GAS CHROMATOGRAPHIC-MASS SPECTROMETRIC ANALYSIS OF HIGH PURITY GERMANE

V. A. Krylov, O. Iu. Chernova, A. Iu. Sozin, A. D. Zorin

Аннотация


The use of capillary adsorption columns in combination with mass spectrometric detection for determining the content of impurities in high-purity germane has been studied. The influence of the amount of the main substance on the separation and determination of impurities was investigated. Increase in the number of dosed germane leads to the substantial broadening of the peaks of impurities located at the end of its chromatographic band and limits the lowering of their limits of detection. The impurity composition of germane has been investigated. The impurities of permanent gases, hydrocarbons С1–С9, fluorine-, chlorine-containing and aromatic hydrocarbons, esters, hydrogen sulfide, homologs of germane, alkyl-derivatives of germane, and chlorogermane have been determined. It is for the first time that the impurities of С6–С9 hydrocarbons, trigermane, ethyl germane and a number of chlorine- and fluorine-containing hydrocarbons have been discovered. The content of the individual impurities in high-purity germane was 1.2∙10–3-2∙10–6 % vol. The achieved limits of detection correspond to the best results available in the literature and for a number of substances they are by 2-5000 times less. The accuracy of the analysis has been proven by the method of varying the sample volume and by comparison with the results of the independent gas-chromatographic analysis.

         Keywords: gas chromatography–mass spectrometry, germane, impurities, detection limit, trueness

(Russian)

DOI:http://dx.doi.org/10.15826/analitika.2015.19.1.010

 

V.A. Krylov1, 2,  O.Iu. Chernova1, A.Iu. Sozin1, A.D. Zorin 2

1G.G. Devyatykh Institute of Chemistry of High-Purity Substances of the Russian Academy of Sciences, Russian Federation, Nizhny Novgorod 

2N.I. Lobachevsky Nizhny Novgorod State University, Russian Federation, Nizhny Novgorod


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Литература


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