| 冷凝回流三酸体系消解—ICP-MS法测定高纯石墨中的痕量杂质元素 |
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| 引用本文： | 贾静,张英新,童坚,李文军.冷凝回流三酸体系消解—ICP-MS法测定高纯石墨中的痕量杂质元素[J].质谱学报,2009,30(4):229-233. |
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| 作者姓名： | 贾静 张英新 童坚 李文军 |
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| 作者单位： | 1. 北京科技大学，应用科学学院化学系，北京 100083；
2. 北京有色金属研究总院，分析测试技术研究所，北京 100088
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| 基金项目： | 国家科技支撑计划项目 |
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| 摘 要： | 建立冷凝回流混合酸消解，ICP-MS法测定高纯石墨中35种痕量元素的方法。采用1 mL HNO3，1 mLHClO4和3 mL H2SO4于220 ℃消解0.2 g 样品，以Sc、Rh、Cs、Re作内标，ICP-MS法测定各元素的方法检出限为0.000 6~0.1 μg?L-1，加标回收率达82%~110%，相对标准偏差（RSD，n=10）为0.58%～5.8%。该方法适用于高纯石墨中痕量杂质含量的测定。
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| 关 键 词： | 冷凝回流 高纯石墨 电感耦合等离子体质谱(ICP-MS) 痕量杂质 |
| 收稿时间： | 2009-02-05 |
Determination of Impurity Elements in High Purity Graphite by ICP-MS after Mixture Acid Digestion in Reflux Condenser System |
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| JIA Jing,ZHANG Ying-xin,TONG Jian,LI Wen-jun.Determination of Impurity Elements in High Purity Graphite by ICP-MS after Mixture Acid Digestion in Reflux Condenser System[J].Journal of Chinese Mass Spectrometry Society,2009,30(4):229-233. |
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| Authors: | JIA Jing ZHANG Ying-xin TONG Jian LI Wen-jun |
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| Affiliation: | 1. Department of Chemistry, University of Science and Technology Beijing, Beijing 100083, China;
2. Beijing General Research Institute for Non Ferrous Metals，Beijing 100088, China
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| Abstract: | The method of determination of 35 trace impurity elements in high purity graphite was established. Samples were digested by the mixture of 1 mL HNO3，1 mL HClO4 and 3 mL H2SO4 at 220 ℃ in reflux condenser system. Sc, Rh, Re and Cs were utilized as internal standards to correct the signal drift. The detection limit of various elements is from 0.000 6 μg?L-1 to 0.1 μg?L-1, the recovery rates are between 82% and 110%, the RSD(n=10) is in the range of 0.58% and 5.8%. The method is suitable for the determination of impurity elements in high purity graphite. |
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| Keywords: | refluxcondense highpuritygraphite inductivelycoupledplasmamassspectrometry(ICP MS) impurityelements |
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