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Field-Based Analytical Methods for Explosive Compounds
Field-Based Analytical Methods for Explosive Compounds
Locations for Sampling Studies
Locations for Sampling Studies
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Field-Based Analytical Methods for Explosive Compounds

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1Field-Based Analytical Methods for 40good qualitatively, but not quantitatively
Explosive Compounds. Dr. Thomas F. Jenkins Was commercially available from Supelco No
Marianne E. Walsh USA Engineer Research corresponding method for RDX.
and Development Center– Cold Regions 41Currently Available On-Site
Research and Engineering Laboratory 72 Technologies for Explosives. EXPRAY Kit
Lyme Road, Hanover NH 03755 603-646-4385 (Plexus Scientific) EnSys Colorimetric TNT
(FAX-4785) tjenkins@crrel.usace.army.mil and RDX/HMX Kits (SDI) DTECH Enzyme
marianne@crrel.usace.army.mil. 1. Immunoassay Kits (SDI) Fast 2000 (Research
2Outline of Presentation. Important International) GC-Ionscan (Barringer
properties of nitroaromatic (TNT) and Instruments) GC-TID (SRI Instruments)
nitramine (RDX) explosives Accepted SPREETA TNT Sensor (Texas Instruments)*
laboratory methods for explosives RIDASCREEN TNT Kit (Accurate Chemical
chemicals Detection criteria for & Sci.) *Not commercially available at
explosives-related chemicals Why should present.
you consider using on-site methods? 42EXPRAY Kit. Simplest screening kit
Sampling considerations for explosives in (Colorimetric) Useful for surfaces and
soil and water Verified methods for unknown solids Can be used to provide
on-site determination of explosives in qualitative test for soils Kit contains
soil and water Advantages / disadvantages three spray cans EXPRAY 1 - Nitroaromatics
of various on-site methods. (TNT) ESPRAY 2 - Nitramines (RDX) and
3***Safety***. Chunks of high Nitrate esters (NG) EXPRAY 3 - Black
explosives often found at contaminated powder, ANFO Spray cans used sequentially.
sites Concentrations of TNT or RDX in soil 4343.
greater than 12% are reactive (can 44Use of EXPRAY Kit. For surfaces or
propagate a detonation)* Neither chunks unknown solid Wipe surface with sticky
nor soil with concentrations of TNT and collection paper Spray paper with EXPRAY
RDX greater than 10% can be shipped off For soil Place soil on top of two filter
site using normal shipping procedures papers Soak soil with acetone Spray the
*Kristoff et al. 1987. bottom filter paper with EXPRAY reagents
4Physical and Chemical Properties of (Spray cans used sequentially) Detection
Explosive Chemicals. Most are solids at limit - 20 ng.
environmental temperatures Sources often 4545.
particulate at soil surface Low aqueous 46EnSys Colorimetric Test Kits EPA SW846
solubilities, slow rates of dissolution Methods 8515 and 8510. Initial TNT method
Surface contamination persists for long developed by CRREL 1990* (8515) Initial
periods (50-100 years) Once dissolved, RDX RDX method developed by CRREL 1991**
can migrate rapidly through vadose zone (8510) Commercialized by EnSys, now SDI
TNT readily biotransforms Relatively Colorimetric methods for TNT and RDX / HMX
non-volatile Thermally labile. Successfully used at variety of explosives
5EPA SW846 Standard Laboratory Methods sites Results correlate well with Method
for Nitroaromatic and Nitramine Explosives 8330 TNT kits cost $410 for 20 tests
in Soil and Water. Sample preparation ($20.50 / sample) RDX kits cost $500 for
Water: Salting-out or solid-phase 20 tests ($25 / sample) * Jenkins 1990;
extraction Soil: Ultrasonic extraction **Walsh and Jenkins 1991.
with acetonitrile Determination SW846 47Characteristics of Colorimetric Kits.
