United States Office of Emergency and EPA/540/8-89 012
Environmental Protection Remedial Response December 1988
Agency Washington, DC 20460
Superfund
oEPA User's Guide to Contract
Laboratory Program
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EPA/540/8-89/012
December 1988
USER'S GUIDE TO CONTRACT LABORATORY PROGRAM
U.S. Environmental Protection Agency
Library, Room 1670
230 S. Dearborn Street
Chicago, Illinois 60604
U.S. ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF EMERGENCY AND REMEDIAL RESPONSE
401 M STREET SW
Washington, DC 20460
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DISCLAIMER
This document has been subjected to the Environmental Protection
Agency's administrative and peer review and has been approved for publication.
Mention of trade names or commercial products does not constitute endorsement
or recommendation for use.
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FOREWORD
This document has been prepared by the CLP Sample Management Office specifically for the
guidance and direction of program clients. The organic and inorganic analytical program
descriptions herein outline the requirements and analytical procedures of the new CLP
protocols developed from technical caucus recommendations. These protocols were
implemented into CLP analysis contracts in 1987 (inorganic) and 1988 (organic). Other
analytical programs, procedures and documentation described herein reflect the status of the
program as of December 1988. Critical information for CLP samplers and user groups is
contained in Chapter III and Appendix D. This information should be distributed to all
contractors collecting samples for the CLP and to each user group of the EPA and of the
States. For further information on the CLP or to obtain additional copies of the User's Guide,
contact the Sample Management Office at 703/557-2490 or FTS 557-2490.
Fourth Printing
Issued: December 1988
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TABLE OF CONTENTS
Page
CHAPTER I BACKGROUND AND INTRODUCTION 1
A. CLP Objectives and Orientation 2
B. CLP Structure 2
CHAPTER II DESCRIPTION OF ANALYTICAL SERVICES 9
A. Organic Routine Analytical Services 14
B. Inorganic Routine Analytical Services 17
C. Dioxin Routine Analytical Services 21
D. Special Analytical Services 23
E. Analytical Methodology Improvement/Development 27
CHAPTER III UTILIZATION OF ANALYTICAL SERVICES 29
A. Analysis Request Procedures 30
B. Regional Organic/Inorganic Allocation System 36
C. Sample Documentation 36
D. Sample Packaging and Shipment 40
E. Procedures for Problem Resolution 42
CHAPTER IV AUXILIARY SUPPORT SERVICES 45
A. Sample Bottle Repository Program 46
B. Shipment Managment Program 50
C. Environmental Services Assistance Teams 51
D. Information Services 51
E. Enforcement Support 52
F. Cost Recovery Substantiation 54
G. Contract Compliance Screening 56
H. Data Review Services 56
iii
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Page
CHAPTER V LABORATORY SELECTION AND STARTUP. 59
A. Laboratory Selection Process 60
B. Laboratory Startup Process 61
C. Laboratory Performance Evaluation 61
CHAPTER VI PROGRAM QUALITY ASSURANCE 63
A. Laboratory Quality Control Criteria -.... 64
B. Analytical Data Review 66
C. Quarterly Blind Performance Evaluation Samples 68
D. GC/MS Tape Audits 68
E. Onsite Laboratory Evaluations 69
F. Quality Assurance and Data Trend Analysis 70
IV
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INDEX TO APPENDICES
Page
APPENDIX A: LIST OF ACRONYMS A-l
APPENDIX B: CLP DIRECTORY
CLP National Program Office B-l
Sample Management Office B-5
USEPA Regions B-7
Regional Deputy Project Officers B-27
Regional Sample Control Centers B-28
APPENDIX C: RAS DELIVERABLES AND DATA REPORTING FORMS
RAS Organics Delivery Requirements C-l
RAS Organics Data Reporting Forms C-9
RAS Inorganics Delivery Requirements C-47
RAS Inorganics Data Reporting Forms C-53
RAS Dioxin Delivery Requirements C-73
RAS Dioxin Data Reporting Forms C-75
APPENDIX D: SAMPLE INFORMATION AND DOCUMENTATION
Organic Sample Collection Requirements D-l
Inorganic Sample Collection Requirements D-2
Dioxin and High Hazard Sample Collection Requirements D-3
Special Analytical Services Client Request Form D-4
Sample Documentation:
Organic Traffic Report and Completed Example D-9
Inorganic Traffic Report and Completed Example D-ll
Dioxin Shipment Record and Completed Example D-13
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Index to Appendices (cont'd.)
Page
SAS Packing List and Completed Example D-15
Examples of Sample Tag and Custody Seal D-17
Chain of Custody Record and Completed Example D-18
Sample Packaging and Shipment
Sample Packaging Summary D-23
Sample Shipment Coordination Checklist D-24
Potential Problems with Sample Shipment and Analysis D-25
Regional/Laboratory Communication System Telephone Record Log D-26
APPENDIX E: AUXILIARY SUPPORT SERVIES DOCUMENTATION
Regional Backlog Inventory Report E-l
Case File Purge Materials E-3
Cost Recovery Documentation Checklist E-4
Data Review Request Form E-9
Contract Compliance Screening
Organic Screens E-l5
Inorganic Screens E-19
Dioxin Screens E-22
APPENDIX F: REFERENCES
Analytical References F-l
Quality Assurance References F-2
Safety References F-3
Sampling References F-3
Shipping References F-4
VI
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CHAPTER I
BACKGROUND AND INTRODUCTION
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CLP User's Guide Chapter 1
A. CLP Objective and Orientation
The Contract Laboratory Program (CLP) supports the Environmental Protection Agency's
(EPA) Superfund effort, originally under the 1980 Comprehensive Environmental Response,
Compensation, and Liability Act (CERCLA) and presently under the 1986 Superfund
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 CLP
is structured to provide legally defensible analytical results for use in supporting ongoing
Agency enforcement actions or other requirements of the user community. Therefore, a level
of quality assurance and documentation appropriately designed for the intended purposes of
the data has been incorporated into all aspects of program activities.
Client orientation is a key factor in the design and application of all CLP services and
responses. The CLP supplies analytical services in direct response to requests from the EPA
Regions, the primary users of the program. Recently, states and other Agency programs have
also become part of the CLP user community.
The ongoing CLP objective is to develop, manage and improve its analytical programs in
support of all Superfund requirements. This objective is accomplished by continually
increasing analytical capacity and adjusting analytical program requirements and related
support services to better meet Agency needs.
B. CLP Structure
CLP services involve numerous Agency programs, contractors and other groups throughout the
country. These organizations are identified and their role in the program described in the
following sections. The following figure, "Interrelationships of Program Principals," illustrates
the interaction of these groups in CLP operation. In addition, a directory listing addresses and
telephone numbers of key program personnel is located in Appendix B.
1. Program Management
a. National Program Office
The CLP is directed by the National Program Office (NPO), in EPA Headquarter's Analytical
Operations Branch (AOB), Hazardous Site Evaluation Division (HSED), Office of Solid Waste
and Emergency Response (OSWER), located in Washington, DC. The NPO is comprised of the
AOB Branch Chief; National Organics and Inorganics Program Managers; a Regional
Operations Chief; a Quality Assurance Coordinator; and Organics, Inorganics and Dioxin
Technical Project Officers.
NPO responsibilities include: overall management of the CLP in terms of program objectives;
expansion and interface with clients and other groups; policy and budget formation and
implementation; development and administration of CLP analytical and support services
contracts; development and technical review of analytical protocols; review of Special
Analytical Services subcontracts and 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.
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Background and Introduction
December 1988
INTERRELATIONSHIP OF PROGRAM PRINCIPALS
CLP CLIENT/USERS
RSCC
o Analyses Scheduling and Prioritization
REGIONAL
DPOs
o Problem
Resolution
o Contract
Monitoring
Management Reporting!
Program Admin. Supper
SAS Work Assignments!
Contract Status!
RTP
CONTRACTS
o Contract
Procurement
o Contract
Modifications
NATIONAL
PROGRAM
OFFICE/
SAMPLE
MANAGEMENT
OFFICE
o Scheduling
o SAS Contracts
o Contract
Compliance
Screening
o Audit Reports
o Data
o Invoicing
c
EMSL/LV
oQA/QC
o Protocol
Development
o Standards
o QA Data Base
Audit Reports
Lab/Method Performance
Reports
Audit Reports
DATA
SENT
J
NEIC
o Contract
Evidence Audit
Team
o Document Audit
Contractor
CONTRACT LABORATORIES
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CLP User's Guide Chapter 1
The National Organics and Inorganics Program Managers (NPMs), in addition to directing
organics and inorganics section staff, are responsible for the formulation of CLP policies and
direction. By communicating with Regional and Agency communities on a continuing basis,
the NPMs keep all parties apprised of program activities and receive input on program
effectiveness. The NPMs also direct annual technical caucuses for the purpose of reporting
initiatives and progress of the past year.
The Regional Operations Chief directs a staff responsible for the Sample Management Office
contract, the Environmental Services Assistance Teams contracts, the Sample Bottle Repository
contracts, and the Shipment Management contract. In addition, the Regional Operations
Section manages the supply and demand between CLP capacity and client needs, and provides
budget support and administration.
The Quality Assurance (QA) Coordinator manages all aspects of program application of QA
procedures. The QA Coordinator works closely with Office of Research and Development's
Environmental Monitoring Systems Laboratory in Las Vegas (ORD EMSL/LV) in
administering and improving the QA program. The QA Coordinator interacts with the Project
Officers in refining and updating analytical method QA and communicates with the Regions
and other program users to resolve QA issues related to analytical data. For purposes of QA
procedures review and guidance development, the QA coordinator conducts volunteer
workgroups throughout the year.
The Technical Project Officers (POs) are responsible for technical program decisions, contract
monitoring and contractor performance evaluation. On a daily basis, the POs work closely
with the Regional Deputy Project Officers and contract laboratories to resolve technical issues.
The POs also direct the ongoing effort to improve contract language and analytical
methodologies. For the purposes of CLP protocol review and method development, the POs
conduct volunteer workgroups throughout the year.
b. Sample Management Office
The contractor-operated Sample Management Office (SMO) provides management, operations
and administrative support to the CLP. The primary objective of SMO is to facilitate optimal
use of program analytical resources. SMC activities fall into the following areas: 1) sample
scheduling and tracking, 2) Contract Compliance Screening, 3) Special Analytical Services
subcontracting, 4) laboratory invoice processing, 5) maintenance of CLP records and
management reporting, 6) procurement/IFB development and Statement of Work production,
7) coordinating CLP meetings and conferences and 8) NPO management, technical and
administrative support.
SMO routinely 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 nonroutine types of analyses, SMO
subcontracts for Special Analytical Services (SAS), scheduling and tracking for SAS efforts as
outlined above. SMO maintains a comprehensive database of CLP services, performance and
utilization in order to generate a variety of management and user reports.
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Background and Introduction December 1988
c. Office of Research and Development. Environmental Monitoring Systems Laboratory/Las
Vegas
ORD provides program QA support through EMSL/LV. EMSL/LV assists in performing
preaward and postaward onsite laboratory evaluations; prepares performance evaluation (PE)
samples for preaward and postaward evaluations of laboratory performance; evaluates
preaward and postaward PE sample data; performs QA audits on CLP-generated data; and
assists in the evaluation and development of CLP analytical methods and protocols.
Additionally, EMSL/LV 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 Investigations 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 utilized in the CLP to maintain
the validity of sample analyses for supporting Agency enforcement actions. NEIC routinely
performs 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 E.
2. Regional Program Support
The Regions play an integral role in program activities, both as the primary CLP user and as 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 requirements.
a. Regional Deputy Project Officers
In 1984, Regional Administrators appointed a CLP Technical Deputy Project Officer (DPO)
for each Regional office. Under the direction of the NPO, the Regional DPO monitors the
contract laboratories located in the Region. The DPO works closely with the PO in responding
to identified problems in laboratory operations and participating in laboratory onsite
evaluations.
b. Regional Sample Control Centers
In 1984, each Region established a Regional Sample Control Center (RSCC) to centralize
scheduling of CLP sample analyses within the Region. The RSCC is comprised of one or
more individuals with one individual 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. The primary RSCC makes final determinations
regarding Regional analysis priorities when conflicts occur. The RSCC routinely places all
Regional requests for CLP 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.
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CLP User's Guide Chapter 1
c. Regional/Laboratory Communication 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. In this communication system,
designated Regional communication contacts routinely call designated laboratory
communication contacts to resolve technical questions concerning program data. This
communication link also benefits the laboratory by providing direct feedback on its data
product.
3. Clients/Users
a. EPA Regions
The ten EPA Regions are the primary clients of the CLP. As previously described, each
Region has established an RSCC that schedules all Regional CLP analysis requests. The RSCC
balances Regional sampling with allocated numbers of CLP sample analyses available each
month and prioritizes the Region's analytical workload when conflicts occur. RSCC personnel
coordinate closely with SMO throughout Regional sampling events, assisting in tracking sample
shipments to the laboratory and resolving any 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
Under RCRA - CERCLA Cooperative Agreements, any state undertaking initial site
investigations and entering into cooperative agreements with the Government for clean up of
local waste sites can utilize CLP services. States must access CLP analytical services through
the RSCC. Data packages are also distributed to states through the RSCC.
c. NonSuoerfund Clients
Program services are available to support nonSuperfund clients. NonSuperfund analyses and
other support are provided by the CLP through transfer of funds from the nonSuperfund
program to the CLP. NonSuperfund clients currently include other government agencies and
EPA programs, such as the Office of Acid Deposition, the Office of Solid Waste, the Office
of Water, and the Resource Conservation and Recovery Act.
4. Analytical and Support Services Contractors
a. Contract Analytical Laboratories
The CLP's analysis contractors come from the nationwide community of chemical analytical
laboratory facilities. To become part of the CLP, 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 assure compliance with the terms and conditions of the contract. Details of
preaward and postaward evaluations are addressed in Chapter V.
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Background and Introduction December 1988
b. Sample Bottle Repository
In 1982, the NPO established the Superfund Sample Bottle Repository program in order to
provide a common source of clean, quality control tested sample containers for samples
processed through the CLP. The objective of the Repository program is to eliminate the
potential of bottle contamination that would affect the validity of sample data. The
contractor-operated repositories serve as a central source for several types of precleaned
sample containers which are routinely utilized by Regional and contract personnel performing
Superfund sampling activities. Containers are also available through the Repository program
for nonSuperfund sampling activities such as those under the National Surface Water Survey
and the Resource Conservation and Recovery Act. Repository services are detailed in Chapter
IV, Section A.
c. Shipment Management Program
The Shipment Management program was created by the NPO in 1988 to provide a consistent
means of tracking the various shipping accounts established for CLP use. The Shipment
Management Contractor is responsible for establishing, maintaining and monitoring 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 Chapter IV, Section B.
d. Environmental Services Assistance Teams
In 1985, the NPO initiated the concept of Environmental Services Assistance Teams (ESAT) to
provide a wide range of technical, management and other related resource support for
Superfund and nonSuperfund Agency programs. ESAT contractors assist EPA Headquarters
and the Regions in the following task areas: 1) analytical support, 2) data review, 3) logistical
and administrative support, 4) quality assurance/quality control support, 5) management and
reporting, and 6) other task-related activities. ESAT services are detailed in Chapter IV,
Section C.
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CHAPTER II
DESCRIPTION OF ANALYTICAL SERVICES
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CLP User's Guide Chapter 2
The CLP provides routine and specialized analytical services 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 increasing analytical demands of Regional clients, the
CLP has continually expanded its capacity for standardized analyses through frequent contract
solicitations. On the average, the CLP provides over 6,000 sample 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 CLP operates the following analytical programs:
o Organic Routine Analytical Services (RAS),
o Volatile Organic RAS,
o Inorganic RAS,
o Dioxin RAS, and
o Special Analytical Services (SAS).
In the future, many other analytical programs will be included under RAS:
o High Concentration Organics
o High Concentration Inorganics
o Organics Low Concentration (Drinking Water)
o Inorganics Low Concentration (Drinking Water)
o GC/EC Pesticides/Aroclors
o Fast Turnaround GC Screen Organics
o Dioxins/Furans
o ICP/MS (method to be included in Inorganic RAS), and
o Microwave Digestion (method to be included in Inorganic RAS).
Laboratories operating under firm, fixed-price contracts with the EPA provide routine
analytical services to Superfund clients. NonSuperfund clients can also access RAS programs
once special funding arrangements have been made.
The SAS program provides nonstandardized analytical services to Superfund and
nonSuperfund clients for organics, inorganics, dioxin and 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.
The following tables outline the services available under the CLP's RAS and SAS programs.
The client should carefully consider the provisions of each CLP analytical program during the
planning stages of a sampling event to determine the applicability of the analysis to user
needs. For detailed analytical information, users are instructed to consult the Region's Master
Copy Statements of Work under which CLP RAS laboratory contractors operate.
10
-------
Description of Analytical Services
December 1988
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CLP User's Guide Chapter 2
MENU OF SPECIAL ANALYTICAL SERVICES
RAS Plus SAS Category
o Fast Turnaround Analysis by RAS Organic, Inorganic or Dioxin IFB Protocol
o RAS Organic Analysis with Additions/Adjustments to IFB Protocol
o RAS Inorganic Analysis with Additions/Adjustments to IFB Protocol
o RAS Dioxin Analysis with Additions/Adjustments to IFB Protocol
All SAS Category
o Organic Analysis Per Non-RAS Protocols, Matrices, Compounds
o Inorganic Analysis Per Non-RAS Protocols, Matrices, Compounds
o Dioxin Analysis Per Non-RAS Protocols, Matrices, Compounds
o Organic and Inorganic High Concentration Sample Preparation and Analysis
o Special Topics Analysis (As Requested)
NOTE: The client is responsible for designating IFB method adjustments 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. All information must accompany
the client's request for SAS services.
12
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Description of Analytical Services December 1988
Routine analytical services apply to the analysis of water and soil/sediment samples. Samples
for analysis should be single-phase and homogeneous. Sample matrices other than water or
soil/sediment are processed through the SAS program.
Organic and inorganic RAS contract methods determine low to medium concentrations of
organic target compounds and inorganic target analytes, respectively. The sampler identifies
low and medium levels of concentration in the field to determine sample collection volume
and 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 element may comprise
as much as fifteen percent of the total sample, are most often those collected onsite 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.
Required sample volume and container types used for sample collection for RAS analyses are
detailed in the following sections and are illustrated in Appendix D. Cleaned, quality
controlled sample containers are available through the Sample Bottle Repository as described in
Chapter IV, Section A. Containers provided by the Repository 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, whichever occurs first:
o each Case of field samples; or
o each twenty field samples within a Case; or
o each fourteen calendar day 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 financial considerations for late delivery and incentives for early
delivery of the data package. Illegible or incomplete data reports are unacceptable, and the
laboratory must resubmit readable versions of any illegible pages.
The CLP QC program for RAS laboratory analysis is structured to provide consistent results of
known and documented quality. Sample data packages contain QC documentation that allow
an experienced chemist to determine the quality of 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 CLP 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 falling 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.
13
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CLP User's Guide Chapter 2
A. Organic Routine Analytical Services
1. Compounds Identified and Quantified
The organic RAS program identifies and quantifies organic target compounds (VOA, B/N/A
and pesticide/PCB fractions). These compounds are listed on the organic data reporting sheets
in Appendix C.
In addition, the contract laboratory is required to execute a maximum of thirty NBS Mass
Spectral Library searches for compounds not identified on the Target Compound List (TCL).
The ten peaks of greatest apparent concentration in the VOA fraction and the twenty peaks in
the B/N/A fraction are tentatively identified, and the concentration estimated, following a
visual comparison of sample spectra with the nearest library matches. The tentative
identification of non-target organic compounds provides information on potential organic
contaminants outside of the analytical parameters of the RAS program.
2. Volumes Required and Preservation Techniques
For low level organic water samples, a one gallon volume is required for extractables analysis;
80 mL is required for volatiles analysis. The extractables aliquot is collected in two 80-ounce,
four 1-liter, or one 4-liter amber glass bottle(s). The volatiles aliquot is collected in two 40-
mL glass vials. For medium level organic water samples, a four liter volume is required for
extractables analysis; 80 mL is required for volatiles analysis. The extractables aliquot is
collected in four 32-ounce glass jars; the volatiles aliquot is collected in two 40-mL glass vials.
For low/medium level organic soil samples, a six ounce volume is required for extractables
analysis and 240 mL is required for volatiles analysis. The extractables aliquot is collected in
one 8-ounce glass jar, and the volatiles aliquot is collected in two 120-mL glass vials. Water
and soil samples for volatile analysis should be collected so that the containers are completely
filled, leaving no headspace. Because it is not certain whether a sample is actually low or
medium level, samplers should collect volumes as specified for low level samples, but follow
packaging and shipment procedures as prescribed for medium level samples. Packaging and
shipment procedures are detailed in Chapter III, Section D.
Water samples for VOA analysis should be preserved with HCL. No chemical preservation is
necessary for water samples for extractables analysis or for soil samples.
For a laboratory to perform matrix spikes, matrix spike duplicates, and contractual reanalyses,
triple the sample volume is required for at least one sample in twenty of the same
concentration and matrix for each Case. For water samples, one field blank should be
supplied per Case, and one volatile trip blank should be supplied per shipment. No additional
volume is required for duplicate analyses of soil samples. EMSL/LV supplies soil blanks to
the Regions; aqueous blanks must not be used for soil samples. If the sampler does not
provide sufficient volume, analysis of all required parameters and complete QA/QC
determinations may not be possible. If this occurs, SMO will contact the RSCC to determine
appropriate adjustments in analysis.
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Description of Analytical Services December 1988
3. Contract Delivery Requirements
The organic RAS program specifies contractual requirements for sample extraction, volatile
analysis and data reporting. These requirements include:
o Completion of sample extraction for water samples within five days of sample receipt
and for soil samples within ten days of sample receipt;
o Completion of volatile analysis within ten days of sample receipt;
o Completion of extractable analysis and reporting of data within thirty-five days of
sample receipt.
Each organic RAS data package includes the following components:
o Narrative report describing analytical problems encountered and internal QC processes
applied.
o Copies of sample Traffic Reports.
o Quality control summary containing surrogate, method blank, matrix spike and matrix
spike duplicate analyses recoveries, and instrument tuning and performance
information.
o Sample data including tabulated results of the organic target compounds identified
and quantified, and the tentative identification and estimated concentration of up to
thirty non-target organic compounds in greatest apparent concentration reported in
ug/L or mg/kg.
o Raw sample analytical data including sample chromatograms, spectra, quantitation
reports and calculations.
o Standards data package including chromatograms, spectra and data system printouts,
and initial and continuing calibration reports.
o Raw QC data package documenting instrument tuning and analytical QC criteria.
Each organic RAS package submitted to SMO must be accompanied by a diskette which
contains machine readable information. This information must be sufficient to produce all
data on the hard copy summary reporting forms. Explicit formats for diskette records are
specified in the analytical Statement of Work. The organic RAS delivery requirements and
copies of organic data reporting sheets are contained in Appendix C.
4. Analytical Protocols
The standardized organic analytical methods are based on Federal Register (FR) Methods 625
(B/N/A), 608 (pesticide) and 624 (VGA). Analysis for organic target compounds includes an
optional GC screen (to determine appropriate dilution fraction or aliquot sizes for GC/MS
analysis), GC/MS analysis (B/N/A and VGA) and GC/EC analysis (pesticide/PCB).
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CLP User's Guide Chapter 2
a. Water and Soil Methods
Water samples (VOA, B/N/A and pesticide/PCB fractions) are prepared and/or solvent
extracted. Soil samples (B/N/A and pesticide/PCB fractions) are prepared by Bonification
prior to solvent extraction. Extracts are cleaned up using optional column chromatography
techniques when necessary.
Organic target compounds are identified and quantified by GC/MS for VOA and B/N/A
fractions and by GC/EC for the pesticide/PCB fraction. In addition, the twenty highest non-
TCL B/N/A peaks and the ten highest non-TCL VOA peaks are tentatively identified and
their concentrations estimated using a forward search of the NBS Mass Spectral Library.
b. Contract Required Quantitation Limits
Low level analysis contract required quantitation limits (CRQLs) for water samples are based
on CRQLs for each organic compound using FR Methods 624, 625 and 608 and are at the
part-per-billion (ppb) level. Approximate achievable sample quantitation levels for low water
and low/medium soil samples can be calculated based on the sample size and on
concentration/dilution factors.
CRQLs are provided for analytical guidance since the levels are highly matrix dependent.
Matrix interferences vary considerably depending on the nature and homoijeneity of the
sample, on the interferent contaminants which coextract from the sample, and on the sample
volume taken for analysis.
5. Contract Quality Control Requirements
QC procedures that must be performed and documented under the organic RAS program
include, but are not limited to, the following:
Instrument QC procedure:
o GC/MS instrument tunes for both volatile and semivolatile compound analyses.
o Initial multilevel calibration for each target compound.
o Continuing calibration for each target compound.
Sample QC procedure:
o Addition of surrogate compounds to each sample and blank for determining percent
recovery information.
o Duplicate matrix spike analysis.
o Method blank analysis.
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Description of Analytical Services December 1988
Certain QC procedures demonstrate that the instrument is operating within contract
specifications. These procedures include:
o Demonstration that the two tuning compounds (DFTPP for extractables and BFB for
volatiles) meet the defined ion abundance criteria.
o Determination of an average response factor based on a calibration using five
concentrations of each target compound. Specification of a subset of target
compounds that must meet a defined relative standard deviation and minimum
response factor.
o A continuing calibration at a single concentration for each target compound where
specified compounds are flagged as controls and must meet defined percent
difference from the initial response factor or a new initial calibration must be
performed.
Other QC procedures are required to demonstrate the quality of the analytical data generated.
These procedures include:
o Addition of surrogate spikes to all samples and blanks to monitor sample preparation
and analysis and to provide percent recovery information for each sample so that the
suitability of the method for each sample, regardless of matrix, may be established.
o Analyses of duplicate matrix spiked samples to display the precision of the method
for the particular matrix and also to provide percent recovery information for
defined target compounds (specified matrix spikes) as for surrogates.
o Analysis of reagent blanks for each Case or each set of twenty samples (whichever is
less) and for each matrix within a Case to ensure that laboratory contaminants are not
reflected in data results.
B. Inorganic Routine Analytical Services
1. Analytes Identified and Quantified
The inorganic RAS program identifies and quantifies metals and cyanide. These analytes are
listed on the inorganic data reporting forms in Appendix C.
2. Volumes Required and Preservation Techniques
For low level inorganic water samples, a one liter volume is required for metals analysis and a
one liter volume is required for cyanide analysis. These samples should be collected in a 1-
liter polyethylene bottle. For medium level inorganic water samples, a sixteen ounce volume
is required for metals analysis and a sixteen ounce volume is required for cyanide analysis.
These samples should be collected in a 16-ounce glass jar. For low/medium level soil samples,
a six ounce sample volume is required for both metals and cyanide analyses. These samples
should be collected in an 8-ounce glass jar.
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Different preservation techniques apply to the metals and cyanide portions of low level water
samples. For "total" metals analysis, the sample is acidified to pH < 2 with HNO^. ("Total"
meaning inclusion of particulate and dissolved fractions.) For dissolved metals analysis, the
sample is filtered and then acidified to pH < 2 with HNO^ at the laboratory. If the sample
contains a significant particulate fraction, acidification without filtration could result in
deceptively high metal values for the water sample. Varying amounts of particulate matter
can also give large differences in metal values for duplicate acidified water samples. The
following guidelines should be utilized for the cyanide aliquot:
o Test a drop of sample with potassium iodide-starch test paper (Kl-starch paper). A
resulting blue color indicates the presence of oxidizing agents and the need for
treatment. Add ascorbic acid, a few crystals at a time, until a drop of sample
produces no color on the indicator paper. Then add an additional 0.6 g of ascorbic
acid for each liter of sample volume.
o Test a drop of sample on lead acetate paper moistened with acetic acid buffer
solution. Darkening of the paper indicates the presence of 82". If 82" is present,
add powdered cadmium carbonate until a drop of the treated solution does not darken
the lead acetate test paper. Filter the solution before raising the pH for stabilization.
o Preserve samples with 2 mL of 10 N sodium hydroxide per liter of sample (pH > 12).
o Store the samples at 4°C until the time of analysis.
No chemical preservation is required for medium level water samples or for low/medium level
soil samples unless otherwise directed.
For homogenization of water samples, the contract laboratory shakes the sample in its original
sample container and transfers 100 mL aliquots to a 250 mL beaker. For water samples with a
high solids content, the user can specify that the sample not be mixed and the analysis be
performed on the supernatant. For homogenization of soil samples, the laboratory thoroughly
mixes the contents of the sample container. For soil samples with significant amounts of
water, the user has the option to specify that the supernatant be decanted and the remaining
sample be mixed thoroughly and analyzed.
If it is not certain whether a sample should be categorized as low or medium concentration,
volume should be collected and the sample preserved as specified for low level samples.
Packaging and shipment procedures should be followed as designated for medium level
samples. For water samples, one field blank should be supplied for each Case. Soil blanks are
currently not available, and the user should not submit soil field blanks for analysis. If the
user submits a rinsate blank with a Case of soil samples, the blank will be treated as a separate
aqueous matrix sample with full QC, and accordingly, a sufficient volume for analysis should
be provided to the laboratory. When a suitable soil blank material becomes available,
EMSL/LV will supply one soil blank for each Case. No additional volume is required for
duplicate analyses of water or soil samples; however, the user may specify that the duplicate
and matrix spike be performed on a particular sample. If the sampler does not provide
sufficient volume, analysis of all required parameters and complete QA/QC determinations
may not be possible. If this occurs, SMO will contact the RSCC to determine appropriate
adjustments in analysis.
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Description of Analytical Services December 1988
3. Contract Delivery Requirements
The inorganic RAS program specifies the completion of metals and cyanide analysis and the
submission of the final data package within thirty-five days following sample receipt at the
laboratory. Each inorganic RAS data package includes the following components:
o Cover page listing the samples included in the report and narrative comments
describing problems encountered in analysis.
o Tabulated results, reported in ug/L or mg/kg, of inorganic analytes identified and
quantified. These results include a brief description of the sample. Individual
analytical results are flagged by the laboratory when QC indicates potential bias due
to matrix effects, homogeneity, etc.
o QC results for preparation blanks, calibration blanks, calibration verification
standards, matrix spikes, matrix spike duplicates, laboratory control samples,
interference check samples, analytical spikes and serial dilution analyses.
o Tabulation of instrument detection limits determined in pure water solutions.
o Digestion/distillation logs, sample Traffic Reports, and raw data system printouts
identifying calibration standards, calibration blanks, preparation blanks, samples and
any atypical dilution, duplicates, spikes, interference checks and any instrument
adjustments or apparent anomalies on the measurement record.
Each inorganic RAS package submitted to SMO must be accompanied by a diskette which
contains machine readable information. This information must be sufficient to produce all
data on the hard copy summary reporting forms. Explicit formats for diskette records are
specified in the analytical Statement of Work. A summary of inorganic RAS delivery
requirements and copies of data reporting forms are contained in Appendix C.
4. Analytical Protocols
The standardized inorganic analytical methods are based on FR Methods, EPA Methods for
Chemical Analysis of Water and Wastes, and Test Methods for Evaluating Solid Waste (SW-
846). Analysis for specified metals and cyanide is performed by flame, furnace and cold
vapor atomic absorption (AA), colorimetric, distillation, and inductively coupled argon plasma
(ICP) methods.
a. Water and Soil Methods
Samples for metals analysis are prepared and acid digested. The digestate is filtered to remove
insoluble materials prior to analysis. Sample are analyzed by AA or ICP methods, and
dilutions are performed where any analyte concentration exceeds the calibrated range.
A quantitative determination for cyanide is made by midi-distillation and colorimetric or
titrimetric analysis. Mercury is quantitated in water samples by the cold vapor technique.
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b. Contract Required Quantitation Limits
Inorganic RAS contracts contain minimum CRQLs that must be met by all laboratories for
each of the metals and cyanide in pure water. On a quarterly basis, the contract laboratories
are required to verify that their instrument detection limits (IDLs) meet the CRQLs.
CRQLs for low level water samples can be achieved in the ppb to low part-per-million (ppm)
range; CRQLs for medium level water and low/medium level soil samples can be achieved in
the low- to mid-ppm range. Matrix interferences and other sample parameters that vary with
sample nature and homogeneity, with interferent contaminants that coextract from the sample,
and with the analytical method can affect quantitation levels. Since achievable quantitation
levels are dependent on the inorganic species and matrix of each sample, the laboratory must
estimate levels based on extrapolations from the pure water IDLs. The laboratory brackets
results below the CRQL to indicate a value near the IDL. Although data is reported down to
the pure water IDL, results below the CRQL should be used with caution.
5. Contract Quality Control Requirements
Inorganics RAS contracts define extensive QA procedures that must be performed and
documented. These include, but are not limited to, the following:
o Initial calibration verification,
o Continuing calibration verification,
o ICP interference check sample analysis,
o ICP serial dilution analysis,
o Preparation blank analysis,
o Spiked sample analysis,
o Duplicate sample analysis,
o Furnace AA QC analysis, and
o Laboratory control sample analysis.
The instrument QC operations include initial and continuing calibration checks which are
performed daily and/or every ten samples. These checks determine that the analytical system
is meeting contract required criteria.
