United States
Environmental Protection
Agency
Office of Research and
Development
Washington DC 20460
EPA/540/R-95/517
August 1995
EnviroGard PCB Test Kit,
Millipore,

Innovative
Evaluation
Inc.

Technology
 Report

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                                          CONTACT
Jeanette Van Emon and Steve Rock are the EPA contacts for this report. Jeanette Van Emon is presently
with the new Characterization Research Division (formerly the Environmental Monitoring Systems
Laboratory) in Las Vegas, NV, which is under the direction of the National Exposure Research Laboratory
with headquarters in Research Triangle Park, NC.

 Steve Rock is presently with the new Land Remediation and Pollution Control Division (formerly the Risk
Reduction Engineering Laboratory) in the newly organized National Risk Management Research Laboratory
in Cincinnati, OH.

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                                            EPA/540/R-95/517
                                            August 1995
ENVIROGARD PCB TEST KIT, MILLIPORE, INC.

       INNOVATIVE TECHNOLOGY EVALUATION REPORT
   NATIONAL RISK MANAGEMENT RESEARCH LABORATORY
         OFFICE OF RESEARCH AND DEVELOPMENT
        U.S. ENVIRONMENTAlL PROTECTION AGENCY
                CINCINNATI, OHIO 45268
       NATIONAL EXPOSURE RESEARCH LABORATORY
         OFFICE OF RESEARCH AND DEVELOPMENT
        U.S. ENVIRONMENTAL PROTECTION AGENCY
               LAS VEGAS, NEVADA 39193
                                        Printed on Recycled Paper

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                                            Notice
The information in this document has been funded wholly or in part by the U.S. Envkonmental Protection
Agency (EPA) in partial fulfillment of Contract No. 68-CO-0047, Work Assignment No. 0-40, to PRC
Envkonmental Management, Inc. It has been subject to the Agency's peer and administrative review, and it
has been approved for publication as an EPA document  The opinions, findings, and conclusions expressed
herein are those of the contractor and not necessarily those of the EPA or other cooperating agencies.
Mention of company or product names is not to be construed as an endorsement by the agency.
                                                11

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                                             I.  •
                                            Foreword
        The U.S. Environmental Protection Agency is charged by Congress with protecting the Nation's land,
air, and water resources. Under a mandate of national environmental laws, the Agency strives to formulate and
implement actions leading to a compatible balance between human activities and the ability of natural systems
to support and nurture life. To meet this mandat
;, EPA's research program is providing data and technical
support for solving environmental problems today and building a science knowledge base necessary to manage
our ecological resources wisely, understand how pollitants affect our health, and prevent or reduce environmental
risks in the future.

        The National Risk Management  Researdh Laboratory is the Agency's center for investigation of
technological and management approaches for reducing risks from threats to human health and the environment.
The focus of the Laboratory's research program is oh methods for the prevention and control of pollution to air,
land,  water and subsurface resources; protection of water quality in public water systems ; remediation of
contaminated sites and ground water; and prevention and control of indoor air pollution. The goal of this research
effort is to catalyze development and implementation of innovative, cost-effective environmental technologies;
develop scientific and .engineering information needed by EPA to support regulatory and policy decisions; and
provide technical support and information transfer to ensure effective implementation  of environmental
regulations and strategies.

        This publication has been produced as part of the Laboratory's strategic long-term research plan.  It is
published and made available by EPA's Office of Research and Development to assist the user community and
to link researchers with their clients.

                                              i. Timothy Oppelt, Director
                                              Tational Risk Management Research Laboratory
                                                m

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                                              Abstract
This report describes the demonstration and evaluation of an immunoassay field screening technology designed to
determine polychlorinated biphenyl (PCB) contamination hi soil. The immunoassay technology was the EnviroGard
PCB Test developed by Millipore, Inc. The technology was demonstrated in Kansas City, Missouri, in August 1992,
by PRC Environmental Management, Inc. (PRC), under contract to the Environmental Protection Agency's (EPA)
Environmental Monitoring Systems Laboratory-Las Vegas (EMSL-LV).

The principal objective of the demonstration was to evaluate the technology for accuracy and precision at detecting
high and low levels of PCB in soil samples by comparing their results to those attained by a confirmatory laboratory
using standard EPA  analytical methods.  The technology also was qualitatively evaluated for the length of time
required for analysis, ease of use, portability, and operating cost.  Accuracy was also assessed through analysis of
performance evaluation (PE) samples, and  precision was further assessed by comparing the results  obtained on
duplicate samples. A secondary objective of the demonstration was to evaluate the specificity of the technology.  The
evaluation of specificity was performed by examining any problems due to naturally occurring matrix effects,
site-specific matrix effects, Aroclor sensitivity, and chemical cross reactivity. Information on specificity was gathered
from the developer, from the analysis of demonstration samples, and from a specificity study performed during the
demonstration.

This report was submitted in fulfillment of contract No.  68-CO-0047 by PRC, under sponsorship of the EPA. This
report covers a period from February 10, 1992, to August 31, 1992,  and work was completed as of February 28,
1993.
                                                    IV

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                                     Table of Contents
Section
Notice	
Foreword  	
Abstract  	
List of Figures	
ListofTables	
List of Exhibits  	
List of Abbreviations and Acronyms
Acknowledgments	
1   Executive Summary
2   Introduction	J.		......
       EPA's SITE Program and MMTP: An Overview		
              The Role of Monitoring and Measurement Technologies
              Defining the Process 	,	
              Components of a Demonstration	
       Demonstration, Purpose, Goals, and Objectives  		..'...
3   Predemonstration Activities	
       Identification of Developers	
       Site Selection	
       Selection of Confirmatory Laboratory and Method
       Operator Training	
       Sampling and Analysis  	
    Demonstration Design and Description ..
       Sample Collection	
       Quality Assurance Project Plan	
       Experimental Design	
              Statistical Analysis of Results
       Field Analysis Operations	
   Confirmatory Analysis Results	
       Confirmatory Laboratory Procedures
              Soil Sample Holding Times 	
              Soil Sample Extraction	
              Initial and Continuing Calibrations
              Sample Analysis	
              Detection Limits	
              Quality Control Procedures 	
.  iii
.  iv
. vii
. vii
.,vii
 viii
.  ix
  1 -f
.  1

.  3
.  3
.  3
.  3
.  4
.  4

.  6
.  6
.  6
.  7
.  7
.  7

.  8
.  8
.  9
 10
 10
 13

 14
 14
 14
 14
 15
 15
 15
 16

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                             Table of Contents (Continued)
Section
              Confirmation of Analytical Results	 16
                     Second Column Confirmation	 16
                     Gas Chromatographic and Mass Spectrometer Confirmation 	 16
              Data Reporting	 17
              Arociors Reported by the Confirmatory Laboratory	 17
       Data Quality Assessment of Confirmatory Laboratory Data	 17
              Accuracy	 17
              Precision	'•	•	 17
              Completeness	 18
       Use of Qualified Data for Statistical Analysis	 18

6   Millipore EnviroGard PCB Test	•	 19
       Theory of Operation and Background Information  	 19
       Operational Characteristics	 19
       Performance Factors	 22
              Detection Limits and Sensitivity	 22
              Sample Matrix Effects  	:	 23
              Sample Throughput	 23
              Drift	 23
       Specificity  	 24
       Intramethod Assessment	 26
       Comparison of Results to Confirmatory Laboratory Results		28
              Accuracy	 28
              Precision	•	 32
       Quantitative Evaluation	•	 32
              Theory of Operation and Background Information	 32
              Operational Characteristics	 •	 32
              Performance Factors	•	 32
              Specificity	• • • •	 35
              Intramethod Assessment	 37
              Comparison of Results to Confirmatory Laboratory Results 	 39

7   Applications Assessment	 41

8   References	 42
                                              VI

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                                             i

                                      List of Figures
Figure
6-1 Assessment of Semiquantitative EnviroGard PCB Test Data
6-2 Assessment of Quantitative EnviroGard PCB Test Data	
                                             Page
                                               31
                                               35
                                       List
 i
j
Table
f Tables
6-1 Semiquantitative Results for the Aroclor Specifbity Test	.".'.'	........
6-2 Semiquantitative Results for Laboratory and Field Duplicate Samples	
6-3 Comparison of Semiquantitative Data for EnviroGard PCB Test and Confirmatory Laboratory
6-4 Comparison of Quantitative Data for EnviroGar^l PCB Test and Confirmatory Laboratory
6-5 Quantitative Results for the Aroclor Specificity Test	!	
6-6 Quantitative Matrix Spike and Matrix Spike Duplicate Results  ......		
6-7 Quantitative Laboratory and Field Duplicate Sample Results	.......		
                                               25
                                               27
                                               29
                                               33
                                               36
                                               39
                                               40
                                      List of Exhibits
Exhibit

6-1 Assay Flow Chart,
                                               20
                                             | VII

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            List of Abbreviations and Acronyms
A1CO         Abandoned Indian Creek Outfall
CCAL         continuing calibration
CLP          Contract Laboratory Program
CMS          corrective measures study
CRQL         contract required quantitation limit
DOE          Department of Energy
DQO          data quality objective
ECD          electron capture detector
EMSL-LV      Environmental Monitoring Systems Laboratory-Las Vegas
EPA          Environmental Protection Agency
ERA          Environmental Research Associates
GC           gas chromatograph
ICAL          initial calibration
IDW          investigation-derived waste
ITER          Innovative Technology Evaluation Report
KCP          Kansas City Plant
pL            microliter
pg/kg         micrograms per kilogram
mg/kg         milligrams per kilogram
Millipore       Millipore, Inc.
mL           milliliters
MMTP         Monitoring and Measurement Technologies Program
MS           mass spectrometer
NRMRL       National Risk Management Research Laboratory
ORD          Office of Research and Development
OSWER       Office of Solid Waste and Emergency Response
PCB          polychlorinated biphenyl
PE           performance evaluation
PRC          PRC Environmental Management, Inc.
QA/QC        quality assurance/quality control
QAPP         quality assurance project plan
r2            correlation coefficient
RCRA         Resource Conservation and  Recovery Act
RFI           RCRA facility investigation
RPD          relative percent difference
SARA         Superfund Amendments and Reauthorization Act of 1986
SITE          Superfund Innovative Technology Evaluation
SOP          standard operating procedures
SOW         statement of work
TCL          Target Compound  List
TPM          technical project manager
UV           ultraviolet
                               viii

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                                         Acknowledgments
This demonstration and the subsequent preparation of this report required the services of numerous personnel from the
Environmental Protection Agency, Environmental Monitqring Systems Laboratory (Las Vegas, Nevada); Environmental
Protection Agency, Region 7 (Kansas City, Kansas); Mijlipore, Inc. (Bedford, Massachusetts); the U.S. Department of
Energy Kansas City Plant (Kansas City, Missouri); Alliedj-Signal, Inc. (Kansas City, Missouri); and PRC Environmental
Management, Inc.  (Kansas  City, Kansas; Cincinnati, Ohio; and Chicago, Illinois). The cooperation and efforts of these
organizations and personnel are gratefully acknowledged.

Additional information concerning the demonstration described in this report can be obtained by contacting Mr. Lary Jack,
the Environmental Protection Agency, Environmental Monitoring Systems Laboratory technical project manager, at (702)
798-2373, or Mr.  Eric Hess, the PRC Environmental Management, Inc., project manager, at (913) 573-1822.
                                                  I            •
Additional information on the innovative technology  described in this report can be obtained by writing the developer,
Millipore, Inc., at Mail Stop E-5A,' 80 Ashby Road, Bedford, Massachusetts  01730, or by telephoning l-800-225-138o!
                                                   IX

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                                               Section 1
                                        Executive Summary
     This innovative technology evaluation report (ITER)
 presents information on the demonstration and evaluatiok
 of the EnviroGard PCB Test produced by Millipore, Inc.
 (Millipore).  The EnviroGard PCB Test is designed tj>
 detect polychlorinated biphenyl (PCB) contamination in
 soil.   The  demonstration was  conducted by  PRC
 Environmental Management, Inc. (PRC), under contracjt
 to  the  Environmental  Protection Agency's  (EPAj)
 Environmental Monitoring  Systems Laboratory—LaS
 Vegas (EMSL-LV).  The demonstration was developed
 under the Monitoring and Measurement Technologies
 Program (MMTP)  of  the  Superfund  Innovativi
 Technology Evaluation (SITE) Program.
     The EnviroGard PCB Test was demonstrated
evaluated hi August  1992 at a site hi Kansas  City!
Missouri.  The demonstration of the test was done in
conjunction with  the  demonstration of three  other
innovative field screening technologies: the Clor-N-Soil
PCB Test Kit and the L2000 PCB/Chloride Analyzer!
both manufactured by the Dexsil Corporation, and  the
Field  Analytical  Screening  Program PCB  Method
developed under the Field Investigative Team Contracj,
with the EPA Superfund Program. The demonstratioii
results  for these other  technologies  are  presented hi
separate ITERs.                                   !
                                                  i
     The EnviroGard PCB Test is designed to quick!}}
provide semiquantitative results for PCB concentration^
hi soil samples. The technology can be customized td
report  specific  results  over  a particular range  of
concentrations.  As part of the SITE demonstration, the
technology also was evaluated for its ability to produce
quantitative results.

     The EnviroGard  PCB Test  is an immunoassayj
system  that  uses  polyclonal  antibodies  to produce
compound-specific reactions to PCBs allowing  theuj
detection and  quantitation.   An anti-PCB antibody is
fixed to the inside wall of a test tube to bind  PCBi
compounds.  An enzyme conjugate containing a  PCBi
derivative labeled with horseradish peroxidase is added
to the test tube where it  competes with  PCBs for!
 anti-PCB antibody binding  sites.   Reagents  are  then
 added to the test tube where they react with the enzyme
 conjugate, causing a color change.  Results can be
 estimated by observing the degree of color change.  For
 a more precise quantitative measurement of  the PCB
 concentration in the sample, the color of the solution can
 be compared to Aroclor standards using a differential
 photometer.

     The EnviroGard PCB  Test is portable,  easy to
 operate, and useful under a variety of site conditions.
 The differential photometer requires electricity but can
 be operated using a rechargeable battery.  Reagents must
 be kept refrigerated.

     Calibrating the technology  was initially  difficult
 because  of  the small volume of Aroclor standards
 required. As the operator gained experience hi using the
 EnviroGard PCB Test, the calibrations became easier.

     The EnviroGard  PCB Test costs $1,495, which
 includes the differential photometer and other equipment
 needed to run the test.  Additional disposable equipment
 and reagents  needed to  perform  12  analyses  cost
 $253.  The differential photometer required to obtain
 quantitative results costs $799.

    The developer reports that the detection limit is
 3.3  milligrams  per kilogram  (mg/kg)  for  Aroclor
 1248.   This was the  detection limit used during the
 demonstration.  The detection limit differs depending on
 the Aroclor.  The highest number of samples analyzed hi
 an 8-hour day was 52; the average number analyzed per
 8-hour day was 25.

    Results produced  with the EnviroGard PCB  Test
may be affected by the cross-reactivity of compounds
other than PCBs to the anti-PCB antibody binding sites.
The developer has evaluated a number of compounds to
determine their levels of cross-reactivity, although this
evaluation was  not independently assessed during this
demonstration.

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    PRC evaluated  field  and  laboratory  duplicate
samples to determine the technology's precision in the
semiquantitative mode.  Thirty-seven duplicate sample
pairs were used in this semiquantitative evaluation.  Of
these 37 duplicate sample pairs, the EnviroGard PCB
Test produced the same results 35 times.  One laboratory
duplicate and one field duplicate did not agree with their
respective soil  sample results.  Based on this data, the
precision of the EnviroGard PCB Test was found to be
95 percent.  This meets the demonstration's criteria for
acceptable precision.

    PRC evaluated  the accuracy of the test in its
semiquantitative mode by comparing its data to that of
the confirmatory laboratory. This comparison showed
that 71 percent of the time the technology was correct.
The other 29 percent of the time, the technology gave
false positive results.  It never gave a false negative
result. The technology is conservative when used in the
semiquantitative mode. Using an absolute definition of
accuracy, it was  accurate only 71 percent of the tune.
The production of false positive results, though, may not
affect  its use  in environmental  assessments.  False
positive  results  will  incorrectly  label soil  as being
contaminated above a test's threshold level.  At worst,
this would lead to the overestimation of contaminated
area or volume.

    To   assess  this technology's  precision in  a
quantitative mode,  PRC evaluated the results produced
from the analysis of laboratory and  field duplicate
sample  pairs.    The  EnviroGard  PCB  Test  had
27 duplicate sample pairs in which both a sample and its
duplicate had positive results. PRC used the data from
the duplicate sample analyses  to establish precision
control limits.  The  control limits were set  at 0 and
91 percent.  All but two  of the  27 relative percent
differences (RPD) fell within the  control limits.  This
equates to a precision of 93 percent, which is below the
95  percent  precision  deemed acceptable  for  this
demonstration.   However,  the technology's precision
would have exceeded this threshold  if only one more
duplicate sample pair had fallen within the control limits.
When PRC used the Dunnett's Test to compare the
RPDs between the EnviroGard PCB Test's data and the
confirmatory  laboratory's  data,  a  probability  of
97.5 percent resulted.  This indicates that the technology
is as precise as the confirmatory laboratory.

    PRC used linear regression analysis to assess the
accuracy of the technology in its quantitative mode when
compared to the confirmatory laboratory's data.  The
regression of 83 matched pairs of positive sample results
defined a correlation coefficient (r2) of 0.87, indicating
that  a relationship did exist between  the two data sets.
The  regression  line  calculated had  a  y-intercept of
17.8 mg/kg and a slope of 0.76. These results indicate
that  the results from this technology are not accurate.
Although the technology was found to be inaccurate hi
its  quantitative  mode,  the results  produced by the
technology  were  linear,  indicating  that the  results
can   be  corrected  mathematically.    If   10  to
20 percent of the soil samples are sent to a confirmatory
laboratory,  then the results  from  the other 80 to
90 percent can be  corrected.  This  could result in a
significant savings in analytical costs.  The Wilcoxon
Signed Ranks Test was used to verify these results.  It
indicated,  at a 95  percent confidence level,  that the
EnviroGard PCB Test's data was significantly different
from that  of the  confirmatory  laboratory.    This
confirmed  the linear regression analysis and indicated
that  the EnviroGard PCB Test's data was not accurate.

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      !
  Section 2
Introduction
     This ITER  summarizes the procedures used  to|
 demonstrate the  EnviroGard PCB Test,  discusses the)
 results   of  the  demonstration,  and  evaluates  the
 effectiveness and possible uses of the test at various
 hazardous  waste  sites.    The primary  goal of the
 demonstration was  to  evaluate the  technology and  to
 provide Superfund decision makers with information on its
 performance and cost effectiveness.

 EPA's SITE Program and MMTP:
 An Overview

    At the  time of the  Superfund Amendments and!
 Reauthorization  Act of 1986  (SARA),  it  was  well
 recognized that the environmental cleanup problem needed
 to be attacked  with new and better methods.   The
 Superfund Innovative Technology Evaluation  Program
 (SITE) , therefore, was created to fulfill a requirement of
 SARA that the EPA address the potential of alternative  or
 innovative technologies. The EPA made this program a
joint  effort  between the  Office  of Solid Waste and
 Emergency  Response  (OSWER)  and the Office  of
 Research and Development (ORD). The SITE Program
 includes four component programs:

    •   The  Demonstration Program  (for remediation
        technologies)

    •   The Emerging Technology Program

    •   The  Measuring   and  Monitoring   Program
        (MMTP)

    «   The Technology Transfer Program

    The  largest  part   of the  SITE Program,  the
Demonstration Program, is concerned with  treatment
technologies and is administered by  ORD's National Risk
Management  Research  Laboratory     (NRMRL)  in
          Cincinnati,  Ohio.   The  MMTP  is  administered by
          EMSL-LV. The MMTP is concerned with monitoring and
          measurement technologies  that identify,  quantify, or
          monitor changes in contaminants occurring at hazardous
          waste sites or that are used to characterize a site.

