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投稿时间:2021-01-06 修订日期:2021-01-12
投稿时间:2021-01-06 修订日期:2021-01-12
中文摘要: 炭质页岩中含有大量的炭化有机质,其中的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。本文采用HCl-HF-HNO3-HClO4四酸体系消解,加盖形成蒸汽回流;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法(ICP-MS)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0.01~200.0 μg/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0.011~0.045 μg/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 %~107% 之间。
中文关键词: HCl-HF-HNO3-HClO4 电感耦合等离子体质谱法(ICP-MS) 炭质页岩 钨 钼 钪
Abstract:Carbon shale contains a large amount of carbonized organic matter, the molybdenum and tungsten are easily hydrolyzed in a single hydrochloric acid solution, and The complete digestion of samples and the prevention of formation of tungstic acid and molybdic acid are the keys to the accurate determination of tungsten, Molybdenum and scandium in carbonaceous shale.
In this paper, HF-HNO3-HClO4 was added to cover the digestion. The formation of steam reflux, complete solution sample, using tartaric acid-hydrochloric acid system leaching, effective prevention of 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 ~ 200.0 μg/L, the correlation coefficient is above 0.9999, and the detection risk of the method is 0.011~0.045 μg/g. The relative standard deviation (RSD, n=11) was 0.77% ~ 2.6%, and the recovery rate was 94 %~107%.
keywords: HCl-HF-HNO3-HClO4 Inductively coupled plasma mass spectrometry (ICP-MS) Carbonaceous shale W Mo Sc
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基金项目:广西科学研究与技术开发计划项目(桂科AD18126020);中国有色桂林矿产地质研究院有限公司创新(KDY2017007);广西自然科学基金(2020GXNSFAA159139)
引用文本:
张征莲,施意华,唐碧玉,古行乾,李学彪.电感耦合等离子体质谱法测定炭质页岩中的钨钼钪[J].中国无机分析化学,2021,11(4):39-44.
ZHANG Zheng-lian,SHI Yi-hua,TANG Bi-yu,GU Xing-qian,LI Xue-biao.Determination of Tungsten, Molybdenum and Scandium in Carbon Shale by Inductively Coupled Plasma Mass Spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2021,11(4):39-44.
张征莲,施意华,唐碧玉,古行乾,李学彪.电感耦合等离子体质谱法测定炭质页岩中的钨钼钪[J].中国无机分析化学,2021,11(4):39-44.
ZHANG Zheng-lian,SHI Yi-hua,TANG Bi-yu,GU Xing-qian,LI Xue-biao.Determination of Tungsten, Molybdenum and Scandium in Carbon Shale by Inductively Coupled Plasma Mass Spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2021,11(4):39-44.