegaol idao(tbes saspla
• CUeS un fle dcidiflc1 ioa number
• Target analyte na s
• Co e rauoaa of the spikes added 10 the sa Ie
• Coaceseraucce found in the spiked uncle
• Co c ra&ioo found in the unspiked sa I.
• Petce meOVCIIeS
• QCUm i ta-pcrcci recoYci7
• All outliers flagged
• Co c rauoa qualifier.
• Analytical method used for each analyte (unndly i d with a symbol)
Separite fonna are used to rrport matrix spike reaths and po -dige oe spike ree.atts.
DUPUCATE SAMPLE
RESULTS
S Saa Ie matrix
• Level of analysis (low, medium)
• Percc solids of the original wick and duplicate unspie
• CILCt1 uaçlc idetrification auaibcr
• Target analyte names
• Coc cesrauon of the original esoWle remk
• Co ei1rsucc of duplicate uncle re tlt
• Relative pcrcc diffcrc e
• QCIinüia
• All outlier, flagged
• Cooce ratioa qualifiers
• Analytical method used for each analyte (untally 4 ’d with a symbol)
LABOL4 TORY CONTROL
SAMPLE RESULTS
S Source o(the aboratoty control sample
S Matrix of the L.
• Targnt analyle names
• True coocentntions
• Coaccntrsuoca found
• Petcent recoveries
• QClindta
• Coocentration qualifiers
Because a laboratory control san le should be dlgcmed for each matrix sod digemon batch,
l;t osnd forma me be present u appropriate if t than ona LCS for a matrix was analyzed.
MEI’HOD OP STANDARD
ADDITIONS RESULTS
• Client sample identification number
• Coeceundoca of each MSA spike added
• Abaorbance A,i ’i in each MBA spike u well u the sample itself
• Final COOCCntI*ZI0Q
• Coerelailos coefficient
• All outlier, flagged
Reseki for different samples for each analyte int be reponed sequentially.
ICP S 1AL DILLTI1ON
RESULTS
• Sample matrix
• Level of analysis (low, medium)
• IC? iniritment ID
• Client sansple idcntiflcadoc macther
• Targnt analyte names
• Cooeeiintaoca of the un.4 1ufr4 umple reaak
• Concentrations of the diluted uncle resiak
• vent difference
• QC louts - percent difference
• AU outliers flagged
• Concesarsuon qualifier.
Analytical method ued t t mfh11e (uatally i -nd with
11
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LABORATORY DATA PACKAGE COMPLETENESS
CONTENTS - INORGANIC TABULATED SUMMARY FORMS
DOCUMENT CONT9IT S
INSTRUMENT DETECTION
• In z &me ID numbers used for the CDL detee nauoa
uMrrS
Ds e the IDLa wcm determined
• Wavslength and background used foe each analyte
• Target analyte names
• Type o(backgzvund correcUoc used where applicable
• Inmrunicet detection limbs
• Coetract required detection limits
• Cone rathoo units
• Analytical method used for each analyte (un al1y indicated with a gymbol
ICP INT fl .D (a T
• Wavelength for each acalyle used for the determination
CORRECTION FACTORS
• IC ? in z tment CD number
• Data of inierclcment correction (actor determination
• Target ICP analyla names
• !etnr(cricg snalytca with which the in&crekme ccrrcctio (actors were determined
• Ictetelameet correCUOO (actors for each analyte
IC? LINEAR RANGES
• IC? ingtuneet ID number
• Date of the Linear range determination
• Integration time foe cach analyte
• Target IC? snalytes
• Conecetas.ioa of the upper Limit of the Linear range for each snalytc
PREPARATION LOG
• Analytical method (each anslytical n ”d on a .cparaie form)
• CUeet uncle ID member of all Geld sa lca. QC uncles, atamiards, and bLanka
d igeetad/diet elled
• Sa Lo preparation date
• Sa le weight
• Sancle volume
ANALYSIS RUN LOG
In emcat ID
• Analytical method
• Start and cod dazes of the analytical aequcaca
• Cleat uncle ID numbers in chronological order
• Dihn (actors
• Time of anaiysia for each analytical uncle and andard
• Analytea for which the run acqucece pezuena
Furnace AA QC analyses rendua are also typically pcovidcd on this form - ace below.
FURNACE AA QC RESULTS
In 4i’ ”i the information required on dun Analy a Run Log (see shoes):
• Perceat reLative Macdud deviation of duplicate injections (owlicti wtally indicated
with lags on the tabtilatcd Geld uncle reatha form. Form 1)
• crecat recoveries of poic-digeatica spikes
The above information mu be reported on separate (cema for each furnace AA analyte.
12
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LABORATORY DATA PACKAGE COMPLETENESS
CONTENTS - INORGANIC RAW DATA
DOC1JP T Ii CONT 4TS
RAW DATA
The kbora&07 data package mud cmn raw data (or all flald aamplea, gandazda. QC umplea.
matrix ipike and dupticaic sançlca, a d blank,. Th. exaci formai and cocieci of the raw data
wtU dcpcnd on the paz tculu analyau method raquc cd/co ctad. However, for each reported
value for. particular prnject. the laboratory mu hjde all raw data uaed to obtain hat reported
value.
Typical raw data (or inorganic ana.ly.es include, but is D C I limited to the following:
• Inatumcci pncieuzi. drip chart recordings, etc., for all field u ,lca. QC umples,
ø aedazda. and blank, co. mng the following inIor.”.”ort laboratory uaiple
idc i&atio mambcr, Clica sample ID csin ,er, date and time of analysis,
ahao banedemeanon value,. analyte c c aiioc, in nznicci ID, lab file ID, and
in umcci cig
• Standard curve raw data, plotted andazd curves, Linear regreaaion equations, and
CO(TOQ COCffiC IC C IL
13
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ATTACMMENT VI
REGION I CSF COMPLETENESS EVIDENCE AUDIT PROGRAM
JULY 3, 1991
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REGION I CS? CQBPLET ESS
EVI E1ICE AUDIT PROGR. M
JuJ.y 3, iggi.
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TABLE OF CONTE 1TS
Section Page
1.0 INTRODUCTION
2.0 COMPON TSOFTHECSF . 1
3.0 ThE CSF TRP CKING PROCEDURE 2
3.]. Tracking Overview 2
3.2 CSF Tracking Procedure 3
3.3 Laboratory Resubmittal Tracking 4
3.4 Data Validation Oversight 5
4.0 THE CSF AUDIT P .FORMANCE PROCEDURE
4.]. CSFAudjtovervjew .
4.2 Inorganic Completeness Evidence Audit . . . . 5
4.3 Organic Completeness Evidence Audit 9
5.0 POT ’rIAL PROBL S WI TEE CSF AUDIT PROCESS . . 12
5 • 1 Guidelines for Contacting the Laboratory . . 13
5.2 Guidelines for Not Contacting the
La.borator r . . . . . . . . . . 13
6.0 COMPLETION OF EVID (CE AUDIT AND DISTRIBUTION OF
A IT • • . . . • . . • . . . . . . . • . . • . . 15
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1.0 INTRODUCTION
- Evidence audits are conducted to ensure that laboratory
documentation and data will be admissible in potential
litigation. Prior to the jmplementation of the OLMO1.0
5 rganic and ILMOi..0 Inorganic Statements of Work, evidence
audits for all Routine Analytical Services case files were
performed by CEAT-Techlaw. However, under the ILXO1.o and
OLMO1.0 Inorganic and Organic Statements of Work,
laboratories must now develop Complete Sample Delivery Group
Files (CSFs). The CSFs consist of the original Sa.mple Data
Package and all related documentation. Laboratories
operating under the new contracts will submit the CSFs
directly to the regions, who will now be responsthle for
conducting the evidence audits. This process allows the EPA
to quickly monitor the quality of the laboratory
documentation.
To easily integrate the evidence audit into the
validation procedure, the Region I Quality Assurance Office
has developed the Region I CSF Co leteness Evidence Audit
Program . The program addresses two fundamental areas of
res onsibility necessary to ensure the admissibility of
laboratory—generated documentation and analytical data as
evidence. First, the integrity of the cs must be
maintained during all transfers. Second, the completeness of
the CSF documentation must be assured through the evidence
audit process.
The Region I CSF Ccm 1eteness Evidence Audit pro
replaces the procedure described by CEAT-Techiaw in EPA
Regional CSF Comt 1eteness Evidence Audit Guidelines . None of
the forms supplied by CEAT-Techiaw at the Complete SDG File
Training s minar held on February 20, 1991 will be necessary
to complete the Region I CSF Completeness Evidence Audit or
to perform the CSP tracking procedures.
A flowchart outlining the Region I CS? Com 1eteness
Evidence Audit Proqra is included in Attachment I.
2 • 0 C0! ON lTS OF TEE CS?
The CS? Consists of the original Sample Data Package and
all related documentation. The laboratory is required to
assemble the CS? and Submit it directly to the Region (as
specified in Exhibit B, Section II, 3—22 of OLMO1.o and
Exhibit B, Section II,B—13 of ILMO]..o). The laboratory
submits a Complete SDG File (CS?) Inventory Sheet, DC-2 Form,
(inorganic pages 1—2, organic pages 1—4), which indexes all.
1—1—03—01 1
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documents submitted in the CSF. rn addition to t ie original
Sample Data Package, the CSF cOns ists of the following
original documents:
• A completed, signed, and dated Com ].ete SDG File
(CSF) Inventory Sheet, DC-2 Por’ ;
• Al]. original, shipping documents iflClUding the EPA
chain of custody records, airbills, EPA traffic
reDorts, and sample tags sealed in plastic bags;
• AU. original. receiving documents, including the
sample log-in sheet (DC-i Form), and other
receiving forms or copies of receiving logbooks;
• All original laboratory records, not already
submitted in the Sample Data Package, conce. ing
internal laboratory sample transfer/tracking,
preparation and analysis;
• All other original SDG—specjfjc documents in the
laboratory’ S possession including telephone
contact logs, copies of persona], logbook pages,
and hand written case—specific notes.
3 • 0 THE CSF TRAC&LNG PROCEDURE
3.1. Tracking Overview
1 ro comply with evidence requirements, signed and dated
custody seals must be affixed to the CSF whenever it is
transferred. The CS? is Considered transferred whenever it
changes location upon shipment or hand—delivery. This occurs
when the CS? is shipped from the laboratory to the Regional
Sample Control Canter (RSCC), from the RSCC to the Prime
Contractor, from the Prime Contractor to the Data Validation
Subcontractor, from the Data Validation Subcontractor to the
Prime Contractor, whenever the CS? is requested for oversight
by the Region I EPA Quality Assurance Office, or any other
time the CS? must change custody.
Data Validation SubContractora will, not be responzjble
for conducting evidence audits; however, they must be
informed of and. adhere to the Region I CS? Com letene
Evidence Audit Proqrp , C F Tracking Procedures. The Prime
Contractors are responsth le for ensuring that all Data
Validation Subcontractors are properly trained in the
procedures outlined in the tracking procedure.
1—1—03—01 2
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The CSF Tracking Procedure is initiated when the CSF is
received at the RSCC by the Sample Control Coordinator (SCC).
The SCC will initiate the CS? Recelpt/Tran3fer Form, which
will remain with the CSP through every transfer. The curpose
of the CS? Receipt/Transfer Form is to document the presence
and condition of custody seals, which must be affixed to the
data package in
compliance with evidence audit requirements during all
transfers. Examples of blank and completed CSF
Receipt/Tramsf or Forms are included in Attachment hA and
IIB.
3.2 CSF Tracking Procedure
The CS? is received at the RSCC from the laboratory
under custody seal. The SCC initiates a CS? Receipt/Transfer
Form, which will remain with the CSF with every transfer. For
each transfer, the following protocol for CSF tracking and
completion of the CS? Receipt/Transfer Form must be followed:
1. Inspect the unopened CS? shipment. Determine if
custody seals are present or absent. If present,
determine if custody seals are intact or broken.
