Abstract
The impurity composition of 28SiF4 has been studied for the first time by gas chromatography/mass spectrometry using gas-adsorption capillary columns. For identification and determination of impurity substances by gas chromatography/mass spectrometry, we have proposed using cryogenic preconcentration of the impurities from 28SiF4. The presence of C2–C4 hydrocarbon impurities and sulfur hexafluoride has been confirmed. We have identified 35 impurity substances in 28SiF4, including linear and branched C5–C8 saturated hydrocarbons, aromatic hydrocarbons, chlorine- and fluorine-containing hydrocarbons, and silicon- and sulfur-containing substances, of which 28 have been detected for the first time.
Similar content being viewed by others
References
Volkov, N.F. and Trubnyakov, Yu.I., Addressing some issues pertaining to more accurate determination of Avogadro’s number, Tr. Metrol. Inst. SSSR, 1979, no. 234/239, pp. 10–13.
Devyatykh, G.G., Bulanov, A.D., Gusev, A.V., et al., High-purity single-crystal monoisotopic silicon-28 for precise determination of Avogadro’s number, Dokl. Chem., 2008, vol. 421, no. 1, pp. 157–160.
Bulanov, A.D., Sennikov, P.G., Krylov, V.A., et al., Hydrocarbon impurities in SiF4 and SiH4 prepared from it, Inorg. Mater., 2007, vol. 43, no. 4, pp. 364–368.
Chernov, R.V. and Kovzun, I.G., Thermal dissociation of sodium fluorosilicate in the presence of mineral additives, Ukr. Khim. Zh. (Russ. Ed.), 1972, vol. 38, no. 4, pp. 318–323.
Schmidt, F.A., Rehbein, D., and Chiotti, P., US Patent 4 446 120, 1984.
Bulanov, A.D., Pryakhin, D.A., and Balabanov, V.V., Preparation of high-purity silicon tetrafluoride by thermal dissociation of Na2SiF6, Russ. J. Appl. Chem., 2003, vol. 76, no. 9, pp. 1393–1395.
Nikolaev, N.S., Suvorova, S.N., Gurovich, E.I., et al., Analiticheskaya khimiya ftora (Analytical Chemistry of Fluorine), Moscow: Nauka, 1970.
Krylov, V.A., Sennikov, P.G., Chernova, O.Yu., Sorochkina, T.G., Sozin, A.Yu., Chuprov, L.A., Adamchik, S.A., and Kotkov, A.P., Molecular analysis of isotopically enriched 28SiF4 and 28SiH4 prepared from it, Inorg. Mater., 2008, vol. 44, no. 7, pp. 766–772.
Krylov, V.A. and Sorochkina, T.G., Gas-chromatographic determination of C1–C4 hydrocarbon trace impurities in high-purity silicon tetrafluoride, J. Anal. Chem., 2005, vol. 60, no. 12, pp. 1125–1128.
Sozin, A.Yu., Analysis of high-purity isotopically enriched silane by gas chromatography/mass spectrometry, Perspekt. Mater., 2008, no. 5, pp. 226–231.
Margrave, I.L., Sharp, K.G., and Wilson, P.W., Silicon–fluorine chemistry. IX. The reactions of silicon difluoride and silicon tetrafluoride with water and some reactions of tetrafluorodisiloxane, J. Am. Chem. Soc., 1970, vol. 92, no. 6, pp. 1530–1532.
Ignatov, S.K., Sennikov, P.G., Chuprov, L.A., and Razuvaev, A.G., Thermodynamic and rate parameters of elementary steps in silicon tetrafluoride gas-phase hydrolysis, Izv. Akad. Nauk, Ser. Khim., 2003, no. 4, pp. 797–805.
Loginov, A.V. and Garbar, A.M., Properties, preparation, and application of silicon tetrafluoride, Vysokochist. Veshchestva, 1989, no. 5, pp. 27–34.
Ishikawa, N. and Kobayashi, Y., Fluorine Compounds. Chemistry and Application, Tokyo: Kodansha, 1979 (in Jpn).
Berezkin, V.G., Korolev, A.A., and Khotimskii, V.S., Polytrimethylsilylpropyne as a chromatographic adsorbent in capillary gas chromatography, Dokl. Phys. Chem., 2000, vol. 370, nos. 1–3, pp. 1–4.
Krylov, V.A., Sozin, A.Yu., Zorin, V.A., et al., Gas chromatography/mass spectrometry determination of impurities in high-purity isotopically enriched silane, Mass-Spektrom., 2008, vol. 4, pp. 225–233.
Krylov, V.A. and Sorochkina, T.G., Gas-chromatographic determination of C1–C4 hydrocarbons and sulfur hexafluoride in high-purity germanium tetrafluoride of natural and isotopically enriched composition, Zavod. Lab., Diagn. Mater., 2008, vol. 74, no. 11, pp. 22–26.
Agafonov, I.L. and Devyatykh, G.G., Mass-spektrometricheskii analiz gazov i parov osoboi chistoty (Mass Spectrometric Analysis of Extrapure Gases and Vapors), Moscow: Nauka, 1980.
Krylov, V.A., Sorochkina, T.G., Bulanov, A.V., and Lashkov, A.Yu., C1–C4 hydrocarbon release in the preparation of SiF4 through Na2SiF6 pyrolysis, Inorg. Mater., 2012, vol. 48, no. 1, pp. 7–9.
Author information
Authors and Affiliations
Corresponding author
Additional information
Original Russian Text © T.G. Sorochkina, A.D. Bulanov, A.Yu. Sozin, O.Yu. Chernova, 2017, published in Neorganicheskie Materialy, 2017, Vol. 53, No. 12, pp. 1331–1336.
Rights and permissions
About this article
Cite this article
Sorochkina, T.G., Bulanov, A.D., Sozin, A.Y. et al. Impurity composition of monoisotopic 28SiF4 silicon tetrafluoride. Inorg Mater 53, 1300–1306 (2017). https://doi.org/10.1134/S0020168517120160
Received:
Published:
Issue Date:
DOI: https://doi.org/10.1134/S0020168517120160