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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