摘要
样品的均匀性和稳定性研究是标准物质研制过程中非常重要的环节之一。按照一级标准物质均匀性和稳定性的相关要求,在研制黑色页岩贵金属成分分析标准物质时,对标准物质候选物开展了均匀性和稳定性研究。对标准物质候选物的Au、Ag、Pt、Pd、Rh、Ir、Os、Ru等8个贵金属定值元素进行了均匀性检验,经单因素方差分析法统计,所有元素的F实测值均低于F临界值,表明样品均匀;考察了样品在低温-20℃及高温60℃极端条件下和在运输过程的短期稳定性,结果保持一致;在21个月内先密后疏共分5个时间点对样品各定值元素和易变成分进行了检测,通过单因素方差分析法检验,F实测值均小于理论值,表明考察期内特性量值均能保持稳定。研制的黑色页岩贵金属成分分析标准物质均匀性和稳定性满足标准物质研制的要求。通过稳定性评估,对本标准物质的稳定性定为5 a。
The study of homogeneity and stability of samples is one of the most important links in the research and development of reference materials.According to the requirements of homogeneity and stability of the first-class certified reference materials,the homogeneity and stability of reference material candidates for the analysis of the precious metal composition of black shale were studied in this paper.The homogeneity test of 8 precious metal valuation elements(Au,Ag,Pt,Pd,Rh,Ir,Os,Ru)of the reference material candidates was carried out,the measured F values of all elements were lower than the F theoretical critical value by single factor analysis of variance,which indicated that the samples were homogeneous;the short-term stabilities of the samples under the extreme conditions of low temperature-20℃and high temperature-60℃and during transportation were investigated,and the results were consistent;in 21 months,the valuation elements and variable components of the samples were tested at 5 time points,the frequency of which is carried out dense at first and scattered after,and through one-way variance test,the measured F value is less than the theoretical value,the results indicating that the values of the characteristic parameters were stable during the investigation period.The homogeneity and stability of the prepared reference material for the analysis of the precious metal composition of black shale meet the research and development requirements for reference materials.Through the stability evaluation,the stability of this reference material is defined as 5 a.
作者
颜芝
夏彬涵
王芦越
唐艺秋
宋祖光
Yan Zhi;Xia Binhan;Wang Luyue;Tang Yiqiu;Song Zuguang(Geological Disaster Prevention Center of Henan Geological Bureau;Key Laboratory of Precious Metals Analysis and Exploration Technology,Ministry of Natural Resources;Henan Vocational College of Geology and Mining)
出处
《黄金》
CAS
2023年第10期100-105,共6页
Gold
基金
国家重点研发计划项目(2016YFF020110311)。
关键词
黑色页岩
贵金属
标准物质
均匀性
稳定性
black shale
precious metals
reference material
homogeneity
stability