United States Office of Research and EPA/600/R-98/1173

Environmental Protection Development December 1998

Agency Washington, D.C. 20460

Environmental Technology

Verification Report

Immunoassay Kit

EnviroLogix, Inc.

PCB in Soil Tube Assay
Superfund Innovative Technology

Evaluation Program

EPA/600/R-98/173

December 1998

Environmental Technology

Verification Report

Immunoassay Kit

EnviroLogix, Inc.

PCB in Soil Tube Assay

By

Amy B. Dindal

Charles K. Bayne, Ph.D.

Roger A. Jenkins, Ph.D.

Oak Ridge National Laboratory

Oak Ridge Tennessee 37831-6120

Eric N. Koglin

U.S. Environmental Protection Agency

Environmental Sciences Division

National Exposure Research Laboratory

Las Vegas, Nevada 89193-3478

This demonstration was conducted in cooperation with 

U.S. Department of Energy

David Bottrell, Project Officer

Cloverleaf Building, 19901 Germantown Road

Germantown, Maryland 20874
ii

Notice

The U.S. Environmental Protection Agency (EPA), through its Office of Research and Development

(ORD), and the U.S. Department of Energy’s Environmental Management (EM) Program, funded and

managed, through Interagency Agreement No. DW89937854 with Oak Ridge National Laboratory, the

verification effort described herein. This report has been peer and administratively reviewed and has been

approved for publication as an EPA document. Mention of trade names or commercial products does not

constitute endorsement or recommendation for use of a specific product.
EPA-VS-SCM-29 The accompanying notice is an integral part of this verification statement. December 1998

iii

TECHNOLOGY TYPE: POLYCHLORINATED BIPHENYL (PCB) FIELD ANALYTICAL

TECHNIQUES

APPLICATION: MEASUREMENT OF PCBs IN SOILS AND SOLVENT EXTRACTS

TECHNOLOGY NAME: PCB IN SOIL TUBE ASSAY

COMPANY: ENVIROLOGIX INC.

ADDRESS: 55 INDUSTRIAL WAY

PORTLAND, ME 04103

PHONE: (207) 797-0300

UNITED STATES ENVIRONMENTAL PROTECTION AGENCY 

Office of Research and Development

Washington, D.C. 20460

ENVIRONMENTAL TECHNOLOGY VERIFICATION PROGRAM

VERIFICATION STATEMENT

The U.S. Environmental Protection Agency (EPA) has created a program to facilitate the deployment of innovative

technologies through performance verification and information dissemination. The goal of the Environmental Technology

Verification (ETV) Program is to further environmental protection by substantially accelerating the acceptance and use

of improved and more cost-effective technologies. The ETV Program is intended to assist and inform those involved in

the design, distribution, permitting, and purchase of environmental technologies. This document summarizes the results

of a demonstration of EnviroLogix Inc. PCB in Soil Tube Assay.

PROGRAM OPERATION

EPA, in partnership with recognized testing organizations, objectively and systematically evaluates the performance of

innovative technologies. Together, with the full participation of the technology developer, they develop plans, conduct

tests, collect and analyze data, and report findings. The evaluations are conducted according to a rigorous demonstration

plan and established protocols for quality assurance. EPA’s National Exposure Research Laboratory, which conducts

demonstrations of field characterization and monitoring technologies, with the support of the U.S. Department of

Energy’s (DOE) Environmental Management (EM) program, selected Oak Ridge National Laboratory (ORNL) as the

testing organization for the performance verification of polychlorinated biphenyls (PCBs) field analytical techniques.

DEMONSTRATION DESCRIPTION 

In July 1997, the performance of six PCB field analytical techniques was determined under field conditions. In September

1998, the performance of EnviroLogix Inc.’s PCB in Soil Tube Assay kit was evaluated similarly. Each technology was

independently evaluated by comparing field analysis results with those obtained using approved reference methods.

Performance evaluation (PE) samples were also used to assess independently the accuracy and comparability of each

technology.

The demonstration was designed to detect and measure PCBs in soil and solvent extracts. For EnviroLogix, the

demonstration was conducted at ORNL in Oak Ridge, Tennessee, from September 21 through 25, 1998. The study was

conducted under two environmental conditions. The first site was outdoors, with naturally fluctuating temperatures and

relative humidity conditions. The second site was inside a controlled environmental chamber, with generally cooler

temperatures and lower relative humidities. Multiple soil types, collected from sites in Ohio, Kentucky, and Tennessee,

were analyzed in this study. Solutions of PCBs were also analyzed to simulate extracted surface wipe samples. The

results of the soil and extract analyses conducted under field conditions by the technology were compared with results

from analyses of homogenous replicate samples conducted by conventional EPA SW-846 methodology in an approved
EPA-VS-SCM-29 The accompanying notice is an integral part of this verification statement. December 1998

iv

reference laboratory. Details of the demonstration, including a data summary and discussion of results, may be found

in the report entitled Environmental Technology Verification Report: Immunoassay Kit, EnviroLogix Inc., PCB in Soil

Tube Assay, EPA/600/R-98/173.

TECHNOLOGY DESCRIPTION

The EnviroLogix PCB in Soil Tube Assay applies the principles of enzyme linked immunosorbent assay (ELISA) to the

determination of PCB. In such an assay, an enzyme has been chemically linked to a PCB molecule or PCB analog to

create a labeled PCB reagent. The labeled PCB reagent (called a conjugate) is mixed with an extract of native sample

containing the PCB contaminant. A portion of the mixture is applied to a surface (i.e., the inside of a test tube) to which

an antibody specific for PCB has been affixed. The native PCB and PCB-enzyme conjugate compete for a limited

number of antibody sites. After a period of time, the solution is washed away, and what remains is either PCB-antibody

complexes or enzyme-PCB-antibody complexes attached to the test surface. The proportion of the two complexes on

the test surface is determined by the amount of native PCB in the original sample. The enzyme present on the test surface

is used to catalyze a color change reaction in a solution added to the test surface. Because the amount of enzyme present

is inversely proportional to the concentration of native PCB contaminant, the amount of color development is inversely

proportional to the concentration of PCB contaminant. The color development is quantified through the use of a hand-held

photometer.

The EnviroLogix PCB in Soil Tube Assay is designed for semi-quantitative field screening for PCBs in soil. The kit is

supplied with calibrators equivalent to 1 part per million (ppm) and 10 ppm PCB (Aroclor 1254) in soil. These

calibrators are used to evaluate threshold levels of 1 and 10 ppm. A threshold level of 50 ppm can also be evaluated

using the 10 ppm calibrator by preparing a 1:5 sample extract dilution into methanol. For the extract samples, the

threshold levels are 0.4, 4, and 20 μg/mL. 

VERIFICATION OF PERFORMANCE

The following performance characteristics of the PCB in Soil Tube Assay were observed:

Throughput: Throughput was 8 samples/hour under outdoor conditions and 7 samples/hour under chamber conditions

for one operator. This rate included sample preparation and analysis.

Ease of Use: One operator analyzed samples during the demonstration. Minimal training (4 h) is required to operate the

kit, provided the user has a fundamental understanding of basic chemical and field analytical techniques. 

Completeness: The PCB in Soil Tube Assay generated results for all 232 PCB samples for a completeness of 100%.

False positive/negative results: All of the blank samples (soils and extracts) were reported as the lowest reporting

interval, which included zero; therefore, the percentage of false positive results was 0%. The kit reported no false negative

results for extracts, and 4% (7 of 192 samples) for soils.

Precision: The overall precision—based on the percentage of combined sample sets where all four replicates were

reported as the same interval—was 56% for the PE soils, 68% for the environmental soils, and 75% for the extracts. 

Accuracy: Accuracy was assessed using PE soil and extract samples. Accuracy, defined as the percentage of the PCB

in Soil Tube Assay results that agreed with the accepted concentration, was 78% for PE soils and 92% for extracts. In

general, the fraction of samples that was biased high was comparable (10% for PE soils and 0% for extracts) to the

fraction that was biased low (13% for PE soils and 8% for extracts).

Comparability: Comparability, like accuracy, was defined as the percentage of results that agreed with, was above (i.e.,

biased high), or was below (i.e., biased low) the reference laboratory result. The percentage of samples that agreed with

the reference laboratory results was 82% for all soils (PE and environmental). The fraction of samples that was biased
EPA-VS-SCM-29 The accompanying notice is an integral part of this verification statement. December 1998

v

NOTICE: EPA verifications are based on an evaluation of technology performance under specific, predetermined criteria and the

appropriate quality assurance procedures. EPA makes no expressed or implied warranties as to the performance of the technology and

does not certify that a technology will always, under circumstances other than those tested, operate at the levels verified. The end user

is solely responsible for complying with any and all applicable Federal, State, and Local requirements.

high was again comparable (12%) to the fraction that was biased low (7%). Extract results could not be compared

because no reference laboratory data was generated for these samples.

Regulatory Decision-making: One objective of this demonstration was to assess the technology’s ability to perform at

regulatory decision-making levels for PCBs, specifically 50 ppm for soils. For PE and environmental soil samples in the

range of 40 to 60 ppm, 66% of the PCB in Soil Tube Assay results agreed with the reference laboratory, 32% were

biased high, and 2% were biased low. The test kit results for this concentration range were different from what was

observed for the entire data set in that the fraction of samples that were biased high was significantly higher (32% versus

12%). 

Data quality levels: The performance of the test kit was characterized as unbiased, because most (78%) of the PCB in

Soil Tube Assay results agreed with the certified PE values, but imprecise, because nearly half (44%) of the PE replicate

results were not reported as the same interval. It should be noted that almost all of the imprecision occurred when the

concentration of the sample was near one of the test kit’s threshold values (i.e., 1, 10, or 50 ppm).

The results of the demonstration show that the PCB in Soil Tube Assay can provide useful, cost-effective data for

environmental problem-solving and decision-making. Undoubtedly, it will be employed in a variety of applications,

ranging from serving as a complement to data generated in a fixed analytical laboratory to generating data that will stand

alone in the decision-making process. As with any technology selection, the user must determine if this technology is

appropriate for the application and the project data quality objectives. For more information on this and other verified

technologies, visit the ETV web site at http://www.epa.gov/etv.

Gary J. Foley, Ph.D.

Director

National Exposure Research Laboratory

Office of Research and Development
vi
vii

Foreword

The U.S. Environmental Protection Agency (EPA) is charged by Congress with protecting the nation’s natural

resources. The National Exposure Research Laboratory (NERL) is EPA’s center for the investigation of

technical and management approaches for identifying and quantifying risks to human health and the

environment. NERL’s research goals are to (1) develop and evaluate technologies for the characterization and

monitoring of air, soil, and water; (2) support regulatory and policy decisions; and (3) provide the science

support needed to ensure effective implementation of environmental regulations and strategies. 

EPA created the Environmental Technology Verification (ETV) Program to facilitate the deployment of

innovative technologies through performance verification and information dissemination. The goal of the ETV

Program is to further environmental protection by substantially accelerating the acceptance and use of

improved and cost-effective technologies. The ETV Program is intended to assist and inform those involved

in the design, distribution, permitting, and purchase of environmental technologies. This program is

administered by NERL’s Environmental Sciences Division in Las Vegas, Nevada.

The U.S. Department of Energy’s (DOE’s) Environmental Management (EM) program has entered into active

partnership with EPA, providing cooperative technical management and funding support. DOE EM realizes

that its goals for rapid and cost-effective cleanup hinge on the deployment of innovative environmental

characterization and monitoring technologies. To this end, DOE EM shares the goals and objectives of the

ETV.

Candidate technologies for these programs originate from the private sector and must be commercially ready.

Through the ETV Program, developers are given the opportunity to conduct rigorous demonstrations of their

technologies under realistic field conditions. By completing the evaluation and distributing the results, EPA

establishes a baseline for acceptance and use of these technologies. 

Gary J. Foley, Ph.D.

Director

National Exposure Research Laboratory

Office of Research and Development

ix

Abstract

In July 1997, the U.S. Environmental Protection Agency (EPA) conducted a demonstration of polychlorinated

biphenyl (PCB) field analytical techniques. The purpose of this demonstration was to evaluate field analytical

technologies capable of detecting and quantifying PCBs in soils and solvent extracts. The fundamental

objectives of this demonstration were (1) to obtain technology performance information using environmental

and quality control samples, (2) to determine how comparable the developer field analytical results were with

conventional reference laboratory results, and (3) to report on the logistical operation of the technology. The

demonstration design was subjected to extensive review and comment by EPA’s National Exposure Research

Laboratory (NERL) Environmental Sciences Division in Las Vegas, Nevada; Oak Ridge National Laboratory

(ORNL); EPA Regional Offices; the U.S. Department of Energy (DOE); and the technology developers.

The demonstration study was conducted at ORNL under two sets of environmental conditions. The first site

was outdoors, with naturally variable temperature and relative humidity conditions typical of eastern Tennessee

in the summer. A second site was located inside a controlled environmental chamber having lower, and

relatively stable, temperature and relative humidity conditions. The test samples analyzed during this

demonstration were performance evaluation (PE) soil, environmental soil, and extract samples. Actual

environmental soil samples, collected from sites in Ohio, Kentucky, and Tennessee, were analyzed and ranged

in concentration from 0.1 to 700 parts per million (ppm). Extract samples were used to simulate surface wipe

samples, and were evaluated at concentrations of 0, 10, and 100 μg/mL. The reference laboratory method used

to evaluate the comparability of data was EPA SW-846 Method 8081.

In September 1998, EnviroLogix’s PCB in Soil Tube Assay was evaluated. Six other field analytical

technologies were tested in July 1997: the L2000 PCB/Chloride Analyzer (Dexsil Corporation), the PCB

Immunoassay Kit (Hach Company), the 4100 Vapor Detector (Electronic Sensor Technology), and three

immunoassay kits—D TECH, EnviroGard, and RaPID Assay System (Strategic Diagnostics Inc.). The

purpose of an Environmental Technology Verification Report (ETVR) is to document the demonstration

activities, present demonstration data, and verify the performance of the technology. This ETVR presents

information regarding the performance of EnviroLogix’s PCB in Soil Tube Assay. Separate ETVRs have been

published for the other technologies demonstrated.

The PCB in Soil Tube Assay is an immunoassay kit used to determine PCB concentrations as interval results.

The test kit uses a competitive binding enzyme immunoassay to perform rapid testing for PCBs in soils and

solutions at specified threshold values of 1, 10, and 50 ppm. The test kit is standardized using Aroclor 1254.

The presence of PCBs is detected by a photometer based on a colored reaction in which the color development

is inversely proportional to the concentration of PCB in the sample (e.g., the darker the color, the less analyte

PCB is present in the sample). The kit provides no information on Aroclor identification.

The kit’s quantitative results were based on the analysis of calibration standards with every batch of 12 to 17

samples. Because the test kit is an interval technique, method detection limits are not applicable. Precision,

defined as the percentage of the sample sets where all four replicates were reported as the same interval range,
x

was 56% for PE soils, 68% for environmental soils, and 75% for extracts. Accuracy, defined as the percentage

of PCB in Soil Tube Assay results that agreed with the accepted concentration, was 78% for PE soils and 92%

for extracts. In general, the percentage of samples that was biased high was comparable (10% for PE soils and

0% for extracts) to the percentage that was biased low (13% for PE soils and 8% for extracts). Comparability

was defined similarly to accuracy, but the test kit result was compared with the reference laboratory result

rather than with the accepted concentration to determine comparability. For all soil samples (PE and

environmental), the percentage of samples that agreed with the reference laboratory results was 82%. The

percentage of samples that was biased high was again comparable (12%) to the percentage that was biased

low (7%). Comparability could not be assessed for extract samples because no reference laboratory data were

generated for these samples.

The demonstration found that the PCB in Soil Tube Assay was simple to operate in the field, requiring about

an hour for initial setup and preparation for sample analysis. Once the kit was operational, the sample

throughput of the kit by a single analyst was 8 samples/hour under outdoor conditions and 7 samples/hour

under chamber conditions. Minimal training (4 hours) is required to operate the test kit, provided the user has

a fundamental understanding of basic chemical and field analytical techniques. The performance of the test kit

was characterized as unbiased, because most (78%) of the PCB in Soil Tube Assay results agreed with the

certified PE values, but imprecise, because nearly half (44%) of the PE replicate results were not reported as

the same interval. It should be noted that almost all of the imprecision occurred when the concentration of the

sample was near one of the test kit’s threshold values (i.e., 1, 10, or 50 ppm). The test kit had no false positive

results (i.e., a result in which the technology detects PCBs in the sample above the detection limit when there

actually are no PCBs present), and 4% of the soil sample results were false negatives (i.e., the technology

indicates that there are no PCBs present in the sample, when there actually are). For extract samples, the test

kit had no false positive or false negative results.
xi

Table of Contents

Notice ....................................................................... ii

Verification Statement .......................................................... iii

Foreword .................................................................... vii

Abstract .................................................................... ix

List of Figures ................................................................ xv

List of Tables ............................................................... xvii

List of Abbreviations and Acronyms .............................................. xix

Acknowledgments ............................................................ xxi

Section 1 — Introduction ............................................................ 1

Technology Verification Process ................................................... 2

Needs Identification and Technology Selection ...................................... 2

Demonstration Planning and Implementation ....................................... 3

Report Preparation .......................................................... 3

Information Distribution ...................................................... 3

Demonstration Purpose .......................................................... 4

Section 2 — Technology Description ................................................... 5

Objective ..................................................................... 5

Principle ..................................................................... 5

Applications and Advantages ...................................................... 5

Procedure .................................................................... 6

Materials .................................................................. 6

Extraction ................................................................. 6

Assay .................................................................... 6

Interpreting Results .......................................................... 7

Precautions and Notes ........................................................ 8

Sensitivity and Cross-Reactivity ................................................ 8
xii

Section 3 — Site Description and Demonstration Design .................................... 9

Objective ..................................................................... 9

Demonstration Site Description .................................................... 9

Site Name and Location ....................................................... 9

Site History ................................................................ 9

Site Characteristics ......................................................... 10

Experimental Design ........................................................... 10

Environmental Conditions during Demonstration ...................................... 13

Sample Descriptions ........................................................... 13

Performance Evaluation Materials .............................................. 13

Environmental Soil Samples .................................................. 13

Extract Samples ........................................................... 14

Sampling Plan ................................................................ 14

Sample Collection .......................................................... 14

Sample Preparation, Labeling, and Distribution .................................... 14

Predemonstration Study and Results ............................................... 16

Deviations from the Demonstration Plan ............................................ 16

Section 4 — Reference Laboratory Analytical Results and Evaluation ......................... 19

Objective and Approach ......................................................... 19

Reference Laboratory Selection ................................................... 19

Reference Laboratory Method .................................................... 20

Calibration ............................................................... 20

Sample Quantification ....................................................... 20

Sample Receipt, Handling, and Holding Times ..................................... 21

Quality Control Results ......................................................... 21

Objective ................................................................. 21

Continuing Calibration Verification Standard Results ............................... 22

Instrument and Method Blank Results ........................................... 22

Surrogate Spike Results ...................................................... 22

Laboratory Control Sample Results ............................................. 23

Matrix Spike Results ........................................................ 23

Conclusions of the Quality Control Results ....................................... 23

Data Review and Validation ...................................................... 24

Objective ................................................................. 24

Corrected Results .......................................................... 24

Suspect Results ............................................................ 24

Data Assessment .............................................................. 25

Objective ................................................................. 25

Precision ................................................................. 26

Performance Evaluation Samples ............................................ 26

Environmental Soil Samples ............................................... 27

Extract Samples ........................................................ 27
xiii

Accuracy ................................................................ 27

Representativeness ......................................................... 29

Completeness ............................................................. 30

Comparability ............................................................. 30

Summary of Observations ....................................................... 30

Section 5 — Technology Performance and Evaluation ..................................... 33

Objective and Approach ......................................................... 33

Interval Reporting ............................................................. 33

Data Assessment .............................................................. 33

Objective ................................................................. 33

Precision ................................................................. 34

Performance Evaluation Samples ............................................ 34

Environmental Soil Samples ............................................... 35

Extract Samples ........................................................ 37

Precision Summary ...................................................... 37

Accuracy ................................................................. 37

Performance Evaluation Soil Samples ........................................ 38

Extract Samples ........................................................ 39

False Positive/False Negative Results ........................................ 40

Representativeness ......................................................... 41

Completeness ............................................................. 41

Comparability ............................................................. 41

Summary of PARCC Parameters .................................................. 42

Regulatory Decision-Making Applicability ........................................... 42

Additional Performance Factors ................................................... 44

Sample Throughput ......................................................... 44

Cost Assessment ........................................................... 44

PCB in Soil Tube Assay Costs ............................................. 45

Reference Laboratory Costs ............................................... 46

Cost Assessment Summary ................................................ 47

General Observations ....................................................... 47

Performance Summary ......................................................... 48

Section 6 — Technology Update and Representative Applications ............................ 51