             The  MMTP  seeks  to  identify and  demonstrate
          innovative technologies that may provide a less expensive,
          better, faster, or safer means of completing this monitoring
          or characterization. The managers of hazardous waste
          sites are often reluctant to use any method, other  than
          conventional ones, to generate critical data on the nature
          and extent of contamination.  It is generally understood
          that the courts recognize data generated with conventional
          laboratory methods; still, there is a tremendous need to
          generate data more cost effectively.  Therefore, the EPA
          must  identify  innovative  approaches,  and  through
          verifiable  testing of the technologies  under the SITE
          Program,  to ensure that the innovative technologies are
          equivalent or better than conventional technologies.

          The  Role of  Monitoring and Measurement
          Technologies

             Effective measurement and monitoring technologies
         are  needed  to  accurately  assess   the  degree  of
         contamination; to  provide data  and  information to
         determine  the effects of those contaminants on public
         health and the environment; to supply data for selection of
         the most appropriate remedial action; and to monitor the
         success or failure of a selected remedy. • Thus, the MMTP
         is broadly concerned with evaluating screening (including
         remote sensing),  monitoring, and analytical technologies
         for all media.

             Candidate  technologies may come from within the
         federal government or from the private sector. Through
         the program, developers are provided with the opportunity
         to rigorously evaluate the performance of their

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technologies.   Finally,  by distributing the results and
recommendations of those evaluations, the market for the
technologies is enhanced.

Defining the Process

    The innovative  technology  demonstration  process
begins by canvassing the EPA's 10 regional offices (with
input by OSWER and ORD) to  determine their needs.
Concurrently, classes of technologies are identified. An
ideal match is made when there is a single clear need by
EPA's regions  and a reasonable number of innovative
technologies  that  can address  that  need.     The
demonstrations are designed to  judge each technology
against existing stand_ards and not one against the other.

    The demonstration is designed to provide for detailed
quality assurance and quality control (QA/QC).  This is
done to ensure that  a  potential user  can evaluate the
accuracy, precision, representativeness, completeness, and
comparability  of  data  derived  from  the  innovative
technology.  In addition, a description of the  necessary
steps and  activities associated  with  operating the
innovative  technology is prepared. Cost data, critical to
any  environmental  activity, is   generated during the
demonstration  and allows  a potential  user to  make
economic comparisons.  Finally, information on practical
matters  such as operator training  requirements, detection
levels, and ease of operation are reported.   Thus, the
demonstration report and other  informational materials
produced by the MMTP  provide a real-world comparison
of that technology to traditional technologies.  With cost
and performance data, as well as "how to" information,
users can  more comfortably determine whether a new
technology better meets  their needs.

Components of a Demonstration

    Once  a decision has been made to demonstrate
technologies to meet a particular EPA need, the MMTP
performs  a number  of activities.  First, the  MMTP
identifies potential participants and determines whether
they are interested in participating.  Each developer is
advised  of  the  general  nature  of  the   particular
demonstration and is provided with information common
to all MMTP demonstrations.  Information is sought from
each developer about its  technology to ensure  that the
technology meets the parameters of the demonstration.
Then, after evaluation of the information, all respondents
are  told  whether  they have been accepted into the
demonstration  or  not.   While  participants  are  being
identified, potential sites  also are identified, and basic site
information is  obtained.  These activities  complete the
initial component of an MMTP demonstration.
    The next component, probably the most important, is
the development of plans that describe how various aspects
of the demonstration will be conducted.  A major part of
the  EPA's  responsibility  is  the  development of a
demonstration plan,  a quality  assurance project plan
(QAPP),  and a health and safety plan.  While the EPA
pays for and  has the primary  responsibility  for these
plans,  each is developed with  input from all of  the
demonstration's  participants.    The plans define how
activities will be conducted and how the technologies will
be evaluated.  MMTP also provides each developer with
site information and often predemonstration samples so die
developer can maximize the field performance of its
innovative technology. Typically,  the developers tram
demonstration personnel to ensure each operator is trained
appropriately.  This also ensures  mat potential users have
valid information on training requirements and the types of
operators who typically use a technology successfully.

    The  field  demonstration itself is the shortest part of
the process.   During the field demonstration,  data is
obtained  on cost, technical effectiveness (compared to
standard methods),  and limiting factors.  In addition,
standardized field methods are developed and daily logs of
activities and observations (including photos or videotape)
are produced.   The EPA is also responsible  for  the
comparative, conventional method analytical costs and the
disposal   of  any  wastes  generated  by  the  field
demonstration.

    The  final component of an MMTP demonstration
consists of reporting the results and ensuring distribution
of demonstration information.  The primary product of the
demonstration is an  ITER,  like  this one,  which is
peer-reviewed and distributed as part of the technology
transfer responsibility of the MMTP.  The ITER fully
documents  the  procedures  used  during  the  field
demonstration, QA/QC results, the field demonstration's
results, and its conclusions.  A separate QA/QC  data
package  also  is  made available for those interested in
evaluating the demonstration in greater depth. Also, short
technical  summaries  are  prepared to summarize  the
demonstration results, and to ensure rapid and  wide
distribution of the information.

    Each developer  is  responsible  for providing  the
equipment or technology  product  to be demonstrated,
funding its own mobilization, and training EPA-designated
operators.   The MMTP does not provide any funds to
developers  for  costs associated with  preparation of
equipment for demonstration or for development, and it
does not cover the costs  developers incur to demonstrate
their technologies.

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Demonstration Purpose, Goals,
and Objectives
    During this demonstration, the EnviroGard PCB Test
was evaluated for its accuracy and precision in detecting
high and low levels of PCBs in soil samples, and the
effects, if any, of matrix interferences on the test.  The
accuracy   and    precision   of   the    test   was.
statistically compared to the  accuracy  and precision
attained in a conventional, fixed laboratory using standard
EPA analytical methods. The EnviroGard PCB Test also
was qualitatively evaluated for the length of time required
for analysis, ease of use, portability, and operating cost.

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                                              Section 3
                                  Predemonstration Activities
    Several predemonstration activities were conducted
by  EMSL-LV,  PRC, and  the  other demonstration
participants.   These activities  included  identifying
developers, selecting the demonstration site, selecting the
confirmatory  laboratory   and  analytical  method,
conducting   operator  training,   and   conducting
predemonstration sampling and analysis.  This section
summarizes these activities and presents the results of
the predemonstration sampling and analysis.

Identification of Developers

    EMSL-LV identified the EnviroGard PCB Test as
one of four technologies showing promise for use in
PCB field screening.  After a review of available data on
these four technologies, EMSL-LV concluded that they
warranted evaluation under the MMTP.

Site Selection

    The following  criteria  were used to select  a
hazardous waste site suitable for the demonstration:

    •   The four technologies had to be tested at a site
        with a wide range of PCB contamination.

    •   Contaminant concentrations had  to be  well
        characterized and documented.  Thorough site
        background information was needed so that a
        demonstration sampling plan could be designed
        with  a  high degree of confidence mat the
        desired range of PCB concentrations would be
        present in samples.

    •   The  site  had  to  be  accessible  so   that
        demonstration activities could be conducted
        without interfering  with  other  planned  site
        activities.

    Based on these criteria, the Abandoned Indian Creek
Outfall (AICO) site at the Department of Energy (DOE)
Kansas City Plant (KCP) was selected as the location for
this  demonstration.   The soil  at  the  AICO site  is
contaminated with a wide range of PCB concentrations.
PCB levels range from not detected at a concentration of
0.16 mg/kg to 9,680 mg/kg.  DOE has conducted
numerous investigations at the site, including a Resource
Conservation  and  Recovery  Act  (RCRA)  facility
investigation (RFI) and corrective measures study (CMS)
in 1989 (DOE 1989). PCB concentrations at the AICO
site are well documented, which made possible collecting
samples with a wide range of PCB concentrations.

    The DOE KCP is located about 20 miles south of
downtown Kansas City, Missouri, at the northeast corner
of Troost Avenue and 95th Street. The facility is owned
by the government and operated by Allied-Signal, Inc.,
for DOE.   The plant has been used  since  1949  to
manufacture nonnuclear components for nuclear weapons
systems.  The facility occupies more than 300 acres and
includes three main buildings and numerous outbuildings
with over 3 million square feet under roof. Land around
the plant is primarily occupied by suburban residential
and commercial developments (DOE 1989).

    The AICO site is located immediately south of the
DOE KCP between 95th Street and Bannister Road. The
site is located hi a former channel of Indian Creek and
is the former location of a storm water outfall (Outfall
002), which discharged from KCP into the creek.  In the
early 1970s,  Indian Creek was rerouted as part of a
flood protection project and the construction of Bannister
Road.  When the creek was rerouted, the storm water
outfall also was rerouted by extending a box culvert
from the former outfall to the new creek channel. The
outfall now discharges into Indian Creek about 500 feet
south of the AICO site. The former creek channel in the
AICO area was covered with about 10 feet of fill (DOE
1989).

     PCBs are the  only significant contaminants at the
site.   During the  RFI  and  CMS,  samples from
12 borings were analyzed for priority pollutants other
than PCBs.   Only one of  these  borings contained
non-PCB priority pollutants.  This boring was  found to

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 contain  several  base  neutral  organics,  including
 anthracene, fluoranthene, pyrene, and chrysene.  It is
 believed that this sample included a piece of asphalt from
 the material used to fill the old creek channel and tjiat
 the presence of these compounds was not the result! of
 DOE KCP discharges through Outfall 002 (DOE .1989).

     According to logbooks kept by Allied-Signal, Int.,
 when boreholes were drilled during the investigationsjof
 the AICO site, the former Indian Creek channel!is
 overlain  by  7 to 15  feet of fill material composed
 primarily  of  mottled clays.    Shale and  limestojne
 fragments, wood, asphalt, and concrete slag up to 4 feet
 wide are found in the fill material. Near the surface, jip
 to 20 percent of the fill is composed of organic matter,
 such as roots,  peat, and wood (DOE 1989).         )

     Sediments overlying bedrock consist of soft, dark
 brown to gray, homogenous, medium to high plasticity,
 moist clayey silt with traces of fine sand. This material
 varies in depth from 7 to 15 feet and appears to have Idw
 permeability  (DOE  1989).  The aquifer of concern
 beneath the AICO site is the shallow groundwater lyipg
just above bedrock.                              I
Selection of Confirmatory Laboratory  and
Method
      ...          •  •                       .    j
    EPA Region 7 Laboratory personnel selected one
laboratory  participating  in  the  Contract .Laboratory
Program (CLP) to perform .the confirmatory analysis of
samples  for this demonstration.   All samples were
analyzed using the method described in the  CLJP
1990 Statement of Work (SOW) for analyzing PCBs arid
pesticides.  The EPA Region 7 Laboratory conducted! a
 Level II data review of the confirmatory laboratory's
 data.

 Operator Training

     The EnviroGard PCB Test was demonstrated by
 PRC field personnel.  Prior to the demonstration, the
 PRC operator was trained in the use of the technology.
 This training included a review of operating procedures
 and instructions provided by Millipore and informal field
 training conducted by Millipore  at the start of the
 demonstration.    Training  was  equivalent to  that
 recommended   by   Millipore   for    actual   site
 characterization projects.

 Sampling and Analysis

     In  May  1992, PRC  prepared a predemonstration
 sampling plan (PRC 1992a), and on July 14, 1992, PRC
 collected predemonstration soil samples from areas at the
 AICO site previously identified as containing high,
 medium, low, and not detected concentrations of PCBs.
 These samples were split into replicates. One replicate
 of each sample was submitted to Millipore, and the
 confirmatory laboratory analyzed one replicate.

    The predemonstration sampling was conducted so
 that Millipore could refine its technology and revise its
 operating  instructions,  if  necessary,  before   the
 demonstration.   The sampling  also allowed potential
 matrix effects or interferences to be evaluated prior to
 the demonstration.  The  principal finding from  the
predemonstration sampling was that the soil at the AICO
 site was more clayey than expected.   The high clay
content  of  the  soil made homogenizing the  samples
difficult (see Section 4).

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                                             Section 4
                           Demonstration Design and Description
    This  section  describes  the  sample  collection
procedures and the experimental design used to evaluate
the EnviroGard PCB Test. This innovative technology
was evaluated  in conjunction with three  other field
screening technologies that also analyze PCBs in soil.
The demonstration design and  description, and  the
experimental design described  in  this  section,  are
common to all four evaluations.  The four evaluations
also shared'a single demonstration plan and QAPP. Key
elements  of the QAPP (PRC 1992b), field analysis
operations,  and  data  management activities  are
summarized in this section.

Sample Collection

    For the demonstration, 112 soil samples and 32 field
duplicate samples were collected from the AICO site.
Each sample was thoroughly homogenized and then split
into six  replicate samples.  One replicate from each
sample was submitted to the confirmatory laboratory for
analysis using the CLP 1990 SOW  method. A second
replicate  was submitted  to  EMSL-LV for separate
analysis  at the request of the EPA technical  project
manager  (TPM),  although  the  data  generated by
EMSL-LV was not used in this demonstration.  A third
replicate was analyzed in the field using the EnviroGard
PCB Test. The remaining replicates were analyzed hi
the field using the three other technologies described hi
separate ITERs.

     Samples were collected using  a drill rig to reach
areas of the AICO site that, based on data from past
investigations,  exhibited   a  wide  range  of PCB
concentrations.  All samples were collected by PRC
using  the  sample  collection  and  homogenization
procedures specified in the sampling plan (PRC  1992b).
All PRC  field  activities   also  conformed  with
requirements hi the health and safety plan prepared for
this demonstration (PRC 1992b).

     Samples were collected from areas known to exhibit
PCB concentrations ranging from  not detected (at a
concentration of 0.16 mg/kg) to 9,680 mg/kg. Most of
the samples  were  collected  from  areas  previously
identified  as containing  PCBs in the not detected to
100 mg/kg range, for two reasons.  First, this range
encompasses typical regulatory thresholds  for PCBs,
such as the 10 mg/kg level for cleanups hi unrestricted
access areas and the 50 mg/kg level for cleanups hi
industrial  areas.   Second, most of the  four  field
screening  technologies  demonstrated,  including  the
EnviroGard PCB Test,  were designed primarily  for
operation hi this range.

    Samples were also collected from areas previously
identified as containing PCBs at concentrations ranging
from 100  to 1,000 mg/kg, and from areas previously
identified as containing PCBs at concentrations between
1,000 and  10,000 mg/kg. These samples were analyzed
to  evaluate  the  abilities of the  field  screening
technologies to monitor PCBs hi higher concentrations as
well as hi the average range.  After collection,  soil
samples were placed hi plastic bags and  thoroughly
homogenized.  Samples  were then split and placed hi
sample  containers.    Samples  to  be  submitted  for
confirmatory laboratory analysis were placed in 8-ounce,
wide-mouth glass jars with Teflon-lined lids.  Samples
for submittal to EMSL-LV and for analysis by the field
screening   technologies   were  placed  hi 4-ounce,
wide-mouth glass jars with Teflon-lined lids.

    Homogenization of the samples  was monitored by
adding a small amount of powdered uranine, the sodium
salt of fluorescein dye (fluorescein), to each soil sample.
Homogenization was then  performed.   PRC  then
examined each sample under an ultraviolet (UV) lamp in
a portable darkroom.  Because fluorescein fluoresces
under UV light,  PRC  was  able to ensure   that
homogenization was complete.  While  under the  UV
light, PRC sliced each sample hi a minimum of  five
different   places  and  examined  each   slice  for
fluorescence.  If any of the slices did not contain signs
of fluorescence, then homogenization  of  the sample
continued and the examination process was repeated.

-------
  The use of small amounts of fluorescein was found not
  to interfere with sample analysis for any of the field
  screening   technologies,  nor  for  the  confirmatory
  laboratory.                                      >
               <-  .  •         '                  •   |
      After confirmatory laboratory results were received,
  PRC used  the results from samples and their respective
  field duplicate samples to statistically determine whether
  the homogenization efforts were successful.  Because the
  duplicate samples were collected as splits, the expectjed
  difference between a sample and its duplicate was zero.
  This assumes that there was perfect homogenization and
  that there  was no  difference introduced by  analytical
  error.  Using a matched pair  Student's t-test, it w;as
  possible to determine if  the mean of the differences
  between  the  samples   and   their  duplicates  was
  significantly different  from  zero at  a  95 percent
  confidence  level.   The matched pair Student's t-test
  showed that this mean was  not significantly different.
  Therefore,  though the results of a few pairs of samples
  and duplicates seem to  indicate  that homogenization
  could have been better,  overall the homogenization
 technique used was  highly effective.                ]
                                                  I
     To  apply the matched pair Student's t-test, it wjis
 necessary to have a normally distributed data population.
 The  differences  between  confirmatory  laboratory
 samples and their respective duplicates  were statistically
 evaluated and  found to be normally distributed.  Tw,o
 data point outliers were noted in the frequency plot. The
 matched pan-  Student's  t-test, however,  was found
 acceptable even when the outliers  were included hi the
 data set.                                  • .       j
                                                 . I
     The   statistical  analysis   indicates  that  the
 homogenization was  acceptable, but even at a 95 percent
 confidence level, a few anomalous duplicate results can
 exist in  a data set without the  analysis being greatly
 affected.  For  example, a single pair  of samples witp
 high RPDs  relative  to  the population's  mean RPD  is
 masked  and does not  affect the  overall  assessment.
 Therefore,  even with a  statistical   assessment that
 indicates  overall effective sample homogenization,  ja
 limited number of poorly homogenized samples may
 have been included hi the demonstration.  The analysis
 of such data could produce limited cases of inaccuratk
 data. For this reason, a large number of samples werp
 collected and analyzed to prevent any anomalous sampleSs
 from affecting the overall results.                   j
                                                  i
 Quality Assurance Project Plan

    To ensure  that  all activities associated with this
demonstration met demonstration objectives, a QAPP
was prepared (PRC  1992b).  The QAPP, which was
incorporated into the demonstration plan, defined project
  objectives,  how those objectives would be achieved,
  data quality objectives (DQO),  and the steps taken to
  ensure that these objectives were achieved.    All
  demonstration participants were given the opportunity to
  contribute  to  the  development of the  QAPP,  and
  ultimately, all participants agreed to its content.

      The primary purpose of the QAPP was to outline
  steps to be taken to ensure that data resulting from the
  demonstration was of known quality and that a sufficient
  number of critical measurements were taken.  Based on
  the EMSL-LV SOW, this demonstration is considered a
  Category H project.   The  QAPP addressed the  key
  elements  required for Category II  projects prepared
  according to guidelines hi "Preparing Perfect Project
  Plans"  (EPA  1989) and  "Interim Guidelines  and
  Specifications for Preparing Quality Assurance Project
  Plans" (Stanley and Verner 1983).

     For sound conclusions to be drawn on the four field
  screening technologies,  the data obtained  during  the
  demonstration had to be  of known quality.  For  all
 monitoring and  measurement activities conducted  for
 EPA, the agency requires that  DQOs be established
 based on how the data will  be used. DQOs must include
 at   least    five   indicators   of   data   quality:
 representativeness,    completeness,    comparability,
 accuracy,  and precision.   Each  of these indicators is
 discussed  in more detail below.   The success  of  the
 demonstration required  that DQOs be  met by  the
 confirmatory  laboratory.     Some  DQOs   for  the
 confirmatory laboratory were indicated  in  the CLP
 1990 SOW, and others were derived from data generated
 while using  the  method.   It was  critical  that  the
 confirmatory laboratory analyses be sound and within
 CLP 1990 SOW method specifications so that the data it
 generated could be compared to that obtained by the
 technologies.      High    quality,    well-documented
 confirmatory  results  were essential  for  making this
 comparison.

