United States	Office of Research and
Environmental Protection	Development	August 2000
Agency	Washington, D.C. 20460
<&EPA Environmental Technology
Verification Program
Verification Test Plan
Evaluation of Field Polychlorinated
Biphenyl (PCB) Detection
Technologies
Oak Ridge National Laboratory
ElVEiVetV

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August 2000
Environmental Technology
Verification Program
Verification Test Plan
Evaluation of Field Polychlorinated
Biphenyl (PCB) Detection Technologies
By
Oak Ridge National Laboratory
Oak Ridge, Tennessee 37831-6120
and
U.S. Environmental Protection Agency
Environmental Sciences Division
National Exposure Research Laboratory
Las Vegas, Nevada 89193-3478

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APPROVAL SIGNATURES
This document is intended to ensure that all aspects of the verification are documented, scientifically sound, and
that operational procedures are conducted within quality assurance/quality control specifications and health and
safety regulations.
The signatures of the individuals below indicate concurrence with, and agreement to operate compliance with,
procedures specified in this document.
U. S. ENVIRONMENTAL PROTECTION AGENCY
Project Manager: 	
Eric Koglin
ESD Quality Manager: 	
George Brilis
OAK RIDGE NATIONAL LABORATORY
Program Manager: 	
Roger Jenkins
Technical Lead:		
Amy Dindal
QA Specialist:		
Janet Wagner
Statistician:		
Charles Bayne
U. S. DEPARTMENT OF ENERGY, Oak Ridge Operations Office
Program Manager: 			
Regina Chung	Date
Date
Date
Date
Date
Date
Date
i

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SITE APPROVAL
ES&H Coordinator:
Dexsil Corporation:
Hybrizyme:
Fred Smith
TECHNOLOGY VENDORS
Ted Lynn
Randy Allen
ii

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TABLE OF CONTENTS
LIST OF FIGURES 	 vi
LIST OF TABLES 	vii
EXECUTIVE SUMMARY	viii
ABBREVIATIONS AND ACRONYMS	 ix
1	INTRODUCTION	1
1.1	Verification Objectives	1
1.2	What is the Environmental Technology Verification Program? 	1
1.3	Technology Verification Process	2
1.3.1	Needs Identification and Technology Selection	2
1.3.2	Verification Planning and Implementation 	2
1.3.3	Report Preparation	3
1.3.4	Information Distribution	3
1.4	Purpose of this Verification Test Plan	3
2	VERIFICATION RESPONSIBILITIES AND COMMUNICATION 	3
2.1	Verification Organization and Participants	4
2.2	Organization	5
2.3	Responsibilities	5
3	TECHNOLOGY DESCRIPTIONS 	6
3.1	Dexsil Corporation's L2000DX Analyzer	6
3.1.1	General Technology Description	6
3.1.2	Transformer Oil Sample Preparation	6
3.1.3	Instrument Calibration 	6
3.1.4	Sample Analysis	7
3.2	Hybrizyme'sDELFIAPCB Assay	7
3.2.1	General Technology Description	7
3.2.2	Sensitivity	7
3.2.3	Cross-Reactivity 	7
3.2.4	Quantitative Assay Procedure	7
4.1 Soil Sample Descriptions 	9
4.1.1	Environmentally-Contaminated Samples	9
4.1.2	Performance Evaluation (PE) and Blank Samples	10
5 SAMPLE COLLECTION AND PREPARATION	12
5.1 Soil Sample Collection	12
5.1.1	Sample Collection Procedures	12
5.1.2	Preliminary Soil Characterization	12
in

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5.1.3	Sample Preparation for Verification Test	13
5.1.4	Sample Stability Study	13
5.2	Extract Samples	14
5.3	Oil Samples 	14
5.3.1 Sample Collection	14
6	REFERENCE LABORATORY ANALYSES 	14
6.1	Methods Selection	15
6.2	Reference Laboratory Selection	15
6.2.1	Analysis of PCB Soils - LAS Laboratories	15
6.2.2	Analysis of PCB Oils - United Power Services Inc	16
7	VERIFICATION TEST DESIGN	16
7.1	Pre-Demonstration Study	16
7.2	Objective of the Verification Test	17
7.3. Summary of Verification Activities 	17
7.3.1	Environmental Conditions for the Test	21
7.4	Sample Distribution	21
7.5	Archive Samples 	21
7.6	Submission of Results	21
7.7	Verification Performance Factors	21
8	QUALITY ASSURANCE PROJECT PLAN (QAPP) 	22
8.1	Purpose and Scope 	22
8.2	Quality Assurance Responsibilities 	22
8.3	Field Operations 	22
8.3.2	Communication and Documentation	22
8.4	Performance and System Audits	22
8.4.1	Technical Systems Audit	23
8.4.2	Data quality audit of the reference laboratory 	23
8.4.3	Surveillance of Technology Performance	23
8.5	Quality Assurance Reports	23
8.5.1	Status Reports	23
8.5.2	Audit Reports 	23
8.6	Corrective Actions	23
8.7	Reference Laboratory Quality Control Checks	23
8.8	Data Management 	24
8.9	Data Reporting, Validation, and Analysis 	24
8.9.1	Data Reporting	24
8.9.2	Data Validation	24
8.9.2.1	Completeness of Laboratory Records	24
8.9.2.2	Holding Times	25
8.9.2.3	Correctness of Data	25
8.9.2.4	Correlation Between Replicates	25
8.9.2.5	Evaluation of QC Results	25
iv

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8.9.2.6 Evaluation of Spiked Sample Data	25
8.9.3 Data Analysis	25
8.9.3.1	Precision	25
8.9.3.2	Accuracy	26
8.9.3.3	False Positive/False Negative Results	27
8.9.3.4	Comparability 	27
8.9.3.5	Completeness 	28
9 HEALTH AND SAFETY PLAN 	28
9.1	Contact Information	28
9.2	Health and Safety Plan Enforcement	28
9.3	Site Access 	28
9.4	Waste Generation 	29
9.5	Hazard Evaluation	29
9.6	Personal Protection	29
9.7	Physical Hazards	29
9.8	Fire	30
9.9	Mechanical, Electrical, Noise Hazards 	30
9.10	Unstable/Uneven Terrain 	30
9.11	Inclement Weather	30
9.12	Heat Stress 	30
9.13	Insect and Other Animal Stings and Bites	31
9.14	Medical Support 	31
9.15	Environmental Surveillance	31
9.16	Safe Work Practices 	31
9.17	Complaints 	31
9.18	Radiological Hazards	31
REFERENCES	32
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LIST OF FIGURES
2-1.	Organization chart for the verification test	5
3-1.	Hybriyzme'sDELFIAPCB Assay	7
5-1. K-25 personnel collect a PCB sample from a 55-gallon drum	12
5-2.	K-25 sampling personnel sift through the collected soil to remove rocks and other large debris. . . 12
5-3. Transformer yard at ORNL	14
5-4.	Transformers at ORNL containing oils with PCB concentrations greater than 50 ppm	14
vi

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LIST OF TABLES
2-1.	Verification Participants in PCB Field Analytical Technology Verification Test	
3-1.	Summary of DELFIA PCB Assay's Cross-Reactivity	
3-2.	Chart for well use 	
4-1.	Summary of Environmentally-Contaminated Soil Sample Descriptions	1
7-1.	Summary of Environmental Soil Sample Analyses ( by Drum Number)
7-2.	Summary of Performance Evaluation Soil Samples	
7-3.	Summary of Extract Sample Analyses 	
7-4.	Summary of Oil Sample Analyses	
7-5.	Summary of Oil PE Samples 	
7-6.	Summary of Verification Analyses 	
vii

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EXECUTIVE SUMMARY
EPA created the Environmental Technology Verification (ETV) Program to facilitate the
deployment of innovative technologies through performance verification and information dissemination. The
goal of the ETV Program is to further environmental protection by substantially accelerating the acceptance
and use of improved and cost-effective technologies. The ETV Program is intended to assist and inform
those involved in the design, distribution, permitting, and purchase of environmental technologies. The
verification study described in this test plan will be conducted by the Site Characterization and Monitoring
Technologies Pilot (SCMT), one of 12 pilots of the ETV program. The SCMT pilot is administered by the
EPA's National Exposure Research Laboratory in Las Vegas, Nevada. The Oak Ridge National
Laboratory (ORNL) will serve as the verification organization for the test.
This test plan has been developed to describe the verification of two PCB field analytical
technologies: Dexsil Corporation's L2000DX and Hybrizyme's DELFIA PCB assay. The purpose of this
verification is to obtain performance information regarding the PCB field analytical technology, to compare
the results to conventional fixed-laboratory results, and to provide supplemental information (e.g., cost,
sample throughput, and training requirements) regarding the operation of the technology. The vendor will
have a choice of analyzing PCB-contaminated soils (208 samples), methanol extracts (24 samples), and/or
transformer oils (152 samples). Each matrix will include blanks, spikes, and environmentally-contaminated
samples. The verification of soil and extracts will be conducted under two climatic conditions. One set of
activities will be conducted outdoors, with naturally fluctuating temperatures and relative humidity
conditions. A second set will be conducted in a controlled environmental facility, with lower, relatively
stable temperatures and relative humidities. The oil analyses will be conducted under the outdoor field
conditions only. The soil samples, collected from sites in Ohio, Kentucky, and Tennessee, will have PCB
concentrations ranging from approximately 0.1 to 700 parts per million (ppm). Methanol solutions of
known PCB concentration will simulate extracted surface wipe samples, and range in PCB concentration
from 0 to 100 |j,g/mL. The oil samples, collected from active and in-active transformers at Oak Ridge
National Laboratory, will range in PCB concentration from 0 to 200 ppm.