Objective .................................................................... 51

Technology Update ............................................................ 51

Representative Applications ...................................................... 51

Data Quality Objective Example .................................................. 51

Section 7 — References ............................................................ 53
xiv

Appendix A — Description of Environmental Soil Samples ................................. 55

Appendix B — Characterization of Environmental Soil Samples .............................. 59

Appendix C — Temperature and Relative Humidity Conditions .............................. 63

Appendix D — PCB in Soil Tube Assay PCB Technology Demonstration Sample Data ........... 67

Appendix E — Data Quality Objective Example ......................................... 77

Disclaimer ................................................................... 79

Background and Problem Statement ................................................ 79

DQO Goals .................................................................. 79

Use of Technology Performance Information to Implement the Decision Rule ................. 80

Determining the Number of Samples ............................................... 80

Alternative FP Parameter ........................................................ 83
xv

List of Figures

 3-1 Schematic map of ORNL, indicating the demonstration area. ........................... 11

C-1 Summary of temperature conditions for outside site ................................... 65

C-2 Summary of relative humidity conditions for outdoor site .............................. 65

C-3 Summary of temperature conditions for chamber site ................................. 66

C-4 Summary of relative humidity conditions for chamber site .............................. 66

xvii

List of Tables

 2-1 Interpretation of photometer readings for undiluted samples ............................. 7

 2-2 Interpretation of photometer readings for diluted samples ............................... 7

 2-3 Sensitivity of PCB in Soil Tube Kit to various Aroclors ................................ 8

 3-1 Summary of experimental design by sample type .................................... 12

 3-2 Summary of PCB in Soil Tube Assay predemonstration results .......................... 16

 4-1 Suspect measurements within the reference laboratory data ............................. 25

 4-2 Precision of the reference laboratory for PE soil samples ............................... 26

 4-3 Precision of the reference laboratory for environmental soil samples ...................... 28

 4-4 Accuracy of the reference laboratory for PE soil samples .............................. 29

 4-5 Summary of the reference laboratory performance .................................... 31

 5-1 PCB in Soil Tube Assay reporting intervals ........................................ 33

 5-2 Classification of precision results ................................................ 34

 5-3 Precision of the PCB in Soil Tube Assay for PE soil samples ........................... 35

 5-4 Precision of the PCB in Soil Tube Assay for environmental soil samples ................... 36

 5-5 Precision of the PCB in Soil Tube Assay for extract samples ............................ 37

 5-6 Overall precision of the PCB in Soil Tube Assay for all sample types ..................... 38

 5-7 PCB in Soil Tube Assay accuracy data for PE soil samples ............................. 39

 5-8 Evaluation of agreement between PCB in Soil Tube Assay’s PE sample results 

and the certified PE values as a measure of accuracy .................................. 40

 5-9 Accuracy of the PCB in Soil Tube Assay for extract samples ........................... 40

5-10 Evaluation of agreement between PCB in Soil Tube Assay’s extract results and the spike concentration

as a measure of accuracy ...................................................... 40

5-11 Evaluation of agreement between PCB in Soil Tube Assay’s soil results and the reference laboratory’s

results as a measure of comparability ............................................. 42

5-12 Comparison of the PCB in Soil Tube Assay results with the reference laboratory’s suspect measurements

......................................................................... 43

5-13 PCB in Soil Tube Assay performance for precision, accuracy, and comparability ............ 43

5-14 Estimated analytical costs for PCB soil samples ..................................... 45

5-15 Performance summary for the PCB in Soil Tube Assay ................................ 49

 A-1 Summary of soil sample descriptions ............................................. 57

 B-1 Summary of environmental soil characterization ..................................... 61

 C-1 Average temperature and relative humidity conditions during testing periods ................ 64

 D-1 PCB in Soil Tube Assay technology demonstration soil sample data ...................... 69

 D-2 PCB in Soil Tube Assay technology demonstration extract sample data ................... 74

 D-3 Corrected reference laboratory data .............................................. 75

 E-1 Comparison of PCB in Soil Tube Assay Results with the reference laboratory at 50 ppm level . . 81

xix

List of Abbreviations and Acronyms

ASTM American Society for Testing and Materials

BHC benzenehexachloride

CCV continuing calibration verification standard

CSCT Consortium for Site Characterization Technology

DCB decachlorobiphenyl

DOE U.S. Department of Energy

DQO data quality objective

ELISA enzyme-linked immunosorbent assay

EM Environmental Management (DOE)

EPA U.S. Environmental Protection Agency

ERA Environmental Resource Associates

ETTP East Tennessee Technology Park

ETV Environmental Technology Verification Program

ETVR Environmental Technology Verification Report

EvTEC Environmental Technology Evaluation Center

fn false negative result

FN false negative decision error rate

fp false positive result

FP false positive decision error rate

HEPA high-efficiency particulate air

ID identifier

LCS laboratory control sample

LV Las Vegas

MS matrix spike
xx

MSD matrix spike duplicate

n number of samples

NRC Nuclear Regulatory Commission

OD optical density

ORNL Oak Ridge National Laboratory

ORO Oak Ridge Operations (DOE)

PARCC precision, accuracy, representativeness, completeness, comparability

PCB polychlorinated biphenyl

PE performance evaluation

ppm parts per million (equivalent units: mg/kg for soils and μg/mL for extracts)

Pr probability

QA quality assurance

QC quality control

R coefficient of determination 2

RDL reporting detection limit

RH relative humidity

RFD request for disposal

RPD relative percentage difference

RSD relative standard deviation (percent)

SARA Superfund Amendments and Reauthorization Act of 1986

SD standard deviation

SITE Superfund Innovative Technology Evaluation

SMO Sample Management Office

SOP standard operating procedure

SSM synthetic soil matrix

TCMX tetrachloro-m-xylene
xxi

Acknowledgments

The authors wish to acknowledge the support of all those who helped plan and conduct the demonstration,

analyze the data, and prepare this report. In particular, we recognize the technical expertise of Mitchell

Erickson (Environmental Measurements Laboratory), Viorica Lopez-Avila (Midwest Research Institute), and

Robert F. O’Brien (Pacific Northwest National Laboratory), who were peer reviewers of this report. For

internal peer review, we thank Stacy Barshick (ORNL); for technical support during the demonstration, Todd

Skeen and Ralph Ilgner (ORNL); for site safety and health support, Kim Thomas, Marilyn Hanner, and Fred

Smith (ORNL); for administrative support, Betty Maestas and Linda Plemmons (ORNL); for sample collection

support, Wade Hollinger, Charlotte Schaefer, and Arlin Yeager (LMES), and Mike Rudacille and W. T.

Wright (EET Corporation); for preliminary soil characterization support, Frank Gardner, John Zutman, and

Bob Schlosser (ORNL, Grand Junction, Colo.); for sample management support, Angie McGee, Suzanne

Johnson, and Mary Lane Moore (LMES); for providing performance evaluations samples, Michael Wilson

(EPA’s Office of Solid Waste and Emergency Response’s Analytical Operations and Data Quality Center);

and for technical guidance and project management of the demonstration, David Carden, Marty Atkins, and

Regina Chung (DOE’s Oak Ridge Operations Office), David Bottrell (DOE, Headquarters), Deana Crumbling

(EPA’s Technology Innovation Office), and Stephen Billets, Gary Robertson, and Eric Koglin (EPA’s National

Exposure Research Laboratory, Las Vegas, Nevada). The authors also acknowledge the participation of

EnviroLogix, Inc., in particular, Jonathan Matt, who performed the analyses during the demonstration.

For more information on the PCB Field Analytical Technology Demonstration, contact

Eric N. Koglin

Project Technical Leader

Environmental Protection Agency

Characterization and Research Division

National Exposure Research Laboratory

P. O. Box 93478

Las Vegas, Nevada 89193-3478

(702) 798-2432

For more information on the PCB in Soil Tube Assay, contact

Jonathan Matt

EnviroLogix Inc.

55 Industrial Way

Portland, ME 04103

(207) 797-0300
1

Section 1

Introduction

The performance evaluation of innovative and alternative environmental technologies is an integral part of the

U.S. Environmental Protection Agency’s (EPA’s) mission. Early efforts focused on evaluating technologies

that supported the implementation of the Clean Air and Clean Water Acts. In 1987, the Agency began to

evaluate the cost and performance of remediation and monitoring technologies under the Superfund Innovative

Technology Evaluation (SITE) program. This was in response to the mandate in the Superfund Amendments

and Reauthorization Act (SARA) of 1986. In 1990, the U.S. Technology Policy was announced. This policy

placed a renewed emphasis on “making the best use of technology in achieving the national goals of improved

quality of life for all Americans, continued economic growth, and national security.” In the spirit of the

Technology Policy, the Agency began to direct a portion of its resources toward the promotion, recognition,

acceptance, and use of U.S.-developed innovative environmental technologies both domestically and abroad.

The Environmental Technology Verification (ETV) Program was created by the Agency to facilitate the

deployment of innovative technologies through performance verification and information dissemination. The

goal of the ETV Program is to further environmental protection by substantially accelerating the acceptance

and use of improved and cost-effective technologies. The ETV Program is intended to assist and inform those

involved in the design, distribution, permitting, and purchase of environmental technologies. The ETV Program

capitalizes upon and applies the lessons that were learned in the implementation of the SITE Program to the

verification of twelve categories of environmental technology: Drinking Water Systems, Pollution

Prevention/Waste Treatment, Pollution Prevention/ Innovative Coatings and Coatings Equipment, Indoor Air

Products, Air Pollution Control, Advanced Monitoring Systems, EvTEC (an independent, private-sector

approach), Wet Weather Flow Technologies, Pollution Prevention/Metal Finishing, Source Water Protection

Technologies, Site Characterization and Monitoring Technology [also referred to as the Consortium for Site

Characterization Technology (CSCT)], and Climate Change Technologies. The performance verification

contained in this report was based on the data collected during a demonstration of polychlorinated biphenyl

(PCB) field analytical technologies. The demonstration was administered by CSCT.

For each pilot, EPA utilizes the expertise of partner “verification organizations” to design efficient procedures

for conducting performance tests of environmental technologies. To date, EPA has partnered with federal

laboratories and state, university, and private sector entities. Verification organizations oversee and report

verification activities based on testing and quality assurance protocols developed with input from all major

stakeholder/customer groups associated with the technology area. 

In July 1997, CSCT, in cooperation with the U.S. Department of Energy’s (DOE’s) Environmental

Management (EM) Program, conducted a demonstration to verify the performance of six field analytical

technologies for PCBs: the L2000 PCB/Chloride Analyzer (Dexsil Corporation), the PCB Immunoassay Kit
2

(Hach Company), the 4100 Vapor Detector (Electronic Sensor Technology), and three immunoassay kits from

Strategic Diagnostics, Inc.: D TECH, EnviroGard, and RaPID Assay System. Another technology, the

EnviroLogix, Inc., PCB in Soil Tube Assay, was evaluated in September 1998. This environmental technology

verification report (ETVR) presents the results of the demonstration study for 

the PCB in Soil Tube Assay. Separate ETVRs have been published for the other six technologies.

Technology Verification Process

The technology verification process is intended to serve as a template for conducting technology demonstrations

that will generate high-quality data that EPA can use to verify technology performance. Four key steps are

inherent in the process:

• Needs identification and technology selection

• Demonstration planning and implementation

• Report preparation

• Information distribution

Needs Identification and Technology Selection

The first aspect of the technology verification process is to determine technology needs of EPA and the

regulated community. EPA, DOE, the U.S. Department of Defense, industry, and state agencies are asked to

identify technology needs and interest in a technology. Once a technology need is established, a search is

conducted to identify suitable technologies that will address this need. The technology search and identification

process consists of reviewing responses to Commerce Business Daily announcements, searches of industry and

trade publications, attendance at related conferences, and leads from technology developers. Characterization

and monitoring technologies are evaluated against the following criteria:

C meets user needs;

C may be used in the field or in a mobile laboratory;

C is applicable to a variety of environmentally impacted sites;

C has high potential for resolving problems for which current methods are unsatisfactory;

C is cost competitive with current methods;

C performs better than current methods in areas such as data quality, sample preparation, or analytical

turnaround time;
3

C uses techniques that are easier and safer than current methods;

C is a commercially available, field-ready technology.

Demonstration Planning and Implementation

After a technology has been selected, EPA, the verification organization, and the developer agree to the

responsibilities for conducting the demonstration and evaluating the technology. The following tasks are

undertaken at this time:

C identifying demonstration sites that will provide the appropriate physical or chemical environment,

including contaminated media;

C identifying and defining the roles of demonstration participants, observers, and reviewers;

C determining logistical and support requirements (for example, field equipment, power and water

sources, mobile laboratory, communications network);

C arranging analytical and sampling support;

C preparing and implementing a demonstration plan that addresses the experimental design, sampling

design, quality assurance/quality control (QA/QC), health and safety considerations, scheduling of

field and laboratory operations, data analysis procedures, and reporting requirements.

Report Preparation

Innovative technologies are evaluated independently and, when possible, against conventional technologies. The

field technologies are operated by the developers in the presence of independent technology observers. The

technology observers are provided by EPA or a third-party group. Demonstration data are used to evaluate the

capabilities, limitations, and field applications of each technology. Following the demonstration, all raw and

reduced data used to evaluate each technology are compiled into a technology evaluation report, which is

mandated by EPA as a record of the demonstration. A data summary and detailed evaluation of each

technology are published in an ETVR. 

Information Distribution

The goal of the information distribution strategy is to ensure that ETVRs are readily available to interested

parties through traditional data distribution pathways, such as printed documents. Documents are also available

on the World Wide Web through the ETV Web site (http://www.epa.gov/etv) and through a Web site supported

by the EPA Office of Solid Waste and Emergency Response’s Technology Innovation Office (http://CLUin.com).
4

Demonstration Purpose

The purpose of this demonstration was to obtain performance information for PCB field analytical

technologies, to compare the results with conventional fixed-laboratory results, and to provide supplemental

information (e.g., cost, sample throughput, and training requirements) regarding the operation of the

technology. The demonstration was conducted under two climatic conditions. One set of activities was

conducted outdoors, with naturally fluctuating temperatures and relative humidity conditions. A second set was

conducted in a controlled environmental facility, with lower, relatively stable temperatures and relative

humidities. Multiple soil types, collected from sites in Ohio, Kentucky, and Tennessee, were used in this study.

PCB soil concentrations ranged from approximately 0.1 to 700 parts per million (ppm). The developer also

analyzed 24 solutions of known PCB concentration that were used to simulate extracted wipe samples. The

extract samples ranged in concentration from 0 to 100 μg/mL.
5

Section 2

Technology Description

Objective

The objective of this section is to describe the technology being demonstrated, including the operating principles

underlying the technology and the overall approach to its use. The information provided here is excerpted from

that provided by the developer. Performance characteristics described in this section are specified by the

developer; they may or may not be substantiated by the data presented in Section 5.

Principle

The EnviroLogix PCB in Soil Tube Assay applies the principles of enzyme-linked immunosorbent assay

(ELISA) to determine PCB concentration. In such an assay, an enzyme has been chemically linked to a PCB

molecule or a PCB analog to create a labeled PCB reagent. The labeled PCB reagent (called a conjugate) is

mixed with an extract of native sample containing the PCB contaminant. A portion of the mixture is applied

to a surface (i.e., the inside of a test tube) to which an antibody specific for PCB has been affixed. The native

PCB and PCB-enzyme conjugate compete for a limited number of antibody sites. After a period of time, the

solution is washed away, and what remain are either PCB-antibody complexes or enzyme-PCB-antibody

complexes attached to the test surface. The proportion of the two complexes on the test surface is determined

by the amount of native PCB in the original sample. The enzyme present on the test surface is used to catalyze

a color change reaction in a solution added to the test surface. Because the amount of enzyme present is

inversely proportional to the concentration of native PCB contaminant, the amount of color development is

inversely proportional to the concentration of PCB contaminant. The color development is quantified through

the use of a hand-held photometer.

The EnviroLogix PCB in Soil Tube Kit is designed for semi-quantitative field-screening for PCBs in soil. The

kit is supplied with calibrators equivalent to 1 part per million (ppm) and 10 ppm PCB (Aroclor 1254) in soil.

These calibrators are used to evaluate threshold levels of 1 and 10 ppm. A threshold level of 50 ppm can also

be evaluated using the 10-ppm calibrator by preparing a 1:5 sample extract dilution into methanol. For the

extract samples, the threshold levels are 0.4, 4, and 20 μg/mL.

Applications and Advantages

The EnviroLogix PCB test kit can be used in a number of applications, including initial site characterization

and mapping, real-time testing during remediation, and screening of negatives prior to gas chromatography

confirmation. The test kit has a number of advantages:

• real-time progress monitoring while crews and equipment are on-site;

• clear, accurate pass/fail determinations at meaningful threshold values;

• meets site-specific calibration needs without a special kit;

• reduces wastes and costs.
6

Procedure

Materials

The EnviroLogix PCB in Soil Tube Kit contains the following items: 

• 40 antibody-coated test tubes

• 1 vial negative control

• 1 vial 1 ppm calibrator

• 1 vial 10 ppm calibrator

• 1 bottle of PCB-enzyme (horseradish peroxidase) conjugate

• 1 bottle of substrate

• 1 bottle of stop solution

The following items will need to be provided:

• EnviroLogix Soil Extraction Kit

• methanol (10 mL per sample)

• repeater pipettes

• (3) 12.5 mL combos-syringes

• positive displacement pipette

• marking pen

• timer

• distilled water

• portable photometer (Ariel Differential Photometer or equivalent)

• test tube rack

Extraction

Five grams of soil are weighed into a soil extraction bottle containing two ball bearings. (The ball bearings are

used to agitate the soil and may not be necessary for dry, sandy soils.) Then 10 mL of methanol are added to

the bottle, and the bottle is capped tightly and shaken vigorously by hand for 2 min. After the contents are

allowed to settle for 1 min, the extract is poured into the base of the UniprepTM and the filter plunger is slowly

pushed into the base until it stops at the bottom. To evaluate the samples relative to the 1 and 10 ppm

calibrators, the filtered extract is poured into labeled 4-mL glass amber vials and capped tightly. To evaluate

a 50 ppm threshold value, 800 μL of methanol are added to a 4-mL amber glass vial and then 200 μL of the

sample extract are added. This is a 1:5 dilution. 

Assay

All reagents should be at room temperature before assay begins. The number of antibody-coated test tubes

needed (up to 20) are removed from the kit and placed in the test tube rack; the tester should label one each for

the negative control, for the two calibrators, and for each of the samples. After dispensing 500 μL of conjugate

into each tube, dispensing down the side of the tubes with the syringe tip at an angle to prevent splashback, the

tester adds 50 μL of sample to the tube(s) labeled for samples and 50 μL of negative control and calibrators

to the appropriate tubes. The contents of the tubes are thoroughly mixed by moving the rack in a rapid circular

motion for 20 to 30 seconds. After the tubes have been allowed to incubate for 10 min, the tube contents are
7

emptied into a suitable container. The tubes are then filled with distilled water, emptied, and shaken to remove

any remaining drops. This wash process is repeated three times, after which the tubes are inverted and tapped

on paper towels to remove excess water. Next, 500 μL of substrate is added to each tube and the contents

mixed thoroughly by moving the rack in a rapid circular motion for 20 to 30 seconds. The tubes are left to

incubate for 10 min. If blue color does not develop in the negative control tube, the assay is invalid and

should be repeated. Now, 500 μL of stop solution is added to each tube. The tubes are read within 30 min

of addition of the stop solution.

Interpreting Results

An Ariel Differential Photometer (or an equivalent) is used to measure the optical density of each tube’s

contents. The wavelength on the photometer should be set to 450 nanometers (nm). If the photometer has dual

wavelength capability, 600, 630, or 650 nm should be used as the reference wavelength. If the photometer does

not auto-zero on air, the instrument should be zeroed against 1 mL water in a blank tube. The optical density

(OD) of each tube’s contents is then measured and recorded. The information shown in Tables 2-1 and 2-2

is used to interpret the results.

The test kit results are reported as concentration ranges designated as intervals incorporating

parenthesis/bracket notation. The parentheses indicate that the end-points of the concentration range are

excluded, while brackets indicate that the end-points are included. As shown in Table 2-1, the interval [0, 1)

indicates that the PCB concentration range is $0 and <1. If the sample is >10 ppm, a 1:5 dilution of the sample

can be prepared and assayed to determine if the concentration is >50 ppm. This diluted sample can be evaluated

using the 10-ppm calibrator, as shown in Table 2-2. 

