ORNL/CP-96484

CON F- go/ 3 1 - - Field Technology Evaluations in EPA's Environmental Technology Verification (ETV) Programt

Amy Dindal', Charles Bayne', Roger Jenkins', David Carden3, David Bottrel14, and Stephen Billets'

Lockheed Martin Energy Research Corporation Oak Ridge National Laboratory ' Chemical and Analytical Sciences Division

Computer Science and Mathematics Division P.O. Box 2008

Oak Ridge, Tennessee 3783 16120

' U. S. Department of Energy Oak Ridge Operations Office

Three Main Street Oak Ridge, Tennessee 37830

' U. S. Department of Energy 19901 Germantown Road

Cloverleaf Buildinn Germantown, MD 20874

5 U. S. Environmental Protection Agency National Exposure Research Laboratory

P.O. Box 93478 1 9 9 8 0 4 0 6 1 4 0

Las Vegas, Nevada 89 193-3478

Environmental Technology Verification (ETV) Program Overview

The performance evaluation of innovative environmend technologies is an integral part ofthe U.S.

Environmental Protection Agency's (EPA) mission. 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 by providing independent and credible assessments of environmental technologies.

The ETV Program is intended to assist and inform those involved in the design, distribution, permitting,

t R e n d qorrrond by the ~ n v i ~ e n t d h t e c l i o n Agency, Nationd Eaporun R e m m h Laboratoty, Los Vegw, Nevada, under intcmgrng a@eement1824JO93CI and the E & ~ t d M a n o g e m . n t Pmgnrm, U. S. Deporment afEnrrrgy under conrroct DE-ACO5-WR224M with Ook Ridge N o t b n d h b z r O t ~ , manoged by h h e e d Mwtin Energy Reaemh Corporation.

lite 5ubmitd manwnipt has bem a u t h ~ d

contract No. DE-ACOSWRZ24rj4. ACUXdmdy. the U. S. Govemmrnt retains a

nonexclusive. r0ydty-h license to publish or reproduce the pubkhed form of thL conmbubon. or dow others to do so.

by a eontract of the u. s. Govmunmt unda

for u. s. Govmmt PurpoJes.

DISCLAIMER

This report was prepared as an account of work sponsored by an agency of the United States Government. Neither the United States Government nor any agency thereof, nor any of their employees, makes any warranty, express or implied, or assumes any legal liability or responsibility for the accuracy, completeness, or use- fulness of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Reference herein to any spe- cific commercial product, process, or service by trade name, trademark, manufac- turer, or otherwise does not necessarily constitute or imply its endorsement, recom- mendation, or favoring by the United States Government or any agency thereof. The views and opinions of authors expressed herein do not necessarily state or reflect those of the United States Government or any agency thereof.

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Innovative technologies are evaluated independently against conventional technologies. The field

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

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 environmental technology

verification report (ETVR).

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 OEce of Solid Waste and Emergency Response’s Technology

Innovation Office (http://cIii-in. corn).

Oak Ridge National Laboratory (ORNL) is one of the verification organizations in ETV’s Site

Characterization and Monitoring Technology pilot. The goal of this pilot, also known as the Consortium

for Site Characterization Technology (CSCT), is to facilitate the acceptance and use of site

characterization and monitoring technologies. This manuscript will overview ORNL’s verification

activities, including evaluations of polychlorinated biphenyl (PCB) field analytical techniques, decision

support software (DSS), and field extraction technologies. Specific information on ORNL’s ETV activities

can be found on the program’s web site (http://www. ornl. gov/divisions/cas~~~n~ns/ornl-eh.l. htm).

PCB Field Analytical Technology Demonstration

A July 1997 demonstration at ORNL evaluated field analytical technologies capable of detecting

and quantifying polychlorinated biphenyls (PCBs). The purpose of this demonstration was to provide

rigorous, statistically defensible testing of field monitoring equipment for PCBs under actual field

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conditions. A hdamental objective of this demonstration was to evaluate how well the technologies can

assist in regulatory decision-making processes for PCB-contaminated waste.

Participant Selection

Potential developers were invited to attend a Developers Conference on February 19, 1997, in Atlanta, GA

(hosted by EPA Region 4). The purpose of this informational meeting was to bring together candidate

participants and demonstration organizers for an exchange of information. Based on the detailed technology

descriptions presented by the developers at the conference, a group of developers were selected as the best

candidates for participation in the demonstration. Final selection and qualification for the demonstration

was based on successful analyses of a series of pre-demonstration samples that were representative of the

ones analyzed in the actual demonstration. The technology developers who participated in the PCB

demonstration were: Dexsil Corporation (Hamden, CT), Hach Corporation (Loveland, CO), Strategic

Diagnostics, Inc. (Newark, DE), and Electronic Sensor Technology (Newbury Park, CA). Sentex Systems,

Inc. was selected to participate, but was unable to complete the study because of instrumental difficulties.

An overview of the developers and their technologies follows.