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ABBREVIATIONS AND ACRONYMS
CASD
Chemical and Analytical Sciences Division
DOE
U. S. Department of Energy
EPA
U. S. Environmental Protection Agency
ERA
Environmental Resource Associates
ESD-LV
Environmental Science Division-Las Vegas
ESH&Q
Environmental Safety, Health, and Quality
ETTP
East Tennessee Technology Park
ETV
Environmental Technology Verification Program
ETVR
Environmental Technology Verification Report
&
false negative result
*
false positive result
GC
gas chromatography
HASP
Health and Safety Plan
LCS
Laboratory Control Sample
LMES
Lockheed Martin Energy Systems
MS/MSD
matrix spike/matrix spike duplicate
ORNL
Oak Ridge National Laboratory
ORNL-GJ
Oak Ridge National Laboratory, Grand Junction, Colorado
PCBs
polychlorinated biphenyls
PE
performance evaluation
PPE
personal protective equipment
ppm
parts per million, mg/kg for soils or |j,g/mL for extracts and oils
QA
quality assurance
QAPP
Quality Assurance Project Plan
QC
quality control
RFD
request for disposal
RSD
relative standard deviation
ix

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SCMT
Site Characterization and Monitoring Technology Pilot, ETV
SMO
Sample Management Office
SPE
solid phase extraction
SOP
standard operating procedure
SOW
statement of work
SSM
synthetic soil matrix
SVOCs
semivolatile organic compounds
UPSI
United Power Services Inc.
VOCs
volatile organic compounds
X

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1 INTRODUCTION
This chapter discusses the purpose of the verification and the verification test plan, describes the
elements of the verification test plan, and provides an overview of the Environmental Technology
Verification (ETV) Program and the technology verification process.
1.1	Verification Objectives
The purpose of this verification test is to evaluate the performance of commercially available field
analytical technologies for performing polychlorinated biphenyl (PCB) analyses in soil, methanol extract,
and/or transformer oil samples. Specifically, this plan defines the following elements of the verification test:
Roles and responsibilities of verification test participants;
Procedures governing verification test activities such as sample collection,
preparation, analysis, data collection, and interpretation;
Experimental design of the verification test;
Quality assurance (QA) and quality control (QC) procedures for conducting the
verification and for assessing the quality of the data generated from the verification;
and,
Health and safety requirements for performing work at hazardous waste sites.
1.2	What is the Environmental Technology Verification Program?
The U.S. Environmental Protection Agency (EPA) created the Environmental Technology
Verification Program (ETV) to facilitate the deployment of innovative or improved environmental
technologies through performance verification and dissemination of information. The goal of the ETV
Program is to further environmental protection by substantially accelerating the acceptance and use of
improved and cost-effective technologies. ETV seeks to achieve this goal by providing high-quality, peer-
reviewed data on technology performance to those involved in the design, distribution, financing, permitting,
purchase, and use of environmental technologies.
ETV works in partnership with recognized standards and testing organizations and stakeholder
groups consisting of regulators, buyers, and vendor organizations, with the full participation of individual
technology vendors. The program evaluates the performance of innovative technologies by developing
verification test plans that are responsive to the needs of stakeholders, conducting field or laboratory tests
(as appropriate), collecting and analyzing data, and preparing peer-reviewed reports. All evaluations are
conducted in accordance with rigorous quality assurance (QA) protocols to ensure that data of known and
adequate quality are generated and that the results are defensible.
ETV is a voluntary program that seeks to provide objective performance information to all of the
participants in the environmental marketplace and to assist them in making informed technology decisions.
ETV does not rank technologies or compare their performance, label or list technologies as acceptable or
unacceptable, seek to determine "best available technology," or approve or disapprove technologies. The
program does not evaluate technologies at the bench or pilot scale and does not conduct or support
research. Rather, it conducts and reports on testing designed to describe the performance of technologies
under a range of environmental conditions and matrices.
The program now operates 12 pilots covering a broad range of environmental areas. ETV has
begun with a 5-year pilot phase (1995-2000) to test a wide range of partner and procedural alternatives in
various pilot areas, as well as the true market demand for and response to such a program. In these pilots,
EPA utilizes the expertise of partner "verification organizations" to design efficient processes for conducting
performance tests of innovative technologies. These expert partners are both public and private
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organizations, including federal laboratories, states, industry consortia, and private sector entities.
Verification organizations oversee and report verification activities based on testing and QA protocols
developed with input from all major stakeholder/customer groups associated with the technology area. The
verification test described in this plan will be administered by the Site Characterization and Monitoring
Technologies (SCMT) Pilot, with Oak Ridge National Laboratory (ORNL) serving as the verification
organization. (To learn more about ETV, visit ETV's Web site at www, epa. gov/etv and ORNL's web site
at www.ornl.gov/etv). The SCMT pilot is administered by EPA's National Exposure Research Laboratory
(NERL), Environmental Sciences Division, in Las Vegas, Nevada. Note that seven PCB technologies have
already been verified for soils and solvent extracts; the reports can be viewed at either of the above-
mentioned web sites.
1.3 Technology Verification Process
The technology verification process is intended to serve as a template for conducting technology
verifications that will generate high quality data which can be used to verify technology performance. Four
key steps are inherent in the process:
Needs identification and technology selection
Verification test planning and implementation
Report preparation
• Information distribution
1.3.1	Needs Identification and Technology Selection
The first step in the technology verification process is to determine technology needs of the user-
community (typically state and Federal regulators and the regulated community). Each Pilot utilizes
stakeholder groups. Members of the stakeholder groups come from EPA, the Departments of Energy and
Defense, industry, and state regulatory agencies. The stakeholders are invited to identify technology needs
and to assist in finding technology vendors with commercially available technologies that meet the needs.
Once a technology need is established, a search is conducted to identify suitable technologies. The
technology search and identification process consists of reviewing responses to Commerce Business Daily
announcements, searches of industry and trade publications, attendance at related conferences, and leads
from technology vendors. The following criteria are used to determine whether a technology is a good
candidate for the verification:
Meets user needs
May be used in the field or in a mobile laboratory
Applicable to a variety of environmentally impacted sites
High potential for resolving problems for which current methods are unsatisfactory
Costs are competitive with current methods
Performance is better than current methods in areas such as data quality, sample preparation, or
analytical turnaround
Uses techniques that are easier and safer than current methods
Is commercially available and field-ready.
1.3.2	Verification Planning and Implementation
After a vendor agrees to participate, EPA, the Verification Organization, and the vendor meet to
discuss each participants responsibilities in the verification process. In addition, the following issues are
addressed:
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Site selection. Identifying sites that will provide the appropriate physical or chemical environment,
including contaminated media
Determining logistical and support requirements (for example, field equipment, power and water
sources, mobile laboratory, communications network)
Arranging analytical and sampling support
Preparing and implementing a verification test plan that addresses the experimental design, sampling
design, QA/QC, health and safety considerations, scheduling of field and laboratory operations,
data analysis procedures, and reporting requirements
1.3.3	Report Preparation
Innovative technologies are evaluated independently and, when possible, against conventional
technologies. The technologies being verified are operated by the vendors in the presence of independent
observers. The observers are EPA staff, state staff or from a independent third-party organization. The data
generated during the verification test are used to evaluate the capabilities, limitations, and field applications
of each technology. A data summary and detailed evaluation of each technology are published in an
Environmental Technology Verification Report (ETVR). The original complete data set is available upon
request.
An important component of the ETVR is the Verification Statement, which consists of three to five
pages, using the performance data contained in the report, are issued by EPA and appear on the ETV
Internet Web page. The Verification Statement is signed by representatives of EPA and ORNL.
1.3.4	Information Distribution
Producing the ETVR and the Verification Statement represents a first step in the ETV outreach
efforts. ETV gets involved in many activities to showcase the technologies that have gone through the
verification process. The Program is represented at many environmentally-related technical conferences and
exhibitions. ETV representatives also participate in panel sessions at major technical conferences. ETV
maintains a traveling exhibit that describes the program, displays the names of the companies that have had
technologies verified, and provides literature and reports.
We have been taking advantage of the Web by making the ETVRs available for downloading to
anyone interested. The ETVRs and the Verification Statements are available in Portable Document Format
(.pdf) on the ETV Web site (http://www.epa.gov/etv).
1.4 Purpose of this Verification Test Plan
The purpose of the verification test plan is to describe the procedures that will be used to verify the
performance goals of the technologies participating in this verification. This document incorporates the
QA/QC elements needed to provide data of appropriate quality sufficient to reach a credible position
regarding performance. This is not a method validation study, nor does it represent every environmental
situation which may be appropriate for these technologies. But it will provide data of sufficient quality to
make a judgement about the application of the technology under conditions similar to those encountered in
the field under normal conditions.
2 VERIFICATION RESPONSIBILITIES AND COMMUNICATION
This section identifies the organizations involved in this verification test and describes the primary
responsibilities of each organization. It also describes the methods and frequency of communication that will
be used in coordinating the verification activities.
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2.1 Verification Organization and Participants
Participants in this verification are listed in Table 2-1. The specific responsibilities of each
verification participant are discussed in Section 2.3 This verification test is being coordinated by the Oak
Ridge National Laboratory (ORNL) under the direction of the U.S. Environmental Protection Agency's
(EPA) Office of Research and Development, National Exposure Research Laboratory, Environmental
Sciences Division - Las Vegas, Nevada (ESD-LV). ESD-LV's role is to administer the verification
program. ORNL's role is to provide technical and administrative leadership and support in conducting the
verification.
Table 2-1. Verification Participants in PCB Field Analytical Technology Verification Test
Organization
Point(s) of Contact
Role
Oak Ridge National Laboratory
P.O. Box 2008
Bethel Valley Road
Bldg. 4500S, MS-6120
Oak Ridge, TN 37831-6120
Program Manager: Roger Jenkins
phone: (865) 576-8594
fax: (865) 576-7956
email: ienkinsrafStornl.eov
Technical Lead: Amy Dindal
phone: (865) 574-4863
fax: (865) 576-7956
email: dindalabfStornl.aov
verification
organization
U. S. EPA
National Exposure Research Laboratory
Environmental Science Division
P.O. Box 93478
Las Vegas, NV 89193-3478
Project Officer: Eric Koglin
phone: (702) 798-2432
fax: (702) 798-2261
email: k02lin.ericfffieDa.20v
EPA project
management
U. S. DOE
ORNL Site Office
P.O. Box 2008
Bldg. 4500N, MS-6269
Oak Ridge, TN 37831-6269
Program Coordinator: Regina Chung
phone: (865) 576-9902
fax: (865) 574-9275
email: chunarf®,ornl.aov
DOE/ORO
project
management
Dexsil Corporation
One Hamden Park Drive
Hamden, CT 06517
Contact: Ted Lynn
1-800-433-9745
fax: (203) 248-6523
tblvnn® dexsil .com
technology
vendor
Hybrizyme
2801 Blue Ridge Rd, Suite G-70
Raleigh, NC 27607
Contact: Randy Allen
phone: (919)783-9595
fax: (919) 782-9585
rallenf®,hvbrizvme. com
technology
vendor
LAS Laboratories
975 Kelly Johnson Drive
Las Vegas, NV 89119
no longer in business
reference
laboratory for
soil analyses
United Power Services Inc.
817 Fesslers Parkway
Nashville, TN 37210
Contact: Janet Lloyd
phone: (615)255-3700
fax: (615)256-0915
reference
laboratory for
oil analyses
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2.2 Organization
In Figure 2-1 is presented an organizational chart depicting the lines of communication for the
verification.
reference
laboratory
technology
vendors
test site
personnel
EPA Project Management
Las Vegas, NV
ORNL
Oak Ridge, TN
Verification
Organization
Figure 2-1. Organization chart for the verification test.
2.3 Responsibilities
The following is a delineation of each participant's responsibilities for the verification test.
Henceforward, the term "vendor" applies to Dexsil and Hybrizyme.
The Vendor, in consultation with ORNL and EPA, is responsible for the following elements of this
verification test:
Contribute to the design and preparation of the verification test plan;
Provide detailed procedures for using the technology;
Prepare field-ready technology for verification;
Operating and monitoring the technology during the verification;
Documenting the methodology and operation of the technology during the
verification;
Furnish data in a format that can be compared to reference values;
Logistical, and other support, as required.
ORNL has responsibilities for:
Preparing the verification test plan;
Developing a quality assurance project plan (QAPP) (Section 8 of the verification
test plan);
Preparing a health and safety plan (HASP) (Section 10 of the verification test plan)
for the verification activities;
Developing a test plan for the verification;
Acquiring the necessary reference analysis data;
Performing sampling activities (including collecting, homogenizing, dividing into
replicates, bottling, labeling, and distributing).
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ORNL and EPA have coordination and oversight responsibilities for:
Providing needed logistical support, establishing a communication network, and
scheduling and coordinating the activities of all verification participants;
Auditing the on-site sampling activities;
Managing, evaluating, interpreting, and reporting on data generated by the
verification;
Evaluating and reporting on the performance of the technologies.
Site access;
• Characterization information for the site;
Other logistical information and support needed to coordinate access to the site for
the field portion of the verification, such as waste disposal.
3 TECHNOLOGY DESCRIPTIONS
This section provides descriptions of the technologies participating in the verification test. These
descriptions were provided by the technology vendors, with minimal editing by ORNL. This section also
describes that performance factors that will be assessed based on the data generated during the verification.
3.1 Dexsil Corporation's L2000DX Analyzer
This technology will be verified for the analysis of transformer oils only. The performance of a
previous version of this instrument (L2000 PCB/Chloride Analyzer) was verified by ETV for soil and
solvent extracts in 1998 [1],
3.1.1	General Technology Description
The L2000DX Analyzer (dimensions: 9" x 9.5" x 4.25") is a field portable instrument, weighing
approximately 5 lbs. 12oz., designed to quantify PCB, chlorinated solvents and pesticides in soils, water,
transformer oils, and surface wipes. The L2000 can be operated in the field powered by a rechargeable 8
V gel cell, or in the laboratory using 120V A.C. power. PCBs in transformer oil can be quantified over a
range of 2 ppm to 2000 ppm. Total time for analysis of transformer oil is 5 minutes.
3.1.2	Transformer Oil Sample Preparation
Five milliliters of the oil is collected in a polyethylene reaction tube. Two glass ampules contained in
the reaction tube are broken, introducing metallic sodium to the oil. The mixture is then shaken for ten
seconds and allowed to react for a total of one minute. The sodium strips the covalently bonded chlorine
atoms off the PCB molecule. An aqueous extraction solution is added to the reaction tube to adjust the pH,
destroy the excess sodium, and to extract and isolate the newly formed chloride ions in a buffered aqueous
solution. The aqueous layer is decanted, filtered, and collected in an analysis vial. The ion specific electrode
is put into this aqueous solution to measure the millivolt potential. The potential is then converted to the
equivalent PCB concentration.
3.1.3	Instrument Calibration
A one point calibration is performed prior to sample analysis. The analyst simply follows the menu
driven instructions prompted in the LCD. When prompted, the instrument will ask if the calibration solution
is ready. The analyst inserts the ion specific electrode into the 50 ppm chloride solution, then pushes the
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yes button. The instalment will then prompt the user when calibrated. Additional calibration is required
when the instrument prompts the user, approximately every fifteen minutes.
3.1.4 Sample Analysis
The analyst chooses the appropriate A rod or from the programmed menu. If the Aroclor is not
known or if there is a mixture of Aroclors, Aroclor 1242 should be employed for the most conservative
results. To analyze the sample, the electrode is placed into the aqueous extract solution and the enter
button is pushed. After approximately 30 seconds, the PCB concentration of the samples (in ppm) is then
displayed on the L2000DX LCD.
3.2 Hybrizyme's DELFIA PCB Assay
This technology will be verified for the analysis of soils and solvent extracts.
3.2.1	General Technology Description
The Hybrizyme bioassay contains an antibody that binds
polychlorinated biphenyls (PCB) and has been developed for the
quantitative detectionofPCB in sample extracts. The signals from
sample extracts are compared with a control signal to determine
the relative amount of PCB present.
The Hybrizyme DELFIA'' PCB assay is a solid phase
fluoroimmunoassay. During an incubation with sample and PCB
Antibody, any PCB that is present is bound to the antibody. A
second antibody, which binds the PCB Antibody, is attached to
the microtiter plate wells, and traps the Ab-PCB complex. The
first wash step removes matrix interferences that may be in the
sample. A Europium-labeled PCB compound (PCB Tracer) is then allowed to bind to any PCB Antibody
binding sites that are empty. A wash step separates antibody-bound and free tracer. Following the wash
step, the addition of Enhancement Solution forms highly fluorescent chelates with the bound europium ions.
The amount of fluorescence measured is inversely proportional to the concentration of PCB in the sample.
Flybrizyme PCB DELFIA Reagent Kit provides 40 duplicate sample analysis. Retail price is $25 per
samples result (includes duplicates and controls)
3.2.2	Sensitivity
The sensitivity of the test is determined by the dilution factor used during sample processing. The
detection limit is defined as the minimum concentration of PCB that can be distinguished from a blank
standard with 95% confidence. Hybrizyme reports that a detection limit of 0.1 ppm Aroclor 1248 in
methanol (0.2 ppm in soil) has been demonstrated with this product.
3.2.3	Cross-Rea ctivity
The ability of the assay to detect various Aroclors is shown in the Table 3-1.
3.2.4	Quantitative Assay Procedure
The quantitative detection of PCB in sample extracts is performed by comparing the test response
of sample extracts to the test response of a control.
Figure 3-1. Hybriyzme's DELFIA PCB
Assav.
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Table 3-1. Summary of DELFIA PCB Assay's Cross-Reactivity
Aroclor
% Reactivity
1262
110
1260
130
1254
160
1248
100
1242
40
1016
25
1232
20
1.	A.C.S. reagent grade methanol is used as the Control. Perform each determination in duplicate for the
Control and samples. All sample extracts must be in methanol for analysis. All reagents and samples must
be brought to room temperature prior to use.
2.	Prepare the needed volume of PCB Tracer Solution by diluting 50 |j,L of PCB Tracer stock solution in
1.5 mL of PCB Assay Buffer per strip of wells used. Example: If three strips of wells will be used, dilute
150 |j,L of tracer stock solution into 4.5 mL of PCB Assay Buffer. Use within one hour of preparation.
3.	Prepare the PCB Antibody Solution by diluting 50 |j,L of PCB Antibody stock solution in 1.5 mL of
PCB Assay Buffer per strip of wells used. Use within one hour of preparation.
4.	Place the required number of microtitration strips in a strip frame. Wash the strips using the
"PREWASH" program of the platewasher. Tap the strips upside-down gently on a paper towel to blot
away any excess wash solution that may remain in the wells.
5.	Pipet 100 |j,L of the diluted PCB Antibody Solution into each well.
6.	Pipet 4 |j,L of each Control or sample into a well using the sequence shown in the table below. Use
columns 1 and 2 for Controls on each strip of wells used.
Table 3-2. Chart for well use