Table 2-1. Interpretation of photometer readings for undiluted samples

Samples with OD values . . . Contain . . . And are reported as . .

.

> OD of 1-ppm calibrator <1 ppm PCB [0, 1)

Between OD of 1-ppm and OD of 1 #ppm PCB < 10 [1, 10)

10-ppm calibrators

<OD of 10-ppm calibrator $10 ppm PCB [10, 4)

Table 2-2. Interpretation of photometer readings for diluted samples

Diluted (1:5) samples with OD Contain . . . And are reported

values . . . as . . .

>OD of 10 ppm calibrator 10 # ppm PCB < 50 [10, 50)

<OD of 10 ppm calibrator $ 50 ppm PCB [50, 4)
8

Precautions and Notes

The following items should be noted about the test kit:

• All components should be stored at 4E to 8EC when not in use. Reagents must be allowed to come

to ambient temperature before use. The components should not be used after the expiration date. It

is important that the substrate solution not be exposed to direct sunlight during pipetting or while

incubating in the test tubes.

• The stop solution is 1.0 N hydrochloric acid and should be handled with caution.

• It is recommended that positive results be confirmed by an alternate method (such as gas

chromatography). 

Sensitivity and Cross-Reactivity

The test kit can be calibrated with other Aroclors. Table 2-3 shows the degree of sensitivity with the other

Aroclors. It should also be noted that at 1000 ppm, the following compounds had low cross-reactivity (i.e., did

not result in a positive response) at the 1-ppm interpretation level: 1,2-dichlorobenzene, 1,3-dichlorobenzene,

1,4-dichlorobenzene, 3,4-dichlorophenol, 2,5-dichlorophenol, biphenyl, pentachlorophenol, and humic acid.

Table 2-3. Sensitivity of PCB in Soil Tube Kit to various Aroclors

Aroclor Limit of Detection in Soil (ppm)

1242 1.7

1248 0.6

1254 0.3

1260 0.3
9

Section 3

Site Description and Demonstration Design

Objective

This section describes the demonstration site, the experimental design for the verification test, and the sampling

plan (sample types analyzed and the collection and preparation strategies). Included in this section are the

results from the predemonstration study and a description of the deviations made from the original

demonstration design.

Demonstration Site Description

Site Name and Location

The demonstration of PCB field analytical technologies was conducted at Oak Ridge National Laboratory

(ORNL) in Oak Ridge, Tennessee. PCB-contaminated soils from three DOE sites (Oak Ridge; Paducah,

Kentucky; and Piketon, Ohio) were used in this demonstration. The soil samples used in this study were

brought to the demonstration testing location for evaluation of the field analytical technologies.

Site History

Oak Ridge is located in the Tennessee River Valley, 25 miles northwest of Knoxville. Three DOE facilities are

located in Oak Ridge: ORNL, the Oak Ridge Y-12 Plant, and East Tennessee Technology Park (ETTP).

Chemical processing and warhead component production have occurred at the Y-12 Plant, and ETTP is a

former gaseous diffusion uranium enrichment plant. At both facilities, industrial processing associated with

nuclear weapons production has resulted in the production of millions of kilograms of PCB-contaminated soils.

Two other DOE facilities—the Paducah plant in Paducah, Kentucky, and the Portsmouth plant in Piketon,

Ohio—are also gaseous diffusion facilities with a history of PCB contamination. During the remediation of the

PCB-contaminated areas at the three DOE sites, soils were excavated from the ground where the PCB

contamination occurred, packaged in containers ranging in size from 55-gal to 110-gal drums, and stored as

PCB waste. Samples from these repositories (referred to as “Oak Ridge,” “Portsmouth,” and “Paducah”

samples in this report) were used in this demonstration.

In Oak Ridge, excavation activities occurred between 1991 and 1995. The Oak Ridge samples comprised PCBcontaminated soils from both Y-12 and ETTP. Five different sources of PCB contamination resulted in soil

excavations from various dikes, drainage ditches, and catch basins. Some of the soils are EPA-listed hazardous

waste due to the presence of other contaminants (e.g., diesel fuels). 

A population of more than 5000 drums containing PCB-contaminated soils was generated from 1986 to 1987

during the remediation of the East Drainage Ditch at the Portsmouth Gaseous Diffusion Plant. The ditch was

reported to have three primary sources of potential contamination: (1) treated effluent from a radioactive liquid

treatment facility, (2) runoff from a biodegradation plot where waste oil and sludge were disposed of, and (3)

storm sewer discharges. In addition, waste oil was reportedly used for weed control in the ditch. Aside from
10

PCB contamination, no other major hazardous contaminants were detected in these soils. Therefore, no EPA

hazardous waste codes are assigned to this waste.

Twenty-nine drums of PCB-contaminated soils from the Paducah plant were generated as part of a spill

cleanup activity at an organic waste storage area (C-746-R). The waste is considered a listed hazardous waste

for spent solvents (EPA hazardous waste code F001) because it is known to contain trichloroethylene. Other

volatile organic compounds, such as xylene, dichlorobenzene, and cresol, were also detected in the preliminary

analyses of some of the Paducah samples. 

Site Characteristics

PCB-contaminated environmental soil samples from Oak Ridge, Portsmouth, and Paducah were collected from

waste containers at storage repositories at ETTP and Paducah. Many of the soils contained interfering

compounds such as oils, fuels, and other chlorinated compounds (e.g., trichloroethylene). Specific sample

descriptions of the environmental soils used in this demonstration are given in Appendix A. In addition, each

sample was characterized in terms of its soil composition, pH, and total organic carbon content. Those results

are summarized in Appendix B. 

Field demonstration activities occurred at two sites at ORNL: a natural outdoor environment (the outdoor site)

and inside a controlled environmental atmosphere chamber (the chamber site). Figure 3-1 shows a schematic

map of a section of ORNL indicating the demonstration area where the outdoor field activities occurred.

Generally, the average September temperature for eastern Tennessee is 71EF. Average temperatures during

the testing periods ranged from 74 to 82EF, as shown in Appendix C. Studies were also conducted inside a

controlled environmental atmosphere chamber, hereafter referred to as the “chamber,” located in Building 5507

at ORNL. Demonstration studies inside the chamber were used to evaluate performance under environmental

conditions that were markedly different from the ambient outdoor conditions at the time of the test. Average

temperatures in the chamber during the testing periods ranged from 56 to 57EF. The controlled experimental

atmosphere facility consists of a room-size walk-in chamber 10 ft wide and 12 ft long with air processing

equipment to control temperature and humidity. The chamber is equipped with an environmental control

system, including reverse-osmosis water purification that supplies the chamber humidity control system. Highefficiency particulate air (HEPA) and activated charcoal filters are installed for recirculation and building

exhaust filtration.

Experimental Design

The analytical challenge with PCB analysis is to quantify a complex mixture that may or may not resemble the

original commercial product (i.e., Aroclor) because of environmental aging, and to report the result as a single

number [1]. The primary objective of the verification test was to compare the performance of the field

technology with laboratory-based measurements. Often, verification tests involve a direct one-to-one

comparison of results from field-acquired samples. However, because sample heterogeneity can preclude

replicate field or laboratory comparison, accuracy and precision data must often be derived from the analysis

of QC and performance evaluation (PE) samples. In this study, replicates of all three sample types (QC, PE,

and environmental soil) were analyzed. The ability to use environmental soils in the verification test was made
11

Figure 3-1. Schematic map of ORNL, indicating the demonstration area.

possible because the samples, collected from drums containing PCB-contaminated soils, could be thoroughly

homogenized and characterized prior to the demonstration. This facet of the design, allowing additional

precision data to be obtained on actual field-acquired samples, provided an added performance factor in the

verification test. 

Another objective of this demonstration was to evaluate the field technology’s capability to support regulatory

compliance decisions. For field methods to be used in these decisions, the technology must be capable of

informing the user, with known precision and accuracy, that concentrations are greater than or less than an

action level, such as 50 ppm for soil samples and 100 μg/100 cm for wipe samples[2]. The samples selected 2 

for analysis in the demonstration study were chosen with this objective in mind.

The experimental design is summarized in Table 3-1. This design was approved by the developer prior to the

start of the demonstration study. In total, the developer analyzed 208 soil samples, 104 each at both locations

(outdoors and chamber). The 104 soil samples comprised 68 environmental samples (17 unique environmental

samples prepared in quadruplicate) ranging in PCB concentration from 0.1 to 700 ppm and 36 PE soils (9

unique PE samples in quadruplicate) ranging in PCB concentration from 0 to 50 ppm. To determine the impact

of different environmental conditions on the technology’s performance, each batch of 104 samples contained

five sets of quadruplicate soil samples from DOE’s Paducah site. These were analyzed under both sets of

environmental conditions (i.e., outdoor and chamber conditions). In addition, 12 extracts ranging in

concentration from 0 to 100 μg/mL were analyzed in each location (chamber and outdoors). All samples were

analyzed without prior knowledge of sample type or concentration and were analyzed in a randomized order.
12

Table 3-1. Summary of experimental design by sample type

Concentration samples

range analyzed

Sample ID Total # a

Outdoor site Chamber site

PE materials

0 126 226 8

2.0 ppm 118 218 8

2.0 ppm 124 224 8

5.0 ppm 120 220 8

10.9 ppm 122 222 8

20.0 ppm 119 219 8

49.8 ppm 125 225 8

50.0 ppm 121 221 8

50.0 ppm 123 223 8

Environmental soils

0.1–2.0 ppm 101, 107, 108, 109, 113, 114 201, 202, 206 36

2.1–20.0 ppm 102, 103, 104, 115 203, 207, 212, 213 32

20.1–50.0 ppm 111, 116 204, 208, 209, 214, 215 28

50.1–700.0 ppm 105, 106, 110, 112, 117 205, 210, 211, 216, 217 40

Extracts

0 132 232 8

10 μg/mL 130 230 8

100 μg/mL 131 231 8

Grand total 116 116 232 b

 Each sample was analyzed in quadruplicate. a

 All samples were analyzed in random order. b

Environmental Conditions during Demonstration

As mentioned earlier, field activities were conducted both outdoors under natural environmental conditions and

indoors in a controlled environmental atmosphere chamber to evaluate the effect of environmental conditions

on technology performance. The weather outside during the September demonstration consisted of highs

approaching 90EF and 90% relative humidity (RH). Daily average temperatures were around 78EF with 50%
13

RH. While outside, the developer set up a canopy to provide shade and protection from late afternoon

thundershowers. In the indoor chamber tests, conditions were set to 55EF and 50% RH. An independent check

of the conditions inside the chamber indicated that the temperature ranged from 54 to 58EF, while relative

humidities ranged from 44 to 55%. Appendix C contains a summary of the environmental conditions

(temperature and relative humidity) during the demonstration.

Sample Descriptions

PCBs (C12H10-xClx) are a class of compounds that are chlorine-substituted linked benzene rings. There are 209

possible PCB compounds (also known as congeners). PCBs were commercially produced as complex mixtures

beginning in 1929 for use in transformers, capacitors, paints, pesticides, and inks [1]. Monsanto Corporation

marketed products that were mixtures of 20 to 60 PCB congeners under the trade name Aroclor. Aroclor

mixtures are identified by a number (e.g., Aroclor 1260) that represents the mixture’s chlorine composition as

a percentage (e.g., 60%).

Performance Evaluation Materials

Samples of Tennessee reference soil [3] served as the blanks. Pre-prepared certified PE samples were obtained

from Environmental Resource Associates (ERA) of Arvada, Colorado, and the Analytical Operations and Data

Quality Center of EPA’s Office of Solid Waste and Emergency Response. The soils purchased from ERA had

been prepared using ERA’s semivolatile blank soil matrix. This matrix was a topsoil that had been dried,

sieved, and homogenized. Particle size was approximately 60 mesh. The soil was approximately 40% clay. The

samples acquired from EPA’s Analytical Operations and Data Quality Center had been prepared using

contaminated soils from various sites around the country in the following manner: The original soils had been

homogenized and diluted with a synthetic soil matrix (SSM). The SSM had a known matrix of 6% gravel, 31%

sand, and 43% silt/clay; the remaining 20% was topsoil. The dilution of the original soils was performed by

mixing known amounts of contaminated soil with the SSM in a blender for no less than 12 h. The samples were

also spiked with target pesticides (", $, ), and )-BHC, methoxychlor, and endrin ketone) to introduce some

compounds that were likely to be present in an actual environmental soil. The hydrocarbon background from

the original sample and the spiked pesticides produced a challenging matrix. The PE soils required no additional

preparation by ORNL.

Environmental Soil Samples

As noted in the site description, PCB-contaminated environmental soil samples from Oak Ridge, Portsmouth,

and Paducah were used in this demonstration. The soils were contaminated with PCBs as the result of spills

and industrial processing activities at the various DOE facilities. Originally, the contaminated soils were

excavated from dikes, drainage ditches, catch basins, and organic waste storage areas. The excavated soils were

then packaged into waste containers and stored at the repositories in ETTP and Paducah in anticipation of

disposal by incineration. The environmental soil samples used in this study were collected from these waste

containers. Many of the soils contained interfering compounds such as oils, fuels, and other chlorinated

compounds, while some contained multiple Aroclors. For more information on sampling locations and sample

characteristics (soil composition, pH, and total organic carbon content), refer to Appendices A and B,

respectively. 
14

Extract Samples

Traditionally, the amount of PCBs on a contaminated surface is determined by wiping the surface with a cotton

pad saturated with hexane. The pad is then taken to the laboratory, extracted with additional hexane, and

analyzed by gas chromatography. Unlike soil samples, which can be more readily homogenized and divided,

equivalent wipe samples (i.e., contaminated surfaces or post-wipe pads) were not easily obtainable. Therefore,

interference-free methanolic solutions of PCBs were analyzed to simulate an extracted surface wipe pad.

Extract sample analyses provided evaluation data that relied primarily on the technology’s performance rather

than on elements critical to the entire method (i.e., sample collection and preparation). A total of 12 methanolic

solutions were analyzed per site; these consisted of four replicates each of a blank and two concentration levels

(10 and 100 μg/mL). 

Sampling Plan

Sample Collection

Environmental soil samples were collected from April 17 through May 7, 1997. Portsmouth and Oak Ridge

Reservation soils were collected from either storage boxes or 55-gal drums stored at ETTP. Briefly, the

following procedure was used to collect the soil samples. Approximately 30 lb of soil were collected from the

top of the drum or B-25 box using a scoop and placed in a plastic bag. The soil was sifted to remove rocks and

other large debris, then poured into a plastic-lined 5-gal container. All samples were subjected to radiological

screening and were determined to be nonradioactive. Similarly, soil samples were collected from 55-gal drums

stored at Paducah and shipped to ORNL in lined 5-gal containers.

Sample Preparation, Labeling, and Distribution

Aliquots of several of the environmental soils were analyzed and determined to be heterogeneous in PCB

concentration. Because this is unsatisfactory for accurately comparing the performance of the field technology

with the laboratory-based method, the environmental soils had to be homogenized prior to sample distribution.

Each Portsmouth and Oak Ridge environmental soil sample was homogenized by first placing approximately

1500 g of soil in a glass Pyrex dish. The dish was then placed in a large oven set at 35EC, with the exhaust and

blower fans turned on to circulate the air. After drying overnight, the soil was pulverized using a conventional

blender and sieved using a 9-mesh screen (2 mm particle size). Last, the soil was thoroughly mixed using a

spatula. A comparison of dried and undried soils showed that a minimal amount of PCBs (< 20%) was lost as

the result of sample drying, making this procedure suitable for use in the preparation of the soil samples. The

Paducah samples, because of their sandy characteristics, required only the sieving and mixing preparation

steps. Extract sample preparation involved making solutions of PCBs in methanol at two concentration levels

(10 and 100 μg/mL). Multiple aliquots of each sample were analyzed using the analytical procedure described

below to confirm the homogeneity of the samples with respect to PCB concentration.

To provide the developer with soils contaminated at higher concentrations of PCBs, some of the environmental

soils (those labeled with an “S” in Appendix B) were spiked with additional PCBs. Spiked soils samples were

prepared after the soil was first dried in an oven set at 35EC overnight. The dry soil was ground using a

conventional blender and sieved through a 9-mesh screen (2 mm particle size). Approximately 1500 g of the

sieved soil were spiked with a diethyl ether solution of PCBs at the desired concentration. The fortified soil was

agitated using a mechanical shaker and then allowed to air-dry in a laboratory hood overnight. A minimum of

four aliquots were analyzed using the analytical procedure described below to confirm the homogeneity of the

soil with regard to the PCB concentration.
15

The environmental soils were characterized at ORNL prior to the demonstration study. The procedure used to

confirm the homogeneity of the soil samples entailed the extraction of 3 to 5 g of soil in a mixture of solvents

(1 mL water, 4 mL methanol, and 5 mL hexane). After the soil/solvent mixture was agitated by a mechanical

shaker, the hexane layer was removed and an aliquot was diluted for analysis. The hexane extract was analyzed

on a Hewlett Packard 6890 gas chromatograph equipped with an electron capture detector and autosampler.

The method used was a slightly modified version of EPA’s SW-846 dual-column Method 8081 [4]. 

After analysis confirming homogeneity, the samples were split into jars for distribution. Each 4-oz sample jar

contained approximately 20 g of soil. Four replicate splits of each soil sample were prepared for each

developer. The samples were randomized in two fashions. First, the order in which the filled jars were

distributed was randomized so that the same developer did not always receive the first jar filled for a given

sample set. Second, the order of analysis was randomized so that each developer analyzed the same set of

samples, but in a different order. The extract samples were split into 10-mL aliquots and placed into 2-oz jars.

The extracts were stored in the refrigerator (at #4EC) until released to the developers. Each sample jar had

three labels: (1) developer order number, (2) sample identifier number, and (3) a PCB warning label. The

developer order number corresponded to the order in which the developer was required to analyze the samples

(e.g., 1001 through 1116). The sample identifier number was in the format of “xxxyzz,” where “xxx” was the

three-digit sample ID (e.g., 101) listed in Table 3-1, “y” was the replicate (e.g., 1 to 4), and “zz” was the

aliquot order of each replicate (e.g., 01 to 11). For example, sample identifier 101101 corresponded to sample

ID “101” (an Oak Ridge soil from RFD 40022, drum 02), “1” corresponded to the first replicate from that

sample, and “01” corresponded to the first jar filled in that series. 

Once the samples were prepared, they were stored at a central sample distribution center. During the

demonstration study, the developer was sent to the distribution center to pick up his samples. Samples were

distributed sequentially in batches of 12 to ensure that samples were analyzed in the order specified.

Completion of chain-of-custody forms and scanning of bar code labels documented sample transfer activities.

Some of the developers received information regarding the samples prior to analysis. This was provided at the

request of the developer to simulate the type of information that would be available during actual field testing.

EnviroLogix elected not to receive sample information prior to analysis. The developer returned the unused

portions of the samples with the analytical results to the distribution center when testing was completed. The

sample bar codes were scanned upon return to document sample throughput time.

Three complete sets of extra samples, called archive samples, were available for distribution in case the

integrity of a sample was compromised. No archive samples were utilized over the course of the EnviroLogix

demonstration.

Predemonstration Study and Results

Ideally, environmental soil samples are sent to the developers prior to the demonstration study to allow them

the opportunity to analyze representative samples in advance of the verification test. This gives developers the

opportunity to refine and calibrate their technologies and revise their operating procedures on the basis of the

predemonstration study results. The predemonstration study results can also be used as an indication that the

selected technologies are of the appropriate level of maturity to participate in the demonstration study. 
16

According to ORNL regulations, however, one of two conditions must exist in order to ship environmental soils

that were once classified as mixed hazardous waste: either the recipient—in this case, the developer’s

facilities—must have proper Nuclear Regulatory Commission (NRC) licensing to receive and analyze

radiological materials; or the soils must be certified as entirely free of radioactivity, beyond the no-rad

certification issued from radiological screening tests based on ORNL standards. Because the developer did not

have proper NRC licensing, and proving that the soils were entirely free of radioactivity was prohibitive, PE

soils were used for the predemonstration study. The developer also analyzed a solvent extract.

The predemonstration samples were sent to the developer on August 17, 1998. Predemonstration results were

received by August 19, 1998. Table 3-2 summarizes the test kit’s results for the predemonstration samples.

Results indicated that EnviroLogix’s PCB in Soil Tube Assay was ready for field evaluation. 

