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《化学分析计量》 2020年第01期
DOI:10.3969/j.issn.1008-6145.2020.01.008
电感耦合等离子体质谱法测定煤矸石中微量锗和镓
王小强,梁倩,姚永生,余文丽,赵亚男,朱尧伟
(河南省有色金属地质勘查总院,河南省有色金属深部找矿勘查技术研究重点实验室,河南省有色金属地质矿产局联合实验室,郑州 450052) 
Determination of micro-amounts of germanium and gallium in coal gangue by inductively coupled plasma mass spectrometry
WANG Xiaoqiang, LIANG Qian, YAO Yongsheng, YU Wenli, ZHAO Yanan, ZHU Yaowei
(General Institute for Non-ferrous Metals and Geological Exploration of Henan Province, Key Laboratory of Deep Ore-prospecting Technology Research for Non-ferrous Metals of Henan Province, Joint Laboratory of Henan Province Non-ferrous Metals Geological and Mineral Resources Bureau, Zhengzhou 450052, China) 
摘要:建立了测定煤矸石中微量锗和镓的电感耦合等离子体质谱法。煤矸石试样经高温灰化,用硝酸-氢氟酸- 高氯酸-磷酸分解,以电感耦合等离子体质谱法测定其中的锗和镓。通过在线三通加入内标元素铑,消除非质谱干扰; 通过选择干扰元素的异质同位素进行定量测定,采用数学公式在线校正,消除质谱干扰。与分光光度法进行比对,锗、 镓测定结果的相对偏差为-0.63%~0.28%。克服了常规化学分析方法步骤繁琐、耗时长、工作量大的不足。该法测定 结果的相对标准偏差小于3%(n=6),加标回收率为97.4%~102.5%。该方法具有检出限低、快速、简便、线性范围宽、 多元素同时测定等优点,分析误差满足化学分析法的要求,可用于煤矸石中锗和镓的测定。 
Abstract:A method of inductively coupled plasma mass spectrometry (ICP-MS) was established to determine microamount of germanium and gallium in coal gangue. After high temperature ashing, coal gangue samples were decomposed by HNO3-HF-HClO4-H3PO4 mixed acid, micro-amounts of germanium and gallium in sample solutions were directly determined by ICP-MS. The non-mass spectrum interference was eliminated by adding internal standard element rhodium into the on-line tee; the heterogeneous isotopes of interfering elements were selected for quantitative determination, and the mathematical formula was used for on-line correction to eliminate mass spectrum interference. The relative deviation of germanium and gallium was between -0.63% and 0.28% by comparison with spectrophotometry. The method overcomes the cumbersome procedure, time consuming, heavy workload of the conventional chemical analysis methods. The relative standard deviation was less than 3%(n=6), and the recovery of standard addition was 97.4%-102.5%. The method has the advantages of low detection limit, rapidity, simplicity, wide linear range and simultaneous determination of multiple elements. The analysis error meets the requirements of chemical analysis method and it is suitable for the determination of germanium and gallium in coal gangue. 
关键词:煤矸石;锗;镓;电感耦合等离子体质谱法 
Keywords:coal gangue; germanium; gallium; inductively coupled plasma mass spectrometry 
基金:河南省2016 年度“两权价款”地质科研项目(2015199203) 
本文引用格式:
王小强,梁倩,姚永生,等. 电感耦合等离子体质谱法测定煤矸石中微量锗和镓[J]. 化学分析计量,2020,29(1):31-34.
WANG X Q,LIANG Q,YAO Y S,et al. Determination of micro-amounts of germanium and gallium in coal gangue by inductively coupled plasma mass spectrometry[J]. Chemical analysis and meterage,2020,29(1):31-34. 

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