1
2
3
4
5
6
7
8
9
10
11
12
A
control
control
1st
1st
2nd
2nd
3rd
3rd
4th
4th
5th
5th



UK
UK
UK
UK
UK
UK
UK
UK
UK
UK
B
control
control
6th
6th
yth
yth
etc.








UK
UK
UK
UK






7. Shake the wells for 15 minutes.
8. Wash the strips using the "3 WASHES" program on the platewasher. Tap the strips upside-down gently
on a paper towel to blot away any excess wash solution that may remain in the wells.
8

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9.	Pipet 100 |j,L of the diluted PCB Tracer Solution into each well.
10.	Shake the wells for 5 minutes.
11.	Wash the strips using the "3 WASHES" program on the platewasher. Tap the strips upside-down
gently on a paper towel to blot away any excess wash solution that may remain in the wells.
12.	Add 150 |j,L of Enhancement Solution to each well.
13.	Select "PCB Quant" from the list of protocols in the Time-Resolved Fluorometer and measure the
fluorescence in each well. The protocol will automatically shake the wells for one minute and calculate the
concentration of PCB in the extracts. The amount of PCB in the sample must be correlated using the
sample processing concentration factor or dilution factor.
4 SAMPLE DESCRIPTIONS
This section discusses the history and characteristics of the verification test samples.
4.1 Soil Sample Descriptions
4.1.1 Environmentally-Contaminated Samples
Oak Ridge, Tennessee, is located in the Tennessee River Valley, 25 miles northwest of Knoxville.
Three Department of Energy (DOE) facilities are located in Oak Ridge: ORNL, the Y-12 plant, and the
East Tennessee Technology Park (ETTP). Chemical processing and production of components for nuclear
devices have occurred at the Y-12 Plant, and ETTP is a former gaseous diffusion uranium enrichment plant.
At both facilities, industrial processing associated with nuclear weapons production has resulted in the
production of millions of kilograms of PCB-contaminated soils. Two other DOE facilities—the Paducah
plant in Paducah, Kentucky, and the Portsmouth plant in Piketon, Ohio—are also gaseous diffusion
facilities with a history of PCB contamination. During the remediation of the PCB-contaminated areas at
the three DOE sites, soils were excavated from the ground where the PCB contamination occurred,
packaged in containers ranging in size from 55-gallon to 110-gallon drums, and stored as PCB waste.
Samples from these repositories, referred to as "Oak Ridge", "Portsmouth", and "Paducah" samples, will
be used in this verification. The characteristics of these soils are summarized in Table 4-1.
In Oak Ridge, excavation activities occurred between 1991 and 1995. The Oak Ridge samples
were comprised of PCB-contaminated soils from both Y-12 and ETTP. Five different sources of PCB
contamination resulted in soil excavations from various dikes, drainage ditches, and catch basins. Some of
the soils are EPA-listed hazardous waste due to the presence of other contaminants (e.g. diesel fuels).
A population of over 5,000 drums containing PCB-contaminated soils was generated from 1986 to
1987 during the remediation of the East Drainage Ditch at the Portsmouth Gaseous Diffusion Plant. The
ditch was reported to have three primary sources of potential contamination: (1) treated effluent from a
radioactive liquid treatment facility, (2) run-off from a biodegradation plot where waste oil and sludge were
disposed, and (3) storm sewer discharges. In addition, waste oil was reportedly used for weed control in
the ditch. Aside from PCB contamination, no other major hazardous contaminants were detected in these
soils. As such, no EPA hazardous waste codes are assigned to this waste.
Twenty-nine drums of PCB-contaminated soils from the Paducah plant were generated as part of a
spill cleanup activity at an organic waste storage area (C-746-R). The waste is considered a listed
hazardous waste for spent solvents (EPA hazardous waste code F001) because it is known to contain
9