Table 3-2. Summary of PCB in Soil Tube Assay predemonstration results

Sample concentration Aroclor Acceptance range 

Certified Total PCB concentration (ppm)

a

 Result #1 Result #2

1 0 n/a n/a [0, 1) [0, 1) b

2 5.0 ppm 1254 2.1–6.2 ppm [1, 10) [1, 10)

3 49.8 ppm 1254, 1260 23.0–60.8 ppm [50, 4) [50, 4)

4 20.0 ppm 1248 11.4–32.4 ppm [10, 50) [10, 50)

5 10 μg/mL 1254 n/a [4, 20) [4, 20)

 Acceptance ranges were provided by the supplier of the performance evaluation material. a

 The notation [0, 1) indicates that the sample concentration was $0 and <1. See Sections 2 and 5 for more information b

on interval reporting.

Deviations from the Demonstration Plan

A few deviations from the demonstration plan occurred. In Appendix B of the technology demonstration plan

[5], the reference laboratory’s procedure states that no more than 10 samples will be analyzed with each

analytical batch (excluding blanks, standards, QC samples, and dilutions). The analytical batch is also stated

as 10 samples in the Quality Assurance Project Plan of the demonstration plan. The reference laboratory

actually analyzed 20 samples per analytical batch. Because a 20-sample batch is recommended in SW-846

Method 8081, this deviation was deemed acceptable. In addition, the parentheses and bracket notations in

Tables 3-1 and 3-2 are slightly different than what was used in the demonstration. See Tables 2-1 and 2-2 of

this report for the correction notation.

During the demonstration study, EnviroLogix noted the following deviations from the procedure described in

the technology demonstration plan [5] for the PCB in Soil Tube Assay: 
17

• Instead of two, one or no ball bearings were used for extraction. The purpose of the ball bearings is to aid

in the extraction by agitating the soil. Since the soils were sandy and dry, the ball bearings were not

necessary.

• Multiple filtrations (usually 12 tubes at a time) were performed by pushing the plungers down on the

UniPrep tubes simultaneously using a small board. The procedure in the demonstration plan describes the

filtration as being performed individually.

• Three washes of the coated tubes were performed instead of four.

19

Section 4

Reference Laboratory Analytical Results and Evaluation

Objective and Approach

This section presents the evaluation of the PCB data generated by the reference laboratory. Evaluation of the

results from the analysis of PE, environmental soil, and extract samples was based on precision, accuracy,

representativeness, completeness, and comparability (PARCC) parameters [6]. This section describes how the

analytical data generated by the reference laboratory were used to establish a baseline performance for PCB

analysis.

EnviroLogix demonstrated the PCB in Soil Tube Assay kit using the same samples that were used in the July

1997 demonstration of six PCB technologies. Soil samples were available for the EnviroLogix demonstration

because extra samples were prepared and stored since 1997. ORNL performed chemical analyses of

representative samples to verify that significant amounts of PCBs had not been lost due to storage for one year.

Duplicate analyses from each unique soil sample were performed. It was confirmed that no considerable losses

in PCB concentration had occurred. Therefore, all soil samples were utilized in the EnviroLogix demonstration,

and the reference laboratory data described in this section was used for comparison with the PCB in Soil Tube

Assay results. Because the original extract samples were prepared in methanol, new extract samples were

prepared by ORNL. Therefore, no reference laboratory results are presented for these samples. Instead of a

reference laboratory result, the EnviroLogix’s result was compared to the nominal concentration value only.

Confirmational analyses at ORNL indicated that the extracts were prepared to the nominal concentrations. 

Reference Laboratory Selection

The Oak Ridge Sample Management Office (SMO) has been tasked by DOE Oak Ridge Operations (DOEORO) with maintaining a list of qualified laboratories to provide analytical services. The technology

demonstration plan [5] contains the SMO’s standard operating procedures (SOPs) for identifying, qualifying,

and selecting analytical laboratories. Laboratories are qualified as acceptable analytical service providers for

the SMO by meeting specific requirements. These requirements include providing pertinent documentation

(such as QA and chemical hygiene plans), acceptance of the documents by the SMO, and satisfactory

performance on an on-site prequalification audit of laboratory operations. All laboratory qualifications are

approved by a laboratory selection board, composed of the SMO operations manager and appointees from all

prime contractors that conduct business with the SMO. 

All of the qualified laboratories were invited to bid on the demonstration study sample analysis. The lowest-cost

bidder was LAS Laboratories, in Las Vegas, Nevada. A readiness review conducted by ORNL and the SMO

confirmed the selection of LAS as the reference laboratory. Acceptance of the reference laboratory was

finalized by satisfactory performance in the predemonstration study. The SMO contracted LAS to provide full

data packages for the demonstration study sample analyses within 30 days of sample shipment.
20

The SMO conducts on-site audits of LAS annually as part of the laboratory qualification program. At the time

of selection, the most recent audit of LAS had occurred in February 1997. Results from this audit indicated

that LAS was proficient in several areas, including program management, quality management, and training

programs. No findings regarding PCB analytical procedure implementation were noted. A second on-site audit

of LAS occurred August 11–12, 1997, during the analysis of the demonstration study samples. This

surveillance focused specifically on the procedures that were currently in use for the analysis of the

demonstration samples. The audit, jointly conducted by the SMO, DOE-ORO, and EPA-Las Vegas (LV),

verified that LAS was procedurally compliant. The audit team noted that LAS had excellent adherence to the

analytical protocols and that the staff were knowledgeable of the requirements of the method. No findings

impacting data quality were noted in the audit report.

Reference Laboratory Method

The reference laboratory’s analytical method, also presented in the technology demonstration plan [5], followed

the guidelines established in EPA SW-846 Method 8081 [4]. According to LAS’s SOP, PCBs were extracted

from 30-g samples of soil by sonication in hexane. Each extract was then concentrated to a final volume that

was further subjected to a sulfuric acid cleanup to remove potential interferences. The analytes were identified

and quantified using a gas chromatograph equipped with dual electron-capture detectors. Each extract was

analyzed on two different chromatographic columns with slightly different separation characteristics (primary

column: RTX-1701, 30 m × 0.53 mm ID × 0.5 μm; confirmatory column: RTX-5, 30 m × 0.53 mm ID × 0.5

μm). PCBs were identified when peak patterns from a sample extract matched the patterns of standards for

both columns. PCBs were quantified based on the initial calibration of the primary column.

Calibration

Method 8081 states that, because Aroclors 1016 and 1260 include many of the peaks represented in the other

five Aroclor mixtures, it is only necessary to analyze two multilevel standards for these Aroclors to demonstrate

the linearity of the detector response for PCBs. However, per LAS SOPs, five-point (0.1 to 4 ppm) initial

calibration curves were generated for Aroclors 1016, 1248, 1254, and 1260 and the surrogate compounds

[decachlorobiphenyl (DCB) and tetrachloro-m-xylene (TCMX)]. Single mid-level standards were analyzed for

the other Aroclors (1221, 1232, and 1242) to aid in pattern recognition. All of the multi-point calibration data,

fitted to quadratic models, met the QC requirement of having a coefficient of determination (R ) of 0.99 or

2

better over the calibration range specified. The detection limits for soil samples were 0.033 ppm (μg/g) for all

Aroclors except Aroclor 1221, which was 0.067 ppm. For extract samples, the detection limits were 0.010 ppm

(μg/mL) for all Aroclors except Aroclor 1221, which was 0.020 ppm. Reporting detection limits were

calculated based on the above detection limits, the actual sample weight, and the dilution factor. 

Sample Quantification

For sample quantification, Aroclors were identified by comparing the samples’ peak patterns and retention

times with those of the respective standards. Peak height ratios, peak shapes, sample weathering, and general

similarity in detector response were also considered in the identification. Aroclor quantifications were

performed by selecting three to five representative peaks, confirming that the peaks were within the established

retention time windows, integrating the selected peaks, quantifying the peaks based on the calibrations, and

averaging the results to obtain a single concentration value for the multicomponent Aroclor. If mixtures of

Aroclors were suspected to be present, the sample was typically quantified in terms of the most representative

Aroclor pattern. If the identification of multiple Aroclors was definitive, total PCBs in the sample were
21

calculated by summing the concentrations of both Aroclors. Aroclor concentrations were quantified within the

concentration range of the calibration curve. If PCBs were detected and the concentrations were outside of the

calibration range, the sample was diluted and reanalyzed until the concentration was within the calibration

range. If no PCBs were detected, the result was reported as a non-detect (i.e., “# reporting detection limit”).

Sample Receipt, Handling, and Holding Times

The reference laboratory was scheduled to analyze a total of 256 PCB samples (208 soil samples, 24 iso-octane

extract samples, and 24 methanol extract samples). Of these same samples, the developer was scheduled to

analyze a total of 232 PCB samples (208 soil samples and 24 extract samples in solvent of choice). The

samples were shipped to LAS at the start of the technology demonstration activities (July 22). Shipment was

coordinated through the SMO. Completion of chain-of-custody forms documented sample transfer. The

samples were shipped on ice in coolers to maintain <6EC temperatures during shipment. Samples were shipped

with custody seals to ensure sample integrity and to prevent tampering during transport.

Upon receipt of the samples, the reference laboratory checked the receipt temperature and conditions of the

sample containers, assigned each sample a unique number, and logged each into its laboratory tracking system.

All samples were received at the proper temperature and in good condition. Demonstration samples were

divided into 11 analytical batches (with no more than 20 samples per batch). The samples were analyzed in an

order specified by ORNL to ensure that the analysis of sample types was randomized. Analyses of QC samples,

supplied by the reference laboratory to indicate method performance, were performed with each analytical

batch of soils.

Prior to analysis, samples were stored in refrigerators kept at 4 to 6E C to maintain analyte integrity. The

reference laboratory was required to analyze the extract samples and to extract the soil samples within 14 days

of shipment from ORNL. Once the soils were extracted, the reference laboratory had an additional 40 days to

analyze the soil extracts. Maximum holding times were not exceeded for any of the demonstration samples. The

final reference laboratory data package for all samples was received at ORNL in 72 days, on October 1, 1997.

The contractual obligation was 30 days. 

The remainder of this section is devoted to summarizing the data generated by the reference laboratory and to

assessing the analytical performance.

Quality Control Results

Objective

The purpose of this section is to provide an assessment of the data generated by the reference laboratory’s QC

procedures. The QC samples included continuing calibration verification standards (CCVs), instrument blanks,

method blanks, surrogate spikes, laboratory control samples (LCSs), and matrix spike (MS) /duplicate matrix

spike (MSD) samples. Each control type is described in more detail in the following text and in the technology

demonstration plan [5]. Because extraction of these liquid samples was not required, calibration check

standards and instrument blanks were the only control samples implemented for the extract samples. The

reference laboratory’s implementation of QC procedures was consistent with SW-846 guidance.
percent recovery '

measured amount

actual amount

× 100%

22

Continuing Calibration Verification Standard Results

A CCV is a single calibration standard of known concentration, usually at the midpoint of the calibration range.

This standard is evaluated as an unknown and is quantified against the initial calibration. The calculated

concentration is then compared with the nominal concentration of the standard to determine whether the initial

calibration is still valid. CCVs were analyzed with every 10 samples or at least every 12. The requirement for

acceptance was a percentage difference of less than 15% for the CCV relative to the initial calibration. This

QC requirement was met for all Aroclors and surrogates, except for one standard that had a 16% difference

for DCB. These results indicated that the reference laboratory maintained instrument calibrations during the

course of sample analysis. 

Instrument and Method Blank Results

Instrument blanks (hexane) were analyzed prior to each CCV. The QC requirement was that instrument blanks

must contain less than the reporting detection limit for any analyte. All instrument blanks were acceptable. 

A method blank is an analyte-free soil matrix sample that is taken through the extraction process to verify that

there are no laboratory sources of contamination. One method blank was analyzed for each analytical batch.

The QC requirement was that method blanks must contain less than the reporting detection limit for any

Aroclor. No PCBs were detected in any of the eleven method blanks that were analyzed. These results

demonstrated that the reference laboratory was capable of maintaining sample integrity, and that it did not

introduce PCB contamination to the samples during preparation.

Surrogate Spike Results

A surrogate is a compound that is chemically similar to the analyte group but is not expected to be present in

the environmental sample. A surrogate is added to test the extraction and analysis methods to verify the ability

to isolate, identify, and quantify a compound similar to the analyte(s) of interest without interfering with the

determination. Two different surrogate compounds, DCB and TCMX, were used to bracket the retention time

window anticipated in the Aroclor chromatograms. All soil samples, including QC samples, were spiked with

surrogates at 0.030 ppm prior to extraction. Surrogate recoveries were deemed to be within QC requirements

if the measured concentration fell within the QC acceptance limits that were established by past method

performance. (For LAS this was 39 to 117% for DCB, and 66 to 128% for TCMX). The results were

calculated using the following equation:

(4-1)

In all undiluted samples, both of the surrogates had percentage recoveries that were inside the acceptance limits.

Surrogate recoveries in diluted samples were uninformative because the spike concentration (0.030 ppm, as

specified by the method) was diluted below the instrument detection limits. The surrogate recovery results for

undiluted samples indicated that there were no unusual matrix interferences or batch-processing errors for these

samples.
RPD '

* MS recovery & MSD recovery *

average recovery

× 100%

23

Laboratory Control Sample Results

An LCS is an aliquot of a clean soil that is spiked with known quantities of target analytes. The LCS is spiked

with the same analytes and at the same concentrations as the MS. (MSs are described in the next section.) If

the results of the MS analyses are questionable (i.e., indicating a potential matrix effect), the LCS results are

used to verify that the laboratory can perform the analysis in a clean, representative matrix. 

Aroclors 1016 and 1260 were spiked into the clean soil matrix at approximately 0.300 ppm, according to the

reference laboratory’s SOP. The QC requirements (defined as percent recovery) for the LCS analyses were

performance-based acceptance limits that ranged from 50 to 158%. In all but 1 of the 11 LCSs analyzed, both

Aroclor percent recoveries fell within the acceptance limits. Satisfactory recoveries for LCS verified that the

reference laboratory performed the analyses properly in a clean matrix.

Matrix Spike Results

In contrast to an LCS, a MS sample is an actual environmental soil sample into which target analytes are

spiked at known concentrations. MS samples are used to assess the efficiency of the extraction and analytical

methods for real samples. This is accomplished by determining the amount of spiked analyte that is

quantitatively recovered from the environmental soil. An MSD sample is spiked and analyzed to provide a

measure of method precision. Ideally, to evaluate the MS/MSD results, the environmental soil is analyzed

unspiked so that the background concentrations of the analyte in the sample are considered in the recovery

calculation. 

For the demonstration study samples, one MS and MSD pair was analyzed with each analytical batch. The MS

samples were spiked under the same conditions and QC requirements as the LCS (50 to 158% acceptance

limits), so that MS/MSD and LCS results could be readily compared. The QC requirement for MS and MSD

samples was a relative percentage difference (RPD) of less than 30% between the MS/MSD pair. RFD is

defined as

(4-2)

A total of 11 MS/MSD pairs were analyzed. Because the MS/MSD spiking technique was not always properly

applied (e.g., a sample which contained 100 ppm of Aroclor 1254 was spiked ineffectively with 0.300 ppm of

Aroclor 1260), many of the MS/MSD results were uninformative. For the samples that were spiked

appropriately, all MS/MSD QC criteria were met.

Conclusions of the Quality Control Results

The reference laboratory results met performance acceptance requirements for all of the samples where proper

QC procedures were implemented. Acceptable performance on QC samples indicated that the reference

laboratory was capable of performing analyses properly. 
24

Data Review and Validation

Objective

The purpose of validating the reference laboratory data was to ensure usability for the purposes of comparison

with the demonstration technologies. The data generated by the reference laboratory were used as a baseline

to assess the performance of the technologies for PCB analysis. The reference laboratory data were

independently validated by ORNL and SMO personnel, who conducted a thorough quality check and reviewed

all sample data for technical completeness and correctness. 

Corrected Results

Approximately 8% of the results provided by the reference laboratory (20 of 256) were found to have

correctable errors. So as not to bias the assessment of the technology’s performance, errors in the reference

laboratory data were corrected. These changes were made conservatively, based on the guidelines provided in

the SW-846 Method 8081 for interpreting and calculating Aroclor results. The errors (see Appendix D, Table

D-3) were categorized as transcription errors, calculation errors, and interpretation errors. The corrections

listed in Table D-3 were made in the final data set that was used for comparison with the demonstration

technologies.

Suspect Results

Normally, one would not know if a single sample result was “suspect” unless (1) the sample was a PE sample,

where the concentration is known, or (2) a result was reported and flagged as suspect for some obvious reason

(e.g., no quantitative result was determined). The experimental design implemented in this demonstration study

provided an additional indication of the abnormality of data through the inspection of the replicate results from

a homogenous soil sample set (i.e., four replicates were analyzed for each sample ID). 

Data sets were considered suspect if the standard deviation (SD) of the four replicates was greater than 30 ppm

and the percent relative standard deviation (RSD) was greater than 50%. Five data sets (sample IDs 106, 205,

216, 217, 225) contained measurements that were considered suspect using this criteria, and the suspect data

are summarized in Table 4-1. A number of procedural errors may have caused the suspect measurements (e.g.,

spiking heterogeneity, extraction efficiencies, dilution, etc.). In the following subsections for precision and

accuracy, the data were evaluated with and without these suspect values to represent the best- and worst-case

scenarios.
25

Table 4-1. Suspect measurements within the reference laboratory data

Criteria Sample ID Data usability

 PCB concentration (ppm)

Replicate results Suspect result(s)

(ppm) (ppm)

SD > 30 ppm 

RSD > 50% 

106 255.9, 269.9, 317.6 649.6

205 457.0, 483.3, 538.7 3305.0

216 47.0, 54.3, 64.0 151.6

217 542.8, 549.8, 886.7 1913.3

225 32.1, 36.5, 56.4 146.0

 Performed data analysis with

and without this value

Qualitative result

110 # reporting detection #66, #98, #99, #490 Used as special case for

112 #66, #130, #200, results

limits comparison with developer

#200

Samples that did not fall into the above criteria, but were also considered suspect, were non-blank samples that

could not be quantified and were reported as “# the reporting detection limit.” This was the case for

environmental soil sample IDs 110 and 112. It is believed that the reference laboratory had trouble quantifying

these soil samples because of the abundance of chemical interferences. These samples were diluted by orders

of magnitude to reduce interferences, thereby diluting the PCB concentrations to levels that were lower than

the instrument detection limits. With each dilution, the reporting detection limits values were adjusted for

sample weight and dilution, which accounts for the higher reporting detection limits (up to 490 ppm). It is

believed that these samples should have been subjected to additional pre-analytical cleanup to remove these

interferences before quantification was attempted. Sample IDs 110 and 112 were collected from the same

cleanup site (see Appendix B), so it is not surprising that similar difficulties were encountered with both sample

sets. Because the results for sample IDs 110 and 112 were not quantitative, these data were compared with the

technology data only on a special case basis.

Data Assessment

Objective

The purpose of this section is to provide an evaluation of the performance of the reference laboratory results

through statistical analysis of the data. The reference laboratory analyzed 72 PE, 136 environmental soil, and

48 extract samples. All reference laboratory analyses were performed under the same environmental conditions.

Therefore, site differentiation was not a factor in data assessment for the reference laboratory. For comparison

with the technology data, however, the reference laboratory data are delineated into “outdoor site” and

“chamber site” in the following subsections. For consistency with the technology review, results from both sites

were also combined to determine the reference laboratory’s overall performance for precision and accuracy.

This performance assessment was based on the raw data compiled in Appendix D. All statistical tests were

performed at a 5% significance level. 
RSD '

Standard Deviation

Average Concentration

× 100%

26

Precision

The term “precision” describes the reproducibility of measurements under a given set of conditions. The SD

of four replicate PCB measurements was used to quantify the precision for each sample ID. SD is an absolute

measurement of precision, regardless of the PCB concentration. To express the reproducibility relative to the

average PCB concentration, RSD is used to quantify precision, according to the following equation:

(4-3)

Performance Evaluation Samples

The PE samples were homogenous soils containing certified concentrations of PCBs. Results for these samples

represent the best estimate of precision for soil samples analyzed in the demonstration study. Table 4-2

summarizes the precision of the reference laboratory for the analysis of PE samples. One suspect measurement

(sample ID 225, 146.0 ppm) was reported for the PE soil samples. The RSDs for the combined data ranged

from 9 to 33% when the suspect measurement was excluded, and from 9 to 79% including the suspect

measurement. The overall precision, determined by the mean RSD for all PE samples, was 21% for the worst

case (including the suspect result) and 18% for the best case (excluding the suspect result).

