Abstract
A method of chromato-mass spectrometry is used to study the impurity composition of monosilane obtained in the reaction of magnesium silicide with ammonium chloride in liquid ammonia. To improve the reliability of the impurity identification along with the study of pure monosilane samples we analyzed monosilane fractions isolated upon purification by low temperature rectification. To separate the impurities of permanent gases, hydrocarbons C 1 – C 3 , volatile inorganic hydrides, disilane, and alkylsilanes we used an adsorption capillary column GS-GasPro 60 m × 0.32 mm with a modified silica gel. To separate the homologues of monosilane, siloxanes, and alkylsilanes we used a column 25 m × 0.26 mm, d f = 0.25 μm with a polytrimethylsilylpropyne (PTMSP) sorbent. Identification of the impurities was performed by comparison of their experimental mass spectra with the NIST database. In the absence of the mass spectra of analytes in the NIST electronic database or a low coincidence of the spectra identification was performed using data of mass spectra and retention time published in the literature. The impurities of permanent gases, carbon dioxide, hydrocarbons C 1 – C 3 , volatile inorganic hydrides, monosilane homologues, siloxanes, and alkylsilanes were identified in monosilane. Quantitative determination of the impurities was carried out in the mode of selective ion detection by the mass numbers having the maximum signal/noise ratio. Calculation of their concentrations was performed using a method of absolute calibration by the peak areas. The concentrations of the impurities in the lack of reference samples were determined using the dependence of the sensitivity coefficients of their detection on the magnitude of the total ionization cross sections. The detection limits of the impurities range within 1 × 10 –5 — 2 × 10 –7 % mol. The accuracy of the analysis was confirmed by the method of sample size variation. The results of determination of the impurities in monosilane after synthesis, in that purified by low temperature rectification, and in the isolated fractions with concentrated higher- and lower-boiling impurities.
Highlights
© Àíäðåé Þðüåâè÷ Ñîçèí1, Àíàòîëèé Ïàâëîâè÷ Êîòêîâ2, Íàòàëüÿ Äìèòðèåâíà Ãðèøíîâà2, Îëåã Ñåðãååâè÷ Àíîøèí2, Àëåêñåé Èãîðåâè÷ Ñêîñûðåâ2, Äìèòðèé Ôåäîðîâè÷ Àðõèïöåâ2, Îëüãà Þðüåâíà ×åðíîâà1, Òàòüÿíà Ãåííàäüåâíà Ñîðî÷êèíà1
A method of chromato-mass spectrometry is used to study the impurity composition of monosilane obtained in the reaction of magnesium silicide with ammonium chloride in liquid ammonia
Identification of the impurities was performed by comparison of their experimental mass spectra with the NIST database
Summary
© Àíäðåé Þðüåâè÷ Ñîçèí1, Àíàòîëèé Ïàâëîâè÷ Êîòêîâ2, Íàòàëüÿ Äìèòðèåâíà Ãðèøíîâà2, Îëåã Ñåðãååâè÷ Àíîøèí2, Àëåêñåé Èãîðåâè÷ Ñêîñûðåâ2, Äìèòðèé Ôåäîðîâè÷ Àðõèïöåâ2, Îëüãà Þðüåâíà ×åðíîâà1, Òàòüÿíà Ãåííàäüåâíà Ñîðî÷êèíà1. Ìåòîäîì õðîìàòî-ìàññ-ñïåêòðîìåòðèè èññëåäîâàí ïðèìåñíûé ñîñòàâ ìîíîñèëàíà, ïîëó÷åííîãî ïî ðåàêöèè âçàèìîäåéñòâèÿ ñèëèöèäà ìàãíèÿ ñ õëîðèäîì àììîíèÿ â ñðåäå æèäêîãî àììèàêà. Äëÿ ðàçäåëåíèÿ ïðèìåñåé ïîñòîÿííûõ ãàçîâ, óãëåâîäîðîäîâ C1 – C3, ëåòó÷èõ íåîðãàíè÷åñêèõ ãèäðèäîâ, äèñèëàíà, àëêèëñèëàíîâ èñïîëüçîâàëè êàïèëëÿðíóþ àäñîðáöèîííóþ êîëîíêó GS-GasPro 60 ì × 0,32 ìì ñ ìîäèôèöèðîâàííûì ñèëèêàãåëåì, à äëÿ ðàçäåëåíèÿ ïðèìåñåé ãîìîëîãîâ ìîíîñèëàíà, ñèëîêñàíîâ, àëêèëñèëàíîâ — êîëîíêó 25 ì × 0,26 ìì, df = 0,25 ìêì ñ ñîðáåíòîì ïîëèòðèìåòèëñèëèëïðîïèíîì (ÏÒÌÑÏ).
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