Analytical QC operations include:
o ICP Interference Check Sample Analysis: Performed at least twice per eight hour
shift to verify interelement and background correction factors.
o ICP Serial Dilution Analysis: Performed for samples of a similar matrix and
concentration for each Case of samples, or for each twenty samples received
(whichever is more frequent), to ascertain whether significant chemical or physical
interferences exist due to sample matrix.
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Description of Analytical Services December 1988
o Preparation Blank Analysis: Performed for each batch of samples or for each set of
twenty samples to ascertain whether sample concentrations reflect contamination.
o Spiked Sample Analysis and Duplicate Sample Analysis: Performed for each
concentration and matrix within a Case of samples, or for each set of twenty samples
of a similar matrix within a Case, to provide information concerning sample
homogeneity, analytical precision and accuracy, and the effect of the sample matrix
on the analytical methodology, and to enable the Agency to evaluate the longterm
precision of the method.
o Furnace AA QC Analysis: Required for quantitation; incorporates duplicate
injections and analytical spikes in order to evaluate the precision and accuracy of the
individual analytical determinations on each sample.
o Laboratory Control Sample Analysis: Standards carried through sample preparation
and analysis procedures to document the performance of the entire analytical process.
On a quarterly basis laboratories verify their instrument detection limits, ICP linear
ranges, ICP interelement correction factors and ICP integration times.
C. Dioxin Routine Analytical Services
1. Isomer Identified and Quantified
The dioxin RAS contract method identifies and quantifies the 2,3,7,8-tetrachlorodibenzo-p-
dioxin (2,3,7,8-TCDD) isomer. No concentration levels are designated in the dioxin program.
All samples suspected to contain dioxin are considered hazardous and should be handled
accordingly.
2. Volumes Required
The sample volume required for dioxin analysis is four ounces of soil/sediment or two liters of
water. Each soil sample should be collected in either one 4-ounce glass jar or one 8-ounce
glass jar. Each water sample should be collected in two 1-liter amber glass bottles. The
collection of more than the required sample volume is strongly discouraged due to the
hazardous nature and difficulty in disposing of dioxin-contaminated waste.
One or more field blanks should be included with each sample batch (no more than 24
samples). A rinsate sample, consisting of trichloroethylene used in rinsing sampling
equipment, may be included in a batch. One sample with duplicate volume should be
collected for duplicate analyses. QA samples, provided by EMSL/LV, should be included as
part of the sample batch.
3. Contract Delivery Requirements
The dioxin RAS program specifies the completion of sample extraction, analysis and data
reporting within twenty-one days of sample receipt at the laboratory. The delivery
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CLP User's Guide Chapter 2
requirements include automatic reextraction and reanalysis of samples when certain criteria are
not met in the initial analysis. Each dioxin RAS data package includes the following
components:
o Completed data reporting sheets with appropriate selected ion current profiles (SICPs)
and spectra attached indicating instrumental (GC/MS) operating parameters during
data acquisition and including all rejected sample runs.
o Results of analyses of multilevel concentration calibration solutions including SICPs,
calculated response factors and computer-generated quantitation reports.
o SICPs generated during each performance check solution analysis and each
concentration calibration solution analysis.
o Chronological list of all analyses performed.
A summary of dioxin RAS delivery requirements and copies of data reporting forms are
contained in Appendix C.
4. Analytical Protocols
a. Soil and Water Methods
EPA-developed methods for the analysis of 2,3,7,8-TCDD are performed on a batch basis. A
sample batch consists of up to twenty-four field samples and normally includes an equipment
rinse solvent (trichloroethylene or hexane) sample, one or more field blanks, and a QA sample.
Prior to analysis, soil samples are prepared, homogenized and centrifuged when necessary. All
samples are then solvent extracted according to matrix. The concentrated extract is analyzed
by GC/MS using fused silica capillary column techniques. The 2,3,7,8-TCDD isomer is
identified and quantified using selected ion monitoring (SIM) GC/MS instrumentation and data
systems with the capability to acquire, store and retrieve SIM data for six ions.
b. Contract Required Ouantitation Limits
The RAS contract method provides procedures for the detection and measurement of 2,3,7,8-
TCDD in soil and water samples at concentrations as low as one ppb. Column chromatography
and other clean up procedures are used to eliminate coextracted sample components, such as
PCBs, which may interfere with the detection of very low levels of TCDD. Matrix
interferences may also occur depending on the nature and homogeneity of the sample, and
may prevent the achievement of the lowest CRQLs.
5. Contract Quality Control Requirements
Dioxin RAS contracts define extensive QC procedures that must be performed and
documented. These include, but are not limited to, the following:
o Initial and continuing calibration and instrument performance checks.
o Reagent blank analysis.
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Description of Analytical Services December 1988
o Field blank analysis.
o Fortified matrix spike analysis (2,3,7,8-TCDD spiked field blank).
o Rinsate (equipment solvent) sample analysis.
o Duplicate sample analysis.
o Reanalysis including reextraction (and/or additional clean up of the sample extract)
when QC criteria are not met in the initial analysis.
The instrument QC operations include initial and continuing calibration and instrument
performance checks. Continued calibration is performed at the beginning of each twelve hour
shift. Performance checks are performed at least twice during each twelve hour shift to
demonstrate continued acceptable GC/MS resolution, sensitivity, response factor
reproducibility, and mass range calibration, and to validate sample data.
Analytical QC operations include:
o Reagent blank analysis to demonstrate that identified compound concentrations do not
reflect laboratory contamination.
o Field blank analysis to provide information on false-positive results, on the matrix
effect of the sample on the analytical methodology, and on the accuracy of the
method.
o Rinsate sample analysis to ensure that samples have not been contaminated by
sampling equipment.
o Duplicate sample analysis to determine precision of the method.
D. Special Analytical Services
In addition to the standardized analyses available under the RAS program, the CLP provides
Regional clients with limited specialized analyses under the SAS program. While these
analytical services are beyond the scope of RAS contract protocols, they are consistent with
CLP 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 nonpriority pollutant and 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, the CLP 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 and
QA/QC requirements. SMO procures SAS by subcontracting with RAS laboratories with IFB
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
demonstrated the ability to meet program performance requirements. RAS contract
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CLP User's Guide Chapter 2
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 available laboratory community is determined, SMO contacts a minimum of five
laboratories (contingent upon availability of a particular analytical service) and describes the
requirements via telephone. Laboratories are asked to bid firm, fixed prlce(s) for the
performance of specific types of analyses on a defined number of samples. 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 client's analytical requirement.
A written, individual SAS subcontract agreement is then made between the laboratory and
Viar and Company.
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. Due to the fluctuation of these factors on a weekly and
often daily basis, the CLP may not be able to accommodate all SAS requests. SAS services are
provided on a first-come basis; however, Agency requirements can necessitate that certain
work be given priority. In this event, SMO notifies the involved RSCCs who determine
Regional sampling priorities.
SAS requests are separated into two basic categories, "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 described below.
1. RAS Plus SAS
a. Fast Turnaround
Fast turnaround requests require the application of existing RAS analytical parameters,
methodologies and detection limits with a shorter timeframe for performance of analysis
and/or delivery of data. Procurement for fast turnaround SAS is dependent upon program
sample load, laboratory capacities and laboratory operating conditions at the time of the
request. Because of constant fluctuations of these factors, it is not 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:
o RAS volatile organic target compound analysis with VOA analysis and data delivery
in seven days.
o RAS inorganic target compound analysis with data turnaround in fourteen davs.
o RAS dioxin target compound analysis with data turnaround in ten davs.
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Description of Analytical Services December 1988
b. Special Requirements 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 SAS
portion is underlined:
(1) Organic
o Volatile target compound analysis at lower detection limits than required bv the
IFB.
o Full organics analysis with additional non-target pesticide/herbicide compounds.
o Pesticide target compound analysis with minor alterations or additional procedures
applied.
o B/N/A target compound extraction with analysis bv a non-RAS method.
(2) Inorganic
o Metals and cyanide analyses plus non-RAS parameters - nitrate, sulfate. ammonia.
sulfide. total organic carbon and chloride.
o Metals and cyanide analyses with special rigorous sample homoeenization
requirements.
o Metals analysis at lower detection limits than required bv the RAS requirements.
o RAS metals and cyanide analysis with minor alterations or additional analytical
procedures applied.
(3) Dioxin
o 2,3,7,8-TCDD analysis of soil/sediment samples with a detection limit lower than
the one PPD required bv the RAS contracts.
o 2,3,7,8-TCDD analysis by the RAS protocol plus analysis of other dioxin or furan
2. All SAS
CLP clients 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. Five
categories of "All SAS" requests are described in the following sections.
*Future RAS protocol.
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CLP User's Guide Chapter 2
a. Organic
o Seven TCL Aroclors analysis only (i.e., not the entire IFB pesticide fraction).
o Non-target compound analyses*.
o Organic extraction of non-aaueous and non-soil/sediment samples (e.g., oil, tar or
biological tissue samples by a non-RAS extraction procedure).
o Organic analysis by non-RAS methods.
b. Inorganic
o Specified RAS element analysis only (e,g., cadmium, mercury and selenium).
o Non-RAS parameter analysis (e.g., total organic carbon, Sulfate, TSS, EP toxicity
tests).
o Any inorganic preparation/analysis of non-aqueous and non-soil/sediment samples
(e.g., oil, tar or biological tissue).
o Metals analysis by non-RAS methods.
c. Dioxin
o 2,3,7,8-TCDD in fish tissue (e.g., matrix other than soil/sediment).
o 2.3.7.8-TCDF (furan) in any matrix*.
o Total tetra- through octa- dioxin and/or furan classes in varied matrices*.
o Analysis by HRGC/HRMS. or GC/MS/MS*.
d. High Concentration Sample Analysis - Organic and Inorganic*
o Organic extraction and analysis for target compounds by GC/MS with tentative
identification of thirty non-target compounds of greatest concentration.
o Inorganic preparation/analysis for total metals including four procedures: KOH
fusion, pneumatic nebulization ICP, hydride generation ICP, and mercury analysis.
In addition to metals, cyanide and sulfide are quantitated.
e. Special Topics Analysis
The SAS program can usually accommodate unusual analytical requests on an "All SAS" basis
when sufficient lead-time is allowed and complete methodology and QA/QC specifications
accompany the request. These types of analyses include, but are not limited to, the following:
o Biological samples (e.g., fish, turtle tissue) for specific organic, inorganic or dioxin
analyses.
o Air samples (e.g., tenax, charcoal and flurosil tubes) for specific organic analyses.
*Future RAS Protocol
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Description of Analytical Services December 1988
o Wipe samples for specific organic or inorganic analyses.
o Methods comparison/evaluation studies.
o Asbestos analysis.
o Acid deposition parameters.
o NonSuperfund analytical services of any type.
3. Contract Delivery and Quality Control Requirements
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. Delivery 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 should
specify all deliverables required to ensure that the appropriate data packages are received.
Clients are encouraged to maintain a high level of QC in all analysis request, unless there is
substantial reason for deleting certain QC requirements.
E. Analytical Methodology Improvement/Development
1. Protocol Standardization and Improvement
CLP participants are constantly refining and improving analytical protocols to maintain state-
of-the-art status and to reflect newly defined or changed requirements of the Superfund
effort. In order to accomplish this effort, all program participants submit comments or
suggestions to the NPO on an ongoing basis. The NPO then reviews all submitted information
and considers recommendations for program application on a periodic basis.
Since 1982, the NPO has utilized technical meetings as a means to consistently employ the
scope of available resources in updating analytical program methodologies and data reporting
requirements. Technical meetings are initiated by the NPO on a periodic basis and consist of
workgroups, caucuses and an annual conference. Participants of these sessions include the
Regions, the NPO, EMSL/LV, EMSL/Cincinnati, NEIC, SMO, contract laboratories, program
support contractors, and other EPA programs and government agencies, as appropriate. These
meetings are instrumental in improving CLP protocols and orienting deliverables to 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
concurrently to maintain consistency within the program. NPO-approved protocol revisions
are included in any new IFB solicitations.
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CLP User's Guide Chapter 2
2. Method Development
Development of new analytical methods may be initiated by a newly identified or redefined
Agency analysis requirement. Analytical methods utilized in the CLP are based on
methodologies developed and approved by EPA. The NPO, EMSL/LV, EMSL/Cincinnati, 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.
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CHAPTER III
UTILIZATION OF ANALYTICAL SERVICES
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CLP User's Guide Chapter 3
The CLP provides clients with prompt access to laboratory services through a documented
system of sample scheduling. The CLP scheduling process is based on two fundamental
requirements: 1) maintenance of ongoing communication among the RSCC, field sampler,
SMO and laboratory personnel, and 2) correct use of sample scheduling and tracking
documents by the RSCC, field sampler and laboratory personnel.
SMO coordinates the scheduling of sample analyses through the CLP and tracks the progress
of samples from collection through final data production. To effectively match the analytical
needs of program clients with the capabilities of contract laboratories, SMO documents current
utilization, availability of resources and laboratory performance limitations for each program.
SMO is authorized to accept analytical requests only through the RSCC, which is established
by the EPA Regional Administrator and is centered in each Region's Environmental Services
Division or Waste Management Division. The RSCC, consisting of one or more identified
individuals (primary and secondary), routinely places analytical requests with SMO and
coordinates those requests throughout sample shipment and analysis. 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 conflicts occur.
Individuals interested in obtaining CLP analytical support should contact their Regional EPA
office's RSCC (see Appendix B).
A. Analysis Request Procedures
1. RAS Initiation Process
a. User Information Required
To initiate a RAS request, the RSCC contacts the appropriate SMO Coordinator by telephone
and provides a complete description of the analytical requirement. (SMO personnel are
identified in Appendix B.) SMO requires the following information to initiate a RAS request:
o Name of the individual RSCC.
o Name(s), association and telephone number(s) of sampling personnel.
o Name, city and state of the site to be sampled.
o Superfund site/spill ID (2 digit alpha-numeric code).
o Number and matrix of samples to be collected.
o Type of analyses required.
Organic: Full (VGA, B/N/A and pesticide/PCB), VGA and/or B/N/A and/or
pesticide/PCB, or VGA only fractional analyses.
Inorganic: metals and/or cyanide.
Dioxin: 2,3,7,8-TCDD.
o Scheduled sample collection and shipment dates.
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o Nature of sampling event.
Preliminary Assessment
Site Investigation
Expended Site Investigation
Remedial Investigation/Feasibility Study
Remedial Design
Remedial Action
Enforcement Lead
Emergency Response (Removal)
National Priorities List Delete
Operation and Maintenance
State Lead Preliminary Assessment
State Lead Site Investigation
State
National Dioxin Study
Facility Assessment
Compliance Monitoring Effort
Enforcement
Ground Water Monitoring Task Force
Resource Conservation and Recovery Act
Office of Water
Clean Air
o Suspected contaminants associated with the sample and/or site.
o Other pertinent information which may affect sample scheduling or shipment (i.e.,
anticipated delays due to site access, weather conditions, sampling equipment).
o Name(s) of Regional or contractor contacts for immediate problem resolution.
The RSCC 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 thus renders the program less than maximally responsive to all clients.
Underestimation of the number and types of samples to be collected may result in unavailable
services for any additional analyses needed.
b. Lead-time Requirement
At least one week prior to the scheduled start of a planned sampling activity, the RSCC
telephones SMO to place a specific request for RAS services. The RSCC is required to
provide scheduling information to SMO by noon on the Wednesday of the week prior to
sample shipment. This lead-time facilitates laboratory scheduling and resolution of questions
concerning sampling and analysis procedures, and allows the sampler adequate time to prepare
the required sample documentation. Advance scheduling is available and should be utilized
whenever possible.
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c. Case Number Assignment and Laboratory 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 single group of samples collected at one site or geographical location during a predetermined
and finite time period. The RSCC records the Case number and uses it in referencing that
request throughout sampling and analysis.
SMO then schedules the requested analyses through an appropriate RAS laboratory.
Laboratory selection is determined by the types of analyses, number of samples, contract
capacity, sample balance among the various laboratories, and laboratory loading and
instrument conditions. Organic laboratory selection is also based on the Regional Distribution
of Laboratories System developed by the NPO and designed to minimize the number of
laboratories producing data for any one Region. When possible, the nearest available
laboratory is assigned in order to minimize sample shipping costs.
Once RAS laboratory assignments are made, SMO contacts the RSCC to confirm the 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 must
indicate all known or anticipated sample scheduling changes. Any other changes occurring
after this time should be communicated to SMO immediately upon identification to ensure the
timely resolution of conflicts and the optimal allocation of program resources. After the
initial placement of the RAS request, the RSCC may choose to 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 sample shipment.
d. User Knowledge of Analytical Protocol
Each RSCC is responsible for acquiring and maintaining a working knowledge of current RAS
protocols and analytical services. SMO provides each Regional DPO (listed in Appendix B)
with Master Copy notebooks of each RAS program IFB Statement of Work (SOW). The
Master Copy notebooks are periodically updated to reflect program protocol changes.
The SOW represents the standardized requirements which each individual RAS laboratory is
contractually bound to follow. The analytical SOWs contain specific information on sample
types suited to RAS analysis, compounds identified and quantified, analytical methods,
protocols, detection limits, deliverable requirements, and quality control requirements.
Program users should consult the appropriate SOW to confirm that the RAS program is suited
to an analytical request.
2. SAS Initiation Process
a. User Information Required
Analytical requirements differing from RAS parameters are processed through the SAS
program as described in Chapter II, Section D. To initiate a SAS request, the RSCC contacts
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the appropriate SMO Coordinator by telephone and provides a complete description of the
analytical requirement. SMO requires the following information to initiate a SAS request:
o Name of RSCC.
o Name(s), association and telephone number(s) of sampling personnel.
o Name, city and state of the site to be sampled.
o Superfund site/spill ID (2 digit alpha-numeric code).
o Number and matrix of samples to be collected.
o Specific analyses required, appropriate protocols and QA/QC.
o Required detection limits.
o Matrix spike, matrix spike duplicate, duplicate or LCS frequency, if applicable.
o Data turnaround and data format.
o Justification for fast turnaround request, if appropriate.
o Scheduled sample collection and shipment dates.
o Nature of sampling event.
Preliminary Assessment
Site Investigation
Expended Site Investigation
Remedial Investigation/Feasibility Study
Remedial Design
Remedial Action
Enforcement Lead
Emergency Response (Removal)
National Priorities List Delete
Operation and Maintenance
State Lead Preliminary Assessment
State Lead Site Investigation
State
National Dioxin Study
Facility Assessment
Compliance Monitoring Effort
Enforcement
Ground Water Monitoring Task Force
Resource Conservation and Recovery Act
Office of Water
Clean Air
o Suspected contaminants associated with the samples and/or site.
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o Other pertinent information which may affect sample scheduling or shipment (i.e.,
anticipated delays due to site access, weather condition, sampling equipment).
o Name(s) of Regional or contractor contacts for immediate problem resolution.
In follow up to the verbal request, the RSCC must submit a completed SAS Client Request
form to SMO. This form serves as the written record to clarify and confirm the client's
requirement for specialized analytical work. A copy of the SAS Client Request form is
included in Appendix D.
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, and
thus renders the program less than maximally responsive to all clients. 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 resolicited and sampling plans postponed accordingly.
b. Lead-time Requirements
When a sampling activity has been planned, the RSCC telephones SMO and places the specific
request for SAS services. Because SAS services are individually procured on a competitive
basis, a minimum lead-time of two weeks is required to process a completely defined SAS
request. More lead-time is strongly 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 will cause the entire process to begin again. Fully defined
requests initiated with less than two weeks lead-time may not be solicited and awarded in time
to meet the original shipment date.
Certain types of SAS requests require a longer lead-time. A minimum 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 nonSuperfund SAS requests. Award of nonSuperfund SAS
subcontracts may only be made after the appropriate funding process is complete. The RSCC
should contact SMO several 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 single group of samples collected at one site or
geographical location during a predetermined and finite time period. The RSCC records the
SAS number and Case number (if applicable) and uses both numbers in referencing the request
throughout sampling and analysis.
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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 RSCC 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 specify
modifications or additions to these protocols. If such changes are extensive, the RSCC 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 of a method that is not
commonly available, the RSCC must submit the method two to three weeks in advance of
sample shipment. Additional lead-time is required for protocol distribution and review by
solicited laboratories.
SAS requests which cite the application of 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:
o Methods for Chemical Analysis of Water and Waste. USEPA, 1983.
o Test Methods for Evaluating Solid Waste. Physical/Chemical Methods, SW-846,
USEPA Office of Water and Waste Management, 1983.
o Standard Methods for the Examination of Water and Waste Water. APHA, AWWA,
WPCF, Current Edition.
Further analytical references are supplied in Appendix F. The RSCC should contact SMO
several weeks in advance if there is a question as to whether a particular method will require
additional lead-time for distribution.
3. Procedures for Making Changes to Analytical Requests
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, detection limits, shipping dates, postponements or
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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, or analysis data inappropriate for client purposes.
B. Regional Organic/Inorganic Allocation System
The NPO has established an allocation system to equitably apportion available laboratory
capacity to the Regions during periods of heavy sampling activity. 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 given week on the Wednesday preceding that 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,
utilizing available laboratory capacity, then makes laboratory assignments for sampling
activities as prioritized by the NPO. For additional information concerning the allocation
system, user's should contact SMO's Group Leader for Analytical Services (see Appendix B).
C. Sample Documentation
Each sample processed by the CLP 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 CLP 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 point in time for a specific
analysis. A sample may reference field samples, duplicates, replicates, splits, spikes or blanks
that are shipped from the field to a laboratory. Whenever questions arise, samplers should
contact SMO for direction and clarification concerning the proper completion and distribution
of CLP paperwork.
1. Sample Traffic Report
RAS organic and inorganic samples are documented with corresponding CLP sample Traffic
Reports (TRs), a four part carbonless form. Each TR may document up to twenty samples
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shipped to one CLP 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 the two types of TRs, as well as examples of properly completed TR
forms, are included in Appendix D.
TR forms must also be used when an individual sample is to be analyzed for both RAS and
SAS parameters. A SAS Packing List is not required and should not be used in addition to the
TR. Both the Case number and the SAS number must be entered at the top right of the form
in order to clearly identify and track the sampling event. Samplers must take caution not to
include the Case number on "All 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").
Samplers record every sample on the TR form by completing the columns for sample number,
sample description, concentration, RAS analytical fraction, special handling and station
location. In addition, samplers complete the boxes for type of activity, site name, Regional
information, analysis laboratory, sampling date and shipping information.
After completing the TR, the sampler includes the bottom two copies with the sample
shipment to the laboratory, returns the top copy to SMO, and retains the remaining copy for
their file. Upon receipt of the sample shipment, the laboratory documents sample condition
and signs the TR. The laboratory returns a copy of the signed TR to SMO and retains a copy
for their file. Copies of the signed TRs are provided to the RSCC as part of the data
package.
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. Dioxin Shipment Record
The CLP Dioxin Shipment Record (DSR), a four part carbonless form, is used as sample
documentation for the RAS dioxin program. These forms must also be used for any "RAS
plus SAS" dioxin samples. The DSR provides a record for one shipment batch of dioxin
samples (up to twenty-four samples). A copy of the DSR, as well as an example of a properly
completed DSR form, is included in Appendix D.
To provide a permanent record of each sample collected, the sampler records the appropriate
Case number and batch/shipment number on the DSR form. The sampler then enters header
information including type of activity, Regional information, shipping information and
analysis laboratory. The sampler records sample matrix and description (e.g., soil/sediment
field sample, solvent rinsate) for each sample by checking the appropriate box following each
sample number.
After completing the DSR, the sampler includes the bottom two copies with the sample
shipment to the laboratory, returns the top copy to SMO, and retains the remaining copy for
their file. Upon receipt of the sample shipment, the laboratory documents sample condition
and signs the DSR. The laboratory returns a copy to SMO and retains a copy for their file.
Copies of the laboratory-signed DSRs are provided to the RSCC as part of the data package.
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SMO provides DSR forms to each Region through the RSCC. The RSCC should contact SMO
two or more weeks in advance to order additional DSR forms.
3. SAS Packing List
For "All SAS" samples, samplers are to utilize the SAS Packing List (PL), 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 hyphen and progressive numerical
designation, starting with 1 (e.g., 2000E-1, 2000E-2, 2000E-3, 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. A copy of the SAS PL, as well as an example of a properly completed PL
form, is included in Appendix D. Regions should consult SMO to verify that the PL is
appropriate to use in their situation.
The sampler completes the PL by recording the SAS number, site name and location, sampling
date, shipment date, analysis laboratory, sampling office, sampler name and telephone number,
individual SAS sample numbers, sample description and analytical parameters requested. After
completing the PL, the sampler includes the bottom two copies with the sample shipment to
the analysis laboratory. Following sample shipment, the sampler sends the top copy to SMO
and retains the second copy as a file copy. Upon receipt of samples, the analysis laboratory
documents sample condition and signs the PL, returns a copy to SMO and keeps a laboratory
file copy. Copies of the laboratory-signed PLs are provided to the RSCC as part of the SAS
data package.
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.
4. Sample Number
A unique sample number, recorded on the TR, DSR and SAS PL, identifies each sample.
Inorganic and organic/VOA sample numbers have different formats and are not
interchangeable. Strips of adhesive labels preprinted with individual sample numbers are
provided by SMO with TR and DSR forms. Samplers must provide sample labels, marked in
indelible ink with the appropriate SAS sample numbers, for use with "All SAS" samples.
The sampler affixes the sample label to the corresponding containers that make up the sample
and, if appropriate, to the outside of the metal can in which the sample is packed (see Section
D for packaging requirements). The 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 clear, waterproof
tape.
5. Sample Tag
Each sample removed from a waste site and transferred to a laboratory for analysis is
identified by a sample tag which contains specific sample information as defined by NEIC.
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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.
The information recorded on the sample tag includes:
o CLP Case/SAS No(s). - The unique number(s) assigned by SMO to identify the
sampling event. (Entered under "Remarks" heading.)
o CLP Sample No. - The unique sample identification number (from the TR, DSR, or
PL) used to document that sample. (Entered under "Remarks" heading.)
o Project Code - The number assigned by EPA to the sampling project.
o Station No. - A two digit number assigned by the sampling team coordinator.
o Date - A six digit number indicating the month, day and year of collection.
o Time - A four digit number indicating the military time of collection.
o Station Location - The sampling station description as specified in the project plan.
o Samplers - Signatures of samplers on the project team.
o Remarks - Case/SAS and sample numbers, as well as any pertinent comments, are
entered here.
o Tag No. - A unique serial number preprinted or stamped on the tag.
o Lab Sample No. - Reserved for laboratory use.
Additionally, the sample tag contains appropriate spaces for noting that the sample has been
preserved and indicating the analytical parameter(s) for which the sample will be analyzed.
After the sample tag is completed, each tag is securely attached to the sample container.
Samples are then shipped under chain-of-custody procedures as described in the following
section. An example of a properly completed sample tag is provided in Appendix D.
6. Chain-of-Custody Record
In accordance with Agency enforcement requirements, official custody of samples must be
maintained and documented from the time of collection until the time of introduction as
evidence during litigation. The following custody documentation procedure was developed by
NEIC and is used in conjunction with CLP documentation (i.e., TR, DSR and SAS PL) for all
samples processed through the program.
A sample is considered to be in an individual's custody if any of the following criteria are
met: 1) the sample is in your possession or it is in your 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 followed during the field work.
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The Chain-of-Custody Record is employed as physical evidence of sample custody. The
sampler completes a Chain-of-Custody Record to 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 project number, samplers' signatures and the Case and/or SAS
number as header information on the Chain-of-Custody Record. The commonly 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, CLP 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. A copy of the Chain-of-Custody Record, as well as
an example of a properly completed custody record, is included in Appendix D.
The custody record is completed using waterproof ink. Any corrections are made by drawing
a line through and initialing the error, then entering the correct information. Erasures are not
permissible.
The original signature copy of the Chain-of-Custody Record is enclosed in plastic (with CLP
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 splits.
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 transfer
process is complete, the laboratory is responsible for maintaining internal logbooks and records
that provide a custody record throughout sample preparation and analysis.
D. Sample Packaging and Shipment
1. Packaging Requirements
Samples processed through the CLP must be packaged for shipment in compliance with
current U.S. Department of Transportation and commercial carrier regulations. All required
government and commercial carrier shipping papers must be filled out and shipment
classifications made according to these regulations. (Consult Appendix F for shipping
references.)
Waterproof, metal or hard plastic ice chests or coolers are the only acceptable type of sample
shipping container. Inside the cooler, sample containers must be enclosed in clear plastic bags
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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 scalable lid (e.g., paint cans). The outer metal can must be
labeled with the number of the sample contained inside. Containers which do not fit into
paint cans should be double bagged.
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 transport. Earth or ice should never be used to pack samples; earth is a contaminant,
and ice melts resulting in container breakage.
Water samples for low/medium 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
matrix/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 lab.
Low level inorganic and VOA water samples require chemical preservation. Users should
consult Chapter II for preservation techniques.
TRs, DSRs, SAS PLs, Chain-of-Custody Records, and any other sample documentation
accompanying 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. A summary of correct sample packaging is
illustrated in Appendix D.
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 shipment requires
more than a 24-hour period, sample holding times can be exceeded compromising the integrity
of the sample analysis. Samples for inorganic analysis should be held until sampling for the
Case is complete and then shipped for two-day delivery. In the RAS inorganic program, three
days is the recommended period for collection of a Case of samples.
The NEIC/Denver and the ERT/Cincinnati hazardous waste site manuals provide extensive
information on EPA-approved sample packaging and shipment techniques. References for
these materials are provided in Appendix F. In addition, general questions concerning sample
packaging and shipment may be directed to SMO.
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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:
o Sampler name and phone number.
o Case number and/or SAS number of the project.
o Site name/code.
o Batch numbers (dioxin only).
o Exact number(s), matrix(ces) and concentration(s) of samples shipped.
o Laboratory(ies) to which samples were shipped.
o Carrier name and airbill number(s) for the shipment.
o Method of shipment (e.g., overnight, two-day).
o Date of shipment.
o Suspected contaminants associated with the samples or site.
o Any irregularities or anticipated problems with the samples, including special
handling instructions, or deviations from established sampling procedures.
o Status of the sampling project (e.g., final shipment, update of future shipping
schedule).
Sample shipments made after 5:00 p.m. EST should be called 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 sample
shipments intended for Saturday delivery. CLP laboratories remain open to receive Saturday
shipments only upon advance notification 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, changes in the number or type of samples
to be collected or changes in shipping dates must be communicated to SMO immediately.
Appendix D contains a checklist for coordinating sample shipment.
E. Procedures for Problem Resolution
1. Resolving Problems Concerning Sample Shipment and Analysis
Program laboratories routinely notify SMO upon encountering problems with sample receipt or
during sample analysis. (Examples of these types of problems are listed in Appendix D.) In
response, SMO immediately contacts the RSCC to relay the problem and to assist in
formulating a solution. SMO then contacts the laboratory involved to communicate the
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recommended action and to authorize processing of the sample(s) in question. Timeliness is
the key to this type of problem resolution since 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. Technical questions regarding contract analytical procedures
should be referred to the PO or the DPO of the laboratory through the NPO.
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,
subject of the discussion and its resolution. In 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. An example of the Telephone Record Log is included in Appendix D.
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 through SMO. Depending on the nature of the question, SMO
will respond or will direct the client to the appropriate NPO official for resolution. Comments
regarding laboratory performance, whether positive or negative, should be directed in writing
to the DPO of the laboratory with a copy provided to the PO.
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CHAPTER IV
AUXILIARY SUPPORT SERVICES
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The CLP provides several supplementary services that have developed as a natural adjunct to
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. Sample Bottle Repository Program
1. Types of Containers Available
The Sample Bottle Repository program provides CLP clients with eleven types of cleaned,
quality controlled sample containers for use in hazardous waste sampling collection. Sample
coolers and sample preserving agents are not supplied through the program.
To ensure that no contamination exists that might affect sample data results, each container
type is cleaned and quality control tested by specified procedures. These methods are
directly related to the analyses that may be performed on samples collected in the container.
The following chart lists the types of containers provided through the program and the
type(s) of samples appropriate for collection in each container. To ensure appropriate quality
control, samplers should use containers only to collect samples as listed on the following
chart.
2. Ordering Procedures
The Sample Bottle Repository program may be accessed by Regional and contractor clients
for sample collection under the Superfund program and other nonSuperfund Agency
programs. Two individuals from each organization are designated as Authorized Requestors
(ARs); only these individuals may place container requests through the program. Users
interested in accessing the Repository program should contact their RSCC or SMO for further
information. State personnel should access the program through their Regional EPA office.
Once a user has become authorized to request containers from a Repository, SMO provides
them with a supply of Delivery Requests (DRs), a three part carbonless form, so that the AR
can request containers directly from the Repository. Since the Repository can respond only
to requests submitted by a designated AR, users must promptly notify SMO of any changes in
AR designations.
Container requests are defined by the amount of time between the date the Repository
receives the request (verbal or written) and the required delivery date:
o Routine Request: Fifteen or more working days lead-time for delivery.
o Fast Turnaround Request: More than three but less than fifteen working days lead-
time for delivery.
o Emergency Request: Less than three working days lead-time for delivery.
All DRs must be signed by an AR. For routine requests, the original copy of the completed
DR is sent to the Repository at the address indicated on the form, the second copy is retained
for the user's file, and the third copy is sent to SMO. Because of short lead-times, fast-
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turnaround and emergency requests should be telephoned to the Repository at the number
provided on the form. The written DR must be distributed per routine procedure to confirm
the request.