Table 4-2. Precision of the reference laboratory for PE soil samples

Outdoor site Chamber site Combined sites

Sample Average SD RSD Sample Average SD RSD Average SD RSD

ID concentration (ppm) (%) ID concentration (ppm) (%) concentration (ppm) (%)

(ppm) (ppm) (ppm)

 126 0 n/a n/a 226 0 n/a n/a 0 n/a n/a a

118 1.6 0.6 39 218 2.6 0.2 6 2.1 0.7 33

124 1.7 0.2 13 224 1.7 0.5 29 1.7 0.4 21

120 5.0 1.0 20 220 5.8 1.8 31 5.4 1.4 26

122 11.1 0.9 8 222 12.8 0.3 3 11.9 1.1 9

119 20.1 3.4 17 219 23.3 6.1 26 21.7 4.9 23

125 37.9 6.9 18 225 41.7 12.9 31 39.5 9.2 23 b b b c c c

121 54.6 3.4 6 221 44.9 11.3 25 49.8 9.3 19

123 60.1 4.6 8 223 55.8 7.7 14 58.0 6.3 11

 All PCB concentrations were reported as non-detects. a

Results excluding the suspect value (results including the suspect value: mean = 67.8 ppm, SD = 53.2 ppm, RSD = 79%). b

 Results excluding the suspect value (results including the suspect value: mean = 52.8 ppm, SD = 38.6 ppm, RSD = 73%). c
27

Environmental Soil Samples

The precision of the reference laboratory for the analysis of environmental soil samples is reported in Table 4-

3. In this table, results including suspect measurements are presented in parentheses. Average concentrations

were reported by the reference laboratory as ranging from 0.5 to 1196 ppm with RSDs that ranged from 7 to

118% when the suspect results were included. Excluding the suspect results, the highest average concentration

decreased to 660 ppm, and the largest RSD decreased to 71%. Because the majority of the samples fell below

125 ppm, precision was also assessed by partitioning the results into two ranges: low concentrations (< 125

ppm) and high concentrations (> 125 ppm). For the low concentrations, the average RSD was 23% excluding

the suspect value and 26% including the suspect value. These average RSDs were only slightly larger than the

RSDs for the PE soil samples of comparable concentration (18% for best case and 21% for worst case). Five

soil sample sets (sample IDs: 106, 117, 205, 211 and 217) were in the high-concentration category. The

average precision for high concentrations was 56% for the worst case and 19% for the best case. The precision

estimates for the low and high concentration ranges were comparable when the suspect values were excluded.

This indicated that the reference laboratory’s precision for the environmental soils was consistent

(approximately 21% RSD) and was comparable to the PE soil samples when the suspect values were excluded.

The Paducah soils (indicated as bold sample IDs in Table 4-3) were analyzed by the technologies under both

outdoor and chamber conditions to provide a measure of the effect that two different environmental conditions

had on the technology’s performance. Although this was not an issue for the reference laboratory (because all

the samples were analyzed under laboratory conditions), the reference laboratory’s results were delineated into

the different site categories for comparison with the technologies. Sample IDs 113 and 201, 114 and 202, 115

and 203, 116 and 204, and 117 and 205 each represent a set of eight replicate samples of the same Paducah

soil. The RSDs for four of the five Paducah pairs (excluding the suspect value for sample ID 205) ranged from

11 to 17%. The result from one pair (sample IDs 113 and 201) had an RSD of 42%, but the reported average

concentration was near the reporting limits.

Extract Samples

The extract samples, which were used to simulate surface wipe samples, were the simplest of all the

demonstration samples to analyze because they required no extraction and were interference-free. Three types

of extract samples were analyzed: solvent blanks, spikes of Aroclor 1248 at 10 μg/mL, and spikes of Aroclor

1016 at 100 μg/mL. The reference laboratory did not analyze the extract samples for the EnviroLogix

demonstration.

Accuracy 

Accuracy represents the closeness of the reference laboratory’s measured PCB concentrations to the accepted

values. Accuracy was examined by comparing the measured PCB concentrations in the PE soils with the

certified PE values and known spiked extract concentrations. Percent recovery was used to quantify the

accuracy of the results. The optimum percent recovery value is 100%. Percent recovery values greater than

100% indicate results that are biased high, and values less than 100% indicate results that are biased low.
28

Table 4-3. Precision of the reference laboratory for environmental soil samples

Outdoor site Chamber site

Sample RSD Sample RSD

ID (%) ID (%)

Average Standard Average Standard

concentration deviation concentration deviation

(ppm) (ppm) (ppm) (ppm)

101 0.5 0.1 16 206 1.9 0.9 49

102 2.0 0.3 16 207 18.8 3.5 19

103 2.3 0.6 27 208 30.5 7.9 26

104 9.4 4.0 43 209 40.2 28.5 71

105 59.4 16.5 28 210 88.6 25.6 29

106 281.0 32.4 12 211 404.5 121.8 30

(373.2) (186.2) (50) a

107 1.3 0.3 20 212 3.2 1.6 50

108 1.8 0.1 8 213 8.1 1.6 20

109 2.0 0.4 20 214 25.2 3.7 15

110 n/a n/a n/a 215 26.7 3.2 12 b

111 38.7 4.3 11 216 55.1 8.5 15 

(79.2) (48.7) (62)

112 n/a n/a n/a 217 659.8 196.6 30 

(973.2) (647.0) (66)

 113 c 1.1 0.6 55 201 0.9 0.2 24

114 1.3 0.3 20 202 1.4 0.2 12

115 14.8 1.8 12 203 13.9 1.7 12

116 41.3 5.9 14 204 44.3 2.9 7

117 383.9 55.2 14 205 493.0 41.7 8 

(1196.0) (1406.4) (118)

Data in parentheses include suspect values. a

N/a indicates that qualitative results only were reported for this sample. b

 Bold sample IDs were matching Paducah sample pairs (i.e., 113/201, 114/202, 115/203, 116/204, 117/205). c

The reference laboratory’s performance for the PE samples is summarized in Table 4-4. Included in this table

are the performance acceptance ranges and the certified PCB concentration values. The acceptance ranges,

based on the analytical verification data, are guidelines established by the provider of the PE materials to gauge

acceptable analytical results. As shown in Table 4-4, all of the average concentrations were within the

acceptance ranges, with the exception of sample ID 218. The average result of sample ID 225 was outside of
29

the acceptance range only when the suspect result was included. All of the replicate measurements in sample

ID 225 were biased slightly high. Average percent recoveries for the PE samples (excluding suspect values)

ranged from 76 to 130%. Overall accuracy was estimated as the average recovery for all PE samples. The

overall percent recovery was 105% as a worst case when the suspect value was included. Excluding the suspect

value as a best case slightly lowered the overall percent recovery to 101%. A regression analysis [7] indicated

that the reference laboratory’s results overall were unbiased estimates of the PE sample concentrations.

Table 4-4. Accuracy of the reference laboratory for PE soil samples

Certified

concentration

(ppm)

(acceptance 

range, ppm)

Outdoor site Chamber site Combined sites

Sample Recovery Sample Recovery Recovery

ID (%) ID (%) (%)

Average Average Average

conc conc conc

(ppm) (ppm) (ppm)

0

a

(n/a)

126 0 n/a 226 0 n/a 0 n/a

2.0 118 1.6 79 218 2.6 130 2.1 105

(0.7-2.2)

2.0 124 1.7 85 224 1.7 85 1.7 85

(0.9-2.5)

5.0 120 5.0 99 220 5.8 117 5.4 108

(2.1-6.2)

10.9 122 11.1 102 222 12.8 117 11.9 109

(4.0-12.8)

20.0 119 20.1 100 219 23.3 116 21.7 109

(11.4-32.4)

49.8 125 37.9 76 225 41.7 84 79 

(23.0-60.8)

b b

 39.5 c c

50.0 121 54.6 109 221 44.9 90 49.8 100

(19.7-63.0)

50.0 123 60.1 120 223 55.8 112 58.0 116

(11.9-75.9)

All PCB concentrations reported as non-detects by the laboratory. a

Results excluding the suspect value (results including the suspect value: average = 67.8 ppm and recovery = 136%). b

Results excluding the suspect value (results including the suspect value: average = 52.8 ppm and recovery = 106%). c

Representativeness

Representativeness expresses the degree to which sample data accurately and precisely represent the capability

of the method. Representativeness of the method was assessed based on the data generated for clean-QC

samples (i.e., method blanks and laboratory control samples) and PE samples. Based on the data assessment

discussed in detail in various parts of this section, it was determined that the representativeness of the reference

laboratory data was acceptable. In addition, acceptable performance on laboratory audits substantiated that
30

the data set was representative of the capabilities of the method. In all cases, the performance of the reference

laboratory met all requirements for both audits and QC analyses.

Completeness

Completeness is defined as the percentage of measurements that are judged to be usable (i.e., the result was

not rejected). Usable results were obtained for 248 of the 256 samples submitted for analysis by the reference

laboratory. Eight results (for sample IDs 110 and 112) were deemed incomplete and therefore not valid because

the measurements were not quantitative. To calculate completeness, the total number of complete results were

divided by the total number of samples submitted for analysis, and then multiplied by 100 to express as a

percentage. The completeness of the reference laboratory was 97%, where a completeness of 95% or better is

typically considered acceptable.

Comparability

Comparability refers to the confidence with which one data set can be compared with another. The

demonstration study was designed to have a one-to-one, sample-by-sample comparison of the PCB results

obtained by the reference laboratory and the PCB results obtained by the technology being evaluated. Based

on thorough examination of the data and acceptable results on the PE samples, it was concluded that the

reference laboratory’s SOPs for extraction and analysis, and the data generated using these procedures, were

of acceptable quality for comparison with the field technology results. Additional information on comparability

was available because the experimental design incorporated randomized analysis of blind, replicate samples.

Evaluation of the replicate data implicated some of the individual data points as suspect (see Table D-2). The

reference laboratory’s suspect data were compared with the technology data on a special-case basis, and

exceptions were noted. 

Summary of Observations

Table 4-5 provides a summary of the performance of the reference laboratory for the analysis of all sample

types used in the technology demonstration study. As shown in the table, the precision of the PE soils was

comparable to that of the environmental soils. A weighted average, based on the number of samples, gave a

best-case precision of 21% and a worst-case precision of 28% for all the soil data (PE and environmental).

Evaluation of overall accuracy was based on samples with certified concentrations. The overall accuracy, based

on percent recovery, for the PE samples (which ranged from 0 to 50 ppm) was 105% for the worst case (which

included the suspect value) and 101% for the best case (which excluded the suspect value). These results

indicated that the reference laboratory results were unbiased estimates of the certified PE concentrations. The

reference laboratory correctly reported all blank samples as non-detects but had difficulty with two soil samples

(IDs 110 and 112) that contained chemical interferences. Overall, it was concluded that the reference laboratory

results were acceptable for comparison with the developer’s technology. 
31

Table 4-5. Summary of the reference laboratory performance

Sample matrix Sample type Number of Precision Accuracy 

samples (average % RSD) (average % recovery)

Blank Soil 8 n/a a All samples reported as

non-detects

Environmental soil with Sample ID 110 4 All samples reported as

interferences Sample ID 112 4 non-detects n/a a

Soil — Best case PE 63 18 101

(excluding suspect data) Environmental

< 125 ppm 107 23

> 125 ppm 17 19

n/a b

n/a b

Overall 187 21 101

Soil — Worst case PE 64 21 105

(including suspect data) Environmental

< 125 ppm 108 26

> 125 ppm 20 56

n/a b

n/a b

 Overall 192 28 105

 Because the results were reported as non-detects, precision assessment is not applicable. a

Accuracy assessment calculated for samples of known concentration only. b
32
33

Section 5

Technology Performance and Evaluation

Objective and Approach

This section presents the evaluation of the data generated by EnviroLogix’s PCB in Soil Tube Assay. The

technology’s precision and accuracy are presented for the data generated in the demonstration study. In

addition, an evaluation of comparability, through a one-to-one comparison with the reference laboratory data,

is presented. An evaluation of other aspects of the technology (such as cost, sample throughput, hazardous

waste generation, and logistical operation) is also presented in this section.

Interval Reporting

The PCB in Soil Tube Assay results were reported as concentration ranges that were designated as intervals

incorporating parenthesis/bracket notation. The parentheses indicated that the end-points of the concentration

range were excluded, while brackets indicated that the end-points were included. The reporting intervals for

soils and extracts are presented in Table 5-1. Note that the intervals are different for the soils and extracts

because the soils incorporate an extraction step into the procedure. As shown in the table, the interval [1, 10)

indicates that the PCB concentration range is $1 and <10. 

Table 5-1. PCB in Soil Tube Assay reporting intervals

Interval Interval Soil concentration Extract concentration

range range

[0, 1) 0# PCB ppm < 1 [0, 0.4) 0# PCB ppm < 0.4

[1, 10) 1# PCB ppm < 10 [0.4, 4) 0.4# PCB ppm < 4

[10, 50) 10 # PCB ppm < 50 [4, 20) 4 # PCB ppm < 20

[50, 4) PCB ppm $ 50 [20, 4) PCB ppm $ 20

Data Assessment

Objective

The purpose of the data assessment section is to present the evaluation of the performance of EnviroLogix’s

PCB in Soil Tube Assay through a statistical analysis of the data. PARCC parameters were used to evaluate

the test kit’s ability to measure PCBs in PE soil, environmental soil, and extract samples. The developer

analyzed splits of replicate samples that were also analyzed by the reference laboratory (72 PE soil samples

and 136 environmental soil samples). See Section 4 for a more detailed analysis of the reference laboratory’s

results. Replicate samples were analyzed by the developer at two different sites (under outdoor conditions and

inside an environmentally controlled chamber) to evaluate the effect of environmental conditions on the test
34

kit’s performance; see Section 3 for further details on the different sites. Evaluation of the measurements made

at each site indicated that there were no significant differences between the two data sets. Because

environmental conditions did not appear to affect the results significantly, data from both sites were also

combined for each parameter—precision and accuracy—to determine the test kit’s overall performance. All

statistical tests were performed at the 5% significance level. Appendix D contains the raw data that were used

to assess the performance of the kit.

Precision

Precision is the reproducibility of measurements under a given set of conditions. The frequency with which the

same interval was reported within a set of replicates was used to quantify precision. Examples of how the

precision was classified are presented in Table 5-2. Reporting a higher number of replicates in the same interval

for a given replicate set indicates higher precision. In other words, reporting all four replicate results as the

same interval indicates the highest possible precision.

Table 5-2. Classification of precision results

If the replicate results are . . . . . . then the number reported . . . and the precision

in identical intervals are . . . classification is . . .

[1, 10), [1, 10), [1, 10), [1, 10) 4 high

[0, 1), [1, 10), [1, 10), [1, 10) 3 medium

[0, 1), [1, 10), [1, 10), [10, 50) 2 low

[0, 1), [1, 10), [10, 50), [50, 4) 0 none

Performance Evaluation Samples

Table 5-3 summarizes the precision information for the test kit’s analysis of the PE samples. The PCB in Soil

Tube Assay reported all four replicates as the same interval (i.e., high precision) for five of the eight PE sample

sets under outdoor conditions, and four of the eight PE sample sets under the chamber conditions. Operating

under the outdoor conditions, all eight replicate sets were classified as having either medium or high precision.

Under the chamber conditions, medium to high precision was achieved for five of eight replicate sets, with the

remaining three replicate sets classified as having low precision. A more detailed analysis of the data showed

that the replicates classified as having medium to low precision were never more than one interval away from

the most frequently reported interval. None of the replicate sets were classified with the lowest precision (i.e.,

none) under either set of environmental conditions. With the exception of sample ID 119, the sample sets with

low to medium precision had concentrations that were near threshold values (i.e., 10 and 50 ppm), which

caused the results to be split into two intervals. For example, for sample ID 222, which had a nominal

concentration of 10.9 ppm, the technology reported two results in the [1, 10) interval and two results in the

[10, 50) interval.
35

Table 5-3. Precision of the PCB in Soil Tube Assay for PE soil samples

Outdoor site Chamber site

Certified

PE Conc. Number of replicates reported in Number of replicates reported in 

(ppm) identical intervals identical intervals Sample Sample

ID ID

precision precision 

 none +!!!!!!!!!!!!!!!!!, +!!!!!!!!!!!!!!!!!, high none +!!!!!!!!!!!!!!!!!!, +!!!!!!!!!!!!!!!!!!, high

0 2 3 4 0 2 3 4

a a

0 126 x 226 x

b b

2.0 118 x 218 x

2.0 124 x 224 x

5.0 120 x 220 x

10.9 122 x 222 x

20.0 119 x 219 x

49.8 125 x 225 x

50.0 121 x 221 x

50.0 123 x 223 x

No. in each precision classification 0 0 3 5 0 3 1 4

 Indicates that all four replicates were reported as different intervals. a

 Blank data were not included in the determination of the overall precision. b

Environmental Soil Samples

The PCB in Soil Tube Assay results for the replicate environmental soil sample measurements are presented

in Table 5-4. Under the outdoor conditions, the highest precision classification (i.e., the same interval reported

for all four replicates) was achieved for 12 of 17 replicate sets. Under the chamber conditions, 11 of 17 sample

sets were classified as high-precision. None of the replicate sets were classified with the lowest precision (i.e.,

none) under either set of environmental conditions. Of the sample sets for which precision was classified as

medium to low, only sample ID 203 had one replicate result that differed by more than one interval range.

Because most of the measurements fell below 125 ppm, precision was also assessed by partitioning the results

into two ranges: low concentration (reference laboratory values < 125 ppm) and high concentration (reference

laboratory values > 125 ppm). See Section 4 for the delineation of which sample IDs were in the low and high

categories. For the low concentrations, 62% of the sample sets (18 of 29) were reported with
36

Table 5-4. Precision of the PCB in Soil Tube Assay for environmental soil samples

Outdoor site Chamber site

Sample Sample

ID ID

precision precision 

none +!!!!!!!!!!!!!!!!!, +!!!!!!!!!!!!!!!!!, high none +!!!!!!!!!!!!!!!!!, +!!!!!!!!!!!!!!!!!, high

Number of replicates reported in Number of replicates reported in

identical intervals identical intervals

0 2 3 4 0 2 3 4

a a

101 x 206 x

102 x 207 x

103 x 208 x

104 x 209 x

105 x 210 x

106 x 211 x

107 x 212 x

108 x 213 x

109 x 214 x

110 x 215 x

111 x 216 x

112 x 217 x

113 201 b x x

114 x 202 x

115 x 203 x

116 x 204 x

117 x 205 x

No. in each

precision 0 2 3 12 0 2 4 11

classification

 Indicates that all four replicates were reported as different intervals. a

 Bold sample IDs were matching Paducah sample pairs (i.e., 113/201, 114/202, 115/203, 116/204, 117/205). b

all four replicates in the same interval (i.e., highest possible precision). For the high concentration category,

100% of the sample sets (five of five) were reported with the highest possible precision.

The Paducah soils (indicated by bold sample IDs in Table 5-4) were analyzed at both sites to provide an

assessment of the test kit’s performance under different environmental conditions. For these samples, the data

generated under both environmental conditions were also combined to provide an overall assessment of

precision. Sample IDs 113 and 201, 114 and 202, 115 and 203, 116 and 204, and 117 and 205 represented

replicate Paducah soil sample sets; the 100 series were samples analyzed under the outdoor conditions, and the

200 series were samples analyzed inside the chamber. Additional statistical analysis was used to compare the

effect of the two environmental conditions on the measurements. Results from this analysis showed that there

were no significant differences in the data generated at each site. This indicated that these different

environmental conditions did not affect the performance of the test kit.
37

Extract Samples

The PCB in Soil Tube Assay results for the replicate extract measurements are presented in Table 5-5. All

three sample sets analyzed under the chamber conditions were reported with the highest possible precision (i.e.,

all four replicates were within the same interval). Two sample sets analyzed under the outdoor conditions

achieved the highest precision, and the remaining sample set (sample ID 132) was reported with low precision

(i.e., two replicates were reported in the same interval).

Table 5-5. Precision of the PCB in Soil Tube Assay for extract samples

Outdoor site Chamber site

Sample ID identical intervals Sample ID identical intervals

precision precision 

none +!!!!!!!!!!!!!!!!!, +!!!!!!!!!!!!!!!!!, high none +!!!!!!!!!!!!!!!!!, +!!!!!!!!!!!!!!!!!, high

Number of replicates reported in Number of replicates reported in 

0 2 3 4 0 2 3 4

 a a

130 x 230 x

b b

131 x 231 x

132 x 232 x

No. in each

precision 0 1 0 1 0 0 0 2

classification

 Indicates that all four replicates were reported as different intervals. a 

 Blank data were not included in the determination of the overall precision b

Precision Summary

A summary of the test kit’s overall precision is presented by sample type (PE, environmental soil, and extract

samples) in Table 5-6. For PE and environmental soil samples, 56% and 68% of the samples, respectively,

achieved the highest possible precision (i.e., all four sample replicates were reported as the same interval). For

the extract samples, 75% of the samples achieved the highest precision.