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trichloroethylene. Other volatile organic compounds, such as xylene, dichlorobenzene, and cresol, were
also detected in the preliminary analyses of some of the Paducah samples.
4.1.2 Performance Evaluation (PE) and Blank Samples
Pre-prepared certified PE samples were obtained from Environmental Resource Associates (ERA)
and EPA's Office of Solid Waste and Emergency Response's Analytical Operations and Data Quality
Center for use in this study. The soils purchased from ERA (Arvada, CO) were prepared using ERA's
semivolatile blank soil matrix. This matrix is a top soil that has been dried, sieved, and homogenized.
Particle size is approximately 60 mesh. The soil is approximately 40% clay. Samples acquired from the
EPA's Office of Solid Waste and Emergency Response's Analytical Operations and Data Quality Center
were prepared using contaminated soils from various sites around the country in the following manner: The
original soils were homogenized and diluted with a synthetic soil matrix (SSM). The SSM had a known
matrix of 6% gravel, 31% sand, and 43% silt/clay; the remaining 20% was top soil. The dilution of the
original soils was performed by mixing known amounts of contaminated soil with the SSM in a blender for
no less than 12 hours. The samples were also spiked with target pesticides (BHC, methoxychlor, and
endrin ketone) to introduce some compounds that were likely to be present in an actual environmental soil.
The hydrocarbon background from the original sample and the spiked pesticides produced a challenging
matrix. The soil that will be used as the uncontaminated (blank) soil is a Captina silt loam from Roane
County, Tennessee. It is slightly acidic (pH ~5) and low in organic carbons (-1.5%). The soil composition
is 7.7% sand, 29.8% clay, and 62.5% silt [2], The environmental soil samples were characterized in terms
of composition (% sand, % gravel, % silt/ clay, etc.), total organic carbon, and pH. This data will be
reported in the technology verification report.
4.2	Extract Sample Descriptions
Traditionally, the amount of PCBs on a contaminated surface is determined by wiping the surface
with a cotton pad saturated with hexane. The pad is then taken to the laboratory, extracted with additional
hexane, and analyzed by gas chromatography. Unlike soil samples that can be more readily homogenized
and divided, equivalent wipe samples (i.e., contaminated surfaces or post-wipe pads) are not easily
obtainable. Therefore, for this study, interference-free solutions of PCBs prepared in methanol will be
analyzed to simulate an extracted surface wipe pad. Extract sample analyses will provide evaluation data
that primarily relies on the technology's performance rather than elements critical to the entire method (i.e.,
sample collection and preparation). For these samples, the vendor results will be compared to the nominal
concentration values only, instead of a reference laboratory result.
4.3	Transformer Oil Sample Descriptions
4.3.1 Environmentally-Contaminated Samples
Oils contaminated with various levels of PCBs were collected from active and in-active
transformers at ORNL. These transformer oils have been in-service for decades. Because of the lack of
computerized records, historical information about these oils (such as when the PCBs were added, what
are the oil's chemical characteristics, etc.) is unavailable. It is thought that these are all composed from
mineral oil. The concentration range of these samples is < 5 ppm to nearly 200 ppm PCBs, consisting of
single and multiple Aroclor mixtures (primarily 1242, 1254, and 1260, although other Aroclors may be
present). Because most of the native total PCB concentrations in these samples were less than 50 ppm,
ORNL augmented the Aroclor concentration of several of these samples to increase the total PCB
concentration. The spiking procedure is described in Section 5.
10

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Table 4-1. Summary of Environmentally-Contaminated Soil Sample Descriptions
Location
Request
for
Disposal
(RFD) #
Drum #
Description
Oak Ridge
40022
02
Soil from spill cleanup at the Y-12 Plant in Oak Ridge, Tennessee.
This soil is PCB-contaminated soil excavated in 1992.
Oak Ridge
40267
01
02
03
04
Soil from the Elza Gate area, a DOE Formerly Utilized Sites Remedial
Action Program site in Oak Ridge, Tennessee. This soil is PCB-
contaminated soil that was excavated in 1992.
Oak Ridge
24375
01
02
03
Catch-basin sediment from the K-711 area (old Powerhouse Area) at
the DOE East Tennessee Technology Park (formerly known as Oak
Ridge Gaseous Diffusion Plant) in Oak Ridge, Tennessee. This soil
is PCB-contaminated storm drain sediment that was excavated in
1991.
Oak Ridge
43275
01
02
Soil from the K-25 Building area at the DOE East Tennessee
Technology Park (formerly known as Oak Ridge Gaseous Diffusion
Plant) in Oak Ridge, Tennessee. This soil is PCB-contaminated soil
that was excavated in 1993.
Oak Ridge
134555
03
Soil from the K-707 area at the DOE East Tennessee Technology
Park (formerly known as Oak Ridge Gaseous Diffusion Plant) in Oak
Ridge, Tennessee. This soil is PCB-contaminated soil from a dike
spillage that was excavated in 1995.
Paducah
97002
01
02
03
04
Soil from the DOE Paducah Gaseous Diffusion Plant in Kentucky.
This soil is PCB-contaminated soil from a spill cleanup at the C-746-
R (Organic Waste Storage Area) that was excavated in 1989.
Portsmouth
7515
858
1069
1096
1898
2143
2528
3281
538
940
4096
Soil from the DOE Portsmouth Gaseous Diffusion Plant in Ohio.
This soil is PCB-contaminated soil from a probable PCB oil spill into
the East Drainage Ditch that was excavated in 1986.
4.3.2 Performance Evaluation and Blank Samples
PE samples and certified blanks were obtained from ERA. The oil used as blank and as the spiking
material was purchased from Calumet Lubricants (Princeton, LA). It is called transformer oil, with its
chemical name being a "severely hydrotreated light naphthenic petroleum oil", CAS # 64742-53-6. PE
samples were prepared at concentrations ranging from 5 to 175 ppm, containing single Aroclors (1254 and
1260) and 50:50 mixtures of 1254 and 1260. (See Section 7 for more detailed information.)
11

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5 SAMPLE COLLECTION AND PREPARATION
5.1 Soil Sample Collection
In Appendix A is presented the sample collection plan that was utilized in 1997 to collect the soil
samples. This plan specifies the procedures that were used to ensure the consistency and integrity of the
samples. In addition, this plan outlines the sample collection procedures necessary to meet the verification
test purpose and objectives.
5,1.1 Sample Collection Procedures
Sampling occurred at the K-25 site for several days over the period of April 17 through May 7,
1997. Portsmouth and Oak Ridge Reservation soils were collected from B-25 storage boxes and from 55-
gallon drums. Figure 6-1 is a photo of the sampling team acquiring some PCB soil samples from a 55-
gallon drum.
Soil was collected from the top of the daim and
placed in a plastic bag. The soil was then sifted by hand to
remove rocks and other large debris, and placed in a
plastic-lined 5-gallon container. Figure 6-2 shows the
samplers performing this procedure. The amount of soil
collected half-filled the 5-gallon container, amounting to
approximately 12 kg of soil. Once the sifting was
completed, the plastic liner was then removed from the
container. To homogenize the soil sample, the liner was
rolled on the ground in a back and forth motion, such the
sample was kneaded and thoroughly mixed. Two 40-mL
amber vials were fill with the homogenized soil for
preliminary analytical characterization. A third sample was
taken for total radiological activity screening. Paducah soil
samples were collected at the site and shipped to ORNL for use in the verification test.
Figure 5-1. K-25 personnel collect a PCB
sample from a 55-gallon drum.
5.1.2 Preliminary Soil Characterization
The two analytical samples taken of each field-
homogenized soils were analyzed by ORNL-based Grand
Junction, Colorado (ORNL-GJ) field team who
performed a preliminary on-site analyses of the PCB-
contaminated soils. In Appendix B is presented ORNL-
GJ's analytical procedures. ORNL's Chemical and
Analytical Sciences Division (CASD) also performed
preliminary characterization of the PCB-contaminated soils
using a similar procedure. The total PCB concentration
was measured in each analytical sample to determine
which samples would be used in the verification. Results
from the total activity screening indicated that the soils
were not considered radioactive.
Figure 5-2. K-25 sampling personnel sift through
the collected soil to remove rocks and other large
debris.
12