Whenever possible, users should submit requests a minimum of two weeks in advance of the
required delivery date to ensure timely and complete delivery of containers. The Repository
may not be able to respond to all emergency and fast-turnaround requests; response depends
on Repository inventory and in-house requests.
In the event that requested containers are no longer needed, the user must immediately
contact the Repository to verbally cancel the request, follow up with a cancellation
memorandum to the Repository, and send a copy of the memorandum to SMO. Cancellation
memos, as well as all other project-related correspondence, should cite the appropriate DR
number.
3. Shipment Information
Upon receipt of the DR, Repository personnel begin preparing the request and schedule
shipment. Repository personnel immediately notify the AR, if for any reason, the request
cannot be met in full by the required delivery date. Often partial shipments can be arranged
over several days to meet the AR's requirement. If concurrent requests are received at the
Repository that cannot be filled in a timely manner and if partial shipments cannot be
satisfactorily arranged, the Repository immediately notifies SMO. SMO then coordinates with
the involved RSCC in determining the priority of container requests based on the Region's
sampling needs.
Each carton in a shipment is marked "Box of ," and a Repository Packing List
(PL) is included in Box 1 of each shipment so that the recipient can verify that the entire
shipment has been received. In addition, the Repository sends two copies of the PL to the
AR at the time of shipment. The AR confirms with the recipient that the entire shipment
was received in good condition, then enters the date of receipt and signs the PL in the space
indicated to confirm receipt. The AR must return a copy of the signed PL to SMO within
seven days of shipment receipt. The second copy of the PL is retained for the AR's files.
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Chapter 4
CONTAINERS SUPPLIED THROUGH THE
USEPA SAMPLE BOTTLE REPOSITORY
Container Type
A
B
C
D*
H
K
Description
80-oz. amber glass bottle
w/teflon-lined black phenolic cap
40-mL glass vial w/teflon-backed
silicon septum cap
1-L high-density polyethylene bottle
w/poly-lined, baked poly cap
120-mL glass vial w/telflon-lined,
white poly cap
16-oz. wide-mouth glass jar
w/teflon-lined, black poly cap
8-oz. wide-mouth glass jar
w/teflon-lined, black poly cap
4-oz. wide-mouth glass jar
w/teflon-lined, black poly cap
1-L amber glass bottle w/teflon-
lined, black poly cap
32-oz. wide-mouth glass jar
w/teflon-lined, black poly cap
4-L amber glass bottle w/teflon-
lined, black phenolic cap
500-mL high-density polyethylene
bottle w/poly-lined, baked poly cap
Used for Sample Type
Extractable
Organics
Volatile
Organics (Water)
Metals, Cyanide
& Sulfide
Volatile Organics
(Soil)
Ext. Organics & Metals
In Soils & Med/High Water
(same as Type E)
(same as Type E)
(same as Type A)
(same as Type E)
(same as Type A)
(same as Type C)
*The NPO recommends the use of container type B, instead of container type D, for volatile
organics (soil). A suitable cap liner for container type D is currently under consideration.
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4. Summary of Container Cleaning and Quality Control Procedures
Containers provided under this program are cleaned in Lots of approximately one hundred
containers. (Exact Lot sizes for each container type are determined as a multiple of a case so
that a container Lot is not split between cases.) Each container Lot is assigned a unique
identifying number. This Lot number is permanently affixed to each container in the Lot,
recorded in the Repository logbook, and entered on the PL when containers from that Lot are
shipped. For quality assurance purposes, each container's Lot number must be permanently
associated with the sample collected in that particular container. Samplers should record each
container Lot number and associated CLP sample numbers in their field records at the time
of sample collection.
The Repository routinely performs QC analyses on one percent of the number of containers
per Lot. If a container fails to pass the QC test(s), the associated Lot of containers is
reprocessed through the system. No Lot is released for shipment until acceptable QC results
are verified.
An additional container is removed from each Lot and stored for QC purposes. QC storage
containers are kept in a contaminant-free area of the Repository which is monitored for
volatile compounds. The QC storage containers are retained for one year in order to recheck
for cleanliness should possible contamination of a Lot of containers come into question at a
later date.
A QC release number, assigned to each Lot of containers that passes QC analysis, is marked
on both the analysis and storage QC containers for each Lot. The QC release number is
cross-referenced with the Lot number in Repository records, so that all QC records can be
accessed based on the Lot number identification.
5. Procedures for Problem Resolution
a. Resolving Problems Concerning Container Shipment
If there are problems relating to shipment (i.e., shipment does not arrive by scheduled date,
shipment is incomplete, or contents are damaged), the AR or shipment recipient (as
appropriate to the situation) should contact the Repository immediately to resolve the
problem. If the problem is not satisfactorily handled, the AR should then contact SMO for
resolution.
b. Resolving Problems Concerning Container Contamination
If a user has definitive cause to suspect that container contamination may affect sample
analysis results, the concerned RSCC should notify SMO by telephone and follow up with an
explanatory memorandum directed to the Repository PO and copied to SMO. The
memorandum should include a description of the problem, rationale for suspecting container
contamination, supporting documentation (if available), and Lot number(s) for all containers
concerned. The user should verify that the contamination encountered is not a result of
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either improper field procedures (e.g., use of contaminated water for field blanks) or poor
laboratory practice (e.g., background contamination) and include this information as part of
the rationale in the memorandum submitted to the PO.
Upon PO request, the Repository will check the QC analysis record for the concerned Lot(s)
of containers and verify that contract procedures were correctly followed and that the Lot
passed the QC analysis. Should an error be identified in this process, the Repository will
immediately notify SMO.
As a second step, following PO authorization, the Repository will pull the QC storage
container for the Lot(s) and analyze the container(s) for suspected contaminants. SMO will
notify the RSCC of the analysis results so that if there is a contamination problem, analysis
data from samples collected in other containers in that Lot can be appropriately flagged.
Should contamination be confirmed by analysis of the QC storage container, the Repository
will immediately identify the problem and correct procedures as necessary to resolve it.
Should a wide-spread problem be identified at any time, SMO would notify ARs in a timely
manner so that affected containers could be pulled before use in the field.
B. Shipment Management Program
The Shipment Management Contractor establishes, maintains and monitors all shipping
accounts for the transportation of CLP 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 CLP use may also be addressed by this
program at the request of the NPO.
1. Sample Containers
A packing list accompanies all cases of containers that are shipped from the Sample Bottle
Repository to designated recipients. At the time of shipment, the Repository sends a copy of
the packing list to the Shipment Management Contractor who utilizes the list to verify and
pay shipping invoices. SMO notifies the Contractor of any shipments that require special
tracking (e.g., shipments for overnight delivery, shipments not originating at a Repository).
If any questions arise regarding the shipment of sample containers, the Contractor contacts
the appropriate Repository for resolution.
2. Sample Coolers
Field samplers package samples into coolers for transportation to contract laboratories per the
procedures specified in Chapter III, Section D. Sampling contractors are responsible for
clearly marking a return address on the outside of each cooler. Contract laboratories are
required to return each cooler to the indicated sampling office within fourteen days of
sample receipt. The Shipment Management Contractor is responsible for tracking and paying
for cooler shipments from the laboratories to the sampling offices.
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3. Contract Compliance Screening Results
After reviewing each data package via the Contract Compliance Screening (CCS) process (see
Section G), SMO distributes the results to EMSL/LV, the appropriate Region and the relevant
laboratory. SMO also sends a copy of the air carrier manifest to the Shipment Management
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.
C. Environmental Services Assistance Teams
ESAT contracts provide technical, management and other related resource support for
Superfund and nonSuperfund Agency programs. The two ESAT contracts are defined by
zones with ESAT Zone 1 supporting Regions I, II, III and V, and ESAT Zone 2 supporting
EPA Headquarters and Regions IV, VI, VII, VIII, IX and X.
ESAT contractors provide assistance in the following task areas: 1) analytical support
including chemical analysis and data reporting per CLP or other designated methods; 2)
review of CLP and other analytical data to determine data quality for purposes of usability;
3) logistical and administrative support including sample, data and document control; 4)
QA/QC support including preparation and review of QA project plans, CLP special analytical
services method definition, and CLP IFB protocol review; 5) management and reporting; and
6) other task related activities to be defined through EPA technical direction as the needs
occur. Unless otherwise directed, ESAT contractors apply CLP protocols and follow program
guidelines.
D. Information Services
1. Regional Backlog Inventory Report
Upon request, SMO distributes a Regional Backlog Inventory Report to the DPO. This
computerized report provides a summary of the Region's use of CLP resources during a
specified time period. The following information is included in the Backlog Inventory
Report:
o Case number
o Sample number
o Laboratory name and contract number
o Laboratory sample receipt date
o Sample weight and components analyzed
o Sample type
o Data due date
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o Days late/early calculations for contractually required deliverables (i,e, extraction,
VOA analysis and sample data package)
o Invoice numbers
o CCS results to lab date
o Data complete date
The Region utilizes the Backlog Inventory Report for management and resource planning as
well as verifying monthly sample receipts and analyses performed. An example of the
Regional Backlog Inventory Report is contained in Appendix E.
2. Sample Status Information
After scheduling analysis, SMO tracks samples from shipment through data reporting via
manual and computerized tracking systems. SMO maintains ongoing communication with the
DPOs, RSCCs and laboratories regarding sample status and responds to inquires from
concerned parties, as appropriate. A backlog report listing each laboratory's samples and the
number of days the samples have been in-house is sent bimonthly to the DPOs and
laboratories.
3. General Program Information
Under the direction of CLP management, SMO serves as the program's information center for
incoming calls and correspondence. Upon request, SMO provides program participants and
interested parties with information and materials on program services and procedures, and
refers callers to the proper sources for additional information.
E. Enforcement Support
1. Generation of Enforcement Quality Data
One major objective of Superfund is to recover costs incurred in the investigation and clean
up of hazardous waste sites from responsible parties. The process by which these parties are
identified and determined to be responsible often involves litigation. Frequently, the
Agency's case uses CLP data generated from the analysis of samples collected at a given site.
The CLP supports these and other enforcement requirements of Superfund by ensuring that
CLP analytical data is documented and available for litigation. Through NEIC, the CLP has
established detailed procedures and documentation to ensure that sample data meet Agency
enforcement standards.
a. Chain-of-Custodv and Document Control
Each CLP analytical contract requires the laboratory contractor to implement a comprehensive
document control system and to employ strict chain-of-custody procedures in the receipt and
handling of samples throughout the analytical and data reporting process. The laboratory
must have written standard operating procedures for receipt and log-in of samples,
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maintenance of sample security after log-in, tracking of samples through all steps of
preparation and analysis, and organization and assembly 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, instrument logbook pages,
correspondence and document inventory.
Before a laboratory is awarded a CLP 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.
b. NEIC Evidence Audits
Laboratories are contractually required to submit a complete Case file purge package,
containing all evidence and other documentation relating to sample analysis, within 270 days
after submission of analytical data. The Contractor Evidence Audit Team (CEAT) reviews all
Case file purge packages to verify that the documentation is complete and conforms to
contractual requirements; CEAT routinely audits a selected number of packages to determine
adherence to procedure. Following review and/or audit, NEIC sends laboratory Case file
purge packages to the Region, where the packages are filed with the analytical data and may
be subject to additional review. A list of Case file purge materials is included in Appendix
E.
NEIC evidence audits may involve production of sample profiles. A sample profile traces the
path and handling of specific samples from the point of collection through shipping,
laboratory receipt, chemical analysis and data reporting. The profile identifies all evidence
and sequence of events necessary to reconstruct the sample history and thus present to the
case attorney a depiction of the sample integrity. In addition to the routine generation of
sample profiles in evidence audits, authorized Regional personnel and enforcement attorneys
may request NEIC to prepare Case-specific sample profiles to support enforcement activities.
2. Additional CLP Enforcement Support
Court appearances and other mandated deadlines often do not allow sufficient time for
completion of the normal Case file purge package submission, review and audit process. In
this event, enforcement activities require direct CLP support. Data package evaluation
and/or testimony from laboratory or CLP personnel may also be needed. Through SMO, the
CLP has established procedures to coordinate and respond to short term enforcement-related
requirements.
a. Request Procedures
Regional counsel, NEIC or other designated EPA personnel submit enforcement-related
requests in a memorandum to the NPO. The NPO reviews the memorandum, determines
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necessary CLP action and forwards the request along with directions for action to SMO. If a
request requires immediate response, the requestor should contact SMO directly by telephone
and follow up with the written request memorandum to the NPO.
b. Requestor Information Required
To initiate CLP action, the following information must be provided by the requestor:
o Name and telephone number of Regional contact coordinating the enforcement
activity
o Case/SAS number(s) of specific site sampling(s)
o Sample number(s)
o Date(s) of sample collection
o Laboratory(ies) that performed the analysis
o Type of support needed
Most requests can be met quickly; however, a two week lead-time is strongly recommended.
c. Documentation/Support Provided by CLP
In responding to enforcement-related requests, SMO provides the following support:
o Arranges for the timely delivery of all laboratory and evidence documentation
relating to specific sample analyses (within a minimum of seven days of request, if
designated).
o Obtains information relating to sample analysis or handling not specifically required
under laboratory contracts.
o Assists in arranging for expert testimony by laboratory or CLP personnel.
o Augments Regional resources for analytical data review.
F. Cost Recovery Substantiation
The CLP provides documentation for program analytical costs to the EPA's Office of Waste
Programs Enforcement (OWPE) in support of Superfund cost recovery efforts.
1. Request Procedures
Requests for cost recovery documentation must be made by completing a Cost Recovery (CR)
checklist and mailing it to OWPE. This checklist is designed to provide basic site information
needed to compile cost documentation from the CLP and other sources. A copy of the OWPE
CR checklist is included in Appendix E.
In response to requests, OWPE collects and organizes cost-related documentation from the
CLP and several other sources, such as the EPA Financial Management Division, the EPA
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Office of Solid Waste and Emergency Response, and REM, FIT, TAT and other Agency
contractors. In case of conflicts, OWPE is responsible for prioritizing incoming requests. A
minimum lead-time of four to six weeks is required to provide the requestor with a full site
cost recovery report.
2. Requestor Information Required
To enable the CLP to prepare its cost documentation package, requestors must supply the
following information on the CR checklist:
o Identification number. The appropriate CLP Case or SAS number must be entered
here. Although rare, if the Case or SAS number refers to more than one site, the
specific sample numbers (from the Case Traffic Reports or SAS Packing Lists)
related to the sites in question must be provided.
o Name and location of site.
o Date the cost report is needed. A minimum of four weeks from the date of request
must be given. Six week lead-time is recommended whenever possible.
3. Documentation Provided by CLP
The following information is assembled by SMO and submitted to OWPE:
o Financial Summary for Cost Analysis—This summary lists analytical and sample
management costs on a Case and/or SAS basis and shows total expenses for a
particular site. Information on how sample management costs are computed is
included.
o Summary of Invoices, Vouchers and Canceled Checks—This report lists all SAS
laboratory invoice numbers and includes SAS canceled check numbers. The
summary is organized by SAS number and laboratory name.
o Routine Analytical Services Cost Report—This computerized report is organized by
Case number and laboratory contract. The report includes laboratory invoice
numbers, net analysis costs, total of adjustments for contractual noncompliance,
early delivery considerations, and sample management costs; and lists total costs on a
sample-by-sample, laboratory contract and Case basis.
o Routine Analytical Services Case Sample List—This computerized report is organized
by Case number and laboratory contract with laboratory invoice references. The
report provides detail on deliverable turnaround times, analysis components and
sample types.
o Special Analytical Services Cost Report—This computerized report provides a brief
description of the service provided and includes the number of samples analyzed,
data turnaround time, contract start date, laboratory receipt date, unit costs sample
management costs, and contract status. The report also lists total contract costs on
SAS and laboratory bases.
o Copies of all SAS-Related Canceled Checks and Laboratory Invoices.
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OWPE provides this CLP information along with documentation gathered from other sources
to the Regional case development team in the full cost recovery package.
G. Contract Compliance Screening
SMO performs CCS on all RAS data produced by the CLP. Modified CCS can also be
performed on a case-by-case basis on "RAS Plus SAS" or "All SAS" data.
CCS is a structured review which determines 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
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 have some
payment recommendation withheld, either temporarily or permanently, depending on the
nature and extent of the defect identified.
Structurally similar CCS procedures are applied to organic, inorganic and dioxin data. CCS
results are produced on a fast-turnaround basis (fifteen days) and identify compliance
discrepancies 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. Examples of CCS result forms
are included in Appendix E.
H. Data Review Services
A full range of review services are used to assess CLP data. Objectives of the review
services are:
o To determine the usability and limitations of data given particular field or policy
assessment criteria.
o To maximize the amount of usable data by identifying critical properties of data and
by resolving or proposing solutions to analytical or quality control problems.
o To provide systematic and standardized data quality assessment and status summary
to determine method, laboratory and program performance.
These review services are performed by a number of operations:
o Review for data usability is performed by Regional personnel and contractors.
Recommended review procedures have been standardized and organized into
functional guidelines for evaluating CLP data. EPA Data Validation Workgroups
have produced specific documents for review of organic, inorganic and dioxin
analyses.
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o 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.
o Under direction of the CLP management, EMSL/LV and/or SMO may perform
additional data review to assess a problem Case or provide a second opinion on
usability.
All requests for SMO data review services should be placed using the SMO Data Review
Request memorandum available from SMO. An example of this memorandum is provided in
Appendix E. Copies of the request should be submitted to SMO (Attention: Data Review
Team), the SMO PO and the RSCC. Upon authorization by the PO, 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.)
1. Requestor Information Required
In completing the Data Review Request form, the client must provide the following
information for each Case:
o SMO Case number
o Site name
o Analytical laboratory name(s)
o Number of samples
o Sample list
o Type(s) of review requested
o Requested date for review completion
o User name and contact
o Intended use of data
A minimum lead-time of two weeks is required for data review. However, review time is
variable depending upon the number of samples involved and the nature of the review. If
conflicts occur, the appropriate DPO(s) will be notified and asked to prioritize requests.
2. Documentation Provided by CLP
An evaluation report that includes a sample/result matrix and supporting statistics and
documentation is produced for each type of review. For each sample fraction, the report
indicates whether the data are considered acceptable, acceptable given qualifications noted or
unacceptable. Reasons for the designation are discussed and completed data review forms for
each of the areas of performance are included in the report to the client.
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CHAPTER V
LABORATORY SELECTION AND STARTUP
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A. Laboratory Selection Process
1. Qualification Requirements
a. Preaward Performance Evaluation Sample Analysis
The first criterion for laboratory selection is preaward performance evaluation (PE) sample
analysis. Laboratories request preaward PE samples through the Contracting Officer (CO)
and, if required, submit a deposit that is returned upon submission of the PE sample data
results.
PE samples, distributed by EMSL/LV, 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 standard turnaround time for PE
sample data submission is twenty-one days. 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 NPO and EMSL/LV; currently, the acceptable
performance score is seventy percent.
b. Bid Price
The second criterion for laboratory selection is bid price. Following bid opening, bid
abstracts are reviewed and evaluated by NPO and Contracts Management Division (CMD)
officials. The lowest competitive bidders that have received acceptable performance scores
for their PE samples are evaluated for bidder responsibility as detailed below.
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 documentation includes: 1)
functional descriptions and detailed resumes of key personnel, 2) inventory of laboratory
equipment and description of laboratory space, and 3) 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 SOPs to the PO.
b. Laboratory Site Evaluation
NPO, CMD, EMSL/LV and NEIC personnel participate in onsite evaluations of laboratory
facilities of bidders which scored acceptably on the PE sample analyses and are within the
EPA-determined competitive range. The results of the onsite evaluation are considered in
the final determination of bidder responsibility for contract award.
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B. Laboratory Startup Process
Laboratories entering the program undergo a learning curve process during which they
become fully familiarized and obtain expertise in the application of program methodologies
and QC procedures. To reduce the learning curve period, the CLP utilizes a series of
laboratory startup procedures during the laboratory's initial contract operations and whenever
problems are identified during contract performance.
1. Provision of Standards to Laboratory
Immediately following contract award, laboratories are required to order analytical reference
standards from the Agency's contractor-operated QA Materials Bank. These standards are
used by the laboratory to verify laboratory supplied standards throughout contract
performance. Chapter VI, Section A provides further information on analytical standards.
2. PO Review of First Data Packages
Initial data packages are targeted for immediate review and evaluation by the PO, EMSL/LV
and the Region. This intensive review focuses on any problems the laboratory may have in
applying methodologies or in reporting data. The PO and DPO 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 PO or DPO may visit the laboratory facility and work onsite with
laboratory personnel to rectify problems.
3. PO/DPO/SMO/Laboratory Communication
Telephone communication is the most widely applied method for problem-solving and
maintaining efficient laboratory operations 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 or any difficulties
encountered in analysis. SMO routinely resolves sample-related problems in coordination
with the Regional client and refers technical problems to the PO or DPO, 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 Case record. The laboratory also records the problem and resolution in the
narrative portion of the sample data report so that the Region will consider this information
when evaluating and using the data.
C. Laboratory Performance Evaluation
1. Performance Evaluation Sample Analysis
On a quarterly basis, EMSL/LV distributes PE samples to contract laboratories for analysis.
EMSL/LV then evaluates the laboratories' PE sample data, and the NPO uses this evaluation
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in formally assessing laboratory contract performance. Additionally, EMSL/LV enters PE
sample 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 criteria. Refer to
Chapter VI, Section C for a more detailed description of PE samples.
2. Onsite Laboratory Evaluation
Regional, NEIC and EMSL/LV personnel visit each contract laboratory facility in order to
evaluate laboratory procedures. The frequency of onsite evaluation depends, in part, upon
laboratory performance. The NPO utilizes the evaluation reports which result from these
onsite visits in identifying and remedying laboratory performance problems. Chapter VI,
Section E details the onsite laboratory evaluation process.
3. Corrective Action
The PO and DPO work closely 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. 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 CMD 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 delineates the Government-accepted recovery plan that the Contractor must
follow to avoid contract termination. The recovery plan includes 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 Government's next and
final step may be contract termination for default. In addition to terminating the laboratory's
contract, this action affects the evaluation of the laboratory's responsibility for award under
future CLP solicitations.
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CHAPTER VI
PROGRAM QUALITY ASSURANCE
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CLP User's Guide Chapter 6
Quality assurance (QA) and quality control (QC) are integral parts of the CLP. The QA process
consists of management review and oversight at the planning, implementation, and completion
stages of environmental data collection. The QA process ensures that the data provided is of
the quality required. The QC process includes the 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 collection effort, QA activities ensure that
the QC system is functioning effectively, and that the deficiencies 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 QA/QC program includes internal laboratory QC criteria that must be met at
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 EMSL/LV. Blind performance samples, magnetic tape
audits and laboratory onsite evaluations provide an external QA reference for CLP. A feedback
loop supplies the results of the various review functions to the contract laboratories through
direct communication with the POs and DPOs. The following sections describe overall QA/QC
operations and how the CLP meets the QA/QC objective.
A. Laboratory Quality Control Criteria
1. Standard Operating Procedures
In any operation that is performed on a repetitive basis, assurance of data quality and
reproducibility is best accomplished through the use of SOPs. All SOPs, as prepared and
presented to the Agency by the Contractor, reflect activities as they are currently performed in
the laboratory. In addition, laboratory SOPs:
o Are consistent with current EPA regulations, guidelines, and CLP contractual
requirements.
o Are consistent with instrument manufacturers' specific instruction manuals.
o Are available to EPA personnel during an onsite laboratory evaluations.
o Provide documentation that is sufficiently complete to record the performance of all
tasks required by the analytical protocol.
o Demonstrate the validity of data reported by the Contractor and explain the cause of
missing or inconsistent results.
o Describe the corrective measures and feedback mechanisms utilized when analytical
results do not meet protocol requirements.
o Are updated as necessary when contract, facility, or contractor procedural
modifications are made.
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Program Quality Assurance December 1988
o Are archived for future reference in usability or evidentiary situations.
o Have the appropriate portions available at the appropriate work stations.
o Are subject to a document control procedure which precludes the use of outdated or
inappropriate SOPs.
The Agency requires SOPs for sample storage and preparation, glassware cleaning, calibration,
analytical procedures and standards, maintenance activities, and data reduction, documentation
and validation procedures. In addition, evidentiary SOPs are required as stated in each
analytical Statement of Work. The SOP format may vary depending upon the kind of activity
for which the SOP is prepared.
Following contract award, the laboratory sends a complete set of SOPs to the DPO, EMSL/LV
(quality assurance SOPs) and NEIC (evidentiary SOPs). Once SOPs have been submitted, the
laboratory is responsible for providing any revised or new SOPs to the DPO, EMSL/LV and
NEIC, as appropriate.
2. Quality Assurance Plan
Each contract laboratory establishes a QA program with the objective of providing sound
analytical chemical measurements. The program incorporates the QC procedures, any necessary
corrective action, and all documentation required during data collection as well as the quality
assessment measures performed by management to ensure acceptable data production. As
evidence of such a program, the Contractor prepares a written Quality Assurance Plan (QAP)
which achieves the following:
o Maintains data integrity, validity and usability.
o Ensures that analytical measurement systems are maintained in an acceptable state of
stability and reproducibility.
o Ensures a consistent number of qualified personnel sufficient to meet contract
requirements and deliver the product in a timely fashion.
o Detects problems through data assessment and establishes corrective action procedures
which keep the analytical process reliable.
o Documents all aspects of the measurement process in order to provide data which are
technically sound and legally defensible.
The QAP presents the policies, organization, objectives, functional guidelines, and specific
QA/QC activities designed to achieve the data quality requirements in the analytical contract.
Elements of a QAP include organization and personnel, facilities and equipment, document
control, analytical methodology, data generation, and QA/QC. Where applicable, the Contractor
includes or references SOPs pertaining to each element as part of the QAP. In addition, the
QAP is available during onsite laboratory evaluations. Appendix F contains references relevant
to the preparation of a QAP.
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CLP User's Guide Chapter 6
3. Analytical Standards Traceability Requirements
As an element of overall QA, the Agency has established a repository of analytical standards
and calibration materials for use in the CLP. All analytical data generated by the CLP are
required to be traceable to EPA Repository standards. Traceability must be applied by the
contract laboratories to all calibration and QC solutions used to generate data for CLP
requirements. Standards supplied by the EPA Repository are provided for the purpose of
traceability only and are not routinely used as working standards. Each contract laboratory is
responsible for establishing its own specific standards traceability program.
After contract award, the Contractor is required to request a series of calibration and QC
solutions from the EPA Repository. In response, the EPA Repository supplies ampoules
containing single or multiple analyte solutions. All ampoules are labeled with a lot number,
date of preparation, component concentration(s), and solvent(s). The Contractor retains the
EPA Repository standards in such a manner as to preserve their integrity. At present, storage
at 4°C is required.
Contract laboratories prepare working standards from material obtained from EPA or from
commercial sources. Laboratory working standards are not provided by the EPA Repository.
Whenever new laboratory working standards (calibration or QC solutions) are prepared, the
Contractor demonstrates equivalence of each batch of standards by providing traceability
directly to a dilution of an EPA Repository standard. The EPA Repository standard and the
laboratory working standard are analyzed by the conditions specified in the analytical Statement
of Work. Verification of traceability includes qualitative and quantitative criteria, and specific
requirements are system dependent (i.e. GC, GC/MS).
To demonstrate that the laboratory working standards have not degraded while in use, the
Contractor compares the working standard concentration against EPA Repository standards
according to the traceability requirements described in the Statement of Work. If the laboratory
working standard does not meet the quantitative traceability requirements, a new working
standard is prepared.
Records and raw data for all standard solution traceability verification include signed and dated
logbooks with sufficient information to trace the analysis of a sample, or analyte, to a specific
pair of working and EPA Repository standards. Thus a standard chain-of-custody exists
creating documentation that verifies the acceptability of qualitative and quantitative
determinations based on a specific standard lot.
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 CCS review identifies contractual
discrepancies; EMSL/LV review determines technical quality and consistency; and Regional data
review relates usability of the data to a specific site.
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Program Quality Assurance December 1988
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 results are used in conjunction with other information
to measure overall contractor performance and to take appropriate actions to correct
deficiencies in performance.
Upon receipt, SMO screens every RAS CLP-generated data package on a fast-turnaround basis.
To ensure a uniform review, a set of standardized procedures have been developed to evaluate
the sample data package against the technical and completeness requirements of the contract.
The following key areas are reviewed for compliance with the contract: holding times, GC/MS
tunes, initial and continuing calibrations, blanks, surrogate recoveries, and matrix spikes and
matrix spike duplicates.
CCS results are distributed to the Contractor and all other data recipients. If any problems with
the data package are identified, the Contractor has a period of time to correct the deficiencies,
send all corrections to SMO, EMSL/LV and the Regional client, and include the corrected
resubmittals in the purge of their Case files.
2. EMSL/LV Data Review
Periodically, EMSL/LV performs a comprehensive QA audit on a subset of CLP sample data
packages using a Mil. Standard 105D approach. EMSL/LV also provides data audits and data
evaluation, and participates in special projects (e.g., Dioxin Incineration Study, Love Canal
Habitability Study) and special requests such as enforcement support, and preparation and
evaluation of data review SOPs.
In addition, EMSL/LV and the NPO manage the program's QA and Results Database. This
database includes spike recoveries, blanks, duplicates, tuning, calibration, method of standard
additions, ICP check, and analytical results. These data are statistically evaluated and utilized
to determine and update contract QC acceptance windows for CLP-generated data and to
characterize laboratory, method and program performance.
3. Regional Data Review
Contract laboratory data are generated to meet the specific needs of the Regional client. In
order to verify the usability of data for the intended purpose, each Region reviews data from
the perspective of end-user based upon functional aspects of data quality. As the bases for
data evaluation, the Region uses general guidelines for data review that have been developed
jointly by the Region and the NPO. Individual Regions may augment the basic guideline
review process with additional review based on Region-specific or site-specific concerns.
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CLP User's Guide Chapter 6
C. Quarterly Blind Performance Evaluation Samples
As a means of measuring contractor and method performance, contract laboratories participate
in interlaboratory comparison studies conducted by the Agency. Results from the analysis of
PE samples are used by the Agency to verify the contractors' 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 laboratories on a quarterly basis as either single
blind (recognizable as PE material and of unknown composition) or double blind (not
recognizable as PE material and of unknown composition) samples. 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, quantitation, and sample
contamination. Confidence intervals for the quantitation of target compounds are based on
reported values using population statistics. Contractors are required to use the NBS 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.
If a Contractor performs unacceptably, the PO or DPO will notify the Contractor concerning
the remedy for their unacceptable performance. A Contractor may expect, but the Agency is
not limited to, the following actions: reduction of the number of samples sent under the
contract, suspension of sample shipment to the Contractor, a site visit, a full data audit, and/or
analysis of remedial PE samples.
D. GC/MS Tape Audits
In order to accomplish tape audits, the Agency periodically requests the GC/MS magnetic tapes
corresponding to a specific Case. 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 onsite audits, and specific Regional requests.
Depending upon the reason for an audit, the tapes from a recent Case, a specific Case, or a
performance 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 hard
copy/floppy diskettes with the data generated on the GC/MS tapes. This function provides
external monitoring of program QC requirements and checks contractor adherence to internal
QA procedures. In addition, tape audits enable the Agency to evaluate the utility, precision,
and accuracy of the analytical methods.
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Program Quality Assurance December 1988
The GC/MS tape includes raw data and quantitation reports for samples, blanks, matrix spikes,
matrix spike duplicates, initial calibrations, continuing calibration, BFB and DFTPP associated
with the requested Case. In order to reference raw data to the delivered hard copy, the GC/MS
tape submission also includes user-generated spectral libraries, extraction laboratory bench
sheets, analysts' laboratory notebook pages, and instrumental reference logbook pages associating
the tape files to the raw data files.
£. Onsite Laboratory Evaluations
At a frequency dictated by a contract laboratory's performance, the PO or an authorized
representative conducts an onsite laboratory evaluation in order to monitor the Contractor's
ability to meet contract terms and conditions. The evaluation process incorporates two separate
categories, a QA evaluation and an evidentiary audit.
1. Quality Assurance Onsite Evaluation
QA evaluators inspect contractor facilities to verify the adequacy and maintenance of
instrumentation, the continuity of personnel meeting training requirements, and the acceptable
performance of analytical and QC procedures. Items that are evaluated include, but are not
limited to, the following:
o Size and appearance of the facility.
o Quantity, age, availability, scheduled maintenance and performance of instrumentation.
o Availability, appropriateness, and utilization of SOPs.
o Staff qualifications, experience, and personnel training programs.
o Reagent, standards, and sample storage facilities.
o Standard preparation and traceability logbooks and raw data.
o Bench sheets and analytical logbook maintenance and review.
Prior to an onsite 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 onsite reports, PE scores, Regional review of data, Regional QA
materials, GC/MS tape audit reports, CCS results, and data trend reports.