Method 8330 (RP-HPLC) SW846 Method 8095 TNT and RDX / HMX tests produce reddish
(GC-ECD) (Draft). colored solutions Concentrations are
6Other Laboratory Methods. CHPPM Method proportional to intensity of color TNT
for Explosives in Water GC-ECD developed test also responds to 2,4-DNT, Tetryl, TNB
by Hable et al. 1991 Excellent method but RDX / HMX test also responds to NG, PETN,
not generally available commercially LC-MS NC, Tetryl TNT test is subject to
Method (SW846 Method 8321) Available at interference from yellow color produced
several commercial labs Explosives not from reaction with humic substances and
target analytes. molecular sulfur (EnSys only) RDX/HMX test
7Target Analytes for SW846 Methods 8330 is subject to interference from nitrate
and 8095. Method 8330 8095 Nitroaromatics ion unless the optional ion exchange step
TNT, TNB, DNB, 2,4-DNT, 2,6-DNT, tetryl, ? is used.
? nitrobenzene, o-,m-,and p-nitrotoluene 4848.
Nitramines RDX, HMX ? ? 4949.
Aminodinitrotoluenes 2-ADNT, 4-ADNT ? ? 50Advantages / Disadvantages of
3,5-dinitroaniline ? Nitrate esters NG, Colorimetric Methods. Advantages Easy to
PETN ? use in the field Good quantitative
8Detection Capabilities for Soil agreement with laboratory results
Analysis. SW846 Method SW846 Method 8330 Dilutions do not require use of an
8095 RP-HPLC-UV GC-ECD TNT 80 µg/kg 0.45 additional kit Screens for presence of
µg/kg RDX 740 µg/kg 3.4 µg/kg HMX 1300 non-targeted explosives Successfully used
µg/kg 25 µg/kg NG ND 13 µg/kg. at many contaminated sites Good method to
9Example Detection Capabilities for assess reactivity of soil prior to
Water Analysis. SW846 Method SW846 Method shipping Disadvantages Requires some
8330 8095 RP-HPLC-UV GC-ECD TNT 0.1 µg/L experience with chemical analysis Class
0.01 µg/L RDX 0.8 µg/L 0.004 µg/L HMX 1.0 specific but not analyte specific Yellow
µg/L 0.004 µg/L NG ND 0.2 µg/L. color from humics can interfere with TNT
10Method 8330 vs. Method 8095. SW846 test Use for water samples requires
Method SW846 Method 8330 8095 RP-HPLC-UV preconcentration (SPE).
GC-ECD more rugged in lower detection 51DTECH Immunoassay Test Kits EPA SW846
routine use capability requires less Methods 4050 and 4051. TNT method
stringent simultaneous determination QA developed by SDI 1993* RDX method
program of nitroaromatics, nitramines, and developed by SDI 1994** Immunoassay
nitrate esters Most commercial labs are methods for TNT and RDX More selective
set up to do Method 8330 but not Method than colorimetric, but some
8095. GC-ECD equipment is generally crossreactivity Successfully used at
available. variety of sites Results given in
11Sampling Studies. Investigated concentration range; ranges in general
traditional sampling approaches for agreement with results from Method 8330
explosives site characterization Surface TNT kits cost $130 for 4 tests ($32.50 /
soils Groundwater. sample) RDX kits cost $130 for 4 tests
12Sampling Problem for TNT in ($32.50 / sample) * Hutter et al. 1993; **
Groundwater. First observed by Goerlitz Teaney and Hudak 1994.
and Franks (1989) at Hawthorne AAP 52Advantages / Disadvantages of DTECH
Concentration of TNT increased from 2.0 to Immunoassay Methods. Advantages Configured
32.0 µg/L after 60 gal of water bailed for ease of use in the field Requires less
Observation confirmed by Pennington et al. training / experience Relatively specific
(1999) at Louisiana AAP Low flow (minimal for TNT and RDX Successfully used at many
drawdown) protocol by Puls and Barcelona contaminated sites No preconcentration
(1996). required for water analysis Disadvantages
13Microbiological Transformation of TNT. Fair quantitative agreement with
14Soil Sampling Strategy for Nature and laboratory results Provides only
Extent of Contamination. Traditional concentration range Provides no
approach uses large sampling grids, small information on non-target analytes
number of discrete samples, and off-site Dilutions require use of additional kit.
analysis Sampling studies characterized 53Studies Evaluating Performance of Test
degree of spatial heterogeneity Compared Kits Relative to Method 8330. Myers et al.
sampling error to analytical error 1994 Haas and Simmons 1995 Jenkins et al.
