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T. A. Bolotnik, A. D. Smolenkov, R. S. Smirnov, O. A. Shpigun
Determination of rocket kerosene in soil by
static headspace analysis with gas chromatography-mass spectrometry
Abstract
The method for the determination of rocket kerosene (RG-1 and T-1) in
soil by static headspace analysis with following use of gas chromatography-mass
spectrometry is developed. It has been shown that headspace analysis of solid
sample is a preferred approach of sample pretreatment rather than the
ultrasonic extraction by methanol and analysis of equilibrium vapor phase over
extract. Effects of temperature, incubation time of the sample, its moisture on
the extraction and sensitivity of the headspace determination of rocket
kerosene for soils of various nature were considered. It has been found that 1
cm3 of vapor above the sample at a temperature of 90°C for 20 min
should be injected into the chromatograph for the determination of the mass
concentration of kerosene in the soil in the range of 50–500 mg∙kg–1
(injection mode is splitless). To determine the content in the range of
500–20000 mg∙kg–1, 0.1 cm3 of vapor above the
sample under similar conditions should be injected into the chromatograph
(injection mode is split 1:10). Intra-day precision of the results of
measurements for the studied concentration is from 12 to 6%, and inter-day
precision ranges from 14.3 to 7.4%. GC analysis time is 41 min.
Key words: rocket
kerosene, oil, gas chromatography, mass spectrometry, headspace analysis.
Copyright (C) Chemistry Dept., Moscow State University, 2002
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