2. Evidentiary Audit
Evidence auditors conduct an onsite laboratory evaluation to determine if laboratory policies
and procedures are in place to satisfy evidence handling requirements as stated in the Statement
of Work. The evidentiary audit is comprised of the following three activities: the procedureal
audit, the written SOPs audit, and the analytical project file audit. The procedural audit
consists of review and examination of actual standard operating procedures and accompanying
documentation. The written SOPs audit determines accuracy and completeness of the written
SOPs. The procedural and written SOPs audits are conducted for the following laboratory
operations: sample receiving, sample storage, sample identification, sample security, sample
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CLP User's Guide Chapter 6
tracking (from receipt to completion of analysis) and analytical project file organization and
assembly. The analytical project file evidence audit consists of review and examination of the
analytical project file documentation. The auditors review the files to determine the accuracy
of the document inventory, the completeness of the file, the adequacy and accuracy of the
document numbering system, traceability of sample activity, identification of activity recorded
on the documents, and error correction methods.
3. Discussion of the Onsite Team's Findings and Corrective Action Reports
The QA and evidence auditors discuss their findings with the PO/DPO prior to debriefing the
Contractor. During the debriefing, the auditors present their findings and recommendations for
corrective actions necessary to the contractor personnel.
Following the evaluation, QA and evidentiary audit reports which discuss deficiencies found
during the onsite are forwarded to the Contractor. The Contractor must discuss the corrective
actions taken to resolve the deficiencies discussed during the onsite visit and in the onsite
reports in a letter to the PO, DPO, EMSL/LV (response to the QA report) and NEIC (response
to the evidentiary report) within a specified length of time. If SOPs are required to be written
or amended, the Contractor must provide the SOPs to the DPO, EMSL/LV (QA/technical SOPs)
and NEIC (evidentiary SOPs).
If the Contractor fails to take appropriate corrective action to resolve the deficiencies, a
Contractor may expect, but the Agency is not limited to, the following actions: reduction of
the number of samples sent under the contract, suspension of sample shipment to the
contractor, a follow-up site visit, a full data audit, and/or analysis of remedial PE samples.
F. Quality Assurance and Data Trend Analysis
The QC prescribed in the analytical methods provides information that is continually used by
the Agency to assess sample, contractor and program data quality via data trend analysis.
Statistical reports that evaluate specific anomalies or disclose trends in many areas are generated
from a computerized database. These areas include surrogate spike recovery, matrix
spike/duplicate spike recovery, method blanks, GC/MS tuning and mass calibration, initial and
continuing calibration data, and other QC and method parameters.
Program-wide statistical results are used to rank laboratories in order to observe the relative
performance of each contractor in a given protocol against its peers. The reports are also used
to identify trends within laboratories. The results of many of these trend analyses are included
in overall evaluation of a contractor's performance, and are reviewed to determine if corrective
action or an onsite 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 QC levels, and to provide an early
warning of contractor QA/QC problems which may not be apparent from the results of an
individual Case.
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Program Quality Assurance December 1988
As a further benefit to the CLP, the database provides the information needed to establish
performance-based criteria in updated analytical protocols. The 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 QC and performance
criteria specifications of what is routinely achievable and expected of environmental chemistry
laboratories in mass production analysis of environmental samples. These specifications assist
the Agency in meeting its objectives of obtaining data of known and documented quality.
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APPENDIX A
LIST OF ACRONYMS
AA Atomic Absorption
AOB Analytical Operations Branch
AR Authorized Requestor
B/N/A Base, Neutral, Acid
CCS Contract Compliance Screening
CEAT Contractor Evidence Audit Team
CERCLA Comprehensive Environmental Response, Compensation and Liability Act
CLP Contract Laboratory Program
CMD Contracts Management Division
CO Contracting Officer
CR Cost Recovery
CRQL Contract Required Quantitation Limit
DPO Deputy Project Officer
DR Delivery Request
DSR Dioxin Shipment Record
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 Silica Capillary Column
GC/EC Gas Chromotography/Electron Capture
GC/MS Gas Chromotography/Mass Spectrometry
HRGC High Resolution Gas Chromotography
HRMS High Resolution Mass Spectrometry
HSED Hazardous Site Evaluation Division
ICP/MS Inductively Coupled Plasma/Mass Spectrometry
IDL Instrument Detection Limit
IFB Invitation for Bid
LCS Laboratory Control Sample
NBS National Bureau of Standards
NEIC National Enforcement Investigations Center
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
PCB Polychlorinated Biphenyl
PE Performance Evaluation
PEST Pesticides
PL ' Packing List
PO Project Officer
QA Quality Assurance
QAP Quality Assurance Plan
QC Quality Control
RAS Routine Analytical Services
REM Remedial Action Team
RSCC Regional Sample Control Center
SARA Superfund Amendments and Reauthorization Act
A-l
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List of Acronyms (cont'd.)
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 Semivolatile
TAT Technical Assistance Team
TCL Target Compound List
TIC Tentatively Identified Compound
TR Traffic Report
VOA Volatile
A-2
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APPENDIX B
CLP DIRECTORY
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CLP NATIONAL PROGRAM OFFICE
DECEMBER 1988
USEPA ANALYTICAL OPERATIONS BRANCH (OS-230)
401 M Street, S.W.
Room M-2624
Washington, DC 20460
202/382-7906 FTS 382-7906
Joan Barnes, Branch Chief
202/382-7906 FTS/382-7906
Lynn Beasley, ESAT Project Officer, Regional Operations Section
202/475-8607 FTS 475-8607
Emile Boulos, CLP Project Officer, Organics Section
202/382-7942 FTS 387-7942
Angelo Carasea, CLP Project Officer, Organics Section
202/382-7911 FTS 382-7911
Mike Carter, Chief, Regional Operations Section-SMO Project Officer
202/382-7909 FTS 382-7909
Carla Dempsey, QA Coordinator
202/382-5746 FTS 382-5746
Joan Fisk, National Organics Program Manager-Chief, Organics Section
202/382-3115 FTS 382-3115
Howard Fribush, CLP Project Officer, Organics Section
202/382-2239 FTS 382-2239
Michael Hurd, CLP Project Officer, Inorganics Section
202/382-7908 FTS 382-7908
Bill Langley, National Inorganics Program Manager-Acting Chief, Inorganics Section
202/382-7906 FTS 382-7906
Mary Mahsetky, CLP Program Technician
Sylvia Miller, Branch Secretary
Rona Haley, Secretary, Organics Section
USEPA CONTRACTS MANAGEMENT DIVISION (MD-33)
Alexander Drive
Res. Tri. Park, NC 27711
Frank Rzasa, Deputy Director
919/541-3046 FTS 629-3046
Marian Bernd, Solicitations and Contract Awards
202/382-0532 FTS 382-0532
Janet Simmons, Contract Placement
919/541-4081 FTS 629-4081
Larry Presnell, Contract Administration
919/541-3166 FTS 629-3166
B-l
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USEPA ENVIRONMENTAL MONITORING SYSTEMS LABORATORY (EMSL/LV)
944 East Harmon Avenue
Las Vegas, NV 89109
(Mailing Address: P.O. Box 93478, Las Vegas, NV 89193-3478)
Data To: EMSL/LV Executive Center
944 East Harmon Ave.
Las Vegas, NV 89119
Attn: Data Audit Staff
Llewellyn Williams, Director, QA Division
702/798-2103 FTS 545-2103
Steve Billets, Deputy Director, QA Division
702/798-2609 FTS 545-2609
Jim D. Petty, Chief, QARB, QAD
702/798-2383 FTS 545-2383
Larry Butler, Research Chemist, QARB, QAD
702/798-2114 FTS 798-2114
Edward Kantor, Chemist, QARB, QAD
702/798-2690 FTS 545-2690
Harold Vincent, Chemist, QARB, QAD
702/798-2129 FTS 545-2129
Dave Bottrell, Chemist, QAD (Organics Method Contract)
702/798-2142 FTS 545-2142
William Newberry, Chemist, QARB, QAD (Inorganics Method Contract)
702/798-2167 FTS 545-2167
Gareth Pearson, Director, Exposure Assessment Research Division
702/798-2203 FTS 545-2203
Bob Schonbrod, Exposure Assessment Research Division
702/798-2229 FTS 545-2229
Lou Blume, Exposure Assessment Research Division
702/798-2213 FTS 545-2213
Gene Meier, Director, Adv. Monitoring Division
702/798-2203 FTS 545-2203
USEPA NATIONAL ENFORCEMENT INVESTIGATIONS CENTER (NEIO
Denver Fed. Cntr. 53, E-2
P.O. Box 25227
Denver, CO 80225
303/236-5111 FTS 776-5111
Tom Gallagher, Director
303/236-5100 FTS 776-5100
Carroll G. Wills, Deputy Director
303/236-5120 FTS 776-5120
Ted Meiggs, Assistant Director, Lab Services
303/236-5132 FTS 776-5132
Joe Lowry, Chief, Environmental Chemistry Branch
303/236-9963 FTS 776-5122
Dean Hill, Pesticides
303/236-8138 FTS 776-8138
B-2
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Gerri Hilden, Evidence Audit (Chain of Custody)
303/236-5122 FTS 776-5122
Donald Roche, Audit Rep. (Primary Contact)
303/236-5122 FTS 776-5122
Robert Laidlaw, Enforcement
303/236-5111 FTS 776-5111
USEPA ENVIRONMENTAL MONITORING SYSTEMS LABORATORY
(EMSL/CINCINNATD
26 W. Martin Luther King Dr.
Cincinnati, OH 45268
Thomas A. Clark, Acting Lab Director
513/569-7301 FTS 684-7301
Gerald D. McKee, Acting Deputy Lab Director
513/569-7303 FTS 684-7303
Bill Budde, Chief, Adv'd. Instrumentation-CLP Specialist
513/569-7309 FTS 684-7309
Ed Berg, Chief, Project Mgmt. Section-Performance Evaluation
513/569-7325 FTS 684-7325
James J. Lichtenberg, Chief, Phys. & Chem. Methods Branch
513/569-7306 FTS 684-7306
John A. Winter, Chief, QA Branch
513/569-7325 FTS 684-7325
Tom Bellar, Research Chemist
513/569-7512 FTS 684-7512
Ted Martin, Inorganic Chemist-Methods Development
513/569-7312 FTS 684-7312
FIELD CONTRACTORS - MAIN OFFICE;
NUS Corporation (FIT II - East)
1300 North 17th Street
Suite 1320
Arlington, VA 22209
703/522-8802
Paul Clay
Tom Centi
Ecology & Environment (FIT II-West)
1700 North Moore Street
Rosslyn Center
Arlington, VA 22209
703/522-6065
Lou Welzel
Wendell Fields
B-3
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COM Federal Programs Corp. (REM II)
13135 Lee Jackson Mem Hwy
Suite 200
Fairfax, VA 22033
703/968-0900
Gary Dunbar
Steve Paquette
Andy Szilagyi
Ebasco Services. Inc. (REM HI)
Zone Program Management Office
2000 Fifteenth St., North
Arlington, VA 22201
703/558-7555
Michael Yates
CH2M Hill. Inc. (REM IV)
625 Herndon Parkway
Herndon, VA 22070
703/471-1441
Kent Robinson
B-4
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SAMPLE MANAGEMENT OFFICE DIRECTORY
November 1988
Mailing Address: Street Address:
CLP Sample Management Office Viar and Company, Inc.
P.O. Box 818 209 Madison Street, #200
Alexandria, Virginia 22313 Alexandria, Virginia 22314
703/557-2490 FTS 557-2490 703/684-5678
DAVID H. STEWART
SMO PROJECT DIRECTOR
Don Trees, Program Manager Data Processing and Scientific Services
Peter Isaacson, Project Manager
Scientific Support Groups (SSG)
Sa'ad Masri, Project Leader Contract Compliance Screening (CCS)
Inorganics & Organics
Dipti Singh, QA Chemist CCS Organics
Fida Abdelwahab, QA Chemist CCS Inorganics
Paul Ssenyonga, Data Systems Coordinator CCS Diskette Deliverables
Harry McCarty, Project Leader Data Review & Method Development
Marianne Lynch, Chemist Method Development
Bill Eckel, Chemist Data Review
Ruth Bleyler, QA Chemist Regional QA/QC Support
R. Richard Thacker, Program Manager SMO Operations/Management Planning
Linda Boynton, Project Manager
Analytical Services Group (ASG)
Lulu Eager, Senior Bookkeeper SAS Invoice Processing
Maka Grogard, Senior Environmental Program Analyst Operations - ASG
Coordination & Implementation of CLP
Sample Scheduling & Tracking Systems
Sean Kolb, Environmental Program Analyst
Lynn Riddick, Environmental Program Coordinator Region VIII
Diane Cutler, Environmental Program Coordinator Region II
Jeb Livingood, Environmental Program Coordinator Region VI, V SAS
Cindy Schreyer, Environmental Program Coordinator Region I, V RAS
Susan Barrell, Environmental Program Coordinator (TBA)
B-5
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(Analytical Services Group continued)
Carol Shaeffer, Environmental Program Analyst
Terri Shaughnessy, Environmental Program Coordinator Region III
Karen Elm, Environmental Program Coordinator Region IX
Tom Sigler, Environmental Program Coordinator Region IV, VII
Anne Babyak, Environmental Program Coordinator (TEA)
Leslie Braun, Environmental Program Analyst Management Information Systems - ASG
Hoang Ho, MIS Coordinator SAM & SAS Data Base
Sally Boyar, MIS Coordinator Contract Funding Status System &
Distribution of Program Lists
Michelle Kosloski, MIS Coordinator Extract Disposal System &
Backlog Inventory
Deborah Miller, Project Manager
Program/Contracts Support Group (P/CSG)
Mike Tindle, Environmental Program Analyst Computer Systems Documentation,
IFB/Procurement Support
Talia Peters, Sr. Environmental Program Coordinator IF B/Procurement Development
Heidi Janss, Environmental Program Coordinator Computer Systems Documentation
IFB/'Procurement Support
Susan Wilkins, Environmental Program Coordinator Meeting Coordination
IFB/Procurement Support
Peter Ziu, Environmental Program Coordinator Bottle Repository Support,
Automated Address System
Cheryl Shriver, Environmental Program Coordinator Meeting Coordination
Materials Distribution
Tina DeYoung, Project Manager
Management Information Group (MIC)
(Ad Hoc Requests & Annual Site/Cost Accounting)
Tina Rodgers DPO Reports & Blue Book Reports
Pam Werntz Simons, Management Information Systems Manager Site/Cost Accounting,
Invoicing, Reconciliation, Closeout, Data Control
Rhonda Harmon Task Manager, Payment Activities
John Reynolds Team Leader, Payment Processing
Marta Meixner Team Leader, Payment Processing
B-6
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USEPA REGION I
USEPA Region I, ESD
60 Westview Street
Lexington, MA 02173
617/860-4320
Mary Ann Becker, Communications Contact (ESAT)
617/860-4612
John Carlson, ESAT DPO
617/860-4320
Edward Conley, Director, ESD
617/860-4320
Elio Goffi, Communications Contact (Alt)
617/860-4630
Vicki Howell, Communications Contact (Alt - ESAT)
617/229-2050
Thomas Spittler, Chief, Technical Support Branch
617/860-4320
Deb Szaro, Technical DPO, Communications Contact
617/860-4312
USEPA Region I, WMD
J.F. Kennedy Federal Bldg
Boston, MA 02203
(Data Submission: JFK. Federal Bldg; Room 1903)
Rosalie Baldassari, Primary RSCC-Data Submission
617/573-5798 FTS 833-1798
Merrill Hohman, SF Coordinator-Director, Waste Mgmt. Div.
617/573-5700 FTS 833-1700
Susan Willis, Non-Primary RSCC
617/573-5607 FTS 833-1607
Camp Dresser & McKee, Inc. (REM II)
1 Center Plaza
Boston, MA 02108
617/742-5151
Jim Occhialini
Ebasco (REM III)
211 Congress St.
8th floor
Boston, MA 02110-2410
617/451-1201
Russ Boyd
Lee Dixon
B-7 12-15-88
-------
USEPA Region I (cont'd)
NUS Corporation (FIT II)
19 Crosby Drive
Bedford, MA 01730
617/275-2970
Martha Lee
B-8 12-15-88
-------
USEPA REGION II
USEPA Region II
26 Federal Plaza
New York, NY 10278
Stephen Luftig, SF Coordinator-Director, Emerg. & Remed. Response
212/264-1574 FTS 264-1574
USEPA Region II, ESD
Woodbridge Avenue
Building 209
Edison, NJ 08837
Darvene Adams, Non-Primary RSCC
201/321-6705 FTS 340-6705
Lou Bevilacqua, Chief, Toxic & Haz. Waste-Technical DPO
201/321-6702 FTS 340-6702
Lisa Gatton-Vidulich, Technical DPO (Alt)
201/321-6676 FTS 340-6676
Stelios Gerazounis, Dioxin Contact
201/321-6778 FTS 340-6718
Amelia Jackson, Organics Contact
201/321-6164 FTS 340-6164
Leon Lazarus, Data Review-Organics Contact (Alt)
201/321-6778 FTS 340-6778
Dan Lillian, Chief, Tech. Support Branch-ESAT DPO-Lab Director
201/321-6707 FTS 340-6707
Gayatri Mehta, ESAT Non-Primary RSCC
201/321-6705 FTS 340-6705
Frank Messina, Inorganics Contact
201/906-6170 FTS 340-6170
Barbara Metzger, Director, ESD
201/321-6754 FTS 340-6754
Regina Odubo-Sullivan, ESAT Primary RSCC
201/321-6705 FTS 340-6705
Laura Scolise, Inorganics Contact (Alt)
201/906-6717 FTS 340-6717
Richard Spear, Chief, Surv. & Monitoring Branch-Data Submission
201/321-6685 FTS 340-6685
Sharon Steltz, Primary RSCC
201/321-6705 FTS 340-6705
Dan Sullivan, Deputy Director, ESD
201/321-6755 FTS 340-6755
B-9 12-15-i
-------
USEPA Region II (conI'd)
NUS Corporation (FIT II)
Raritan Plaza III
Fieldcrest Avenue
Edison, NJ 08837
201/225-6160
Roberta Riccio, Primary Sampling Contact
B-10
-------
USEPA REGION III
USEPA Region HI, CRL
839 Bestgate Road
Annapolis, MD 21401
301/266-9180
John Austin, Organic Chemist
301/266-9180
Diana Baldi, ESAT DPO-Dioxin & Organics (Alt) Contact
301/266-9180
Dan Donnelly, Acting Chief, Lab Section
301/266-9180
Jeanne Hankins, Inorganics Contact
301/266-9180
Patricia Krantz, Section Chief, QA/QC-Data Submission
301/266-9180
Annette Lage, Non-Primary RSCC
301/266-9180
Chuck Sands, Technical DPO-Organics & Dioxin (Alt) Contact
301/266-9180
John Scalera, Organics Contact (Alt)
301/266-9180
Orteria Villa, Jr., Director, CRL
301/266-9180
Colleen Walling, Primary RSCC
301/266-9180
Claudia Walters, Inorganics Contact (Alt)
301/266-9180
USEPA Region III, SF Branch
841 Chestnut Street
Philadelphia, PA 19107
Catherine Hodgkiss, Chief, CERCLA Enforcemetnt Section
215/597-8177 FTS 597-8177
Green Jones, Director, ESD
215/597-4532 FTS 597-4532
Neil Swanson, Acting Chief, CERCLA Remedial Enforcemet
215/597-3186 FTS 597-3186
Thomas Voltaggio, SF Coordinator
215/597-8132 FTS 597-8132
Stephen Wassersug, Director, Waste Mgmt. Div.
215/597-8131 FTS 597-8131
Ebasco Services, Inc. (REM III)
One Oxford Valley
Suite 414
Langhorne, PA 19047-1829
215/752-0212
Carol Chatelain
Anthony Enweze
B-ll 12-15-88
-------
USEPA Region III (cont'd)
NUS Corporation (FIT II)
999 West Valley Road
Wayne, PA 19087
215/687-9510
Eric Blischke, Primary Requestor
Russ Sloboda, Chemist-Data Reviewer
Donna Wallace, Director
NUS Corporation (REM III - ARCS)
Park West Two
Cliff Mine Road
Pittsburgh, PA 15275
412/788-1080
Greg Zimmerman
Roy F. Weston, Inc. (REM II)
1 Weston Way
West Chester, PA 19380
213/692-3030
Ralph Shapot
Weston-SPER (TAT)
53 Haddon Field Road
Suite 306
Cherry Hill, NJ 08002
609/482-0222
Bhupi Khona
B-12 12-15-88
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USEPA REGION IV
USEPA Region IV
Superfund Branch
345 Courtland St., N.E.
Atlanta, GA 30365
Jack Stonebraker, SF Branch Chief
404/347-2967 FTS 257-2967
Patrick Tobin, Director, Waste Mgmt. Division
404/347-3454 FTS 257-3454
USEPA Region IV, ESD (ASB)
Analytical Support Branch
College Station Road
Athens, GA 30613
Gary Bennett, Secondary Communications Contact
404/546-3286 FTS 250-3286
Tom B. Bennett, Jr., Technical DPO-Chief, Org. Chem. Sctn.-Data Submission
404/546-3112 FTS 250-3112
Bobby Carroll, ESAT DPO-Chief, ASB
404/546-3309 FTS 250-3309
Debbie Colquitt, Non-Primary RSCC
404/546-3388 FTS 250-3388
James Finger, Director, ESD
404/546-3136 FTS 250-3136
Sandy Fitzgerald, Receptionist
404/546-3111 FTS 250-3111
Charles Hooper, Primary Communications Contact
404/546-3286 FTS 250-3286
Myron Stephenson, Non-Primary RSCC
404/546-3385 FTS 250-3385
USEPA Region IV, ESD (ECB)
Env. Compliance Branch
College Station Road
Athens, GA 30613
Steve Hall, RCRA Team Leader
404/546-3173 FTS 250-3173
Doug Lair, Primary RSCC
404/546-3300 FTS 250-3300
Doug Mundrick, SF Team Leader
404/546-3321 FTS 250-3321
Camp Dresser & McKee, Inc. (REM II)
2100 River Edge Parkway
Suite 400
Atlanta, GA 30328
404/952-8643
Tom Duffy
B-13 12-15-88
-------
USEPA Region IV (cont'd)
Ebasco
145 Technology Park
Norcross, GA 30092-2979
404/662-2439
Loring Pitts
NUS Corporation (FIT)
1927 Lakeside Parkway
Suite 614
Tucker, GA 30084
404/938-7710
Phil Blackwell
B-14 12-15-88
-------
USEPA REGION V
USEPA Region V, ESD
536 S. Clark Street
Tenth Floor, CRL
Chicago, IL 60605
Al Alwan
312/353-6619 FTS 353-6619
Pat Churilla, Technical DPO-ESAT DPO
312/353-9087 FTS 353-908/
Carsten Falkenburg, Communications Contact (Alt - ESAT)
312/353-2893 FTS 353-2893
Ed Johnson, Organics Contact
312/886-5482 FTS 886-5482
Duane Kruse, Primary Communications Contact (ESAT)
312/353-2893 FTS 353-2893
David Payne, Inorganics Contact (Alt)
312/886-1973 FTS 886-1973
Jan Pels, Primary RSCC
312/353-2720 FTS 353-2720
Ray Piccione
312/886-1974 FTS 886-1974
Curtis Ross, Director, CRL-Data Submission
312/353-8370 FTS 353-8370
William Sanders, III, Director, ESD
312/353-3808 FTS 353-3808
Nidia Seliciano
312/886-0651 FTS 886-0651
Jay Thakkar, Inorganics Contact
312/886-1972 FTS 886-1972
Ira Wilson, Primary Communications Contact (ESAT)
312/353-2893 FTS 353-2893
Thomas Yeates, Deputy Director, ESD
312/353-3808 FTS 353-3808
USEPA Region V, WMD
230 S. Dearborn St.
13th Floor (HR-13)
Chicago, IL 60604
312/353-8370 FTS 353-8370
Basil Constantelos, Director, Waste Mgmt. Div.
312/886-7579 FTS 886-7579
William Miner, SF Enforcement
312/886-4658 FTS 886-4658
B-15 12-15-88
-------
USEPA Region V (cont'd)
CH2M Hill, Inc. (REM IV)
310 W. Wisconsin Ave.
Suite 700
Milwaukee, WI 53201
(Mailing Address: P.O. Box 2090)
414/272-2426
Jeff Keiser, Non-Primary RSCC (RAS only)
Dave Shekoski, Non-Primary RSCC (RAS only)
Shirley Stringer, Non-Primary RSCC (RAS only)
Camp Dresser & McKee, Inc. (REM II)
200 West Adams
Suite 1600
Chicago, IL 60606
312/786-1313
Cynthia Clark, Non-Primary RSCC (RAS only)
Wendy Dewar, Sampling & Analytical Coordinator
Jill Line, Non-Primary RSCC (RAS only)
Ecology & Environment (FIT II)
111 W. Jackson Blvd.
Chicago, IL 60604
312/663-9415
Tom Clyne, Organics & Dioxin Contact (Alt)
Zena Gold-Kaufman, Non-Primary RSCC
Renee Hix-Mays, Sample Coordinator
Michigan Dept. of Nat. Resources
P.O. Box 30028
Lansing, MI 48909
517/373-4825
Denise Grubin, Non-Primary RSCC
Minn. Pollution Control Agency
520 Lafayette Road
St. Paul, MN 55155
612/296-7735
Dave Kouloski, Non-Primary RSCC
Becky Lofgrim, Non-Primary RSCC
B-16 12-15-88
-------
USEPA Region V (cont'd)
Roy F. Weston, Inc. (TAT)
111 N. Canal Street
Suite 855
Chicago, IL 60606
312/993-1067
Eileen Helmer, Non-Primary RSCC (RAS only)
Maureen O'Mara, Non-Primary RSCC (RAS only)
Melodic Sullivan, Non-Primary RSCC (RAS only)
Wisconsin Dept. of Nat. Resources
101 South Webster
3rd Floor, GEF-2
Madison, WI 53703
608/267-5063
Dick Alberg, Non-Primary RSCC-Organics Contact
Maureen McCurdy, Non-Primary RSCC
Kim McCutchen, Non-Primary RSCC-Inorganics Contact
B-17 12-15-88
-------
USEPA REGION VI
USEPA Region VI Laboratory
Monterey Park PI. Bldg. C
6608 Hornwood Drive
Houston, TX 77074
713/953-3425 FTS 526-9425
Diana Ayres, Acting Branch Chief
713/953-3425 FTS 526-9425
William Blanton, Communications Contact (ESAT)
713/953-3425 FTS 526-9425
Victor Chapman, Communications Contact (ESAT)
713/953-3425 FTS 526-9425
Michael Daggett, ESAT DPO-Lab Director-Organics & Dioxin Contact (Alt)
713/953-3425 FTS 526-9425
Mahmond El Feky, Inorganics Contact
713/953-3425 FTS 526-9425
Harry FCreigh, Communications Contact (Alt - ESAT)
713/953-3425 FTS 526-9425
Myra Perez, Primary RSCC
713/953-3425 FTS 526-9425
Melvin Ritter, Organics & Dioxin Contact-Data Submission
713/953-3425 FTS 526-9425
David Stockton, Technical DPO
713/953-3425 FTS 526-9425
USEPA Region VI, ESD
Allied Bank Tower
1445 Ross Avenue
Dallas, TX 75202
214/665-6491 FTS 255-6491
Allyn Davis, Director, Waste Mgmt. Div.
214/665-6491 FTS 255-6491
Charles Gazda, Emergency Response Branch
214/665-6491 FTS 255-6491
Dick McGlothlin, Forms
214/665-6491 FTS 255-6491
Martha McKee, SF Coordinator
214/665-6491 FTS 255-6491
Russell Rhoades, Director, ESD
214/665-6491 FTS 255-6491
Hank Thompson, Non-Primary RSCC
214/665-6491 FTS 255-6491
CH2M Hill, Inc. (REM IV)
6060 South Willow Drive
Greenwood Vill., CO 80111-5112
(Mailing Address: P.O. Box 22508; Denver, CO 80222)
303/771-0900
Jane Grogan, CLP Coordinator
B-18 12-15-88
-------
USEPA Region VI (cont'd)
Ecology & Environment (FIT II)
1509 Main Street
Suite 814
Dallas, TX 75201
214/742-6601
David Anderson, Non-Primary RSCC (RAS only)
Lloyd Collins, Non-Primary RSCC (RAS only)
Jairo Guevera, Non-Primary RSCC (RAS only)
K. Malone, Regional Program Manager
Gene McDonald, FIT Training Coordinator
John Totin, Asst. Regional Program Manager
B-19 12-15-88
-------
USEPA REGION VII
USEPA Region VII
726 Minnesota Avenue
Kansas City, KS 66101
David Wagoner, SF Coordinator-Director, Air & Waste Mgmt. Div.
913/236-2850 FTS 757-2850
USEPA Region VII, ESD
25 Funston Road
Kansas City, KS 66115
913/236-3881 FTS 757-3881
Bill Bunn, CLP QA Chief-Comm Contact (Alt)-ESAT DPO
913/236-3881 FTS 757-3881
Joyce W. Casper, Primary RSCC-Data Submission
913/236-3881 FTS 757-3881
Peggy Cox, Communications Contact (TAT)
913/236-3881 FTS 757-3881
Paul Dougherty, FIT RPO
913/236-3888 FTS 757-3888
Ron McCutcheon, TAT RPO
913/236-3881 FTS 757-3881
Debra Morey, Technical DPO-Communications Contact
913/236-3881 FTS 757-3881
Ron Ross, Inorganics Contact (Alt)
913/236-3881 FTS 757-3881
Loren Thompson, Communications Contact (ESAT)
913/236-3881 FTS 757-3881
CH2M Hill, Inc. (REM IV)
6060 South Willow Drive
Greenwood Vill., CO 80111-5112
(Mailing Address: P.O. Box 22508; Denver, CO 80222)
303/771-0900
Beth Baruth, CLP Coordinator (Alt)
Jane Grogan, CLP Coordinator
B-20 12-15-88
-------
USEPA REGION VIII
USEPA Region VIII Laboratory
Denver Federal Center
Box 25366
Lakewood, CO 80225
Alan Curtis
303/236-5091 FTS 776-5091
Eva Hoffman, Technical DPO-ESAT DPO-Data Submission
303/236-7371 FTS 776-7371
James Lehr, Director, ESD
303/236-5061 FTS 776-5061
Deanna Peterson, Primary RSCC
303/236-7370 FTS 776-7370
Jon Yeagley, Chief, Lab Services Section
303/236-5073 FTS 776-5073
USEPA Region VIII, ESD
Denver Place
Suite 500
Denver, CO 80202-2405
Robert Duprey, Director, Hazardous Waste Management Division
303/293-1720 FTS 564-1720
J. William Geise, Jr., Chief, SF Branch
303/293-1518 FTS 564-1518
Jay Silvernale, SF Program Section
303/293-1518 FTS 564-1518
Judy Wong, SF Enforcement Section
303/293-1520 FTS 564-1520
C.C. Johnson & Malhotra (REM II)
2300 Fifteenth Street
Suite 330
Denver, CO 80202
303/433-6966
Jeff Benson, Dioxin Contact (Alt)
Bill Berning, Non-Primary RSCC (RAS only)
Richard Cheatham, Policy Contact-Inorganics & Organics (Alt) Contact
Jerilyn Guthrie, Non-Primary RSCC (RAS only)
B-21 12-15-88
-------
USEPA Region VIII (cont'd)
CH2M Hill, Inc. (REM IV)
6060 South Willow Drive
Greenwood Vill., CO 80111-5112
(Mailing Address: P.O. Box 22508; Denver, CO 80222
303/771-0900
Dewey Brigham, Non-Primary RSCC (RAS only)
Jane Grogan, Non-Primary RSCC (RAS only)
Dennis Neuman, Inorganics Contact (Alt)
406/994-4822
Jim Schwing, Regional Manager
Ecology & Environment (FIT II)
1776 S. Jackson St.
Suite 200
Denver, CO 80210-3802
303/757-4984
Kent Alexander, Dioxin Contact
Lynn Fischer, Non-Primary RSCC (RAS only)
Steve Ignelzi, Non-Primary RSCC (RAS only)
Randy Perliss, Organics Contact
Stuart Richardson, Regional Program Manager
ICF Technology
P.O. Box 280041
Lakewood, CO 80228-2213
303/236-7412
Regina Rehm, Communications Contact (ESAT)
Jacobs Engineering (TES)
12600 West Coif ax Avenue
Suite A300
Lakewood, CO 80215
303/232-7093
Pam McDevitt, Non-Primary RSCC (RAS only)
Joyce Miyagishima, Non-Primary RSCC (RAS only)
Montana EPA Office
301 South Park
P.O. Drawer 10096
Helena, MT 59626
406/449-5414 FTS 585-5414
Mike Bishop, Regional Project Manager
Eric Fink, Regional Project Manager
James Knoy, Regional Project Manager
Liane Shanklin, Remedial Project Manager
John Wardell, Director, Montana Operations Office
B-22 12-15-88
-------
USEPA REGION IX
USEPA Region IX Laboratory
944 East Harmon Avenue
Las Vegas, NV 89119
James Johnson, Organics Contact
702/798-2118 FTS 545-2118
Ralph Smiecinski, Inorganics Contact
702/798-2117 FTS 545-2117
USEPA Region IX, OPM
215 Fremont Street
San Francisco, CA 94105
(Data Submission: Environ. Serv. Branch, P-3-2)
Karen Bankert, Analytical Specialist
415/974-8856 FTS 454-8856
David Bingham, Team Leader
415/974-8149 FTS 454-8149
Thomas Huetteman, Primary RSCC
415/974-0923 FTS 454-0923
Lester Kaufman, Lab Section Chief
415/974-7484 FTS 454-7484
Kent Kitchingman, Technical DPO-Data Submission
415/974-0924 FTS 454-0924
David Mowday, Deputy Director, OPM
415/974-8189 FTS 454-8189
Lilya Rikshpun, Organics & Inorganics Contact (Alt)
415/974-8801 FTS 454-8801
Terry Stumph, Chief, ESB-ESAT DPO
415/974-7483 FTS 454-7483
Denise Toll, Non-Primary RSCC
415/974-8004 FTS 454-8004
Jeff Zelikson, SF Coordinator-Director, Tox. & Waste Mgmt. Div.
