THE ENVIRONMENTAL TECHNOLOGY VERIFICATION

PROGRAM

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Oak Ridge National Laboratory

Joint Verification Statement

TECHNOLOGY TYPE:

EXPLOSIVES DETECTION



APPLICATION:

MEASUREMENT OF EXPLOSIVES IN CONTAMINATED
SOIL AND WATER

TECHNOLOGY NAME:

GC-IONSCAN™



COMPANY:

Barringer Instruments



ADDRESS:

30 Technology Drive
Warren, NJ 07059

PHONE: (908) 222-9100
FAX: (908) 222-1557

WEB SITE:
EMAIL:

www.barringer.com
rdebono@bii.barringer.com



The U.S. Environmental Protection Agency (EPA) has created the Environmental Technology Verification
Program (ETV) to facilitate the deployment of innovative or improved environmental technologies through
performance verification and dissemination of information. The goal of the ETV Program is to further
environmental protection by substantially accelerating the acceptance and use of improved and cost-effective
technologies. ETV seeks to achieve this goal by providing high quality, peer reviewed data on technology
performance to those involved in the design, distribution, financing, permitting, purchase, and use of
environmental technologies.

ETV works in partnership with recognized standards and testing organizations, stakeholder groups consisting
of regulators, buyers, and vendor organizations, with the full participation of individual technology developers.
The program evaluates the performance of innovative technologies by developing test plans that are
responsive to the needs of stakeholders, conducting field or laboratory tests (as appropriate), collecting and
analyzing data, and preparing peer-reviewed reports. All evaluations are conducted in accordance with
rigorous quality assurance protocols to ensure that data of known and adequate quality are generated and that
the results are defensible.

The Department of Defense (DoD) has a similar verification program known as the Environmental Security
Technology Certification Program (ESTCP). The purpose of ESTCP is to demonstrate and validate the most
promising innovative technologies that target DoD's most urgent environmental needs and are projected to
pay back the investment within 5 years through cost savings and improved efficiencies. ESTCP
demonstrations are typically conducted under operational field conditions at DoD facilities. The

EPA-VS-SCM-45

The accompanying notice is an integral part of this verification statement.

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demonstrations are intended to generate supporting cost and performance data for acceptance or validation of
the technology. The goal is to transition mature environmental science and technology projects through the
demonstration/ validation phase, enabling promising technologies to receive regulatory and end user
acceptance in order to be fielded and commercialized more rapidly.

The Oak Ridge National Laboratory (ORNL) is one of the verification organizations operating under the Site
Characterization and Monitoring Technologies (SCMT) program. SCMT, which is administered by EPA's
National Exposure Research Laboratory, is one of 12 technology areas under ETV. In this demonstration,
ORNL evaluated the performance of explosives detection technologies. This verification statement provides a
summary of the test results for Barringer Instruments' GC-IONSCAN™. This verification was conducted
jointly with the Department of Defense's (DoD's) Environmental Security Technology Certification Program
(ESTCP).

DEMONSTRATION DESCRIPTION

This demonstration was designed to evaluate technologies that detect and measure explosives in soil and
water. The demonstration was conducted at ORNL in Oak Ridge, Tennessee, from August 23 through
September 1, 1999. Spiked samples of known concentration were used to assess the accuracy of the
technology. Environmentally contaminated soil samples, collected from DoD sites in California, Louisiana,
Iowa, and Tennessee and ranging in concentration from 0 to approximately 90,000 mg/kg, were used to
assess several performance characteristics. Explosives-contaminated water samples from Tennessee,

Oregon, and Louisiana with concentrations ranging from 0 to 25,000 |jg/L also were analyzed. The primary
constituents in the samples were 2,4,6-trinitrotoluene (TNT); isomeric dinitrotoluene (DNT), including both
2,4-dinitrotoluene and 2,6-dinitrotoluene; hexahydro-l,3,5-trinitro-l,3,5-triazine (RDX); and octahydro-1,3,5,7-
tetranitro-l,3,5,7-tetrazocine (HMX). The results of the soil and water analyses conducted under field
conditions by the GC-IONSCAN were compared with results from reference laboratory analyses of
homogenous replicate samples determined using EPA SW-846 Method 8330. Details of the demonstration,
including a data summary and discussion of results, may be found in the report entitled Environmental
Technology Verification Report: Explosives Detection Technology — Barringer Instruments, GC-
IONSCAN™ EPA 600-R-00/046.