2. Open the CS? shipment and complete the CS?
Receipt/Transfer Form. The case number, SDG
number, and data package number will be com leted
by the SCC.
• Receipt Date — Enter the date that the
contractor/valjdator received the CS?;
• Received By - Enter the name and initials of
the contractor/va].idator who has opened the
CS?, and list the affiliation, i.e. RSCC,
Weston/ ESAT, NUS/ARCS, Dynamac, EPA, etc.;
• CS? Activity - List the CS? activity. For
ic tple, the SCC will list the activity as
“CSF Receipt”. The contractor/valjdator will
list the activity as “validation”,
“resubmittals”, “data validation oversight”
or “CS? storage”;
• Custady Seals - Indicate whether the custody
seals were present and intact;
1—1—03—01 3
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• Released — If the CS ’ must be transferred to
a new location, identify which organization
the package will be released to and the date
of release, i.e. shipment data or hand—
delivery date.
3.3 Laboratory Resu.bmitta]. Tracking
All laboratory resu.bmittals requested during the
evidence audit and/or data validation must be shipped under
custody seal. The Prime Contractor Lead Chemist is the only
one authorized to request and receive resubm .ttals. The Data
Validation Subcontractor cannot request or receive
resubmittals. The laboratory may send resubmittals to either
the RSCC or the Prime Contractor.
If the laboratory sends resubmittals to the RSCC, a new
CSF Receipt/Transfer Form will be initiated by the scc. The
resubmittals and new CS? Receipt/Transfer Form will be
shipped to the Prime Contractor Lead Chemist as stated in
section 3.2. The Prime Contractor will complete the
appropriate section of the new CS? Receipt/Transfer Form and
will indicate the “CS? Activity” as “Resubi dttals”. The Prime
contractor will then forward the resubmittals to the Data
Validation Subcontractor under custody seal.
However, if the laboratory sends resubmittals directly
to the Prime Contractor, a new CS? Receipt/Transfer Form will
be initiated by the Prime Contractor. The Prime Contractor
will complete the appropriate section of the new CS?
Receipt/Transfer For and will indicate the “CS? Activity 1 ’ as
“Resubmittals”. The Prime Contractor will then forward the
resubmittals to the Data Validation Subcontractor under
custody seal.
If the Prime Contractor receives resubmittals from both
the laboratory and the RSCC, the Prime Coutractor must verify
that the resubmittals received from the R.SCC are identical to
those received directly from the laboratory. The Prima
Contractor may then discard and recycle the sat of
resubinittals received from the RSCC. If the two sets of
resubmittals are not identical, the Prime Contractor must
contact the laboratory to determine which set of res ittals
is correct.
Upon receipt of the resubmittals, the Data Validation
Subcontractor will complete the appropriate section of the
new CS? Receipt/Transfer Form. Under “Released”, the Data
1—1—03—01 4
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Validation Su.bcontractor should indicate “Included with cSF”.
All CSP Racaipt/Transfer Forms and laboratory resubmjttals
must be kept with the CEF.
3.4 Data Validation Oversight
If the QA OffIce requests a CSF for data validation
oversight, the Prime Contractor must Complete the appro rjate
sections of the CSP Receipt/Transfer Porn and shj the CSF
under custody seal to the EPA. When the data validation
oversight is complete, the EPA will complete the appropriate
sections of the CS? Receipt/Transfer Form and ship the CSP
under custody seal to the Prime Contractor.
4 • 0 THE CSF AUDIT P FORMAMCE PROC URE
4.1. CSF Audit Overview
The purpose of the evidence audit is to determine
completeness of the CSF as shipped from the laboratory. The
auditor must verify that all documents are present as stated
by the laboratory on the DC-2 Form and that JJ pages in the
CS? are accounted for on the DC-2 Porn. A].]. evide.ntiary
documents must be clearly identified with the case number and
SDG number, and must be signed and dated where required. The
accuracy of the Sample Data Package submitted as part of the
CS? is determined during the normal data validation procedure
and is not part of the evidentiary audit.
The CS? Audit Performance Procedure outlines the
protocol that Prime Contractors must follow to complete the
evidence audit. The evidence audit must be completed by
Prime Contractors only. Data Validation Subcontrpctors
performing data validation will not be responsible for
conducting the evidence audit, although they will be required
to adhere to all CS? tracking procedures, The Prima
Contractor will perform the evidence audit by reviewing the
EC-2 Form, which is submitted by the laboratory as part of
the CS?. ples of blank organic and inorganic DC-2 Forms
are included in Attachment lilA. eam 1es of laboratory-
completed organic and inorganic DC-2 Forms are included in
Attachment IIIB. P eamples of laboratory-completed and Prime
Contractor-completed organic and inorganic DC-2 Forms are
included in Attachment iiic.
4 • 2 Inorganic Completeness Evidence Audit
The following describes the Region I guidelines for
1—1—03—01 5
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conducting completeness evidence audits of inorganic C Fs.
The CST will be shipped to tile Prime Contractor Lead Chemist
by the RSCC. A CS? Raceiptf Transfer Form, initiated by the
SCC, will be shipped with the CS?.
The Prime Contractor Auditor/Validator will perform the
evidence audit using a riococo v of each completed and signed
DC-2 Form which is submitted by the laboratory as part of the
CS? or which is submitted with resubmitted documents. The
Prime Contractor Auditcr/Valjdator must not write on the
original DC-2 Form, which will remain with the CS?,
unmodified.
When resubmitta].s are requested, the Prime Contractor
Auditcr/Valjdator should request that the laboratory number
the resubmitted pages so that they may be appended to the end
of the CSF. Pages should not be inserted into tile CSF, and
original pages in the CS? should not be replaced by
resubmitted pages.
When the laboratory resubmittals are received, r otocopy
the new DC-2 Form and perform the evidence audit for the
resubmitted sections only. The Prime Contractor
Auditor/Vajjdator must not write on the original DC-2 Porn,
which will remain with the CS?, unmodified.
The Prime Contractor Auditor/Validator must generate
telephone counicaticn logs whenever the laboratory is
contacted for resi-thi iittals or clarification.
Complete the evidence audit according to the following
protocol:
1. Inspect the package for custody seals and follow
the protocol outlined in the CSF Tracking
Procedure. Alter completing the appropriate
sections of tile CS? Rsc.ipt/Tran fer Form, proceed
with the evidence audit.
2. Locate the CS? Inventory Sheet, DC-2 Form,
submitted by the laboratory. Make one photocopy
of this DC-2 Porn to perform the evidence audit.
At the top of the first page, label the photocopy
“Evidence Audit Photocopy”. The original DC-2
Porn submitted by the laboratory must remain with
the CS?, unmodified.
If the DC-2 Porn is flat included with tile CS?,
contact the laboratory for submittal and complete
1—1—03—01 6
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a telephone communication log. Resubmjttal of
just the DC-2 Form is not reaujred to be under
custody seal. Proceed with the evidence audit
after the DC-2 Form has been submitted by the
laboratory and photocopied by the Prime Contractor
Auditor/ Val.idatcr.
3. Review the documents in the CSF. Compare the
document page numbers to the page numbers listed
on the DC-2 Form. Ensure that all documents are
accounted for and legible. If extra pages were
included with the CSF but were flot listed on the
DC-2 Form, or if page numbers listed on the DC-2
Form were incorrect, recuest that a corrected DC-2
Form be su.bmitted. Complete a telephone
ccunication log.
4. For items 1—27 on the DC-2 Form, if the
information is accurate and legible, place a check
in the EPA column for those items.
If any pages are missing, inaccurate, or
illegible, do not put a check in the EPA column.
Request resubm.ittal of the pages from the
laboratory and complete a telephone Communication
log.
S. For item 28, check whether the traffic report is
present. If no, leave EPA column blank, request
resubmitta]. of the pages from the laboratory and
complete a telephone communication log.
Check whether the traffic report was signed and
dated. If yes, place a check in the EPA column.
If no, leave EPA column blank and indicate the
non-compliance directly next to item 28 n the DC-
2 Porm. Do not request a laboratory resubmittal
of the traffic report if it was present but not
signed or dated.
6. Proceed to ‘item 29. Check whether airbills, chain
of custody records, sample tags, sample log-in
sheets (DC-i Form and/or lab form), and the SDG
cover sheet are present. If no, leave EPA column
blank, request resuh j taj from the laboratory,
and complete a telephone cOmmunication log.
Check whether the airbilis, chain of custody
records and SDG cover sheets were signed and
1—1—03—0]. 7
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dated. If yes, place a check in tj EPA
If no, leave EPA column blank and indicate the
non—compliance directly next t item 29 on the C-
2 Yor . Do not recuesc laboratory resubmittals of
these documents if they were resent but not
signed and dated.
Check whether the sample log-in sheet/ DC-i Fora
are complete and accurate. If yes, place a check
in the EPA column. If no, leave EPA column bl ’Jc
and indicate the non—compliance directly next to
item 29 on the C—2 Term. Do not request
laboratory resubmittals of these documents i they
were present but not complete or accurate.
7. Items 30, 31, and 32 concern laboratory
documentation including aiscellaneous
shipping/receiving records, telephone logs,
internal laboratory sample transfer/ tracking
sheets, and sample preparation and analysis
records. confirm that EPA samle numbers, S G
numbers, and Case numbers are correctly referenced
to this particular Case and. SDG on all documents
suhmitted by the laboratory. If yes, place a
check in the EPA columns. If no, leave EPA
columns blank, request that the laboratory
resubmit the correct documents and complete a
telephone co=unicaticn lag.
8. If there are documents listed in item ,
that EPA sample numbers, SDG numbers, and. Case
numbers are correctly referenced to this
particular Case and SDG on all documents s1th tted
by the laboratory. If yes, place a check in the
EPA col” n . If no, leave EPA calumn blank,
request that the laboratory resub t the correct
documents, and complete a telephone communication
log.
9. The evidence auditor should sign the “Audited by 1 ’
section at the bottom of each photoccoied C-2
Perm. The evidence auditor’ s printed name, title,
and date should also be completed. In addition,
the evidence auditor should indicate their company
name/contract below the “Printed &ame/Title ” line.
10. Since resubmittals may be requested during
validation, hold all DC-2 Porms until the data
validation is complete before proceeding with the
1—1—03—01 8
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distribution of the forms.
Li. When requested resuiinittals and new DC-2 Form are
received from the laboratory, make a phot:copy of
the new DC-2 Form. At the top of the first page,
label the photocopy “Evidence Audit Photo py”.
The original DC-2 Form submitted by the laboratory
must remain with the CSF, unmodified. Perform the
evidence audit for the resubmitted sections on the
photocopy of the new DC-2 Form. The column on the
photocopied DC-2 Form for the original data
package, which was left blank during the evidence
audit pending resubmittals, remains blank.
4.3 Organic Completeness Evidence Audit
The following describes the Region I guidelines for
conducting completeness evidence audits of organic C Fs. The
C P will be shipped to the Prime Contractor Lead Chemist by
the RSCC. A CSP Receipt/ Transfer Form, initiated by the
SCC, will be shipped with the CS?.
The Prime Contractor Auditor/Valjdator will perform the
evidence audit using a photocopy of each comnleted and signed
DC-2 Form which is subm .tted by the laboratory as part of the
CSF or which is submitted with resubmitted documents. The
Prime Contractor Auditor/Valjdator must not writs on the
original DC-2 Form which will remain unmodified with the CSF.
When resubmittals are requested, the Prime Contractor
Auditor/Validator should request the laboratory to number the
resubmitted pages so that they may be appended to the end of
the CS?. Pages should not be inserted into the CS? and
original pages in the CS? should not be replaced by
resubmitted pages.