Dexsil Corporation: The L2000 PCB analyzer is a field portable ion specific electrode instrument

designed to quantify PCB concentration in soils, dielectric fluids, and surface wipes. PCBs in soil can be

quantified over a range of 2 ppm to 2000 ppm with the abiIity to extend the range over 2000 ppm by

reducing the sample size. Total time for analysis of soil is 10 minutes, dielectric fluid is 5 minutes and

surface wipes is 12 minutes. Cost for analysis of soil is $8.00 to $lO.OO/sample, dielectric fluid is $3.75 to

$5.00/sampIe and $12.00 to $16.00/sample for surface wipes. Sample preparation consists of extraction

and dehalogenation of the PCBs. The resulting chloride ions are then isolated in an aqueous buffered

solution for analysis by the L2000 Analyzer.

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Hach Corporation: Using Hach’s immunoassay test kit for PCBs, samples, standards and reagents are

added to test tubes coated with an antibody specific for PCBs. The concentration of PCBs in a sample is

determined by comparing the developed color intensity to that of a PCB standard. The PCB concentration

is inversely proportional to the color development; the lighter the color, the higher the PCB concentration,

This method is a semiquantitative screening method which indicates whether the PCB concentration is

above or below 1 ppm and/or 10 ppm threshold values.

Strategic Diagnostics, Inc. (SDI): This company was formed by the 1996 mergers of Strategic

Eiagnostics, EnSys, and Ohmicron Environmental Diagnosiics, all producers of immunoassay kits for

environmental analyses. SDI demonstrated three different field testing formats of immunoassay test kits for

PCBs. While the core technology for these products is the same, each utilizes a distinct format, provides

differing result types, and is best suited to different field testing applications. The D TECH latex particle

format provides very rapid (< 20 min) field testing capability with semiquantitative screening results. The

D TECH test is ideal for rapid testing applications where a rough and fast yes/no answer is required, and

where project resources do not permit training. The EnviroGard coated tube technology provides rapid

semiquantitative field analysis with a higher level of analytical precision. The EnviroGard calibrators are

set up to represent common project action levels. The Ohmicron M I D Assay magnetic particle format

represents the highest level of analytical precision. The RaPID Assay format can be used to generate semi-

quantitative or quantitative results. It is ideal in high volume testing applications.

Electronic Sensor Technology: Surface Acoustic Wave/Gas Chromatography (SAW/GC) provides a

cost-effective system for collecting field screening data for characterization of matrices contaminated with

organic compounds. The Model 4 100 SAW/GC can be used in a field screening mode to produce

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chromatograms in 10 seconds. The components of the 4100 are shock mounted into a rugged field portable

fiberglass shipping case. The solid state resonator has excellent recovery characteristics and provides

sensitivity to picogram levels and spans a dynamic range of more than 8 orders of magnitude.

Experimental Design

The technology demonstration plan [ 11 was developed with input from ORNL, the Department of

Energy (DOE), EPA, the developers, and external peer reviewers. The purpose of the document was to

capture all of the demonstration details, including the experimental design, the quality assurance plan, and

the health and safety plan. The plan was derived from the template outlined in CSCT’s Guidance Manual

[2]. The fundamental areas of evaluation for the demonstration were to; (a) assess performance relative to

conventional analytical methods, (b) examine the impact of sample matrix on performance, (c) determine

the influence of environmental conditions on performance, and (d) observe the operational logistics of the

technologies. Secondary objectives for this demonstration were to evaluate each PCB field analytical

technique in terms of its reliability, ruggedness, cost, range of usefulness, data quality, and ease of

operation.

The demonstration of PCB field analytical techniques was conducted in Oak Ridge, Tennessee.

Field activities occurred at two sites: outdoors (Site #1) and inside a controlled environmental atmosphere

chamber (Site #2). The controlled experimental atmosphere (CEA) facility consists of a room-size, walk-in

chamber ten feet wide and twelve feet in length with air processing equipment for temperature and relative

humidity. The chamber is equipped with an environmental control system including reverse osmosis water

purification supplying the chamber humidity control system. Highefficiency particulate air (HEPA) and

activated charcoal filters are installed for recircuration and building exhaust filtration. Analytical

instrument performance tests were performed inside the CEA chamber to test performance in a climate

different from the ambient outdoor conditions. Because the temperature and humidity were relatively high

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(approximately 90 "F and 90% RH) outdoors, the chamber conditions were set to cooler temperatures and

lower relative humidity (approximately 55 OF and 50% RH).

The developers analyzed real environmental samples consisting of PCB-contaminated soils

excavated at DOE facilities in Oak Ridge (TN), Paducah (KY), and Portsmouth (OH). Prior to the

demonstration, the samples were thoroughly homogenized (dried, blended, sieved, and mixed). In addition

to real environmental samples, performance evaluation (PE) soil samples were analyzed. PE samples were

provided by Environmental Resource Associates (Arvada, CO) and EPA's Office of Solid Waste and

Emergency Response's Analytical Operations Center. An optional set of PCB extracts were also available

for the developers to evaluate.

