黑色页岩样品中痕量级铂族元素地球化学成分标准物质研制

介绍了黑色页岩样品中6个铂族元素铂、钯、钌、锇、铑、铱的标准物质研制过程。黑色页岩样品采自贵州黄家湾,为一次采集、一次混样的原始样品,随机抽取包装好后的样品进行检验与定值。均匀性、稳定性符合要求后,按照国际标准化组织(ISO)34、35指南的基本要求和我国一级标准物质的技术规范,采用多个实验室协同测试的定值方式,利用不同原理的分析方法对此样品的6个铂族元素进行定值。以各实验室组数据作为最小统计单元,用Grubbs准则、Dixon法检验剔除离群数据,Shapiro-Wilk法检验各元素数据分布的正态性。检验结果100%的元素呈正态或近似正态分布。定值的6个元素均符合标准值水平。

Preparation of Geochemical Standard Reference Black Shale Samples for Trace Platinum Group Element Analysis

A geochemical certified reference black shale sample for trace platinum group elements(PGEs) analysis was prepared.The original black shale sample was collected from Huangjiawan in Guizhou province.The sample was prepared to grain size of 74 μm through the primary crushing and fine grinding.The samples which had passed through the granularity examination,the homogeneity examination and the stable examination were distributed to 11 national authority geological laboratories for six PGEs(Pt,Pd,Ru,Os,Rh,Ir) analysis based on the basic requirements of ISO GUIDE 34,ISO GUIDE 35 and 《The National Technical Specifications for Preparation of Primary Standard Reference Materials》.Six analytical methods with different principles were used for the certification.In the certification,each set of the data from the laboratories was regarded as the smallest statistical unit.Grubbs criteria and Dixon′s method were used for analytical data processing and Shapiro-Wilk method was used for testing the normality of the element distribution.The results from the tests showed that 100% of certified values of six PGEs presented the normal distribution or near-normal distribution and were in accordance with the quality requirements of the standards.