When the laboratory resubmittals are received, photocp y
the new DC-2 Form arid perform the evidence audit for the
resttb ittad sections only. The Prime Contractor
Auditor/Va].idator must not write on the original DC-2 Form
which will remain with the CS?, unmodified.
The Prime Contractor Auditor/Validator must generate
telephone counication logs whenever the laboratory is
contacted for resubmittals or clarification.
1—1—03—01 9
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Complete the evidence audit according to the following
protocol:
1.. Inspect the package for custody seals and follow
the protocol outlined in the CSF Tracking
Procedure. After completing the appropriate
sections at the CSP Recei.pt/Traflsfer Form, proceed
with the evidence audit.
2. Locate the CS ’ Inventory Sheet, DC-2 Form,
submitted by the laboratory. Malcé one photococy
of this DC—2 Form to perform the evidence audit.
At the top of the first page, label the photocopy
?lEvidence Audit Photocopy 11 . The original DC-2
Form su.bmitted by the laboratory must remain with
the CSF, unmodified.
If the DC-2 Form is not included with the CSF,
contact the laboratory for sub ittal and complete
a telephone cotiriication log. Resubmittal of
just the C—2 Form is not required to be under
custody seal. Proceed with the evidence audit
after the DC-2 Form has been submitted by the
laboratory and photocopied by the Prime Contractor
Auditor/Va lidator.
3. Review the dccents in the CSF. Compare the
document numbers to the page numbers listed on the
DC’-2 Form. Ensure that all documents are
accounted f or arid legible.
If extra pages were included with the CSF but were
not listed on the DC-2 Form, or it page numbers
listed on the DC-2 Form were incorrect, request
that a corrected C-2 Form be s tittad. Com lete
a telephone ccunicatiofl log.
4 • For items 2, 4, 5, and 6 on the DC 2 Form, if the
information is accurate and legible, place a check
in the EPA column for those items.
If any pages are missing, inaccurate, or
illegible, do not check off the EPA column.
Request resubmittals from the laboratory and
complete a telephone communication log.
5. For item 3, check whether the traffic report is
present. If no, leave EPA column blank, request
resubmittal of the form, and complete a telephone
courzication log.
1—1—03—01 10
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Check whether the traffic retort was signed and
dated. If yes, place a check in the EPA column.
If no, leave the EPA column blank and indicate the
non-compliance directly next to item 3 or the DC-2
Porm. Do not request a laboratory resubmittal of
the traffic retort if it was present but not
signed or dated.
6. Item 7 concerns laboratory documentation including
internal laboratory sample transfer/tracking
sheets, sample preparation and analysis logbook
pages, screening records, and all instrumeiit
output, including strip charts from screening
activities. Confirm that EPA sample numbers, SDG
numbers, and Case numbers are correctly referenced
to this particular Case and SDG on al]. documents
submitted by the laboratory. If yes, place a
check in the EPA co luiuns. If no, leave the EPA
column blank, request that the laboratory resubmit
the correct documents, and comlete a telephone
counication log.
7. Proceed to item 8. Check whether airbills, chain
of custody records, sample tags, sample log—in
sheets (DC-i Form and/or lab form), the SOG cover
sheet, and miscellaneous sb.ipping/recajvjng
records are present. If no, leave the EPA column
blank, request re.submittals from the laboratory,
and complete a telephone coiuinunicatjon log.
Check whether the airbills, chain of custody
records and SCG cover sheets were signed and
dated. If yes, place a check in the EPA column.
If no, leave EPA column blank and indicate the
non—compliance directly next to item 8 on the DC-2
Form. Do not request laboratory resubmittals of
these documents i.e they were present but not
signed and dated.
Check whether the sample log-in sheet/DC- i Form
are complete and accurate. If yes, place a check
in the EPA column. If no, leave EPA column blank
and indicate the non-compliance directly next to
item 8 on the DC—2 Term. Do not request
laboratory resubmittais of these documents if they
were present but not complete or accurate.
8. Item 9 lists all internal laboratory sample
transfer records and tracking sheets. Confirm
1—1—03—01 11
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that EPA sample numbers, SDG numbers, and Case
numbers are correctly referenced by the
laboratory. If yes, place a check in the EPA
columns. If no, leave EPA columns blanjc, recuest
resubmittals from the laboratory, and comujete a
telephone communicat.cn log.
9. If there are documents listed in item 10, confirm
that EPA sample numbers, SOG numbers, and Case
numbers are correctly referenced to this
particular Case and SOG on all documents submitted
by the laboratory. If yes, place a check in the
EPA columns. If no, leave EPA columns blank,
request resubmittals from the laboratory, and
complete a telephone communication log.
10. The evidence auditor should sign the “Audited by”
section at the bottom of eac i photocopied DC—2
Porm. The evidence auditor’s printed name, title,
and date should also be completed. In addition,
the evidence auditor should indicate their com any
name/contract below the “Printed Name/Tjtlels line.
11. Since resubm.jttals may be requested during
validation, hold all DC-2 Porms until the data
validation is complete before proceeding with the
distribution of the forms.
12. When requested resnF imittals and new DC-2 Porm are
received from the laboratory, make a photocopy of
the new DC-2 Porn. At the top of the first page,
label the photocopy “Evidence Audit Photoco y”.
The original DC-2 Porn submitted by the laboratory
must remain with the CSP, unmodified. Perform the
evidence audit f or the rest’b ittad sections on the
photocopy of the new DC-2 Porn. The column on the
photocopied DC—2 Porn for the original data
package, which was left blank during the evidence
audit pending resubmittals, remains blank.
5 • 0 POT TIAL PROBL S WITE TEE CSP AUDIT PROCESS
The following is a list of guidelines to aid the auditor
in determining the appropriate action to take when a CSP or
DC-2 deviates from the required format. ‘ples of
situations which would and would not require contacting the
laboratory for resubmittals are also included.
1—1—03-01 12
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5.1 Guidelines for Contacting the Laborato r
The laboratory usz be contacted for any problem that
affects the comoleteness or accuracy or the CSF. For
example:
• If the CS? contains pages identjfie with only a
laboratory identifier, such as a LD S project
number, the laboratory must be contacted. All
pages of the CS? must reference the ZP Case
Number and SDG to maintain data completeness y
pages with only a laboratory or L S project
number must be resubmitted.
• If the laboratory mistakenly indicates “Not
Applicable” fcr an item and it is Obvious that the
item is applicable, i.e. the document is Present
in the CSF, the laboratory must be contacted. For
example, if the laboratory mistakenly indicates
that the airbi.Us are “NA”, then the laboratory
must be contacted and the revised DC—2 Form must
be resubmitted to indicate the exact page number
of the airbills.
• If the DC-2 Form used by the laboratory does not
itemize all pages present in the CS , the
laboratory must be contacted. The laboratory may
use their own version of the DC-2 Form as long as
all items/pages are listed. If the DC—2 Form does
not accurately reflect the concexita of the CSF,
then the laboratory must resubmit the DC-2 Form.
• If the laboratory submits photocopied
documentation instead of original documentation,
and if the location of the originals is not noted
on each photocopy, then the laboratory must be
contacted. The entire CSF must be suhmjtt with
all, original documentation, or the location of the
originals must be noted on each photocopy.
For example, sample tags and air bills must be
original documentation. Sample preparation logs
and standard preParation , which are usually
in bound logbooks, may be photocopjeg.
5.2 Guidelines for Not Contacting the Laboratory
The laboratory does not need to be contacted if problems
1—1—03—01 13
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do not affect the completeness or accuracy of the CSF. For
examDle:
• U the laboratory uses a different DC-2 Form than
the one included in the Region I procram (i.e.
individual items on the DC-2 Form have slightly
different headers than those on the CLP forms),
the laboratory does not need to be contacted. As
long as all documents are accurately
inventoried on the laboratory DC-2 Form and the
DC-2 Form accurately reflects the contents of the
CSF, then the
laboratory does not need to be contacted.
• If the Traffic Report includes the Chain of
Custody form, as is the case with the new Traffic
Reports, the laboratory does not need to be
contacted. The laboratory may list then
individually. The duplication of page numbers is
inevitable.
• If the laboratory has inserted resubmitted pages
into the CSP, the laboratory does not need to be
contacted. The laboratory has the option to add
the requested resubmittals in an addendum, insert
additional pages in the package and renumber the
pages or resubmit the page with the original page
number.
• If other inconsistencies are found on the DC-2
Form, but the integrity of the package is not
affected, then comolete the audit and note the
deficiency. For example, some laboratories may
not check each item individually on the DC-2 Form,
but may instead draw a continuous arrow down the
column to indicate that all items were checked.
If, however, an item that is not applicable to the
case is indicated as present by the cOntinuous
arrow, note the inconsistency on the DC-2 Form.
• If the laboratory listed both the original and
photocopied pages of the shipping documents on the
DC-2 Form, the laboratory does not need to be
contacted. The laboratory may have listed the
photocopied documents under the “Traffic Report”
and “EPA Shipping/Receiving Documents” sections
and the original documents under “Other Records”.
As long as the original doCumentation is included
with the CSF, it is not necessary for the
1—1—03-01 14
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laboratory to resubmit the DC-2 Form wi.th the
original documents listed under the “Traffic
Report” and “EPA Shipping/Receiving Documents”
sections.
6.0 CO LETION OF EVD 1CE AUDIT AND DISTRIBUTION OF AUDIT
FOBZ S
The audit is com lete after data validation has been
performed and when aLl. DC—2 Forms have been received and
audited. Even if data validation is performed by a Data
Validation Subcontractor, the Prime Contractor is still
responsthle for obtaining any resubmittals recuir by the
validation and new DC-2 Forms following the protocol outlined
above for CSF tracking and auditing.
The pbotocooied DC-2 Forms completed by the evidence
auditor, the original laboratory—submitted DC-2 Form, and the
CSP Roceipt/Tramsfer Porn should remain with the CSF. The
evidence auditor should make a copy of all DC-2 Forms that
were previously photocopied and completed during the audit
procedure. These copies, along with copies of the telephone
counlcation logs, should be sent to:
Contract Evidence Audit Team (CEAT-TechLaw)
12600 West Colfax Avenue
Suite C—310
Lakawood, Colorado 30215
Attn: Kern Luka, Project Leader
When the validation and evidence audit procedures are
completed, the CSF remains with the Prime Contractor until
contract expiration or until further use of the CSF is
required by Region I.
1—1—03—01 15
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Attachment H
“EPA Region I Performance Evaluation Program Guidance”,
July 1996, Revision
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EPA REGION I
PERFORMANCE EVALUATION PROGRAM GUIDANCE
July 1996
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PREFACE
This document, the EPA Region I Performance Evaluation Program Guidance , July 1996, has
been created to replace in its entirety, the U.S. EPA Region I Performance Evaluation Program
Guidance , February 1995, Update. All documents that reference and/or utilize EPA Region I
Performance Evaluation Program requirements must be revised to reflect these new procedures.
The use of single and/or double blind FE samples helps to ensure that environmental data
collection activities result in the delivery of analytical data of known and documented quality,
suitable for its intended use.