    Representativeness refers to the degree to which the
 data accurately and precisely represents the condition or
 characteristic of the parameter represented by the data
 (Stanley and  Verner 1983).   In this demonstration,
 representativeness was ensured by executing a consistent
 sample   collection,  homogenization,   and  handling
program. Representativeness also was ensured by using
each technology at its optimum capability to provide
results that represented the most  accurate and precise
measurements it was capable of achieving.

    Completeness refers to the amount of data collected
from a measurement process compared to the amount  •
that was expected to be obtained (Stanley and Verner
1983).  For this demonstration, completeness refers  to
                                                  i  9

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the proportion of valid, acceptable data generated using
each of the technologies and the confirmatory laboratory.
The completeness objective for each technology during
this demonstration was 90 percent, which was achieved.

    Comparability refers to the confidence with which
one data set can be compared to another (Stanley and
Verner 1983).  The main focus of this demonstration
was to compare data generated from the EnviroGard
PCB Test and the other technologies with confirmatory
laboratory results using the  experimental design and
statistical methods discussed  in Section 4. Additional
QC for comparability  was achieved by analyzing QC
samples, blanks, and Aroclor standards, and by adhering
to standard EPA  analytical methods and standard
operating procedures (SOP) for preparing samples and
operating instruments.

    Accuracy  refers  to the difference  between  the
sample result and the reference or true value for the
sample. Bias, a measure of the departure from complete
accuracy, can be caused by instrument calibration, loss
of  analyte  in  the  sample'  extraction   process,
interferences, and systematic contamination or carryover
of analyte from one sample to  the next.   During this
demonstration, accuracy was measured by making the
statistical  comparisons discussed under Experimental
Design in this section.

     Precision refers to the degree of mutual agreement
 among individual measurements and provides an estimate
 of random error.  Precision for this  demonstration was
 measured by comparing the RPDs of samples  and their
 duplicates  to  control  limits established through the
 statistical methods detailed under Experimental Design
 in this section.

 Experimental Design

     The primary objective of the demonstration was to
 evaluate the efficiency of the EnviroGard PCB Test and
 three   other   technologies   at  determining  PCB
 contamination in soil.  This evaluation included defining
 the precision, accuracy, cost, and range of usefulness for
 each of these technologies. This objective also included
 determining the DQOs that each technology was capable
 of achieving. An additional objective was  to evaluate the
 specificity of each technology to different Aroclors.

     Accuracy  and precision were the most  important
 quantitative factors  evaluated,  particularly  for PCB
 concentrations near 10 mg/kg, a common cleanup goal.
 A significant part of PRC's  statistical evaluation was to
 evaluate these factors.
    The cost of using each field screening technology
was another important factor. Costs include expendable
supplies,  nonexpendable  equipment,   labor,   and
investigation-derived waste (IDW) disposal.  These costs
were tracked during the demonstration. Although batch
analysis of samples can have major effects on per sample
costs,  the number  of  samples  collected  for  this
demonstration were within the range of a normal site
investigation.    Similar-sized sample batches  were
analyzed by each of the field screening technologies.

    Many analytical techniques can have significant
operator  effects  in which individual differences  hi
technique have a  significant effect on  the numerical
results. To reduce the potential impact of measurement
variation, PRC used a single operator  for each field
screening  technology  and accepted that the  error
introduced   by   operator  effect  would   not   be
distinguishable from error inherent in the various field
screening  technologies.    This  policy  was  selected
because  it approximates ordinary field conditions in
which only one screening method is typically used.

     All analytical  methods have a specific usable range
with lower and upper limits. The usable range for each
field screening technology was determined by comparing
results from  each technology  to  those  from the
confirmatory laboratory.  Statistical analysis of these
results were then used to identify the contaminant range
in which results from each technology were comparable
to the confirmatory laboratory result.

     The Aroclor expected to be found at the AICO site
 was Aroclor 1242, which is a common PCB.  However,
 there  are other  common Aroclors  as  well.   In  the
 planning stages of this demonstration,  interest was shown
 in  the  cross-reactivity between Aroclors  for each
 technology.   To assess this factor, cross-reactivity for
 each technology was evaluated through the use of matrix
 spikes for each of the seven Aroclors (1016, 1221, 1232,
 1242, 1248, 1254, and 1260) typically analyzed using
 standard EPA analytical methods.  This information was
 then  used  to  determine  the   sensitivities  of  the
 technologies to each Aroclor.

 Statistical Analysis of Results

     This demonstration required comparisons of various
 groups of data.  Sample results from each technology
 were statistically compared to duplicate sample results
 and other QA/QC sample results.   These  are called
 intramethod comparisons.  The  sample  results, also,
 were statistically compared to the results from the
 confirmatory laboratory, which were  considered as
  accurate and precise as possible. Finally, in some cases,
  the precision obtained by a technology was statistically
                                                     10

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  compared to the precision obtained by the confirmatory
  laboratory.

      All of the statistical tests used for this demonstration
  were stipulated hi the demonstration plan, which vfas
  approved  hi  advance   of data  collection  by  [all
  demonstration participants (PRC 1992b).  Also stipulated
  hi the demonstration plan was that all sample pairs that
  included a not detected result would be  removed from
  data sets.   PRC felt that the  variance  introduced (by
  eliminating these data pairs would be less than, or no
  more than equal to, the variance introduced by giving
  not detected results an arbitrary value.
     In  cases  where  field  duplicate  samples  were
 collected, the demonstration plan stated that the results
 of the two duplicates would be averaged and this average
 used in subsequent statistical analysis.  PRC followed
 this guideline, as well. .In this way, samples were not
 unduly weighted in the statistical analyses.          j
     The intramethod comparisons involved a statistical
 analysis of RPDs.  First, the RPDs of the results for
 each sample pair,  hi which both the sample and its
 duplicate were found to contain PCBs, were determine*!.
 The equation below was used to calculate the RPDs:
           RPD  =
           where
                    (R, + RJ/2
                                    100
              RPD = relative percent difference.
              R, = initial result.
              R, = duplicate result.
                                                 ' i
     Acceptable RPD values for field duplicate data are
difficult to assess.  These ranges are rarely published for
organic parameters and are mainly  dependent on the
heterogeneity  of  contaminant  distribution,  sample
collection activities, and analytical precision.  For this
demonstration, acceptable RPD values for field duplicate
data were established by determining an upper control
limit using guidance stated in SW-846 Method 8000.
Because  the  technologies being demonstrated  wei}e
themselves being assessed, the control limits used were
calculated from data provided during  this investigation.
To determine the upper  control limit,  the standard
deviation   of  the  RPDs  was  calculated  for  eacji
technology. This standard deviation was then multiplied
by two and added to its respective mean RPDs.  This
established the upper control limit for the technology1.
Because an RPD of zero would mean that the duplicate
samples matched their respective samples perfectly, zero
was used as the lower control limit.  This resulted hi a
  large  range of acceptable values.  Because duplicate
  analyses seldom match perfectly, even for established
  technologies, all samples that fell  within  the  control
  limits were considered acceptable.  PRC determined that
  if at least 95 percent of the duplicate  samples fell within
  these  control  limits,  the technology had  acceptable
  precision.

      Each  field screening  technology's   data  was
  compared  to  the  confirmatory  laboratory data  to
  determine its'accuracy. This comparison involved three
  statistical  methods:   linear regression analysis,  the
  Wilcoxon Signed Ranks Test, and the Fisher's Test.

     Linear  regression   was   calculated  for   the
  technologies  that   were  capable   of  determining
  quantitative results.  One of those was the EnviroGard
  PCB Test.  PRC calculated this data by the method of
  least squares.  Calculating linear regression hi this way
  makes  it possible to determine whether two sets of data
  are  reasonably related,  and  if so,  how closely.
 Calculating linear regression results hi an equation that
 can be visually expressed as a line.  Three factors are
 determined during  calculations of  linear regression.
 These three factors  are the y-intercept, the slope of the
 line, and the coefficient of determination, also called r2.
 All three of these factors had to have acceptable values
 before   a  technology's  accuracy  was  considered
 acceptable.

     The r2 expresses the mathematical relationship
 between two data sets.  If r2 is 1, then the two data sets
 are perfectly correlated. Lower r2 values indicate less of
 a relationship.  Because of the nature of environmental
 samples,    r2    values     between    0.80     and
 1 were  considered acceptable for this demonstration.

    If  an  r2 below 0.80 was found,  the data was
 reviewed to determine whether any  particular results
 were skewing the r2.   This skewing may sometimes
 occurs  because  technologies are often more accurate
 when  analyzing samples hi one range than  when
 analyzing samples hi another range.   In particular,
 samples with either very  high  or  very low  levels of
 contamination  often  skew  the  results.     For this
 demonstration, the technique used to identify outliers that
 might have skewed the results was residual examination
 (Draper and Smith 1981).   The computer program used
 for calculating the linear regression,  hi fact, identified
 most of the outliers.  When outliers were identified, they
 were  removed  and  linear regression was calculated
 again.

    If the corrected data set resulted hi an r2 between
0.80 and 1, then the regression line's y-intercept and
slope were examined to determine how closely the two
                                                  !  11

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data sets matched.  A slope of 1 and a y-intercept of zero
would mean that the results of the technology matched
those  of   the  confirmatory  laboratory  perfectly.
Theoretically, the farther the slope and y-intercept differ
from these expected values, the  less  accurate  the
technology.  Still, a slope or y-intercept can differ
slightly from its expected value without that difference
being statistically significant.  To determine whether
such differences were statistically significant, PRC used
the nprmal deviate test  statistic.   This test statistic
calculates a value that is compared to a table. The value
at the 95  percent  confidence level was used for  the
comparison.

    If an r2 between 0.80 and  1 was not found, then the
technology's data  was  considered inaccurate.   The
technology's data was also considered inaccurate if an r2
between 0.80 and 1 was found, but the normal deviate
test statistic indicated that either the y-intercept or the
slope differed significantly from its  expected  result.
However, in this case, the data could be mathematically
corrected if 10 to 20 percent of the samples were sent to
a confirmatory laboratory. Analysis of a percentage of
the samples by a confirmatory laboratory would provide
a basis for determining a correction factor.  Only in
cases where the r2, the y-intercept, and the slope were
all found to be acceptable did PRC determine that the
technology's data was accurate.

    A  second statistical method used  to assess  the
accuracy of the data from each technology was the
Wilcoxon   Signed  Ranks  Test.    This  test  is  a
nonparametric method for comparing matched pairs of
data. It can be used to evaluate whether two sets of data
are significantly  different.   The  test  requires  no
assumption regarding the population distribution of the
two sets of data being evaluated other than that  the
distributions will occur identically.   In other  words,
when one data point deviates, its respective point in the
other set of data will deviate similarly.  Because the only
deviation  expected during the demonstration  was a
difference  in the concentrations  reported  by  each
technology, the two sets of data were expected to deviate
in the same way.

     The calculation performed in the Wilcoxon Signed
Ranks Test uses the number of samples  analyzed and a
ranking of the number that results when a sample's result
obtained by using one analytical  method is subtracted
from the corresponding result obtained by using another
method.     The  rankings   can  be   compared   to
predetermined   values   on   a  standard  Wilcoxon
 distribution table, which indicates whether, overall, the
 two methods have produced similar results.
    Although the Wilcoxon Signed Ranks Test and the
linear  regression  analysis perform similar types of
comparisons, the assumptions on which each is based are
different. By running both tests on the data, PRC was
able to determine whether either test's assumptions were
violated, and if so, whether the  statistical results were
affected.

    The    EnviroGard   PCB    Test    produced
semiquantitative results. Linear regression analysis and
the Wilcoxon  Signed Ranks  Test cannot be used to
compare semiquantitative results.  Instead, PRC used a
2 by 2 contingency table and a  Fisher's Test.  The
Fisher's Test determines whether both data sets are
correlated. When used in a two-tailed manner, as it was
in  this  case,  its  formula  is  usually  conservative.
Therefore, use of a modified Chi-square  formula is
recommended  (Pearson  and Hartley  1976).   This
formula, as used hi this demonstration, is:
                                               (4-2)
        2 _ ^[(observed value - expected value) - .5f
                       expected value
     The Fisher's Test statistics were compared to the
95 percent confidence level obtained from a standard
Chi-square distribution table. This comparison indicated
whether,  overall, there was a correlation between the
results of the two methods.  If a correlation existed, the
technology's data was considered accurate.

     Finally,  the precision obtained by each technology
was statistically compared to the precision obtained by
the confirmatory laboratory using Dunnett's Test.  This
test was  used to assess whether the precision of the
technology and that of the confirmatory laboratory were
statistically equivalent.  First, the mean RPD for all
samples and their respective duplicates analyzed by the
confirmatory laboratory was determined.  The RPDs of
each duplicate pair analyzed by each of the technologies
was then statistically compared  to this mean.   The
Dunnett's Test results hi a single statistical value which
indicates the degree of certainty that the precision of the
 two methods is the same. In other words, a 90 percent
value indicates that one can  be 90 percent sure the
precision is the same. During this demonstration, values
of 95 percent or better indicated that the precisions  were
 statistically the same.

     It should be noted that results below 95 percent do
 not mean that the precision of the technology was not
 acceptable,  only  that  it may be different  from the
 precision of the confirmatory laboratory.  In particular,
 Dunnett's Test has no way of determining whether or not
                                                     12

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any difference  between  the  two  data  sets  actually
resulted because a technology's data was more precise
than the confirmatory laboratory's.                I
                                                i
Field Analysis Operations                  j
                                                I
    The field analysis portion of the demonstration >jras
performed hi a rented 28-foot trailer.  Electricity was
supplied for the  equipment,  refrigerators,  and  air
 conditioners.  Space within the trailer was divided to
 provide an area for each technology, sample storage, and
 the storage of sample collection equipment.  All of the
 equipment,  supplies,  reagents,  and office supplies
"needed for the demonstration were moved into the trailer
 during   the  weekend  before  the  start  of   the
 demonstration.  All analytical equipment was powered
 up and checked to ensure that it was operable.   All
 problems found were corrected.
                                                 13

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                                              Section 5
                                Confirmatory Analysis Results
    All samples  collected  during  this demonstration
were  submitted to the EPA Region 7 Laboratory for
analysis under its CLP.   The data supplied by the
confirmatory laboratory is discussed in more detail in the
following sections.

Confirmatory  Laboratory Procedures

    The samples collected during the demonstration
were  sent to the EPA Region 7 Laboratory where they
were  assigned EPA  activity  number DSX06.   The
samples  were then   shipped  to   the  confirmatory
laboratory for CLP 1990 SOW method analysis.  This
method requires that organochlorine pesticides and PCBs
be analyzed using a gas chromatograph (GC) equipped
with an electron capture detector (ECD).

    EPA Region 7 Laboratory personnel conducted a
Level II data review on the results provided by the
confirmatory laboratory.  This data review involved
evaluating reported values and specific QC criteria. A
Level II data review does not include an evaluation of
the raw data or a check of calculated sample values. A
review of the raw data and a check of the calculations
was performed by the confirmatory laboratory before
submitting the data package to EPA.  PRC was not able
to review the raw data generated from the analysis of
samples.   However,  PRC  did review  the  EPA's
comments generated by the Level II data review.

    The following sections discuss specific procedures
used  to identify  and  quantitate PCBs using the CLP
1990  SOW method. Most of these procedures involved
requirements  that were mandatory to guarantee the
quality of the data generated.

    In addition to being generally discussed in this
Section, all of the confirmatory laboratory results used
to assess  the Millipore EnviroGard PCB Test are
presented in tables in Section 6.
Soil Sample Holding Times

    The CLP 1990 SOW method requires that all soil
sample extractions be completed within 7 days from the
laboratory's validated sample receipt. The analysis of
soil  samples must be completed  within  40 days of
validated sample receipt.  The holding time requirements
for the samples collected during this demonstration were
met.

Soil Sample Extraction

    Soil  samples were extracted according to the
procedures outlined hi the CLP 1990 SOW method for
organochlorine pesticides and PCBs. This procedure
involves placing 30 grams of soil into a beaker and then
adding 60 grams of purified  sodium sulfate.  This
mixture is thoroughly mixed to a grainy texture. One
hundred milliliters (mL) of a 50:50 ratio mixture of
acetone and methylene chloride then is added to the
beaker containing the soil and sodium sulfate. Pesticides
and PCBs are extracted into the organic solvent with the
aid of a sonic disrupter.  This sonic disrupter bombards
the soil with sonic waves, which facilitates the transfer
of pesticides and PCBs into the organic solvent. The
organic solvent is vacuum-filtered through filter paper to
separate it from the soil particles. Sonication is repeated
two  more  times  with 100 mL  of the  acetone and
methylene  chloride mixture.  The organic solvent is
filtered and combined hi a vacuum flask.

    After  filtration,  the solvent  is  transferred to  a
Kuderna-Danish   apparatus.    The  Kuderna-Danish
apparatus is placed hi a hot water bath, and the organic
solvent is concentrated. Once concentrated, the solvent
is transferred from the acetone and methylene chloride
mixture into hexane  by using a  nitrogen evaporation
system.  The  soil sample extract, now in hexane, is
concentrated to a known volume using this system. The
soil sample extract is taken through a florisil solid-phase
                                                   14

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                                                I
 extraction column to remove any polar compounds fr6m
 the extract.  The soil sample extract is diluted to 10 mL
 with hexane and is transferred to a  test tube to await
 sample analysis.                                 I

 Initial and Continuing Calibrations        I

     The CLP 1990 SOW method for analyzing PCJBs
 involves an initial calibration (ICAL) for PCBs, which
 consists of analyzing one concentration of each of ijie
 seven Aroclors listed in the Target Compound  List
 (TCL). The ICAL is used to determine peaks to identify
 Aroclors and to determine factors to quantitate PCBs Jin
 samples.  The ICAL is performed before sample analyks
 begins.  PCBs cause multipeak patterns when analyzed
 using gas chromatography.   For each Aroclor,  three to
 five peaks are chosen to monitor retention time shift and
 to determine factors used for quantitation.          i

     Continuing calibrations  (CCAL) are performed py
 analyzing instrument blanks and performance evaluation
 (PE) mixture  standards.    The  retention times  aiid
 calibration factors  determined during  the ICAL are
 monitored through  CCALs.   The CCAL standard 'is
 typically  a mid-level pesticide  standard; howevqr,
 because  PCBs were  the compounds of interest,  an
 Aroclor was used as the CCAL standard for analyzing
 these samples.                                   J
    Retention times were monitored through evaluating
the amount of retention time shift from the PCB CC^L
standard as compared to the PCB ICAL standard. The
retention time window was defined as + 0.07 minute fbr
each peak identified in the ICAL.  According to the CLP
1990 SOW method, any time a peak of an Aroclor fajls
outside of its window, a new ICAL must be conducted.
During the analysis of samples for this demonstration,
the retention times of the peaks chosen for monitoririg
during  the  CCAL never exceeded  the  windows
established for them in the ICAL.

    Calibration factors were monitored in accordance
with the CLP 1990 SOW method and were acceptable,
as the CCAL  calibration  factor never exceeded 25
percent.                                         j

                                              ysis
                                                      Sample Analysis

                                                          PCBs are identified in samples by matching peak
                                                      patterns found after analyzing the sample with those
                                                      found in Aroclor standards.  Peak patterns may not
                                                      match  exactly  because  of the  way the PCBs were
                                                      manufactured or because of the effects of weathering.
                                                      When the patterns do not match, the analyst must choose
                                                      the Aroclor that most closely matches the peak pattern
                                                      present in the sample.   For this reason,  peak pattern
                                                      identification is highly dependent on the experience and
                                                      interpretation of the analyst.

