海泡石化学成分分析标准物质研制

海泡石是一种十分重要的非金属矿,被广泛应用于航空、畜牧、化工环保等领域中,贸易活动十分活跃。鉴于中国一直没有海泡石标准物质,国际上的海泡石标准物质定值组分少,为了满足相关研究需求,本文研制了湖南湘潭的海泡石标准物质（GBW07138）。对Ba、Be、Bi、Cd、Ce、Co、Cr、Cs、La、Li、Lu、U、Nb、Nd、Ni、Pb、SiO₂、Al₂O₃、Fe₂O₃、MgO、CaO、Na₂O、K₂O、TiO₂共24种组分进行均匀性和稳定性检验。针对不同含量、不同性质的组分,采用合理的国家标准方法检验了20种组分的RSD小于3%,其余4种组分Bi、La、Lu、Mo的RSD略大于3%,方差检验的F值均小于列表临界值F_0.05（29,60）=1.65],表明该标准物质均匀性良好。在稳定性考察期内,24种组分的含量无统计学上的明显变化,表明该标准物质稳定性良好。由9家实验室采用重量法、容量法、X射线荧光光谱法、电感耦合等离子体质谱法等传统化学分析方法和现代仪器分析方法协作定值,最终定值组分63种,涵盖了主量、微量及全部稀土元素,其中海泡石特征组分MgO和烧失量（LOI）的含量分别为18%±0.2%和8.55%±0.19%,这两种组分与现有的标准物质形成一定阶梯性,能够更好地满足海泡石成分分析测试需求。该海泡石标准物质可用于地质找矿、地球化学调查、地质矿产产品测试以及其他行业相关领域样品测试的质量监控标准。而且在研制该标准物质过程中,改良或开发的一些新方法可为后续开发海泡石标准物质提供技术支持。

Preparation of Sepiolite Reference Material for Chemical Composition Analysis

BACKGROUND: Sepiolite is a very important non-metallic mineral, which is widely used in aviation, animal husbandry, the chemical industry, environmental protection and other fields. Sepiolite is in great demand and needs a lot of analysis and testing. However, the existing sepiolite reference materials are inadequate and do not satisfy the needs of sepiolite composition analysis. Furthermore, there are no sepiolite reference materials in China, making it necessary to develop one.OBJECTIVES: To prepare a reference material for composition analysis of sepiolite whose certified value components cover as many elements as possible.METHODS: Sepiolite samples were collected from Xiangtan, Hunan Province. The samples were subjected to primary crushing, coarse-grain sieving, inactivation, fine grinding and fine grain sieving. After passing the initial inspection, samples were bottled and numbered. Random samples were taken for homogeneity test, stability test. 24 components were selected for homogeneity and stability test.RESULTS: The results showed that the RSD of 20 components were less than 3%, and the F value of the variance test was less than the critical value of the listF_0.05(29, 60)=1.65], indicating that the homogeneity of the reference material was good. During the investigation period, the contents of 24 components had no significant change, indicating that the standard material was stable. Nine laboratories cooperated with traditional chemical analysis methods and modern instrumental analysis methods to determine the value. The final values were 63 components, covering major, trace and all rare earth elements. The contents of characteristic components MgO and LOI were 18% and 8.55%, respectively. These two components form a certain ladder with the existing reference materials, which can better satisfy the requirements of sepiolite composition analysis.CONCLUSIONS: The developed sepiolite reference material can be used as the quality control standards for geological prospecting, geochemical investigation and testing of geological and mineral products, as well as for other industries to analyze similar materials. Moreover, in the process of developing the reference material, improvements and developments to the new methods will provide technical support for the subsequent development of the sepiolite reference material.