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|Title:||Development of an analytical method for explosive residues in so|
|Authors:||U.S. Army Toxic and Hazardous Materials Agency.|
Jenkins, Thomas F.
Walsh, Marianne E.
High-performance liquid chromatography
|Publisher:||Cold Regions Research and Engineering Laboratory (U.S.)|
Engineer Research and Development Center (U.S.)
|Series/Report no.:||CRREL report ; 87-7.|
Abstract: An analytical method was developed to determine the concentrations of HMX, RDX, TNB, DNB, Tetryl, TNT and 2,4-DNT in soil. The method involves extracting a 2-g sample with 50 mL of acetonitrile using an ultrasonic bath procedure for 18 hr. A 10-mL portion of the extract is diluted with 10 mL of water, filtered through a 0.45-~m Millex SR filter, and analyzed by RP-HPLC using a fixed 254-nm UV detector. Separations were obtained on an LC-18 column eluted with 50:50 water-methanol. Retention times were 2.55, 3.82, 5.16, 6.25, 7.04, 8.47 and 10.15 min for HMX, RDX, TNB, DNB, Tetryl, TNT and 2,4-DNT, respectively. Confirmation of analyte identities is recommended by RP-HPLC on an LC-CN column using 50:50 water-methanol. Kinetic studies using naturally contaminated soil indicated that equilibrium was achieved within 24 hr for the majority of soils and analytes studied. The method provides linear calibration curves over a wide range of concentrations. Reporting limits were conservatively estimated at 1.6, 1.8, 1.5, 0.5, 5.5, 0.8 and 0.8 ~g/g for HMX, RDX, TNB, DNB, Tetryl, TNT and 2,4-DNT. Analytical precision was estimated at ± 0.44, 0.51, 0.43, 0.13, 1.24, 0.27 and 0.20 ~g/g, respectively, in the range of homogeneous variance near the detection limits. At higher concentrations the relative standard deviation was constant at 2% for HMX, RDX, DNB and TNB, 3% for TNT and 2,4-DNT, and 6% for Tetryl. Recovery was found to be greater than 96% for all analytes from a spike-recovery study. The method was successfully tested using contaminated soil from the Iowa Army Ammunition Plant, which gave a range of analyte concentrations from near the detection limit to the percent levels. Several types of commercial 0.45-mm filters were tested. No loss of analytes was found when 50:50 acetonitrile-water solutions were filtered. Note: The presence of the symbol ~ indicates the absence of a scientific or mathematical symbol that could not be rendered by the character set of this system. The downloaded will contain the missing symbols.
|Rights:||Approved for public release; distribution is unlimited.|
|Appears in Collections:||CRREL Report|