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EPA REGION I
PERFORMANCE EVALUATION PROGRAM GUIDANCE
TABLE OF CONTENTS
1.0 CONTEXT FOR THE PERFORMANCE EVALUATION (PE) PROGRAM .... PE PROGRAM-i
2.0 PURPOSE OF THE PE PROGRAM PE PROGRAM-i
3.0 USE OF PE SAMPLES PE PROGRAM-i
3.1 Superfund Program PE PROGRAM-i
3.1.1 EPA Fund-lead and PRPIFederal Facility
Oversight Projects PE PROGRAM-i
3.1.2 Fund-lead Projects Performed by States
or other Federal Agencies PE PROGRAM-2
3.1.3 Non Fund-lead Projects PE PROGRAM-2
3.1.4 EPA Region I PE Program Requirements for
Superfund Projects PE PROGRAM-2
3.2 Non-Superfund Programs PE PROGRAM-3
4.0 APPLICATION OF PE SAMPLES PE PROGRAM-3
5.0 PLANNING FOR PE SAMPLE USE PE PROGRAM-4
6.0 RESPONSIBILITIES IN THE PE PROGRAM PE PROGRAM-4
6.1 Superfund Program PE PROGRAM-4
6.1.1 EPA-NE Performance Evaluation Chemist PE PROGRAM-4
6.1.2 EPA-NE Data Validation Chemist PE PROGRAM-5
6.1.3 EPA Field Sampling Contractor Lead
Chemists and EPA Field Sampling Personnel PE PROGRAM-S
6.1.4 States and Other Federal Agencies PE PROGRAM-6
6.1.4.1 Fund-lead CLP Projects PE PROGRAM-6
6.1.4.2 Fund-lead Non-CL? Projects PE PROGRAM-6
6.1.5 Non Fund-lead Projects PE PROGRAM-6
6.2 Non-Superfund Programs PE PROGRAM-7
7.0 DETAILED PROCEDU1 S FOR THE PE PROGRAM PE PROGRAM-8
7.1 Superfund Program PE PROGRAM-8
7.2 Non-Superfund Programs PE PROGRAM-9
FIGURE 1 - SUPERFUND PE PROGRAM PROCESS PE PROGRAM-lO
ATTACHMENT 1 - EPA REGION I PERFORMANCE EVALUATION
SAMPLES (7/96 Update) Aft. 1-1
ATI’ACHMENT 2- EPA REGION I PERFORMANCE EVALUATION AND
STANDARD REFERENCE MATERIALS VENDOR’S LIST Aft. 2-1
ATTACHMENT 3 - EPA REGION I PERFORMANCE EVALUATION (PE)
SAMPLE REQUEST FORM AU. 3-1
TOC-1 7/96
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1.0 CONTEXT FOR THE PERFORMANCE EVALUATION (PE) PROGRAM
This guidance provides the details on how to implement the EPA Region I PE Program requirements
supporting the data quality system described in the Region I, EPA-NE Data Validation Functional
Guidelines for Evaluating Environmental Analyses , Part 1, dated July 1996 or most recent revision. The
use of single and/or double blind PE samples helps to ensure that environmental data collection activities
result in the delivery of analytical data of known and documented quality, suitable for its intended use.
2.0 PURPOSE OF THE PE PROGRAM
The EPA Region I PE Program serves three major functions:
1. To identify a community of technically capable laboratories during laboratory pre-award
evaluations,
2. To evaluate the performance of analytical laboratories over a period of time,
3. To provide information on a laboratory’s ability to accurately identify and quantitate
analytes of interest during the period of sample preparation and analysis.
In the third function, the EPA Region I PE Program works in conjunction with the tiered data validation
approach that is described in the Region I. EPA-NE Data Validation Functional Guidelines for Evaluating
Environmental Analyses .
3.0 USE OF PE SAMPLES
3.1 Superfünd Program
The EPA Region I PE Program applies to all Superfund fixed laboratory, field laboratory (full protocol
analytical methods performed in a mobile or transportable field laboratory), and field screening analyses;
regardless of the mechanism used to obtain analytical services, the funding source for the project, or the
project lead (EPA or non-EPA entity) for the site work.
3.1.1 EPA Fund-lead and PRP/Federal Facility Oversight Projects
For EPA Fund-lead and PRPlFederal Facility Oversight Superfluid projects, the EPA Region I
PE Program applies to all analytical services obtained through Contract Laboratory Program
(CLP) and non-CLP vehicles. Non-CLP vehicles include fixed laboratory, field laboratory and
field screening analytical services provided directly by EPA or by EPA prime contractors and/or
subcontractors under the Delivery of Analytical Services (DAS) mechanism. EPA-provided PE
samples, which meet project Data Quality Objectives (DQOs), should be utilized when available
as described in Section 4.0 of this guidance document. If appropriate PE samples meeting project
DQOs are not available from EPA, then they should be obtained from commercial vendors.
PE PROGRAM-i 7/96
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3.1.2 Fund-lead Projects Performed by States or other Federal Agencies
For Fund-lead projects performed by States (under Cooperative Agreements) or other Federal
Agencies (under Interagency Agreements) that utilize the CLP to obtain analytical services, EPA-
provided PE samples should be utilized. When non-CL? vehicles are utilized to provide fixed
laboratory, field laboratory, or field screening analytical services for these Superfund projects,
then PE samples should be obtained from commercial vendors.
3.1.3 Non Fund-lead Projects
For Non Fund-lead Superfund projects undertaken by Potentially Responsible Parties (PRPs) or
other Federal Agencies, the EPA Region I PE Program applies to all fixed laboratory, field
laboratory, and field screening analytical services utilized for these projects. Appropriate PE
samples meeting project DQOs must be utilized whenever environmental samples are collected.
These PE samples are not generally available from EPA and should be obtained from commercial
vendors.
3.1.4 EPA Region I PE Program Requirements for Superfund Projects
The following EPA Region I PE Program requirements apply to all Superfund projects:
• One single or double blind PE sample should be used for each sample matrix, analysis
parameter, and concentration level for each Sample Delivery Group (SDG) that is sent
to a laboratory. An SDG is defined as a group of 20 or fewer field samples within a
project, received over a period of up to 14 calendar days. The PE samples should be
counted as field samples in the 20 sample SDG total.
• PE samples are required for all analytical testing when they are available from EPA or
commercial vendors in the appropriate matrix and at the proper concentration level.
Additionally, PE samples should contain as many target analytes as possible, but they
must contain at least one of the target analytes, preferably a contaminant of concern at
the site.
• For soil/sediment/solid sampling events, it is not necessary to include an aqueous PE
sample when the only aqueous samples are equipment and/or trip blanks and when a PE
sample exists (from either EPA or a commercial vendor) for the soil/sediment/solid
samples. However, an aqueous PE sample should be included with soillsediment/solid
samples when a soil/sediment/solid PE sample (from either EPA or a commercial vendor)
does not exist for that analysis parameter.
The EPA-NE Data Validation (DV) Chemist should be contacted (as per Section 6.1.2) to obtain
advice on identifying available commercial vendors of PE samples and choosing a proper PE
sample.
PE PROGRAM-2 7/96
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3.2 Non-Superfund Programs
The EPA Region I QA Unit recommends that Non-Superfund programs utilize PE samples whenever
enviroruriental samples are collected. These PE samples are not available from EPA and should be
obtained from commercial vendors. This recommendation applies to environmental sampling performed
by EPA (OEME, OEP, etc.) and non-EPA entities (facilities, manufacturers, generators, States, other
Federal Agencies, etc.) in support of Non-Superfurid federal regulations such as RCRA, UST, CWA,
NPDES, CAA, TSCA, FIFRA, etc.
The following PE Program requirements apply to all Non-Superfund projects:
S One single or double blind PE sample should be used for each sample matrix, analysis
parameter, and concentration level for each Sample Delivery Group (SDG) that is sent
to a laboratory. An SDG is defined as a group of 20 or fewer field samples within a
project, received over a period of up to 14 calendar days. The PE samples should be
counted as field samples in the 20 sample SDG total.
• PE samples are required for all analytical testing when they are available from
commercial vendors in the appropriate matrix and at the proper concentration level.
Additionally, PE samples should contain as many target analytes as possible, but they
must contain at least one of the target anaiytes, preferably a contaminant of concern at
the site.
• For soil/sediment/solid sampling events, it is not necessary to include an aqueous PE
sample when the only aqueous samples are equipment and/or trip blanks and when a PE
sample exists from a commercial vendor for the soil/sediment/solid samples. However,
an aqueous PE sample should be included with soil/sediment/solid samples when a
soil/sediment/solid PE sample does not exist for that analysis parameter.
The EPA-NE DV Chemist should be contacted (as per Section 6.1.2) to obtain advice on identif ’ing
available commercial vendors of PE samples and choosing a proper PE sample.
4.0 APPLICATION OF PE SAMPLES
Attachment 1 provides a list of EPA-provided PE samples that are currently available through the Region
I QA Unit for Fund-lead and PRP/Federal Facility Oversight Superfund work. Included for each PE
material on the list is an example of an analytical application. Use of the PE samples is NOT limited
to the example application. For instance, #90-001 or #95-001, LowfMedium Volatiles in Water, could
be used for analysis by the CLP OLMO3. 1 Statement of Work, SW-846 method 8260, 40 CFR method
624, etc. Note that several catalogue numbers may exist for a particular method description and matrix.
Generally, different catalogue numbers for a specific method description and matrix contain different
analyte mixes and/or concentrations.
Note also that #90-005, metals in soil PE samples, now contain mercury plus the other metals. However,
one bottle does not contain enough soil to carry out both mercury and metals preparation and analysis.
If both analyses are to be performed on the soil, then two bottles of #90-005 must be requested when
ordering.
PE PROGRAM-3 7/96
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If an aqueous PE sample is needed for mercury analysis, then #95-004 must be ordered since the aqueous
#90-004 PE samples contain metals but do not contain mercury.
A list of PE samples that are available from commercial vendors is provided in Attachment 2 for use in
Fund-lead Superfund projects, for Non Fund-lead Superfluid projects, as well as for Non-Superfluid
projects. Tables I and II list the parameters and matrices for which various vendors can supply PE
samples and Standard Reference Materials (SRMs), respectively. SRMs can be utilized as PE samples.
Table LU provides vendor telephone and telefax numbers. Individual vendors should be contacted directly
to obtain current catalogue information. Current catalogue information must be consulted to ensure that
particular PE samples will meet project DQOs for specific compounds/parameters, matrices and
concentration levels. The list provided in Attachment 2 is not inclusive of all potential PE/SRM vendors
and does not constitute an endorsement by EPA of any particular vendor or any specific PE sample. It
is provided solely for reference in identi ing potential commercial PE sample sources.
5•O: PLANNING FOR PE SAMPLE USE
The use of PE samples should be stipulated as an analytical Quality Control measure during the planning
stage of each project. The utilization of PE samples in accordance with this guidance document, the A
Region I Performance Evaluation Program Guidance , dated July 1996 or most recent revision, should be
stipulated in every DQO Sitmm iry Form, Quality Assurance Project Plan (QAPJP) and/or Sampling
and Analysis Plan (SAP) along with the frequency, analysis parameters, matrices, and concentration
levels for which a FE sample will be used. The origin of the FE sample (EPA-provided or commercial
vendor) should also be documented in the QAPJP and/or SAP.
Additionally, preparation and analysis of FE samples must be written into laboratory Technical
Specifications as a QC requirement when obtaining analytical services from fixed and/or field
laboratories.
PE samples are to be included in the sample count per SDG for CLP and DAS analyses, as well as any
other analytical services mechanism. For example, 20 field samples and one equipment blank (for a
specified concentration level, matrix, and analysis parameter) would require two SDGs and therefore two
PE samples for a total of 23 samples.
6.0 RESPONSIBILITIES IN IKE PE PROGRAM
6.1 Superfund Program
Figure 1 contains a flow chart that outlines the process, roles/responsibilities, and time frames for
planning, obtaining, analyzing, scoring, and evaluating results for EPA-provided and commercial PE
samples used in Superfluid projects.
6.1.1 EPA-NE Performance Evaluation Chemist
The Performance Evaluation (PE) Chemist of the Region I Quality Assurance Unit (telephone #
617/860-4630, telefax # 617/860-4397) is responsible for the following activities:
• Providing a current list of EPA PE samples upon request,
PE PROGRAM-4 7/96
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• Supplying EPA PE samples to EPA Field Sampling Contractor Lead Chemists and EPA
Field Sampling Personnel,
• Scoring analytical results for the EPA PE samples,
• Providing EPA PE sample score results to EPA Field Sampling Contractor Lead
Chemists and EPA Field Sampling Personnel.