                                                          Quantitation of PCBs is performed by measuring the
                                                      response of the peaks hi the sample to those same peaks
                                                      identified in the ICAL standard. The reported results of
                                                      this calculation are based on dry weights, as required by
                                                      the CLP  1990  SOW  method.    Because the field
                                                      screening technologies all reported wet weight results,
                                                      PRC converted the results reported by the confirmatory
                                                      laboratory from dry to wet weights to account for  any
                                                      loss of sample weight caused by drying.

                                                          The calculation to convert dry weight results to  wet
                                                      weight results is shown below:
                                                                                                   (4-1)
                                                       ww = own -MC

                                                       where

                                                          WW = Wet weight results.
                                                          DW = Dry weight results.
                                                          MC = Moisture content ratio provided by confirmatory
                                                               laboratory.
                                                          Sample extracts frequently exceed the calibration
                                                      range determined during the ICAL. When they do so,
                                                      they must be diluted to obtain peaks that fall within the
                                                      linear range of the instrument.  For PCBs, this linear
                                                      range is defined as 16 tunes the response of the Aroclor
                                                      standards analyzed during the ICAL.  Once a sample is
                                                      diluted to within the linear range, it is analyzed again.
                                                      Dilutions were performed when  appropriate  on  the
                                                      samples for this demonstration.
    Once an ICAL has been performed, sample analysis    Detection Limits
begins.  Usually, sample analysis begins by analyzing
method blank to verify that it meets the CLP 1990 SOW
method  requirements. After this, sample analysis mdy
continue for 12 hours. After every 12-hour period, a
CCAL standard must be analyzed. Sample analysis may
continue as long as CCAL standards meet the CLJP
1990 SOW method requirements.
                                                         One concentration of each Aroclor was analyzed
                                                     during the ICAL.  The concentration of each Aroclor
                                                     standard should correspond to the contract required
                                                     quantitation limit (CRQL) when corrected for the sample
                                                     extraction concentration factors.  The concentration used
                                                     for Aroclor 1221 was 200 micrograms per kilogram
                                                     0*g/kg); the level used for the other six Aroclors was
                                                  15

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100 pig/kg.  This corresponds to soil sample detection
limits of 67 /*g/kg for Aroclor 1221 and 33 jig/kg for the
other Aroclors.

    Because of CLP 1990 SOW method requirements,
these detection limits are based on samples that have no
moisture content.   Because almost all soil samples
contain moisture, the detection limits stated above are
raised to correct for the percent moisture present in the
soil  sample.   However,  PRC did not  correct the
detection limits  to  account for the percent moisture
present in the samples because the CRQLs were listed in
/tg/kg and the detection limits of the EnviroGard PCB
Test and the other technologies were listed hi mg/kg.
Even when corrected to account for percent moisture,
the CRQLs would be significantly below the detection
limits for each technology.

Quality Control Procedures

    A  number of  QC measures  were used  by the
confirmatory laboratory  as  required  in the  CLP
1990 SOW  method, including analysis of resolution
standard mixes, method blanks, and instrument blanks,
all  requirements  of  which  were   met  for  this
demonstration.

    Also,  surrogate  standards were  added to  all
standards, method  blanks,  matrix spikes, and soil
samples analyzed using the CLP 1990 SOW method.
The  percent recovery of each surrogate was calculated
and  compared to the advisory control limits of  60 to
150 percent found in the CLP 1990 SOW. No corrective
action is needed when surrogate recoveries fall outside
of the advisory control limits. The surrogate recoveries,
though, are reported with the other QC data.  During
this demonstration,  12 soil samples and field duplicate
samples from the confirmatory laboratory analysis were
outside the  advisory  control  limits  for  surrogate
recoveries.

    During  the  demonstration, 46 samples and their
respective duplicate samples required dilution to obtain
peaks that were within the linear range required by the
CLP 1990 SOW; however, the dilutions decreased the
amount of the surrogate standards that were injected onto
the GC. The result was that the surrogates were not
detected in the samples.  PRC was not able to obtain
information regarding actual surrogate standard recovery
for each of the samples analyzed by the confirmatory
laboratory.   Comments from the EPA Level II data
review, though, indicated that 88 of the samples and
their respective duplicate samples resulted in acceptable
surrogate recovery data.
    The CLP 1990 SOW requires that matrix spike and
matrix spike  duplicate samples be prepared with six
organochlorine pesticides and analyzed with each batch
of samples.   Because the demonstration was  only
concerned with PCB results, the matrix spike results
were not reported.

Confirmation of Analytical Results

    The CLP 1990 SOW also requires that all positive
sample results be confirmed. There are two methods of
confirming sample  results.  The  first, required in  all
cases, is to analyze the sample again using a second GC
column.   If concentrations  identified this way are
sufficiently high, the second method, analyzing the
sample again using a GC and mass spectrometer (MS),
must also be used.

Second Column Confirmation

    As required, all samples that were found to contain
PCBs during analysis on the first column were analyzed
on the second column.  In all cases, the presence of
PCBs were confirmed.  There were  122 samples that
required second column confirmations.

    The CLP 1990 SOW states that results from the two
columns should be  within 25 percent of  each other.
When this requirement is not met, the result for that
sample must be coded to indicate that it is estimated.
For the analysis of the samples from this demonstration,
17 sample results were above the 25 percent requirement
of the CLP 1990 SOW.  These results were J-coded to
indicate that the results were estimated but were not
validated  by  approved  QC procedures.    Finally,
following the CLP 1990 SOW method, the lower of the
two values was reported.

Gas  Chromatographic and Mass Spectrometer
Confirmation

    The CLP 1990 SOW requires that when pesticides
or PCBs are present in samples at sufficient quantities,
they  must be confirmed  by GC and  MS analysis.
Twenty samples from this  demonstration  contained
sufficient  quantities of PCBs to  require GC and MS
confirmation. These samples were compared to Aroclor
standards.  None of the  20 samples were confirmed
through GC and MS analysis.  Lack of GC and MS
confirmation is not uncommon for Aroclors because they
are a  mixture of congeners, and the GC and MS analysis
is better  suited  for identifying  individual  congeners.
Because all 20 samples were confirmed on the second
GC column, the lack of GC and MS confirmation was
determined to be insignificant during the EPA Level
                                                  16

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 II data review.   Therefore,  these samples were not
 coded.

 Data Reporting

    The data report PRC received from the EPA Region I
 7 Laboratory included a standard EPA Region 7 Analysis
 Request Report.   PCBs  were the only compounds)
 reported.  Results were reported on a dry weight basis,
 as required in the CLP 1990 SOW.  PRC obtained data j
 on the  percentage of solids  hi the sample from the|
 confirmatory laboratory and used this data to convert the j
 results to wet weight. This  conversion was required |
 because the data was to be compared to data from the
 EnviroGard PCB Test and three other technologies, all
 of which reported concentrations  based on wet soil
 weight.  PRC also converted the confirmatory laboratory
 results from /tg/kg to mg/kg.

    The results reported by the confirmatory laboratory
 contained three different codes. Every result was coded
 with a "V," indicating that the data had been reviewed
 and reported correctly.  Some data was  coded with a
 "K," indicating that the actual  PCB concentration hi the
 sample was less than the reported value,  or that PCBs (
 were not found in the sample.  The third code used was
 "J", which indicated that the data was estimated but not
 validated by approved  QC procedures. Twenty-nine of
 the 146 total  samples submitted  for analysis  were
 J-coded.

 Aroclors  Reported  by the Confirmatory
 Laboratory

    According to  RFI and CMS results from April
 1989, the only Aroclor believed to be present at the
 AICO  site was  Aroclor  1242.    However,  the
 confirmatory laboratory found three additional Aroclors
 in the samples collected during the demonstration. Most
 of the samples analyzed by the confirmatory laboratory
 were  found to  contain either Aroclor 1242 or Aroclor
 1243. Seventy-three samples were found to contain only
 Aroclor 1242, while 33 samples were found to contain
 only Aroclor 1248.   Sixteen samples were found to
 contain mixtures of two of the four Aroclors found.  The
predominant mixture was  Aroclor  1242 and Aroclor
 1248.   Seven samples  were found to  contain  this
mixture.  Four samples were found to contain a mixture
of Aroclor 1242 and Aroclor 1260.  Three  samples were
found to contain a mixture of Aroclor 1248 and Aroclor j
 1260. Two samples were found to contain a mixture of
Aroclor 1242 and Aroclor 1254. In all, 122 soil samples
 submitted to the  confirmatory  laboratory for  this
demonstration were found to contain detectable levels of
PCBs.  Twenty-four  samples were  reported as not
containing PCBs above the CRQLs.
 Data Quality Assessment of Confirmatory
 Laboratory Data

     This section discusses the accuracy, precision and
 completeness of the confirmatory laboratory data.

 Accuracy

     Accuracy for  the confirmatory laboratory results
 was assessed through the use of PE samples, purchased
 from Environmental Research Associates (ERA), that
 contained a known quantity of Aroclor 1242.  ERA
 supplied data sheets for each PE sample, which included
 the true concentration and an acceptance range for the
 sample.   The acceptance range was  based on  the
 95 percent confidence interval taken from data generated
 by ERA and EPA interlaboratory studies.

     The  two  PE  samples   contained   different
 concentrations, one low and one high.  These  samples
 were extracted and analyzed hi exactly the same manner
 as the other soil samples.  The confirmatory laboratory
 knew that the samples were PE samples, but  the true
 concentrations and acceptance  ranges of the  samples
 were not known to the confirmatory laboratory.  The
 true  concentration  of   sample  047-4024-114  (the
 high-level sample)  was 110 mg/kg, with an acceptance
 range of 41 to 150  mg/kg. The result reported for this
 sample by the confirmatory laboratory was 67 mg/kg of
 Aroclor 1242, which was within the acceptance range.
 The percent recovery of this sample by the confirmatory
 laboratory was 61 percent. The true value concentration
 of sample 047-4024-113  (the low-level sample) was
 32.7  mg/kg,  with an  acceptance  range of 12 to
 43 mg/kg.   The result reported  by the confirmatory
 laboratory for this  sample was 15 mg/kg,  which was
 within the acceptance range. The percent recovery of
 this  sample  by  the confirmatory laboratory  was
 46 percent. Based on the results of the PE samples, the
 accuracy of the confirmatory laboratory was acceptable.

 Precision

    Precision for the confirmatory laboratory results was
 determined by evaluating field duplicate sample results.
 Other types of data typically used to measure precision
 were not available.  Laboratory duplicate samples were
not required by the CLP 1990 SOW. Two other types
 of data  commonly  used to measure precision, matrix
 spike and matrix spike duplicate RPDs,  also were not
available because matrix spike compounds required by
the CLP 1990 SOW method are pesticide compounds,
not PCBs,

    The evaluation of field duplicate sample results was
used to  assess the precision of the analytical method.

-------
Precision can be evaluated by determining the RPDs for
sample results and their respective field duplicate sample
results.  The RPDs for the 32 field duplicates and their
respective  samples averaged  31.8  percent, but this
included two pairs of samples with extremely dissimilar
results.  Sample 102 had a result of 293 mg/kg while its
duplicate, Sample 102D, had a result of 1.77 mg/kg.
The RPD  for the  sample  pair was calculated  as
197.6 percent.   Also, Sample 097 had  a result  of
1.23  mg/kg  while  its  duplicate  had  a result  of
0.285 mg/kg. The RPD for Sample 097 and 97D was
124.8 percent.  The other RPDs, though, had much
lower percentages.  Without these  two samples, the
mean RPD fell to 20 percent. Overall, this data shows
excellent agreement between the samples and  their
respective field duplicates, indicating a high degree of
precision by the confirmatory laboratory.  The mean
RPD also indicated that the method used to homogenize
the samples before splitting them for analysis was highly
effective.

Completeness

    This demonstration resulted  in the collection  of
112 samples, 32 field duplicate samples, and two PE
samples. Results were obtained for all of these samples.
Of the 146 total samples analyzed by the confirmatory
laboratory, 29 were J-coded.  The J-code is defined by
EPA Region 7 Laboratory as data  estimated but not
validated by approved  QC procedures.  Based on the
definition of completeness given above, these 29 samples
cannot  be  considered complete.   Because of  this,
completeness  for  the  samples  analyzed  by  the
confirmatory laboratory was 80 percent, which is below
the completeness objective of 90 percent. However, the
J-coded data was  determined to be acceptable by  PRC
and EMSL-LV. For this reason, the actual completeness
of data used was 100 percent.
Use of Qualified Data for Statistical Analysis

    As noted previously, 20 percent of the confirmatory
laboratory results were reported as data not validated by
approved  QC  procedures.   The  EPA  Level II data
review indicated that  this J-coded data was not valid
because it had failed  at least one of the two QA/QC
criteria specified in the CLP 1990 SOW.

    Twelve  samples  were determined to be invalid
because one of the two surrogate compound recoveries
was outside of the advisory control limits.  In all cases,
the second surrogate recovery was within the advisory
control  limit.    The remaining  17 samples  were
considered invalid because results from the two  GC
columns used for sample quantitation differed by more
than 25 percent.

    Neither of these QA/QC problems was considered
serious enough to preclude the use of J-coded data for
this demonstration.   The surrogate  recovery control
limits are for advisory purposes only,  and no corrective
action was required for the  surrogate recoveries that
were  outside of this range.  High percent differences
between the sample results analyzed on the two  GC
columns is a frequent problem when analyzing samples
with very complex  chromatograms.   In all cases, the
reported value was the lower of the  two, reducing the
effect of interferants on the results.

    As discussed in the QAPP (PRC 1992b), a rejection
of a large percentage of data would  increase the apparent
variation between the confirmatory laboratory data and
the data from the technologies. This apparent variation
would be  of a similar magnitude to that introduced by
using the data.  For these reasons, PRC, after consulting
with EMSL-LV, elected to use the  J-coded data despite
the fact  that  the  EPA Region  7  Laboratoiy had
determined the results to be invalid under approved QC
procedures.
                                                   18

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                                                   I
                                               Section 6
                                 Millipore EnviroGard PCB Test
     This section provides information on the EnvkoGard
 PCB   Test,   including   background'  information,
 operational   characteristics,   performance   factors,!
 specificity, a data quality assessment, and a comparisonj
 of its results with those of the confirmatory laboratory. |
 Observations on the technology made by the operator)
 during the demonstration are presented throughout this!
 section.                                            ;

     The  EnviroGard  PCB  Test  was  designed by
 Millipore for use hi a semiquantitative mode. Most of 1
 this   section   discusses   the  technology   as  a
 semiquantitative analytical method.  However, after
 consulting with both Millipore and EMSL-LV, PRC also
 tested the technology's ability  to produce quantitative
 results.  Details of its quantitative abilities are included j
 in this section.                                     I

 Theory  of  Operation   and  Background
 Information

     The EnviroGard PCB Test is designed to provide
 quick, semiquantitative results for PCB concentrations in
 soil samples using an immunoassay approach.   The
 approach uses polyclonal antibodies  to detect  and
 quantify PCBs in a sample.   These results indicate
 whether  PCB concentrations are above or  below a
 specific level within a 99 percent confidence level.  The j
 technology can be customized to report specific results
 over a particular range of concentrations.

    The  EnvkoGard PCB Test is designed  to  report
 levels  of PCBs that are above  or below three known
 concentrations. These known concentrations are defined
by the standards used to calibrate the technology.  The
EnvkoGard PCB Test comes with standards of Aroclor
 1248 in the  following PCB concentrations: 5, 10,  and
50 mg/kg.

    Before sample analysis can take place, soil samples
must be extracted.  Soil samples are extracted using an
organic solvent and steel ball bearings. An aliquot of the
 soil sample extract is then diluted and placed in a test
 tube coated with the anti-PCB antibodies.  This solution
 is mixed and allowed to incubate for 5 minutes so that all
 of the  PCBs  in the sample extract can  attach to the
 anti-PCB antibody binding sites.  After the incubation
 period, the test tube is emptied and vigorously washed
 with  four test-tube volumes of tap or distilled water.
 Four drops of enzyme conjugate are then added to the
 test tube and  allowed to incubate for 5 minutes while
 periodically mixed.  The enzyme conjugates compete
 with PCBs for the binding sites of anti-PCB antibodies
 on the test tube.  After the 5-minute incubation time, the
 test tube is agaki emptied and vigorously washed with
 four test-tube volumes of tap or distilled water.

    Next,  color reagents are  added to the test tube.
 Four drops of substrate are added to the test tube,
 followed by four drops of chromogen. This mixture is
 swirled in the test tube and allowed to  incubate  for
 5 minutes.  After 5 minutes, a stop solution is added to
 the test tube to stop color development. Test results are
 estimated visually by observing the color development.
 A blue  color indicates the absence of PCBs, while a
 lighter blue or clear color indicates  the presence of
 PCBs.  To obtain semiquantitative results, the color of
 the solution is compared to the colors resulting from the
 analysis of the  Aroclor standards and a negative control
 sample.  For a more precise measurement of the PCB
 concentration, the color of the solution is  compared to
 the color resulting from the analysis of the  Aroclor
 standards  and a  negative  control  sample using a
 differential photometer (see Exhibit 6-1).

 Operational Characteristics

    Overall, the EnvkoGard PCB Test was found to be
portable.   The  test  is  made up  of three kits:  the
 EnvkoGard PCB Field Lab, the EnviroGard Field Soil
 Extraction Kit  II, and the EnvkoGard PCB Test Kit.

    The EnvkoGard PCB Field Lab is a starter kit and
consists of a portable carrying case about 18 inches long,

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EXHIBIT 6-1.  ASSAY FLOW CHART.
MILLIPORE ENVIROGARD PCB TEST PROCEDURE

STEP "1" _
Wainh«!oil ^ Extract thB ll.uuiimnla
sampla 	 Polychlorinated * Filter the sample


STEP 5: STEP 6: STEP 7:
Add standards ,, Dilute the 	 ...^ Washmrt
controls or samples samples test tubes

STEP 9: STEP 10: STEP 11:
test tubes reagent reagent

STEP 14a:

Samples can be white background I



STEP 4:


STEPS:
^ Add conjugate 	 ^
reagent

STEP 12: STEP 13:
. |nrj ihatn fnr ^ Add Stop ~^-
5 minutes solution

STEP 14b:
se photometer to
obtain the optical
isities for standards
and samples

 18 inches wide, and 6 inches high.  The carrying case
 and all  the equipment contained in it weighs nearly
 10 pounds. That equipment includes (1) a differential
 spectrophotometer equipped with an electrical cord and
 rechargeable  battery,  (2)  a  positive displacement
 precision pipettor for dispensing volumes between 1 and
 25 microliter <>L), (3) an Eppendorf Repeater pipettor,
 (4) an electronic  tuner, (5)  a portable balance with a
 50-gram calibrator weight, (6) a 500-mL wash bottle,
 (7) two six-position test tube racks, (8) a rack of pipette
 tips for the positive displacement precision pipettor, and
 (9) an instruction card. Several other items needed to
 complete  this kit were  provided by  Millipore hi a
 cardboard box.  These items included (1) one 12- by
 75-mm  polystyrene  test tube used for blanking  the
 spectrophotometer, (2) eight 5-mL pipette tips for the
 Eppendorf Repeater pipettor,  for dispensing volumes
 between 0.1 and 0.5 mL, (3) four 12.5-mL pipette tips
 for the Eppendorf Repeater  pipettor for dispensing
 volumes between 0.25 and 0.625  mL,  and (4) one
 50-mL pipette tip for the Eppendorf Repeater pipettor,
 for dispensing volumes between 1.0 and 5.0 mL.

     The EnviroGard Field Soil Extraction Kit II and its
 associated equipment are provided hi a small cardboard
 box.   The equipment includes (1)  12 polypropylene
 extraction bottles with screw caps containing five steel
 ball bearings, (2)  12 filter devices consisting of 12 upper
 and 12 lower units, (3) 12 polyethylene prefilters,
(4) 15 wooden spatulas, (5) 12 4-mL, screw-top glass
vials, and (6) 15 polyethylene weigh boats.