415/974-7460 FTS 454-7460
CH2M Hill, Inc. (REM IV)
2510 Redhill Avenue
Suite A
Santa Ana, CA 92705
714/250-5500
Michael Bitner, Project Engineer
Edward J. Rogan, Project Manager
B-23 12-15-i
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USEPA Region IX (cont'd)
Camp Dresser & McKee, Inc. (REM II)
100 Spear Street
Suite 700
San Francisco, CA 94105
415/495-5009
Eric Hinzd, Regional Manager
John Wondolleck, Principal Engineer
Ebasco Services (REM III)
One Market Plaza
Spear Street Tower #600
San Francisco, CA 94105
415/777-3000
Dale Rowlison, Regional Manager
Jim Wilder, Senior Engineer
Ecology & Environment (FIT II)
160 Spear Street
14th Floor
San Francisco, CA 94105
415/777-2811
P. K. Chattopadhyay, Data Review Coordinator-Dioxin Contact (Alt)
Ron Karpowitz, FIT Leader
John Moe, Sampling Advisor
ICF Technology
160 Spear Street
Suite 1380
San Francisco, CA 94105-1535
415/957-0110
Santiago Lee, Dioxin & Organics (Alt) Contact
Greg Nicholl, Inorganics Contact (Alt)
B-24 12-15-88
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USEPA REGION X
USEPA Region X Laboratory
P.O. Box 549
Manchester, WA 98353
(Shipping: 7411 Beach Dr. East, Port Orchard, WA 98366)
206/442-0370 FTS 399-0370
Raleigh Farlow, Secondary Communications Contact
206/442-1193 FTS 399-1193
Mike Johnston, Chief, Lab Section
206/442-0370 FTS 399-0370
Gerald Muth, Technical DPO-ESAT DPO-Organics Contact (Alt)
206/442-0370 FTS 399-0370
USEPA Region X, ESD
1200 Sixth Avenue
M/S 329
Seattle, WA 98101
(Data Submission: Mail Stop ES/096)
206/442-1200 FTS 399-1200
Robert Courson, Director, ESD
206/442-0404 FTS 399-0404
Joyce Crosson, QA Specialist-Data Submission-Non Primary-RSCC
206/442-2111 FTS 399-2111
Charles Findley, Director, Waste Mgmt. Div.
206/442-1200 FTS 399-1200
Phil Millam, SF Coordinator
206/442-1090 FTS 399-1090
John Osborn, FIT RPO
206/442-0837 FTS 399-0837
Kelsey Ramey, Non-Primary RSCC
206/442-4323 FTS 399-4323
William Schmidt, Chief, Field Oper. & Tech. Support Branch
206/442-1526 FTS 399-1526
Rhonda Wregglesworth, Primary RSCC
206/442-7121 FTS 399-7121
CH2M Hill, Inc. (REM IV)
777 - 108th Ave., N.E.
Bellevue, WA 98009-2050
206/453-5000
Stuart Brown
Ecology & Environment (FIT II)
101 Yesler Way
Suite 600
Seattle, WA 98104
206/624-9537
Andrew Hafferty, Sr Chemist-QA, FIT-Communications Contact
B-25 12-15-88
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MISCELLANEOUS INFORMATION
Bottle Repositories:
I-Chem Research Corporation (East)
104 Quigley Blvd.
New Castle, DE 19720
302/322-5019
William Luzzo, Repository Manager
Eagle-Picher Research Lab (West)
200 Ninth Avenue, N.E.
Miami, OK 74354
918/540-1507 800/331-3144
Robert Greer, Repository Manager
Cooler Returns:
T. Head and Company
950 Herndon Parkway
Suite 230
Herndon, VA 22070
703/478-3886
John Carria
Johnetta Sowell
ERT Edison:
USEPA Environ. Response Branch
GSA Raritan Depot
Woodbridge Avenue
Edison, NJ 08837
FTS 340-6649, 6689, 6743
Royal Nadeau
George Prince
B-26 12-15-i
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CONTRACT LABORATORY PROGRAM
REGIONAL DEPUTY PROJECT OFFICERS
12/1/88
Deb Szaro
USEPA Region I, ESD
60 Westview Street
Lexington, MA 02173
617/860-4312
Lou Bevilacqua
USEPA Region II, ESD
Woodbridge Avenue
Building 209
Edison, NJ 08837
201/321-6702
FTS 340-6702
Chuck Sands
USEPA Region III, CRL
839 Bestgate Road
Annapolis, MD 21401
301/266-9180
Tom B. Bennett, Jr.
USEPA Region IV, ESD (ASB)
Analytical Support Branch
College Station Road
Athens, GA 30613
404/546-3112
FTS 250-3112
Pat Churilla
USEPA Region V, ESD
536 S. Clark Street
Tenth Floor, CRL
Chicago, IL 60605
312/353-9087
FTS 353-9087
David Stockton
USEPA Region VI Laboratory
Monterey Park PI. Bldg. C
6608 Hornwood Drive
Houston, TX 77074
713/953-3425
FTS 526-9425
Debra Morey
USEPA Region VII, ESD
25 Funston Road
Kansas City, KS 66115
913/236-3881
FTS 757-3881
Eva Hoffman
USEPA Region VIII Laboratory
Denver Federal Center
Box 25366
Lakewood, CO 80225
303/236-7371
FTS 776-7371
Kent Kitchingman
USEPA Region IX, OPM
215 Fremont Street
San Francisco, CA 94105
415/974-0924
FTS 454-0924
Gerald Muth
USEPA Region X Laboratory
P.O. Box 549
Manchester, WA 98353
206/442-0370
FTS 399-0370
B-27
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REGIONAL SAMPLE CONTROL CENTERS
November 1988
CLIENT
Region I
Region II
Region III
Region IV
AUTHORIZED REQUESTORS
Rosalie Baldassari*
617/573-5798; FTS 833-1798
Susan Willis
617/573-5607; FTS 833-5607
Darvene Adams
201/321-6705; FTS 340-6705
Gayatri Mehta
201/321-6705; FTS 340-6705
Regina Odubo-Sullivan
201/321-6705; FTS 340-6705
Sharon Steltz*
201/321-6705; FTS 340-6705
John Austin
301/266-9180
Dan Donnelly
301/266-9180
Patricia Krantz
301/266-9180
Annette Lage
301/266-9180
Colleen Walling*
301/266-9180
Tom B. Bennett, Jr.
404/546-3112; FTS 250-3112
Debbie Colquitt
404/546-3388; FTS 250-3388
Doug Lair*
404/546-3300; FTS 250-3300
Doug Mundrick
404/546-3321; FTS 250-3321
Myron Stephenson
404/546-3385; FTS 250-3385
*Primary Authorized Requestor
B-28
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Region V
Region VI
RAS Only
CH2M Hill:
COM:
E & E:
Michigan DNR:
Minnesota PCA:
Weston:
Wisconsin DNR:
RAS Only
E & E
Jan Pels*
312/353-2720; FTS 353-2720
Curtis Ross
312/353-8370; FTS 353-8370
Jeff Keiser
Dave Shekoski
Shirley Stringer
414/272-2426
Cynthia Clark
Wendy Dewar
Jill Line
312/786-1313
Renee Hix-Mays
312/663-9415
Denise Grubin
517/373-4825
Dave Kouloski
Becky Lofgrim
612/296-7735
Eileen Helmer
Maureen O'Mara
Melodic Sullivan
312/993-1067
Maureen McCurdy
Kim McCutchen
608/267-5063
Myra Perez*
713/953-3425; FTS 526-9425
Hank Thompson
214/665-6491; FTS 255-6491
John Totin
214/742-6601
*Primary Authorized Requestor
B-29
-------
Region VII
Region VIII
RAS Only
CCJM:
CH2M Hill:
E& E
Jacobs:
Region IX
Region X
Bill Bunn
913/236-3881; FTS 757-3881
Joyce W. Casper*
913/236-3881; FTS 757-3881
Debra Morey
913/236-3881; FTS 757-3881
Barbara Daboll*
303/236-7370; FTS 776-7370
Bill Berning
Jerilyn Guthrie
303/433-6966
Dewey Brigham
Jane Grogan
303/771-0900
Lynn Fischer
Steve Ignelzi
303/757-4984
Pam McDevitt
Joyce Miyagishima
303/232-7093
Thomas Huetteman*
415/974-0923; FTS 454-0923
Denise Toll
415/974-8004; FTS 454-8004
Joyce Crosson
206/442-2111; FTS 399-2111
Kelsey Ramey
206/442-4323; FTS 399-4323
Rhonda Wregglesworth*
206/442-7121; FTS 399-7121
*Primary Authorized Requestor
B-30
-------
APPENDIX C
RAS DELIVERABLES AND DATA REPORTING FORMS
-------
RAS Organics
Delivery Requirements
A. Contract Start-Up Plan
The contract laboratory must submit a start-up plan for PO approval that details the
laboratory's proposed schedule for receiving samples. The laboratory will be required to
receive samples within thirty days of contract award.
B. Updated Standard Operating Procedures
The contract laboratory must submit updated copies of all required SOPs that were
submitted prior to contract award. The updated SOPs must address all issues of
laboratory performance and operation identified during the preaward evaluation process.
C. Sample Traffic Reports
The original Sample TR must be returned to SMO with laboratory receipt information for
each sample in the SDG. TRs must be submitted in SDG sets with an SDG coversheet
attached.
D. Sample Data Summary Package
A sample data summary package must be delivered to SMO with other required sample
data. The sample data summary package consists of copies of specified items from the
sample data package. The sample data summary package must contain data for samples in
an SDG, as follows:
1. Case Narrative
2. By fraction (VOA, SV, PEST) and by sample within each fraction - tabulated target
compound results (Form I) and tentatively identified compounds (Form I,
TIC)(VOA and SV only)
3. By fraction (VOA, SV, PEST) - surrogate spike analysis results (Form II) by matrix
(water and/or soil) and for soil, by concentration (low or medium)
4. By fraction (VOA, SV, PEST) - matrix spike/matrix spike duplicate results
(Form III)
5. By fraction (VOA, SV, PEST) - blank data (Form IV) and tabulated results (Form
I) including tentatively identified compounds (Form I, TIC)(VOA and SV only)
6. By fraction (VOA, SV only) - internal standard area data (Form VIII)
E. Sample Data Package
The sample data package is divided into the five major units described below. The last
three units are each specific to an analytical fraction (volatiles, semivolatiles,
pesticides/PCBs). The sample data package must include data for analyses of all samples
in one SDG, including field samples, reanalyses, blanks, matrix spikes, and matrix spike
duplicates. The sample data package must include the following:
C-l
-------
1. Case Narrative
The Case Narrative must contain: laboratory name; Case number; sample numbers
in the SDG, differentiating between initial analyses and reanalyses; SDG number;
contract number; and detailed documentation of any quality control, sample,
shipment and/or analytical problems encountered in processing the samples reported
in the data package.
2. Traffic Reports
A copy of the Sample TRs in Item C must be submitted for all of the samples in an
SDG. The TRs must be arranged in increasing EPA sample number order.
3. Volatiles Data
a. QC Summary
(1) Surrogate Percent Recovery Summary (Form II VOA)
(2) Matrix Spike/Matrix Spike Duplicate Summary (Form III VOA)
(3) Method Blank Summary
(If more than a single form is necessary, forms must be arranged in
chronological order by date of analysis of the blank.)
(4) GC/MS Tuning and Mass Calibration (Form V VOA)
BFB in chronological order; by instrument
(5) Internal Standard Area Summary (Form VIII VOA)
In chronological order; by instrument
b. Sample Data
Sample data must be arranged in packets with the Organic Analysis Data
Sheet (Form I VOA, including Form I VOA-TIC) followed by the raw data.
Sample packets should be placed in increasing EPA sample number order.
(1) TCL Results - Organic Analysis Data Sheet (Form I VOA)
(2) Tentatively Identified Compounds (Form I VOA-TIC)
This form must be included even if no compounds are found. If so,
indicate this on the form by entering "0" in the field for "Number
found."
(3) Reconstructed total ion chromatograms (RIC) for each sample or sample
extract
(4) For each sample, by each compound identified:
(a) Copies of raw spectra and copies of background-subtracted mass
spectra of target compounds
C-2
-------
(b) Copies of mass spectra of Tentatively Identified Compounds with
associated best-match spectra (three best matches)
c. Standards Data
(1) Initial Calibration Data (Form VI VOA) - in order by instrument, if
more than one instrument used
(a) VOA standard(s) reconstructed ion chromatograms and
quantitation reports for the initial calibration. Spectra are not
required.
(b) All initial calibration data must be included, regardless of when it
was performed and for which case. When more than one initial
calibration is performed, the data must be put in chronological
order, by instrument.
(2) Continuing Calibration (Form VII VOA) - in order by instrument, if
more than one instrument used
(a) VOA standard(s) reconstructed ion chromatograms and
quantitation reports for all continuing calibrations. Spectra are
not required.
(b) When more than one continuing calibration is performed, forms
must be in chronological order, within fraction and instrument.
(3) Internal Standard Area Summary (Form VIII VOA) - in order by
instrument, if more than one instrument used
When more than one continuing calibration is performed, forms must be
in chronological order, by instrument.
d. Raw QC Data
(1) BFB for each GC/MS system utilized
(a) Bar graph spectrum
(b) Mass listing
(2) Blank Data - in chronological order
(a) Tabulated results (Form I VOA)
(b) Tentatively Identified Compounds (Form I VOA-TIC) even if
none found
(c) Reconstructed ion chromatogram(s) and quantitation report(s)
(GC/MS)
(d) TCL spectra with lab generated standard. Data systems which are
incapable of dual display must provide spectra in order:
C-3
-------
o Raw TCL compound spectra
o Enhanced or background subtracted spectra
o Laboratory generated TCL standard spectra
(e) GC/MS library search spectra for Tentatively Identified
Compounds.
(f) Quantitation/Calculation of Tentatively Identified Compounds.
(3) Matrix Spike Data
(a) Tabulated results (Form I VOA) of nonspiked TCL compounds.
Form I VOA-TIC is not required.
(b) Reconstructed ion chromatogram(s) and quantitation report(s)
(GC/MS). Spectra are not required.
(4) Matrix Spike Duplicate Data
(a) Tabulated results (Form I VOA) of nonspiked TCL compounds.
Form I VOA-TIC is not required.
(b) Reconstructed ion chromatogram(s) and quantitation report(s)
(GC/MS). Spectra are not required.
(c) TCL spectra with lab generated standard. Data systems which are
incapable of dual display must provide spectra in order:
o Raw TCL compound spectra
o Enhanced or background subtracted spectra
o Laboratory generated TCL standard spectra
(d) GC/MS library search spectra for Tentatively Identified
Compounds.
(e) Quantitation/Calculation of Tentatively Identified Compounds.
(3) Matrix Spike Data
(a) Tabulated results (Form I) of nonspiked TCL compounds. Form 1
SV-TIC is not required.
(b) Reconstructed ion chromatogram(s) and quantitation report(s)
(GC/MS). Spectra are not required.
4. Semivolatiles Data
a. QC Summary
(1) Surrogate Percent Recovery Summary (Form II SV)
(2) Matrix Spike/Matrix Spike Duplicate Summary (Form III SV)
C-4
-------
(3) Method Blank Summary (Form IV SV)
(If more than a single form is necessary, forms must be arranged in
chronological order by date of analysis of the blank.)
(4) GC/MS Tuning and Mass Calibration (Form V SV)
DFTPP in chronological order; by instrument
(5) Internal Standard Area Summary (Form VIII SV)
In chronological order; by instrument
b. Sample Data
Sample data must be arranged in packets with the Organic Analysis Data
Sheet (Form I SV, including Form I SV-TIC) followed by the raw data.
Sample packets should be placed in increasing EPA sample number order.
(1) TCL Results - Organic Analysis Data Sheet (Form I SV-1, SV-2)
(2) Tentatively Identified Compounds (Form I SV-TIC)
This form must be included even if no compounds are found. If so,
indicate this on the form by entering "0" in the field for "Number
found".
(3) Reconstructed total ion chromatograms (RIC) for each sample, sample
extract, standard, blank, and spiked sample
(4) For each sample, by each compound identified:
(a) Copies of raw spectra and copies of background-subtracted mass
spectra of target compounds
(b) Copies of mass spectra of Tentatively Identified Compounds with
associated best-match spectra (three best matches)
(c) GPC chromatograms (if GPC performed)
c. Standards Data
(1) Initial Calibration Data (Form VI SV-1, SV-2) - in order by instrument,
if more than one instrument used
(a) BNA standard(s) reconstructed ion chromatograms and
quantitation reports for the initial calibration. Spectra are not
required.
(b) All initial calibration data must be included, regardless of when it
was performed and for which case. When more than one initial
calibration is performed, the data must be put in chronological
order, by instrument.
C-5
-------
(2) Continuing Calibration (Form VII SV-1, SV-2) - in order by
instrument, if more than one instrument used
(a) BNA standard(s) reconstructed ion chromatograms and
quantitation reports for all continuing calibrations. Spectra are
not required.
(b) When more than one continuing calibration is performed, forms
must be in chronological order, by instrument.
(3) Internal Standard Area Summary (Form VIII SV-1, SV-2) - in order by
instrument, if more than one instrument used
When more than one continuing calibration is performed, forms must be
in chronological order by instrument.
d. Raw QC Data
(1) DFTPP for each GC/MS system utilized
(a) Bar graph spectrum
(b) Mass listing
(2) Blank Data - in chronological order
(a) Tabulated results (Form I SV-1, SV-2)
(b) Tentatively Identified Compounds (Form I SV-TIC) - even if
none found
5. Pesticide/PCB Data
a. QC Summary
(1) Surrogate Percent Recovery Summary (Form II PEST)
(2) Matrix Spike/Matrix Spike Duplicate Summary (Form III PEST)
(3) Method Blank Summary (Form IV PEST)
(If more than a single form is necessary, forms must be arranged in
chronological order by date of analysis of the blank.)
b. Sample Data
Sample data must be arranged in packets with the Organic Analysis Data
Sheet (Form I PEST) followed by the raw data. Sample packets should be
placed in increasing EPA sample number order.
(1) TCL Results - Organic Analysis Data Sheet (Form I PEST)
(2) Copies of pesticide chromatograms
C-6
-------
(3) Copies of pesticide chromatograms from second GC column
confirmation
(4) GC Integration report or data system printout and calibration plots (area
vs. concentration) for 4,4'-DDT, 4,4'-DDD, 4,4'-DDE or toxaphene
(where appropriate)
(5) Manual work sheets
(6) UV traces from GPC (if available)
(7) Copies of raw spectra and copies of background-subtracted mass spectra
of target compounds (if pesticide/PCBs are confirmed by GC/MS)
c. Standards Data
(1) Form VIII PEST - Pesticide Evaluation Standards Summary (all GC
columns)
(2) Form IX PEST - Pesticide/PCB Standards Summary (all GC columns)
(3) Form X PEST - Pesticide/PCB Identification (only required for positive
results)
(4) Pesticide standard chromatograms and data system printouts for all
standards
d. Raw QC Data
(1) Blank Data - in chronological order
(a) Tabulated results (Form I PEST)
(b) Chromatogram(s) and data system printout(s) (GC) for each GC
column and instrument used for analysis
(2) Matrix Spike Data
(a) Tabulated results (Form I PEST) of nonspike TCL compounds
(b) Chromatogram(s) and data system printout(s) (GC)
(3) Matrix Spike Duplicate Data
(a) Tabulated results (Form I PEST) of nonspike TCL compounds
(b) Chromatogram(s) and data system printout(s) (GC)
F. Data in Computer-Readable Form
The contract laboratory must provide a computer-readable copy of the data on data
reporting Forms I-X for all samples in an SDG. Computer-readable data deliverables
must be submitted on IBM or IBM-compatible, 5.25 inch floppy double-sided, double
C-7
-------
density 360 K-byte or a high density 1.2 M-byte diskette. The data must be recorded in
ASCII text file format and must adhere to the file, record and field specifications listed
in the SOW.
G. GC/MS Tapes
The contract laboratory must store all raw and processed GC/MS data on magnetic tape,
in appropriate instrument manufacturer's format. This tape must include data for
samples, blanks, matrix spikes, matrix spike duplicates, initial calibrations, continuing
calibrations, BFB and DFTPP, as well as all laboratory-generated spectral libraries and
quantitation reports required to generate the data package. The Contractor must maintain
a written reference logbook of tape files to EPA sample number, calibration data,
standards, blanks, matrix spikes, and matrix spike duplicates.
H. Extracts
The contract laboratory is required to retain extracts, preserved at 4°C (±2°C), for 365
days following data submission. A logbook of stored extracts must be maintained, listing
EPA sample numbers and associated Case and SDG numbers.
I. Complete Case File Purge
The complete case file purge includes all laboratory records received or generated for a
specific Case that have not been previously submitted to EPA as a deliverable. These
items include but are not limited to: sample tags, custody records, sample tracking
records, analysts logbook pages, bench sheets, chromatographic charts, computer printouts,
raw data summaries, instrument logbook pages, correspondence, and the document
inventory.
-------
RAS ORGANICS
DATA REPORTING FORMS
-------
1A
VOLATILE ORGANICS ANALYSIS DATA SHEET
EPA SAMPLE NO.
Lab Name:
Lab Code:
Case No.:
Contract:
SAS No.:
SDG No.:
Matrix: (soil/water)
Sample wt/vol:
Level: (low/med)
% Moisture: not dec.
Column: (pack/cap)
CAS NO.
Lab Sample ID:
Lab File ID:
Date Received:
Date Analyzed:
COMPOUND
Dilution Factor:
CONCENTRATION UNITS:
(ug/L or ug/Kg)
74-87-3 Chloromethane
74-83-9 Bromomethane
75-01-4 Vinyl Chloride
75-00-3 Chloroethane
75-09-2 Methylene Chloride
67-64-1 Acetone
75-15-0 Carbon Disulfide
75-35-4 1,1-Dichloroethene
75-34-3 1,1-Dichloroethane
540-59-0 1,2-Dichloroethene (total)
67-66-3 Chloroform
107-06-2 1,2-Dichloroethane
78-93-3 2-Butanone
71-55-6 1,1,1-Trichloroethane
56-23-5 Carbon Tetrachloride
108-05-4 Vinyl Acetate
75-27-4 Bromodichloromethane
78-87-5 1, 2-Dichloropropane
10061-01-5 cis-1,3-Dichloropropene
79-01-6 Trichloroethene
124-48-1 Dibromochlorome thane
79-00-5 1,1, 2-Trichloroethane
71-43-2 Benzene
10061-02-6 trans-1,3-Dichloropropene
75-25-2 Bromoform
108-10-1 4-Methyl-2-Pentanone
591-78-6 2-Hexanone
127-18-4 Tetrachloroethene
79-34-5 1,1,2,2-Tetrachloroethane
108-88-3 Toluene
108-90-7 Chlorobenzene
100-41-4 Ethylbenzene_
100-42-5 Styrene
1330-20-7 Xylene (total)
FORM I VGA
1/87 Rev.
-------
IB
SEMIVOLATILE ORGANICS ANALYSIS DATA SHEET
EPA SAMPLE NO.
Lab Name:
Lab Code:
Case No.:
Contract:
SAS No. :
SDG No.:
Matrix: (soil/water)
Sample wt/vol:
Level: (low/med)
% Moisture: not dec.
(g/mL).
dec.
Extraction: (SepF/Cont/Sonc)
GPC Cleanup: (Y/N) pH:
Lab Sample ID:
Lab File ID:
Date Received:
Date Extracted:
Date Analyzed:
CAS NO.
COMPOUND
Dilution Factor:
CONCENTRATION UNITS:
(ug/L or ug/Kg)
108-95-2 Phenol
111-44-4 bis(2-Chloroethyl)ether
95-57-8 2-Chlorophenol
541-73-1 1, 3-Dichlorobenzene
106-46-7 1,4-Dichlorobenzene
100-51-6 Benzyl alcohol
95-50-1 1,2-Dichlorobenzene
95-48-7 2-Methylphenol
108-60-1 bis(2-Chloroisopropyl) ether
44-5 4-Methylphenol
6.7-72-1 Hexachloroethane
98-95-3 Nitrobenzene
88-75-5 2-Nitrophenol
105-67-9 2
65-85-0 Benzoic acid
111-91-1 1
120-83-2 2 , 4-Dichlorophenol
120-82-1 l,2,4-Trichlorobenzene_
91-20-3 Naphthalene
106-47-8 4-Chloroaniline
87-68-3 Hexachlorobutadiene
59-50-7 4-Chloro-3-methylphenol
91-57-6 2-Methylnaphthalene
77-47-4 Hexachlorocyclopentadiei
88-06-2 2, 4 , 6-Trichlorophenol
95-95-4 2 , 4 , 5-Trichlorophenol
91-58-7 2
88-74-4 2
131-11-3 Dimethylphthalate
208-96-8 Acenaphthylene
606-20-2 2
FORM I SV-1
1/87 Rev.
-------
Lab Name:
Lab Code:
1C
SEMIVOLATILE ORGANICS ANALYSIS DATA SHEET
Contract:
SAS No. :
EPA SAMPLE NO.
Case No.:
SDG No.:
Matrix: (soil/water)
Sample wt/vol:
Level: (low/med)
% Moisture: not dec.
_(g/mL)_
dec.
Extraction: (SepF/Cont/Sonc)
GPC Cleanup: (Y/N) pH:
Lab Sample ID:
Lab File ID:
Date Received:
Date Extracted:
Date Analyzed:
CAS NO.
COMPOUND
Dilution Factor:
CONCENTRATION UNITS:
(ug/L or ug/Kg)
1 *3 O — fiA Q — — — —
Q yi — £ £_o _«__.
*7 n ("1 R — "7 O — T —
i n r\ « r^ i c
Q f _ o n.c
i ni RR *3
1 1 Q — "7 /I — 1 «...
Q7 Q £ — R
QC n i — Q — —
i on — T ->— '?— — — —
QA *7A_O— — — —
TOO f\r\ r\
O 1 Q O1 Q
1 1 "7 Q 1 "7 —
-L -L / OX /
o n"7 — no —Q
T QO OQ C_
1 Q1 — .O A .O — — — —
m ^-1»4» Vt x^v-k j^
—fc • « ^
r\ •* 4-Vmrl Vh4-l%**l -k 4-
Ji ^V* T **. V* *-tir"1 Vxxvv^irl j-k4-V» •*•
. . — • » 1 ^ »
A f T\ ' * 4- O 4-1* 1 Vt 1
VT *.T * I l*Vi T * /T\
,• D-v-j-k'V¥»*^-^xV1 rtwi rl •m.'W «-WNV r "1 ^N 4* V^ XN -w-
— t±— Diroinopneny x—pnenyxeunsir
T~» 4- V» 1 X*. T
T^l r-* *-» ^ \
f: ^.A-V. •*•-.
r\ -I *-t Vk 4- "1 V*4-Vt T 4-
T-i-l 4.1-
_.
tyivGriG
Y3 4- • T I "1141 1*-
O O 1 I~\ * .nVt 1 j-s.^-j-^V%. * *J -I xx
— j , o "~uicnxoi7ODenziuine
TJ / \ — .4- V* •*•-*
/*^l
~ cnrysene
I * / O T^ ^ V- Tl T\ I A 1 T i_
~ DIS(Z btnyinexyi) pntnaiate
r% * I T 1 i 1 T <
"" ui n ocT.yxpni.ncix cite
r> /i \ -f^ T i i-
— oenzo^Dy rxuoiTcinT..nene
n /l\fl 41
"~ benzo(K) tiuorantnene
Q / -* \ %-v i r -b- XN. «-k j-x
-y J / 1 O O J \
~ inaeno ( i , 2 , J— ca) pyrene
r\ " i / i \ *• w
uioenz ( a , n ) ancnracene
T5 / 1 * \ 1
(1) - Cannot be separated from Diphenylamine
FORM I SV-2
1/87 Rev.
-------
Lab Name:
Lab Code:
ID
PESTICIDE ORGANICS ANALYSIS DATA SHEET
Contract:
SAS No.:
EPA SAMPLE NO.
Case No.:
SDG No.:
Matrix: (soil/water)
Sample wt/vol:
Level: (low/med)
% Moisture: not dec.
.(g/mL).
dec.
Extraction: (SepF/Cont/Sonc)
GPC Cleanup: (Y/N) pH:
Lab Sample ID:
Lab File ID:
Date Received:
Date Extracted:
Date Analyzed:
CAS NO.
COMPOUND
Dilution Factor:
CONCENTRATION UNITS:
(ug/L or ug/Kg)
oXy~oD~/
o xy — OD*"O
Do—by y —
*7 £i~~ A A O
/ t>""4 4 o
1 m >1 K~7 ~3 __.__
XU*i 4 O I J— — — —
Q C Q Q Q _ Q
y oy y o~o
a r\ _ c^"? _ T
DU™"D / X
jj^xj— OD y
n r\ o n r\-7 o
en o Q 'ri
DU ^y j
C;T/IQ/I *7n R ...
DiU J / X y
c T n "5 "7 A O
1 O C~7 yl IT O
i^i D / *1 XX ^i
cro//rQ ->i Q
oj^oy <;X y
1 O £ *7 O "> Q — £.
xz D / z ^y "~o
1THQ"7 *^Q 1
"""•axpna tiric
— — — Vi^+- a — RM/^
— WH/^o1 t*a— T*Hr*
— — A 1 HT-T n
™— nspT-cicnxojr epoxxae
™ uxexairxn
4 A i nr\T?
— r/naixn
"•""•"rinQOSUXxan XX
4 A i — T^r\r\
, ** uuu
4 A \ nr^rp
/ ft UJJX
-1 •. /~1\~ 1 Vf3 -* Vt
— cixpnci—v^nxoircicine
/^W T x«>.'k>*x^ r» >•* *-i
— AJT OCXOi "~XUXO
"• AJTOCXOi XZ^*i
— *. &TTM"*! rNV— 1 *)^f\
FORM I PEST
1/87 Rev.
-------
Lab Name:
Lab Code:
IE
VOLATILE ORGANICS ANALYSIS DATA SHEET
TENTATIVELY IDENTIFIED COMPOUNDS
Contract:
SAS No.:
EPA SAMPLE NO.
Case No.:
SDG No.:
Matrix: (soil/water)
Sample wt/vol:
Level: (low/med)
% Moisture: not dec.
Column: (pack/cap)
Number TICs found:
(g/mL)
Lab Sample ID:
Lab File ID:
Date Received:
Date Analyzed:
Dilution Factor:
CONCENTRATION UNITS;
(ug/L or ug/Kg)
CAS NUMBER
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.
COMPOUND NAME
RT
EST. CONC.
Q
FORM I VOA-TIC
1/87 Rev.
-------
Lab Name:
Lab Code:
IF
SEMIVOLATILE ORGANICS ANALYSIS DATA SHEET
TENTATIVELY IDENTIFIED COMPOUNDS
Contract:
SAS No.:
EPA SAMPLE NO.
Case No.:
SDG No.
Matrix: (soil/water)
Sample wt/vol:
Level: (low/med)
% Moisture: not dec.
.(g/mL)_
dec.
Extraction: (SepF/Cont/Sonc)
GPC Cleanup: (Y/N) pH:
Number TICs found:
Lab Sample ID:
Lab File ID:
Date Received:
Date Extracted:
Date Analyzed:
Dilution Factor:
CONCENTRATION UNITS;
(ug/L or ug/Kg)
CAS NUMBER
I.
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.
COMPOUND NAME
RT
EST.CONC.
—
Q
FORM I SV-TIC
1/87 Rev.
-------
2A
WATER VOLATILE SURROGATE RECOVERY
Lab Name:
Lab Code:
Case No.:
Contract:
SAS No. :
SDG No.
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
EPA
SAMPLE NO.
SI
(TOL) #
S2
(BFB)#
S3
(DCE)#
OTHER
TOT
OUT
QC LIMITS
SI (TOL) = Toluene-d8 (88-110)
S2 (BFB) = Bromofluorobenzene (86-115)
S3 (DCE) = l,2-Dichloroethane-d4 (76-114)
# Column to be used to flag recovery values
* Values outside of contract required QC limits
D Surrogates diluted out
page
of
FORM II VOA-1
1/87 Rev.
-------
Lab Name:
Lab Code:
2B
SOIL VOLATILE SURROGATE RECOVERY
Contract:
Case No.: SAS No.:
Level:(low/med)
SDG No.
| EPA
| SAMPLE NO.
oil
02|
03|
04|
05|
06|
07|
08|
09|
10|
HI
12|
13|
14|
15|
16|
17|
18|
19|
20|
21|
22 [
231
24|
25|
26|
27[
28|
29 |
30|
SI
(TOL) #
S2
(BFB)#
S3
(DCE) #
^^^
OTHER
TOT
OUT
QC LIMITS
SI (TOL) = Toluene-d8 (81-117)
S2 (BFB) = Bromofluorobenzene (74-121)
S3 (DCE) = l,2-Dichloroethane-d4 (70-121)
# Column to be used to flag recovery values
* Values outside of contract required QC limits
D Surrogates diluted out
page
of
FORM II VOA-2
1/87 Rev.