6.1.2 EPA-NE Data Validation Chemist
The EPA-NE Data Validation (DV) Chemist of the Region I Quality Assurance Unit (telephone
# 617/860-4634) is responsible for the following activities:
• Tracking EPA PE samples and their analytical results,
• Notifying EPA Field Sampling Contractor Lead Chemists and EPA Field Sampling
Personnel when EPA PE sample score results indicate laboratory performance problems,
• Trending laboratory performance based upon EPA PE sample score results,
• Providing advice on identifying commercial vendors of PE samples, choosing a proper
PE sample, and evaluating resultant data quality.
6.1.3 EPA Field Sampling Contractor Lead Chemists and EPA Field Sampling Personnel
EPA Field Sampling Contractor Lead Chemists and EPA Field Sampling Personnel are
responsible for the following activities (when CLP and/or non-CLP vehicles are used to obtain
analytical services for EPA Fund-lead and PRP/Federal Facility Oversight projects):
• Determining PE sample needs during the project planning phase (scoping meetings, DQO
Summary Forms, Quality Assurance Project Plans and/or Sampling and Analysis Plans),
• Identifying PE sample sources (EPA and commercial),
• Procuring commercial PE samples if necessary,
• Obtaining EPA PE samples from the EPA-NE PE Chemist according to the procedures
outlined in Section 7.0 of this guidance document,
• Ensuring that every laboratory which is analyzing project samples receives and analyzes
appropriate PE samples according to the frequency requirements described in Section 3.0
of this guidance document,
• Obtaining score results for EPA and/or commercial PE samples,
• Evaluating PE sample score results in accordance with the most recent revision of the
Region I, EPA-NE Data Validation Functional Guidelines for Evaluating Environmental
Analyses , and including a discussion of the PE sample score results in Tier I Validation
Cover Letters and Tier 111111 Data Validation Reports,
PE PROGRAM-S 7/96
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• Notifying the EPA-NE DV Chemist if EPA PE sample performance causes reduced
payment or rejection of any CL? data.
6.1.4 States and Other Federal Agencies
6.1.4.1 Fund-lead CLP Projects
For Fund-lead projects performed by States or other Federal Agencies that utilize the
CL? to obtain analytical services, the States and other Federal Agencies are responsible
for performing the activities described in Section 6.1.3 of this guidance document.
6.1.4.2 Fund-lead Non-CLP Projects
When non-CL? vehicles are utilized for these projects (and, therefore, commercial PE
samples must be used), then States or other Federal Agencies are responsible for the
following activities:
• Determining PE sample needs during the project planning phase (scoping
meetings, DQO Summary Forms, Quality Assurance Project Plans and/or
Sampling and Analysis Plans),
• Identifying commercial PE sample sources,
• Procuring commercial PE samples,
• Ensuring that every laboratory which is analyzing project samples receives and
analyzes appropriate commercial PE samples according to the frequency
requirements described in Section 3.0 of this guidance document,
• Obtaining score results for commercial PE samples,
• Evaluating commercial PE sample score results in accordance with the most
recent revision of the Region 1. EPA-NE Data Validation Functional Guidelines
for Evaluating Environmental Analyses , and including a discussion of the PE
sample score results in Tier I Validation Cover Letters and Tier H/Ill Data
Validation Reports.
6.1.5 Non Fund-lead Projects
For Non Fund-lead Superfund projects undertaken by PRPs or other Federal Agencies, the PRP
or other Federal Agency is responsible for the following activities:
• Determining PE sample needs during the project planning phase (scoping meetings, DQO
Summary Forms, Quality Assurance Project Plans and/or Sampling and Analysis Plans),
• Identifying commercial PE sample sources,
PE PROGRAM-6 7/96
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• Procuring commercial PE samples,
• Ensuring that every laboratory which is analyzing project sampies receives and analyzes
appropriate commercial FE samples according to the frequency requirements described
in Section 3.0 of this guidance document,
• Obtaining score results for commercial PE samples,
• Evaluating commercial PE sample score results in accordance with the most recent
revision of the Region 1. EPA-NE Data Validation Functional Guidelines for Evaluating
Environmental Analyses , and including a discussion of the FE sample score results in
Tier I Validation Cover Letters and Tier 111111 Data Validation Reports.
6.2 Non-Superfund Programs
EPA Site Managers and EPA Project Officers are responsible for ensuring that the EPA Region I PE
Program requirements contained in Sections 3.0 through 5.0 of this guidance document are applied to
environmental sampling performed by EPA (OEME, OEP, etc.) and non-EPA entities (facilities,
manufacturers, generators, States, other Federal Agencies, etc.) in support of Non-Superfund federal
regulations within EPA Region I.
The EPA or non-EPA entity performing sampling is responsible for:
• Determining PE sample needs during the project planning phase (scoping meetings, DQO
Summary Forms, Quality Assurance Project Plans and/or Sampling and Analysis Plans),
• Identifying commercial PE sample sources,
• Procuring commercial PE samples,
• Ensuring that every laboratory which is analyzing project samples receives and analyzes
appropriate commercial PE samples according to the frequency requirements described
in Section 3.0 of this guidance document,
• Obtaining score results for commercial PE samples,
• Evaluating commercial PE sample score results in accordance with the most recent
revision of the Region I. EPA-NE Data Validation Functional Guidelines for Evaluating
Environmental Analyses , and including a discussion of the PE sample score results in
Tier I Validation Cover Letters and Tier H/Ill Data Validation Reports.
The EPA-NE DV Chemist should be contacted (as per Section 6.1.2) to obtain advice on identifying
available commercial vendors of FE samples, choosing a proper PE sample, or evaluating resultant
analytical data quality.
PE PROGRAM-7 7/96
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7.0 DETAILED PROCEDURES FOR THE PE PROGRAM
7.1 Superfiind Program
Specific procedures for obtaining and utilizing EPA-provided PE samples for the EPA Region I
Performance Evaluation Program are provided below. These procedures must be followed by EPA Field
Sampling Contractor Lead Chemists and EPA Field Sampling Personnel (whenever CLP and/or non-CLP
vehicles are used to obtain analytical services for EPA Fund-lead and PRPIFederal Facility Oversight
projects) and by States or other Federal Agencies that utilize the CLP to obtain analytical services for
Fund-lead projects.
I. The Lead Chemist (LC) from the EPA Field Sampling Contractor (ARCS, START,
RACS, etc.), State, or other Federal Agency (ACOE, etc.), or the EPA Field Sampling
Personnel (EFSP) telefaxes the EPA Region I PE Sample Request Forms to the EPA-NE
PE Chemist at least one week prior to sampling. In an emergency, PE samples can be
picked up within 24 hours of ordering, but this service cannot be guaranteed. The Lead
Chemist should confirm by phone that the telefaxed request was received by the EPA-NE
PE Chemist.
The EPA Region I PE Sample Request Form must specify the catalogue numbers for
requested PE samples, number of PE samples ordered, method description and applicable
matrix, exact reference titlef# for the analytical method which will be used to prepare and
analyze the PE and field samples, and the requested date and time for pick-up. Any
specific analytes or special concentrations needed for the project must be clearly indicated
on the EPA Region I PE Sample Request Form in the “Required Analyte Concentration”
field. If a specific analyte or special concentration, as requested by the Lead Chemist or
EPA Field Sampling Personnel in the “Required Analyte Concentration” field, cannot be
provided by an existing EPA PE sample, then the EPA-NE PE Chemist will notify the
LC/EFSP by telephone. The LC/EFSP will then determine, based upon project DQOs,
whether an EPA PE sample that does not contain that specific analyte or special
concentration will be sufficient to meet project DQOs or whether a commercial PE
sample will be utilized. Copies of blank and completed EPA Region I PE Sample
Request Forms are provided in Attachment 3.
2. EPA PE samples with preparation instructions are received, verified, and logged out from
the EPA-NE PE Chemist by the Lead Chemist or EPA Field Sampling Personnel at the
pre-arranged date and time. The Lead Chemist or EPA Field Sampling Personnel
ensures that PE samples are handled and stored properly until laboratory receipt.
3. EPA sample numbers are assigned to the EPA PE samples during the sampling episode
by the Lead Chemist (or sampling designee) or EPA Field Sampling Personnel. The
EPA PE ampule numbers must be documented on the Traffic Report/Chain of Custody
Forms to cross-reference EPA sample numbers and EPA PE ampule numbers.
4. The Lead Chemist (or sampling designee) or EPA Field Sampling Personnel then submits
the EPA PE samples, along with the preparation instructi-’ns and field samples, to the
laboratories performing the analytical work.
PE PROGRAM-8 7/96
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5. The laboratories analyze the EPA PE samples along with their respective SDGs of field
samples according to the specified methods. For CL?, the laboratories provide the
resultant data packages to the RSCC. For non-CL?, the laboratories provide the resultant
data packages to the Lead Chemist.
6. When the RSCC submits the CLP data packages to the Lead Chemist or EPA Field
Sampling Personnel, or when the Lead Chemist or EPA Field Sampling Personnel
receives the non-CLP data package from the laboratory, then the Lead Chemist or EPA
Field Sampling Personnel immediately (within 3 business days) telefaxes the EPA PE
sample data (Form Is) to the EPA-NE PE Chemist. The corresponding EPA PE ampule
number (ID#) must be written on the Form Is by the Lead Chemist or EPA Field
Sampling Personnel. The complete analytical method reference (full method name,
number, revision date, etc.) must also be written on the Form Is by the Lead Chemist or
EPA Field Sampling Personnel.
7. The EPA PE Chemist scores the EPA PE data and telefaxes the resuits back to the Lead
Chemist or EPA Field Sampling Personnel, usually within 2 business days.
8. The EPA PE sample score results are evaluated by the Lead Chemist or EPA Field
Sampling Personnel, and the EPA PE sample score results are incorporated into the data
validation process in accordance with the most recent revision of the Region I. EPA-NE
Data Validation Functional Guidelines for Evaluating Environmental Analyses , Part I,
Sections 8.5.3 and 8.5.4. A discussion of the PE sample score results must be provided
in Tier I Validation Cover Letters and Tier 11/Ill Data Validation Reports.
9. If poor performance on the EPA PE sample causes reduced payment or rejection of any
CL? data, the Lead Chemist or EPA Field Sampling Personnel contacts the EPA-NE DV
Chemist to initiate the reduced payment/data rejection process in accordance with the
most recent revision of the Region I. EPA-NE Data Validation Functional Guidelines for
Evaluating Environmental Analyses , Part I. For non-CLP data, the Lead Chemist does
not contact the EPA-NE DV Chemist to initiate the reduced payment/data rejection
process. For situations when resampling is recommended, the Lead Chemist or EPA
Field Sampling Personnel (whichever performed the field sampling) must also contact the
EPA Site Manager by telephone or electronic mail to alert them to the situation.
Similar procedures should be employed for obtaining and utilizing commercial PE samples for Fund-lead
projects performed by States or other Federal Agencies that utilize non-CLP vehicles to obtain analytical
services and for Non Fund-lead Superfund projects undertaken by PRPs or other Federal Agencies.
7.2 Non-Superftmd Programs
EPA Site Managers and EPA Project Officers should establish SOPs for implementing use of PE samples
in their Non-Superfund projects, containing similar activities and roles/responsibilities as described above
for the Superfund Program. SOPs serve to augment the project’s Quality Assurance documentation and
to document project-specific procedures. SOPs are critical to producing environmental data that are
consistent, comparable, credible and defensible.