    The EnviroGard PCB  Test Kit comes hi a small
cardboard box and includes enough reagents and. other
equipment to analyze 16 samples. Most of its contents
require   refrigeration.     This   kit   contains   (1)
20 polystyrene tubes coated  with  anti-PCB antibody,
(2) a 14-mL vial of assay diluent, (3) a 4.8-mL vial of
PCB enzyme conjugate, (4) a 0.5-mL vial of negative
control solution, (5) a 4.8-mL vial of peroxide solution
(substrate), (6) a 4.8-mL vial of chromogen solution,
(7)  a 15-mL vial of  1.0-normal  sulfuric acid (stop
solution), (8) three 0.5-mL vials of 5, 10, and 50 mg/kg
Aroclor 1248 standards, and (9) a plastic six-position test
tube rack.   Aroclor  standards can  be  obtained hi
different concentrations by  contacting Millipore.

     Electricity is needed for the differential photometer.
Millipore offers a photometer that can be operated using
either a 115-volt or 230-volt electrical supply.  The
differential   photometer also  is   equipped  with  a
rechargeable battery. This battery requires 8 to 2A hours
of charging, and when fully charged can perform up to
500 tests without being recharged.  A battery also is
needed to operate the portable balance.  A refrigerator
must be available  to  keep reagents  cool to avoid a
decrease hi the activity of  the enzyme conjugate.  The
recommended storage temperature of the reagents is
                                                     20

-------
between 2 and 8 °C.   The  activity  of the enzym6
conjugate can be decreased by freezing the reagents, by
exposing  them to temperatures  above 37 °C, or  bj^
repeated exposure to ambient temperatures.          j
                                                   . i
                                                   !
     Miscellaneous provisions needed to analyze sampled
include (1) methanol for sample extraction and dilution!
(2)  distilled or tap water for washing the test tubes
coated  with anti-PCB antibodies, (3) a table or work
space of at least 8 square feet, (4) a permanent marker
for writing sample numbers on test tubes and sampl^
containers, (5) a logbook or a report form for recording
sample results, and (6) an ink pen.

     The EnviroGard PCS Test is designed for use in the
field or laboratory.  Some of its, instrumentation an4
equipment  require special  handling,  such as  the
differential photometer,  portable  balance,  and  two
pipettors.   This equipment must be handled carefully to
avoid damage.                                      j

     The reliability of the EnviroGard PCB Test was|
evaluated by monitoring instrument calibrations.  Thej
ICAL  problems  experienced by  the  operator  were
attributed  to the  small volumes used  to prepare the
Aroclor standards and to the operator's inexperience in1
using the  pipette  required to measure  these small
volumes.    Preparing  the  Aroclor standards required
measuring 5 /*L each of the three concentrations. Using
such a small volume  may  produce  large errors!
especially  if a single drop of Aroclor  standard is left
outside the pipette tip or if the pipette tip is not placed
completely into the vial containing the Aroclor standard,!
allowing air into the pipette tip rather than the Aroclor
standard.                                           I

     Thirty-one total calibrations were performed during
this demonstration to produce both the semiquantitative
and  quantitative  data on  PCB concentrations in the
samples. Initially, each calibration consisted of two sets
of Aroclor standards, each containing three concentration1
levels:  Aroclor 1248 (5, 10, and 50 mg/kg) provided by!
Millipore,  and Aroclor 1242 (1,  5, and 25 mg/kg}
prepared  by  PRC.    PRC  prepared  the   Aroclor!
1242 standards and used them to perform the quantitative
evaluation, discussed later in this  section. The Aroclor
1248 standards were used for  the semiquantitative
evaluation  of the technology.   Semiquantitative  and
quantitative analyses were conducted concurrently, and!
therefore,  the semiquantitative and quantitative batch
calibrations were done at the same tune.  The following!
paragraphs discuss problems with the semiquantitative'
calibrations; a discussion of problems found during}
calibrations for the quantitative evaluation is found  lateij
in this section.
     Five calibration failures occurred within the first
 16 semiquantitative calibrations.  The first calibration
 failure  was  attributed to operator error and errors
 attributed to measuring the small volumes associated
 with the analysis step.  This  problem appeared to be
 resolved after a reanalysis of these standards and further
 training of the operator. Because of the failures, the use
 of the three Aroclor 1248 standards was discontinued.
 AH   subsequent  calibrations   with   the   Aroclor
 1248 standard involved only the 10 mg/kg concentration.
 This concentration was selected  as the sole Aroclor
 1248 calibration standard because it is a common action
 level for PCB cleanups.

     Reanalysis of samples associated  with  the  first
 16 Aroclor 1248 standards was required for only two of
 the unacceptable calibrations. This is because acceptable
 Aroclor  1242 calibration was obtained  for  the  other
 three, even though the Aroclor 1248 calibrations failed.
 It also should be noted that the predominant Aroclor
 expected at the site was Aroclor 1242.

     The  frequent   problems   with   the   Aroclor
 1248 standards may have occurred because the actual
 concentrations  of  the   standards  were  not  the
 concentrations shown on the standards' containers.  The
 actual concentrations were different because Millipore
built a safety margin into the  Aroclor standards.  The
 stated concentrations of the .Aroclor 1248 standards were
5, 10, and 50 mg/kg. The actual concentrations of these
 standards were 3, 5, and 22 mg/kg, respectively.  Three
of the five Aroclor 1248 calibrations that failed did so
because  the  response  for the 5 mg/kg  standard was
greater  than the response of  the  10 mg/kg  standard.
Because the concentrations of these two standards were
actually 3 and 5 mg/kg, the color changes that resulted
when they were analyzed were very similar. The small
differences in the actual concentrations of the standards
magnified the  possibility of errors associated with
analysis of the standards.

    Between the 17th and 31st calibrations, there were
two failures.  These failures were not associated with
either the Aroclor 1242 or 1248 standards.  The first
calibration failure  was  due  to a positive  response
exhibited by the negative control sample.  A negative
control sample was analyzed with each standard and used
as an assay blank.  The samples analyzed during this
unacceptable calibration were reanalyzed during another
acceptable calibration.  The second calibration failure
was due to  a lack of color formation in any of the
samples, Aroclor standards, or negative control samples.
The cause of this failure was unknown.

 .   The EnviroGard PCB Test requires  the use of
chemicals to perform the analysis. The chemicals used
                                                    21

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include methanol, a  flammable solvent that can be
absorbed through the skin, and sulfuric acid, which can
cause chemical burns.   Chemical resistant clothing,
gloves, and safety glasses should be worn when using
this solution to protect against injury while using these
chemicals

    The operator chosen to use the EnviroGard PCB
Test was Mr.  Keith Brown, an employee of PRC.  He
earned a B.G.S. degree in Environmental Science from
the University of Kansas hi 1990. While at PRC,  Mr.
Brown has conducted preliminary site assessments and
investigations  at hazardous waste sites throughout EPA
Regions 5,  7,  and  9.    He  also  has  performed
hydrogeologic investigations at similar sites. Mr. Brown
has more than 2  years  experience performing  these
investigations with PRC and a previous employer.

    Mr. Brown reviewed'the information provided by
Millipore concerning the analysis of soil samples using
the EnviroGard PCB Test  before  the start of  the
demonstration. This information included a 20-minute
videotape   that   explained  the   fundamentals  of
immunoassay analysis  and introduced  the  sample
extraction and analysis techniques used.  Additional
training was provided by Dr. Alan Weiss  of Millipore at
the start of the demonstration. This training included an
in-depth explanation  of the sample  preparation and
analysis steps. In addition, Mr. Brown analyzed five
predemonstration samples using the technology under the
supervision of Dr.  Weiss.  Mr. Brown noted that he felt
comfortable  using the EnviroGard PCB  Test  after
analyzing the five  predemonstration samples.

    Millipore states that this product is intended for use
by individuals with little or no training in PCB testing.
The operator for  this technology had  no prior PCB
testing experience and noted that the sample preparation
and analysis steps were simple and straightforward. As
described above,  the operator  did  experience  some
problems  with the technology's ICAL.  The first attempt
at calibration resulted in a higher PCB concentration for
the  5  mg/kg Aroclor  1248 standard  than  for the
10 mg/kg Aroclor  1248 standard. These  standards were
reanalyzed, and an acceptable calibration was obtained.
Analysis  of samples  then proceeded.   All samples
analyzed  following the unacceptable calibrations were
reanalyzed.

     The EnviroGard PCB Field Lab Kit includes most
 of the equipment needed to analyze soil samples.  The
 cost of this kit is $1,495. Most of this equipment can be
 reused for a number of projects, although a few  of the
 items will wear out over time and eventually need to be
 replaced.  The EnviroGard Field Soil Extraction Kit
II includes the equipment required to extract  12 soil
samples.  The cost of this kit is $60.  The kit must be
purchased each tune an analysis is conducted because the
equipment is disposable.  The EnviroGard PCB Test Kit
includes the reagents  needed to perform 16 analyses.
The cost of this kit is $185.  According to  Millipore,
these  reagents have a 6-month shelf life.   Reagents
should not be used after the expkation date  printed on
the product label.  Millipore also sells the methanol used
to extract PCBs from soil.  The cost for 100 mL of
methanol is $7.90.   Methanol  also  may  also  be
purchased from a number of other chemical supply
companies. A differential photometer can be used with
the  technology  to  obtain   more  accurate  results.
Millipore offers a differential photometer that uses either
115- or 230-volt sources of electricity. The cost of this
photometer  is  $799.   The  photometer  should  be a
one-time purchase.

    Operator costs using the EnviroGard PCB Test will
vary depending on the technical level of the operator.
During this demonstration,  about  200  samples  were
analyzed  with  this  technology,  including  QA/QC
samples.  The waste generated from this analysis  filled
half a 55-gallon drum. The appropriate way to dispose
of this waste would be  through  an approved  PCB
incinerator facility. The cost for disposal of one  drum
of this waste is estimated at $1,000.

Performance Factors

    The following sections  describe the EnviroGard
PCB  Test's performance factors,  including detection
limits  and sensitivities, sample matrix effects, sample
throughput, and drift.  Specificity, due to its complexity,
it is discussed separately in Section 6.

Detection Limits  and Sensitivity

    Millipore reports that the limit of quantitation for
the EnviroGard PCB Test is 3.3  mg/kg for  Aroclor
 1248.    This  is the lowest  concentration  of  Aroclor
 1248 that can be accurately identified in a  soil sample
99 percent of the tune. The limit of quantitation differs
for each Aroclor.

    The limit of quantitation for the EnviroGard PCB
Test depends on a number  of factors.  These factors
 include the number of active sites present on the wall of
 the anti-PCB antibody-coated test tube, the amount of
 PCBs present in the  sample analyzed,  the amount of
 enzyme conjugate added to the test tube, and the amount
 of coloring reagent added to the test tube.  Millipore has
 designed the test so that the only factor that  will change
 when analyzing a soil sample  is the amount of PCBs
 present.
                                                    22

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     The technology is designed so that the number of
active sites in the test tube will always be  the same'
within  a certain percentage of error.   This will bei
especially true when the same test-tube lots  are used.j
There may be some variance between different test-tube!
lots, so it is advisable to use the same lot throughout any!
particular project.                       .           I

     The kits are also designed so  that the amount of!
enzyme conjugate and coloring reagent will be the same!
for each sample analyzed.  Measured amounts of the!
enzyme conjugate solution  and coloring reagents are
added to each Aroclor standard, negative control sample,
and sample analyzed.
                                                   i
     Another factor  that  will affect  the  limit  of)
quantitation is the particular Aroclor in the sample.  The)
EnviroGard PCB  Test cannot differentiate between!
Aroclors, but it will respond differently to each Aroclor. j
Millipore states that the response of the technology toi
Aroclors 1016, 1242, 1254, and 1260 should be within!
two  tunes its  response for  Aroclor 1248.  Aroclor
specificity for this technology is discussed later in this)
section.                                            I

Sample. Matrix Effects

    Most of the  soil  samples collected during this!
demonstration consisted of clay, which caused some)
problems during extraction  and analysis.   The most
common problem was that a colloidal suspension formed
for  some  of  the  samples  after   the initial sample
extraction.  The colloidal suspension either (1) prevented
good recovery of the organic extraction solvent from the
filtering device or (2) clogged the filter, making it
impossible to push the extraction  solvent through the
filter.    Many of the samples  resulted in  organic
extraction  solvent  recoveries  of  less than  2  mL.
Millipore suggested that PRC extract another sample
when this filter problem occurred.  It was recommended
that  this extraction be performed using the standard
5 grams of soil sample and doubling the standard volume
of extraction solvent from 5 mL  to 10  mL.  If this
approach did not solve the problem, less than 5 grams of
the soil sample was used in the extraction step.  Nineteen
samples required this approach: 033, 034, 035, 035D,
048, 056, 057, 065, 070, 071, 071D, 072, 077, 080,
083B, 086, 086D, 104, and 106.  Results for these
19 samples were S-coded by the operator to indicate that
due to sample matrix effects, the extraction and analysis
process was modified as described above.

    This extra dilution required that a correction factor
be used when calculating the results for these samples.
The correction factor caused results and detection limits
to double those normally used. For semiquantitative
 results, when the response of the sample was less than
 the response of the 10 mg/kg Aroclor 1248 standard, the
 reported result of the sample was raised from "less than
 10 mg/kg" to "less than 20 mg/kg."

    Another  sample  matrix  effect  observed  was
 differences   between   some   samples   and  their
 corresponding field duplicate samples.  This problem
 was noted during the predemonstration activities, and
 steps were taken to improve sample homogenization.

 Sample Throughput

    Millipore  recommends  that  no   more   than
 20 individual immunoassay analyses be performed at the
 same time. Every analysis performed requires that three
 concentrations of  Aroclor standards and  a negative
 control sample be prepared.  This means  a  total of
 16 actual sample analyses can be performed at a time.
 The operator found that a minimum of 30 minutes was
 required to extract 16 samples arid that between 30 and
 45 minutes were required to analyze the sample extracts.
 The operator also noted that the time required for the
 extraction and analysis steps did not include the time
 required for sample handling,   data documentation,
 diluting samples when required, difficult extractions,, or
 the  preparation  of  QC   samples.    During  this
 demonstration, the highest number of samples analyzed
 in a single 8-hour day was 52. The average number of
 samples analyzed during an 8-hour day was 25.  This
 information indicates that the EnviroGard PCB Test can
 provide rapid analysis of PCBs hi soil samples.

 Drift

    Drift normally is a measurement of an instrument's
variability in quantitating a known amount of a standard.
 The EnviroGard PCB  Test eliminates the variability
 associated with drift by requiring that a new calibration
be performed with each set of samples analyzed.

    During this demonstration, the optical density values
obtained from the Aroclor standards placed into the
differential photometer were evaluated.  These values
were found to drift during the 31 calibrations performed.
The optical density values for the Aroclor 1242 standards
decreased over tune.  The standards were stored in a
refrigerator when  not  hi use to reduce evaporation.
However, the decrease may have been caused by the
evaporation of solvent used to dilute the standards.

    The optical  density  values  for  the  Aroclor
 1248 standards also decreased over time, although not as
dramatically as values for the Aroclor 1242 standards.
This is also believed  to  result  from evaporation of
solvent.  Although Millipore supplied standards with
                                                   23

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each EnviroGard PCB Test, new standards were not
used for each new calibration.  This was because the
volume of standards provided with the technology was
more than enough  to perform a single or multiple
calibration.  This may have contributed to the decrease
in optical density for the Aroclor 1248 standards.

Specificity

    Immunoassay techniques typically use a "lock and
key" type of chemical bonding to trap both the PCB and
enzyme conjugate.  This chemical must be specific to
PCBs to prevent a large number of similar chemicals
from binding to the active sites.  The affinity of other
compounds  to these sites  is  called cross-reactivity.
Millipore has designed the EnviroGard  PCB Test to
produce a specific binding site for  PCBs that is not
cross-reactive to most other compounds.

    Millipore   has   performed   studies   of   the
cross-reactivity of other chemicals to the active sites of
the anti-PCB antibody used. The following compounds
were tested by Millipore and  found to have a cross-
reactivity of 0.5  percent  or less when compared to
Aroclor  1248   on  a   weight-to-weight  basis:
1,2-dichlorobenzene, 1,3-dichlorobenzene, 1,4-dichloro-
benzene,  1,2,4-trichloro-benzene, 2,4-dichlorophenol,
2,5-dichlorophenol,   2,4,5-trichlorophenol,  2,4,6-tri-
chlorophenol, biphenyl, and pentachlorophenol. Milli-
pore explains that for compounds with a cross-reactivity
value of 0.5  percent, a concentration of 200 mg/kg
would be required to produce  the same response as a
sample containing 1 mg/kg of Aroclor 1248.

    Matrix effects also can influence an immunoassay.
Millipore noted  that soils  containing  greater  than
5 percent oil may cause false negative results.  However,
careful field observations can reduce the impact of this
effect. Soil samples containing greater than 5 percent oil
should be visibly different from soil samples containing
less than 1  percent oil, and  the extract from  soils
containing 5 percent oil will appear  cloudy during the
first incubation step of the immunoassay process.

    This technology is designed specifically to react to
the   chlorinated   biphenyls  present  hi   Aroclor
1248.   Many of these chlorinated biphenyls also are
present hi other Aroclors.  Therefore, the technology
will produce a positive response to other Aroclors, but
in  varying  degrees.  During  tins demonstration, an
Aroclor specificity test was used to evaluate the response
of the technology to each of the seven Aroclors.  For
this test, seven soil samples were each divided into four
aliquots.  The aliquots were then spiked with different
Aroclors at approximately 10 mg/kg.  This concentration
was chosen because it  is a common action level at
contaminated sites. While the actual concentration of the
spike was often slightly less than 10 mg/kg, the spike
was  always close enough  that the technology result
should have indicated a positive response. The results of
the Aroclor specificity  test for  the technology hi  its
semiquantitative mode are tabulated hi Table 6-1.

    The Aroclor-spiked samples were identified with
9-character  digit,  alphanumeric identification  codes.
The first three characters of this code referred to the soil
sample  number used  for  spiking.   The  next four
characters, "ARSP," are an abbreviation of the words
"Aroclor spike."   The next character was a letter, A
through G, identifying which Aroclor was used to spike
the sample.  The last character was a number, 1 through
4, referring to the aliquot of the sample. To ensure that
results of the assessment were unbiased by operator
effects, the  operator did not know which Aroclor was
used for spiking  or the Aroclor concentration hi  the
samples.

    Sample  077  was   spiked  with approximately
10 mg/kg of Aroclor  1016. The four spiked samples
indicated that the  PCB  concentrations of the samples
were less than 10 mg/kg when compared to the Aroclor
1248 standard. It appears  that the technology  is less
responsive to Aroclor 1016 than to Aroclor 1248.

    Sample 058  was then spiked witii  10 mg/kg of
Aroclor 1248. Three of the four spiked sample results
indicated PCB concentrations of greater than 10 mg/kg
when compared to the Aroclor 1248 standard.  Two of
these aliquots had been spiked with exactly 10 mg/kg of
Aroclor 1248; the third, with 9.90 mg/kg of Aroclor
1248;  and  the fourth,  with 9.73 mg/kg  of Aroclor
1248.   The response of me technology  to the fourth
aliquot containing 9.73 mg/kg of Aroclor 1248 was less
than its response to  the 10 mg/kg  standard.  This
indicates that the detection limit of the technology for
Aroclor 1248 is 10 mg/kg, as expected.

    Sample 021 was  spiked with about  10 mg/kg of
Aroclor 1232.   The four spiked  sample  results  all
indicated that the PCB  concentrations of the samples
were less than 10 mg/kg when compared to the Aroclor
1248 standard. This indicates that the technology cannot
identify a soil sample containing 10 mg/kg of Aroclor
1232 using the Aroclor 1248 standard.

