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| he Sample Preparation Method for the Determination of Si Isotopic Abundances Ratios using Gas-source Mass-spectrometry |
| LI Hong1,YI Hong2,ZHANG Jing-chang1,YI Wei3 |
1. College of Science, Beijing University of Chemical Technology, Beijing 100029, China
2. National Institute of Metrology, Beijing 100013, China
3. The Hong Kong University of Science and Technology, Kowloon, Hong Kong, China |
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Abstract The development of sample preparation for the determination of Si isotopic abundances ratios with gas-source mass-spectrometry is introduced.The single crystal silicon is converted to SiO2 based on alkaline solution digestion followed by cation-exchange column and calcinating at 850 ℃.After dissolving SiO2 with HF acid, H2SiF6 solution is obtained .BaSiF6 precipitation is formed by drop adding BaCl2 solution.Then BaSiF6 is decomposed to SiF4 and Si isotope ratios is measured by gas-source mass-spectrometry.By Optimizing the sample preparation procedure,high recovery SiF4 gas is obtained.The results indicate that the sample preparation method for the determination of Si isotopic abundances ratios has high repeatability and recovery, meeting the requirement for the accurate measurement of silicon molar mass.
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［1］易洪.阿伏加德罗常数测定的新进展［J］.计量学报, 2007,28(4):394-399.
［2］Fujii Kenichi,Waseda Atsushi,Kuramoto Naoki,et al. Present State of the Avogadro Constant Determination from Silicon Crystals with Natural Isotopic Compositions［J］. IEEE Trans on IM, 2005,54(2):854-859.
［3］Becker P.History and progress in the accurate determination of the Avogadro constant ［J］.Rep Prog Phys, 2001, 64(12):1945-2008.
［4］Engstrm E,Rodushkin I,Baxter D C,et al.Chromatographic Purification for the Determination of Dissolved Silicon Isotopic Compositions in Natural Waters by High-resolution Multicollector Inductively Coupled Plasma Mass Spectrometry［J］.Analytical Chemistry IB,2006,78(1):250-257.
［5］Georg R B, Reynolds B C, Frank M, et al. New sample preparation techniques for the determination of Si isotopic compositions using MC-ICPMS［J］.Chem Geol, 2006,235(1-2):95-104.
［6］Bièvre P D,Lenaers G,Murphy T , et al.The chemical preparation and characterization of specimens for “absolute” measurement of the molar mass of an element, exemplified by silicon, for redeterminations of the Avogadro constant［J］.Metrologia, 1995, 32(2):103-110.
［7］Bièvre D P,Valkiers S. Molar mass determinations for NA(Avogadro) Projects: Present status and potential for the future［J］.Metrologia,1994,31(3):245-249.
［8］丁悌平,万德芳,李金城,等.硅同位素测量方法及其地质应用［J］.矿床地质,1988,7(4): 90-95.
［9］Ding T P, Ma G R, Shui M X, et al.Silicon isotope study on rice plants from the Zhejiang province ［J］.China Chem Geol,2005,218(1-2):41-50.
［10］Inkret Monika, Valkiers Staf, Berglund Michael, et al.Optimization of the Sample Preparation Procedure for the Conversion of Enriched 28Si Single Crystal to Enriched Gaseous 28SiF4［J］.Acta Chim Slov, 2008,55(2):294-301. |
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2011, Vol. 32 