PE PROGRAM-9 7/96
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FIGURE 1 - SUPERFUND FE PROGRAM PROCESS
Project Defined
by_Stakeholders __________________
Scoping Meeting Held;
Analytical Requirements
Defined by Stakeholders
Lead Chemist(LC)/EPA Field ________________
Sampling Personnel(EFSP)
Determines PE Sample Needs
r LC/EFSP Identifies PE
Sample Sources
(EPA & Commercial)
V
Environmental Analyses
EPA PE Samples Are Received
by the EPA-NE FE Chemist
Within 4 Days of Ordering
LC/EFSP Picks Up EPA FE
Samples From the EPA-NE
FE Chemist at the Pre-arranged
Date and Time
LC/EFSP Ships the PE Samples
Along With the Field Samples _________________________
to the Laboratory
Laboratory Analyzes
PE Samples Along With
The Field Samples
LC/EFSP Notifies
EPA-NE DV Chemist
If EPA PE Sample
Performance Causes
Reduced Payment
or Rejection of
Any CLP Data
LC/EFSP Procures
Non-EPA FE Samples
From Commercial
Vendors If
Necessary
LC/EFSP Sends EPA Region I
FE Sample Request Form
to EPA-NE PE Chemist
1 Week Prior to Sampling
To Order EPA PE Samples
LC/EFSP Includes a
Discussion of the FE Sample
Score Resutts in Tier I
Validation Cover Letters
and Tier Il/Ill DV Reports
EPA FE Samples Are Ordered
by the EPA-NE FE Chemist
On the Same Day That
The Request is Received
LC/EFSP Evaluates the FE
Sample Score Results
in Accordance With
the Most Recent Revision 01
the Region I, EPA-NE Data
Validation Functional
Guidelines for Evaluating
4
PE Sample Score Results Ar
Sent Back to LCIEFSP
Within 2 Days
4
EPA-NE PE Chemist Scores
the EPA PE Results Within
2 Days; EPA-NE DV Chemist
Notifies LCIEFSP If Any FE
Sample Score Results
Are Unacceptable
A
Data Package Sent to LC/EFSP
Within Contract Time Frame
L /EFSP Telefaxes Form Is
to the EPA-NE PE Chemist
For Scoring EPA FE Sample
Within 3 Days
LC/EFSP Obtains Score
Results for Commercial
PE Samples
FE PROGRAM-b
7/96
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ATTACHMENT 1
7/96
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Att.1-1
EPA REGION I PERFORMANCE EVALUATION SAMPLES
(7196 Update)
PARAMETER
CATALOGUE
NUMBER
METHOD DESCRIPTION & MATRIX
APPUCATION
ANIONS
91.006
Low Concentration Anions ui Water
fl )1 & Rev.
METALS
91-004
Low Concentration Metals in Water
ILCOI & Rev.
90-004
Low/Medium Metals in Water (No Mercury)
(Use 95-004 for Mercury)
ILMO4 & Rev.
95.017
ICP/Graphite Furnace Metals (Low/Medium Metals in
Water - No Mercury)
ILMO4 & Rev.
95-004
Low/Medium Mercury in Water
ILMO4 & Rev.
90-005
Low/Medium Metals in Sod (With Mercury)
(Send two bottles when Metals and Mercury are required)
ILMO4 & Rev.
91-007
High Concentration Metals in Soil
HCTh 1
91.008
High Concentration Metals in Soil/Oil
HC IN
91.009
High Concentration Metals in Oil
HC IN
91-010
High Concentration Metals in OdiWater
xcn i
94-020
ICC Industxy Category Metals in Sod Chemical and Allied
Products (Various Levels Available)
ILMO4 & Rev.
94-021
ICC Industry Category Metals in Sod - Primary Metals
Indusines (Various Levels Available)
LLMO4 & Rev.
94-022
ICC Industry Category Metals in Soil - Mining (Various
Levels Available)
ILMO4 & Rev.
94-023
ICC Industry Category Metals in Soil - Recyclers (Various
Levels Available)
ILMO4 & Rev
94-024
ICC Industry Category Metals in Sod- Oilier Waste Facilities
(Various Levels Available)
ILMO4 & Rev.
95-009
ICC Industry Category Metals in Soil - Municipal Landfill
(Various Levels Available)
ILMO4 & Rev.
CYANI1)E
91-005
Low Concentration Cyanide in Water
ILCOI & Rev.
90-006
Low/Medium Cyanide in Water
Uv & Rev.
ASBESTOS
I through 20
Asbestos Materials
EMSLRTP Method
7/96
-------
Aft. 1 -2
EPA REGION I PERFORMANCE EVALUATION SAMPLES
(7/96 Update)
PARAMETER
CATALOGUE
NUMBER
METHOD DESCRIPTION & MATRDC
APPLICATION
VOLAT ILES
91.001
Low Concentradon Volaules in Water
OLCOL. Method 524.2
90-001
Low/Medium VolanJes in Water
OLMO3 & Rev.
95.001
Low/Medium Volatiles in Water
OLMO3 & Rev.
Requezts to OEME
Volaules in Air
.ro. 4, j.p p
SEM]VOLATILES
91-002
Low Conccnu-auon Senuvolat,Jes in Water
OLCO! & Rev.
90.002
Low/Medium Semivotatile in Water
OLMO3 & Rev.
95-002
Low/Medium Seunvolavics in Waxer
- OLMO3 & Rev.
95-010
ICC Indusny Casegoty Organics - General
Manufacniring in Sod (PAHs in High PPM Range)
OLMO3 & Rev.
. -
PESTICIDES/PCBs
91-003
Low Concentration PesncidesIPCBs in Water
- OLCO1 & Rev.
90-003
Low/Medium PesncidesfPCBs in Water
OLMO3 & Rev.
95-003
Low/Medium Pes cides/PCBs in Waxer
OLMO3 & Rev.
91-011
Aroclor 1260 in Sod
OLMO3 & Rev.
91.012
Aroclor 1254 in Soil
OLMO3 & Rev.
91-013
Aroclor 1248 in Sod
OLMO3 & Rev.
7/96
-------
Mt. 1-3
EPA REGION I PERFORMANCE EVALUATION SAMPLES
(7/96 Update)
PARAMEThR
CATALOGUE
NUMBER
METHOD DESCRIPTION & MATRD(
APPLICATION
DIO ’aNS(FTJRMJS’
90-007
2.3,7.8-TCDD Ifl soil (0.1-20 PPB)
GCILP.MS
90-009
PCDD/PCDF in Sods (P1 ’S Range PCDDs/PCDFs For Low Resoludon MS)
GC/LRMS, DFLMO1 & Rev.
92-016
PCDD1PCDF With Interferences in Sod (P1’S Range PCDDsIPCDFs and
Interferences For Low ltcsoluaon MS)
GC/LRMS. DFLMO1 & Rev.
91-014
Interference Fortified Blank Sod (P1’S Range Icte erences For Low
Resolution MS 2.3,7,2-TCDD and/or PCDDIPCDF Analyses)
GCILRMs. DFLMOI & Rev.
91-015
Blank Sod (For Low Resolution MS PCDDIPCDF Analyses)
GC/L.RMS. DFLMOI & Rev.
95-011
PCDD/PCDF in Sods (PPT Range PCDDs/PCDFs For High Resolution MS)
GCIHRMS, Mcthod 16135
95-012
PCDDIPCDF With Interferences in Sod (PPT Range PCDDsIPCDFs wuh
P1’S Range Interferences For High Resolution MS) (Use with 95.013 as
Blank)
GCIHRMS. Method 1613B
95-013
In rference Fortified Blank Sod (P1’S Range Interferences For High
Resolution MS PCDDIPCDF Analyses) (Use with 95-012 as Spike)
GC/HRMS. Method 1613B
95.014
Blank Soil (No PCDDsFPCDFs or Ineerferencea >HRMS QL: For High
Resolution MS PCDDIPCDF Analyses)
GC/HRMS, Method 16135
95.015
PCDDIPCDF in Incinerator Fly Ash (Various Levels Available)
Method 16133 & DFLMOI &
Rev.
95-016
PCDD/PCDF in Envimn-rnen tal ’ Sod (Various Levels Available)
Method
&
Rev.
*DIoxin/Furan Analyses require one Blank (or Interference Fortified Blank). one Spike (or Interference Fortified Spike)
at the appropriate concenti-arion for the uiethod. Noie that blank and spike samples should be chosen so that the blank and
spike pair either contains interferences or does not contain interferences, i.e., a spike containing interferences should not
be paired with a blank that does not contain interferences and vice versa.
7/96
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A V] ACHMENT 2
7/96
-------
EPA REGION I
PERFORMANCE EVALUATION
AND
STANDARD REFERENCE MATERIALS
VENDOR’S LIST
November 13, 1995
Revised November 22, 1995
7/96
-------
TABLE OF CONTENTS
Page
1.0 Introduction Att. 2-1
2.0 Performance Evaluation Samples and Standard Reference Materials Vendor’s List . . Mt. 2-1
3.0 Conclusion Au. 2-1
4 0 References Att. 2-2
LIST OF TABLES
I Performance Evaluation Samples Vendor’s List Att. 2-3 through 2-6
II Standard Reference Material Vendor’s List Att. 2-7 through 2-11
Ill List of PE/SRM Vendors Mt. 2-12
7/96
-------
Att. 2 - 1
1.0 INTRODUCTION
The purpose of this report is to compile information concerning commercial vendors supplying
Performance Evaluation (PE) Samples and Standard Reference Materials (SRM) for environmental
analysis. The format of the report provides quick access to information regarding availability and source
of the PEISRM samples.
2.0 PERFORMANCE EVALUATION SAMPLES AND STANDARD REFERENCE
MATERIALS VENDOR’S LIST
The information regarding commercial vendors who supply Performance Evaluation (PE) samples and
Standard Reference Materials (SRM) was compiled into table format. To provide easy access to
information, the data were classified by major analytical parameters and matrix with the particular
vendor’s name who supplies the described samples/materials. The above information is included in
Tables I and II. Table III contains a list of PE/SRM vendors with their full name, telephone and telefax
numbers.
The PE and SRM data were compiled based on the most current available catalogs (refer to Section 4.0
for details).
3.0 CONCLUSION
Upon review of available PE catalogues, it appears that some parameters/matrices do not have
corresponding PE materials. Only the water matrix (including drinking water) is fWly represented by the
PE samples. Generally, the following matrices or parameters do not have PE samples (for specifics refer
to Table I):
• Tissue - all parameters except dioxin
• Ash - all parameters
• Sediment - all paramexe s
• Pesticides in soil
• Herbicides in soil
7/96
-------
Aft. 2-2
4.0 REFERENCES
1. Analytical Products Group, Inc.: Performance Evaluation and Quality Control Drinking
Water Standards, 1995
2. Analytical Products Group, Inc.: The Quality Assurance Challenge, 1995
3. Cambridge Isotope Laboratories: Environmental Contaminant Standards, 1994-1995
4. Chemcyclopedia, 1994
5. ChemService, 1995
6. Environmental Resource Associates (ERA): Environmental Quality Control Standards,
1995
7. Inorganic Ventures, Inc., 1995
8. National Institute of Standards and Technology (NIST): Standard Reference Materials,
January 1994
9. Resource Technology Corporation (RTC): Standard Environmental Reference Materials,
1994
10. SCQtt Specialty Gases Catalog (Date unknown)
11. SPEX Industries, Inc.: Standards and Products for Inorganic Spectroscopy, 1995
12. ULTRA Scientific Quality Control Standards, 1994
7196
-------
TABLEI Att.2-3
PERFORMANCE EVALUATION SAMPLE VENDOR’S LIST
PARAMETER
MATRIX
NAME OF VENDOR’
DEMAND
(BOO, COD. TOC)
Water
APG. ERA. Inorganic Ventures Inc SPEX. ULTRA Scientific
Wastewater
Iziorganic Ventures Inc.. ULTRA Scientific
NUTRIENTS
Drinking Water
APG, Inorganic Ventures Inc.. ULTRA Scientific
Water
APG. ERA. Inorgazuc Ventures Inc., SPEX. ULTRA Scientific
Wastewater
Inorganic Ventures Inc. • ULTRA Scientific
HARDNESS
Drinking Water
Inorganic Ventures Inc., ULTRA Scientific
Water
ERA. Inorganic Ventures Inc.. ULTRA Scientific
Wastewater
Inorganic Ventures Inc. • ULTRA Scientific
SOLIDS
(TSS, TDS)
Drinking Water
APG. Inorganic Ventures Inc.. ULTRA Sciennfic
Water
APG. ERA. Inorganic Ventures Inc.. ULTRA Scientific
Wastewarer
Inorganic Ventures Inc., ULTRA Scientific
OIL & GREASE
Water
APG. ERA. Inorganic Ventures Inc.. SPEX. ULTRA Scientific
Wascewater
Inorganic Ventures Inc. ULTRA Scientific
MINERALS
Drinking Water
APG. Inorganic Ventures Inc.. ULTRA Scientific
Water
APG, ERA, Inorganic Ventures Inc., SPEX, ULTRA Scientific
Wascewater
Inorganic Ventures Inc.ULTRA Scientific
ANIONS
Water
ERA, SPEX
CATIONS
Water
ERA. Inorganic Ventures Inc., ULTRA Scientific
pH
Drinking Water
APG. ERA. Inorganic Ventures Inc.
