Form Approved
REPORT DOCUMENTATION PAGE
OMB No. 0704-0188
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1. AGENCY USE ONLY (Leave blank)
2. REPORT DATE
3. REPORT TYPE AND DATES COVERED
June 1998
4. TITLE AND SUBTITLE
5. FUNDING NUMBERS
Determination of Nitroaromatic, Nitramine, and Nitrate Ester Explosives
in Water Using SPE and GC-ECD:
Comparison with HPLC
6. AUTHORS
Marianne E. Walsh and Thomas A. Ranney
7. PERFORMING ORGANIZATION NAME(S) AND ADDRESS(ES)
8. PERFORMING ORGANIZATION
REPORT NUMBER
U.S. Army Cold Regions Research and Engineering Laboratory
72 Lyme Road
CRREL Report 98-2
Hanover, New Hampshire 03755-1290
9. SPONSORING/MONITORING AGENCY NAME(S) AND ADDRESS(ES)
10. SPONSORING/MONITORING
AGENCY REPORT NUMBER
Office of the Chief of Engineers
U.S. Army Environmental Center
SFIM-AEC-ET-CR-98021
Washington, DC 20314-1000
P2 and Environmental Technology Division
Aberdeen Proving Ground, MD 21010-5401
For conversion of SI units to non-SI units of measurement consult Standard Practice for Use of the
11. SUPPLEMENTARY NOTES
International System of Units (SI), ASTM Standard E380-93, published by the American Society for Testing and Materials,
1916 Race St., Philadelphia, PA 19103.
12a. DISTRIBUTION/AVAILABILITY STATEMENT
12b. DISTRIBUTION CODE
Approved for public release; distribution is unlimited.
Available from NTIS, Springfield, VA 22161.
13. ABSTRACT (Maximum 200 words)
An analytical method for the determination of nitroaromatic, nitramine, and nitrate ester explosives and co-
contaminants in water was developed based on SPE (solid-phase extraction) and GC-ECD (gas chromatograph-
electron capture detector). Water samples are preconcentrated using either cartridge or membrane SPE followed
by elution with acetonitrile. The acetonitrile extract is compatible with both liquid and gas chromatography,
thereby allowing direct comparison of concentration estimates obtained by different methods of determination.
Quantitative GC analyses were obtained by using deactivated direct-injection-port liners, short wide-bore capil-
lary columns, and high linear carrier gas velocities. Recoveries from spiked samples were 90% or greater for each
of the nitroaromatics and nitrate esters, and greater than 70% for nitramines and amino-nitrotoluenes. Estimates
of analyte concentrations in well-water extracts from military sites in the United States and Canada analyzed by
GC-ECD and the standard HPLC (high performance liquid chromatography) method showed good agreement
for the analytes most frequently detected (HMX [octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine], RDX
[hexahydro-1,3,5-trinitro-1,3,5-triazine], TNT [2,4,6-trinitrotoluene], and TNB [1,3,5-trinitrobenzene]). The GC
method provides lower method detection limits for most analytes than HPLC, but accurate calibration is more
difficult. The ultraviolet (UV) detector used for the HPLC analysis has much greater linear range than the ECD
14. SUBJECT TERMS
15. NUMBER OF PAGES
33
Analytical methods
RDX
Water analysis
16. PRICE CODE
Gas chromatography
TNT
17. SECURITY CLASSIFICATION
18. SECURITY CLASSIFICATION
19. SECURITY CLASSIFICATION
20. LIMITATION OF ABSTRACT
OF REPORT
OF THIS PAGE
OF ABSTRACT
UNCLASSIFIED
UNCLASSIFIED
UNCLASSIFIED
UL
Standard Form 298 (Rev. 2-89)
NSN 7540-01-280-5500
Prescribed by ANSI Std. Z39-18
298-102
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