Accuracy 

Accuracy represents the closeness of the PCB in Soil Tube Assay’s measured PCB concentrations to the

certified values. Because the test kit produced interval results, accuracy was evaluated in terms of the

percentage of samples that agreed with, were above (i.e., biased high), and were below (i.e., biased low) the

certified value.
38

Table 5-6. Overall precision of the PCB in Soil Tube Assay for all sample types

Environmental

site

Percentage of samples classified in each precision category

PE samples Environmental soil samples Extract samples

None Low Med High None Low Med High None Low Med High

Outdoor site 0 0 38 63 0 12 18 71 0 50 0 50

Chamber site 0 38 13 50 0 12 24 65 0 0 0 100

Combined sites 0 19 25 56 0 12 21 68 0 25 0 75

Performance Evaluation Soil Samples

Table 5-7 contains a comparison between the PCB in Soil Tube Assay’s interval result and the corresponding

certified PE value. The interval(s) listed under a particular column indicate how many of the four replicates

were reported as that interval. For example, for sample ID 222, two replicates were reported as [1, 10), and

two were reported as [10, 50). For sample ID 119, three are reported as [10, 50), and one is reported as [1, 10).

The table also presents performance acceptance ranges for the PE results, which are the guidelines established

by the provider of the PE materials to gauge acceptable analytical results. These ranges were not used to

evaluate the test kit results because the acceptance ranges overlap several reporting intervals. However, in all

but two individual analyses of PE samples, the reported interval result included a value within the range of

acceptable results.

The data in Table 5-7 were used to derive the accuracy results that are presented in Table 5-8. Accuracy was

based on a comparison of the certified PE value with the interval reported by the test kit. If the interval

encompassed the certified PE value, the PCB in Soil Tube Assay result “agreed” with the certified value. If

the test kit result was above the certified value, the result was classified as “biased high.” If the test kit result

was below the certified value, the result was classified as “biased low.” For example, for sample ID 222, the

certified value was 10.9 ppm (for Aroclor 1260). The comparison would be classified as “agreed” for the PCB

in Soil Tube Assay interval result [10, 50) and as “biased low” for the interval result [1, 10). 

Separate comparisons were made for the two environmental conditions to determine if ambient temperature and

humidity had an effect on the technology performance. Statistical analysis showed that there was no significant

difference between the results obtained by the test kit under the two different environmental conditions

evaluated in this demonstration. Therefore, all PE sample results were combined to determine the overall

percentage of agreement between the PCB in Soil Tube Assay results and the certified PE value. The overall

percentage of agreement was 78%. A comparable number of results were biased high (10%) and biased low

(13%). For most of the samples which did not agree with the certified value, the result was near a test kit

threshold value. For example, six of the eight test kit results for sample IDs 125 and 225 were [50, 4); the other

two results were [10, 50). The nominal concentration for these PE sample was 49.8 ppm, so those reported [10,

50) would be in agreement with the certified value, while the results reported as [50, 4) were biased high. It

appears that the test kit generally reports the more conservative (i.e., higher)
39

Table 5-7. PCB in Soil Tube Assay accuracy data for PE soil samples

Certified

conc. (ppm)

(Acceptance

range, ppm)

Outdoor site Chamber site

Sample Sample

ID ID

# of replicates reported at each interval # of replicates reported at each interval

1 2 3 4 1 2 3 4

0

(n/a) 126 [0, 1) 226 [0, 1)

2.0

(0.7-2.2) 118 [1, 10) [0, 1) 218 [1, 10)

2.0

(0.9-2.5) 124 [1, 10) 224 [1, 10)

5.0

(2.1-6.2) 120 [1, 10) 220 [1, 10)

10.9 [1, 10)

(4.0-12.8) [10, 50) 122 [50, 4) [10, 50) 222 a

20.0

(11.4-32.4) 119 [1, 10) [10, 50) 219 [10, 50) a

49.8 [10, 50)

(23.0-60.8) [50, 4)

125 [50, 4) 225

50.0 [10, 50)

(19.7-63.0) [50, 4)

121 [50, 4) 221

50.0

(11.9-75.9) 123 [50, 4) 223 [10, 50) [50, 4)

 Result not included in the acceptance range. a

interval when the result is near the threshold value of 50 ppm (see Regulatory Decision-Making Applicability

section for more information). Note that in a situation where the sample concentration is near the threshold

value, the operator of the test kit can compare the optical density of the sample assay to that of the calibration

assay and recognize that the sample concentration is near the threshold value.

Extract Samples

Table 5-9 contains a comparison between the PCB in Soil Tube Assay interval result and the corresponding

spike concentration for the extract samples. The test kit’s percentage of agreement with the spike concentration

of the extract samples is summarized in Table 5-10. Statistical analysis showed that environmental conditions

had no significant effect upon the performance of the test kit. Therefore, the data sets generated under the

outdoor and chamber conditions were combined. Overall, 22 of 24 extract samples (92%) agreed with the spike

concentration. Two 100-ppm spiked samples (8%) were biased low relative to the spike concentration. None

were biased high.
40

 Table 5-8. Evaluation of agreement between PCB in Soil Tube Assay’s PE sample results and the 

 certified PE values as a measure of accuracy

Environmental

site

Relative to certified values for performance

evaluation samples

Number of

Biased Agree Biased samples

low high

Outdoor site 11% 75% 14% 36

Chamber site 14% 81% 6% 36

Combined sites 13% 78% 10% 72

 Table 5-9. Accuracy of the PCB in Soil Tube Assay for extract samples

Spike conc. # of replicates reported at each interval # of replicates reported at each interval

(μg/mL)

Outdoor site Chamber site

Sample Sample

ID ID 1 2 3 4 1 2 3 4

0 132 [0, 0.4) 232 [0, 0.4)

10 130 [4, 20) 230 [4, 20]

100 131 231 [20, 4)

[20, 4)

[4, 20)

 Table 5-10. Evaluation of agreement between PCB in Soil Tube Assay’s extract results and the spike 

 concentration as a measure of accuracy

Environmental

site

Relative to spike concentration for extract

samples Number of

samples Biased Agree Biased

low high

Outdoor site 17% 83% 0% 12

Chamber site 0% 100% 0% 12

Combined sites 8% 92% 0% 24

False Positive/False Negative Results

A false positive (fp) result [10] is one in which the technology detects PCBs in the sample above the detection

limit when there actually are no PCBs present. A false negative (fn) result [8] is one in which the technology

indicates that there are no PCBs present in the sample, when there actually are. Both fp and fn results are

influenced by the method detection limit of the technology. All of the eight blank soil samples were reported

as the lowest reporting interval, which included zero, so the fp result was 0%. Of the 192 non-blank soil

samples analyzed, the PCB in Soil Tube Assay reported twelve in the lowest reporting interval (0 to 1 ppm ).
41

Five of the corresponding reference laboratory results fell into the test kit’s reporting interval (0.5 ppm), and

were therefore reported correctly. Seven results were false negatives. Therefore, 4% of the soil sample results

were false negatives. For the eight extract samples, the kit reported all blanks as [0, 1), indicating no fp results.

All other extract samples were reported as non-blanks; therefore, the fn result was 0%.

Representativeness

Representativeness expresses the degree to which the sample data accurately and precisely represent the

capability of the technology. The performance data were accepted as being representative of the technology

because the PCB in Soil Tube Assay was capable of analyzing diverse sample types (PE samples, simulated

wipe extract samples, and actual field environmental samples) under multiple environmental conditions. When

this technology is used, QC samples should be analyzed to assess the performance of the test kit under the

testing conditions.

Completeness

Completeness is defined as the percentage of measurements that are judged to be useable (i.e., the result was

not rejected). Valid results were obtained by the technology for all 232 samples. Therefore, completeness was

100%.

Comparability

Comparability refers to the confidence with which one data set can be compared to another. A one-to-one

sample comparison of the PCB in Soil Tube Assay results and the reference laboratory results was performed

for all soil samples. Accuracy was evaluated in terms of the percentage of samples that agreed with, were above

(i.e., biased high), and were below (i.e., biased low) the certified value. For comparability, the test kit results

were compared with the results generated by the reference laboratory, including both environmental soils and

PE samples. Sample IDs 110 and 112 were excluded because the reference laboratory did not generate

quantitative results for these samples. The results are summarized in Table 5-11. The percentage of PCB in

Soil Tube Assay results that agreed with the reference laboratory results was 81%. Approximately 12% were

biased high, and approximately 7% were biased low relative to the results reported by the reference laboratory.

For the extract samples, the test kit’s results could not be compared with the reference laboratory’s results

because no reference laboratory data were generated for these samples.

The soil data not included in previous comparability evaluations (because the replicate data for the reference

laboratory were considered suspect) are shown in Table 5-12. Refer to Section 4, especially Table 4-1, for

more information on the reference laboratory’s suspect measurements. The reference laboratory’s suspect data

were compared with the PCB in Soil Tube Assay’s matching results. For sample IDs 110 and 112, the

reference laboratory obtained qualitative results only. The test kit appeared to have little difficulty with these

samples, as all four replicates were reported as the same interval. For the other five suspect values for the

reference laboratory data, the test kit generated results that agreed with the replicate means of the reference

laboratory. The only exceptions were sample IDs 216 and 225, where the 
42

 Table 5-11. Evaluation of agreement between PCB in Soil Tube Assay’s soil results and the reference 

 laboratory’s results as a measure of comparability

Environmental Number of

site samples

Relative to reference laboratory results for

soil samples

Biased Agree Biased

low high

Outdoor site 7% 78% 15% 96

Chamber site 6% 85% 10% 104

Combined sites 7% 81% 12% 200

reference laboratory results were near the kit’s threshold value of 50 ppm. These comparisons demonstrated

that the PCB in Soil Tube Assay did not have difficulty with most of the samples that were troublesome for

the reference laboratory.

Summary of PARCC Parameters

Table 5-13 summarizes the test kit’s performance for precision, accuracy, and comparability. Precision was

assessed by the percentage of replicate samples where the highest precision was achieved (i.e., all four

replicates were reported as the same interval), which was 56% for the PE samples, 62% for the environmental

soils, and 75% for the extract samples. The test kit’s performance was based on agreement and disagreement

with the certified PE values (accuracy) and the reference laboratory results (comparability). Overall, the test

kit’s performance was similar for all samples because the percentages of agreement and disagreement were not

significantly different for each sample type. The percentage in agreement ranged from 78 to 92, the percentage

biased high was 10 to 13, and the percentage biased low was 6 to 13.

Regulatory Decision-Making Applicability

One objective of this demonstration was to assess the technology’s ability to perform at regulatory decisionmaking levels for PCBs, specifically 50 ppm for soils. To assess this ability, the test kit’s performance for PE

and environmental soil samples ranging in concentration from 40 to 60 ppm (as determined by the paired

reference laboratory analyses) can be used. For this concentration range, the test kit’s results agreed with the

reference laboratory’s results 66% of the time. Results were biased high 32% of the time, and 2% of the results

were biased low. No false negatives were observed. The test kit results for this concentration range were

different from what was observed for the entire data set, in that the percentage of samples that were biased high

was significantly higher (32% versus 12%). This indicates that the test kit results appear to have a higher

percentage of results that are reported more conservatively (i.e., reported in a higher interval range than the

actual result) for this concentration range than for the entire concentration range of the samples analyzed (0

to 700 ppm).
43

Table 5-12. Comparison of the PCB in Soil Tube Assay results with the reference laboratory’s suspect measurements

Sample ID

Reference laboratory PCB in Soil Tube Assay

 Suspect measurement Replicate mean Suspect-matching No. of replicates

(ppm) (ppm) result reported as this

a

(ppm) interval

110 #RDL #RDL [10, 50) 4

b b

112 #RDL #RDL [50, 4) 4

b b

106 649.6 281.0 [50, 4) 4

205 3,305.0 493.0 [50, 4) 4

216 151.6 55.1 [10, 50) 2

217 1,913.3 659.8 [50, 4) 4

225 146.0 41.7 [50, 4) 2

Mean result excluding the suspect measurement. a

 Measurement reported qualitatively as less than or equal to the reporting detection limit (RDL) for all replicates (See b

Table D-1).

 Table 5-13. PCB in Soil Tube Assay performance for precision, accuracy, and comparability

Sample type

Precision a Accuracy b Comparability c

% 

high

precision

% % % % % % 

biased low agreed biased high biased low agreed biased high

PE 56 13 78 10 8 82 10

Environmental

soil 68 n/a n/a n/a 6 81 13 b

Extract 75 8 92 0 n/a n/a n/a c

Percentage of sample sets that achieved highest precision (i.e., all four replicates were reported as the same interval). a

 PCB in Soil Tube Assay result vs certified value. Note that accuracy cannot be assessed for environmental soils. b

 PCB in Soil Tube Assay result vs reference laboratory result. Comparability cannot be assessed for extract samples. c
44

Additional Performance Factors

Sample Throughput

Sample throughput is representative of the estimated amount of time required to extract the PCBs, to perform

appropriate reactions, and to analyze the sample. Operating under the outdoor conditions, one analyst from

EnviroLogix had a sample throughput rate of about eight samples per hour. Working in the chamber, the

analyst obtained a lower rate, around seven samples per hour. This increased sample throughput under the

outdoor conditions may be attributed to the analysis order: because the EnviroLogix analyst performed sample

analyses under the chamber conditions first, he may have gained valuable experience that was applied during

the analysis of the outdoor samples. Alternatively, EnviroLogix may have had more difficulty with the sample

matrices that were analyzed only under the indoor conditions.

Cost Assessment

The purpose of this economic analysis is to provide an estimation of the range of costs for an analysis of PCBcontaminated soil samples using the PCB in Soil Tube Assay and a conventional analytical reference laboratory

method. The analysis was based on the results and experience gained from this demonstration, costs provided

by EnviroLogix, and representative costs provided by the reference analytical laboratories that offered to

analyze these samples. To account for the variability in cost data and assumptions, the economic analysis was

presented as a list of cost elements and a range of costs for sample analysis using the test kit and by the

reference laboratory.

Several factors affected the cost of analysis. Where possible, these factors were addressed so that decisionmakers can independently complete a site-specific economic analysis to suit their needs. The following

categories are considered in the estimate: 

• sample shipment costs, 

• labor costs, 

• equipment costs, and

• waste disposal costs. 

Each of these cost factors is defined and discussed and serves as the basis for the estimated cost ranges

presented in Table 5-14. Costs for sample acquisition and pre-analytical sample preparation, which are tasks

common to both methods, were not included here. This analysis assumed that the individuals performing the

analyses were fully trained to operate the technology. EnviroLogix provides free assistance, on an as-needed

basis, through its technical service department. It also offers a free one-day training session on the kit at its

facility in Portland, Maine. Training at the user’s facility is handled on a case-by-case basis. 
45

Table 5-14. Estimated analytical costs for PCB soil samples

PCB in Soil Tube Assay EPA SW-846 Method 8081

EnviroLogix Inc. Reference laboratory

Sample throughput rate: 8 samples/hour (outdoors) Typical turnaround time: 14–30 days

 7 samples/hour (chamber) Actual turnaround time: 72 days

Cost category Cost ($) Cost category Cost ($)

Sample shipment 0 Sample shipment

Labor

 Mobilization/demobilization 250–400

 Travel 15–1000 per analyst

 Per diem 0–150 per day per analyst

 Rate 30–75 per hour per analyst

Equipment

 Mobilization/demobilization 0–150 

 Purchase field lab kit 965–1975 

 Reagents/supplies 18 per sample

Waste disposal 135–1790

 Labor 100–200

 Overnight shipping charges 50–150

Labor

 Mobilization/demobilization Includeda

 Travel Included

 Per diem Included

 Rate 44–239 per sample

Equipment

 Mobilization/demobilization Included

 Purchase field lab kit Included

 Reagents/supplies Included

Waste disposal Included

“Included” indicates that the cost is included in the labor rate. a

PCB in Soil Tube Assay Costs

• Sample shipment costs. Because the samples were analyzed on site, no sample shipment charges were

associated with the cost of operating the test kit. 

• Labor costs. Labor costs included mobilization/demobilization, travel, per diem, and on-site labor.

— Labor mobilization/demobilization: This cost element included the time for one person to

prepare for and travel to each site. The estimate ranged from 5 to 8 hours, at a rate of $50 per

hour.

— Travel: This element was the cost for the analyst(s) to travel to the site. If the analyst is

located near the site, the cost of commuting to the site (estimated to be 50 miles at $0.30 per

mile) would be minimal ($15). The estimated cost of an analyst traveling to the site for this

demonstration ($1000) included the cost of airline travel and rental car fees.

— Per diem: This cost element included food, lodging, and incidental expenses and was estimated

ranging from zero (for a local site) to $150 per day per analyst

— Rate: The cost of the on-site labor was estimated at a rate of $30 to $75 per hour, depending

on the required expertise level of the analyst. This cost element included the labor involved

with the entire analytical process comprising sample preparation, sample management,

analysis, and reporting. 
46

• Equipment costs. Equipment costs included mobilization/demobilization, purchase of equipment, and

the reagents and other consumable supplies necessary to complete the analysis.

— Equipment mobilization/demobilization: This included the cost of shipping the equipment to

the test site. If the site is local, the cost would be zero. For this demonstration, the cost of

shipping equipment and supplies was estimated at $150.

— Purchase of field test lab: At the time of the demonstration, EnviroLogix offered a field

laboratory that would include all of the equipment necessary to complete the analyses for a

cost of $1975. The field laboratory includes a Microman M-25 positive displacement pipettor,

an Eppendorf Repeater pipettor, Acculab pocket balance, Artel Differential Photometer, wash

bottle, and black suitcase. The field lab can also be purchased without the photometer for

$965 (photometer alone is $1250).

— Reagents/supplies: These items are consumable and are purchased on a per-sample basis. At

the time of the demonstration, the cost of the reagents and supplies needed to prepare and

analyze PCB soil samples using the test kit was $18 per sample. This cost included the sample

preparation/ extraction supplies (including solvent), assay supplies, and consumable reagents.

• Waste disposal costs. Waste disposal costs are estimated based on the 1997 regulations for disposal

of PCB-contaminated waste. The test kit generated approximately 43 lb of vials containing soils and

liquid solvents (classified as solid PCB waste suitable for disposal by incineration) and approximately

43 lb of other solid PCB waste (used and unused soil, gloves, paper towels, ampules, etc.). The cost

of disposing of PCB solid waste by incineration at a commercial facility was estimated at $1.50 per

pound. The cost for solid PCB waste disposal at ETTP was estimated at $18/lb. The test kit also

generated approximately 21 lb of liquid waste. The cost for liquid PCB waste disposal at a commercial

facility was estimated at $0.25/lb, while the cost at ETTP was estimated at $11/lb.

Reference Laboratory Costs

• Sample shipment costs. Sample shipment costs to the reference laboratory included overnight

shipping charges, as well as labor charges associated with the various organizations involved in the

shipping process. 

— Overnight shipping: The overnight express shipping service cost was estimated to be $50 for

one 50-lb cooler of samples.

— Labor: This cost element included all of the tasks associated with the shipment of the samples

to the reference laboratory. Tasks included packing the shipping coolers, completing the chainof-custody documentation, and completing the shipping forms. Because the samples contained

PCBs, the coolers were inspected by qualified personnel to ensure acceptance with the U.S.

Department of Transportation’s shipping regulations for PCBs. The estimate to complete this

task ranged from 2 to 4 hours at $50 per hour.

• Labor, equipment, and waste disposal costs. The labor bids from commercial analytical reference

laboratories who offered to perform the PCB analysis for this demonstration ranged from $44 per

sample to $239 per sample. The bid was dependent on many factors, including the perceived difficulty

of the sample matrix, the current workload of the laboratory, and the competitiveness of the market.

In this case, the wide variation in bids may also be related to the cost of PCB waste disposal in a

particular laboratory’s state. LAS Laboratories was awarded the contract to complete the analysis as
47

the lowest qualified bidder ($44 per sample). This rate was a fully loaded analytical cost that included

labor, equipment, waste disposal, and report preparation.

Cost Assessment Summary

An overall cost estimate for the PCB in Soil Tube Assay vs the reference laboratory was not made because of

the extent of variation in the different cost factors, as outlined in Table 5-14. The overall costs for the

application of each technology will be based on the number of samples requiring analysis, the sample type, and

the site location and characteristics. Decision-making factors, such as turnaround time for results, must also

be weighed against the cost estimate to determine the value of the field technology vs the reference laboratory.

General Observations

The following are general observations regarding the field operation and performance of the test kit:

• The system was light, easily transportable, and rugged. It took less than an hour for the

EnviroLogix analyst to prepare to analyze samples on the first day of testing. While working

at the outdoor site, the analyst completely disassembled his work station, bringing everything

inside at the close of each day. It took the analyst less than an hour each morning to prepare

for sample analyses.

• The technology was operated by a single person.