Investigated use of composite samples to 1996 EPA 1996 (Crockett et al.) Jenkins et
improve representativeness Compared al. 1997 Thorne and Myers 1997 Crockett et
results from on-site and laboratory al. 1998 EPA 1999 (Crockett et al.).
analyses. 54Environmental Technology Verification
15Locations for Sampling Studies. (ETV). Conducted by Oak Ridge NL for EPA /
16Field Sampling Scheme. Samples DoD 108 blind soil and 176 blind water
arranged in a wheel pattern Surface samples Results compared to SW846 Method
samples 0 cm to 15 cm. Diameter of wheel = 8330 1999 Demonstration (Results on web
122 cm. Diameter of sampler = 5 cm site) Research International/NRL Fast 2000
(stainless steel auger). Barringer GC-Ionscan 2000 Demonstration
1717. (Results will be on web site) SRI / CRREL
1818. GC-Thermionic Texas Instruments SPREETA.
1919. 55Fast 2000 (Research International /
2020. NRL). Biosensor using analyte-specific
21Monite Site, Sampling Location #1 antibodies immobilized on solid support
Major Analyte: TNT (mg/kg). 500 On-site Antibodies are saturated with
416 Lab. 331 On-site 286 Lab. 39,800 fluorescently labeled signal molecule
On-site 41,400 Lab. 1,280 On-site 1,220 creating antibody / signal complex Buffer
Lab. 164 On-site 136 Lab. 24,400 On-site flows over the solid support Sample
27,700 Lab. 27,800 On-site 42,800 Lab. injected into buffer stream If analyte
2222. present, fluorescent tag is displaced and
2323. detected by downstream fluorimeter Two
24Valcartier ATR, Sampling Location #10 separate systems for TNT and RDX
Major Analyte: HMX (mg/kg). 16.0 On-site Instrument cost about $23,000.
15.7 Lab. 54.0 On-site 75.2 Lab. 100 56Research International / NRL Fast 2000
On-site 111 Lab. 324 On-site 325 Lab. 183 ETV Results (water). TNT RDX Precision
On-site 190 Lab. 321 On-site 328 Lab. 111 (%RSD) 76% 52% Accuracy (mean recovery)
On-site 142 Lab. 316% 192% False positives 80% 24% False
25Data Analysis from Sampling Studies. negatives 3% 3% Completeness 80% 80%
Analytical error for each type estimated Throughput 3 samples / hr / analyte.
by: reproducibility of duplicate on-site 57Advantages / Disadvantages of RI / NRL
and laboratory analyses Sampling error Fast 2000. Advantages Two methods
estimated by: differences in mean values relatively specific for TNT and RDX No
between sampling locations Accuracy of preconcentration required for water
on-site methods estimated by: comparison analysis Disadvantages Relatively poor
of mean values between on-site and performance in ETV trials Proven to be
laboratory analyses. difficult to maintain for routine
26Soil Analyses: On-Site & operation at Umatilla Army Depot Detection
Laboratory Methods Monite Site and limits often inadequate for water
Hawthorne AAP. analysis.
27Valcartier ATR: TNT Concentrations 58GC-Ionscan (Barringer Instruments).
On-Site vs. Laboratory Results. Extensive experience in explosives
28Valcartier ATR: HMX Concentrations detection for anti-terrorism applications
On-Site vs. Laboratory Results. y = 1.01x (Airport Security) Uses Ion Mobility
– 0.67 r = 0.990. Field (mg/kg). HPLC Spectrometry (IMS) Very sensitive for most
(mg/kg). 2500 2000 1500 1000 500 <d. explosives Combination with GC allows
<d. multianalyte method Instrument well
29Sampling Considerations for developed; minimum development for
Explosives-Contaminated Sites. Soil environmental methods (water).
