Affiliation:
1. U.S. Army Cold Regions Research and Engineering LaboratoryHanover, N H 03755
2. University of New Hampshire, Chemistry Department, Durham, NH 03824
Abstract
Abstract
An analytical method was developed to determine the concentration of nitroaromatic and nitramine residues in soil. Air-dried soil samples are ground with a mortar and pestle and extracted with acetonitrile in an ultrasonic bath. A portion of extract is diluted with aqueous CaCh to flocculate suspended particles, filtered, and analyzed by liquid chromatography. The method provides linear calibration curves over a wide range of concentration. Detection limits ranged from 0.03 to 1.27 ng/g. Recovery of spiked analyte was better than 80% for all analytes tested. Each step in the analytical procedure was optimized using spiked and field-contaminated soils. This optimization included tests to (1) assess the effectiveness and kinetics associated with various extraction methods, solvents, and soil-to-solvent ratios; (2) compare separations achievable using various combinations of reverse-phase columns and eluants; (3) assess analyte recovery and ease of use for various procedures to remove particles from extracts; and (4) document stability of soil extracts and analytical stock and working standards. A ruggedness test and a preliminary assessment at 2 other laboratories indicated that the method was sufficiently rugged to justify a full-scale collaborative test. A comparison of extraction kinetics for spiked soil vs field-contaminated soil revealed very different kinetic behavior, indicating it is unwise to develop extraction procedures based solely on spiked soils.
Publisher
Oxford University Press (OUP)
Cited by
3 articles.
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