• Operators generally require 4 hours of training. They should have a basic knowledge of field

analytical techniques. 

• Each batch of samples was analyzed with 1 and 10 ppm standards and a negative control. (A

batch generally consisted of 12 to 17 samples). This controlled for changing environmental

conditions (i.e., temperature and humidity), and other causes of batch-to-batch variation.

• Data processing and interpretation was minimal. The results were quantified relative to the

two calibration standards and reported in terms of intervals. The photometer’s optical density

readings were recorded in a laboratory notebook.

• All reagents were allowed to come to ambient temperature before use. It is recommended that

all of the reagents in the test kit be stored under refrigerated conditions. When work was being

done outdoors, the analyst returned the reagents and calibrators to the refrigerator at the end

of the day. During the chamber work, the reagents were stored in the chamber overnight

because of the low temperature (around 57EF). New reagents and calibrators were used for

each site (i.e., outdoor and chamber conditions). 

• The measurement system (photometer) was recharged nightly. The analyst used the

photometer for up to 10 hours without recharging. The manufacturer specifies that 500

measurements can be made on a single battery charge. 

• The test kit generated approximately 43 lb of vials containing soils and liquid solvents

(classified as solid PCB waste suitable for disposal by incineration) and approximately 43 lb
48

of other solid PCB waste (used and unused soil, gloves, paper towels, ampules, etc.). The test

kit also generated approximately 21 lb of liquid waste (aqueous with trace methanol).

Performance Summary

A summary of the performance characteristics of EnviroLogix’s PCB in Soil Tube Assay, presented previously

in this section, is shown in Table 5-15. The performance of the test kit was characterized as unbiased, because

most (78%) of the PCB in Soil Tube Assay results agreed with the certified PE values, but imprecise, because

nearly half (44%) of the PE replicate results were not reported as the same interval. It should also be noted that

almost all of the imprecision occurred when the concentration of the sample was near one of the test kit’s

threshold values (i.e., 1, 10, or 50 ppm). The test kit had no fp and 4% of the soil sample results were fn. For

extract samples, the test kit had no fp or fn results.
49

Table 5-15. Performance summary for the PCB in Soil Tube Assay

Feature/parameter Performance summary

Blank results Soils: Correctly reported all 8 samples as [0,1) ppm

Extracts: Correctly reported all 8 samples as [0,1) ppm

Precision 

Percentage of combined sample sets where all four replicates were

reported as the same interval

PE soils: 56%

Environmental soils: 68%

Extracts: 75%

Accuracy

PE soils Extracts

agreed = 78% agreed = 92%

biased high = 10% biased high = 0%

biased low = 13% biased low = 8%

False positive results Blank soils: 0% (0 of 8 samples)

Blank extracts: 0% (0 of 8 samples)

False negative results PE and environmental soils: 4% (7 of 192 samples)

Spiked extracts: 0% (0 of 16 samples)

Comparison with reference laboratory agreed = 82%

results biased high = 12%

PE and environmental soils

biased low = 7%

Regulatory decision-making applicability agreed = 66%

PE and environmental soils

(40 to 60 ppm)

biased high = 32%

biased low = 2%

Sample throughput 7 samples/hour (chamber)

8 samples/hour (outdoors)

Power requirements Photometer with rechargeable battery

Operator requirements Basic knowledge of chemical techniques; 4 hours technology-specific

training

Cost Incremental: $18 per sample

Field lab: $1975 ($965 without photometer); $1250 photometer alone

Hazardous waste generation

40 lb of solid/liquid (classified as solid PCB waste suitable for disposal by

incineration)

40 lb of solid (used gloves, pipettes, paper towels, etc.)

20 lb of liquid waste (aqueous with trace methanol)
50
51

Section 6

Technology Update and Representative Applications

Objective

The purpose of this section is to allow the developer to provide information regarding new developments with

its technology since the demonstration activities. In addition, the developer has provided a list of representative

applications in which its technology has been or is currently being used.

Technology Update

At the time of the demonstration, the PCB in Soil Tube Assay was just beginning commercialization, so no

changes to the technology were anticipated by EnviroLogix in the near future.

Representative Applications

A typical application of the PCB in Soil Tube Assay would be at a Superfund site where EPA and the site

contractor were mapping the site for PCB contamination. The PCB immunoassay kit would be used to

determine where the samples should be taken and which samples should be sent off-site to the fixed analytical

laboratory for evaluation. In October 1998, EnviroLogix participated in such a study at a small Superfund

site in Kingston, New Hampshire. Other customers of the PCB immunoassay kit are the U.S. Army Corp of

Engineers, General Electric, Metcalf and Eddy, and the Roy F. Weston Corporation.

Data Quality Objective Example

This application of EnviroLogix’s PCB in Soil Tube Assay is based on data quality objective (DQO) methods

for project planning advocated by the American Society for Testing and Materials [9, 10] and EPA [11].

ORNL derived a DQO example from the performance results in Section 5. This example, which is presented

in Appendix E, illustrates the use of the performance data for the test kit from the ETV demonstration in the

DQO process to select the number of samples to characterize the FP and FN error rates for the decision rule.

53

Section 7

References

[1] Erickson, M. D. Analytical Chemistry of PCBs, 2nd ed., CRC Press/Lewis Publishers, Boca Raton,

Fla., 1997. 

[2] “Polychlorinated Biphenyls (PCBs) Manufacturing, Processing, Distribution in Commerce, and Use

Prohibitions,” Code of Federal Regulations, 40 CFR, pt. 761, rev. 7, December 1994.

[3] Maskarinec, M.P., et al. Stability of Volatile Organics in Environmental Soil Samples, ORNL/TM12128, Oak Ridge National Laboratory, Oak Ridge, Tenn., November 1992.

[4] U.S. Environmental Protection Agency. “Method 8081: Organochlorine Pesticides and PCBs as

Aroclors by Gas Chromatography: Capillary Column Technique,” in Test Methods for Evaluating

Solid Waste: Physical/Chemical Methods (SW-846), 3rd ed., Final Update II, Office of Solid Waste

and Emergency Response, Washington, D.C., September 1994.

[5] Oak Ridge National Laboratory. Technology Demonstration Plan: Evaluation of Polychlorinated

Biphenyl (PCB) Field Analytical Techniques, Chemical and Analytical Sciences Division, Oak

Ridge National Laboratory, Oak Ridge, Tenn., September 1998.

[6] U.S. Environmental Protection Agency. Data Quality Objectives for Remedial Response Activities,

EPA 540/G-87/003, EPA, Washington, D.C., March 1987.

[7] Draper, N. R., and H. Smith. Applied Regression Analysis, 2nd ed., John Wiley & Sons, New York,

1981.

[8] Berger, Walter, Harry McCarty, and Roy-Keith Smith. Environmental Laboratory Data Evaluation,

Genium Publishing Corp., Schenectady, N.Y., 1996.

[9] American Society for Testing and Materials (ASTM). Standard Practice for Generation of

Environmental Data Related to Waste Management Activities Quality Assurance and Quality

Control Planning and Implementation, D5283-92, 1997.

[10] American Society for Testing and Materials (ASTM), Standard Practice for Generation of

Environmental Data Related to Waste Management Activities Development of Data Quality

Objectives, D5792-95, 1997.

[11] U.S. Environmental Protection Agency. Guidance for Data Quality Assessment, EPA QA/G-9;

EPA/600/R-96/084, EPA, Washington, D.C., July 1996.
55

Appendix A

Description of Environmental Soil Samples

57

Table A-1. Summary of soil sample descriptions

Location Disposal Description

Request for

(RFD) # 

Drum #

Oak Ridge 40022 02 Soil from spill cleanup at the Y-12 Plant in Oak Ridge, Tennessee.

This soil is PCB-contaminated soil excavated in 1992.

Oak Ridge 40267 01 Soil from the Elza Gate area, a DOE Formerly Utilized Sites Remedial

02 Action Program site in Oak Ridge, Tennessee. This soil is PCB03 contaminated soil that was excavated in 1992.

04

Oak Ridge 24375 01 Catch-basin sediment from the K-711 area (old Powerhouse Area) at

02 the DOE East Tennessee Technology Park (formerly known as Oak

03 Ridge Gaseous Diffusion Plant) in Oak Ridge, Tennessee. This soil is

PCB-contaminated storm drain sediment that was excavated in 1991.

Oak Ridge 43275 01 Soil from the K-25 Building area at the DOE East Tennessee

02 Technology Park (formerly known as Oak Ridge Gaseous Diffusion

Plant) in Oak Ridge, Tennessee. This soil is PCB-contaminated soil

that was excavated in 1993.

Oak Ridge 134555 03 Soil from the K-707 area at the DOE East Tennessee Technology Park

(formerly known as Oak Ridge Gaseous Diffusion Plant) in Oak Ridge,

Tennessee. This soil is PCB-contaminated soil from a dike spillage that

was excavated in 1995.

Paducah 97002 01 Soil from the DOE Paducah Gaseous Diffusion Plant in Kentucky. This

02 soil is PCB-contaminated soil from a spill cleanup at the C-746-R

03 (Organic Waste Storage Area) that was excavated in 1989.

04

Portsmouth 7515 858 Soil from the DOE Portsmouth Gaseous Diffusion Plant in Ohio. This

1069 soil is PCB-contaminated soil from a probable PCB oil spill into the

1096 East Drainage Ditch that was excavated in 1986.

1898

2143

2528

3281

538

940

4096

Tennessee n/a n/a Captina silt loam from Roane County, Tennessee; used as a blank in

Reference Soil this study (i.e., not contaminated with PCBs)

59

Appendix B

Characterization of Environmental Soil Samples

61

Table B-1. Summary of environmental soil characterization

Location Carbon pH Sample RFD

ID Drum # a

Composition Total Organic

% gravel % sand % silt + clay (mg/kg)

Oak Ridge 101 40022-02 0 91.8 8.2 5384 7.12

102 40267-03 0.5 99.3 0.2 13170 7.30

103 40267-01 0.2 96.7 3.1 13503 7.21

104 40267-04 0.6 98.2 1.2 15723 7.07

105 40267-01S 0.5 94.8 4.7 14533 7.28 b

106 24375-03 0.5 87.8 11.7 19643 7.36

107 24375-01 2.5 92.5 5.0 1196 7.26

108 40267-02 0.4 94.2 5.4 9007 7.30

109 24375-02 0.3 93.1 6.6 1116 7.48

110 43275-01 0 89.2 10.8 14250 7.57

111 134555-03S 0.5 88.1 11.4 10422 7.41 b

112 43275-02 0.1 91.4 8.5 38907 7.66

126, 226 non-PCB soil 0 85.6 14.4 9249 7.33

Paducah 113, 201 97002-04 0 92.4 7.6 1296 7.71

114, 202 97002-01 0.2 87.6 12.2 6097 7.64

115, 203 97002-03 0.1 83.6 16.3 3649 7.59

116, 204 97002-02

117, 205 97002-02S b 0.4 93.7 5.8 4075 7.43

Portsmouth 206 7515-4096 0 87.1 12.9 3465 7.72

207 7515-1898 0.2 78.0 21.8 3721 7.66

208 7515-1096 0.4 74.4 25.2 3856 7.77

209 7515-2143 0 74.3 25.7 10687 7.71

210 7515-0940 0.3 73.0 26.7 7345 7.78

216 7515-0538 0.5 73.3 26.3 1328 7.78

211 7515-0538S 

217 7515-0538S 

b

b

212 7515-2528 0.5 70.4 29.1 5231 7.92

213 7515-3281 0.5 72.6 26.8 5862 7.67

214 7515-0858 0 65.8 34.2 6776 7.85

215 7515-1069 1.3 75.0 23.7 4875 7.56

 Request for disposal drum number (see Table A-1). a

 “S” indicates that the environmental soil was spiked with additional PCBs. b

63

Appendix C

Temperature and Relative Humidity Conditions
64

Table C-1. Average temperature and relative humidity conditions during testing periods

Date

Outdoor site Chamber site

Average Average Average Average

temperature relative humidity temperature relative humidity

(EF) (%) (EF) (%)

9/21/98 a a 57 46

9/22/98 a a 57 46

9/23/98 82 43 56 52

9/24/98 78 56 a a

9/25/98 74 59 a a

 The developer was working at the other site on this day. a
0

10

20

30

40

50

60

70

80

90

100

9/23/98 9/24/98 9/25/98

Temperature (deg. F)

Avg Temp

High Temp

Low Temp

0

10

20

30

40

50

60

70

80

90

100

9/23/98 9/24/98 9/25/98

Relative Humidity (%)

Avg RH

High RH

Low RH

65

Figure C-1. Summary of temperature conditions for outdoor site.

Figure C-2. Summary of relative humidity conditions for outdoor site.
0

10

20

30

40

50

60

70

80

90

9/21/98 9/22/98 9/23/98

Temperature (deg. F)

Avg Temp

High Temp

Low Temp

0

10

20

30

40

50

60

70

80

90

100

9/21/98 9/22/98 9/23/98

Relative Humidity (%)

Avg RH

High RH

Low RH

66

Figure C-3. Summary of temperature conditions for chamber site.

Figure C-4. Summary of relative humidity conditions for chamber site.
Appendix D

PCB in Soil Tube Assay

PCB Technology Demonstration Sample Data
68

Legend for Appendix D Tables

Table Heading Definition

Obs Observation

Sample ID Sample identification

101 to 126 = outdoor site soil samples

127 to 130 = outdoor site extract samples

201 to 226 = chamber site soil samples

227 to 230 = chamber site extract samples

Rep Replicate of sample ID (1 through 4)

EnviroLogix Result PCB in Soil Tube Assay’s measured PCB concentration (ppm)

Ref Lab Result LAS reference laboratory measured PCB concentration (ppm)

Values with “#” are samples that the reference laboratory

reported as “# reporting detection limit”

Reference Aroclor Aroclor(s) identified by the reference laboratory

Type Sample = environmental soil

1016, 1248, 1254, 1260 = Aroclor in PE soil samples or

extract spiking solutions

Blank = non-PCB-contaminated sample

Spike Nominal spike concentrations (μg/mL) of extract solutions

prepared by ORNL

Order Order of sample analysis by EnviroLogix (started with

2001–2116, then 1001–1116)
69

Table D-1. PCB in Soil Tube Assay technology demonstration soil sample data

 Sample EnviroLogix Ref Lab Reference

Obs ID Rep Result Result Aroclor Type Order

 (ppm) (ppm)

 1 101 1 [0,1) 0.6 1254 Sample 1048

 2 101 2 [0,1) 0.4 1254 Sample 1085

 3 101 3 [0,1) 0.5 1254 Sample 1018

 4 101 4 [0,1) 0.5 1254 Sample 1043

 5 102 1 [1,10) 2.2 1254 Sample 1070

 6 102 2 [1,10) 2.1 1254 Sample 1033

 7 102 3 [1,10) 1.7 1260 Sample 1067

 8 102 4 [1,10) 2.5 1260 Sample 1042

 9 103 1 [1,10) 3.0 1254 Sample 1104

 10 103 2 [1,10) 2.4 1254 Sample 1022

 11 103 3 [1,10) 2.0 1260 Sample 1034

 12 103 4 [1,10) 1.6 1260 Sample 1031

 13 104 1 [10,50) 6.8 1260 Sample 1076

 14 104 2 [10,50) 6.0 1254 Sample 1092

 15 104 3 [1,10) 14.8 1254 Sample 1019

 16 104 4 [10,50) 9.9 1254 Sample 1053

 17 105 1 [50,4) 49.7 1260 Sample 1086

 18 105 2 [50,4) 84.1 1260 Sample 1082

 19 105 3 [50,4) 50.6 1260 Sample 1098

 20 105 4 [50,4) 53.2 1260 Sample 1060

 21 106 1 [50,4) 269.6 1254 Sample 1007 

 22 106 2 [50,4) 255.9 1254 Sample 1061

 23 106 3 [50,4) 317.6 1254 Sample 1071

 24 106 4 [50,4) 649.6 1254 Sample 1017

 25 107 1 [0,1) 1.0 1254 Sample 1062

 26 107 2 [1,10) 1.6 1254 Sample 1078

 27 107 3 [0,1) 1.2 1254 Sample 1021

 28 107 4 [1,10) 1.2 1254 Sample 1102

 29 108 1 [1,10) 1.7 1254 Sample 1032

 30 108 2 [1,10) 2.0 1254 Sample 1103

 31 108 3 [1,10) 1.7 1254 Sample 1072

 32 108 4 [1,10) 1.9 1254 Sample 1080

 33 109 1 [1,10) 1.5 1254 Sample 1016

 34 109 2 [1,10) 2.1 1254 Sample 1058

 35 109 3 [1,10) 1.8 1254 Sample 1056

 36 109 4 [1,10) 2.4 1254 Sample 1083

 37 110 1 [10,50) #490.0 Non-Detect Sample 1054

 38 110 2 [10,50) #99.0 Non-Detect Sample 1009

 39 110 3 [10,50) #66.0 Non-Detect Sample 1039

 40 110 4 [10,50) #98.0 Non-Detect Sample 1026

 41 111 1 [50,4) 44.5 1254 Sample 1020

 42 111 2 [10,50) 36.0 1254 Sample 1025

 43 111 3 [50,4) 39.3 1254 Sample 1059

 44 111 4 [10,50) 35.1 1254 Sample 1050
70

 Sample EnviroLogix Ref Lab Reference

Obs ID Rep Result Result Aroclor Type Order

 (ppm) (ppm)

 45 112 1 [50,4) #66.0 Non-Detect Sample 1073

 46 112 2 [50,4) #200.0 Non-Detect Sample 1088

 47 112 3 [50,4) #130.0 Non-Detect Sample 1064

 48 112 4 [50,4) #200.0 Non-Detect Sample 1081

 49 113 1 [1,10) 0.7 1260 Sample 1066

 50 113 2 [1,10) 1.1 1260 Sample 1052

 51 113 3 [1,10) 0.6 1260 Sample 1044

 52 113 4 [1,10) 1.9 1248/1260 Sample 1075

 53 114 1 [1,10) 1.1 1260 Sample 1093

 54 114 2 [1,10) 1.2 1260 Sample 1100

 55 114 3 [1,10) 1.3 1260 Sample 1012

 56 114 4 [0,1) 1.7 1260 Sample 1023

 57 115 1 [10,50) 14.9 1248 Sample 1084

 58 115 2 [10,50) 12.4 1016 Sample 1028

 59 115 3 [10,50) 15.0 1248 Sample 1001

 60 115 4 [10,50) 16.9 1248 Sample 1038

 61 116 1 [10,50) 41.4 1248 Sample 1015

 62 116 2 [10,50) 41.2 1016 Sample 1077

 63 116 3 [10,50) 48.5 1248 Sample 1011

 64 116 4 [50,4) 34.0 1016 Sample 1003

 65 117 1 [50,4) 431.6 1016 Sample 1094

 66 117 2 [50,4) 406.3 1016 Sample 1014

 67 117 3 [50,4) 304.7 1016 Sample 1040

 68 117 4 [50,4) 392.8 1016 Sample 1002

 69 118 1 [0,1) 2.1 1248 1248 1037

 70 118 2 [1,10) 1.9 1016 1248 1036

 71 118 3 [0,1) 0.7 1248 1248 1069

 72 118 4 [0,1) 1.6 1248 1248 1027

 73 119 1 [1,10) 21.2 1016 1248 1049

 74 119 2 [10,50) 17.2 1248 1248 1024

 75 119 3 [10,50) 17.4 1248 1248 1005

 76 119 4 [10,50) 24.4 1248 1248 1090

 77 120 1 [1,10) 4.5 1254 1254 1057

 78 120 2 [1,10) 4.0 1254 1254 1099

 79 120 3 [1,10) 6.3 1254 1254 1091

 80 120 4 [1,10) 5.0 1254 1254 1045

 81 121 1 [50,4) 58.7 1254 1254 1087

 82 121 2 [50,4) 55.7 1254 1254 1101

 83 121 3 [50,4) 53.2 1254 1254 1063

 84 121 4 [50,4) 50.9 1254 1254 1047

 85 122 1 [10,50) 12.2 1260 1260 1013

 86 122 2 [50,4) 10.9 1260 1260 1089

 87 122 3 [10,50) 11.3 1260 1260 1041

 88 122 4 [10,50) 10.0 1260 1260 1095
71

 Sample EnviroLogix Ref Lab Reference

Obs ID Rep Result Result Aroclor Type Order

 (ppm) (ppm)