-------
2C
WATER SEMIVOLATILE SURROGATE RECOVERY
Lab Name:
Lab Code:
Case No.:
Contract:
SAS No.:
SDG No.
EPA
SAMPLE NO.
SI
(NBZ)f
S2
(FBP) #
S3
(TPH) #
S4
(PHL) I
S5
(2FP)#
'
S6
(TBP) #
OTHER
TOT
OUT
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
SI (NBZ) = Nitrobenzene-d5
S2 (FBP) = 2-Fluorobiphenyl
S3 (TPH) = Terphenyl-dl4
S4 (PHL) = Phenol-d5
S5 (2FP) = 2-Fluorophenol
S6 (TBP) = 2,4,6-Tribromophenol
QC LIMITS
(35-114)
(43-116)
(33-141)
(10-94)
(21-100)
(10-123)
# Column to be used to flag recovery values
* Values outside of contract required QC limits
D Surrogates diluted out
page
of
FORM II SV-l
1/87 Rev.
-------
2D
SOIL SEMIVOLATILE SURROGATE RECOVERY
Lab Name:
Lab Code:
Case No.:
Contract:
SAS No.:
SDG No,. :
Level:(low/med)
EPA
SAMPLE NO.
SI
(NBZ)#
S2
(FBP)#
S3
(TPH) #
S4
(PHL)#
__.
S5
(2FP)#
S6
(TBP) f
OTHER
TOT|
OUT
02|
03|
04 j
05|
06 |
07|
08 |
09 |
10|
HI
12
15
16|
17 I'
18|
19|
20|
21|.
22|
23f
24|
25|'
26|
27|
28
29|
301
SI (NBZ) = Nitrobenzene-d5
S2 (FBP) = 2-Fluorobiphenyl
S3 (TPH) = Terphenyl-dl4
S4 (PHL) = Phenol-d5
S5 (2FP) = 2-Fluorophenol
S6 (TBP) = 2,4,6-Tribromophenol
QC LIMITS
(35-114)
(43-116)
(33-141)
(10-94)
(21-100)
(10-123)
# Column to be used to flag recovery values
* Values outside of contract required QC limits
D Surrogates diluted out
page of
FORM II SV-2
1/87 Rev.
-------
2E
WATER PESTICIDE SURROGATE RECOVERY
Lab Name:
Lab Code:
Case No.:
Contract:
SAS No. :
SDG No.:
| EPA
| SAMPLE NO.
1
oil
02|
03 |
04|
05|
06 |
07|
08|
09|
10|
HI
12|
131
14|
15| .
16|
17|
18|
19|
20|
21|
22|
23|
24|
25|
26|
27|
28 |
29|
30|
SI
(DEC) #
OTHER
ADVISORY
QC LIMITS
SI (DEC) = Dibutylchlorendate (24-154)
I Column to be used to flag recovery values
* Values outside of QC limits
D Surrogates diluted out
page of
FORM II PEST-1
1/87 Rev.
-------
Lab Name:
Lab Code:
2F
SOIL PESTICIDE SURROGATE RECOVERY
Contract:
Case No.: SAS No.:
Level:(low/med)
SDG No.
| EPA
| SAMPLE NO.
oil
021
03|
041
051
061
07|
08|
09|
10|
HI
12|
131
14|
151
161
171
18|
191
20|
211
22|
23|
24|
25|
26|
27|
28|
29|
30|
SI
(DEC) #
OTHER
ADVISORY
QC LIMITS
SI (DEC) = Dibutylchlorendate (20-150)
# Column to be used to flag recovery values
* Values outside of QC limits
D Surrogates diluted out
page of
FORM II PEST-2
1/87 Rev.
-------
3A
WATER VOLATILE MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name:
Lab Code:
Case No.:
Contract:
SAS No.:
SDG No.:
Matrix Spike - EPA Sample No.:
COMPOUND
1 , 1-Dichloroethene
Trichloroethene
Benzene
Toluene
Chlorobenzene
SPIKE
ADDED
(ug/L)
SAMPLE
CONCENTRATION
(ug/L)
MS
CONCENTRATION
(ug/L)
MS
%
REC #
QC. |
LIMITS j
REC. |
1
- 1
61-145|
71-120)
76-127|
76-1251
75-130)
1
COMPOUND
1, 1-Dichloroethene
Trichloroethene
Benzene
Toluene
Chlorobenzene
SPIKE
ADDED
(ug/L)
MSD
CONCENTRATION
(ug/L)
MSD
%
REC #
1
% | QC LI
RPD #| RPD
1
1 14
1 14
1 11
1 13
1 13
1
EMITS
REC.
61-145
71-120
76-127
76-125
75-130
# 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
COMMENTS:
FORM III VOA-1
1/87 Rev.
-------
3B
SOIL VOLATILE MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name:
Lab Code:
Case No.:
Contract:
SAS No.:
SDG No.:
Matrix Spike - EPA Sample No.:
Level:(low/med)
COMPOUND
1 , 1-Dichloroethene
Trichloroethene
Benzene
Toluene
Chlorobenzene
SPIKE
ADDED
(ug/Kg)
SAMPLE |
CONCENTRATION j
(ug/Kg) |
• ' 1
1
1
1
1
1
1
MS | MS
CONCENTRATION j %
(ug/Kg) | REC #
1
1
1
1
1
1
QC.
LIMITS
REC.
59-172
62-137
66-142
59-139
60-133
COMPOUND
1, 1-Dichloroethene
Trichloroethene
Benzene
Toluene
Chlorobenzene
SPIKE
ADDED
(ug/Kg)
MSD
CONCENTRATION
(ug/Kg)
MSD
%
REC #
%
RPD #
QC LI
RPD
22
23
21
21
21
EMITS
REC.
59-172
62-137
66-142
59-139
60-133
# 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
COMMENTS:
FORM III VGA-2
1/87 Rev.
-------
3C
WATER SEMIVOLATILE MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name:
Lab Code:
Case No.:
Contract:
SAS No.:
SDG No.:
Matrix Spike - EPA Sample No.:
COMPOUND
Phenol
2-Chlorophenol
1 , 4-Dichlorobenzene
N-Nitroso-di-n-prop. (1)
1,2, 4-Trichlorobenzene
4-Chloro-3-raethylphenol
Acenaphthene
4-Nitrophenol
2 , 4-Dinitrotoluene
Pentachlorophenol
Pyrene
SPIKE
ADDED
(ug/L)
SAMPLE
CONCENTRATION
(ug/L)
MS
CONCENTRATION
(ug/L)
MS
%
REC #
QC._
LIMITS
REC.
12- 89
27-123
36- 97
41-116
39- 98
23- 97
46-118
10- 80
24- 96
9-103
26-127
COMPOUND
Phenol
2 -Chlorophenol
1 , 4-Dichlorobenzene
N-Nitroso-di-n-prop. (1)
1, 2,4-Trichlorobenzene_
4-Chloro-3-methylphenol
Acenaphthene
4-Nitrophenol
2 , 4-Dinitrotoluene
Pentachlorophenol
Pyrene
SPIKE
ADDED
(ug/L)
MSD
CONCENTRATION
(ug/L)
—
MSD
%
REC #
%
RPD #
QC L]
RPD
42
40
28
38
28
42
31
50
38
50
31
EMITS
REC.
12- 89
27-123
36- 97
41-116
39- 98
23- 97
46-118
10- 80
24- 96
9-103
26-127
(1) N-Nitroso-di-n-propylamine
# 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
COMMENTS:
FORM III SV-1
1/87 Rev.
-------
3D
SOIL SEMIVOLATILE MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name:
Lab Code:
Case No.:
Matrix Spike - EPA Sample No.:
Contract:
SAS No.:
SDG No.:
Level:(low/med)
COMPOUND
Phenol
2-Chlorophenol
1,4-Dichlorobenzene
N-Nitroso-di-n-prop. (1)
1,2, 4-Trichlorobenzene
4-Chloro-3-methylphenol
Acenaphthene
4 -Nitrophenol
2 , 4-Dinitrotoluene
Pentachlorophenol
Pyrene
SPIKE
ADDED
(ug/Kg)
SAMPLE
CONCENTRATION
(ug/Kg)
MS
CONCENTRATION
(ug/Kg)
MS
%
REC *
LIMITS
REC.
26- 90
25-102
28-104
41-126
38-107
26-103
31-137
11-114
28- 89
17-109
35-142
COMPOUND
Phenol
2 -Chlorophenol
1, 4-Dichlorobenzene
N-Nitroso-di-n-prop. (1)
1,2, 4-Trichlorobenzene
4-Chloro-3-methylphenol
Acenaphthene
4 -Nitrophenol
2 , 4-Dinitrotoluene
Pentachlorophenol
Pyrene
SPIKE
ADDED
(ug/Kg)
'
MSD
CONCENTRATION
(ug/Kg)
MSD
%
REC #
%
RPD #
QC L:
RPD
35
50
27
38
23
33
19
50
47
47
36
EMITS
REC.
26- 90
25-102
28-104
41-126
38-107
26-103
31-137
11-114
28- 89
17-109
35-142
(1) N-Nitroso-di-n-propylamine
# 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
COMMENTS:
FORM III SV-2
1/87 Rev.
-------
3E
WATER PESTICIDE MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name:
Lab Code:
Case No.:
Contract:
SAS No.:
SDG No.:
Matrix Spike - EPA Sample No.:
COMPOUND
gamma-BHC (Lindane)
Heptachlor
Aldrin
Dieldrin
Endrin
4,4' -DDT
SPIKE
ADDED
(ug/L)
SAMPLE
CONCENTRATION
(ug/L)
—
MS
CONCENTRATION
(ug/L)
MS
%
REC #
QC. I
LIMITS |
REC. |
1
56-123|
40-131|
40-120|
52-126J
56-121|
38-127|
1
COMPOUND
gamma-BHC (Lindane)
Heptachlor
Aldrin
Dieldrin
Endrin
4,4' -DDT
SPIKE
ADDED
(ug/L)
MSD
CONCENTRATION
(ug/L)
MSD |
% | %
REC #| RPD #
1
1
1
1
1
1
1
QC LIMITS
RPD | REC.
i
1
15 [56-123
20 (40-131
22 |40-120
18 |52-126
21 |56-121
27 |38-127
1
# 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
COMMENTS:
FORM III PEST-1
8/87 Rev.
-------
3F
SOIL PESTICIDE MATRIX SPIKE/MATRIX SPIKE DUPLICATE RECOVERY
Lab Name:
Lab Code:
Case No.:
Contract:
SAS No.:
SDG No.
Matrix Spike - EPA Sample No.:
Level:(low/med)
COMPOUND
gamma-BHC (Lindane)
Heptachlor
Aldrin
Dieldrin
Endrin
4,4' -DDT
SPIKE
ADDED
(ug/Kg)
SAMPLE | MS | MS
CONCENTRATION | CONCENTRATION | %
(ug/Kg) | (ug/Kg) | REC #
1
1 1
1 1
1 1
1 1
1 1
1 1
QC.
LIMITS
REC.
46-127
35-130
34-132
31-134
42-139
23-134
COMPOUND
gamma-BHC (Lindane)
Heptachlor
Aldrin
Dieldrin
Endrin
4,4' -DDT
SPIKE
ADDED
(ug/Kg)
MSD
CONCENTRATION
(ug/Kg)
MSD
%
REC #
%
RPD #
QC L]
RPD
50
31
43
38
45
50
1
[MITS |
REC. |
i
1
46-127)
35-130J
34-132)
31-134)
42-139)
23-134)
1
# 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
COMMENTS:
FORM III PEST-2
8/87 Rev.
-------
Lab Name:
Lab Code:
4A
VOLATILE METHOD BLANK SUMMARY
Contract:
SAS No.:
Case No.:
Lab File ID:
Date Analyzed:
Matrix: (soil/water)
Instrument ID:
SDG No.:
Lab Sample ID:
Time Analyzed:
Level:(low/med)
THIS METHOD BLANK APPLIES TO THE FOLLOWING SAMPLES, MS AND MSD:
| EPA
| SAMPLE NO.
01|
02|
03|
04|
05|
06|
07|
08 |
09 |
10|
HI
12 |
13|
14|
15|
16|
17|
18|
19|
20|
21|
22|
23|
24|
25|
26|
27|
28|
29|
30|
LAB
SAMPLE ID
LAB
FILE ID
TIME
ANALYZED
COMMENTS:
page
of
FORM IV VGA
1/87 Rev.
-------
Lab Name:
Lab Code:
4B
SEMIVOLATILE METHOD BLANK SUMMARY
Contract:
SAS No.:
Case No.:
SDG No.:
Lab File ID:
Date Extracted:
Date Analyzed:
Matrix: (soil/water)
Instrument ID:
Lab Sample ID:
Extraction:(SepF/Cont/Sonc)
Time Analyzed:
Level:(low/med)
THIS METHOD BLANK APPLIES TO THE FOLLOWING SAMPLES, MS AND MSD:
COMMENTS:
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
EPA
SAMPLE NO.
LAB
SAMPLE ID
LAB
FILE ID
TIME
ANALYZED
page
of
FORM IV SV
1/87 Rev.
-------
Lab Name:
Lab Code:
4C
PESTICIDE METHOD BLANK SUMMARY
Contract:
SAS No.:
Case No.:
SDG No.:
Lab Sample ID:
Matrix:(soil/water)
Date Extracted:
Date Analyzed (1):
Time Analyzed (1):
Instrument ID (2):
GC Column ID (1) :
Lab File ID:
Level:(low/med)
Extraction: (SepF/Cont/Sonc)
Date Analyzed (2):
Time Analyzed (2):
Instrument ID (2):
GC Column ID (1):
THIS METHOD BLANK APPLIES TO THE FOLLOWING SAMPLES, MS AND MSD:
| EPA
j SAMPLE NO.
on
02|
03|
04|
05|
06|
07|
08|
09|
10|
HI
12|
13|
14|
15|
16|
17|
18|
19|
20|
211
22|
23|
24 |
25|
26|
LAB
SAMPLE ID
.
DATE
ANALYZED 1
...
DATE
ANALYZED 2
COMMENTS:
page of
FORM IV PEST
1/87 Rev.
-------
Lab Name:
Lab Code:
5A
VOLATILE ORGANIC GC/MS TUNING AND MASS
CALIBRATION - BROMOFLUOROBENZENE (BFB)
Contract:
SAS No.:
Lab File ID:
Instrument ID:
Case No.:
SDG No.:
BFB Injection Date:
BFB Injection Time:
Matrix:(soil/water)
Level:(low/med)
Column:(pack/cap)
m/e
50
75
95
96
173
174
175
176
177
ION ABUNDANCE CRITERIA
15.0 - 40.0% of mass 95
30.0 - 60.0% of mass 95
Base peak, 100% relative abundance
5.0 - 9.0% of mass 95
Less than 2.0% of mass 174
Greater than 50.0% of mass 95
5.0 - 9.0% of mass 174
Greater than 95.0%, but less than 101.0% of mass 174
5.0 - 9.0% of mass 176
% RELATIVE
ABUNDANCE
_
•
( ) 1
( ) 1
( ) 1
( )2
1-Value is % mass 174
2-Value is % mass 176
THIS TUNE APPLIES TO THE FOLLOWING SAMPLES, MS, MSD, BLANKS, AND STANDARDS
| EPA
| SAMPLE NO.
i
1
oil
02|
03|
04|
05|
06|
07|
08 |
09 |
10|
HI
12|
13|
14|
15|
16|
17|
18|
19|
20)
211
22|
LAB
SAMPLE ID
LAB
FILE ID
DATE
ANALYZED
TIME
ANALYZED
page of
FORM V VOA
1/87 Rev.
-------
5B
SEMIVOLATILE ORGANIC GC/MS TUNING AND MASS
CALIBRATION - DECAFLUOROTRIPHENYLPHOSPHINE (DFTPP)
Lab Name:
Contract:
Lab Code:
Case No.:
SAS No.:
SDG No.:
Lab File ID:
Instrument ID:
DFTPP Injection Date:
DFTPP Injection Time:
m/e
51
68
69
70
127
197
198
199
275
365
441
442
443
ION ABUNDANCE CRITERIA
30.0 - 60.0% of mass 198
Less than 2.0% of mass 69
Mass 69 relative abundance
Less than 2.0% of mass 69
40.0 - 60.0% of mass 198
Less than 1.0% of mass 198
Base Peak, 100% relative abundance
5.0 to 9.0% of mass 198
10.0 - 30.0% of mass 198
Greater than 1.00% of mass 198
Present, but less than mass 443
Greater than 40.0% of mass 198
17.0 - 23.0% of mass 442
% RELATIVE
ABUNDANCE
( )1
( )1
( )2
1-Value is % mass 69
2-Value is % mass 442
THIS TUNE APPLIES TO THE FOLLOWING SAMPLES, MS, MSD, BLANKS, AND STANDARDS
page of
| EPA
j SAMPLE NO.
02 |
03|
04 |
05 |
06 |
07|
08|
09 |
10|
HI
12 |
13 |
14 |
15 |
I O I
17 |
18 |
1 Q 1
20|
21 1
22|
LAB
SAMPLE ID
LAB
FILE ID
DATE
ANALYZED
TIME
ANALYZED
FORM V SV
1/87 Rev.
-------
6A
VOLATILE ORGANICS INITIAL CALIBRATION DATA
Lab Name:
Contract:
Lab Code:
Case No.:
SAS No.:
SDG No.:
Instrument ID:
Matrix:(soil/water)
Calibration Date(s):
Level:(low/med) Column:(pack/cap)
Min RRF for SPCC(#) = 0.300 (0.250 for Bromoform) Max %RSD for CCC(*) = 30.0%
LAB FILE ID: RRF20 = RRF50 =
RRF100= RRF150= RRF200=
1
COMPOUND |RRF20
1.
Chloromethane #
Bromomethane
Vinyl Chloride *
Chloroethane
Methylene Chloride
Acetone
Carbon Disulfide |
1, 1-Dichloroethene *
1, 1-Dichloroethane #
1, 2-Dichloroethene (total) |
Chloroform *
1, 2-Dichloroethane |
2-Butanone
1,1, 1-Trichloroethane
Carbon Tetrachloride
Vinyl Acetate
Bromodichlorome thane
1, 2-Dichloropropane *
cis-1 , 3-Dichloropropene
Trichloroethene
Dibromochloromethane
1,1,2 -Trichloroethane
Benzene
trans-1 , 3-Dichloropropene
Bromoform S
2-Hexanone
Tetrachloroethene
1,1,2,2 -Tetrachloroethane #
Toluene *
Chlorobenzene #
Ethylbenzene *
Styrene
Xylene (total)
Toluene-d8
Bromof luorobenzene
T O r^ •» f^ V*t ~\ 4- V* S*L r3 A
j_ r £ u j-cn. j.oiroGT-fia.nG 0.4
RRF50
RRF100
RRF150
RRF200
RRF
— —
% 1
RSD
i
1
\
*
\
4
*
1
4
4
1
*
i
1
i
FORM VI VGA
1/87 Rev.
-------
6B
SEMIVOLATILE ORGANICS INITIAL CALIBRATION DATA
Lab Name:
Contract:
Lab Code:
Case No.:
SAS No.:
SDG No.:
Instrument ID:
Calibration Date(s):
Min RRF for SPCC(#) = 0.050
Max %RSD for CCC(*) = 30.0%
ILAB FILE ID: RRF20
RRF50 =
IRRF80 = RRF120= RRF160=
1
1 1
j COMPOUND RRF20
| Phenol *
I bis (2-Chloroethyl) ether
| 2-Chlorophenol
| 1, 3-Dichlorobenzene
1 1 , 4 -Dichlorobenzene •>
\ Benzyl alcohol
| 1,2-Dichlorobenzene
| 2-Methylphenol
|bis(2-Chloroisopropyl) ether
j 4-Methylphenol
| N-Nitroso-di-n-propylamine ;
| Hexachloroethane
[Nitrobenzene
| Isophorone
| 2-Nitrophenol *
| 2 , 4-Dimethylphenol
j Benzoic acid
j bis ( 2-Chloroethoxy ) methane
| 2,4-Dichlorophenol *
j 1 , 2 , 4-Trichlorobenzene
(Naphthalene
| 4-Chloroaniline
k
'
IT
IT
| Hexachlorobutadiene *
| 4-Chloro-3-methylphenol *
| 2-Methylnaphthalene
| Hexachlorocyclopentadiene j
j 2,4, 6-Trichlorophenol •>
»
V
| 2 , 4 , 5-Trichlorophenol
| 2-Chloronaphthalene
| 2-Nitroaniline
| Dimethylphthalate
| Acenaphthylene
| 2 , 6-Dinitrotoluene
j 3-Nitroaniline
| Acenaphthene *
j 2 , 4 -Dinitrophenol #
|4-Nitrophenol #
1 1
RRF50
RRF80
RRF120
RRF160
—
RRF
%
RSD
:
4
4
i
4
4
1
*
4
1
1
1
1
<
*
*
1
FORM VI SV-1
1/87 Rev.
-------
Lab Name:
Lab Code:
6C
SEMIVOLATILE ORGANICS INITIAL CALIBRATION DATA
Contract:
Case No.: SAS No.: SDG No.:
Instrument ID:
Calibration Date(s):
Min RRF for SPCC(#) = 0.050
Max %RSD for CCC(*) = 30.0%
ILAB FILE ID: RRF20
RRF50 =
IRRF80 = RRF120= RRF160=
I
1
j COMPOUND
i
j Dibenzof uran
| 2 , 4-Dinitrotoluene
| Diethylphthalate
| 4-Chlorophenyl-phenylether_
j Fluorene
| 4-Nitroaniline
| 4 , 6-Dinitro-2-methylphenol_
JN-Nitrosodiphenylamine (1)_J
| 4-Bromophenyl-phenylether
| Hexachlorobenzene
| Pentachlorophenol *
| Phenanthrene
| Anthracene
| Di-n-butylphthalate
| Fluoranthene *
| Pyrene
| Butylbenzylphthalate
j 3 , 3 ' -Dichlorobenzidine
| Benzo (a) anthracene
| Chrysene
| bis (2-Ethylhexyl) phthalate_
| Di-n-octylphthalate
| Benzo (b) fluoranthene
| Benzo (k) fluoranthene
| Benzo(a)pyrene
| Indeno(l,2, 3-cd)pyrene
| Dibenz (a,h) anthracene
| Benzo(g,h, i) perylene
1
| Nitrobenzene-d5
| 2-Fluorobiphenyl
| Terphenyl-dl4
| Phenol-d5
| 2-Fluorophenol
| 2 , 4 , 6-Tribromophenol
1
RRF20
k
k
k
k
RRF50
RRF80
KRF120
RRF160
RRF
% 1
RSD |
*
*
*
i
(1) Cannot be separated from Diphenylamine
FORM VI SV-2
1/87 Rev.
-------
7A
VOLATILE CONTINUING CALIBRATION CHECK
Lab Name:
Contract:
Lab Code:
Case No.:
SAS No.:
Instrument ID:
Lab File ID:
Calibration Date:
SDG No.:
Time:
Matrix:(soil/water)
Init. Calib. Date(s):
Level:(low/med)
Column:(pack/cap)
Min RRF50 for SPCC(#) = 0.300 (0.250 for Bromoform) Max %D for CCC(*) = 25.0%
1
| COMPOUND
| Chi orome thane
| Bromomethane
| Vinyl Chloride
| Chloroethane
IMethylene Chloride
| Acetone
| Carbon Disulfide
| 1, 1-Dichloroethene
| 1, 1-Dichloroethane
| 1, 2-Dichloroethene (total)
| Chloroform
| 1, 2-Dichloroethane
| 2-Butanone
| 1, 1, 1-Trichloroethane
| Carbon Tetrachloride
| Vinyl Acetate
| Bromodichloromethane
| 1, 2-Dichloropropane *
j cis-l , 3-Dichloropropene
| Trichloroethene
| Dibromochloromethane
| 1 , 1 , 2-Trichloroethane
| Benzene
| trans-1, 3-Dichloropropene
| Bromoform
| 4-Methyl-2-Pentanone
| 2-Hexanone
| Tetrachloroethene
| 1,1,2, 2-Tetrachloroethane |
| Toluene *
\ Chlorobenzene i
| Ethylbenzene <
| Styrene
IXylene (total) |
| Toluene-d8 |
| Bromof luorobenzene
| 1 , 2-Dichloroethane-d4 |
1 1
RRF
\
k
Ic
\
Ic
Ic
f
c
=
r
RRF50
...
%D
_r_ _
1
i
1
4
*
•i
*
'•
%
*
*
*
FORM VII VOA
1/87 Rev.
-------
Lab Name:
Lab Code:
7B
SEMIVOLATILE CONTINUING CALIBRATION CHECK
Contract:
SAS No.:
Case No.:
Instrument ID:
Lab File ID:
Calibration Date:
SDG No.:
Time:
Init. Calib. Date(s):
Min RRF50 for SPCC(#) = 0.050
Max %D for CCC(*) = 25.0%
1
| COMPOUND
I
| Phenol *
| bis (2-Chloroethyl ) ether
| 2-Chlorophenol
| 1 , 3-Dichlorobenzene
| 1,4-Dichlorobenzene *
| Benzyl alcohol
1 1 , 2-DichLprobenzene
| 2-Methylphenol
| bis (2-Chloroisopropyl) ether
|4-Methylphenol
| N-Nitroso-di-n-propylamine
| Hexachloroethane
| Nitrobenzene
| Isophorone
|2-Nitrophenol >
| 2 , 4-Dimethylphenol
| Benzoic acid
| bis (2-Chloroethoxy) methane
| 2,4-Dichlorophenol '
| 1, 2, 4-Trichlorobenzene
| Naphthalene
j 4-Chloroaniline
| Hexachlorobutadiene '
| 4-Chloro-3-methylphenol '
| 2-Methylnaphthalene
| Hexachlorocyclopentadiene
| 2,4,6-Trichlorophenol '
| 2 , 4 , 5-Trichlorophenol
| 2-Chloronaphthalene
| 2-Nitroaniline
| Dimethylphthalate
| Acenaphthylene
| 2 , 6-Dinitrotoluene
| 3-Nitroaniline
| Acenaphthene *
| 2, 4-Dinitrophenol :
|4-Nitrophenol ;
1
RRF
:
k
1
k
k
It
It
»
k
\t
1
f
RRF50
%D
i
i
i
i
*
i
1
1
^
4
1
*
1
FORM VII SV-1
1/87 Rev.
-------
Lab Name:
Lab Code:
7C
SEMIVOLATILE CONTINUING CALIBRATION CHECK
Contract:
SAS No.:
Case No.:
Instrument ID:
Lab File ID:
Calibration Date:
SDG No.:
Time:
Init. Calib. Date(s):
Min RRF50 for SPCC(#) = 0.050
Max %D for CCC(*) = 25.0%
1
| COMPOUND
| Dibenzofuran
| 2 , 4-Dinitrotoluene
| Diethylphthalate
| 4-Chlorophenyl-phenylether
| Fluorene
|4-Nitroaniline
| 4 , 6-Dinitro-2-methylphenol
| N-Nitrosodiphenylamine (1)
| 4-Bromophenyl-phenylether
| Hexachlorobenzene
| Pentachlorophenol
I Phenanthrene
| Anthracene
j Di-n-butylphthalate
| Fluoranthene
| Pyrene
| Butylbenzylphthalate
| 3 , 3 ' -Dichlorobenzidine
| Benzo (a) anthracene
| Chrysene
| bis (2-Ethylhexyl) phthalate
j Di-n-octylphthalate
| Benzo (b) fluoranthene
| Benzo (k) fluoranthene
| Benzo (a) pyrene
| Indeno (1,2, 3 -cd) pyrene
j Dibenz (a, h) anthracene
| Benzo(g,h, i)perylene
| Nitrobenzene-d5
| 2-Fluorobiphenyl
|Terphenyl-dl4
| Phenol-d5
| 2-Fluorophenol
| 2 , 4 , 6-Tribromophenol
1
RRF
it
k
k
k
k
RRF50
%D
4
i
(1) Cannot be separated from Diphenylamine
FORM VII SV-2
1/87 Rev.
-------
Lab Name:
Lab Code:
8A
VOLATILE INTERNAL STANDARD AREA SUMMARY
Contract:
SAS No.:
Case No.:
Lab File ID (Standard):
Instrument ID:
Matrix:(soil/water)
Level:(low/med)
SDG No.:
Date Analyzed:
Time Analyzed:
Column:(pack/cap)
1
1
1
1
| 12 HOUR STD
| UPPER LIMIT
| LOWER LIMIT
I
| EPA SAMPLE
j NO.
1 ============
oil
02|
03|
04|
05|
06|
07 |
08|
09 |
10|
HI
12 |
13|
14|
15|
16|
17|
18|
19|
20|
21|
22|
ISl(BCM)
AREA #
RT
IS2(DFB)
AREA |
RT
IS3(CBZ)
AREA #
=
RT
IS1 (BCM) = Bromochloromethane
IS2 (DFB) = 1,4-Difluorobenzene
IS3 (CBZ) = Chlorobenzene
UPPER LIMIT = + 100%
of internal standard area.
LOWER LIMIT = - 50%
of internal standard area.
# Column used to flag internal standard area values with an asterisk
page of
FORM VIII VOA
1/87 Rev.
-------
8B
SEMIVOLATILE INTERNAL STANDARD AREA SUMMARY
Lab Name:
Lab Code:
Case No.:
Lab File ID (Standard):
Instrument ID:
Contract:
SAS No.:
SDG No.
Date Analyzed:
Time Analyzed:
1
1
| 12 HOUR STD
1
| UPPER LIMIT
| LOWER LIMIT
| EPA SAMPLE
| NO.
oil
02 |
03|
04 |
05|
06|
07|
08 |
09 |
10|
HI
12|
13|
14|
15|
16|
17|
18|
19|
20|
21|
22|
ISl(DCB)
AREA f
==========
RT
_-_——_.___
IS2(NPT)
AREA *
RT
IS3(ANT)
AREA #
RT
======
IS1 (DCB) = l,4-Dichlorobenzene-d4
IS2 (NPT) = Naphthalene-d8
IS3 (ANT) = Acenaphthene-d8
UPPER LIMIT = 4- 100%
of internal standard area.
LOWER LIMIT = - 50%
of internal standard area.
# Column used to flag internal standard area values with an asterisk
page
of
FORM VIII SV-1
1/87 Rev.
-------
8C
SEMIVOLATILE INTERNAL STANDARD AREA SUMMARY
Lab Name:
Lab Code:
Case No.:
Contract:
SAS No.:
SDG No.
Lab File ID (Standard):
Instrument ID:
Date Analyzed:
Time Analyzed:
12 HOUR STD
UPPER LIMIT
LOWER LIMIT
EPA SAMPLE
NO.
IS4(PHN)
AREA #
RT
ISS(CRY)
AREA #
RT
IS 6 (PRY)
AREA #
RT
I T._ I ,_
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
IS4 (PHN) = Phenanthrene-dlO
IS5 (CRY) = Chrysene-dl2
IS6 (PRY) = Perylene-dl2
UPPER LIMIT = + 100%
of internal standard area.
LOWER LIMIT = - 50%
of Internal standard area.
# Column used to flag internal standard area values with an asterisk
page of
FORM VIII SV-2
1/87 Rev.
-------
8D
PESTICIDE EVALUATION STANDARDS SUMMARY
Lab Name:
Lab Code:
Instrument ID:
Dates of Analyses:
Case No.:
Contract:
SAS No. :
SDG No.
GC Column ID:
to
Evaluation Check for Linearity
1
1 PESTICIDE
1
-
I Aldrin
I Endrin
1 4,4* -DDT
| DBC
1
| CALIBRATION |
j FACTOR |
| EVAL MIX A |
1 I ~
1 1
1 1
1 1
1 1
1 1
CALIBRATION
FACTOR
EVAL MIX B
CALIBRATION | %RSD |
FACTOR j ( 10.0% RSD, plot a standard curve and determine the ng
for each sample in that set from the curve.
Evaluation Check for 4,4'-DDT/Endrin Breakdown
(percent breakdown expressed as total degradation)
1
1
| INITIAL
01 | EVAL MIX B
02 | EVAL MIX B
03 | EVAL MIX B
04 | EVAL MIX B
05 | EVAL MIX B
06 | EVAL MIX B
07 j EVAL MIX B
08 | EVAL MIX B
09 | EVAL MIX B
10 | EVAL MIX B
11| EVAL MIX B
12 j -EVAL MIX B
13 | EVAL MIX B
14 | EVAL MIX B
1
DATE
ANALYZED
TIME
ANALYZED
ENDRIN
4,4' -DDT
•
COMBINED |
(2)
(2) See Form instructions.
FORM VIII PEST-1
8/87 Rev.
-------
8E
PESTICIDE EVALUATION STANDARDS SUMMARY
Evaluation of Retention Time Shift for Dibutylchlorendate
Lab Name:
Lab Code:
Case No.:
Contract:
SAS No.:
SDG No.:
Instrument ID:
GC Column ID:
Dates of Analyses:
to
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
EPA
SAMPLE NO.