Concentrations in soil are spatially very 59Barringer GC-Ionscan ETV Results
heterogeneous over very short distances (soil). TNT RDX Precision (%RSD) 51% 54%
For discrete samples Sampling error Accuracy (mean recovery) 136% 55% False
>> Analytical error Composite positives 25% 5% False negatives 13% 2%
samples provide more representative data Completeness 100% 100% Throughput 3
than discrete samples Groundwater samples / hr.
Concentration near well screens often not 60Barringer GC-Ionscan ETV Results
typical of formation water Low flow (water). Method tested: Detection limits
(minimal drawdown) sampling preferable. (DL) inadequate for any normal application
30Advantages of Using Composite Samples. Could be combined with preconcentration
Physical averaging process Vastly improves using Solid Phase Extraction (SPE) to
representativeness of samples Allows a improve DL.
reduction in samples analyzed while 61Advantages / Disadvantages of
improving characterization Provides a Barringer GC-Ionscan. Advantages Provides
greater degree of statistical confidence on-site multianalyte results for all major
than a comparable set of discrete samples target analytes Low false positive / false
Jenkins et al. 1996. negative rates Disadvantages Requires
31Cost Comparisons. TOTAL COST: $ 90 per on-site chemist with experience Requires
composite sample. TOTAL COST: $ 337 per compressed gasses on site Relatively poor
discrete sample. Collection of 7 Discrete performance in ETV trials Instrument cost
Samples, Homogenization, Compositing, and is high ($60,800) Environmental methods
On-Site Analysis PLUS LAB VALIDATION FOR 1 need further improvement.
OF EVERY 10. Collection of 1 Discrete 62SRI / CRREL GC-TID Method. GC-TID
Sample, Shipment, and Lab Analysis. Instrument manufactured by SRI (Model
32Conclusions in Verse. Seven sites were 8610C) Method developed by Hewitt et al.
sampled that contained some TNT, One 2000 (CRREL) Allows on-site determination
Ammonium Picrate, and another DNT. Very of important military high explosives and
heterogeneous were these explosives as degradation products and some primary
they lay, Differing by ten times ten, explosives Nitroaromatics: TNT, 2,4-DNT
though two short feet away, Statistical Nitramines: RDX, HMX Nitrate esters: PETN,
calculations proved conclusively, did they NG Degradation products: TNB, 2-ADNT,
not? That sampling error far exceeded 4-ADNT Instrument costs about $9000.
analytical by a lot! Thus our 63SRI / CRREL GC-TID ETV Results (soil).
recommendations to improve the sampling TNT RDX Precision (%RSD) 17% 13% Accuracy
scheme Are simple and effective and are (mean recovery) 97% 91% False positives 1%
not at all extreme: Homogenize your soil 0% False negatives 3% 1% Completeness 100%
cores as soon as they’re removed, 100% Throughput 3 samples / hr.
Composite them together and analysis is 64Advantages / Disadvantages of SRI /
improved. Finally, to preclude the chance CRREL GC-TID. Advantages Provides on-site
of wrong interpretation, Each sample must results for all major target analytes
provide us with an accurate Excellent quantitative agreement with
representation. Jane G. Mason, CRREL. laboratory Low false positive / false
33Reduction of Within-Sample negative rates Instrument cost only about
Heterogeneity for Soil Samples. Because $9,000 Disadvantages Requires on-site
explosives have low volatility, thorough chemist with GC experience Requires
mixing can reduce within-sample compressed gasses on site New method; no
heterogeneity Very important for track record at real sites.
split-sample analyses Use of adequate 65RIDASCREEN TNT Kit (Accurate Chemical
subsample size (20 g or more) Some vendors & Scientific). Classical competitive
of on-site methods do not understand this immunoassay Uses 96 well plate
problem and specify very small sample Antigen-antibody reaction Photometric
sizes More important for on-site methods measurement at 450 nm Requires microtiter
where sample homogenization is less plate spectrophotometer Detection limits:
complete than in laboratory. 30 ppt for water, 3 ppb for soil
34Sample Processing / Holding Times. Crossreactive to TNB, tetryl Cost $775 for
Nitroaromatics are subject to 96 test well plate.