Water
APG. ERA, Inorganic Ventures Inc.. SPEX
Wastewater
Inorgan ic Ventures Inc.
TRACE METALS
Dnnking Water
APG. ERA
Water
APG, ERA. Inorganic Ventures Inc.. SPEX, ULTRA Scientific
Wa.scewater
Inorganic Ventures Inc.. ULTRA Scientific
Transformer Oil
ULTRA Scientific
METALS
Drinking Water
Inorganic Ventures Inc.. ULTRA Scientific
Water
APG. ERA. Inorganic Ventures Inc. ULTRA Scientific
Soil
ERA
Sewage Sludge
ERA
7196
-------
TABLEI Att.2-4
PERFORMANCE EVALUATION SAMPLE VENDOR’S LIST
J______________________ MATRIX
J NAME OF VENDOR’
BLANK Sand
Soil
ERA
ERA
Water
APG. ERA. Inorganic Ventures Inc., SPEX, ULTRA Scientific
PHENOLICS
Wastewater
Inorganic Ventures Inc., ULTRA Scientific
CYANIDE Drmiung Water
APG, SPEX. ULTRA Scientific
Water
APG, ERA. Inorganic Ventures Inc., SPEX, ULTRA Scientific
Wastewarer
Inorganic Ventures Inc., ULTRA Sciennflc
Soil
ERA
Transformer Oil
ULTRA Scientific
CHLORINE Drinking Water
Water
Wastewater
APG. Inorganic Vennires Inc., ULTRA Scientific
APO. ERA. Inorganic Ventures Inc., SPEX, ULTRA Scientific
Inorganic Ventures Inc., ULTRA Scientific
Water
SPEX
Drinking Water
APG. ERA, Inorganic Ventures Inc., SPEX, ULTRA Scientific
Water
APG, ERA, Inorganic Ventures Inc., SPEX. ULTRA Scientific
- High Level Water
APO
Water
ERA
Water
APG. SPEX
HALIDES Water
APG. SPEX
CHROMIUM Water
APG
Water
APG
7/96
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TABLE! Att.2-s
PERFORMANCE EVALUATION SAMPLE VENDOR’S LIST
PARAMETER [ MATRIX
NAME OF VENDOR’
TRIHALOMETHANES
Dnnkuig Water
APG. ERA. Inorganic Ventures Inc.. ULTRA Scientific
Water
ERA, Inorganic Ventures Inc., ULTRA Scientific
EDB/DBCP
Dnnking Water
APG, ERA. Inorganic Ventures Inc., ULTRA Scientific
Water
ERA, Inorganic Ventures Inc., ULTRA Scientific
VOLATILES
Dnnking Water
APG, ERA. ChemService, Ultra Scientific
Water
APG, ERA, ChernServicc, Inorganic Ventures Inc.. ULTRA Scientific
Wastewater
ULTRA Scientific
Soil
ERA
Transformer Oil
ULTRA Scientific
VOLATIL.ES BLANK
Sand
ERA
Soil
ERA
ACD EXTRACTABLES
Dnnking Water
Inorganic Ventures Inc.
Water
APG, ERA, Inorganic Ventures Inc.. ULTRA Scientific
BASEJNEUTRAL EXTRACTABLES
Water
APO. ERA. ULTRA Scientific
Wastewater
ULTRA Scientific
SEMIVOLATILES
Drinking Water
APG, ERA. Inorganic Ventures Inc.. ChemService, ULTRA Scientific
Water
APG. ERA. Inorganic Ventures Inc., ChemService, ULTRA Scientific
Soil
ERA
Transformer Oil
ULTRA Scientific
SEMIVOLATILES BLANK
Soil
ERA
PESTICDES
Dnnking Water
APO. ERA. Inorganic Ventures Inc., ULTRA Scientific
Water
APO. ERA. Inorganic Ventures Inc., ULTRA Scientific
Wastewacer
ULTRA Scientific
CHLORDANE
Drinking Water
APG. ERA, Inorganic Ventures Inc., ULTRA Scientific
Water
ERA. Inorganic Ventures Inc.
Wastewater
ULTRA Scientific
HERBICIDES
Dnnking Water
APG. ERA. Inorganic Ventures Inc., ULTRA Scientific
Water
ERA, Inorganic Ventures Inc . ULTRA Scientific
7/96
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TABLEI Att.2-6
PERFORMANCE EVALUATION SAMPLE VENDOR’S LIST
PARAMETER MATRIX
NAME OF VENDOR’
PESTICIDES Drinking Water
Water
APG. ERA. CheinService. Inorganic Ventures inc., ULTRA Sicnñfic
ERA. ChemService. Inorganic Ventures Inc.. ULTRA Sc(ennfjc
TOXAPHENE Drinking Water
APG. ERA. Inorganic Ventures Inc.. ULTRA Scientific
Water
ERA. Inorganic Ventures Inc., ULTRA Sciennflc
Wastewater
ULTRA Scientific
PCBs Drinking Water
APG. ERA. Inorganic Ventures Inc.
Water
APG. ERA. Inorganic Ventures Inc., ULTRA Scientific
Wastewater
ULTRA Scientific
Oil
ERA. ULTRA Scientific
Soil
ERA. Cambridge Isotope Laboratories -.
Fish
Cambridge Isotope Laboratories
SCREENING Dnnking Water
508A)
Wastewater
ULTRA Scientific
ULTRA Scientific
DECACHLOROB [ PHENYL Drinking Water
ERA. APG. ERA
Water
APG. ERA
Water
Cambridge Isotope Laboratories
Soil
Cambridge Isotope Laboratories
Fish
Cambridge Isotope Laboratories
Water
APG, ERA. Inorganic Ventures Inc.. ULTRA Scienufic
Soil
ERA. Inorganic Ventures Inc. -
Water
APG. ERA. Inorganic Ventures Inc.. ULTRA Scientific
Soil
ERA
FUEL Water
Sod
APG. ERA. Inorganic Ventures Inc.. ULTRA Scientific
ERA
HYDROCARBON Water
Soil
APG. ERA. ULTRA Scientific
ERA
MIXTURES Air
Matheson Gas Pmductt. Scott Specialty Gases
1 - Refer to Table III to obtain vendor’s full name, telephone and telefax numbers.
7/96
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TABLE II
STANDARD REFERENCE MATERIAL VENDOR’S LIST
Aft. 2- 7
INORGANICS
ANDARD REFERENCE MATERIAL DESCRIPTION
NAME OF VENDOR’
Parameter
Matrix
LEAD
Fuel
NIST
Soil
NIST
Paint Sludge
RTC
Paint Waste
RTC
Dust
RTC
MERCURY
Water
NIST
Sediment
NIST
VANADIUM
Crude Oil
NIST
VANADIUM & NICKEL
Fuel Oil
NIST
TRACE ELEMENTS
Water
NIST
Coal Fired Industrial Plant Ash
Inorganic Ventures Inc.
Indusmaj Incinerator Ash
Inorganic Ventures Inc.
Municipal Incinerator Ash
Inorganic Ventures Inc.
Dry Soil
Inorganic Ventures Inc.
Diatomaceous Earth Cake
Inorganic Ventures Inc.
Sewage Sludge Amended Soil
Inorganic Ventures Inc.
Paint Sludge
Inorganic Ventures Inc.
Plating Sludge
Inorganic Ventures Inc.
Conwrnnated Water Filter Media
Inorganic Ventures Inc.
Paint Chips
Inorganic Ventures Inc.
Dust
Inorganic Ventures Inc.
METALS
Ashes
RTC
Soils
RTC
Sludges
RTC
Urban Paruculates & Water Filtration Wastes
RTC
7/96
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GENERAL
TABLE II
STANDARD REFERENCE MATERIAL VENDOR’S LIST
Estuarine Sediment
Sargasso
INORGANICS
N F
RTC
Att.2-8
STANDARD REFERENCE MATERIAL DESCRIPTION
NAME OF VENDOR’
Parameter
Matrix
TCLP METALS
Municipal Incinerator Ash
Inorganic Ventores Inc., RTC
Superfund Site Soil
Inorganic Vennires Inc., RTC
Urban Particulate Matter
NEST
Used Pellet Autocatalyst
N1ST
Used Monolith Aucocaialyst
NEST
Simulated Rainwater
NEST
Buffalo River Sediment
NIST -
San Joaquin Sod
NIST
Montana Sod
NEST
Sedtmenis Lake
RTC
Sediments Marine
RTC
Sediments. Stream
RTC
Soils
RTC
Soil. Loam
RTC
Soil. Sandy
RTC
Sewage Sludge
RTC
Fish Tissue
RTC
Tuna Homogenate
RTC
Cod Muscle
RTC
Dogfish Liver
RTC
Fish Tissue, Lyophilized
RTC
Plankton
RTC
7/96
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TABLEEI Att.2-9
STANDARD REFERENCE MATERIAL VENDOR’S LIST
ORGANICS
STANDARD REFERENCE MATERIAL DESCRIPTION
NAME OF VENDOR’
Parameter
Maw ix
PHENOLS IN METHANOL
—
NIST
AROMATIC
HYDROCARBONS!HEXANE, TOLUENE
—
NIST
HALOCARBONS FOR H 1 0
—
NIST
PAils
Sepai tor Sludge
Inorganic Ventures Inc., RTC
Contaminated Sod
Inorganic Ventures Inc.. RTC
Contaminated SoWSediment
Inorganic Ventures Inc., RTC
Coal Tar
NIST
PRIORITY POLLUTANTS PAHs
NIST
NITRATED PAil IN METHANOL
—
NIST
NITROPYRENES IN CH 2 CI 2
—
NEST
CHLORINATED PESflCDESIHEX & jE
—
NIST
CHLORINATED
PESTICIDES/ISOOCTANE
—
NEST
PESTICIDE, LINDANE
—
NIST
PESTICIDE. 4,4’-DDE
—
NIST
PESTICIDE. 4.4’-DDT
—
NEST
PCBSIISOOCTANE
—
NEST
PCBs
Oil
NIST
Transformer Oil
Inorganic Ventures Inc., RTC
Soil
Inorganic Ventures Inc., RTC
Soil/Sediment
Inorganic Ventures Inc.