LAB SAMPLE
ID
DATE
ANALYZED
TIME
ANALYZED
D
*
* Values outside of QC limits (2.0% for packed columns,
0.3% for capillary columns)
page
of
FORM VIII PEST-2
1/87 Rev.
-------
PESTICIDE/PCB STANDARDS SUMMARY
Lab Name:
Lab Code:
Case No.:
Contract:
SAS No.:
SDG No.:
Instrument ID:
GC Column ID:
1
| COMPOUND
1
| alpha-BHC
| beta-BHC
| delta-BHC
| gamma-BHC
| Heptachlor
|Aldrin
|Hept. epoxide
JEndosulfan I
|Dieldrin
| 4 , 4 ' -DDE
| Endrin
jEndosulfan II
j 4 , 4 ' -ODD
(Endo. sulfate
| 4 , 4 ' -DDT
| Methoxychlor
| Endrin ketone
|a. Chlordane
|g. Chlordane
| Toxaphene
|Aroclor-1016
|Aroclor-122l
JAroclor-1232
|Aroclor-1242_
j Aroclor-1248
(Aroclor-1254
j Aroclor-1260
1
DATE(S) OF FROM:
ANALYSIS
TO:
TIME(S) OF FROM:
ANALYSIS
RT
i
WIl
FROM
TO:
RT
YDOW
TO
1
CALIBRATION
FACTOR
DATE OF ANALYSIS
TIME OF ANALYSIS
EPA SAMPLE NO.
(STANDARD)
RT
CALIBRATION
FACTOR
IQNT
IY/N
1
| %D
1
Under QNT Y/N: enter Y if quantitation was performed, N if not performed,
%D must be less than or equal to 15.0% for quantitation, and less than
or equal to 20.0% for confirmation.
Note: Determining that no compounds were found above the CRQL is a form of
quantitation, and therefore at least one column must meet the 15.0% criteria.
For multicomponent analytes, the single largest peak that is characteristic
of the component should be used to establish retention time and %D.
Identification of such analytes is based primarily on pattern recognition.
page
of
FORM IX PEST
8/87 Rev.
-------
Lab Name:
Lab Code:
10
PESTICIDE/PCB IDENTIFICATION
Contract:
SAS No.:
EPA SAMPLE NO.
Case No.:
SDG No.:
GC Column ID (1) :
Instrument ID (1) :
Lab Sample ID:
Lab File ID:
GC Column ID (2):
Instrument ID (2):
(only if confirmed by GC/MS)
PESTICIDE/PCB
RETENTION TIME
RT WINDOW
OF STANDARD
From TO
QUANT? GC/MS?
(Y/N) (Y/N)
01
02
03
04
05
06
07
08
09
10
11
12
Comments :
Column
Column
Column
Column
Column
Column
Column
Column
Column
Column
Column
Column
1
2
1
2
1
2
1
2
1
2
1
2
page
of
FORM X PEST
1/87 Rev.
-------
RAS INORGANICS DELIVERY REQUIREMENTS
-------
This page was intentionally left blank
-------
RAS Inorganics
Delivery Requirements
A. Contract Start-Up Plan
The contract laboratory must submit a start-up plan for PO approval that details the
laboratory's proposed schedule for receiving samples. The laboratory will be required to
receive samples within thirty days of contract award.
B. Updated Standard Operating Procedures
The contract laboratory must submit updated copies of all required SOPs that were
submitted prior to contract award. The updated SOPs must address any and all issues of
performance and operation identified during the preaward evaluation process..
C. Sample Traffic Reports
The original Sample TR must be returned to SMO with lab receipt information for each
sample in the SDG. TRs must be submitted in SDG sets with an SDG coversr-eet
attached.
D. Sample Data Package
The sample data package shall include data for analysis of all samples in one SDG,
including field samples, reanalyses, blanks, matrix spikes, matrix spike duplicates, and
laboratory control samples. The sample data package must include the following:
1. Cover Page
The cover page must include: laboratory name; laboratory code; contract number;
Case number; SDG number; SOW number; EPA sample numbers in alphanumeric
order; detailed documentation of any problems encountered in processing the
samples; and completion of the statement on use of ICP background and
interelement corrections for the samples.
2. Sample Data
a. Results — Inorganic Analysis Data Sheet [FORM I - IN]
Tabulated analytical results (identification and quantitation) of the specified
analytes. Appropriate concentration units must be specified and entered on
Form I.
b. Quality Control Data
(!) Initial and Continuing Calibration Verification [FORM II (PART 1) -
IN]
(2) CRDL Standard for AA and Linear Range Analysis for ICP [FORM II
(PART 2) - IN]
(3) Blanks [FORM HI - IN]
(4) ICP Interference Check Sample [FORM IV - IN]
C-47
-------
(5) Spike Sample Recovery [FORM V (PART 1) - IN]
(6) Post Digest Spike Sample Recovery [FORM V (PART 2) - IN]
(7) Duplicates [FORM VI - IN]
(8) Laboratory Control Sample [FORM VII - IN]
(9) Standard Addition Results [FORM VIII - IN]
(10) ICP Serial Dilutions [FORM IX - IN]
(11) Preparation Log [Form XIII - IN]
(12) Analysis Run Log [Form XIV - IN]
c. Quarterly Verification of Instrument Parameters
(1) Instrument Detection Limits (Quarterly) [FORM X - IN]
(2) ICP Interelement Correction Factors (Annually) [FORM XI (PART 1)
- IN]
(3) ICP Interelement Correction Factors (Annually) [FORM XI (PART 2)
- IN]
(4) ICP Linear Ranges (Quarterly) [FORM XII - IN]
(Copies of Quarterly Verification of Instrument Parameters forms for the
current quarter must be submitted with each data package.)
d. Raw Data
For each reported value, all raw data used to obtain that value must be
included in the data package. This applies to all required QA/QC
measurements, instrument standardization, as well as all sample analysis
results. This statement does not apply to the Quarterly Verification of
Instrument Parameters submitted as a part of each data package. Raw data
must contain all instrument readouts used for the sample results. Each
exposure or instrumental reading must be provided, including those readouts
that may fall below the IDL. All AA and ICP instruments must provide a
legible hard copy of the direct real-time instrument readout (i.e., stripcharts,
printer tapes, etc.). A photocopy of the instruments direct sequential readout
must be included. A hardcopy of the instrument's direct instrument readout
for cyanide must be included if the instrumentation has the capability.
Raw data in the data package must be ordered as follows: ICP, Flame AA,
Furnace AA, Mercury, and Cyanide. All raw data must include concentration
units for ICP and absorbances with concentration units for flame AA, furnace
AA, Mercury and Cyanide. All flame and furnace AA data must be grouped
by element.
C-48
-------
Raw data must be labeled with EPA sample number and appropriate codes,
shown in Table 1 following, to identify:
(1) Calibration standards, including source and prep date
(2) Initial and continuing calibration blanks and preparation blanks
(3) Initial and continuing calibration verification standards, interference
check samples, ICP serial dilution samples, CRDL Standard for ICP
and AA, Laboratory Control Sample and Post Digestion Spike
(4) Diluted and undiluted samples and all weights, dilutions and volumes
used to obtain the reported values
(5) Duplicates
(6) Spikes
(7) Instrument used, any instrument adjustments, data corrections or other
apparent anomalies on the measurement record, including all data
voided or data not used to obtain reported values and a brief written
explanation
(8) All information for furnace analysis clearly and sequentially identified
on the raw data, including EPA sample number, sample and analytical
spike data, percent recovery, coefficient of variation, full MSA data,
MSA correlation coefficient, slope and intercepts of linear fit, final
sample concentration (standard addition concentration), and type of
background correction used: BS for Smith-Heiftje, BD for Deuterium
Arc, or BZ for Zeeman
(9) Time and date of each analysis
(10) Integration times for A A analyses
e. Digestion and Distillation Logs
Logs shall be submitted in the following order: digestion logs for ICP, flame
AA, furnace AA and mercury preparations, followed by a copy of the
distillation log for cyanide.
3. A copy of the Sample TRs in Item C must be submitted for all of the samples in an
SDG. The TRs must be arranged in increasing EPA sample number order.
E. Data in Computer Readable Form
The contract laboratory must provide a computer-readable copy of the data on data
reporting Forms I-XIV for all samples in an SDG. Computer-readable data deliverables
shall be submitted on IBM or IBM-compatible, 5.25 inch floppy double-sided, double
density 360 K-byte or a high density 1.2 M-byte diskette. The data must be recorded in
ASCII, text file format, and must adhere to the file, record and field specifications listed
in the SOW.
C-49
-------
Table 1
Codes for Labelling Raw Data
Sample XXXXXX
Duplicate XXXXXXD
Matrix Spike XXXXXXS
Serial Dilution XXXXXXL
Analytical Spike XXX XXXA
Post Digestion/Distillation Spike XXX XXXA
MSA:
Zero Addition XXXXXXO
First Addition XXXXXX 1
Second Addition XXXXXX2
Third Addition XXXXXX3
Instrument Calibration Standards:
ICP S or SO for blank standard
Atomic Absorption and Cyanide SO, SI0,...etc.
Initial Calibration Verification ICV
Initial Calibration Blank ICB
Continuing Calibration Verification CCV
Continuing Calibration Blank CCB
Interference Check Samples:
Solution A ICSA
Solution AB ICSAB
CRDL Standard for AA CRA
CRDL Standard for ICP CRI
Laboratory Control Samples:
Aqueous (Water) LCSW
Solid (Soil/Sediment) LCSS
Preparation Blank (Water) PBW
Preparation Blank (Soil) PBS
Linear Range Analysis Standard LRS
Notes:
1. When an analytical spike or MSA is performed on samples other than field samples, the
"A", "0", "1", "2" or "3" suffixes must be the last to be added to the EPA Sample Number.
For instance, an analytical spike of a duplicate must be formatted "XXXXXXDA."
2. The numeric suffix that follows the "S" suffix for the standards indicates the true value of
the concentration of the standard in ug/L.
3. ICP calibration standards usually consist of several analytes at different concentrations.
Therefore, no numeric suffix can follow the ICP calibration standards unless all the
analytes in the standard are prepared at the same concentrations. For instance, the blank
for ICP must be formatted "SO."
4. The CRDL standard for AA is considered to be a calibration standard if it was a part of
the calibration curve, thus it must be formatted like any other standard. The "CRA"
format must be used if the CRDL standard for AA is not used to establish the calibration
curve.
C-50
-------
F. Results of Intercomparison/Performance Evaluation Sample Analyses
Tabulation of analytical results for Intercomparison/PE Sample analyses include all
requirements specified in Items D and E.
G. Complete Case File Puree
The complete case file purge includes all laboratory records received or generated for a
specific Case that have not been previously submitted to EPA as a deliverable. These
items include but are not limited to: sample tags, custody records, sample tracking
records, analysts logbook pages, bench sheets, instrument readout records, computer
printouts, raw data summaries, instrument logbook pages (including instrument
conditions), correspondence, and the document inventory.
I. Quarterly Verification of Instrument Parameters
The contract laboratory must perform and report quarterly verification of instrument
detection limits and linear range by methods specified in the SOW for each instrument
used. For the ICP instrumentation and methods, the contract laboratory must also report
quarterly interelement correction factors (including method of determination),
wavelengths used and integration times. Quarterly Verification of Instrument Parameters
forms for the current quarter must be submitted in each SPG data package, using Forms
X, XI and XII. Submission of Quarterly Verification of Instrument Parameters must
include the raw data used to determine those values reported.
C-51
-------
RAS INORGANICS
DATA REPORTING FORMS
-------
Lab Name:
Lab Code:
SOW No.:
U.S. EPA - CLP
COVER PAGE - INORGANIC ANALYSES DATA PACKAGE
Contract:
SAS No.:
Case No.:
SDG No.:
EPA Sample No.
Lab Sample ID.
Were ICP interelement corrections applied?
Were ICP background corrections applied?
If yes-were raw data generated before
application of background corrections?
Comments:
Yes/No
Yes/No
Yes/No
Release of the data contained in this hardcopy data package and in the
computer-readable data submitted on floppy diskette has been authorized by
the Laboratory Manager or the Manager's designee, as verified by the
following signature.
Lab Manager:
Date:
COVER PAGE - IN
7/87
-------
U.S. EPA - CLP
EPA SAMPLE NO.
Lab Name:
Lab Code:
INORGANIC ANALYSIS DATA SHEET
Contract:
Case No.:
SAS No.:
SDG No.:
Matrix (soil/water):
Level (low/med):
% Solids:
Lab Sample ID:
Date Received:
Concentration Units (ug/L or mg/kg dry weight):
Color Before:
Color After:
Comments:
CAS No.
7429-90-5
7440-36-0
7440-38-2
7440-39-3
7440-41-7
7440-43-9
7440-70-2
7440-47-3
7440-48-4
7440-50-8
7439-89-6
7439-92-1
7439-95-4
7439-96-5
7439-97-6
7440-02-0
7440-09-7
7782-49-2
7440-22-4
7440-23-5
7440-28-0
7440-62-2
7440-66-6
Analyte
Aluminum
Antimony
Arsenic
Barium
Beryllium
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Mercury
Nickel
Potassium
Selenium
Silver
Sodium
Thallium
Vanadium
Zinc
Cyanide
Concentration
1
M
Clarity Before:
Clarity After:
Texture:
Artifacts:
FORM I
IN
7/87
-------
U.S. EPA - CLP
2A
INITIAL AND CONTINUING CALIBRATION VERIFICATION
Lab Name:
Lab Code:
Case No.:
Contract:
SAS No.:
SDG No.:
Initial Calibration Source:
Continuing Calibration Source:
Concentration Units: ug/L
I
1
| Analyte
1
| Aluminum
| Antimony
(Arsenic
| Barium
| Beryllium
| Cadmium
j Calcium
| Chromium
1 Cobalt
| Copper
| Iron
|Lead
| Magnesium
(Manganese
1 Mercury
(Nickel
| Potassium
I Selenium
(Silver
| Sodium
|Thallium_
| Vanadium_
j Zinc
| Cyanide
1
Initial Calibration
True Found %R(1)
Continuing Calibration
True Found %R(1) Found %R(1)
1
M
(1) Control Limits: Mercury 80-120; Other Metals 90-110; Cyanide 85-115
FORM II (PART 1) - IN
7/87
-------
Lab Name:
Lab Code:
U.S. EPA - CLP
2B
CRDL STANDARD FOR AA AND ICP
Contract:
SAS No.:
Case No.:
AA CRDL Standard Source:
ICP CRDL Standard Source:
SDG No.:
Concentration Units: ug/L
1
1
1
| Analyte
1
| Aluminum
| Antimony
| Arsenic
| Barium
| Beryllium
| Cadmium
| Calcium
| Chromium
I Cobalt
| Copper
| Iron
|Lead
[Magnesium
| Manganese
| Mercury
| Nickel
| Potassium
| Selenium
| Silver
| Sodium
| Thallium
(Vanadium
|Zinc
1
CRDL S
True
tandard fo
Found
r AA
%R
True
CRDL Stai
Initial
Found
idard J
%R
for ICP
Final
Found
L
%R
FORM II (PART 2) - IN
7/87
-------
U.S. EPA - CLP
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 rag/kg):
1
1
1
1
| Analyte
1
| Aluminum
| Antimony
| Arsenic
| Barium
| Beryllium
j Cadmium
| Calcium
| Chromium
| Cobalt
I Copper
|Iron
(Lead
(Magnesium
I Manganese
| Mercury
| Nickel
| Potassium
| Selenium
| Silver
| Sodium
(Thallium
| Vanadium
| Zinc
| Cyanide
1
Initial
Calib.
Blank
(ug/L) C
—
—
Continuing Calibration
Blank (ug/L)
1 C 2 C 3
—
1
C
Prepa-
ration
Blank C
i
M
• —
FORM III - IN
7/87
-------
U.S. EPA - CLP
ICP INTERFERENCE CHECK SAMPLE
Lab Name:
Lab Code: Case No:
ICP ID Number:
Contract:
SAS No. :
ICS Source:
SDG No
Concentration Units: ug/L
1
1
1
| Analyte
1
| Aluminum
j Antimony
| Arsenic
| Barium
| Beryllium
I Cadmium
| Calcium
| Chromium
j Cobalt ~
| Copper
| Iron
|Lead
[Magnesium
! Manganese
| Mercury
(Nickel
| Potassium
| Selenium
| Silver
| Sodium
[Thallium
(Vanadium
| Zinc
1
True
Sol. Sol.
A AB
Initial Found
Sol. Sol.
A AB %R
Final Found
Sol. Sol.
A AB %R
FORM IV - IN
7/87
-------
U.S. EPA - CLP
5A
SPIKE SAMPLE RECOVERY
EPA SAMPLE NO.
I
Lab Name:
Lab Code:
Contract:
Case No.:
SAS No.:
SDG No.:
Matrix (soil/water):
Level (low/med):
Concentration Units (ug/L or mg/kg dry weight):
1
1
1
| Analyte
1
| Aluminum
| Antimony
| Arsenic
| Barium
| Beryllium
I Cadmium
| Calcium
| Chromium
| Cobalt
| Copper
| Iron
[Lead
| Magnesium
| Manganese
| Mercury
| Nickel
| Potassium
| Selenium
(Silver
| Sodium
| Thallium
| Vanadium
j Zinc
| Cyanide
1
Control
Limit
%R
Spiked Sample
Result (SSR)
C
Sample
Result (SR)
C
Spike
Added (SA)
'
%R
Q
M
Comments:
FORM V (PART 1) - IN
7/87
-------
U.S. EPA - CLP
5B
POST DIGEST SPIKE SAMPLE RECOVERY
EPA SAMPLE NO.
r
Lab Name:
Lab Code:
Contract:
Case No.:
SAS No.:
Matrix (soil/water):
SDG No.:
Level (low/med):
Concentration Units: ug/L
1
1
1
| Analyte
1
| Aluminum
| Antimony
| Arsenic
| Barium
| Beryllium
| Cadmium
| Calcium
| Chromium
| Cobalt
| Copper
| Iron
(Lead
(Magnesium
| Manganese
| Mercury
| Nickel
| Potassium
(Selenium
[Silver
| Sodium
(Thallium
(Vanadium
| Zinc
| Cyanide
1
Control
Limit
%R
Spiked Sample
Result (SSR)
Sample
Result (SR) C
Spike
Added (SA)
%R
M
Comments:
FORM V (PART 2) -r IN
7/87
-------
Lab Name:
Lab Code:
U.S. EPA - CLP
DUPLICATES
Contract:
EPA SAMPLE NO.
I
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):
1
1
| Analyte
1
| Aluminum
(Antimony
(Arsenic
| Barium
| Beryllium
| Cadmium
| Calcium
| Chromium
| Cobalt
| Copper
| Iron
(Lead
(Magnesium
(Manganese
| Mercury
| Nickel
| Potassium
| Selenium
| Silver
| Sodium
(Thallium
(Vanadium
| Zinc
| Cyanide
1
Control
Limit
Sample (S)
C
Duplicate (D)
C
RPD
1
Q
M
FORM VI - IN
7/87
-------
Lab Name:
Lab Code:
U.S. EPA - CLP
LABORATORY CONTROL SAMPLE
Contract:
SAS No.:
Case No.:
SDG No.
Solid LCS Source:
Aqueous LCS Source:
1
1
| Analyte
1
| Aluminum
(Antimony
(Arsenic
| Barium
| Beryllium
j Cadmium
j Calcium
(Chromium
| Cobalt
| Copper
(Iron
(Lead
(Magnesium
(Manganese
(Mercury
(Nickel
j Potassium
j Selenium
(Silver
| Sodium
(Thallium
(Vanadium
| Zinc
| Cyanide
1
Aqueous (ug/L)
True Found %R
Sol
True Found
(mg/kg)
Limits %R
FORM VII - IN
12/87 Rev
-------
U.S. EPA - CLP
8
STANDARD ADDITION RESULTS
Lab Name
Lab Code
•
•
: Case No. :
Contract
SAS No . :
•
•
SDG No. :
Concentration Units: ug/L
EPA
Sample
No.
An
Oil
0 ADD
ABS
1 ADD
CON ABS
~~
~~
2 ADD
CON ABS
3 ADD
CON ABS
~~~
Final
Cone.
r
Q
~
FORM VIII - IN
7/87
-------
Lab Name:
Lab Code:
Case No.:
U.S. EPA - CLP
9
ICP SERIAL DILUTIONS
Contract:
SAS No.:
EPA SAMPLE NO.
r
SDG No.:
Matrix (soil/water):
Level (low/med):
Concentration Units: ug/L
1
1
| Analyte
1
| Aluminum
| Antimony
| Arsenic
| Barium
| Beryllium
| Cadmium
| Calcium
| Chromium
| Cobalt
| Copper
llron
|Lead
(Magnesium
| Manganese
| Mercury
I Nickel
| Potassium
| Selenium
I Silver
(Sodium
(Thallium
| Vanadium
| Zinc
1
Initial Sample
Result (I)
c
Serial
Dilution
Result (S)
C
%
Differ-
ence
;
Q
M
FORM IX - IN
7/87
-------
U.S. EPA - CLP
10
HOLDING TIMES
Lab Name:
Lab Code:
Case No.:
Contract:
SAS No.:
SDG No.
EPA
Sample No.
Matrix
Date
Received
Mercury
Prep
Date
Mercury
Holding
Time
Cyanide
Prep
Date
i
Cyanide
(Holding
Time
FORM X - IN
7/87
-------
Lab Name:
Lab Code:
ICP ID Number:
Flame AA ID Number:
Furnace AA ID Number:
U.S. EPA - CLP
11
INSTRUMENT DETECTION LIMITS (QUARTERLY)
Contract:
SAS No.:
Date:
Case No.:
SDG No.
Comments:
1
1
1
| Analyte
1
| Aluminum
[Antimony
| Arsenic
| Barium
| Beryllium
| Cadmium
(Calcium
| Chromium
| Cobalt
| Copper
(Iron
|Lead
(Magnesium
| Manganese
| Mercury
(Nickel
| Potassium
| Selenium
(Silver
| Sodium
(Thallium
| Vanadium
| Zinc
Wave-
length
(nm)
Back-
ground
CRDL
(ug/L)
200
60
10
200
5
5
5000
10
50
25
100
5
5000
15
0.2
40
5000
5
10
5000
10
50
20
IDL
(ug/L)
M
FORM XI - IN
7/87
-------
U.S. EPA - CLP
12A
TCP INTERELEMENT CORRECTION FACTORS (QUARTERLY)
Lab Name:
Lab Code:
Case No.
ICP ID Number:
Contract:
SAS No.:
Date:
SDG No.
1
1
1
1 Analyte
1
| Aluminum
(Antimony
(Arsenic
| Barium
| Beryllium
| Cadmium
(Calcium
| Chromium
(Cobalt
| Copper
| Iron
(Lead
(Magnesium
| Manganese
| Mercury
| Nickel
| Potassium
(Selenium
(Silver
| Sodium
(Thallium
(Vanadium
| Zinc
1
Wave-
length
(nm)
It
Al
iterelement
Ca
Correction
Fe
Factors foi
Mg
. •
Comments:
FORM XII (PART 1) - IN
7/87
-------
U.S. EPA - CLP
12B
ICP INTERELEMENT CORRECTION FACTORS (QUARTERLY)
Lab Name:
Lab Code:
Case No.
ICP ID Number:
Contract:
SAS No.:
Date:
SDG No.
1
1
1
| Analyte
1
| Aluminum
| Antimony
(Arsenic
| Barium
| Beryllium
| Cadmium
| Calcium
| Chromium
| Cobalt
I Copper
llron
[Lead
(Magnesium
| Manganese
| Mercury
| Nickel
| Potassium
| Selenium
(Silver
| Sodium
(Thallium
| Vanadium
(Zinc
1
Wave-
length
(nm)
Ii
vterelement
Correction
Factors foi
f *
Comments:
FORM XII (PART 2) - IN
7/87
-------
U.S. EPA - CLP
13
TCP LINEAR RANGES (QUARTERLY)
Lab Name:
Lab Code:
ICP ID Number:
Case No.:
Contract:
SAS No.:
Date:
SDG No.
1
1
1
| Analyte
!
| Aluminum
| Antimony
! Arsenic
| Barium
| Beryllium
| Cadmium
| Calcium
| Chromium
I Cobalt
I Copper
llron
(Lead
(Magnesium
| Manganese
| Mercury
| Nickel
| Potassium
| Selenium
(Silver
| Sodium
(Thallium
(Vanadium
| Zinc
1
Integ.
Time
(Sec.)
Concentration
(ug/L)
M
Comments:
FORM XIII - IN
7/87
-------
RAS DIOXIN DELIVERY REQUIREMENTS
-------
This page was intentionally left blank
-------
RAS Dioxin
Delivery Requirements
A. Dioxin Shipment Record
The contract laboratory must submit the original Sample DSR with lab receipt
information.
B. Sample Data Summary Package
The contract laboratory is required to submit a hard copy of analytical data and
documentation from the sample data package as follows:
1. Case Narrative
2. Completed data reporting sheets consisting of Forms B-l, B-2, B-3 and B-4.
Original and rerun sample data must be provided on Form B-l.
C. Sample Data Package
Hard copy analytical data and documentation are required as described below:
1. The Case Narrative must contain: the Case number, DSR numbers, contract number
and detailed documentation of any quality control, sample shipment and/or
analytical problems encountered in a specific Case.
2. Copies of completed DSRs for all samples reported in the data package.
3. Results of initial triplicate analyses of four concentration calibration solutions,
including all Selected Ion Current Profiles, Calculated Response Factors, plotted
concentration calibration curves and computer generated quantitation reports.
4. Completed data reporting sheets (Forms B-l, B-2, B-3 and B-4) with appropriate
SICPs.
5. SICPs generated during each performance check solution analysis and each
concentration calibration solution analysis.
6. A chronological list of all analyses performed. If more than one GC/MS system is
used, a chronological list is required for each system.
D. Monthly Sample Status Report
The contract laboratory is required to provide the status of all samples received or in-
house during the calendar month. Required status information includes: samples
received, samples extracted, samples analyzed, and samples rerun. All samples must be
identified by appropriate EPA Sample, Case and Batch/Shipment numbers.
C-73
-------
E. Daily Sample Status Report
In response to verbal request from SMO or the PO, the contract laboratory must verbally
provide sample status information on a same-day basis. Should written confirmation be
requested, the laboratory must send daily sample status information in written form that
same day using first-class mail service.
F. GC/MS Taoes
The contract laboratory must store all raw GC/MS data on magnetic tape, in appropriate
manufacturer's format. This tape must include: samples, blanks, concentration
calibration solutions, and performance evaluation samples. The laboratory must maintain
a written reference/logbook of tape files to EPA sample number, calibration data,
standards and blanks.
G. Extracts and Unused Sample Volume
The contract laboratory must retain extracts, stored at 4°C, for 365 days after data
submission. Unused sample volume must also be retained, stored at ambient temperature,
for 365 days after data submission.
H. Complete Case File Purge
The complete case file purge includes all laboratory records received or generated for a
sample batch that have not been previously submitted to EPA as a deliverable. These
items include but are not limited to: sample tags, custody records, sample tracking
records, analysts logbook pages, bench sheets, chromatographic charts, computer printouts,
raw data summaries, instrument logbook pages, correspondence, and the document
inventory.
C-74
-------
RAS DIOXIN
DATA REPORTING FORMS
-------
Lab:
Case/Batch No:
Instrument ID:
FORM B-1S. TCDD SOIL DATA REPORT FORM
Report Date:
Column:
Page 1 of 2
EPA
Sample No.
Extr.
Date
Wet wt
ug/kg
Meas.
TCDD
MPC
GC/MS Analysis
Date
Time
Surr.
S/N Ratio
*
% REC(IS)
MB = Method Blank FB
N = Native TCDD Spike IS
D = Duplicate/Fortified Field Blank RR
PE = EMSL-LV Performance Evaluation Sample RS
MPC = Maximum Possible Concentration ND
*Note: Relative to 13C.9-l,2,3,4-TCDD
Field Blank
Internal Standard
Rerun
Recovery Standard
Not Detected
9/86
-------
Lab:
Case/Batch No:
Instrument ID:
FORM B-1S. TCDD SOIL DATA REPORT FORM
Report Date:
Column:
Page 2 of 2
EPA
Rel.
Response Ratios
Response (Area)
Sample
Number
320/
322
332/
334IS
3327
334RS
259
320
322
328
332IS
334IS
332RS
334RS
MB = Method Blank FB
N = Native TCDD Spike IS
D = Duplicate/Fortified Field Blank RR
PE = EMSL-LV Performance Evaluation Sample ND
MPC = Maximum Possible Concentration RS
Field Blank
Internal Standard
Rerun
Not Detected
Recovery Standard
9/86
-------
Lab:
Case/Batch No:
Instrument ID:
FORM B-1W. TCDD WATER DATA REPORT FORM
Report Date:
Column:
Page 1 of 2
EPA
Sample No.
Extr.
Date
volume
ng/L
Meas.
TCDD
MFC
GC/MS Analysis
Date
Time
Surr.
S/N Ratio
*
Z REC(IS)
MB =
N =
D =
PE =
MFC =
*Note:
Method Blank FB
Native TCDD Spike IS
Duplicate/Fortified Field Blank RR
EMSL-LV Performance Evaluation Sample RS
Maximum Possible Concentration ND
Relative to 13C12-1 ,2,3,4-TCDD
Field Blank
Internal Standard
Rerun
Recovery Standard
Not Detected
9/86
-------
Lab:
Case/Batch No:
Instrument ID:
FORM B-1W. TCDD WATER DATA REPORT FORM
Report Date:
Column:
Page 2 of 2
EPA
Rel.
Response Ratios
Response (Area)
Sample
Numbe r
320/
322
332/
334IS
3327
334 RS
259
320
322
328
332IS
334IS
332RS
334RS
MB = Method Blank FB
N = Native TCDD Spike IS
D = Duplicate/Fortified Field Blank RR
PE = EMSL-LV Performance Evaluation Sample ND
MFC = Maximum Possible Concentration RS
Field Blank
Internal Standard
Rerun
Not Detected
Recovery Standard
9/86
-------
A. TCDD REPORT FORM (Form B-l)
This form Is used for tabulating and reporting case results.
Complete the header information at the top of the page including instru-
ment ID, laboratory name, case/batch number, report date, and column used.
EPA sample number is tabulated along with date sample was extracted, and
weight (wet) extracted to the nearest tenth (0.1) of a gram or volume extracted
(water) to the nearest 10 milliliters.
Calculate the concentration of 2,3,7,3-TCDD using the formula:
Ax • QlS
cx =
Als . RRFn . W
Cx = 2,3,7,8-TCDD concentration in ug/kg or ug/L
Ax = the sum of integrated ion abundance detected for m/z 320
and 322
A£S = the sum of integrated ion abundances detected for m/z 332
and 334 (characteristic ions of 13C12~2,3,7,8-TCDD the
internal standard).
Qis = quantity (in ng) of 13C12-2,3,7,8-TCDD added to''the sample
before extraction
RRFn = calculated me
relative to
lean response factor for unlabeled 2,3,7,8-TCDD
13C,7-2,3,7,8-TCDD
W = The weight (in g) of soil/sediment extracted or volume of
water extracted (in mL)
Positive samples are quantitated with values >10.0 ug/kg or 100 ng/L
recorded to three (3) significant figures and those values <10.0 ug/kg or
100 ng/L reported to two (2) significant figures.
For samples in which unlabeled 2,3,7,8-TCDD was not detected calculate
the estimated maximum possible concentration, which is the concentration
required to produce a signal with a peak height of 2.5 times the backgrounc".
signal height.
Use the formula:
2.5 . IIX . Qis
MPC =
Hls . RRFn . W
where: MPC = maximum possible ccmcenlrat ion of unlabeled 2 , 3 , / , S-'l'O
required lo produce? llx.
-------
Hx = peak height for m/z 320 or 322 in the same group
of >5 scans used to measure Als.
His = peak height for the appropriate ion characteristic of the
internal standard, m/z 332 when 320 is used to determine Ax,
and m/z 334 when 322 is used to determine Ax.
Qls = quantity (in ng) of 13C12~2,3,7,8-TCDD added to the
sample before extraction.
RRFn = calculated mean response factor for unlabeled 2,3,7,8-TCDD
relative to 13C12~2,3,7,8-TCDD.
W = weight (in g) of wet soil/sediment sample or volume of water
extracted (in mL).
Report GC/MS Instrument ID, the date and time the analysis was performed,
and the signal to noise ratio for the surrogate compound.
-------
FORM B-2
INITIAL CALIBRATION SUMMARY
Page 1 of 2
Laboratory:
Case/Batch No.:
CC Solution Alternative:
Instrument ID:
AREA
Date
Time
Sol.
ID
CC1
CC1
CC1
CC2
CC2
CC2
CC3
CC3
CC3
CCA
CCA
CCA
320
322
328
*
t /
t /
/
/ t
/ t
332IS
33AIS
332RS
33ARS
Solution ID Codes;
CC1 «• Concentration calibration solution #1
CC2 = Concentration calibration solution #2
CC3 • Concentration calibration solution #3
CCA — Concentration calibration solution #A
* Not present in CC Solution
Alternative One.
9/86
-------
Laboratory:
Case/Batch No.:
FORM B-2
INITIAL CALIBRATION SUMMARY
CC Solution Alternative:
Instrument ID:
Page 2 of 2
Date
Time
Sol.