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5.1.3	Sample Preparation for Verification Test
Aliquots of several of the environmental soils were analyzed and determined to be heterogeneous in
PCB concentration. Because this is unsatisfactory for accurately comparing the performance of the field
technology with the laboratory-based method, the environmental soils had to be homogenized prior to
sample distribution. Each Portsmouth and Oak Ridge environmental soil sample was homogenized by first
placing approximately 1500 g of soil in a glass Pyrex dish. The dish was then placed in a large oven set at
35°C, with the exhaust and blower fans turned on to circulate the air. After drying overnight, the soil was
pulverized using a conventional blender and sieved using a 9-mesh screen (2 mm particle size). Last, the soil
was thoroughly mixed using a spatula. A comparison of dried and undried soils showed that a minimal
amount of PCBs (< 20%) was lost due to sample drying, making this procedure suitable for use in the
preparation of the soil samples. The Paducah samples, because of their sandy characteristics, only required
the sieving and mixing preparation steps. Multiple aliquots of each sample were analyzed using the analytical
procedure described below to confirm the homogeneity of the samples with respect to PCB concentration.
To provide the vendors with soils contaminated at higher concentrations of PCBs, some of the
environmental soils were spiked with additional PCBs. Spiked soils samples were prepared after the soil
was first dried in a 35° C oven overnight. The dry soil was ground using a conventional blender and sieved
through a 9-mesh screen (2 mm particle size). Approximately 1500 g of the sieved soil were spiked with a
diethyl ether solution of PCBs at the desired concentration. The fortified soil was agitated using a
mechanical shaker and then allowed to air-dry in a laboratory hood overnight. A minimum of four aliquots
were analyzed using the analytical procedure described below to confirm the homogeneity of the soil with
regard to the PCB concentration.
The procedure used to confirm the homogeneity of the soil samples entailed the extraction of 3 to 5
g of soil in a mixture of solvents (1 mL water, 4 mL methanol, and 5 mL hexane). After the soil/solvent
mixture was agitated by a mechanical shaker, the hexane layer was removed and an aliquot was diluted for
analysis. The hexane extract was analyzed on a Hewlett Packard 6890 gas chromatograph equipped with
an electron capture detector and autosampler. The method used was a slightly modified version of EPA's
SW-846 dual-column Method 8082 [3],
After analysis confirming homogeneity, the samples were split into jars for distribution. Each 4-oz
sample jar contained approximately 20 g of soil. Four replicate splits of each soil sample were prepared for
each participant. The samples were randomized in two fashions. First, the order in which the filled jars were
distributed was randomized, such that the same developer did not always receive the first jar filled for a
given sample set. Second, the order of analysis was randomized so that each developer analyzed the same
set of samples, but in a different order. PE materials were labeled in the same manner, such that the PE
samples are indistinguishable from other samples.
5.1.4	Sample Stability Study
In this study, the vendors will be analyzing the same samples that were used in the July 1997
verification of six PCB technologies and the September 1998 verification of one immunoassay technology.
Soil samples are available for the verification because extra samples were prepared and stored since 1997.
Prior to the 1998 and the 2000 study, ORNL performed chemical analyses of representative samples to
verily that significant amounts of PCBs had not been lost due to storage. Duplicate analyses from each
unique soil sample were performed. It was confirmed that no considerable losses in PCB concentration
had occurred, and therefore, all soil samples (and the reference laboratory analyses performed by LAS
Laboratories in 1997) will be utilized in the verification test.
13

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5.2	Extract Samples
The extract samples were prepared by ORNL at two concentrations levels (10 and 100 ug/hiL) in
methanol. More detailed information is provided in Section 7. The concentrations were confirmed by
ORNL's in-house laboratory. The samples were randomized and labeled similar to the soil samples
(described in Section 5.1.3). The samples were stored at 4 ± 2° C until analyzed by the vendors.
5.3	Oil Samples
5.3.1 Sample Collection
Oil sample collection from active and in-active transformers occurred at ORNL in May and June
2000. Figure 5-3 is a picture of the transformer yard at ORNL's 7000 area where in-active transformers
are stored. The transformers contain various levels of PCB-contamination in the oil, ranging from non-PCB
classification (< 5 ppm) to PCB-containing (50 to 500 ppm). No transformers with oils containing > 500
ppm PCBs remain on the Oak Ridge site. Figure 5-4 shows an active transformer at Building 5507 which
contains PCBs at regulatory levels (> 50 ppm). Samples were collected from this transformer for use in this
study.
5.3.1 Sample Preparation
The oil samples did not require homogenization. The samples, contained in 4-oz glass jars, were
split into 10-mL aliquots using a disposable plastic syringe. The samples were randomized and labeled
similar to the soil samples (described in Section 5.1.3). As mentioned previously, most of the native
concentrations of total PCBs in the environmentally-contaminated oil samples were less than 50 ppm.
Several of the transformer oils were augmented with additional Aroclors (up to -200 ppm), so that a larger
dynamic range could be tested. To spike the samples, approximately 250 mL of oil was poured into a 1-L
wide-mouth jar. A stir bar was added, and the jar was placed on a magnetic stirrer. With the oil being
stirred, hexane solutions of known concentrations of Aroclors were added to increase the total PCB
concentration. A single Aroclor was added to specific transformer oils. The specific augmented
concentration levels are described in Section 7.
Figure 5-4. Transformers at ORNL containing oils
Figure 5-3. Transformer yard at ORNL.	with PCB concentrations greater than 50 ppm.
6 REFERENCE LABORATORY ANALYSES
The verification process is based on the presence of a statistically validated data set against which
the performance goals of the technology may be compared. The choice of an appropriate reference
method and reference laboratory are critical to the success of the verification.
14

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6.1	Methods Selection
The reference analytical method for PCBs in soil is EPA SW-846 Method 8082 [3], The reference
analytical method for PCBs in transformer oil is EPA 600/4-81-045 [4],
6.2	Reference Laboratory Selection
To assess the performance of the PCB field analytical technology, the data obtained using the
technology will be compared to data obtained using conventional analytical methods. This decision is based
on the experience of prospective laboratories with QA procedures, reporting requirements, and data quality
parameters consistent with the goals of the Program. The laboratory must also demonstrate past proficiency
with the method.
Because the PCB soil sample concentrations were statistically unchanged, the reference laboratory
data generated in 1997 by LAS Laboratories will be used for comparison with the field analytical
technology results. Because PCB oil analyses are being added new to this verification test, a new reference
analytical laboratory, United Power Services Inc. (UPSI), Nashville, TN, was selected. The selection
process and analytical methods are described below.
6.2.1 Analysis of PCB Soils - LAS Laboratories
At the time of the 1997 verification, Oak Ridge Sample Management Office (SMO) was tasked by
DOE Oak Ridge Operations with maintaining a list of qualified laboratories to provide analytical services.
In Appendix C are presented the standard operating procedures that SMO used to identify, qualify, and
select analytical laboratories. The first procedure (LMES-ASO-AP-203, REV. 0) describes the process
for selecting, adding and expelling commercial laboratories to the Lockheed Martin Energy Systems
(LMES) Pricing Agreement. The second procedure (LMES-ASO-AP-210, REV. 0) defines the
methodology used by Oak Ridge Sample Management Office personnel in processing statements of work
(SOWs), processing purchase requisitions, and selecting commercial analytical laboratories. These
activities for the procurement of commercial laboratory services were used to support projects sponsored
by the DOE Oak Ridge Operations Office. The procedure served to ensure that as an operation of a DOE
contractor, LMES SMO maintained an optimum level of technical and administrative oversight on each
project, and SMO commercial procurement activities complied with federal acquisition laws and LMES
procurement policy. Using the procedures listed in Appendix C, ORNL and SMO selected LAS
Laboratories, in Las Vegas, NV, as the reference laboratory for the 1997 verification study. In Appendix
D is presented the LAS standard operating procedure.
The SMO conducted on-site audits of LAS annually as part of the laboratory qualification program.
At the time of selection, the most recent audit of LAS had occurred in February 1997. Results from this
audit indicated that LAS was proficient in several areas, including program management, quality
management, and training programs. No findings regarding PCB analytical procedure implementation were
noted. A second on-site assessment of LAS occurred August 11-12, 1997, during the analysis of the
verification study samples. This surveillance focused specifically on the procedures that were currently in
use for the analysis of the verification samples. The audit, jointly conducted by the SMO, DOE-ORO, and
EPA ESD-LV, verified that LAS was procedurally compliant. The audit team noted that LAS had excellent
adherence to the analytical protocols and that the staff were knowledgeable of the requirements of the
method. No findings impacting data quality were noted in the audit report.
15

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6.2.2 Analysis of PCB Oils - United Power Services Inc.
Because LAS Laboratories was no longer in business in 2000, a new reference laboratory had to
be selected for the analysis of the PCBs in oil. The industry standard test method for the determination of
PCBs in transformer oils is EPA Method 600/4-81-045 [4], A copy of the method is presented in
Appendix E. A predemonstration study, described in Section 7, was used as a qualification activity for the
lab. Additionally, an on-site audit of the laboratory will occur while the PCBs in oil samples are being
analyzed.
7 VERIFICATION TEST DESIGN
This section discusses the objectives of the pre-demonstration study, the verification test, factors
that must be considered to meet the performance objectives, and the information that ORNL and EPA will
use to evaluate the results of the verification.
7.1 Pre-Demonstration Study
A pre-demonstration study is required by the SCMT pilot to allow the technology vendors to refine
their technologies and revise their operating instructions, if necessary. The pre-demonstration also serves as
a test of the reference laboratory. This analysis also allows an evaluation of matrix effects or interferences
that may affect the verification. A failure to meet the performance goals at this point could indicate a lack of
maturity of the technology and the verification would be canceled. This requirement has the following
objectives:
To allow the vendors to analyze samples that will be included in the verification in advance,
and, if necessary, refine and calibrate their technologies and revise their operating
instructions
To allow an evaluation of any unanticipated matrix effects or interferences that may occur
during the verification
For the pre-demonstration study, the vendors analyzed five PCB-contaminated soils (1 blank and 4
PEs) and/or six PCB-contaminated oils (1 blank, 1 spike, and 4 environmentally-contaminated); no extract
samples were provided in the pre-demonstration study. PE samples were obtained from Environmental
Resource Associates.
The pre-demonstration samples were sent to the vendors on May 30, 2000. The results for the
pre-demonstration sample analyses were provided to ORNL approximately two weeks after the receipt of
the samples (June 16, 2000).
The soils distributed were all of known concentration, due to complications with shipping DOE
waste materials, and also because there were no reference analyses being performed. The vendor pre-
demonstration results were compared to the performance acceptance ranges. (The acceptance ranges,
based on the analytical verification data, are guidelines established by the provider of the PE materials to
gauge acceptable analytical results.) For the oils, the results were compared to the reference laboratory.
All of the vendors participating in this verification test demonstrated through the pre-demonstration study
that their technology is prepared for rigorous field testing.
Because a new reference laboratory was being selected for the PCBs in oil analyses, a more
extensive pre-demonstration study was conducted with UPSI. Forty oil samples, including environmentally-
contaminated samples, spikes, and replicates, were sent blindly to UPSI for analysis. UPSI produced
results that were comparable to expected concentrations, reproducible on replicate samples, and accurate
on spiked samples.
16

