气相色谱-质谱联用法研究富集同位素德国70GeH4的杂质组成

A. Y. Sozin, V. Krylov, O. Y. Chernova, T. G. Sorochkina, A. D. Bulanov, O. Troshin, S. A. Adamchik, A. Y. Lashkov
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摘要

首次采用气相色谱-质谱联用技术研究了同位素富集锗70GeH4的杂质组成。为了分离杂质,我们使用了GS-GasPro毛细管吸附柱(60 m × 0,32 mm,硅胶为吸附剂),GS-CarbonPLOT毛细管吸附柱(25 m × 0,32 mm × 0,25 μm,碳吸附剂)和25 m × 0,26 mm × 0,25 μm,吸附剂聚三甲基硅丙烯。已经证明,使用它们可以实现色谱物质的高分辨率。通过质谱与NIST文库数据的比较,对杂质进行了鉴定。在日耳曼中发现了气体,它是大气的一部分,C1 - C7碳氢化合物,氯和含氧碳氢化合物,含硫物质,日耳曼的同系物和烷基衍生物。通过对杂质70GeC3H10和70GeC4H12质谱组成的研究,首次获得并描述了文献中未见的杂质70GeC3H10和70GeC4H12的质谱。确定了高纯度锗中杂质的浓度,以及它们在精馏提纯过程中分离出的馏分上的分布。检出限为2·10-7 - 1·10-4 mol。%。
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Study of the impurity composition of isotope enriched german 70GeH4 by the method of gas chromatography-mass spectrometry
For the first time, the impurity composition of isotopically enriched germane 70GeH4 has been studied by gas chromatography-mass spectrometry. To separate impurities, we used a GS-GasPro capillary adsorption column 60 m × 0,32 mm with silica gel as a sorbent, GS-CarbonPLOT 25 m × 0,32 mm × 0,25 μm with a carbon sorbent and 25 m × 0,26 mm × 0,25 μm with sorbent polytrimethylsilylpropine. It has been shown that their use makes it possible to achieve a high resolution of the chromatographed substances. The identification of impurities was carried out by comparing their mass spectra with the data of the NIST library. Gases are found in germane, which are part of the atmosphere, C1 – C7 hydrocarbons, chlorine and oxygenated hydrocarbons, sulfur-containing substances, homologues and alkyl derivatives of germane. As a result of studying the composition of their mass spectra, the mass spectra of impurities 70GeC3H10 and 70GeC4H12, which are absent in the literature sources, were obtained and described for the first time. Concentrations of impurities in high-purity germane, as well as their distribution over fractions isolated during its rectification purification, have been determined. The detection limits of the identified substances were 2·10–7 – 1·10–4 mol. %.
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