The developers analyzed a total of 104 soil analyses (68 environmental samples and 36 PE

samples) at each site, including quadruplicate analyses of each soil sample. Concentrations of total PCB in

the samples ranged fiom 0.5 ppm to 500 ppm. In all, the developers analyzed a total of 208 soil analyses,

including 25 unique environmental samples. All but one of the developers participated in the extract sample

analyses, where a total of 12 samples were analyzed at each site. Two concentration levels of extracts (1 0

ppm and 100 ppm) were analyzed in quadruplicate. For each developer, the order of analyses was

randomized and all sample identities were unknown.

Reference Laboratory

Data generated by a reference analytical laboratory was used as a baseline to assess the

performance of the field analytical technologies for PCB analysis. The Oak Ridge Sample Management

Office (SMO) has been tasked by DOE Oak Ridge Operations with maintaining a list of qualified

laboratories to provide analytical services. The technology demonstration plan [ I ] contains the SMO's

standard operating procedures for identifying, qualifying, and selecting analytical laboratories. All of the

qualified laboratories were invited to bid, and the lowest bidder, LAS Laboratories, in Las Vegas, NV, was

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selected by ORNL and the SMO as the reference laboratory.

The reference analytical method, also presented in the technology demonstration plan [ 11, was EPA

SW-846 Method 808 1. Using this method, the PCBs were extracted from the soils with solvent. Acid or

gel permeation chromatography was used to remove interferences from the extracts. The samples were

analyzed for PCBs on a gas chromatograph equipped with capillary columns two dissimilar phases and

dual electron capture detectors.

FCB Demonstration Summary

Report preparation was on-going during the preparation of this manuscript. The technologies will

not be compared to each d!er, cr be rated as the “best” or “worst” technology. Each techno!sgy wi!!

receive its own verification report. Where possible, the field technology’s results will be evaluated relative

to the reference laboratory’s results, to provide some assessment of how the field technology performs

compared to the conventional fixed laboratory analysis. The performance characteristics of the

technologies that will be evaluated include accuracy, precision, klse positivdfalse negative error rate,

completeness, comparability, ruggedness, portability, and cost. EPA-approved reports are expected to be

completed by early to mid- 1998.

Future Demonstrations

ORNL is currently working on two additional technology demonstrations. ORNL will interact

with other federal agencies and additional EPA program offices to build a strong interagency technical team

to lead the execution of these demonstrations.

Decision Support Software (DSS) Demonstration

Decision support software (DSS) integrates environmental data and simulation models into a

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framework for making site characterization, monitoring, and cleanup decisions, (e.g. where to sample,

costhenefit analysis of additional or reduced sampling, human and ecological risk analysis, etc.). An

effective DSS package should integrate, analyze, and present environmental information to assist a project

manager in developing a cost-effective, defensible, cleanuplmonitoring strategy.

A number of software developers have marketed a variety of programs that manage and present

information about a site. This data can be used to assist and guide the environmental decision maker in a

number of ways. The EPA Regions, several EPA Program Ofices, and other Federal Agencies have

expressed interest in the performance and potential applications of these programs when tested under real-

world situations. To accomplish this goal, a testing and verification program is being developed. A number

of wellcharacterized sites will be selected as referexice points against which the performance of each

technology will be measured. The developers will be given information on the site history and target

compound list. Analytical data from a limited number of sampling points will be provided and, where

available, physical parameters such as groundwater flow rates and site characterization data will be

provided. The developers will be expected to proceed iteratively to predict the location and number of

additional sampling points required to describe the contaminant plume with enough confidence to support

engineering decisions such as a remedial action plan or a long-term monitoring plan.

In order to establish communication with potential participants, a developer’s conference will be

held on February 18, 1998 at the EPA Region 9 Headquarters in San Francisco. Based on the selection

criteria and information presented at this meeting, developers may be invited to participate in the

performance verification test scheduled to be conducted at Oak Ridge, TN in the summer of 1998.

Field Earaction Demonstration

The field extraction demonstration is p~anncd to begin in late 1998. The demonstration will focus

on the evaluation of field techniques for sample preparation, and more specifically extraction technologies.

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Matrices, analytes, and overall experimental design will be determined based on the needs and interests of

EPA and the developers.

Conclusions

ETVKSCT demonstrations provide developers with rigorous, statistically defensible testing of

their technologies. Each technology is assessed for its own merits and not compared to the performance of

the other demonstrating technologies. The technology developers receive an evaluation of their performance

during the demonstration, in the form of an EPA report and verification statement.

Sponsorship

Oak Ridge National Laboratory’s participation in this project was sponsored by the U. S. Environmental

Protection Agency, National Exposure Research Laboratory, Las Vegas, Nevada, and the U. S. Department of

Energy, Environmental Managenicnt Program, Gennantown, Maryland. -

References

[ 11 Oak Ridge National Laboratory, Chemical and Analytical Sciences Division. ‘Technology

Demonstration Plan for the Evaluation of Polychlorinated Biphenyl (PCB) Field Analytical

Techniques,” July 16, 1997.

Billets, Stephen, Robertson, Gary, and Koglin, Eric. “A Guidance Manual for the Preparation of

Characterization and Monitoring Technology Demonstration Plans,” Interim Final Report Version

E21

5.0, October 31, 1996.

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Report Number (141)9 bY8Lf

'ubi. Date (11)

DOE