电感耦合等离子体质谱(ICP-MS)法测定炭质页岩中的钨钼钪

Determination of Tungsten,Molybdenum and Scandium in Carbon Shale by Inductively Coupled Plasma Mass Spectrometry

炭质页岩中含有大量的炭化有机质,其中钨钼在单一盐酸溶液中易水解,样品的完全消解及有效防止钨酸、钼酸的形成是准确测定炭质页岩中钨、钼和钪含量的关键。采用HCl-HF-HNO3-HClO4四酸体系消解样品,加盖形成蒸气回流;采用酒石酸-盐酸体系浸取,有效防止钨酸、钼酸沉淀导致结果偏低问题。建立了电感耦合等离子体质谱(ICP-MS)法测定炭质页岩中的钨、钼、钪的分析方法。测定结果表明,各元素在0.01~200.0μg/L范围内线性关系良好,相关系数均在0.9999以上,方法检出限为0.011~0.045μg/g。按照实验方法测定炭质页岩中的钨、钼、钪,结果的相对标准偏差(RSD,n=11)为0.77%~2.6%,加标回收率在94.0%~107%。能满足炭质页岩中钨、钼和钪含量的测定。

Carbon shale contains a large amount of carbonized organic matter,in which molybdenum and tungsten are easily hydrolyzed in a single hydrochloric acid solution.The complete digestion of samples and the prevention of formation of tungstic acid and molybdic acid are the keys for accurate determination of tungsten,molybdenum and scandium in carbonaceous shale.In this paper,the samples were digested with HCl-HF-HNO3-HClO4,and capped to form a steam reflux.Using tartaric acid-hydrochloric acid system leaching,can effective prevent precipitation of tungstic acid and molybdic acid resulting in low results.A method for the determination of tungsten,molybdenum and scandium in carbonaceous shale by inductively coupled plasma mass spectrometry(ICP-MS)was established.The determination results show that the linear relationship of each element is good in the range of 0.01—200.0μg/L,the correlation coefficient is above 0.9999,and the detection risk of the method is 0.011—0.045μg/g.The relative standard deviation(RSD,n=11)was 0.77%—2.6%,and the recovery was 94.0%—107%.The method can be used to determine the contents of tungsten,molybdenum and scandium in carbon shale.