microbiological transformation and 66Advantages / Disadvantages of
photodegradation Soil and water samples RIDASCREEN TNT Kit. Advantages Provides a
should be kept cold in the dark Water quantitative result Requires less training
samples can be preserved using / experience Relatively specific for TNT
acidification to extend holding times* No preconcentration required for water
Official holding times are 7 days to analysis Disadvantages No corresponding
extraction *Jenkins et al. 1995. method for RDX No independent validation
35What are the Important Target Analytes No track record at real sites.
at Explosive-Contaminated Sites? Study 67Action Criteria for Soils. No
summarized the results from two Corps of universal criteria established Action
Engineers Laboratories (1) What percentage levels are negotiated on a site-specific
of soil and water samples from explosives basis EPA Region 3 Screening Levels
sites had explosives present? (2) When (Residential) TNT: 21 mg/kg RDX: 5.8
explosives were detected, what was the mg/kg.
frequency of detecting specific analytes? 68Human-Health-Related Water-Quality
Walsh et al. 1993 Walsh et al. 1993. Criteria for Explosives-Related Chemicals.
36Frequency of Occurrence of Explosives Drinking Water Health Advisory * (µg/L)
Analytes in Laboratory Analyses. Soil TNT 2 RDX 2 HMX 400 NG 5 1,3-DNB 1
samples (Explosives detected: 28%) *Lifetime exposure (EPA 1996).
Contaminated samples TNT: 66% RDX: 27% 69Detection Limits. Soil (mg/kg) Water
TNT, RDX or 2,4-DNT: 94% Water samples (?g/L) SDI EnSys (TNT, RDX) 1.0 1, 5 SDI
(Explosives detected: 14%) Contaminated DTECH (TNT, RDX) 0.5 5 RI Fast 2000 (TNT,
samples TNT: 56% RDX: 61% TNT or RDX: 94% RDX) -- 20 Barringer GC-Ionscan 0.3 25
Walsh et al. 1993. (TNT, RDX) SRI / CRREL GC-TID 0.005, 0.5
37TNT RDX. Most Important Analytes for -- (TNT, RDX) TI SPREETA (TNT) 0.3 --
On-Site Characterization of Explosives RIDASCREEN (TNT) 0.003 --. 69.
Contamination. 70What About Other Explosives? Ammonium
38Examples of Objectives for On-Site picrate / picric acid Thorne and Jenkins
Analysis of Soils. Determining horizontal 1997 NG and PETN EnSys (SDI) RDX test
and vertical extent of contamination works for these too Barringer GC-Ionscan
Allowing identification of samples for SRI / CRREL GC-TID.
treatment studies Providing data for risk 71Overall Conclusions. On-site analysis
assessments Determining whether soil can be cost effective for site
presents a detonation hazard Providing characterization at
rapid analysis to guide excavation during explosives-contaminated sites In
remediation Determining whether treatment combination with composite sampling, data
goals have been attained. quality can be adequate for many remedial
39Examples of Objectives for On-Site decisions On-site analysis of production
Analysis of Water. Rapid analysis of water from pump-and-treat systems has
well-water samples Evaluation of proven very cost effective A number of
contamination in seeps and surface waters on-site technologies are available SW846
Routine assessment of treatment efficiency and ETV have provided information useful
of pump-and-treat systems. for selecting the technology for various
40Initial On-Site Method for TNT. applications.
Developed by Heller et al. (1982) to 72After viewing the links to additional
detect TNT in water Used colorimetric resources, please complete our online
reaction and ion exchange to produce a feedback form. Thank You. Links to
colored stain Length of stain in tube was Additional Resources.
proportional to concentration Method was
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Field-Based Analytical Methods for Explosive Compounds

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