     Sample 012 was spiked with 10 mg/kg of Aroclor
1260.  The four spiked sample results indicated that the
PCB concentrations hi the samples were greater than
10 mg/kg when compared to the Aroclor 1248 standard.
This indicates that a soil  sample containing 10 mg/kg of
Aroclor 1260 can be  identified using  the Aroclor
1248 standards.
                                                    24

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TABLE 6-1 . SEMIQUANTITATIVE RESULTS F^)R THE AROCLOR SPECIFICITY TEST.
Sample No.
003ARSPA1
003ARSPA2
003ARSPA3
003ARSPA4
012ARSPB1
012ARSPB2
012ARSPB3
012ARSPB4
021ARSPC1
021ARSPC2
021ARSPC3
021ARSPC4
034ARSPD1
034ARSPD2
034ARSPD3
034ARSPD4
040ARSPE1
040ARSPE2
040ARSPE3
040ARSPE4
058ARSPF1
058ARSPF2
058ARSPF3
058ARSPF4
077ARSPG1
077ARSPG2
077ARSPG3
077ARSPG4
Confirmatory
Laboratory
Result
(mq/kq)
0.1
0.1
0.1
0.1
ND
ND
ND
ND
0.06
0.06
0.06
0.06
34.0
34.0
34.0
34.0
4.3
4.3
4.3
4.3
0.7
0.7
0.7
0.7
ND
ND
ND
ND
Soil Sample
Result
(mq/kq)

<10
<10
•
Spiked Sample
Aroclor Spike Amount Result
Spike (ma/kg) (mq/ka)
AR1221
AR1221
AR1221
< 10 AR1221
<10 JAR1260
<10
<10
<10
<10
<10
<10
<10
AR1260
AR1260
AR1260
AR1232
AR1232
AR1232
AR1232
> 10 IAR1254
>10 AR1254
>10 AR1254
> 10 AR1254
> 10 AR1242
> 10 AR1242
>10 AR1242
> 10 AR1242

^248'
< 10 AR1248
< 10 AR1248
< 10 AR1016
< 10 AR1016
< 10 AR1016
< 10 AR1016
9.94 <10
9.84 < 10
9.92 <10
9.77 < 10
9.78 > 10
9.80 > 10
9.65 > 10
9.86 >10
9.98 < 10
9.84 < 10
9.88 < 10
9.82 < 10
9.86 >10
9.77 > 10
9.77 > 10
9.67 > 10
9.86 > 10
9.69 >10
9.86 > 10
9.75 > 10
9.73 < 10
10.00 > 10
10.00 > 10
9.90 > 10
9.65 <10
9.96 < 10
9.75 < 10
9.90 < 10
 Notes:
 ND     PCBs not detected above the detection limit of 1.0 mg/kg.
 mg/kg  Milligrams per kilogram.
    Sample 003 was spiked with 10 mg/kg of Aroclor
1221. Results for the four spiked samples indicated that
the PCB concentrations hi the samples were less than
10 mg/kg when compared to the Aroclor 1248 standard.
                                                  25
This indicates that a soil sample containing 10 mg/kg of
Aroclor 1221 cannot be identified using the Aroclor
1248 standard.

-------
    Sample 034 was then spiked with 10 mg/kg'of
Aroclor 1254, but because the confirmatory laboratory
indicated that Sample 034 had greater than 10 mg/kg of
PCBs  prior  to  these  samples  being spiked,  no
conclusions can be drawn.

    Sample 040 was spiked with 10 mg/kg of Aroclor
1242.   The results  from the  four spiked  samples
indicated that the PCB concentrations  of the samples
were  greater than  10 mg/kg when  compared to the
Aroclor 1248 standard.

Intramethod Assessment

    Six reagent blanks were prepared and analyzed to
evaluate  laboratory-induced  contamination.    These
samples were taken through all extraction, filtration, and
immunoassay  steps of the analysis.   No PCBs  were
detected in any of the reagent blanks analyzed.

    For this demonstration, completeness refers to the
proportion of valid,  acceptable data generated using the
EnviroGard PCB Test.  Semiquantitative results were
obtained for all of the samples; therefore, completeness
for the samples analyzed by the EnviroGard PCB Test
during the demonstration was  100 percent.

    Intramethod  accuracy   was  assessed  for  the
EnviroGard PCB Test by using PE samples and matrix
spike and matrix spike duplicate samples. Accuracy also
was determined  by  comparing  the  results  of the
technology to those of the confirmatory laboratory. A
discussion of this intennethod accuracy is presented later
in Section 6.

    Each PE sample had a different concentration of
PCBs: one was low and the other was high.   These
samples were extracted and analyzed in exactly the same
manner as  all other soil samples.  The operator knew
that the samples were PE samples but did not know their
true values, nor then' ranges.  The true result for sample
047-4024-114 (the high-level sample) was 110 mg/kg of
Aroclor  1242, with  an acceptance  range of  41 to
150 mg/kg.  The semiquantitative result for this sample
showed that the PCB concentration was greater than the
10 mg/kg Aroclor 1248 standard. The semiquantitative
result, therefore, was acceptable.  The true result for
sample  047-4024-113  (the  low-level  sample)  was
32.7 mg/kg of Aroclor 1242.  The semiquantitative
result for this sample showed that the PCB concentration
was greater than the 10 mg/kg Aroclor 1248 standard.
The  semiquantitative   result,  therefore,  also   was
acceptable.

    Matrix spike samples, prepared by adding a known
quantity of PCBs to a sample,  were used to evaluate the
extraction and analysis efficiency of the technology and
to determine accuracy. Enough Aroclor 1242 was added
to a 5-gram soil sample to  produce a matrix spike
concentration of 25 mg/kg.  The spiked sample  was
duplicated to produce a matrix spike duplicate sample.

    Six matrix spike samples  and six matrix spike
duplicate samples were extracted and analyzed using the
EnviroGard PCB Test.  Semiquantitative results were
compared to the 10 mg/kg Aroclor 1248 standard.  The
results of the soil samples before being spiked showed
that all six samples contained less than 10 mg/kg of
PCBs as determined by the Aroclor 1248 standards. Of
the 12 spiked sample results,  11 were found to contain
greater than  10 mg/kg of PCBs as determined by the
Aroclor 1248 standards. The EnviroGard PCB Test was
able to determine that the matrix spike samples contained
more  than 10 mg/kg of PCBs, as determined from the
Aroclor 1248 standards, in 92 percent of the samples.

    For this demonstration, three types of precision  data
were  generated:  laboratory  duplicate  samples, field
duplicate samples, and matrix spike duplicate samples.
Semiquantitative  results   for  laboratory  and field
duplicate samples are provided in Table 6-2.

    Laboratory duplicate samples are single samples on
which two analyses are performed.  Laboratory duplicate
samples were analyzed after each set of 20  samples
submitted for  analysis.    Five pairs  of  laboratory
duplicate samples and their respective soil samples were
analyzed with the EnviroGard PCB Test.  Field duplicate
samples are two samples collected together but delivered
to the laboratory under separate sample numbers. PRC
collected  32  field  duplicate  samples  during  this
demonstration.   Each  sample and  its  duplicate  was
analyzed by  the technology and by the confirmatory
laboratory.

    Typically, field and laboratory duplicate samples are
used to determine problems with collection and analysis,
not problems with the technology itself. The laboratory
duplicates are compared to a window  of  acceptable
values and if one fell outside that window, corrective
action is taken by the laboratory.  Field duplicates are
used to ensure that contamination of samples does not
occur during sample collection and to set boundaries of
variance due to the lack of homogenization inherent in
soil contamination.

    PRC was tasked, though, not with determining the
precision of those  collecting the samples  or of the
laboratory, but with determining the precision of the
technology itself. To do this, PRC attempted to control
any factor other than those inherent in the technology
that might contribute to a difference between a sample
                                                   26

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                                                  I
 TABLE 6-2.  SEMIQUANTITATIVE RESULTS
 FIELD DUPLICATE SAMPLES.
FOR
LABORATORY AND
Sample Duplicate
Result Result
Sample No. (mg/kg) (mq/kq)
047-4024-001 LD > 10 < 10
047-4024-01 5FD > 10 > 10
047-4024-022FD <10 < 10
047-4024-024FD < 10 < 10
047-4024-028FD < 10 < 10
047-4024-035FD < 10 < 10
047-4024-037FD < 10 < 10
047-4024-040LD > 10 > 10
047-4024-042FD > 10 > 10
047-4024-043FD > 10 > 10
047-4024-046FD < 10 < 10
047-4024-047FD < 10 < 10
047-4024-050FD > 10 > 10
047-4024-060FD > 10 < 10
047-4024-062LD > 10 > 10
047-4024-063FD < 1 .0 < 10
047-4024-069FD < 10 < 10
047-4024-071 FD < 10 < 10
047-4024-081 FD < 10 < 10
Sample
Result
Sample No. (mq/kq)
047-4024-082FD < 10
Of7-4024-083FD < 10
047-4024-084FD > 10
047-4024-085FD > 10
047-4024-086FD < 10
0'7-4024-087FD < 10
0< 7-4024-088FD > 10
0< 7-4024-090FD < 10
0' 7-4024-091 FD > 10
0/7-4024-092FD < 10
O<7-4024-095FD > 10 -
0'7-4024-097FD < 10
047-4024-098FD > 10
047-4024-098LD < 10
047-4024-1 OOFD > 10
I
047-4024-102FD > 10
04 7-4024-1 02LD > 10
04 7-4024-1 09FD < 10

Duplicate
Result
(mg/kg)

::
>10
<10
>10
>10
<10
>10
::
>10
<10.

Notes:
mg/kg   Milligrams per kilogram.
LD     Laboratory duplicate.
FD     Field duplicate.

and  its  duplicate.   To control the  problems usually
detected by laboratory duplicates,  PRC used only one
operator for each technology.  It was assumed that any
variance in that operator's laboratory techniques would
be the same for each sample, and therefore, statistically
insignificant.   For the field duplicates,  PRC put each
sample through a homogenization  process designed to
ensure that there was little  difference between  the
contamination  hi  a  sample and  its   duplicate.
Confirmatory laboratory data on the field duplicates and
their respective  samples indicate that,  overall,  this
technique worked (see Section 4).  Only hi a few sam-
       ples did the homogenization appear not to have been
       complete.

           PRC used both the laboratory and field duplicates to
       determine  the  technology's precision.  Thirty-seven
       duplicate pairs were used  in the  semiquantitative
       evaluation.  Of these 37 duplicate pairs, the EnviroGaird
       PCS Test  produced  the same results  35 times.  One
       laboratory   duplicate,  Sample  001,  and  one  field
       duplicate. Sample 060D, did not agree with their res-
       pective corresponding sample  results.  Based on this
       data, the precision of the EnviroGard PCB Test was

-------
found to be 95 percent, which meets the  criteria for
precision.

    Matrix spike duplicate samples were used to further
evaluate the precision of this technology.  The matrix
spike duplicate sample results were compared to the
matrix spike sample results. The semiquantitative results
for the matrix spike samples  were compared to the
Aroclor 1248 standards supplied by Millipore.  Aroclor
1242 was added to each of the matrix spike samples at a
concentration of 25 mg/kg.  Five of the six matrix spike
duplicate sample results matched those  of the matrix
spike samples. The matrix spike duplicate result for
Sample 024  did  not  match the original matrix spike
sample result. From this data, it was determined that the
precision of the semiquantitative data for the EnviroGard
PCB Test was 83 percent.

Comparison  of  Results  to Confirmatory
Laboratory Results

     The following  sections compare the accuracy and
precision  of  the  semiquantitative   data  from  the
EnviroGard  PCB  Test  to that of the confirmatory
laboratory.     The  results  from  the  confirmatory
laboratory are considered accurate, and its precision is
considered acceptable.  The results are summarized in
Table 6-3 and on Figure 6-1, following the table.

Accuracy

     To measure the accuracy of the EnviroGard PCB
Test, PRC compared the data from the technology to the
data from the confirmatory laboratory by using a 2 by
2 contingency table and a Fisher's Test, as approximated
by a corrected Chi-square statistic.

     To  obtain  semiquantitative  results with  the
technology, its results must be evaluated relative to a set
of points or ranges.  PRC evaluated  the technology's
semiquantitative accuracy in two ways:  using  three
concentrations of Aroclor 1242 standards and using one
concentration of Aroclor 1248  standard.

     Results were statistically evaluated  with two 2 by
2 contingency tables, one for each range,  to compare the
number of times the technology's results indicated results
were within each  range to the number of tunes the
confirmatory laboratory indicated results  were within
that range.  A Fisher's Test, at a 95 percent confidence
level, was then used to determine whether a relationship
 existed between the two sets of results.
Aroclor 1242 Standards (5,10, and 50 mg/kg)

    PRC used three Aroclor 1242 standards to determine
the semiquantitative results of 52 samples. These results
placed the concentration of each sample within one of
four ranges:  (1) less than 5 mg/kg; (2) between 5 and
10 mg/kg; (3) between 10 and 50 mg/kg;  and (4) greater
than 50 mg/kg.  The confirmatory laboratory's results
also were placed within one of these ranges.

    For the first  range,  less than  5 mg/kg,  the
technology indicated that 25 sample results were within
the range and 27 results were above this range.  The
confirmatory laboratory indicated that 39 were within the
range and 13 were above it.  The Fisher's Test showed
that results from the two sets of data were  statistically
different. Since the confirmatory laboratory's data is
assumed to be accurate, the lack of correlation indicates
that within the first range the semiquantitative results
were not accurate when these standards were used.

    For the second range, between 5 and 10 mg/kg, the
technology had no sample results within the range and
52 outside the range. The confirmatory laboratory had
five sample  results within the range and 47 outside the
range. The Fisher's Test indicated that these two sets of
data were statistically different and that within this range
the semiquantitative results were not accurate.

    The technology had 10 results within  the  third
range,  which was  between 10  and 50 mg/kg,  and
42 outside it.  The confirmatory laboratory  had five
results within the  range and 47 outside. The Fisher's
Test indicated that the data was not statistically different.
Therefore, within this range and using these standards,
the semiquantitative results were accurate.

    In the  final range, greater than 50  mg/kg,  the
technology had  17 sample results above that level and
35 below it. The confirmatory laboratory had  three
results above that  level and 49 below it. The Fisher's
Test  indicated that the data was statistically different.
Therefore, within the fourth range, the results from the
technology were not accurate.
   >v
     A comparison of the technology's sample results to
the confirmatory laboratory's results shows that 28 of
52 times the technology was correct, or 53.9 percent of
the time. The other 24 tunes the technology gave false
positive results.  It never gave a false negative result
when the three Aroclor 1242 standards were used.
                                                     28

-------
TABLE 6-3. COMPARISON OF SEMIQUANTITAT VE DATA
CONFIRMATORY LABORATORY.
Sample
No.
001
002
003
004
005
006
007
008
009
010
011
012
013
014
015 .
015D
016
017
018
019
020
021
022
022D
023
024
024D
025
026
027
028
028D
EnviroGard Confirmatory
PCB Test Laboratory
(10mg/kga) (0.033 mg/kga)
>10 0.593
>10 1.50
>10 0.114
>10 6.71J
>10 1.37
> 10 0.679
> 10 0.552
> 10 2.00
>10 1.30J
>10 , 0.172J
>10 1.15J
>10 ND
>10 1.13
> 10 0.18
>10 9.13
> 10 9.84
>10 2,110
> 10 2.55
> 10 45.4
> 10 6.70
> 10 0.068 J
> 10 0.063
>10 • 0.535
> 10 0.718
>10 20.8
> 10 0.055
> 10 0.049
>10 11.7
>10 1.96
> 10 0.057
> 10 0.216
> 10 0.224J
Technology
Accuracy
FP
FP
Correct
FP
FP
FP
FP
FP
FP
FP
FP
Correct
Correct
Correct
FP
FP
Correct
FP
Correct
FP
Correct
Correct
Correct
Correct
Correct
Correct
Correct
FP
Correct
Correct
Correct
Correct
Sample
No.
029
Q30
OJ31
032
qss
034
035
CJ35D
0*36
C37
q37D
C38
C39
C40
C41
C42
C42D
OJ43
044
045
CJ46
CJ46D
I
CJ47
C47D
C48
C49
C50
C50D
CJ51
052
053
FOR ENVIROGARD PCB TEST AND
EnviroGard Confirmatory
PCB Test Laboratory
(10 mg/kga) (0.033 mg/kga)
> 10 0.229J
>10 1.15
> 10 0.263
> 10 47.6
>1+0 6.00J
> 10 34.0
>10 ND
>10 ND
>10 816
> 10 0.055J
> 10 0.040J
>10 1.030J
>10 0.676
> 10 4.25
>10 ND
> 10 0.517
>10 0.462J
>10 1.69J
>10 1.74
> 10 0.592J
>10 ND
> 10 , ND
>10 ND
> 10 0.094J
> 10 0.098J
>10 ND
>10 ND
> 10 3.60
> 10 4.41
>10 ND
>10 4.21
> 10 0.958
Technology
. Accuracy
Correct
Correct
Correct
Correct
FP
Correct
Correct
Correct
Correct
Correct
Correct
Correct
Correct
FP
Correct
FP
FP
FP
FP
Correct
Correct
Correct
Correct
Correct
Correct
Correct
Correct
FP
FP
Correct
FP
Correct
29

-------
TABLE 6-3 (Continued). COMPARISON OF SEMIQUANTITATIVE DATA FOR ENVIROGARD PCB
TEST AND CONFIRMATORY LABORATORY.
Sample
No.
054
055
056
057
058
059
060
060D
061
062
063
063D
064
065
066
067
068
069
069D
070
071
071 D
072
073
074
075
076
077
078
079
080
EnviroGard Confirmatory
PCB Test Laboratory
(10mg/kga) (0.033 mg/kga)
> 10 0.51 6J
> 10 2.40
> 10 0.505
>10 ND
> 10 0.681
> 10 7.86
> 10 0.624 J
> 10 0.577
> 10 580
> 10 2.35
> 10 0.092J
> 10 0.1 54J
> 10 19.0
> 10 3.08
>10 1.98
> 10 0.081
> 10 0.504 J
>10 ND
>10 ND
>10 ND
> 10 0.052J
>10 ND
> 10 0.035J
> 10 15.8
> 10 13.3
> 10 23.0
> 10 46.7
>10 ND
> 10 2.27
> 10 42.8
> 10 3.77
Technology
Accuracy
Correct
Correct
Correct
Correct
Correct
FP
FP
Correct
Correct
FP
Correct
Correct
Correct
FP
Correct
Correct
Correct
Correct
Correct
Correct
Correct
Correct
Correct
Correct
Correct
Correct
Correct
Correct
FP
Correct
Correct
Sample No.
081
081 D
082
082D
083
083D
084
084D
085
085D
086
086D
087
087D
088
088D
089
090
090D
091
091 D
092
092D
093
094
095
095D
096
097
097D
098
EnviroGard Confirmatory
PCB Test Laboratory
(10mg/kga) (0.033 mg/kga)
>10 • 0.687
> 10 0.450
>10 ND
> 10 0.244
> 10 0.484
> 10 0.413
>10 1.16
>10 1.08
> 10 428
> 10 465
>10 1.42
>10 1.25
> 10 0.076
>10 ND
>10 2.70
>10 1.77
> 10 45.0
>10 1.01
>10 1.40
>10 1,630
>10 1,704
>10 1.21
> 10 ND
> 10 0.295
> 10 0.362J
> 10 17.5
>10 31.2
>10 0.059 J
>10 1.23
> 10 0.285
>10 1.17
Technology
Accuracy
Correct
Correct
Correct
Correct
Correct
Correct
FP
FP
Correct
Correct
Correct
Correct
Correct
Correct
FP
FP
Correct
Correct
Correct
Correct
Correct
Correct
Correct
Correct
Correct
Correct
Correct
Correct
Correct
Correct
FP
                                    30

-------
TABLE 6-3 (Continued). COMPARISON OF SEMIpUANTITATIVE DATA FOR ENVIROGARD PCB
TEST AND CONFIRMATORY LABORATORY.    I
Sample
No.
098D
099
100
100D
101
102
102D
103
104
105
Notes:
a
FP
J
ND
NA
EnviroGard Confirmatory
PCB Test Laboratory
(10 mg/kg1) (0.033 mg/kg')
>10 0.825
,>10 ND
>10 177
> 10 167
>10 1.21
>10 293
>10 1.77
> 10 40.3
> 10 7.66
>10 0.210

Technology
Accuracy
FP
Correct
Correct
Correct
FP
Correct
FP
Correct
FP
Correct



'
EnviroGard
Sample PCB Test
No. (10 mg/kg')
106 > 10
107 > 10
108 > 10
1109 >10
109D > 10





Detection limit.
False positive.
Reported amount is below detection limit or not v
PCBs not detected above the detection limit.
The technology, the confirmatory laboratory, or b
110 >10
111 >10
112 >10
113 >10
114 >10

Confirmatory
Laboratory
(0.033 mg/kg')
2.50
14.1J
3.84J
ND
ND
ND
ND
315
14.9
66.3

Technology
Accuracy
Correct
Correct
FP
Correct
Correct
Correct
Correct
Correct
Correct
Correct

alid by approved QC procedures!
3th did not detect PCBs.
FIGURE 6-1. ASSESSMENT OF SEMIQUANTI-
TATIVE ENVIROGARD PCB TEST DATA.

