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中国无机分析化学:2022,12(2):46-51
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四酸消解-电感耦合等离子体质谱(ICP-MS)法测定磷矿石中的8种微量重金属元素
郭振华
(中化地质矿山总局地质研究院实验应用研究中心)
Determination of 8 Trace Elements in Phosphate Ores by ICP-MS with Four Mixed Acid Digestion
GUO Zhenhua
(Experimental Application Research Center,China Chemical Geology and Mining Bureau)
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投稿时间:2021-06-11    修订日期:2021-06-22
中文摘要: 本文研究提出了一种混合四酸(硝酸-氢氟酸-高氯酸-硫酸)分解体系,解决了传统四酸(盐酸-硝酸-氢氟酸-高氯酸)或三酸(硝酸-氢氟酸-高氯酸)溶矿耗酸量大、部分元素溶解不完全等缺点。建立了四酸敞口分解-电感耦合等离子质谱法同时测定磷矿样品中钨、钼、铊、镉、铋、铀、钍、铬等8种微量元素的方法,结果和经典碱溶法比对,准确度满意。讨论了分解方法对易挥发元素、难溶元素的影响,选取了合适的分析同位素及采用干扰校正方程以消除质谱干扰,利用103Rh和186Re为内标元素,有效校正了分析信号的动态漂移,方法的检出限为0.010~0.35μg /g、精密度均小于6%、加标回收率在93.4%~108%间。在不增加分析成本的情况下,一份溶液还可以同时用于ICP-OES及ICP-MS法测定其它主量及微量元素,方法简单、快捷、实用,适合推广应用。
Abstract:This article researches and proposes a mixed four acid (nitric acid-hydrofluoric acid-perchloric acid-sulfuric acid) decomposition system, which is compared with traditional four acid (hydrochloric acid-nitric acid-hydrofluoric acid-perchloric acid) or three acid (nitric acid-hydrogen Fluoric acid-perchloric acid) decomposition system has the advantages of less acid, no need to add in batches, and more complete decomposition of elements. A method for the simultaneous determination of tungsten, molybdenum, thallium, cadmium, bismuth, uranium, thorium, and chromium in phosphate rock samples by tetraacid open decomposition-inductively coupled plasma mass spectrometry was established, and the results were compared with the classic alkaline solution method. , Satisfactory accuracy. The effect of decomposition methods on volatile and insoluble elements was discussed. Appropriate analytical isotopes were selected and interference correction equations were used to eliminate mass interference. Using 103Rh and 186Re as internal standard elements, the dynamic drift of the analysis signal was effectively corrected. The detection limit is 0.010~0.35μg/g、 the precision is less than 6%, and the recovery rate of standard addition is between 93.4%~108%. Without increasing the analysis cost, a solution can also be used for the determination of other major and trace elements by ICP-OES and ICP-MS at the same time. The method is simple, fast, practical, and suitable for popularization and application.
文章编号:     中图分类号:O657.63    文献标志码:
基金项目:化工矿产资源测试技术和标准研究团队、中国地质调查局项目“福建浦城地区战略性萤石硼资源调查(DD20190816)资助”
引用文本:
郭振华.四酸消解-电感耦合等离子体质谱(ICP-MS)法测定磷矿石中的8种微量重金属元素[J].中国无机分析化学,2022,12(2):46-51.
GUO Zhenhua.Determination of 8 Trace Elements in Phosphate Ores by ICP-MS with Four Mixed Acid Digestion[J].Chinese Journal of Inorganic Analytical Chemistry,2022,12(2):46-51.

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