岩矿测试

文章摘要

许春雪,王亚平,张旭,董波,孙德忠,安子怡.矽线石成分分析标准物质研制[J].岩矿测试,2017,36(4):396-404

XU Chun-xue,WANG Ya-ping,ZHANG Xu,DONG Bo,SUN De-zhong,AN Zi-yi.Preparation of Certified Reference Materials of Sillimanite for Chemical Composition Analysis[J].Rock and Mineral Analysis,2017,36(4):396-404.DOI:10.15898/j.cnki.11-2131/td.201608190123

矽线石成分分析标准物质研制

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Preparation of Certified Reference Materials of Sillimanite for Chemical Composition Analysis

投稿时间：2016-08-19 修订日期：2017-02-15

DOI：10.15898/j.cnki.11-2131/td.201608190123

中文关键词: 矽线石成分分析物相分析标准物质标准值

英文关键词: sillimanite chemical composition analysis phase analysis reference material certified value

基金项目:中国地质调查局地质调查项目（DD20160095）；国土资源公益性行业科研专项（200911044-02）

作者	单位	E-mail
许春雪	国家地质实验测试中心, 北京 100037
王亚平	国家地质实验测试中心, 北京 100037	wypsm@yeah.net
张旭	黑龙江省地质矿产测试应用研究所, 黑龙江哈尔滨 150036
董波	黑龙江省地质矿产测试应用研究所, 黑龙江哈尔滨 150036
孙德忠	国家地质实验测试中心, 北京 100037
安子怡	国家地质实验测试中心, 北京 100037

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中文摘要:

随着矽线石应用领域的逐步拓展，英国、南非和日本等国家已研制了4种矽线石标准物质，而我国仅有一种矽线石国家二级标准物质，无论从组分的浓度梯度范围还是定值指标等方面，均难以满足我国研究需求。本文针对我国矽线石的分布情况，在黑龙江林口县和河南内乡县采集典型矽线石原矿2种，在黑龙江林口县采集矽线石精矿1种，按照国家一级标准物质研制标准和规范要求，研制了3种矽线石成分分析国家一级标准物质（批准编号为GBW07843、GBW07844、GBW07845）。均匀性检验结果表明，除个别指标（Y-1的TFe₂O₃、Cu和J-1的MnO等）外，3种标准物质检测指标的F值均小于临界值F_{0.05（24，25）}=1.96，组内和组间无明显差异；Y-1的TFe₂O₃、Cu和J-1的MnO等指标的组内和组间差异主要来源于分析方法误差，由此表明此批标准物质均匀性良好。在14个月考察期内，3种标准物质计算得到的拟合直线斜率b₁均不显著，表明3种标准物质有较好的稳定性。经我国10家实验室使用多种分析方法对矿石中的主量元素、痕量元素和矽线石含量（硅铝，SAl₂O₃）等共计39种组分联合定值，各组分的相对扩展不确定度处于0.60%~29.9%区间，3种矽线石标准物质主量成分Al₂O₃的含量分别为25.85%、28.16%和55.06%。该系列矽线石标准物质可满足地质、环境等研究领域相关样品分析质量监控工作的需求。

英文摘要:

With an increasing utilization of sillimanite, some reference materials of sillimanite for chemical composition have been developed in countries such as the UK, South Africa and Japan. In China, there is only one national secondary standard material for chemical compositon of sillimanite. It is difficult to meet the research needs of the country in terms of the concentration gradient range and the value index. For this study, two sillimanite ores were collected from Linkou county in Heilongjiang and Leijiang county in Henan, and one sillimanite concentrate was collected from Linkou county in Heilongjiang. According to national primary reference materials specifications, 3 sillimanite CRMs have been developed and approved as national standard reference materials (GBW07843, GBW07844, GBW07845). For the homogeneity test, the calculated F values in 3 sillimanite CRMs obtained by analysis of variance (ANOVA) were less than the critical F values at the 95% confidence level, with the exception of TFe₂O₃ and Cu in Y-1, and MnO in J-1, indicating no obvious differences between units and within units. The differences of TFe₂O₃ and Cu in Y-1 and MnO in J-1 between units and within units resulted from the error in the analytical methods. The results showed that 3 sillimanite CRMs had good homogeneity. The calculated test statistic b₁ of 3 sillimanite CRMs during the 14-month observation period was statistically insignificant, indicating that 3 sillimanite CRMs were stable. 10 qualified laboratories were selected to give certified values and uncertainties of 39 components, including major elements, trace elements and sillimanite phases in ores. The relative expanded uncertainties of 39 components range from 0.60% to 29.9%. The content of Al₂O₃ in sillimanite reference materials is 25.85%, 28.16%, 55.06% for GBW07843, GBW07844, and GBW07845, respectively. 3 sillimanite CRMs meet the monitoring requirements of chemical composition analysis for sillimanite samples in geology and environment fields.

主管单位：	中国科学技术协会
主办单位：	中国地质学会岩矿测试技术专业委员会国家地质实验测试中心