>-
i
|


_ '
X
?



Falsa Positives f * *
* *** * * **
.';%>**'••
True Negatives ^


*» *
... ».
»t » True Positives
• .

False Negatives









E ««J *l f 1* 1M !**• (MM
O
= Confirmatory Laboratory Concentration (mg/kg)
Aroclor 1248 (10 mg/kg standard)

    A  10 mg/kg Aroclor 1248 standard was used to
assess the results of 94 samples. Each sample result was
reported as above 10 mg/kg of PCBs or below 10 mg/kg
of PCBs. The confirmatory laboratory results also were
placed in one of these two ranges.
    The technology obtained 53 sample results below the
10 mg/kg level and 41 above it.  The confirmatory
laboratory obtained  72 results below that  level and
22 above it. The results of the analysis indicated that the
two data sets were  statistically different.   Since the
confirmatory laboratory's data is considered accurate,
the results from the technology, overall, are considered
not accurate when this Aroclor 1248 standard was used,

    Of the 94 results, the technology had 75 correct
results and 19 false  positive results.  Again, no false
negative results were found.

Summary

    Overall, the EnviroGard PCB Test is a conservative
kit when used semiquantitatively.  It is not accurate
when assessed in this mode, but in all cases where its
results did not  match those from  the  confirmatory
laboratory, it produced false positive results.

    False negatives  are the principal  concern with
semiquantitative technologies.  False negative results
could  lead to the belief that soil is  not  contaminated
                                                 t

-------
above an action level when in fact it is. For this reason,
the EnviroGard  PCB Test  is designed  to produce
numerous false positive results, but few false negative
results.

    It should be noted that depending on the situation,
false positive results also can be of concern because they
indicate soil is more  contaminated than it actually is.
This results in more soil being excavated and disposed of
than necessary. This can be costly and does not comply
with the waste minimization policies of many regulatory
agencies.

Precision

    When used to produce semiquantitative results, the
precision  of the  EnviroGard  PCB  Test  cannot be
compared to that of the confirmatory laboratory.

Quantitative Evaluation

    After consulting with both Millipore and EMSL-LV,
PRC  determined that with a minimal  amount of
additional effort the EnviroGard PCB Test's ability to
produce quantitative results could  be evaluated.   This
evaluation, therefore, was included in the demonstration.
The following sections detail its results.  Table 6-4 and
Figure 6-2 summarize the quantitative results.

Theory  of Operation   and  Background
Information

    The   EnviroGard PCB  Test  used  during  the
quantitative analysis was the same as that used during the
semiquantitative analysis with one exception. Instead of
using the three Aroclor 1248  standards supplied by
Millipore to analyze  samples,  PRC used the Aroclor
1242 standards it had prepared. Originally, the three
concentrations of Aroclor  1242 used were  1, 5, and
25  mg/kg.  The 1 mg/kg concentration was  used to
define the detection limit of the technology. However,
a large number of soil  samples analyzed  with these
concentrations required dilution because the response of
the samples was  not  within the response range of the
standards. To decrease the number  of samples requiring
dilution,   the  three concentrations were  changed to
5, 10, and 50 mg/kg.

    Samples were  prepared  for analysis in the same
manner used for  the semiquantitative evaluation.  The
test tube  was  then  placed  into  the  differential
photometer, and the optical density was recorded.

    Quantitative results were obtained for the samples
through the use of standard curves.  These curves were
produced for each set of Aroclor standards used.  The
curves were manually plotted on graph paper.   The
x-axis of the graph represented the PCB concentration in
the sample; the y-axis represented the optical density, or
absorbance, in the sample.  The Aroclor standards and
the negative control sample were plotted on the graph.
A curve was generated by connecting these points.  The
optical density values obtained for each soil sample were
then traced from the y-axis to the intersection of the
standard curve line, then to the x-axis. The point where
this   line  intercepted  the  x-axis   indicated  the
concentration of PCBs in the sample.  Before the results
were reported, calculations were performed as needed to
correct the concentration for any dilutions performed.

    The standard curve produced for each concentration
of the Aroclor  1242 standard resulted in  a relatively
linear curve.   The  curve  had a negative slope.   The
curve resulted in average slope of -0.29. The slope of
the line did vary somewhat  from  analysis  to analysis.
When the lowest standard was 1 mg/kg, the region of the
standard curve  connecting  the lowest concentration
standard and the negative control sample, which was
always  placed  at  the  y-intercept,  changed   slope
dramatically from sample to sample.  When 5 mg/kg
was used  as the lowest standard, the slope of the line
from the 5 mg/kg standard to the y-intercept was not as
dramatic.   This suggests that a 5 mg/kg detection limit
for Aroclor 1242 may be more reliable than the 1 mg/kg
detection limit used  for this demonstration

Operational Characteristics

    The portability, logistical requirements, ease of
operation,  and health and safety requirements for the
EnviroGard PCB Test operated in the quantitative  mode
are the  same as those  detailed earlier  in this section.
The  same operator operated the technology in both
modes, and the costs of the analyses were the same. In
addition to the calibration problems detailed earlier, the
first calibration using the  Aroclor 1242 standards was
unacceptable.  This was attributed to operator error and
the small amount of  standard  required for analysis. The
problem was corrected, and all other calibrations with
these Aroclor standards were acceptable.

Performance Factors

    Quantitative analysis  of soil  samples during this
demonstration was  performed using  1,  5,  25, and
50 mg/kg  Aroclor  1242  standards.   The 50 mg/kg
Aroclor standard   replaced  the  25  mg/kg  Aroclor
standard to reduce  the number of dilutions needed to
obtain quantitative  results.   Throughout  the demon-
stration, the 1 mg/kg Aroclor 1242 standard consistently
caused  a  greater response  than the negative  control
sample, which was expected. Not all samples analyzed
                                                   32

-------

TABLE 6-4. COMPARISON OF
QUANTITATIVE Di
CONFIRMATORY LABORATORY.
Sample
No.
001
002
003
004
005
006
007

008
009
010
011
012
013
014
015
01 5D
016
017
018
019
020
021
022
022D
023
024
024D
025
026
027
028
028D
029
030
031
032
EnviroGard
PCB Test
(1.0 trig/kg")
10
22
2.5
61
30
13
19

16
17
40
24
17
12
20
50
50
300
12
370
29
2.5
1
5
4 "
50
ND
ND
50
14
ND
1
ND
ND
6
6
50
Confirmatory
Laboratory
(0.033 mg/kga) Difference
0.593
1.50
0.114
6.71J
1.37
0.679
0.552

2.00
1.30J
0.1 72J
1.15J
ND
1.13
0.18
9.13
9.84
2,110
2.55
45.4
6.70
0.068J
0.063
0.535
0.718
20.8
0.055
0.049
11.7
1.96
0.057
0.216
0.224J
0.229J
1.15
0.263
47.6
9.4
20.5
2.4
54.3
28.6
12.3
18.5

14.0
15.7
39.8
22.9
NA
10.9
19.8
40.9
40.2
-1,810
9.5
324.6
22.3
2.4
0.9
4.5
3.3
29.2
NA
NA
38.3
12.0
NA
0.8
NA
NA
4.9
5.7
2.4
Relative
Percent
Difference
177.7
174.5
182.6
160.4
182.5
180.1
188.7

155.6
171.6
198.3
181.7
NA
165.6
196.4
138.2
134.2
150.2
129.9
156.3
124.9
189.4
176.3
161.3
139.1
82.5
NA
NA
124.1
150.9
NA
128.9
NA
NA
135.7
183.2
4.9
(
t

'
OA FOR ENVIROGARD PCB TEST AND

Sample
Mo.
)33
034
035
035D
036
637
037D


038

39
040
041
042
(J42D
C|43
CJ43D
044
045
046
Q46D
°
47
047D
J
48
049
0
0
0
0
50
50D
51
52
053
054
055
056
0
o
57
58
OJ59
0
0
3c
po
boo

EnviroGard
PCB Test
(1. Drug/kg')
64S
40S
ND.S
ND.S
2,300
3
4

1,000
5
44
ND
25
9
30
20
2
ND
ND
ND
ND
ND
ND.S
ND
20
30
2
25
15
3
15
4S
ND.S
4
18
17
12

Confirmatory
Laboratory
(0.033 mg/kga)
6.00J
34.0
ND
ND
816
0.055J
0.040J

1.030J
0.676
4.25
ND
0.517
0.462J
1.69J
1.74
0.592J
ND
ND
ND
0.094J
0.098J
ND
ND
3.60
4.41
ND
4.21
0.958
0.51 6J
2.40
0.505
ND
0.681
7.86
0.624J
0.577

Difference
58
6.0
NA
NA
1,484
2.9
3.9

-30
4.3
39.8
NA
24.5
8.5
28.3
18.3
1.4
NA
NA
NA
NA
NA
NA
NA
16.4
25.6
NA
20.8
14.0
2.5
12.6
3.5
NA
3.3
10.1
16.4
11.4

Relative
Percent
Difference
165.7
16.2
NA
NA
95.3
192.8
196.0

3.0
152.4
164.8
NA
191.9
180.5
178.7
168.0
108.6
NA
NA
NA
NA
NA
NA
NA
139.0
148.7
NA
142.3
176.0
141.3
144.9
155.2
NA
141.8
78.4
185.8
181.6


-------
TABLE 6-4 (Continued). COMPARISON
AND CONFIRMATORY LABORATORY.
OF QUANTITATIVE DATA FOR ENVIROGARD PCB TEST
Sample
No.
061
062
063
063D
064
065
066
067
068
069
069D
070
071
071 D
072
073
074
075
076
077
078
079
080
081
081 D
082
082D
083
083D
084
084D
085
EnviroGard
PCB Test
(Long/kg")
470
25
3
3
60
78S
14
2
4
ND
1
ND.S
ND.S
ND,S
2S
40
41
35
40
ND,S
23
70
19S
4
3
ND
ND
1
5S
50
49
370
Confirmatory
Laboratory
(0.033 rag/kg")
580
2.35
0.092J
0.1 54J
19.0
3.08 •
1.98
0.081
0.504J
ND
ND
ND
0.052J
ND
0.035J
15.8
13.3
23.0
46.7
ND
2.27
42.8
3.77
0.687
0.450
ND
0.244
0.484
0.413
1.16
1.08
428
Difference
-110
22.6
2.9
2.8
41.0
74.9
12.0
1.9
3.5
NA
NA
NA
NA
NA
1.9
24.2
27.7
12.0
-6.7
NA
20.7
27.2
15.2
3.3
2.5
NA
NA
0.5
4.6
48.8
48.9
-58
Relative
Percent
Difference
21.0
165.7
188.1
180.5
103.8
184.8
150.4
184.4
155.2
NA
NA
NA
NA
NA
193.1
86.7
102.0
41.4
15.5
NA
164.1
48.2
133.8
141.4
147.8
NA
NA
69.5
169.5
190.9
191.4
14.5
Sample
No.
085D
086
086D
087
087D
088
088D
089
090
090D
091
091 D
092
092D
093
094
095
095D
096
097
097D
098
098D
099
100
100D
101
102
102D
103
104
105
EnviroGard
PCB Test
(1.0mg/kga)
400
14S
15S
6
3
20
23
20
10
8
1,300
1,600
2
2
2
2
10
10
ND
ND
3
46
30
3
400
470
-
30
30
190
54S
ND
Confirmatory
Laboratory
(0.033 mg/kg°)
465
1.42
1.25
0.076
ND
2.70
1.77
45.0
1.01
1.40
1,630
1,704
1.21
ND
0.295
0.362N
17.5
31.2
0.059J
1.23
0.285
1.17
0.825
ND
177
167
1.21
293
1.77
40.3
7.66
0.210
Difference
-65
12.6
13.7
5.9
NA
17.3
21.2
-25
9.0
6.6
-330
-104
0.8
NA
1.7
1.6
-7.5
-21.2
NA
NA
2.7
44.8
29.2
NA
233
303
NA
-263
28.2
149.7
56.3
NA
Relative
Percent
Difference
15.0
163.2
169.2
195.0
NA
152.4
171.4
76.9
163.3
140.4
22.7
6.3
49.2
NA
148.6
138.7
54.5
102.9
NA
NA
165.3
190.1
189.3
NA
77.3
95.1
NA
162.8
177.7
130.0
150.3
NA
                                     ,34

-------
TABLE 6-4 (Continued). COMPARISON
AND CONFIRMATORY LABORATORY.
Sample
No.
106
107
108
109
109D
EnviroGard
PCB Test
(1.0 mg/kg1)
10S
40
19
2
ND
Confirmatory
Laboratory
(0.033 mg/kg')
2.50
14.1J
3.84J
ND
ND
Difference
7.5
25.9
15.1
NA
NA
OF QUAN
Relative
Percent
Difference
120.0
95.7
132.8
NA
NA
TITATIVE DATA FOR ENVIROGARD PCB
Sample
No.
110
111
112
113
114
EnviroGard
PCB Test
(1 .0 mg/kg")
2
ND
220
28
90
Confirmatory
Laboratory
,(0.033 mg/kg")
ND
ND
315
14.9
66.3
TEST
Relative
Percent
Difference Difference
NA
NA
-95
13.1
23.7
NA
NA
35.5
61.0
30.3
 Notes:
J
S
ND
NA
Detection limit.
Reported amount is below detection limit or not va'lid by approved QC procedures.
Sample matrix effects raised detection limits.
PCBs not detected above detection limit.
The technology, the confirmatory laboratory, or bcjth did not detect PCBs.
No sample result obtained.                     |
FIGURE 6-2. ASSESSMENT OF QUANTITATIVE
ENVIROGARD PCB TEST DATA

^l IOOT
1
roGard Concentr
ti
a

False Positives
-

• f • <*l>
.y :.*•
True Negatives
True Positives
•
: " ."
v*-;" .

False Negatives
» «i i » IK iw m
Conlirmatory Laboratory Concentration (mg/kg)




M
were calibrated using the 1 mg/kg Aroclor standard.
However, because the 1 mg/kg Aroclor 1242 standard
appeared correct each time it was used, all quantitative
results reported for the  EnviroGard  PCB Test were
based on a detection limit of 1 mg/kg.

    The  sample  matrix effects noted in the semi-
quantitative  evaluation also were  noticed  during the
quantitative evaluation.  High concentrations of PCBs in
many of the soil samples presented an additional sample
matrix problem in  the quantitative evaluation.  While
these  high  concentrations  had  no   effect  on the
semiquantitative data, the quantitative data was affected.
The samples that exhibited a higher response than the
highest concentration of the Aroclor 1242 standard had
to be  diluted  to obtain results.   The  dilution was
performed by  serially diluting the  sample extract at a
                                              ratio of 1 to 10. If, after the first dilution, the response
                                              still  exceeded  the  response of the highest Aroclor
                                              1242 standard, the sample was diluted again at the same
                                              ratio. This procedure was continued until the response
                                              of the sample fell  within the range of the Aroclor
                                              1242  standards.  Of the  146 total samples  analyzed
                                              during  this  demonstration,  42  required  dilution.
                                              Thirty-seven of these samples fell within the range of the
                                              Aroclor 1242 standards after  only  one  1  to 10 ratio
                                              dilution. The other five samples required a second 1 to
                                              10 ratio dilution to provide a response within the range
                                              of the Aroclor 1242 standards.  When dilutions were
                                              required, the detection limit was raised appropriately.

                                              Specificity

                                                  The specificity of the EnviroGard PCB  Test in the
                                              quantitative mode  was  assessed using  the approach
                                              discussed earlier in this section. Table 6-5 summarizes
                                              the quantitative results of the Aroclor specificity test.

                                                  Sample 077 was spiked with about 10 mg/kg of
                                              Aroclor 1016.  Results ranged from 8 to 12 mg/kg.  The
                                              average percent recovery of the four spiked samples was
                                              92 . percent;  the  standard deviation  of the percent
                                              recovery was 22 percent. The technology's response to
                                              Aroclor 1016 was close to its response to the Aroclor
                                              1242 standards.

                                                  Sample 058 was spiked with 10 mg/kg  of Aroclor
                                              1248.  Results ranged from 8 to 19 mg/kg. The average
                                              percent recovery of the samples was 118 percent; the
                                              standard deviation of the percent recovery was 48 per-
                                                   35

-------
TABLE 6-5. QUANTITATIVE RESULTS FOR THE AROCLOR SPECIFICITY TEST.
Confirmatory
Laboratory Result
Sample No. (mg/kg)
003ARSPA1
003ARSPA2
003ARSPA3
003ARSPA4
012ARSPB1
012ARSPB2
012ARSPB3
012ARSPB4
021ARSPC1
021ARSPC2
021ARSPC3
021ARSPC4
034ARSPD1 ,
034ARSPD2
034ARSPD3
034ARSPD4
040ARSPE1
040ARSPE2
040ARSPE3
040ARSPE4
058ARSPF1
058ARSPF2
058ARSPF3
058ARSPF4
077ARSPG1
077ARSPG2
077ARSPG3
077ARSPG4
0.1
0.1
0.1
0.1
ND
ND
ND
ND
0.06
0.06
0.06
0.06
34.0
34.0
34.0
4.3
4.3
4.3
4.3
4.3
0.7
0.7
0.7
0.7
ND
ND
ND
ND
Soil Sample
Result
(mg/kg)
2.5
2.5
2.5
2.5
17
17
17
17
1
1
1
1
40
40
40
40
44
44
44
44
4
4
4
4
NDJ
NDJ
NDJ
NDJ
Aroclor
Spike
AR1221
AR1221
AR1221
AR1221
AR1260
AR1260
AR1260
AR1260
AR1232
AR1232
AR1232
AR1232
AR1254
AR1254
AR1254
AR1254
AR1242
AR1242
AR1242
AR1242
AR1248
AR1248
AR1248
AR1248
AR1016
AR1016
AR1016
AR1016
Spike Spiked
Amount Sample Result
(mg/kg) (mg/kg)
9.94
9.84
9.92
9.77
9.78
9.80
9.65
9.86
9.98
9.84
9.88
9.82
9.86
9.77
9.77
•9.67
9.88
9.69
9.86
9.75
9.73
io.oo
10.00
9.90
9.65
9.96
9.75
9.90
5
3
2
4
45
36
36
34
10
12
6
8
120
120
120
120
44
28
42
33
8
16
19
19
12
8
8
8
Percent
Recovery
25
5
0
15
286
194
197
172
. 98
111
51
71
811
819
819
827
0
0
0
0
50
120
150
152
124
80
82
81
Notes:

mg/kg  Milligrams per kilogram.
ND     Not detected above the 1 mg/kg detection limit.
J       Detection limit raised to 2 mg/kg due to dilution of sample.
                                                  36

-------
 cent. The response of the technology to the samples
 spiked with the Aroclor 1248 standard was greater than
 its response to the Aroclor 1242 standards.  Three of the
 four  sample  results  were  higher than  that of  the
 10 mg/kg Aroclor 1242 standard.  This suggests that a
 10  mg/kg sample containing Aroclor  1248 should
 produce a  response   greater  than  the  technology's
 response to a 10 mg/kg Aroclor 1242 standard.