TECHNOLOGY DESCRIPTION

The GC-IONSCAN is a fully transportable field-screening instrument that combines the rapid analysis time of
ion mobility spectrometry (IMS) with the separation ability of gas chromatography (GC). The instrument can
be operated in IONSCAN mode or in GC-IONSCAN mode to detect explosives. The user can switch
between the two modes in less than 30 s through the instrument control panel. In the IONSCAN mode,
samples are deposited on a Teflon filter and thermally desorbed directly to the IMS, permitting the quick
screening analysis of explosives residues in 6 to 8 s. In the GC-IONSCAN mode, extracts are directly
injected onto the GC column and analysis occurs within 1 to 3 minutes, depending on the type of explosive.
The use of the IONSCAN mode permits rapid prescreening of samples with identification of the major
constituents of the sample and semiquantitative analysis, while the GC-IONSCAN mode permits full
characterization and quantitative analysis of the sample. This technology is capable of reporting quantitative
data for all of the Method 8330 analytes. The performance assessment described here is only for TNT and
RDX because a limited amount of data was available for evaluation of the other analytes. Reporting limits for
the GC-IONSCAN ranged from 0.3 to 10 mg/kg for soil and 25 to 1950 |jg/L for water.

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VERIFICATION OF PERFORMANCE

The following performance characteristics of the GC-IONSCAN were observed:

Precision: For the soil samples, the mean relative standard deviations (RSDs) for RDX and TNT were 54%
and 51%, respectively. For water samples, the RSDs were significantly lower, at 20% and 26%, respectively.

Accuracy: For the soil samples, the median percent recoveries for RDX and TNT were 55% and 136%,
respectively. The results were generally biased low for RDX and biased high for TNT. For water samples,
only a few of the RDX and TNT results were reported above the reporting limits in the spiked samples. The
recoveries were significantly lower, with the highest recovery at 46%, indicating that the water results were
biased low for both analytes.

False positive/false negative results: Of the 20 blank soils, Barringer reported RDX in one sample (5%
false positives) and TNT in five samples (25% false positives). No false positives were reported for RDX and
TNT in the 20 blank water samples. False positive and false negative results were also determined by
comparing the GC-IONSCAN result to the reference laboratory result for the environmental and spiked
samples (e.g., whether the GC-IONSCAN reports a result as a nondetect that the reference laboratory
reported as a detection, and vice versa). For the soils, 3% of the RDX results and none of the TNT results
were reported as false positives relative to the reference laboratory results. Significantly more samples were
reported as nondetects by Barringer (i.e., false negatives) when the laboratory reported a detection (2% for
RDX and 13% for TNT). Similar results were observed for water, where 2% of the TNT results and none of
the RDX results were false positives, and a higher percentage (39% of the RDX results and 21% of the TNT
results) were false negatives.

Completeness: The GC-IONSCAN generated results for all 108 soil samples and all 176 water samples, for
a completeness of 100%.

Comparability: A one-to-one sample comparison of the GC-IONSCAN results and the reference laboratory
results was performed for all samples (spiked and environmental) that were reported as detects. The cor-
relation coefficient (r) for the comparison of the entire soil data set for TNT was 0.88 (slope (in) = 4.82).
When comparability was assessed for specific concentration ranges, the r value did not change dramatically
for TNT, ranging from 0.71 to 0.85 depending on the concentrations selected. RDX correlation with the
reference laboratory for soil was similar (r values near 0.80), except for concentrations greater than
1,000 mg/kg, where the correlation was lower (r = 0.28, m = 0.14). For the water samples, comparability with
the reference laboratory results for TNT was much lower than the soil comparison (r = 0.53). For RDX, the
correlation was much higher, at 0.95. Although the correlation was high, the slope of the linear regression line
was 0.08, indicating that the GC-IONSCAN RDX results were biased low (see Accuracy).

Sample Throughput: Throughput was approximately three samples per hour for soil and eight samples per
hour for water. This rate was accomplished by two operators and included sample preparation and analysis.

Ease of Use: Users unfamiliar with ion mobility spectrometry would require approximately two days of
training to operate the GC-IONSCAN. Training is provided by Barringer Instruments. No particular level of
educational training is required for the operator, but knowledge of chromatographic techniques would be
advantageous.

Overall Evaluation: The overall performance of the GC-IONSCAN for the analysis of RDX and TNT was
characterized as precise and biased low (both analytes) for water analyses, and imprecise and biased (low for

EPA-VS-SCM-45

The accompanying notice is an integral part of this verification statement.

March 2000


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RDX and high for TNT) for soil analyses. As with any technology selection, the user must determine if this
technology is appropriate for the application and the project's data quality objectives. For more information on
this and other verified technologies, visit the ETV web site at http://www.epa.gov/etv.

Jeffrey Marqusee, Ph.D.

Department of Defense

Director, Environmental Security Technology Certification Program

NOTICE: EPA and ESTCP verifications are based on evaluations of technology performance under specific,
predetermined criteria and appropriate quality assurance procedures. EPA, ESTCP, and ORNL make no expressed
or implied warranties as to the performance of the technology and do not certify that a technology will always
operate as verified. The end user is solely responsible for complying with any and all applicable federal, state, and

Gary J. Foley, Ph.D.

Director, National Exposure Research Laboratory
Office of Research and Development

David E. Reichle, Ph.D.
Associate Laboratory Director
Oak Ridge National Laboratory

EPA-VS-SCM-45

The accompanying notice is an integral part of this verification statement.

March 2000


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