Human Serum
NEST
River Sediment
NEST
CHLORINATED BIPHENYLS
—
NEST
ISOTOPE LABEL POLLUTANTS
DIOXIN
NEST
NEST
—
7/96
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TABLE II
STANDARD REFERENCE MATERIAL VENDOR’S LIST
Att.2-1O
ORGANICS
STANDARD REFERENCE MATERIAL DESCRIPTION
NAME OF VENDOR’
Parameter
Matrix
GENERAL
Urban Dust
NIST
Diesel Particulate Matter
NIST
Mussel
NIST
Oy5tcr Tissue
N1ST
Shale Oil
NIST
Petroleum Crude CLI
NIST
Copepoda. Dricd!PCBs & Pest
RTC
Fish Tissue, LyophdizedfPCBs & Pest
RTC
Scduncat Hot Spoc!PCBS & Pest
RTC
Tuna Homogenate
RTC
Marine Sedimeet
NLST
Cod Liver Oil
NIST
7/96
-------
TABLEII Att.2-11
STANDARD REFERENCE MATERIAL VENDOR’S LIST
ANALYZED GASES
S1ANDARD REFERENCE MATERIAL DESCRIPTION
VENDORS NAME’
SO 2 Permeation Tube
NIST
NO 2 Permeation Device
NIST
Methane/Air
NIST
Methane + Propane/Air
NIST
S0 2 1N 5
NIST
Propane/Air
NIST
CO/Air
NIST
CO iN 1
NIST
NOIN 2
.
CO 2 . 0 ,/N 2
NIST
Organic Compounds/Nitrogen
Volatile Toxic Organics
NIST
Benzene/Nicrogen
NIST
iizene, To1uene Chiorobeozenc, & Bromobenzene/Nitrogen
NEST
Carbon Tecrachionde, Chloroform, Tctracblorocthylene & Vinyl ChlondelN,
NEST
CO,1N 2 0/Air
NIST
coiio . i r
NIST
C0 1 /N 2
NIST
NO/N 2
NEST
C 3 H ,/N 2
NIST
Oxides of Nitrogen/Air
NEST
0 2 /N 1
NEST
con 2
NEST
IM Gases. 3 Components
NEST
1 - Refer to Table Ill to obtain vendor’s full name, telephone and telefax numbers.
7196
-------
Aft. 2-12
TABLE ifi
LIST OF PEISRM VENDORS
NAME OF VENDOR
SUPPLIES
(PE or SRM)
TELEPHONE
NUMBER
TELEFAX
NUMBER
1. Analytical Products Group. Inc. (APG)
PE
80 0 -2724442
614-423-5588
2. Cambridge Lsotope Laboratories
PE
8003 2 2 .1174
508.749-8000
508-749-2768
3. ChcmService
PE
800-452-9994
610-692-3026
610-692-8729
4 Environmcnral Resource Associates (ERA)
PE
800-372-0122
303-431-8454
303-431-0159
5. Inorganic Ventures, Inc.
PE & SP.M
800-669-6799
908-901-1900
908 .901 . .1903
6. Matheson Gas Products
PE
201-867.4100
201-867-4572
7. National Institute of Standards and Technology (NIST)
SRM
301-975-6776
301-948-3730
8 Resource Technology Corporation (RTC)
PE
307-742-5452
307-745-7936
9. Scoti Specialty Gases
PE
617-245-8707
617-246-5452
10. SPEX Industries, Inc.
PE
800$227739
908.549-7144
9086039647
11. ULTRA Scientific
PE
800-3384754
401.295.2330
7/96
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A11 ACHMENT 3
7/96
-------
EPA REGION I
PERFORMANCE EVALUATION (FE) SAMPLE REQUEST FORM
Date of Request: ________________
Requestor’s Name: ____________
Corporate Name: _______________
Contract Name (if applicable):_
Contract Number (if applicable): —
Telephone Number: _____________
Telefax Number: _______________
Site Name and OU#: __________
Site ID # (CERCLIS, etc.): ______
Site Location: __________________
Sampling Date(s): _______________
Requested Pick-up Date and Time:
PE SAMPLES REQUIRED
CATALOGUE
REQUIRED
NUMBER OF PE
METHOD
ANALYTICAL
NUMBER
ANALYTE
CONCENTRATION
SAMPLES
ORDERED
DESCRIPTION &
MATRIX
METHOD
Au. 3 - 1
7/96
-------
Att. 3-2
Example :
EPA REGION I
PERFORMANCE EVALUATION (PE) SAMPLE REQUEST FORM
Ed Howard
Date of Request: _. L24l96
Requestor’s Name: —
Corporate Name: 3 X
Contract Name (if applicable): ARCS
Contract Number (if applicable): 68-W8- X 0O
Telephone Number: 000-222-Jill _________
Telefax Number:
000-222 2 222
Site Name and OU#: Mac’s Marsh. QU 2
Site ID # (CERCLIS, etc.): MAD000000000
Site Location: Debsville, MA
Sampling Date(s): 7/3/96 and 7/10/96
Requested Pick-up Date and Time:
6/30/96. 1:30 PM
PE SAMPLES REQUIRED
CATALOGUE
NUMBER
REQUIRED
ANALYTE
CONCENTRATION
NUMBER OF PE
SAMPLES
ORDERED
METHOD
DESCRIPTION &
MATRIX
ANALYTICAL
METHOD
90-001 or
95-001
3
L/M VOA in H 2 0
OLMO3 & Rev.
90-002 or
95-002
3
LIM SV in H 2 0
OLMO3 & Rev.
90-003 or
95-003
3
LIM P/P in Ff20
OLMO3 & Rev.
90-005
Arsenic > JO ppm
6
L/M Metals in Soil
ILMO4 & Rev.
7/96
-------
Attachment I
“Standard Operating Procedures for Submitting Data for Reduced Payment!
Data Rejection”, September 9, 1991
-------
ENVIRON}IENTAL SERVICES DIVISION
60 Westview Street, Lexington, NA 02173—3185
MEHORANDUX
: September 9, 1991
SUBJ: Standard Operating Procedures for Submitting Data for Reduced
Payment/Data Rej ection
FROM: Steve Stodola, Region I, Office of Quality Assurance
TO: Lead Chemists, ARC and TES Contractors
THRU: Heidi Horahan, ARC DPO
Several issues have come up recently regarding the submittal of
data for reduced payment/data rejection. Please note the
following:
1) The contact person for these issues is Steve Stodola at 617-
860—4634. If necessary, use the voice mail to leave all the
pertinent information — Case #, SDG #, Laboratory, Contractor
(ARC or TES), Type of action needed reduced, payment or data
rejection.
2) Review the data reduction/reduced payment flow chart and memo
that was handed out at the lead chemist’s meeting last
September(1990). (See attachment.) Specifically, when it is
determined that a package is contractually non-compliant, th.
lead chemist must contact the Region by phone by the end of the
first week (or sooner, if possible). This process is very time
critical because SMO must pay the invoices within 30 days unless
we notify them of a problem.
3) In the Recommendation Letter the lead chemist should not
explicitly state “we recommend reduced payment (or data
rejection)”, since only the TPO can make the actual
recommendation for reduced payment or data rejection. The letter
should state that “the following information and documentation is
provided to the Region to help in your evaluation of this case”.
4) The Recommendation Letter must contain all the items
mentioned in the memo handed out at the lead chemist’s meeting.
See RAS item 6) an .—3A3 item 7-) .
5) The following items must be included with the attachments to
the Recommendation Letter.
a) &? S—Request— 1)/A
b) Case Narrative
c) Traffic Report
d) Chain of Custody
e) Phone Logs
f) Data Validation Worksheets — when appropriate
g) Raw data supporting the claims of noncompliance
-------
TIME LINE
DATA REJECTION/REDUCED PAYMENT OF RAS/SAS EATA/. . , ,
& r gp ctG O
1st Week
2nd Week
2]. days of
EPA stamped
date
Preliminary Review of Data Package indjcateT
Data Is Contractually Noncompliant -
or
Data is Unusable
Decision to
Recommend Rejection
[ Concurrence of RPM 1
Data has Reduced
Value
Decision to
Recc mend Reduced
Payment
**** Call TPO ****
TPO calls SMO to hold invoice
-------
ROUTINE AMALYTI CAL SERVICES-DATA REJECTION/REDUCED PAYMENT
tround -
Prior to the passage of the Amendments of 1988, the Prompt
Payment Act required payment within 30 days of receipt of a valid
invoice and interest payments for late payments. Eowever, the
Agency was granted a 15 day grace period before interest.
penalties were assessed. In October of 1988 the Prompt Payment
Act Amendments were passed which abolished the 15 day grace
period and required automatic interest payments after 30 days
of receipt of .a valid invoice.
What does this Tnean to EPA ?
The data must be rejected or recommended for reduced payment
(referred to as a qualified acceptance) within 30 days of receipt
of a valid invoice. Otherwise, a constructive acceptance of the
data occurs and the invoice is automatically paid when received.
What does this nean to you as a data va].idator ?
It means that in order for you to recover analytical costs for
the RPM on a data package you must submit in writing a letter
detailing the contractual non-compliance of the data package no
later than 21 day after the data package is received by EPA
(stamped date).
RECO 1HENDATION FOR REJECTION/REDUCED PAYMENT FOR RAS DATA
1. Perform preliminary review of the data package within the
first week to determine if data package is contractually
compliant with SOW.
2. Are the data unusable due to contract non-conformities ?
Determine if the entire SDG will be rejected or one
or more fractions. Determine if the RPM has need of
the data even if it is just to document that a sampling
episode occurred. Once the data have been rejected EPA
cannot use then. Obtain verbal concurrence to reject data
from the RPM and document in a telephone log.
Attach a copy of the telephone log to the letter recommending
rejection of data.
3. J oes the data have reduced value because of contractual
non-conformities ? If the data package is non-compliant
but does not warrant rejection, submit recommendation
for reduced payment. It is important at this point
to assess whether or not it is worth pursuing a
reduced payment action.
4. Cal]. the TPO as soon as possible to notify her that
a Data Rejection/Reduced Payment letter is being written.
5. TPO vi] .]. call the SMO Section Leader, Contract Compliance
Screening Group to indicate that Region I may request
Data Rejection/Reduced Payment for the BAS case
and to hold the invoice.
6. Within 21 days of the EPA stamped date write a letter to the
TPO detailing contractual problems with the data package.
-------
Include:
a. CASE and SDG numbers
b. Name of laboratory
c. .Sample numbers
d. Copy of validation memo, if written
e. Parameters of issue,
f Specific references to the SOW by Exhibit, Section
and page number
g. Resolution required (Data Rejection or Reduced
Payment)
h. If recommendation is for rejection, attach all
original data that are being rejected.
1. If recommendation is for reduced payment, attach
copies of supporting documentation.
7. Send the recommendation letter and supporting documentation
in triplicate to the TPO with the original data, if the data
are to be rejected. Do not make copies of the original data
if they a e rejected.
Note: Letters that do not cite specific contractual problems
will not be forwarded by the TPO since non-contractual
technical problems do not constitute reason for non-payment
.by the contracting officer.
8. The TPO will review the recommendation and if she concurs
with it will write a cover letter to the Section leader,
Contract Compliance screening group, with a
REJECTION/REDUCED VALUE COVER SHEET and send it by overnight
delivery to 5110. A copy will be sent to the APO and one kept
on file.
9. While it is the sole responsibility of the Region to reject
or accept the data it remains the APO’s responsibility to
determine payment or non-payment based on our
recommendations.
10. In the case of rejected data, the APO will document in a
memo to the TPO indicating that the decision to reject data
was either approved or not.
If rejected, the entire analytical cost will be recovered
for that sample or sample fraction.
11. In the case of data for reduced payment the APO will
forward the recommendation to the EPA contracting
officer. If the CO concurs with the recommendation she
will negotiate a reduced payment with the laboratory.
The decision to proceed with reduced payment will
be documented in a memo to the TPO.
A Reduced Value report may be obtained for samples
from the contracting office through the APO.
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