     Sample 021 was then spiked with  10 mg/kg of
 Aroclor 1232.  Results ranged from 6 to 12 mg/kg.  The
 average percent recovery of the samples was 83 percent;
 the standard deviation of the percent recovery  was
 27  percent.  Results   indicated that a  soil  sample
 containing 10 mg/kg of Aroclor 1232 should produce a
 response within two times the technology's response to
 die Aroclor 1242 standard.

     Sample 012 was spiked with 10 mg/kg of Aroclor
-.1260.   Results ranged from 34 to 45 mg/kg.   The
 average percent recovery of the samples was 212 per-
 cent; the standard deviation of the percent recovery was
 50 percent. The response of the technology to samples
 containing  Aroclor 1260 was  two to three  times its
 response to the Aroclor 1242 standards. A soil sample
 containing 10 mg/kg of Aroclor 1260 should produce a
 response within two to three tunes its response to a
 10 mg/kg Aroclor 1242 standard.

     Sample 003 was spiked with 10 mg/kg of Aroclor
 1221. Results ranged from 2 to 5 mg/kg.  The average
 percent recovery of the samples was  11  percent; the
 standard deviation of the percent recovery was 11 per-
 cent.  The  response of  the  technology  to samples
 containing Aroclor 1221 was one-fourth, or less, than its
 response to the Aroclor 1242 standards. A soil sample
 containing 10 mg/kg of Aroclor 1221 should produce a
 response equal to or less than one-fourth the response of
 the technology  to a 10 mg/kg Aroclor 1242 standard.

    Sample 034 was found to contain 40 mg/kg of PCBs
 when compared to die Aroclor 1242 standards.  For the
 specificity evaluation,  this sample  was  spiked with
 10 mg/kg  of Aroclor  1254.   The  result  for all  four
 aliquots was 120 mg/kg. The average percent recovery
 of the samples  was 819 percent; the standard deviation
 of die  percent recovery  was  1  percent.    The
 confirmatory laboratory result for Sample 034  was
 34 mg/kg.  This indicates that the high results obtained
 for all four aliquots were caused by the high recoveries
 of Aroclor 1254 in diese samples.

    The response of the technology to Sample 034 may
 have been affected by the  high concentrations of PCBs
 in the soil samples prior to  spiking. Results were nearly
 eight tunes higher  than expected, which suggests  the
  technology is much more sensitive to Aroclor 1254 than
I  to Aroclor 1242.
      Sample 040 was found to contain 44 mg/kg of PCEJs
  when compared  to the Aroclor 1242 standards.  This
  sample was spiked with 10 mg/kg of Aroclor 1242.  Re-
  sults ranged from 28 to 44 mg/kg.  The average percent
  recovery of the  samples was 0 percent; the  standard
  deviation of the percent recovery was 0  percent.  The
  confirmatory laboratory  result for  Sample 040  was
  4.2 mg/kg.  EnviroGard PCB Test result of 44 mg/kg
  does  not  compare well  with die  result from the
  confirmatory laboratory.  It was suspected  that the
  original EnviroGard PCB Test result for this soil sample
  was a false positive result.  The results of the Aroclor
  specificity test seem to support this suspicion.   The
  response of the technology was affected by the high
  concentration of PCBs hi Sample 040. All four spiked
  samples were 0.0 percent, indicating that the 10 mg/kg
  spikes were masked by the high concentration of PCBs
  already hi  the four aliquots.   Because the  original
  EnviroGard PCB Test result for this  sample was much
  greater than the result from the confirmatory laboratory,
  it  is not possible  to  determine  wifli  certainty  die
  technology's specificity to Aroclor 1242.

  Intramethod Assessment

      No PCBs were found hi any of the reagent blanks
  analyzed during either evaluation for this technology.
  Quantitative  results were obtained for all but Sample
  101 because the  soil sample required dilution.   The
  dilution of this sample resulted hi a response comparable
  to the negative' control sample.   This problem was not
  recognized until after die demonstration activities were
  completed. The measure of completeness, therefore, for
  the quantitative analysis was 99 percent.

     Intramethod  accuracy was  assessed using  PE
  samples and matrix spike and  matrix spike duplicate
  samples. The true result for PE sample 047-4024-114
  (die high-level sample)  was 110  mg/kg of Aroclor
  1242, with an acceptance range of 41 to 150  mg/kg.
  The quantitative result for the PE sample was determined
  using the Aroclor 1242 standards prepared by PRC.  The
  actual reported result for this sample when analyzed by
  the EnviroGard PCB Test was 90 mg/kg.  This value-
  was within the acceptance range.  The percent recovery
  for die high-level  PE sample was 82 percent. The true
  result  for  PE sample  047-4024-113  (the  low-level
  sample) was  32.7 mg/kg of Aroclor  1242.  It had an
  acceptance range of 12 to 43 mg/kg.   The quantitative
  result for the PE sample when analyzed was determined.
  with the Aroclor 1242 standards prepared by PRC.  The
  result for this sample when analyzed with die Enviro-
                                                  ,37

-------
Card PCB Test was 28 mg/kg. This value was within
the acceptance range.   The percent recovery for the
low-level PE sample was 86 percent.

    The quantitative recovery results of the matrix spike
and matrix spike duplicate samples are listed in Table
6-6.   They  were evaluated  by comparing them to
Aroclor 1242 standard responses plotted on a standard
curve.  The quantitative results of the soil samples,
before they were spiked, showed that four contained less
than 1 mg/kg of PCBs as determined by the Aroclor
1242 standards.  One soil sample was found to contain
1 mg/kg of PCBs.  Another soil sample was found to
contain 17 mg/kg PCBs.  The average recovery of the
matrix spike samples was 114 percent or 28.5 mg/kg.
The standard deviation of the matrix spike  samples was
40.1  percent or  10.0  mg/kg.    These  results  are
summarized  in Table  6-6.     Following  guidelines
outlined in EPA SW—846 Method 8000, control limits
can be established as ± 2 standard deviations from the
mean percent recovery.  For the matrix spike samples
analyzed  during this  demonstration, the  calculated
control limits ranged from 34  to 194 percent recovery.
All matrix  spike samples analyzed fell within these
control limits. The quantitative accuracy, as measured
by the matrix spike and matrix spike duplicate samples,
therefore, is acceptable.  Based on an evaluation of PE
samples and matrix spike and matrix spike duplicate
samples, the intramethod accuracy of the EnviroGard
PCB Test is acceptable.

    As with the semiquantitative evaluation, three types
of precision data were generated for the quantitative
evaluation: laboratory duplicate samples, field duplicate
samples,  and matrix spike duplicate samples.  Again,
laboratory  and  field  duplicate  samples  were  used
together because the soil samples were homogenized and
only one operator was used.

     Quantitatively, the results of the soil samples ranged
from 1 to 1,300 mg/kg.  The results of the duplicates for
those   samples   ranged  from  2  to  1,600  mg/kg.
Quantitative matrix spike duplicate sample results are
given hi Table  6-6.  Quantitative laboratory and field
duplicate sample results are presented in Table 6-7.

     Even the best technology which determines results
quantitatively can not reproduce its results every time.
Therefore, PRC established control limits like those used
to evaluate laboratory duplicates.  These control limits
were  then  used to  determine whether the difference
between a result from a duplicate and the result from its
 respective sample was  reasonable.  To  establish the
 control limits, all sample pairs  (sample and duplicate)
 that did not produce two positive results were removed
 from  the data  population.  Then, the RPD for each
sample pair was calculated and the mean RPD and
population  standard deviation were determined.   The
lower control limit was set at zero because this would
mean that the results from a duplicate and its respective
soil sample matched perfectly.  The upper control limit
was set by multiplying the standard deviation by two and
adding it to the mean RPD. The RPD of each sample
pair was then compared to these control limits.  Each
RPD was expected to fall within the control limits.  If
greater  than 95  percent fell  within  this range,  the
technology's precision was considered adequate. If fewer
than 95 percent fell within this range, the data was
reviewed, and if no explanation  could be found, the
technology's precision was  considered inadequate.

    The EnviroGard PCB Test had 27 sample pairs in
which both a sample  and its  duplicate had positive
results.  The data from these sample pairs had a mean
RPD of 29 percent and  a standard deviation of 31. The
control limits were, therefore,  set at 0 and 92 percent.
All but two of the 27 RPDs fell within the control limits.
The first of these two sample pairs was Sample 042 and
Sample 042D, which had results of 25 and 9 mg/kg,
respectively. This  resulted in an RPD of 94 percent,
2 percent above the upper control  limit.  The second of
the two sample pairs was Sample 083 and 083D,  which
had results of 1 and 5 mg/kg, respectively.  This resulted
in an RPD of 133 percent, 41 percent above  the upper
control limit. Still, 91.5 percent of the sample pairs had
RPDs within the control limits. While  91.5 percent is
not  between the demonstration's  acceptable range of
95 to 100 percent, the  technology only had two sample
pairs not within the control limits.  If one more pair had
been accurate,  the percentage  acceptable would have
been 96.3.  Because so few pairs were  involved hi the
statistical  evaluation,   this percentage was  deemed
acceptable.

     The quantitative results for the matrix spike samples
were compared to the Aroclor 1242 standards prepared
by PRC. Precision of the matrix spike duplicate samples
was evaluated through the RPD of the matrix spike result
compared to the matrix spike duplicate result. RPD is
the difference between these two  results divided by the
mean of the two results,  expressed as a percentage.
RPD values for the six matrix spike samples ranged
from 0 to 90 percent. The  mean RPD value from these
six samples was 29 percent, and the standard deviation
was 34 percent.  If an upper control limit of two times
the  standard deviation is used, the upper  control limit
was 97 percent.  All RPD values for the matrix spike
 duplicate  samples  fell   within  this  range   (Table
 6-6). Therefore, based on the three types of intramethod
 precision data generated, the precision of the EnviroGard
 PCB Test is acceptable when used quantitatively.
                                                    38

-------
 TABLE 6-6. QUANTITATIVE MATRIX SPIKE AND MATRIX SPIKE DUPLICATE RESULTS.
Sample No.
047-4024-012
047-4024-024
047-4024-049
047-4024-069D
047-4024-082
047-4024-111
Sojl Sample
Result
(mg/kg)
17
ND
ND ,
1.0
ND
ND
Matrix Spik<
Amount
(mg/kg)
25
25
25
25
25
25
i Matrix Spike
Recovery
112
136
96
84
64
184
Matrix Spike
Duplicate
Recovery
100
76
84
84
168
176
RPD
11
57
13
0
90
4
  Notes:                                             !

  mg/kg   Milligrams per kilogram.
  ND     Not detected above the detection limit of 1 mg/kg.
 Comparison  of  Results   to   Confirmatory
•Laboratory Results

     The quantitative results of the EnviroGard PCB Test
 were analyzed by using the linear regression techniques
 detailed hi Section 4.   The initial linear regression
 analysis was based on results from 89 samples.  The
 other results indicated that no PCBs were detected above
 the detection limit 1.0 mg/kg. The r2 for this regression
 was 0.45, indicating that little or no relationship exists
 between the data sets. Therefore, the technology is not
 accurate.   A residual analysis  of the data,  though,
 identified that the r2 was greatly influenced by the results
 for Samples 16, 18, 38,  91, and 100.  All of these
 samples show high  levels of contamination.   PRC
 removed these six points as outliers and recalculated the
 linear regression.

    When the regression was recalculated on the 83 re-
 maining sample results,  it  defined  an r2 factor  of
 0.87, indicating that a  relationship did exist between the
 two data sets.  The regression line that was calculated
 had a  y-intercept  of 17.8  mg/kg and  a slope  of
 0.76. The normal deviate test statistic, though, indicated
 that the slope  of 0.76 is significantly different from
 1, and  the y-intercept of 17.8 mg/kg is  significantly
 different from 0.  This means that the results from this
 technology are not accurate. However, if 10 to 20 per-
 cent of the  soil samples were sent to a confirmatory
laboratory, then the results from the other 80 to 90 per-
cent  could be  corrected.    This could  result in  a
significant savings in analytical costs.

    The Wilcoxon Signed Ranks Test was used to verify
these results.  It indicated, at a 95 percent confidence
level,  that the  EnviroGard  PCB Test's  data  was
significantly different from that  of the confirmatory
laboratory. This confirmed the linear regression analysis
and indicated that the EnviroGard PCB Test's data was
not accurate.

    To compare the precision of the EnviroGard PCB
Test's results  to  the precision of the  confirmatory
laboratory's results, a Dunnett's Test was performed on
the RPDs determined from the field duplicate samples
and  their  respective samples.   The  Dunnett's Test
determines the probability that the data sets on which it
is based  are  the same.    If the RPDs  from the
confirmatory laboratory and those from the technology
are the same, then it can be  assumed that the precisions
are also similar.  Dunnett's Test results in a percentage.
For this demonstration,  probabilities above 95 percent
indicate that the precision of the technology and  that of
the confirmatory laboratory are considered the  same.
When the Dunnett's Test compared the RPDs between
the EnviroGard PCB Test's data and the confirmatory
laboratory's data, a probability of 97,5 percent resulted.
This indicates  that the technology is as precise  as the
confirmatory laboratory.

                                                   39

-------
TABLE 6-7. QUANTITATIVE LABORATORY AND FIELD DUPLICATE SAMPLE RESULTS.
Soil Duplicate
Sample Sample
Result Result
Sample No. (mg/kg) (mg/kg)
047-4024-001 LD 10
047-4024-01 5FD 50
047-4024-022FD 5
047-4024-024FD ND
047-4024-028FD 1
047-4024-035FD ND. J
047-4024-037FD 3
047-4024-040LD 40
047-4024-042FD 25
047-4024-043FD 30
047-4024-046FD ND
047-4024-047FD ND
047-4024-050FD 20
047-4024-060FD 17
047-4024-062LD 25
047-4024-063FD 3
047-4024-069FD ND
047-4024-071 FD ND, J .
047-4024-081 FD 4
Notes:
5
50
4
ND
ND
ND
4
44
9
20
ND
ND
30
12
21
3
1
ND
3

Relative
Percent
Difference
(%)
67
0
22
NA
NA
NA
29
10
94
40
NA
NA
40
34
17
0
NA
NA
29
Sample No.
047-4024-082FD
047-4024-083FD
047-4024-084FD
047-4024-085FD
047-4024-086FD
047-4024-087FD
047-4024-088FD
047-4024-090FD
047-4024-091 FD
047-4024-092FD
047-4024-095FD
047-4024-097FD
047-4024-098FD
047-4024-098LD
047-4024-1 OOFD
047-4024-1 02FD
047-4024-1 02LD
047-4024-1 09FD


Soil
Sample
Result
(mg/kg)
ND
1
50
370
14
6
20
10
1,300
2
10
ND
46
46
400
30
30
2

\
Duplicate
Sample
Result
(mg/kg)
ND
5
49
400
15
3
23
8
1,600
2 i
10
3
30
31
470
30
41
ND


Relative
Percent
Difference
(%)
NA
133
2
8
7
B7
•I 4
21
:>1
0
• 0
NA
42
39
16
0 ~
31
NA


mg/kg Milligrams per kilogram.
LD Laboratory duplicate.
FD Field duplicate.
ND Not detected above the 1 mg/kg detection limit.
NA Not analyzed; the sample, duplicate, or both did not contain PCBs.
J Detection limit raised to 2 mg/kg due to dilution of sample.
                                    40

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                                               Secti on 7
                                     Applications Assessment
    The EnviroGard PCB Test can be operated in either
a semiquantitative or quantitative mode. In either mode,
it  is relatively inexpensive and easy to operate.  The
technology involves a number of different steps, which
increases the chance of operator  error.  In particular,
errors can occur during measurements because of the
small quantities of Aroclor standards and samples used.
For this reason, operators must be thoroughly trained.
Experience in common laboratory practices is helpful,
although  the  technology  can still be  operated  by
nontechnical personnel.

    The technology is very portable.   Electricity is
required to operate it;  however,  electricity can  be
supplied by a rechargeable battery. Reagents used with
the technology must be refrigerated.   It  has a high
sample throughput  and is capable of quickly providing
results, particularly when used in the semiquantitative
mode.   The  ability  of the technology  to  provide
quantitative results is an additional advantage.  When it
is used hi the quantitative mode, however, samples must
frequently be diluted to bring their PCB concentrations
into the linear range of the technology.

    The EnviroGard PCB Test has slight reactions to
some contaminants other than PCBs, such as halogenated
                                                   41
organic compounds.  For this reason, the technology
does not appear to be highly susceptible to false positive
results due  to interferants, unless the interferants are
present in very high concentrations (generally above 200
mg/kg depending on the interferant). The technology
also did not appear prone to  produce  false negative
results.

    The results of the Aroclor specificity test indicated
that the EnviroGard PCB Test will react differently to
different Aroclors.   However, Millipore can provide
Aroclor-specific standards if the Aroclor of concern is
known.    When used with the correct standard, the
technology can provide semiquantitative or quantitative
results for each Aroclor.

    The  EnviroGard   PCB   Test   can   provide
semiquantitative or quantitative results at sites where the
Aroclor of  concern is positively  known so that the
appropriate Aroclor standard can be used. If the Aroclor
is  known and if no interferants are suspected to be
present at high concentrations, this technology would be
useful at  sites where results are needed  quickly.  If
quantitative results are required, the quantitative results
reported by the technology must be corrected if there is
a need for them to be accurate.

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                                             Section 8
                                            References
Department of Energy  (DOE).  1989.  "RCRA Facility Investigation and Corrective Measures  Study for the
        Abandoned Indian Creek Outfall."  Albuquerque Operations Office, Environment and Health Division,
        Environmental  Programs Branch, Kansas City Plant.

Draper, N. R., and H. Smith. 1981. Applied Regression Analyses.  John Wiley & Sons, Inc.  New York. 2nded.

Environmental Protection Agency (EPA). 1989. "Preparing Perfect Project Plans." U.S. Environmental Protection
        Agency.  Cincinnati, OH.  EPA/600/9-89/087.

Pearson, E. S. and H. O. Hartley.  1976. Biometrika Tables for Statisticians.  Charles Griffin and Company, Ltd.
        Third edition with corrections.

PRC Environmental Management,  Inc. (PRC). 1992a. "SITE Demonstration: EnSys, Inc., Immunosystems, and
        Dexsil Corporation, PCB Field Kits, Pre-Demonstration Sampling Plan." May.

—.  1992b.  "Final Demonstration Plan and Quality Assurance Plan for Demonstration of PCB Immunoassay and
        Field Screening Technologies."  July 24.

Stanley, T. W. and S. S. Veraer.  1983.  "Interim Guidelines and Specifications for Preparing Quality Assurance
        Project Plans." U.S. Environmental Protection Agency, Washington D.C.  EPA/600/4-83/004.
                                                  42
* U.S. GOVERNMENT PRINTING OFFICE:  1995-653-291

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