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钛同位素标准溶液研制

Preparation and Certification of A Titanium Isotopic Standard Solution

  • 摘要: 钛同位素组成可用于地球化学和宇宙化学研究中,但目前国内外缺乏钛同位素标准物质。为了满足地质样品钛同位素分析的需要,本文研制了钛同位素标准溶液,报道了钛同位素标准溶液的研制过程和定值结果,包括标准溶液的选择、均匀性和稳定性检验、定值分析及测定数据的统计性检验等。通过初步测定,确定美国Alfa公司生产的Ti单元素溶液作为备选Ti同位素标准溶液。将备选标准溶液分装成150瓶,随机抽取15瓶进行均匀性检验,测试结果的F值均小于临界值,表明备选标准溶液的Ti同位素组成均匀。通过30个月的稳定性检验,标准溶液的特征量值变化在不确定度范围内。采用独家和多家实验室相结合的方法进行定值,标准溶液的特征量值及不确定度推荐为:δ50Ti=-2.23‰±0.14‰,δ49Ti=-1.67‰±0.09‰,δ48Ti=-1.13‰±0.06‰,δ47Ti=-0.57‰±0.05‰。研制的标准溶液可用于钛同位素分析时校正仪器和验证质谱分析过程,有利于不同实验室的测试数据之间的对比和应用。

     

    Abstract: Titanium isotopic compositions have been used to elucidate geochemical and cosmochemical processes. Until now, no Ti isotopic reference material has been reported worldwide, which imposes restriction upon analytical method establishment and laboratory quality control. In this paper, a newly prepared Ti isotopic standard solution is introduced. Ti element standard solution offered by the Alfa Company from U.S.A. was chosen as the starting material, based on the comparison of Ti isotopic measurement results of 3 commercially available Ti element standard solutions. The preparation of the new standard solution was strictly followed using the stipulation on reference material of the metrological technical standard of state, including homogeneity and stability tests, and certification analyses. 150 bottles of the solution were prepared, among which 15 bottles were selected randomly for homogeneity test and no detectable heterogeneity was found by F test. The stability inspection through 30 months indicated no significant changes on δTi values. The certified values and uncertainty at the 95% confidence level were shown to be: δ50Ti=-2.23‰±0.14‰, δ49Ti=-1.67‰±0.09‰,δ48Ti=-1.13‰±0.06‰ andδ47Ti=-0.57‰±0.05‰. This newly certified standard solution can be used to calibrate instruments and verify analytical quality in Ti isotope measurements, and compare inter-laboratory data.

     

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