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7.2 Objective of the Verification Test
The primary objectives of this verification are to evaluate the PCB field analytical technologies in the
following areas: (1) how well each performs relative to conventional analytical methods, (2) PE results, and
(3) the logistical and economic resources necessary to operate the technology. Secondary objectives for
this verification are to evaluate the PCB field analytical technology in terms of its reliability, ruggedness,
cost, range of usefulness, sample throughput, data quality, and ease of operation. Specifically, the
verification process will evaluate the performance of the technology against the performance goals as stated
in Section 3.
7.3. Summary of Verification Activities
The verification test will be held at ORNL (see Figure 7-1) from August 21 through September 1,
2000. The vendors have the option of analyzing soils (208 samples), extracts (24 samples), and/or oils
(152 samples) contaminated with PCBs. The samples evaluated during the verification will consist of (1)
environmental soil samples from the Oak Ridge Reservation, Paducah, and Portsmouth DOE sites, (2)
spiked environmental soil samples, (3) purchased certified soil samples, (4) ORNL-prepared methanol
extract samples, (5) transformer oils, (6) spiked transformer oils, and (7) purchased, certified oil samples.
The verification soil and oil samples have been homogenized and split such that the vendor is supplied with
equivalent samples analyzed by a fixed analytical laboratory (referred to as the reference lab). The field
technology results for the extract samples will be compared to the nominal spike concentration. The
experimental design approach is presented in Tables 7-1 through 7-6.
Building J5D7
(
l.iRmnnslTfttinn
Field Aiea
h

0^*—	\
Figure 5-1. Field Verification Test site at ORNL, near Building 5507.
17

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Table 7-1. Summary of Environmental Soil Sample Analyses ( by Drum Number)
Target
Concentration
Range
Outdoor Site
Chamber Site
Oak Ridge#l
Oak Ridge#2
Paducah#l
Totals #
Samples
Paducah#l
Portsmouth#l
Portsmouth#2
Total #
Samples
0.1 - 2.0 ppm
40022-02 a
24375-01
40267-02
24375-02
97002-04
97002-01
28
97002-04
97002-01
7515-4096

12
2.1 - 20.0 ppm
40267-03
40267-01
40267-04

97002-03
16
97002-03
7515-1898
7515-2528
7515-3281
20
20.1 - 50.0 ppm

134555-03S
97002-02
12
97002-02
7515-1096
7515-2143
7515-1069
7515-0858
24
50.1 -700 ppm
40267-0IS b
24375-03
43275-01
43275-02
97002-02S
12
97002-02S
7515-0940
7515-0538S
7515-0538
7515-0538S
12
Total # samples
24
24
20
68
24
24
20
68
Grand Total
136
¦ Four replicates will be analyzed for each drum number.
6 "S" indicates that the sample is a matrix spiked environmental sample.
18

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Table 7-2. Summary of Performance Evaluation Soil Samples


Number of Replicates
Sample
Concentration (ppm)


Outdoor Site
Chamber Site

2
4
4
Aroclor 1248 a




20
4
4

5
4
4
Aroclor 1254 a




50
4
4

11
4
4
Aroclor 1260 a




50
4
4

2 c
4
4
Mixture of Aroclor 1254 and 1260 b




50 c
4
4
Uncontaminated (blank) soil
n/a
4
4
(Tennessee Reference Soil)



Total # samples
36
36
Grand Total
72
a Provided by the EPA's Office of Solid Waste and Emergency Response's Analytical Operations and Data Quality Center.
6 Provided by Environmental Resource Associates.
c Total PCB concentration
Table 7-3. Summary of Extract Sample Analyses
Sample Concentration
Number of Replicates
Grand Total
Outdoor Site
Chamber Site
10 |ig/mL
4

4
8
100 |ig/mL
4

4
8
Methanol Blank
4

4
8
Total # samples
12
12
24
19

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Table 7-4. Summary of Oil Sample Analyses
Target
Concentration
Range
Number of Samplesa
Environmental
PE
blank
2
5
< 5.0 ppm
2
1
5.1 - 25.0 ppm
4
1
25.1 -40.0 ppm
4
1
40.1 - 50.0 ppm
3
1
50.1 - 75.0 ppm
4
2
75.1 - 100.0 ppm
2
1
> 100 ppm
4
1
Total # samples, including 4 replicates each
100
52
Grand Total
152
a Four replicates will be analyzed for each.
Table 7-5. Summary of Oil PE Samples
Nominal Concentration (ppm)
Aroclor
Ratio in Mixture
5
1254
n/a
25
1260
n/a
40
1254/1260
50/50
50
1254/1260
50/50
60
1254/1260
50/50
75
1260
n/a
100
1254
n/a
175
1254/1260
50/50
Table 7-6. Summary of Verification Analyses
Sample Type
Number of Samples
Environmental soil samples
136
PE soil samples
72
Extract samples
24
Environmental oil samples
100
PE oil samples
52
Grand Total
384
20

