Optimization of accelerated solvent extraction for the analysis of munitions residues in sediment samples

Citation
Fi. Onuska et al., Optimization of accelerated solvent extraction for the analysis of munitions residues in sediment samples, J MICROCOL, 13(2), 2001, pp. 54-61
Citations number
17
Categorie Soggetti
Spectroscopy /Instrumentation/Analytical Sciences
Journal title
JOURNAL OF MICROCOLUMN SEPARATIONS
ISSN journal
10407685 → ACNP
Volume
13
Issue
2
Year of publication
2001
Pages
54 - 61
Database
ISI
SICI code
1040-7685(2001)13:2<54:OOASEF>2.0.ZU;2-5
Abstract
Accelerated solvent extraction (ASE) has been compared with a Soxhlet extra ction for extracting and estimating the concentration of hexahydro-1,3,5-tr initro-s-triazine (RDX) and octahydro-1.3,5,7-tetrazocine (HMX) in sediment samples. Extraction of RDX and HMX was studied in terms of process kinetic s and recovery. A three factor, 16 run triplicate experimental design was u sed to generate data on each of two extraction solvents, acetonitrile and a mixture of acetone-methanol (1:1). Response surface methods were used to m odel the dependence of the concentration on the experimental conditions and to establish the optimum extraction conditions. The results were complex i n that several interactions were found among analyte, method, and solvent. Acetonitrile was superior to acetone-methanol for RDX and HMX from the pers pectives of kinetics and recovery, due in part to a much higher solubility. The accelerated solvent extraction generally recovered more than the Soxhl et. In terms of sample throughput, the accelerated solvent extraction offer s advantages over the Soxhlet. A spike recovery study using fortified sedim ent yielded complete recoveries of HMX and RDX. (C) 2001 John Wiley & Sons. Inc.