 89 123 1 [50,4) 59.2 1260 1260 1004

 90 123 2 [50,4) 56.9 1260 1260 1079

 91 123 3 [50,4) 66.8 1260 1260 1008

 92 123 4 [50,4) 57.5 1260 1260 1006

 93 124 1 [1,10) 1.8 1254 1254/1260 1055

 94 124 2 [1,10) 1.4 1260 1254/1260 1030

 95 124 3 [1,10) 1.9 1254 1254/1260 1096

 96 124 4 [1,10) 1.8 1254 1254/1260 1065

 97 125 1 [50,4) 32.0 1254 1254/1260 1097

 98 125 2 [50,4) 41.3 1254 1254/1260 1051

 99 125 3 [50,4) 46.0 1254 1254/1260 1029

100 125 4 [50,4) 32.2 1260 1254/1260 1046

101 126 1 [0,1) #0.1 Non-Detect Blank 1035

102 126 2 [0,1) #0.1 Non-Detect Blank 1010

103 126 3 [0,1) #0.2 Non-Detect Blank 1074

104 126 4 [0,1) #1.3 Non-Detect Blank 1068

105 201 1 [1,10) 1.0 1016/1260 Sample 2031

106 201 2 [1,10) 1.0 1016/1260 Sample 2035

107 201 3 [1,10) 1.1 1016/1260 Sample 2089

108 201 4 [1,10) 0.6 1260 Sample 2034

109 202 1 [1,10) 1.4 1260 Sample 2104

110 202 2 [1,10) 1.6 1260 Sample 2027

111 202 3 [1,10) 1.2 1260 Sample 2011

112 202 4 [0,1) 1.5 1260 Sample 2061

113 203 1 [10,50) 14.0 1248 Sample 2015

114 203 2 [10,50) 12.8 1248 Sample 2068

115 203 3 [0,1) 16.2 1248 Sample 2010

116 203 4 [10,50) 12.4 1248 Sample 2064

117 204 1 [10,50) 43.1 1248 Sample 2022

118 204 2 [10,50) 45.3 1248 Sample 2050

119 204 3 [50,4) 41.0 1248 Sample 2102

120 204 4 [10,50) 47.7 1248 Sample 2095

121 205 1 [50,4) 3305.0 1016/1260 Sample 2076

122 205 2 [50,4) 538.7 1016 Sample 2065

123 205 3 [50,4) 457.0 1016 Sample 2075

124 205 4 [50,4) 483.3 1016 Sample 2016

125 206 1 [1,10) 2.9 1260 Sample 2001

126 206 2 [1,10) 1.1 1260 Sample 2014

127 206 3 [1,10) 1.1 1016/1260 Sample 2086

128 206 4 [1,10) 2.5 1260 Sample 2090

129 207 1 [10,50) 17.8 1260 Sample 2058

130 207 2 [10,50) 14.3 1260 Sample 2047

131 207 3 [10,50) 21.6 1260 Sample 2002

132 207 4 [10,50) 21.6 1254 Sample 2094
72

 Sample EnviroLogix Ref Lab Reference

Obs ID Rep Result Result Aroclor Type Order

 (ppm) (ppm)

133 208 1 [10,50) 42.0 1260 Sample 2004

134 208 2 [10,50) 27.7 1016/1260 Sample 2018

135 208 3 [50,4) 24.0 1254 Sample 2101

136 208 4 [10,50) 28.4 1260 Sample 2062

137 209 1 [50,4) 32.7 1260 Sample 2063

138 209 2 [50,4) 79.3 1260 Sample 2059

139 209 3 [50,4) 11.0 1260 Sample 2078

140 209 4 [50,4) 37.9 1260 Sample 2005

141 210 1 [50,4) 123.2 1260 Sample 2049

142 210 2 [50,4) 61.5 1260 Sample 2033

143 210 3 [50,4) 84.1 1260 Sample 2081

144 210 4 [50,4) 85.5 1260 Sample 2096

145 211 1 [50,4) 387.8 1254 Sample 2083

146 211 2 [50,4) 581.4 1254 Sample 2025

147 211 3 [50,4) 330.0 1254 Sample 2009

148 211 4 [50,4) 318.7 1254 Sample 2013

149 212 1 [1,10) 3.8 1260 Sample 2053

150 212 2 [1,10) 3.9 1260 Sample 2017

151 212 3 [1,10) 4.3 1260 Sample 2060

152 212 4 [1,10) 0.8 1260 Sample 2030

153 213 1 [1,10) 6.9 1260 Sample 2045

154 213 2 [10,50) 7.3 1260 Sample 2079

155 213 3 [1,10) 7.8 1260 Sample 2056

156 213 4 [10,50) 10.5 1260 Sample 2003

157 214 1 [10,50) 26.0 1260 Sample 2057

158 214 2 [10,50) 25.6 1260 Sample 2077

159 214 3 [10,50) 29.1 1260 Sample 2024

160 214 4 [10,50) 20.2 1260 Sample 2019

161 215 1 [10,50) 25.1 1260 Sample 2020

162 215 2 [10,50) 24.1 1260 Sample 2007

163 215 3 [10,50) 26.2 1260 Sample 2023

164 215 4 [10,50) 31.2 1016/1260 Sample 2038

165 216 1 [10,50) 151.6 1260 Sample 2088

166 216 2 [10,50) 47.0 1260 Sample 2042

167 216 3 [50,4) 54.3 1260 Sample 2026

168 216 4 [50,4) 64.0 1260 Sample 2052

169 217 1 [50,4) 886.7 1254 Sample 2048

170 217 2 [50,4) 549.8 1254 Sample 2046

171 217 3 [50,4) 542.8 1254 Sample 2099

172 217 4 [50,4) 1913.3 1016/1260 Sample 2039

173 218 1 [1,10) 2.8 1248 1248 2029

174 218 2 [1,10) 2.4 1248 1248 2036

175 218 3 [1,10) 2.6 1248 1248 2071

176 218 4 [1,10) 2.6 1248 1248 2012
73

 Sample EnviroLogix Ref Lab Reference

Obs ID Rep Result Result Aroclor Type Order

 (ppm) (ppm)

177 219 1 [10,50) 22.4 1248 1248 2044

178 219 2 [10,50) 26.0 1016 1248 2037

179 219 3 [10,50) 29.4 1248 1248 2069

180 219 4 [10,50) 15.2 1248 1248 2097

181 220 1 [1,10) 8.5 1254 1254 2006

182 220 2 [1,10) 4.9 1254 1254 2054

183 220 3 [1,10) 4.7 1254 1254 2043

184 220 4 [1,10) 5.2 1254 1254 2021

185 221 1 [10,50) 32.0 1016/1260 1254 2087

186 221 2 [10,50) 44.1 1016/1260 1254 2070

187 221 3 [50,4) 43.8 1254 1254 2073

188 221 4 [50,4) 59.6 1254 1254 2092

189 222 1 [10,50) 13.2 1260 1260 2028

190 222 2 [10,50) 12.4 1260 1260 2032

191 222 3 [1,10) 12.7 1260 1260 2008

192 222 4 [1,10) 12.7 1260 1260 2091

193 223 1 [50,4) 56.6 1260 1260 2103

194 223 2 [10,50) 50.3 1260 1260 2072

195 223 3 [50,4) 49.9 1260 1260 2080

196 223 4 [50,4) 66.4 1260 1260 2084

197 224 1 [1,10) 2.2 1254 1254/1260 2082

198 224 2 [1,10) 1.2 1260 1254/1260 2066

199 224 3 [1,10) 1.4 1260 1254/1260 2067

200 224 4 [1,10) 2.1 1254 1254/1260 2055

201 225 1 [50,4) 56.4 1260 1254/1260 2040

202 225 2 [10,50) 36.5 1016/1260 1254/1260 2085

203 225 3 [10,50) 32.1 1260 1254/1260 2041

204 225 4 [50,4) 146.0 1254 1254/1260 2100

205 226 1 [0,1) #0.1 Non-Detect Blank 2093

206 226 2 [0,1) #0.8 Non-Detect Blank 2074

207 226 3 [0,1) #0.1 Non-Detect Blank 2098

208 226 4 [0,1) #0.1 Non-Detect Blank 2051
74

Table D-2. PCB in Soil Tube Assay technology demonstration extract sample data

 Sample EnviroLogix 

Obs ID Rep Result Spike Type Order a

 (ppm) (μg/mL)

 1 130 1 [4,20) 10 1248 1108

 2 130 2 [4,20) 10 1248 1116

 3 130 3 [4,20) 10 1248 1114

 4 130 4 [4,20) 10 1248 1115

 5 131 1 [4,20) 100 1016 1111

 6 131 2 [4,20) 100 1016 1110

 7 131 3 [20,4) 100 1016 1109

 8 131 4 [20,4) 100 1016 1107

 9 132 1 [0,0.4) 0 Blank 1106

 10 132 2 [0,0.4) 0 Blank 1105

 11 132 3 [0,0.4) 0 Blank 1112

 12 132 4 [0,0.4) 0 Blank 1113

 13 230 1 [4,20) 10 1248 2110

 14 230 2 [4,20) 10 1248 2115

 15 230 3 [4,20) 10 1248 2107

 16 230 4 [4,20) 10 1248 2109

 17 231 1 [20,4) 100 1016 2105

 18 231 2 [20,4) 100 1016 2114

 19 231 3 [20,4) 100 1016 2116

 20 231 4 [20,4) 100 1016 2111

 21 232 1 [0,0.4) 0 Blank 2106

 22 232 2 [0,0.4) 0 Blank 2112

 23 232 3 [0,0.4) 0 Blank 2108

 24 232 4 [0,0.4) 0 Blank 2113

 Nominal spike concentration of the extract sample prepared by ORNL. a
75

Table D-3. Corrected reference laboratory data

Error Sample ID Reported Result Corrected Result

(ppm) (ppm)

Transcription 106 #490 255.9

130 5.6 10.3

205 32,000 3,305.0

207 180 17.8

210 160 123.2

Calculation 118 3.6 2.1

119 4.3 17.4

209 2.3 37.9

214 43.0 26.0

219 29.0 22.4

Interpretation 101 #0.7 0.5 a

101 #0.7 0.6 a

107 #1.3 1.2

109 18.0 1.5

113 #0.9 0.6 b

113 #1.0 0.7 b

119 18.0 21.2

127 7.2 10.9

201 # 1.0 0.6

219 21.0 26.0

 Two of four measurements in sample ID 101 were corrected. a

 Two of four measurements in sample ID 113 were corrected. b

77

Appendix E

Data Quality Objective Example

 1. U.S. Environmental Protection Agency, Guidance for Data Quality Assessment, EPA QA/G-9; EPA/600/R-96/084, EPA,

Washington, D.C., July 1996. 

79

General Decision Rule

If all of the PCB sample results show concentrations < [50, 4), then process the soil drum by RCRA

methods.

If any of the PCB sample results are in the intervals [50, 4) then process the soil drum by TSCA

methods.

Disclaimer

The following hypothetical example serves to demonstrate how the information provided in this report may be

used in the data quality objectives (DQO) process. This example serves to illustrate the application of

quantitative DQOs to a decision process, but it cannot attempt to provide a thorough education in this topic.

Please refer to other educational or technical resources for further details. In addition, since the focus of this

report is on the analytical technology, this example makes the simplifying assumption that the contents of these

drums is homogeneous. In the real world, this assumption is seldom valid, and matrix heterogeneity constitutes

a source of considerable uncertainty that must be adequately evaluated if the overall certainty of a site decision

is to be quantified. 

Background and Problem Statement

An industrial company discovered a land area contaminated with PCBs from an unknown source. The

contaminated soil was excavated into waste drums. The drums are to be treated as Resources Conservation and

Recovery Act (RCRA) waste if the PCB concentration of their contents is <50 ppm and as Toxic Substances

Control Act (TSCA) waste if their PCB concentration is $50 ppm. The company’s DQO team was considering

the use of EnviroLogix’s PCB in Soil Tube Assay kit to measure the PCB concentration in each drum. The

plan was to randomly collect soil samples from each drum and test them with the kit to determine if the

measured concentrations fell within one of four intervals: [0, 1), [1, 10), [10, 50), or [50, 4). (Recall that this

notation describes the concentration ranges 0 ppm # PCB < 1 ppm, 1 ppm # PCB < 10 ppm, 10 ppm # PCB

< 50 ppm and PCB $ 50 ppm, as used in Section 5.) The DQO team decided that a drum would be processed

as TSCA waste if any of the test kit results indicated a concentration in the intervals [50, 4); otherwise, the

drum would be processed as RCRA waste. In agreement with the regulator, the DQO team determined that a

decision rule for processing the waste would be based on the number of samples with PCB concentrations in

the intervals [50, 4).

DQO Goals

Section 1.2 of EPA’s Guidance for Data Quality Assessment states: “The true condition that occurs with the

more severe decision error . . . should be defined as the null hypothesis.” The DQO team decided that the more 1

severe decision error would be for a drum to be erroneously processed as RCRA waste if the drum’s PCB

concentration actually exceeded the 50 ppm limit. Therefore, the null hypothesis is constructed to assume that

a drum’s true PCB concentration exceeds the 50 ppm limit; as a “hot” drum, it would be processed as TSCA
80

Permissible FP and FN Error Rates and Critical Decision Point

FP: Pr[Drum is RCRA waste] # 0.05 when true PCB concentration $ 50 ppm

FN: Pr[Drum is TSCA waste] # 0.10 when true PCB concentration < 50 ppm

waste. Drums would be processed as RCRA waste only if the null hypothesis is rejected and it is concluded

that the “true” average PCB concentration is less than 50 ppm.

With the null hypothesis defined in this way, a false positive decision is made when it is concluded that a drum

contains <50 ppm PCBs (i.e., the null hypothesis is rejected), when actually the drum is hot (i.e., the null

hypothesis is true). The team required that the error rate for processing a hot drum as RCRA waste (i.e., FP

= the false positive error rate for the decision) should be 5% or less. This error rate is expressed either as a

percentage or as a probability. Therefore, a sufficient number of samples must be taken from each drum so that

the false positive decision error rate (FP) is 0.05 (or less) if the true drum concentration is $0 ppm. This

scenario represents a maximum risk of 5% for processing a drum containing 50 ppm or more of PCBs as

RCRA waste.

The DQO team did not want to process an excessive number of drums as TSCA waste if the average PCB

concentration was <50 ppm because of the expense. In this situation, a false negative decision is made when

it is concluded that a drum is hot (i.e., the null hypothesis is not rejected), when in actuality, the drum contains

soil with <50 ppm PCBs (i.e., the null hypothesis is actually false). After considering the guidelines presented

in Section 1.1 of EPA’s Guidance for Data Quality Assessment, the DQO team recommended that the false

negative decision error rate (FN) be 0.10 if the true drum concentration was <50 ppm. That is, there would be

a 10% chance of processing a drum as TSCA waste (e.g., FN = Pr[Falsely Processing a Drum as TSCA

waste]) if the true PCB concentration for a drum was <50 ppm. 

Use of Technology Performance Information to Implement the Decision Rule

Technology performance information is used to evaluate whether a particular analytical technology can produce

data of sufficient quality to support the site decision. Because the DQO team is considering the use of the

EnviroLogix PCB kit, the performance of this technology [as reported in this Environmental Technology

Verification (ETV) report] was used to assess its applicability to this project. The question arises: How many

samples are needed from a single drum to permit a statistically valid decision at the specified certainty? Recall

that the simplifying assumption was made that the PCB distribution throughout the soil within a single drum

is homogeneous, and thus, matrix heterogeneity will not contribute to overall variability. The only variability

to be considered in this example, therefore, is the variability in performance of the EnviroLogix test kit’s

analytical method, which is determined by precision and accuracy studies.

Determining the Number of Samples

The number of samples needed to satisfy the FP and FN requirements depends on the misclassification error

rates of the PCB test kit. Two types of misclassifications have to be considered:
FP ' Pr[All EnviroLogix results < 50 ppm for PCB $ 50 ppm] ' ( PU

)

n

.

 Lothar Sachs, Applied Statistics: A Handbook of Techniques, 2nd ed., Springer-Verlag, New York, 1984. 2

81

(E-1)

1. underestimating the PCB concentration—i.e., classifying a sample concentration to be <50 ppm when the

true PCB concentration is $50 ppm 

2. overestimating the PCB concentration—i.e., classifying a sample concentration to be $50 ppm when the

PCB concentration is <50 ppm.

The DQO team compared the experimental conditions for the EnviroLogix ETV demonstration with their

expected project conditions for variables such as soil type and ambient conditions. The team determined that

the relevant variables would be sufficiently similar so that misclassification rates determined from the ETV

demonstration would be adequately predictive of rates for their project. The DQO team then used the ETV data

to prepare Table E-1 to assess the misclassification rates around the 50 ppm action level using all performance

evaluation (PE) and environmental soil samples. Table E-1 summarizes a sample-by-sample comparison of

the reference lab results with the results generated by the EnviroLogix kit (see Appendix D).

Table E-1. Comparison of PCB in Soil Tube Assay results with the reference laboratory at 50 ppm level

Reference laboratory PCB in Soil Tube Assay results Number of samples

results (PE + environmental soils)

[0, 1) or [1, 10) or [10, 50) [50, 4)

Greater or equal to 50 ppm 2 43 45

Less than 50 ppm 139 16 155

Table E-1 can be used to estimate the two types of misclassifications as

PU = Pr [Underestimating the PCB concentration] = 2/45 = 0.044 when reference values $ 50 ppm,

PO = Pr [Overestimating the PCB concentration] = 16/155 = 0.103 when reference values < 50 ppm.

The probability distribution of classifying the number of soil samples in different concentration intervals

follows a binomial probability distribution. This probability distribution and the requirements for FP and FN 2

can be used to determine the number of samples to meet the DQO goals. The FP for the decision rule is related

to PU by 

The FP error rate decreases as the sample size increases. The sample size is solved as
n '

Log( FP )

Log( PU)

.

n '

Log(0.05)

Log(0.044)

'

&1.301

&1.357

' 0.96 1 .

FN ' Pr[Some of EnviroLogix results $ 50 ppm for PCB < 50 ppm] ' 1 & ( 1 & PO)

n

.

n '

Log( 1 & FN )

Log( 1 & PO)

,

n '

Log( 1 & 0.10 )

Log( 1 & 0.103 )

'

&0.046

&0.047

' 0.98 1 .

82

(E-2)

(E-3)

(E-4)

where

n = number of samples from a drum to be measured

FP = false positive decision error rate (e.g., FP = 0.05)

PU = probability of underestimating the PCB concentration

The sample size was rounded up to the next integer, an operation that will decrease the FP for the decision rule.

The DQO team would have to analyze only one sample from each drum to meet the decision rule’s FP

requirement. The FN for the decision rule is related to PO by

The error rate of a false negative decision actually increases with increasing sample size because the chance

that the kit will overestimate a concentration increases with continued testing. The sample size required to meet

the FN requirement is

where

n = number of samples from a drum to be measured

FN = false negative decision error rate (e.g., FN = 0.10)

PO = probability of overestimating a PCB concentration
83

Decision Rule for 5% FP and 10% FN

If one randomly selected soil sample has a PCB test result reported in an interval less than [50, 4), then

process the soil drum as RCRA waste.

If one randomly selected soil sample has a PCB test result in the interval [50, 4), then process the soil

drum as TSCA waste.

Decision Rule for FP = 0.1% and FN = 28%

If all three randomly selected soil samples have PCB test results reported in intervals less than 50 ppm,

then process the soil as RCRA waste.

If any of the three randomly selected soil samples have a PCB test result in the interval [50, 4), then

process the soil drum TSCA waste.

The sample size must be rounded up to n = 1 (fractions of a sample analysis are not possible). When n = 1,

the value of FN = 10.3% which is only slightly higher than the DQO team’s goal of 10% FN. This situation

occurs because the 10.3% overestimation error rate of the kit is nearly equal to 10%. If additional samples were

taken, FN would increase (e.g., for n = 2, FN = 19.5%) and might not meet the DQO team’s goal. The only

way to reduce the FN in this scenario is to use an analytical technology with a lower overestimation error rate.

The DQO team in this example decided that the sampling procedure would be to randomly select one soil

sample from each drum and test the sample with the EnviroLogix’s PCB in Soil Tube Assay kit. (Recall that

for the purposes of this example, the soil in the drum has been assumed to be homogeneous.) The DQO team

would process the drum as RCRA waste if the EnviroLogix result was less than 50 ppm, and process the drum

as TSCA waste if the EnviroLogix result was greater than 50 ppm. The DQO team’s goals of a 5% FP and

a 10% FN would be closely met by this sampling plan.

Alternative FP Parameter

The following statement describes how changing the FP requirement from 5% to 0.1% would affect the decision

rule. Using FP = 0.001, the calculated sample sizes would be n = 2.2, which is rounded up to 3. The FN would

be 28%. The higher FN occurs because any of the three samples have a 10.3% chance of being overestimated,

and if only one is overestimated, the drum is processed as TSCA waste. The decision rule for the lower FP

requirement would be as shown.