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7.3.1 Environmental Conditions for the Test
Verification activities for the soils and extracts will occur at two sites at ORNL: a natural outdoor
environment (the outdoor site) and inside a controlled environmental atmosphere chamber (the chamber
site). Generally, the average August temperature for eastern Tennessee is 77°F. Studies will also be
conducted inside a controlled environmental atmosphere chamber, hereafter referred to as the "chamber",
located in Building 5507 at ORNL. The controlled experimental atmosphere facility consists of a room-size,
walk-in chamber ten feet wide and twelve feet in length with air processing equipment to control
temperature and humidity. Verification studies inside the chamber will be used to evaluate performance
under environmental conditions that are markedly different from the ambient outdoor conditions at the time
of the test. The temperatures in the chamber during the testing periods will be set at 55 °F. The temperature
and relative humidity will be monitored at both sites during the testing.
7.4	Sample Distribution
ORNL will be responsible for sample distribution. The samples will be packaged in 4 ounce (120
mL) jars, as described in Section 6. All samples will be prepared for distribution at the start of the
verification. The vendors will go to a sample distribution table located in Building 5507 to pick-up the
samples. The samples will be distributed in batches of 12. Completion of chains-of-custody will document
sample transfer.
7.5	Archive Samples
Archive samples which are replicates of the vendor samples will be retained by ORNL. An archive
sample will be used during the verification if the integrity of a vendor's sample has been compromised.
Additional unhomogenized material and unused archive samples will also be retained at ORNL at the
completion of the verification, in case any questions arise where reanalysis is necessary.
7.6	Submission of Results
The vendor will provide the results to ORNL. The vendor will be responsible for reducing the raw
data into a presentation format consistent with the evaluation requirements. At the end of the verification
test, the vendor will submit all final results and raw data to ORNL. After the conclusion of the field
activities, the vendors will have one week to review their data and make revisions to their results. These
revisions will not involve re-analysis of any sample. The revisions will be limited to correcting for calculation
and transcription errors.
7.7	Verification Performance Factors
The following are the logistical and technical performance verification factors that will be verified for
each technology.
Accuracy: closeness of technology result to known value;
Precision: reproducibility of technology's results;
Comparability: performance relative to reference laboratory;
False positive results: number of blanks where PCBs detected;
False negative results: number of contaminated samples that technology reported as non-
detect;
Sample throughput: number of samples/hour/number of analysts
Application to regulatory-decision making: performance at regulatory decision-making
levels for PCBs (50 ppm for soils and oils and 100 |j,g/100cm2 for surface wipes).
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These factors and the anticipated statistical analyses are further discussed in Section 8.
8 QUALITY ASSURANCE PROJECT PLAN (QAPP)
The QAPP for this verification test specifies procedures that will be used to ensure data quality and
integrity. Careful adherence to these procedures will ensure that data generated from the verification will
meet the desired performance objectives and will provide sound analytical results.
8.1	Purpose and Scope
The primary purpose of this section is to outline steps that will be taken to ensure that data resulting
from this verification is of known quality and that a sufficient number of critical measurements are taken.
This section is written in compliance with the SCMT Quality Management Plan [5],
8.2	Quality Assurance Responsibilities
The implementation of the verification test plan must be consistent with the requirements of the
study and routine operation of the technology. The ORNL technical lead is responsible for coordinating the
preparation of the QAPP for this verification and for its approval by EPA and ORNL. The ORNL program
manager will ensure that the QAPP is implemented during all verification activities. ORNL's QA specialist
(QAS) will review and approve the QAPP and will provide QA oversight of the verification activities. The
ORNL technical lead will be responsible for the reference laboratory data validation. The ORNL
statistician will primarily be responsible for the reduction of the vendor and reference laboratory data. The
EPA project manager and QA manager will review and approve this plan.
8.3	Field Operations
8.3.1	Site Training
Preliminary site training will be provided to all vendors on the first day of testing. This will be
required before initiation of the field study. This training will be conducted by the ORNL program manager
or his designee. It will entail an overview of the test site, safety information, emergency procedures, and
logistical information regarding the verification test.
8.3.2	Communication and Documentation
Successful field operations require detailed planning and extensive communication. ORNL will
communicate regularly with the verification participants to coordinate all field activities associated with this
verification and to resolve any logistical, technical, or QA issues that may arise as the verification
progresses. Pertinent vendor and ORNL field activities will be thoroughly documented. Field
documentation will include field logbooks, photographs, field data sheets, and chain-of-custody forms.
The ORNL technical lead will be responsible for maintaining all field documentation. Field notes
will be kept in a bound logbook. Each page will be sequentially numbered and labeled with the project
name and number. Completed pages will be signed and dated by the individual responsible for the entries.
Errors will have one line drawn through them and this line will be initialed and dated. Any deviations from
the approved final verification test plan will be thoroughly documented in the field logbook and provided to
the ORNL. Photographs will be taken with a digital camera.
8.4	Performance and System Audits
The following audits will be performed during this verification.
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8.4.1	Technical Systems A udit
ORNL's QAS will perform a surveillance during verification testing to assess compliance with the
demonstration plan.
8.4.2	Data quality audit of the reference laboratory
UPSI will be audited during the analyses of the oil samples. The audit will focus on adherence to
method requirements and procedures, particularly in sample preparation, sample management, and quality
control.
8.4.3	Surveillance of Technology Performance
During verification testing, ORNL staff will observe the operation of the field technology, such as
observing the vendor operations, photo-documenting the demonstration activities, surveying calibration
procedures, and reviewing sample data. The observations will be documented in a laboratory notebook or
by completing a field audit form.
8.5	Quality Assurance Reports
QA reports provide the necessary information to monitor data quality effectively. It is anticipated
that the following types of QA reports will be prepared as part of this verification.
8.5.1	Status Reports
ORNL will regularly inform the EPA project manager of the status of the verification. Project
progress, problems and associated corrective actions, and future scheduled activities associated with the
verification test will be discussed. When problems occur, the vendor and ORNL will discuss them, estimate
the type and degree of impact, describe the corrective actions taken to mitigate the impact and to prevent a
recurrence of the problems, and discuss with EPA, as necessary. Major problems will be documented in
the field logbook.
8.5.2	A udit Reports
Any QA audits or inspections that take place in the field while the verification test is being
conducted will be formally reported by the auditors to the ORNL technical lead, who will forward them to
the EPA project manager. Informal reporting of audit results will be reported immediately to EPA.
8.6	Corrective Actions
Routine corrective action may result from common monitoring activities, such as:
Performance evaluation audits
Technical systems audits
Calibration procedures
If the problem identified is technical in nature, the individual vendors will be responsible for seeing that the
problem is resolved. If the issue is one that is identified by ORNL or EPA, the identifying party will be
responsible for seeing that the issue is properly resolved. All corrective actions will be documented. Any
occurrence that causes discrepancies from the verification test plan will be noted in the technology
verification report. The reference laboratory procedures (See Appendices D and E) describe the corrective
action plan for not meeting minimum QC requirements.
8.7	Reference Laboratory Quality Control Checks
Quality control (QC) samples will be analyzed by UPSI to indicate whether or not the samples
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were analyzed properly. A summary of QC samples include: initial calibration, continuing calibration
verification, and analysis of known samples (spiked Aroclors in isooctane and oil). This data will be
reviewed by ORNL as part of the data validation process. Discrepancies will be noted in the data
validation records.
Note that the LAS reference laboratory data for soil analyses has already been reviewed and
validated by ORNL.
8.8	Data Management
The vendor, ORNL, and EPA each have distinct responsibilities for managing and analyzing
verification data. ORNL is responsible for managing all the data and information generated during the
verification test._The vendor is responsible for obtaining, reducing, interpreting, validating, and reporting the
data associated with their technology's performance. These data should be reported on the chain-of-
custody. Vendor results will be due to ORNL at the conclusion of a day's field activities. The vendor's
final report will be due to ORNL one week after the verification. Any discrepancies between the originally
reported result and the final result must be described. EPA and ORNL are responsible for analysis and
verification of the data
8.9	Data Reporting, Validation, and Analysis
To maintain good data quality, specific procedures will be followed during data reduction, review,
and reporting. These procedures are detailed below.
8.9.1	Data Reporting
Data reduction refers to the process of converting the raw results into a concentration which will be
used for evaluation of performance. The procedures to be used will be technology dependent, but the
following is required for data reporting:
The reported PCB concentration should be either total PCB concentration or PCB
concentration by Aroclor. The result will be definitively labeled as such.
The concentration units for oil and soil samples will be parts per million (i.e., ppm, as
received) and ng/mL for extract samples.
If no PCB is detected, the concentration should be reported as less than the reporting limits
of the technology, with the reporting limits stated (e.g., < 0.5 ppm). If the technology
reports interval results, a non-detect will be reported as the lowest interval (e.g., 0 to 0.5
ppm).
8.9.2	Data Validation
Validation determines the quality of the results relative to the end use of the data. ORNL will be
responsible for validating the reference laboratory data. (Note that the vendor is responsible for validating
its own data prior to final submission.) Several aspects of the data (listed below) will be reviewed. The
findings of the review will be documented in the validation records. As appropriate, the ETVR will
describe instances of failure to meet quality objectives and the potential impact on data quality.
8.9.2.1 Completeness of Laboratory Records
This qualitative review ensures that all of the samples that were sent to the laboratory were
analyzed, and that all of the applicable records and relevant results are included in the data package.
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8.9.2.2	Holding Times
For oil, the method requirement is that the samples be prepared within 14 days of receipt and
analyzed within 40 days of preparation. Adherence to this requirement will be reviewed for all samples.
8.9.2.3	Correctness of Data
So as not to bias the assessment of the technology's performance, errors in the reference
laboratory data will be corrected as necessary. Corrections may be made to data that has transcription
errors, calculation errors, and interpretation errors. These changes will be made conservatively, and will be
based on the guidelines provided in the method used. The changes will be justified and documented in the
validation records.
8.9.2.4	Correlation Between Replicates
Normally, one would not know if a single sample result was "suspect" unless (a) the sample was a
spiked sample, where the concentration is known or (b) a result was reported and flagged by the reference
laboratory as suspect for some obvious reason (e.g., no quantitative result was determined). The
experimental design implemented in this verification study will provide an additional indication of the
abnormality of data through the inspection of the replicate results from homogenous sample sets. Criteria
has been established to determine if data is suspect. Data sets will be considered suspect if the percent
relative standard deviation for replicate samples was greater than 50%, because this criteria would indicate
imprecision. These data would be flagged so as not to bias the assessment of the technology's
performance. Precision and accuracy evaluations may be made with and without these suspect values to
represent the best and worst case scenarios. If both the reference laboratory and the vendor(s) report
erratic results, the data may be discarded if it is suspected that the erratic results are due to a sampling
error.
8.9.2.5	Evaluation ofQC Results
As stated in Section 8.7, QC samples will be analyzed by the reference laboratory with every batch
of samples to indicate whether or not the samples were analyzed properly. Performance on these samples
will be reviewed and major findings will be noted in the validation records.
8.9.2.6	Evaluation of Spiked Sample Data
Spiked samples are homogenous samples containing known concentrations of analyte(s). The
performance of the reference laboratory will be evaluated relative to the spiked samples. Results for these
samples represent the best estimate of accuracy and precision for verification testing.
8.9.3 Data A nalysis
This section contains a list of the five primary performance factors to be evaluated for both the field
technology and the reference laboratory.
8.9.3.1 Precision
Precision, in general, refers to the degree of mutual agreement among measurements of the same
materials and contaminants. Environmental applications often involve situations where "measurements of the
same materials" can take on a number of interpretations. In environmental applications, precision is often
best specified as a percentage of contaminant concentration. The following lists several possible
interpretations of precision for environmental applications.
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1)
The precision involved in repeated measurements of the same sample without adjusting the
test equipment.
2)	The precision involved in repeated measurements of the same sample after reset,
repositioning, or re-calibration of the test equipment or when using different equipment of
the same technology.
3)	The precision of measurements due to spatial variability of soil samples from adjacent
locations.
4)	The precision characteristics of a specific technology in determining contamination at a
specific site or at an arbitrary site.
In general, users of the technology will want to be assured that measurement variability in 1) and 2)
is small. Measurement variability due to spatial variability described in 3) is likely to be site specific and is
minimized in this verification by using homogeneous samples. The measurement variability discussed in 4) is
perhaps of most interest as it includes measurement variability resulting from possible differences in the
design activities and effects of environmental conditions such as temperature that would vary from one site
characterization to another as well as site and technology specific sources.
The strength of this verification's experimental design is that since an equal number of replicates will
be performed for every sample at every concentration level, an equal number of precision comparisons can
be made. However, enough replicates and quality control samples will be analyzed to independently assess
each technology's performance.