ID
CC1
CC1
CC1
CC2
CC2
CC2
CC3
CC3
CC3
CCA
CCA
CCA
Measured
RRFn
Mean
RRFn
Measured
RRFi
Mean
RRFi
Solution ID Codes:
CC1 = Concentration calibration solution tl
CC2 = Concentration calibration solution 92
CCS = Concentration calibration solution #3
CCA = Concentration calibration solution #A
ZRSD: RRFn
CC1=
C€2=
CC3=
CCA =
RRFt
Native Mean
of Means:
IS Mean
of Means:
9/86
-------
B. Initial Calibration Summary (Form B-2 )
Record all routine calibrations (PCS and CC1) performed during initial
calibration on form B-3.
Complete all header Information including laboratory, case/batch number,
and instrument ID and EPA CC Solution Alternative.
Date and time along with response for each ion is recorded for each cali-
bration solution. The response factors are calculated with the following
equations:
RRFn (native Response Factor) RRF^ (internal Standard Response Factor)
Ax • Q!S Ais
RRFn
Where:
Ais • Qn Ars
Ax = the sum of Integrated ion abundance of m/z 320 and 322 for unlabeled
2,3,7,8-TCDD
AJLS = the sura of integrated ion abundancces of m/z 332 and m/z 334 for
13C12-2,3,7,8-TCDD !
Ars = the sum of integrated ion abundance of ra/z 332 and m/z 334 for
13C12-1,2,3,4-TCDD
Qn = quantity of unlabeled 2,3,7,8-TCDD injected
Qls = quantity of 13C12~2,3,7,8-TCDD injected
Qrg = quantity of 13C12~1,2,3,4-TCDD
Calculate the mean RRF and the percent relative standard deviation for the
triplicate runs of each calibration solution.
SD
%RSD = -- x 100
X
-------
Where:
SD =
X = mean of each of the three Response Factors respectively
From the 4 mean native response factors and 4 mean Internal standard
response factors: calculate the mean of means for each respective RRF's.
-------
Laboratory:
Case/Batch No.
FORM B-3
ROUTINE CALIBRATION SUMMARY
CC Solution Alternative:
Instrument ID:
(PCS) PERFORMANCE CHECK SOL.
(CC1)
CON. CALIB. SOL. it I
Date
Time
Response
259
320
322
328
332IS
334IS
332RS
33ARS
Ratios
320/322
332/33AIS
332/334RS
RRFn
RRFt
7, Valley
9/86
-------
Routine Calibration Summary (Form B-3)
Complete the header Information Including the laboratory, instrument ID
Case/Batch number and EPA CC Solution Alternative.
For each performance check solution analyzed complete the date and time
of analysis, the response for m/z 259, 320, and 322 for unlabeled 2,3,7,8-
TCDD 328 for Cl^-2,3,7,8-TCDD, and 332 and 334 for C12~2,3,7,8-TCDD
and 13C12-1,2,3,4-TCDD.
Ion ratios for m/z 320/322, m/z 332/334 for l3C12-2,3,7,8-TCDD and m/z
332/334 for 13C12~1,2,3,4-TCDD are to be calculated and recorded.
Response factors are to be calculated as In the Initial Calibration Summary
(Section B).
For calculation of valley percent see Section D, Section 9.2.6.1.
For each Concentration Calibration Solution #1 used in Routine Calibration,
complete all the above information.
-------
FORM B-4
QUALITY CONTROL SUMMARY
Laboratory Name
Case/Batch No.
Instrument ID
Accuracy, Fortified/
Spike Field Blank:
Relative Difference (%),
Duplicate Analysis:
SOIL
EPA Sample Number:
EPA Sample Number:
WATER
Accuracy, Fortified/
Spike Field Blank:
Relative Difference (Z),
Duplicate Analysis:
EPA Sample Number:
EPA Sample Number:
9/86
-------
D. QC Summary
Complete all the header Information.
Report the sample number Cor the fortified field blank and the % accuracy
of the fortified/spike field blank by using the following equation:
amount measured
% accuracy = x 100
1.0
Record the sample used for duplicate and the Relative Percent Difference
which is calculated as follows:
|Sl - S2|
RPD = x 100
Si - S2
2
Where:
Sj and S2 represent sample and duplicate sample results.
-------
APPENDIX D
SAMPLE INFORMATION AND DOCUMENTATION
-------
ORGANIC SAMPLE COLLECTION
REQUIREMENTS
WATER SAMPLES
REQUIRED
VOLUME
CONTAINER TYPE
EXTRACTABLE ANALYSIS
(LOW LEVEL)
EXTRACTABLE ANALYSIS
(MEDIUM LEVEL*)
VOLATILE ANALYSIS
(LOW OR MEDIUM LEVEL')
1 GALLON
1 GALLON
80 ML
A
A
A
1 x 4-LITER AMBER
GLASS BOTTLES
OR
2 x 80 -O2. AMBER
GLASS BOTTLES
OR
4 x 1 -LITER AMBER
GLASS BOTTLES
4 x 32-OZ. WIDE-MOUTH
GLASS JARS
2 x 40-ML GLASS VIALS
SOIL/SEDIMENT SAMPLES
REQUIRED
VOLUME
CONTAINER TYPE
EXTRACTABLE ANALYSIS
(LOW OR MEDIUM LEVEL*)
6 OZ.
VOLATILE ANALYSIS
(LOW OR MEDIUM LEVEL*)
240 ML
1 x 8-OZ. WIDE-MOUTH
GLASS JAR
OR
2 x 4-OZ. WIDE-MOUTH
GLASS JARS
2 x 120-ML WIDE-MOUTH
GLASS VIALS
*ALL MEDIUM LEVEL SAMPLES TO BE SEALED IN METAL PAINT CAN FOR SHIPMENT
D-l
-------
INORGANIC SAMPLE COLLECTION
REQUIREMENTS
WATER SAMPLES
REQUIRED
VOLUME
CONTAINER TYPE
METALS ANALYSIS
(LOW LEVEL)
1 LITER
A
A
METALS ANALYSIS
(MEDIUM LEVEL*)
CYANIDE (CN~) ANALYSIS
(LOW LEVEL)
16 OZ.
1 LITER
CYANIDE (CN~) ANALYSIS
(MEDIUM LEVEL*)
16 OZ.
A
A
1 x 11-LITER
POLYETHYLENE BOTTLE
OR
2 x BOO ML
POLYETHYLENE BOTTLE
1 x 16-OZ. WIDE-MOUTH
GLASS JAR
1 x 11-LITER
POLYETHYLENE BOTTLE
-OR
2 x 500 ML
POLYETHYLENE BOTTLE
1 x 16-OZ. WIDE-MOUTH
GLASS JAR
SOIL/SEDIMENT SAMPLES
REQUIRED
VOLUME
CONTAINER TYPE
METALS AND CYANIDE (CN~)
ANALYSIS
(LOW OR MEDIUM LEVEL")
6 OZ.
1 x 8-OZ. WIDE-MOUTH
GLASS JAR
OR
2 x 4 OZ. WIDE-MOUTH
GLASS JARS
"ALL MEDIUM LEVEL SAMPLES TO BE SEALED IN METAL PAINT CAN FOR SHIPMENT
D-2
-------
DIOXIN SAMPLE COLLECTION
REQUIREMENTS
WATER
REQUIRED
SAMPLES VOLUME
2.3.7.8-TCDD (S C
ANALYSIS 2 LITERS
(MULTI- CONCENTRATION) (^ j
REQUIRED
SOIL/SEDIMENT SAMPLES VOLUME
2.3.7.
8-TCDD 4 OZ. H
ANALYSIS ^
CONTAINER TYPE
*x
2 x 1- LITER AMBER
GLASS BOTTLES
s
CONTAINER TYPE
1 x 4-OZ. WIDE-MOUTH
GLASS JAR
(MULTI -CONCENTRATION)
D
OR
1 x 8-OZ. WIDE-MOUTH
GLASS JAR
HIGH HAZARD SAMPLE COLLECTION
REQUIREMENTS
REQUIRED
LIQUID OR SOLID SAMPLES VOLUME
CONTAINER TYPE
ORGANIC AND INORGANIC
ANALYSIS
6 OZ.
|
1 x 8-OZ. WIDE-MOUTH
GLASS JAR
•ALL MEDIUM LEVEL SAMPLES TO BE SEALED IN METAL PAINT CAN FOR SHIPMENT
A
X
D-3
-------
ILS. ENVIRONMENTAL PROTECTION AGENCY r. - .. .
CLP Sample Management Office >>A:> NumDer
P.O. Box SIS - Alexandria, Virginia 22313
Phone: 703/557-2*90 - FTS/557-2*90
SPECIAL ANALYTICAL SERVICES
Client Request
D
Regional Transmittal | Telephone Request
A. EPA Region/Client:
B. RSCC Representative:
C. Telephone Number: ( )
D. Date of Request:
E. Site Name:
Please provide below description of your request for Special Analytical Services under
the Contract Laboratory Program. In order to most efficiently obtain laboratory
capability for your request, please address the following considerations, if applicable.
Incomplete or erroneous information may result in a delay in the processing of your
request. Please continue response on additional sheets, or attach supplementary
information as needed.
1. General description of analytical service requested:
Definition and number of work units involved (specify whether whole samples or
fractions; whether organics or inorganics; whether aqueous or soil and sediments;
and whether low, medium or high concentration):
3. Purpose of analysis (specify whether Superfund (enforcement or remedial action),
RCRA, NPDES, etc.):
D-4
-------
Estimated date(s) of collection:
5. Estimated date(s) and method of shipment:
6. Number of days analysis and data required after laboratory receipt of samples:
7. Analytical protocol required (attach copy if other than a protocol currently used in
this program): "
8. Special technical instructions (if outside protocol requirements, specify compound
names, CAS numbers, detection limits, etc.):
9. Analytical results required (if known, specify format for data sheets, QA/QC
reports, Chain-of-Custody documentation, etc.) If not completed, format of results
will be left to program discretion.
10. Other (use additional sheets or attach supplementary information, as needed):
11. Name of sampling/shipping contact:
Phone: ( )
D-5
-------
12. Data Requirements
Precision Desired
Parameter Detection Limit (-% or Concentration)
13. QC Requirements
Limits
Audits Required Frequency oi Audits (Percent or Concentration)
. Action Required if Limits are Exceeded
Please return this request to the Sample Management Office as soon as possible to
.expedite processing of your request- for special analytical services. Should you have any
questions or need any assistance, please contact your Regional representative at the
Sample Management Office.
D-6
-------
SAMPLE DOCUMENTATION
-------
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Si
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D-9
-------
D-10
-------
SAS Na Of appli
nOIXjaniC TraffJC ReDOlt
is. &
.1 |:
a. >:
imen
S
<* £pp^il
1 OT
-------
EM
D-12
-------
USEPA Contract Laboratory Program
Sample Management Office
P.O. Box 816 Alexandria. Virginia 22313
FTS 8-557-2490 703/557-2490
CASE NO:
IT RECORD
BATCH NO:
SAS NO:
(rt applicable)
Type of Activity (circle one) 0
Superfund -- PA SI ESI Rl RO RA ER
NPLO O4M OTHER
Non-Superfund -- Proaram
Site Name:
@
City. State
Site Spill ID:
Sampling Date:.
Region Number:
Sampling Contact:
©
(name)
(company)
Carrier:
Airbill No:_
®
Ship To.
ATTN
Date Shipped:
Sampler Instructions: 1) Ship all samples in paint cans, with sample labels affixed to outside of can.
2) Use TCE or hexane organic solvents for rinsate samples.
3) Sample Volumes Required: Soil or Sediment: 4 oz. per sample in glass jar. Aqueous. 2 Liters per sample in
amber glass. Send one 4 Liter sample per Batch of aqueous samples for lab QC.
4) "Sample to spike' win be analyzed at Lab as a spiked sample only. If this sample requires analysis prior to spiking,
the sampler must supply a separate sample labelled with a unique sample number.
MATRIX (check one/sample)
DESCRIPTION
SAS ONLY
CLP
SAMPLE
NUMBERS
(from labels)
SOIL OR ®
SEDIMENT
AQUEOUS®
^>
^
l8Q ||
WHITE V.1O Cliii
YELLOW rii.'M! ' n|iv
PINK
noi o
D-13
-------
USEPA Contract Laboratory Program
Sample Management Office
P.O. Box 818 Alexandria. Virginia 22313
FTS 8-557-2490 703/557-2490
| CASE NO: 3QOO
IT RECORD
BATCH NO: 03
SAS NO: .i*
(« (pplictfito) M |«
Type ol Activity (circle onej_ ©
Superlund PA SI ESID RA ER
NPLD O4MDTHEH
Non-Supertund Program
Region Number
Sampling Contact:
Sampler Instructions: 1) Ship an samples in paint cans, with sample labels affixed to outside of can.
2) Use TCE or hexane organic solvents for rinsate samples.
3) Sample Volumes Required: Soil or Sediment: 4 oz. per sample In glass jar. Aqueous: 2 Liters per sample in
amber glass. Send one 4 Liter sample per Batch of aqueous samples for lab OC.
4) "Sample to spike" will be analyzed at Lab as a soiled sample only. If this sample requires analysis prior to spiking
the sampler must supply a separate sample labeled with a unique sample number.
MATRIX (check one/sample)
WHITE V.1O '.u|i/ YELLOW C, : <.n\i, PINK I .ih (,.,py LI. H.-Imn 1- • ' ,tf.< I
GOI I) I if
D-14
-------
U.S. ENVIRONMENTAL PROTECTION AGENCY
CLP Sample Management Office
P.O. Box 818 - Alexandria, Virginia 22313
Phone: 703/557-2490 - FTS/557-2490
SAS Number
SPECIAL ANALYTICAL SERVICE
PACKING LIST
Sampling Office:
Sampling Contact:
(name)
(phone)
Sampling Date(s):
Date Shipped:
Site Name/Code:
Ship To:
Attn:
For Lab Use Only
,Date Samples Rec'd:
Received By:
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
Sample
Numbers
Sample Description
i.e., Analysis, Matrix, Concentration
Sample Condition on
Receipt at Lab
For Lab Use Only
White - SMO Copy, Yellow - Region Copy, Pink - Lab Copy for return to SMO, Gold - Lab Copy
D-15
-------
M.S. ENVIRONMENTAL PROTECTION AGENCY
C.LP Sample Management Office
P.O. Box 818 - Alexandria, Virginia 22313
Phone: 703/557-2490 - FTS/557-2490
3AS Number
1000- A
SPECIAL ANALYTICAL SERVICE
PACKING LIST
Sampling Office:
?i?aio/\ t-
J
Sampling Contact:
Jot. Soynplev
(name)
i/n|6£S-rt&«4
(phone)
Sampling C
lljfc'H
Date Shipp
U|4
)ate(s):
4l<&
>ed:
1<
05
Site Name/Code:
-*oi
Ship To:
SAS LA6
100 Mod/\ S4rt
IOOOA -0«i
IOOOA - o£
IOOOA - OU
Sample Description
i.e., Analysis, Matrix, Concentration
Sample Condition on
Receipt at Lab
For Lab Use Only
White - SMO Copy, Yellow - Region Copy, Pink - Lab Copy for return to SMO, Gold - Lab Copy
D-16
-------
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322
Custody Seal
CUSTODY SEAL
<£
I Date
Code
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Station Not
Month/Day/YMT
Station Location
//
Tim*
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Designate
Com p.
Grab
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BOD Anions
SolidS (TSS) (TDS) (SS
YSES
Prese
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tive: .
No 5K
*
o
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s>EPA
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UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
Sample Tag
D-17
-------
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D-19
-------
SAMPLE PACKAGING AND SHIPMENT
-------
SAMPLE PACKAGING SUMMARY
SAMPLE
• ENCLOSE ALL SAMPLE CONTAINERS IN CLEAR
PLASTIC BAGS.
• PACK ALL MEDIUM AND HIGH LEVEL WATER AND
SOIL SAMPLES IN METAL PAINT CANS.
• LABEL PAINT CANS WITH SAMPLE NUMBER OF
SAMPLE CONTAINED INSIDE.
• SURROUND CONTENTS OF CAN WITH NON-
COMBUSTIBLE. ABSORBENT PACKING MATERIAL.
• USING FREEZER PACKAGES OR ICE SEALED IN PLASTIC
BAGS, COOL ORGANIC LOW OR MEDIUM SAMPLES
AND INORGANIC SAMPLES TO BE ANALYZED FOR
CYANIDE TO 4°C.
• ICE IS NOT REQUIRED IN SHIPPING LOW LEVEL SOIL
SAMPLES, BUT MAY BE UTILIZED AT THE
DISCRETION OF THE SAMPLER.
• DO NOT COOL DIOXIN. INORGANIC LOW LEVEL
WATER, INORGANIC MEDIUM/HIGH LEVEL WATER OR
SOIL. OR ORGANIC HIGH LEVEL WATER OR SOIL
SAMPLES.
• PACK SEALED PAINT CANS OR PLASTIC-ENCLOSED
SAMPLE BOTTLES IN SHIPMENT CONTAINER.
• USE A METAL ICE CHEST FOR SHIPMENT (DO NOT
USE CARDBOARD OR STYROFOAM CONTAINERS TO
SHIP SAMPLES).
• SURROUND CONTENTS WITH NON-COMBUSTIBLE,
ABSORBENT PACKING MATERIAL (DO NOT USE
EARTH OR ICE PACKING MATERIALS).
• TAPE PAPERWORK IN PLASTIC BAGS UNDER COOLER
LID.
• CLOSE COOLER AND SEAL WITH CUSTODY SEALS.
D-23
-------
SAMPLE SHIPMENT
COORDINATION CHECKLIST
IMMEDIATELY UPON SHIPMENT OF SAMPLES, SAMPLERS
CALL SMO AT (703/557-2490), WITH THE FOLLOWING
INFORMATION:
O PHONE
"OVERNITE'
EXPRESS
OFFICE
• CASE AND/OR SAS NUMBER
• NAME OF LABORATORY
• DATE OF SHIPMENT
• CARRIER, AIRBILL (SHIPMENT)
NUMBERS AND TYPE OF SERVICE
• NUMBER AND MATRICES
(WATERS, SOILS, ETC.) OF
SAMPLES SHIPPED
• INFORMATION ON COMPLETIONS,
CHANGES, DELAYS,
CONTINUATIONS, ETC.,
PERTINENT TO THE CASE
• SAMPLER'S NAME, REGION, AND
PHONE NUMBER
• SMO MUST BE NOTIFIED BY
3:00 PM ON FRIDAY FOR
SAMPLES INTENDED FOR
SATURDAY DELIVERY/PICKUP
D-24
-------
POTENTIAL PROBLEMS
WITH SAMPLE SHIPMENT AND ANALYSIS
o INCORRECT OR INCOMPLETE PAPERWORK
o LABORATORY RECEIPT OF INCORRECT SAMPLES
o INSUFFICIENT VOLUME FOR ANALYSIS REQUESTED
o BROKEN OR LEAKING SAMPLES
o MATRICES OTHER THAN WATER OR SOIL
(I.E., ROCKS, LEAVES, STICKS, OIL, ETC.)
o NON-HOMOGENEOUS/MULTI-PHASE
WATER OR SOIL SAMPLES
o ANALYTICAL PROBLEMS WITH SAMPLES
o LABORATORY ACCIDENTS INVOLVING SAMPLES
IF ANY OF THESE PROBLEMS ARE ENCOUNTERED,
CONTACT SMO IMMEDIATELY
D-25
-------
In Reference to Case No(s):
Contract Laboratory Program
REGIONAL/LABORATORY COMMUNICATION SYSTEM
Telephone Record Log
Date of Call:
Laboratory Name:
Lab Contact:
Region:
Regional Contact:
Call Initiated By: Laboratory Region
In reference to data for the following sample number(s):
Summary of Questions/Issues Discussed:
Summary of Resolution:
Signature Date
Distribution: (1) Lab Copy, (2) Region Copy, (3) SMO Copy
D-26
-------
APPENDIX E
AUXILIARY SUPPORT SERVICES DOCUMENTATION
-------
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E-2
-------
CASE FILE PURGE MATERIALS
INCLUDE, BUT ARE NOT LIMITED TO:
SAMPLE TAGS
CHAIN-OF-CUSTODY RECORDS
COPIES OF SAMPLE TRACKING RECORDS
ANALYSTS' LOGBOOK PAGES
INSTRUMENT LOGBOOK PAGES
(INCLUDING INSTRUMENT CONDITIONS)
BENCH SHEETS
INSTRUMENT READOUT RECORDS
COMPUTER PRINTOUTS
CHROMATOGRAPHIC CHARTS
RAW DATA SUMMARIES
CORRESPONDENCE MEMOS
DOCUMENT INVENTORY
E-3
-------
COST RECOVERY DOCUMENTATION CHECKLIST
DATE: OF CHECKLIST:
RECEIVED IN HQ
COSTS THRU; MONTH YEAR
REOUIRED DATE FDR REGION
1. SITE NAME: CITY/COUNTY STATE
SITE ID NUMBER: NPL YES NO
(OTHER NAMES USED FOR THIS SITE):
2. STATUS: CHECK ONE:
TRIAL DATE (DATE: ) IN PREPARATION IN REGION FDR
IN DISCOVERY (DEADLINE: ) STATUTE OF LIMITATIONS
FILED PROJECTED/ON GOING NEGOTIATIONS
REFERRED TO DOJ DEMAND LETTER TO BE SENT
REFERRED TO HEADQUARTERS ON SCAP
BANKRUPTCY
3. NAME AND TELEPHONE NUMBER OF OSC/REGIONAL CONTACT:
4. NAME AND TELEPHONE NUMBER OF REGIONAL COUNSEL CONTACT:
5. WHICH, IF ANY, OF THE FOLLOWING FIT CONTRACTORS WERE USED?
A. E&E (CONTRACT NO. ) DATES OF WORK
B. NUS (CONTRACT NO. ) DATES OF WORK
C. CH2M Hil1 SUBCONTRACTOR E&E, (CONTRACT NO. ) (ZONE II)
DATES OF WORK
LIST ALL KNOWN TDDs:
6. WHICH IF ANY OF THE FOLLOWING TAT CONTRACTORS WERE USED?
A. E&E (CONTRACT NO. ) DATES OF WORK
B. ROY F. WES1DN (CONTRACT NO. ) DATES OF WORK
LIST ALL KNOWN TDDs:
7. WAS WORK DONE THROUGH THE CONTRACT LAB PROGRAM (VIAR)? YES NO
A. CONTRACT NO. YES NO
B. CONTRACT NO. YES NO
C. CONTRACT NO. YES NO
IF YES, PLEASE PROVIDE ANY SPECIAL ANALYTICAL SERVICES (SAS) CASE NUMBERS:
E-4
-------
POST RECOVERY DOCUMENTATION CHECKLIST, PAGE 2
WAS LAB WORK OTHER THAN THROUGH VIAR USED? YES NO
IF YES, PLEASE GIVE LAB NAME AND CONTRACT NUMBER:
8. WHICH IF ANY OF THE FOLLOWING REM CONTRACTORS WERE USED?
(DESCRIBE TASKS WITH THE FOLLOWING: RAMP, IWI, RI/FS, DESIGN
CONSTRUCTION, COMMUNITY RELATIONS, ENFORCEMENT, OR OTHER)
A. BLACK & VEATCH (CONTRACT NO: )
DATES OF WORK TASK
B. CAMP DRESSER & MCKEE (COM) (CONTRACT NO. )
DATES OF WORK TASK
C. ROY F. WESTON (CONTRACT NO. )
DATES OF WORK TASK
D. NUS (ZONE I, CONTRACT NO. ) _
DATES OF WORK TASK
E. CH2M HILL (ZONE II, CONTRACT NO. (
DATES OF WORK TASK
F. CAMP DRESSER MCKEE (REM II CONTRACT NO.
DATES OF WORK TASK
G. EBASCO (REM III CONTRACT NO. )
DATES OF WORK TASK
H. CH2M Hill ( REM IV CONTRACT NO.
DATES OF WORK TASK
9. PLEASE PROVIDE THE FOLLOWING INFORMATION ABOUT CONTRACTORS
LET BY AN OSC OR EMERGENCY REMOVAL CLEANUP (ERCS) CONTRACT:
CONTRACTOR:
CONTRACT NO. DELIVERY ORDER No.
DATES OF WORK:
10. WAS WORK DONE BY EMERGENCY RESPONSE TEAM (EDISON LAB) YES NO
PAYROLL & TRAVEL COSTS ONLY
DATES OF VvORK:
E-5
-------
POST RECOVERY DOCUMENTATION CHECKLIST, PAGE 3
11. WAS HDRK DONE THROUGH EERU CONTRACT WITH IT CORP?
A. Mason S, Hanger (CONTRACT NO. ) YES NO
B. IT CORP. (CONTRACT NO. ) YES NO
C. (F.W.) Enviresponse Inc.(CONTRACT NO. •} YES NO
DATES OF WORK:
12. WERE ANY OVERFLIGHTS DONE? YES NO
DATES OF OVERFLIGHTS:
13. VftS WORK DONE BY NEIC? YES NO
DATES OF WORK TASK
14. WAS AN EVIDENCE AUDIT OR OTHER WORK DONE THROUGH NEIC CONTRACT?
A. With Intera (CONTRACT NO. ) YES NO
B. WITH TECH LAW (CONTRACT NO. ) YES NO
C. WITH TECH LAW (CONTRACT NO. ) YES NO
DATES OF WORK
D. FRED C. HART (CONTRACT NO. ) or CONTRACT NO.(
15. WAS ANY WORK DONE UNDER THE TES I CONTRACT? YES NO
A. CONTRACT NO. (PRIME CONTRACTOR: GCA)
DATES OF WORK: TASKS PERFORMED:
B. WAS ANY WORK DONE UNDER THE TES II CONTRACT? YES NO
CONTRACT NO. (PRIME CONTRACTOR: PRC)
DATES OF WORK: TASKS PERFORMED:
C. WAS ANY WORK DONE UNDER TES III CONTRACr?
CONTRACT NO. (PRIME CONTRACTOR: COM)
DATES OF WORK: TASKS PERFORMED:
16. WAS ANY WORK DONE UNDER THE PRE-TES CONTRACT? YES NO
A. LIFE SYSTEMS (CONTRACT NO. ) YES NO
B. A.T. KEARNEY (CONTRACT NO. ) YES NO
DATES OF WORK:
NAME ANY OTHER CONTRACTOR USED:
CONTRACT NO. DATES OF WORK:
E-6
-------
COST RECOVERY DOCUMENTATION CHECKLIST, PAGE 4
17. PLEASE PROVIDE TOE FOLLOWING INFORMATION ABOUT OTHER FEDERAL AGENCIES THAT WORKED
ON THE SITE:
AGENCY IAG * DATES OF WORK CONTACT PERSON/TELEPHONE
HHS
ODE
USCG
FEMA
DOJ
DOI
NOAA
USGS
BRIEF DESCRIPTION OF WORK:
18. WAS THERE A STATE COOPERATIVE AGREEMENT OR CONTRACT? YES NO
STATE: COOPERATIVE AGREEMENT #
CONTRACT No.
19. WERE ANY OTHER CONTRACTORS (e.g., R&D CONTRACTS) USED? IF SO, PLEASE PROVIDE THE
FOLLOWING:
CONTRACTOR:
CONTRACT No:
DATES OF WORK:
BRIEF DESCRIPTION OF WORK:
E-7
-------
COST RECOVERY DOCUMENTATION CHECKLIST, PAGE 5
20. WERE ANY REGIONAL COUNSEL APPROPRIATIONS TOR LEGAL EXPENSES
USED? YES NO
21 PLEASE LIST THE REGIONAL OFFICES WHICH HAVE BEEN INVOLVED IN THE CASE:
22. ANY OTHER PERTINENT INFORMATION NOT PROVIDED ABOVE:
E-8
-------
MEMORANDUM
DATE:
TO: Data Review Team
Sample Management Office
FROM:
USEPA Region
SUBJECT: Data Review Request
COPIES:
Please review the data from the following SMO Case:
SMO Case No.:
Site Name:
Lab Name(s):
I. Sample Information:
A. Number of Samples in Case:
B. Number of Samples to be Reviewed:
(List Numbers if Not All)
C. Organics to be Reviewed? Yes No_
D. Inorganics to be Reviewed? Yes No_
E-9
-------
II. User Information:
A. User Organization: _
B. Contact for Questions:
Name:
C.
Telephone:
Type(s) of Review Requested:
Check All
That Apply
QA/QC Compliance
Problem Case
Applications
Consulting
Other
Specify:
D. Additional Issues to Address in Review:
Date
Needed
E. Intended Use of Data:
Check All
That Apply
Enforcement
Preliminary Assessment
Site Investigation
Remedial Action
Site Monitoring
Undetermined
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Specify:
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APPENDIX F
REFERENCES
NOTE: The references in this appendix are supplied for general information purposes and
do not necessarily represent methods or procedures utilized in the CLP.
-------
ANALYTICAL REFERENCES
American Public Health Association, American Water Works Association, Water Pollution
Control Federation. Standard Methods for Examination 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 Spectrometric
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. Analy. 2; 1970 (p. 317).
Hatch, W.R.; Ott, W.L. Determination of Sub-Microgram Quantities of Mercury by Atomic
Absorption Spectrophotometry. Analytical Chemistry 40:2085; 1968.
Kopp, J.F.; Longbottom, M.C.; Lobring, L.B. Cold Vapor Method for Determining Mercury.
AWWA 64:20; January 1972.
Martin, T.D.; Kopp, J.F.; Ediger, R.D. 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 CLP 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.
Organochlorine Pesticides and PCBs, Method 608; 2,3,7,8-TCDD, Method 613; Purgeables
(Volatiles), Method 624; Base/Neutrals, Acids 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.
F-l
-------
Technicon Industrial Systems. Operation Manual for Technicon Auto Analyzer IIC System.
Technical Pub. No. TA9-0460-00. Tarry town, New York: 1980.
U.S. Environmental Protection Agency. Handbook for Analytical Quality Control in Water and
Wastewater Laboratories. USEPA-600/4-79-019.
U.S. Environmental Protection Agency. Handbook for Monitoring Industrial Wastewater.
USEPA Technology Transfer; 1973.
U.S. Environmental Protection Agency. Methods for Chemical Analysis of Water and
Wastewater. USEPA Technology Transfer; 1974.
U.S. Environmental Protection Agency. Methods from Chemical Analysis of Water and Waste.
USEPA-600/4-79-02; March 1979.
U.S. 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 Lines. USEPA-600/4-79-017,
Wise, R.H.; Bishop, D.F.; Williams, R.T.; Austern, B.M. Gel Permeation Chromatography in
the GC/MS Analysis of Organics in Sludges. Municipal Environmental Research
Laboratory, U.S. Environmental Protection Agency. Cincinnati.
QUALITY ASSURANCE 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 52(14); December 1980.
Environmental Monitoring Systems Laboratory, U.S. Environmental Protection Agency.
Analytical Reference Standards and Supplemental Data: The Pesticides and Industrial
Chemicals Repository. EPA-600/4-84-082; October 1984.
Fisk, J.F.; Manzo, S.M. Quality Assurance/Quality Control in Organics Analysis. Proceedings
from the Water Pollution Control Federation Meeting; May 1986.
Health Effects Research Laboratory, U.S. 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, U.S. Environmental Protection Agency. Manual of
Analytical Quality Control for Pesticides and Related Compounds In Human and
Environmental Samples-Second Revision. EPA-600/2-81-059; April 1981.
F-2
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Laidlaw, R.H. 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 STP 925. C.L. Perket, ed.,
American Society for Testing and Materials. Philadelphia: 1986.
Moore, J.M.; 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. C.L. Perket, ed., American Society for
Testing and Materials. Philadelphia: 1986.
Office of Monitoring Systems and Quality Assurance, U.S. 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. SW-846, 3d ed.; November 1986.
U.S. Environmental Protection Agency. Guidelines Establishing Test Procedures for the
Analysis of Pollutants Under the Clean 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. January 1976.
Wallace, R.A.; 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, U.S. Environmental Protection Agency. Field Monitoring and
Analysis of Hazardous Materials. EPA Training Manual. Course No. 165.4. Cincinnati:
1980.
Huibregtse, K.R.; Moser, J.H. Handbook for Sampling and Sample Preservation of Water and
Wastewater. USEPA-600/4-76-049; 1976.
F-3
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Municipal Environmental Research Laboratory, U.S. 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.
Olson, D.M.; Berg, E.L.; Christensen, R.; Otto, H.; Ciancia, J.; Bryant, G.; Lair, M.D.; Birch,
M.; Keffer, W.; Dahl, T.; Wehner, T. Compliance Sampling Manual. Office of Water
Enforcement, EPA Enforcement Division, Compliance Branch; 1977.
Weber, C.I. Biological Field and Laboratory Methods for Measuring the Quality of Surface
Waters and Effluents. USEPA-670/4-73-001; 1973.
SHIPPING REFERENCES
Federal Express Corporation, Hazardous Materials Department. Telephone: 1-800-238-5592.
U.S. Department of Transportation. A Guide to the Federal Hazardous Materials
Transportation Regulatory Program; 1983.
U.S. Department of Transportation. U.S. Department of Transportation Regulations. 49 CFR,
Parts 100-199; October 1, 1978.
F-4
•fcll.S. GOVERNMENT PUNTING OFFICE: MM - 74S-1W/MMI
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