Precision for this verification will be estimated by the variance, or standard deviation from the
measured data. If "n" PCB concentration measurements are represented by Yb Y2, ..., Yn, the estimated
variance about their average value "7" is calculated by:
* 1 fe-i
The standard deviation is the square root of S2 and implies that the uncertainty is independent of the PCB
concentration values. To express the reproducibility relative to the average PCB concentration, percent
relative standard deviation (RSD) is used to quantify precision, according to the following equation:
RSD = (standard deviation / average concentration) x 100%
Replicate samples at each PCB concentration can be used to establish the relationship between the
uncertainty and the average PCB concentration. RSD cannot be calculated for PCB concentration results
reported as interval data. To assess precision, the frequency of results reported as the same interval will be
determined.
8.9.3.2 Accuracy
Accuracy is a measure of how close, on average, the measured PCB concentrations are to the true
values or to an accepted value. Accuracy for the PCB verification will be relative to a spiked PCB
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concentration in the performance evaluation samples, computed as percent recovery using the equation:
percent recovery = (measured amount / spiked amount) x 100%
The optimum percent recovery value is 100%. Percent recovery values greater than 100% indicate results
that are biased high, and values less than 100% indicate results that are biased low. Percent recovery will
be used to assess the accuracy of the reference laboratory and of technologies which report quantitative
results. For technologies which produce interval results, accuracy will be evaluated in terms of the
percentage of samples which agree with, are above (i.e., biased high), and are below the certified values
(i.e., biased low).
Inaccuracies or biases are the result of systematic differences between measured and true values.
These biases may be due to limited calibration range, systematic errors, standards preparation, storage and
homogeneity of the soil samples either at the PCB verification or at the reference laboratory. Consequently
every effort will be made by ORNL, the technology vendors and the reference laboratory to identify
specific sources of inaccuracies. The verification includes blanks, replicates, and performance evaluation
samples that should provide substantiating evidence to support this partitioning of sources of bias when
results become available.
8.9.3.3	False Positive/False Negative Results
A false positive (fp) result is one in which the technology detects PCBs in the sample when there
actually are none [6], A false negative (fn) result is one in which the technology indicates that no PCBs are
present in the sample, when there actually are [6], The evaluation of fp and & results is influenced by the
actual concentration in the sample and includes an assessment of the reporting limits of the technology.
False positive results will be assessed in two ways. First, the results will be assessed relative to the blanks
(i.e., the technology reports a detected value when the sample is a blank). Second, the results will be
assessed on environmental and spiked samples where the analyte was not detected by the reference
laboratory (i.e., the reference laboratory reports a nondetect and the field technology reports a detection).
False negative results, also assessed for environmental and spiked samples, indicate the frequency that the
technology reported a nondetect (i.e., < reporting limits) and the reference laboratory reported a detection.
The reporting limit will be considered in the evaluation. For example, if the reference laboratory reported a
result as 0.9 ppm, and the technology's paired result was reported as below reporting limits (<1 ppm), the
technology's result will be considered correct and not a false negative result.
8.9.3.4	Comparability
Comparability refers to how well the field technology and reference laboratory data agree. The
difference between accuracy and comparability is that whereas accuracy is judged relative to a known
value, comparability is judged relative to the results of a standard or reference procedure, which may or
may not report the results accurately. A one-to-one sample comparison of the technology results and the
reference laboratory results will be performed in the ETVR.
A correlation coefficient quantifies the linear relationship between two measurements [7], The
correlation coefficient is denoted by the letter r; its value ranges from -1 to +1, where 0 indicates the
absence of any linear relationship. The value r = -1 indicates a perfect negative linear relation (one
measurement decreases as the second measurement increases); the value r = +1 indicates a perfect positive
linear relation (one measurement increases as the second measurement increases). The slope of the linear
regression line, denoted by the letter m, is related to r. Whereas r represents the linear association between
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the vendor and reference laboratory concentrations, m quantifies the amount of change in the vendor's
measurements relative to the reference laboratory's measurements. A value of+1 for the slope indicates
perfect agreement. Values greater than 1 indicate that the vendor results are generally higher than the
reference laboratory, while values less than 1 indicate that the vendor results are usually lower than the
reference laboratory.
In addition, a direct comparison between the field technology and reference laboratory data will be
performed by evaluating the percent difference (%D) between the measured concentrations, defined as
%D = ([field technology\ - \ref lab]) / (ref lab) x 100%.
8.9.3.5 Completeness
Completeness refers to the amount of data collected from a measurement process expressed as a
percentage of the data that would be obtained using an ideal process under ideal conditions. The
completeness objective for data generated during this verification is 95% or better.
There are many instances which might cause the sample analysis to be incomplete. Some of these
are:
•	Instrument failure
•	Calibration requirements not being met
•	Evaluated analyte levels in the method blank
9 HEALTH AND SAFETY PLAN
This section describes the specific health and safety procedures that will be used during the field
work at the Oak Ridge National Laboratory.
9.1	Contact Information
The ORNL project manager will be Roger Jenkins, (865) 576-8594.
The ORNL technical lead will be Amy Dindal, (865) 574-4863.
The ES&H Coordinator will be Fred Smith, (865) 574-4945.
The Environmental Protection Officer will be Kim Jeskie, (865) 574-4947.
The Laboratory Shift Superintendent number is (865) 574-6606.
The Emergency Communications Center number is (865) 574-6646.
IN CASE OF ANY EMERGENCY, DIAL 9-1-1.
Emergency phone numbers will be posted at the test site.
9.2	Health and Safety Plan Enforcement
ORNL project manager, ORNL technical lead, and the ES&H Coordinator will be responsible for
enforcing the health and safety plan. ORNL project manager will ultimately be responsible for ensuring that
all verification participants abide by the requirements of this HASP. ORNL technical lead will oversee and
direct field activities and is also responsible for ensuring compliance with this HASP.
9.3	Site Access
Visitors will be badged and escorted at all times by ORNL personnel. Visitors will follow standard
ORNL safety and health policies and practices. Site training will be provided to the vendors prior to testing.
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9.4	Waste Generation
All hazardous waste generated by the technology vendors will be properly disposed of by the
Environmental Protection Officer. The technology vendors will assist with this process by providing
accurate records of the waste contents and approximate concentrations.
9.5	Hazard Evaluation
PCBs will be the most prevalent chemical hazard at the verification test. PCBs are:
•	Nonflammable liquids;
•	Carcinogenic;
•	Viscous liquids with a mild, hydrocarbon odor.
Some possible health effects from exposure to PCBs are: (1) irritation to the eyes and skin, possibly
forming an acne condition; and (2) liver damage. If PCBs contact the skin, immediately wash the
contaminated skin with soap and water. If PCBs penetrate the clothing, immediately remove the clothing
and wash the skin with soap and water. Get medical attention promptly.
PCBs issues and hazards will be controlled per ORNL procedures (Oak Ridge Reservation
Polychlorinated Biphenyl Federal Facilities Compliance Agreement, ORR-PCB-FFCA, and ORNL-EP-
P04, Management of Polychlorinated Biphenyls). These procedures can be found on ORNL's interval
web site.
Other hazards associated with this verification test include worker exposure to volatile organic
compounds (VOCs), semivolatile organic compounds (SVOCs), and additional physical hazards
associated with the technology's equipment. Plastic ground covers will be placed underneath each
technology set-up, in order to collect any spills of soil or solvent. Ground covers will be replaced as
necessary.
Exposure to VOCs and SVOCs during field activities may occur through inhalations or ingestion.
The most likely exposure to VOCs and SVOCs during the verification test will be through dermal contact.
Dermal contact with contaminated soil will be prevented through the use of personal protective equipment
(PPE), such as gloves. The technology vendors must provide their own PPE. Although unlikely to be
necessary, visitors will be provided with PPE if warranted.
9.6	Personal Protection
Personal Protective Equipment (PPE) shall be appropriate to protect against known and potential
health hazards encountered during routine operation of the technology systems. For this verification, Level
D PPE is required. Level D provides minimal protection against chemical hazards. It consists only as a
work uniform, with gloves worn, where necessary. Level D PPE will be supplied bv the individual
technology vendor. ORNL will provide visitors with PPE if necessary. If site conditions or the results of
Industrial Hygiene surveillance indicates that additional hazards are present, ORNL may recommened
different or additional PPE to the vendors. The following is the list of protective equipment required for
verification operations:
•	Appropriate work clothes (no shorts or open-toed shoes);
•	Safety glasses.
9.7	Physical Hazards
Physical hazards associated with field activities present a potential threat to on-site personnel.
Dangers are posed by unseen obstacles, noise, heat, and poor illumination. Injuries may results from the
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following:
•	Accidents due to slipping, tripping, or falling
•	Improper lifting techniques
•	Moving or rotating equipment
•	Improperly maintained equipment
Injuries resulting from physical hazards can be avoided by adopting safe work practices and by using
caution when working with machinery.
9.8	Fire
The following specific actions will be taken to reduce the potential for fire during site activities:
•	No smoking within 20 feet of the site.
•	Fire extinguishers will be maintained on-site.
•	All personnel will be trained on the location of the portable fire extinguishers.
9.9	Mechanical, Electrical, Noise Hazards
Some technology-specific hazards may be identified once the vendors set-up their equipment.
Proper hazards controls (i.e., guarding or markings) or PPE (i.e., ear plugs for noise hazards) will be
implemented as necessary.
Electrical cables represent a potential tripping hazards. When practical, cables will be placed in
areas of low pedestrian travel. If necessary, in high pedestrian travel areas, covers will be installed over
cables.
9.10	Unstable/Uneven Terrain
The terrain around Building 5507 is uneven and bumpy. Site personnel shall be aware of uneven
terrain to avoid slips, trips, and falls.
9.11	Inclement Weather
The verification test will occur the latter part of August. The possibility of inclement weather
(particularly rain and thundershowers) exists. The vendors should be prepared to deal with a possible
inclement weather situation.
Operating temperatures in the chamber could be as low as 50°F. Vendors should be prepared to
work in those temperatures.
9.12	Heat Stress
Since the verification test will occur in August, the possibility of a heat-related injury during field
work is possible. Heat stress symptoms include heat cramps, heat exhaustion, and heat stroke. Heat
stroke is the most serious condition and can be life-threatening. To combat heat-related injuries, ORNL
will:
•	Provide water to all verification participants;
•	Establish a work regimen that will provide adequate rest periods;
•	Provide access to air-conditioned buildings;
•	Notify all workers of health hazards and the importance of adequate rest.
Some symptoms of heat-related injuries are pale clammy skin, sweating, headache, weakness, dizziness,
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and nausea. Signs of heat stroke include dry, hot, red skin, chills, and confusion. In the case of a
suspected heat-related injury, try to cool the person down and contact medical help.
9.13	Insect and Other Animal Stings and Bites
Building 5507 is located in a relatively secluded part of the Laboratory (see Figure 7-1). A
potential for insect and other animal stings or bites exists during the technology verification. Insect repellent
may be used to minimize insect bite hazards. In the event of snake or other large animal bite, the injury
should be immobilized and immediately reported to medical personnel.
9.14	Medical Support
A complete medical facility is located on-site in Building 4500 North. Medical help can be
summoned from any laboratory phone by dialing 9-1-1. The 911 system automatically contacts the Lab
Emergency Response Center and Emergency Communications Center, and Medical. Pulling a fire alarm
box will summon the fire department and the laboratory shift superintendent's office.
9.15	Environmental Surveillance
The Environmental Protection Officer will be responsible for surveying the site before, during, and
after the verification test. Appropriate personnel will be on-hand to assist all verification participants to deal
with any health or safety concerns.
9.16	Safe Work Practices
Each vendor will provide the required training and equipment for their personnel to meet safe
operating practice and procedures. The individual technology vendor and their company are ultimately
responsible for the safety of their workers.
The following safe work practices will be implemented at the site for worker safety:
Eating, drinking, chewing tobacco, and smoking will be permitted only in designated
areas;
Wash facilities will be utilized by all personnel before eating, drinking, or toilet
facility use;
PPE requirements (See Section 9.6) will be followed.
9.17	Complaints
All complaints should be filed with the ORNL technical lead. All complaints will be treated on an
individual basis and be dealt with accordingly.
9.18	Radiological Hazards
The PCB-contaminated samples that will be used in this verification test have been analyzed and
found not to be radioactive. However, if an issue concerning radioactivity would occur during the
verification ORNL-radiation procedures will be applied, where applicable.
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REFERENCES
[1]	EPA (U.S. Environmental Protection Agency). 1998. Environmental Technology Verification
Report: Electrochemical Technique/Ion Specific Electrode, Dexsil Corporation, L2000
PCB/Chloride Analyzer. EPA/600/R-98/109. U.S. Environmental Protection Agency,
Washington, D.C., August.
[2]	Maskarinec, M. P., C. K. Bayne, L. H. Johnson, S. K. Holladay, R. A. Jenkins, and B. A.
Tomkins. 1991. Stability of Explosives in Environmental Water and Soil Samples. ORNL/TM-
11770. Oak Ridge National Laboratory, Oak Ridge, Tenn., January.
[3]	EPA (U.S. Environmental Protection Agency). 1996. "Method 8082: Polychlorinated Biphenyls
(PCBs) by Gas Chromatography." In Test Methods for Evaluating Solid Waste: Physical/
Chemical Methods, Update II. SW-846. U.S. Environmental Protection Agency, Washington,
D.C., December.
[4]	EPA (U.S. Environmental Protection Agency). 1982. Test Method: The Determination of
Polychlorinated Biphenyls in Transformer Fluid and Waste Oils. EPA/600/4-81-045. U.S.
Environmental Protection Agency, Washington, D.C., September.
[5]	ORNL (Oak Ridge National Laboratory). 1998. Quality Management Plan for the
Environmental Technology Verification Program's Site Characterization and Monitoring
Technologies Pilot. QMP-X-98-CASD-001, Rev. 0. Oak Ridge National Laboratory, Oak
Ridge, Tenn., November.
[6]	Berger, W., H. McCarty, and R-K. Smith. 1996. Environmental Laboratory Data Evaluation
Genium Publishing Corp., Schenectady, N.Y.
[7]	Draper, N. R., and H. Smith. 1981. Applied Regression Analysis. 2nd ed. John Wiley & Sons,
New York.
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