Glow Discharge Mass Spectrometric Determination of 24 Impurity Elements in Pure Tin and Elimination of Memory Effect of Tin
摘 要
采用辉光放电质谱法(GDMS)测定了纯锡中24种杂质元素,分析方法为无标定量分析。分析前纯锡样品须依次用乙醇、水及乙醇冲洗以除去表面的灰尘颗粒,凉干后用于分析。本工作对辉光放电过程中的三项关键因素,即辉光放电电压、放电电流及放电气流三者在辉光放电溅射/电离时的相互关系及其对总离子流强度的影响进行了试验和讨论,并确定了仪器在最佳状态时辉光放电的优化条件为:放电电压590 V,放电电流30 mA,放电气流450 mL·min-1。为排除各元素测定中质谱(MS)干扰的影响,选择了在不同的分辨模式(中/高)下用相对丰度较高、干扰较少的质量数进行分析。所测定元素测定结果的相对标准偏差(n=5)均小于15%。各元素的检出限(3s)为0.003~0.174 μg·g-1之间。本方法所得测定结果与电感耦合等离子体原子发射光谱法(ICP-AES)或电感耦合等离子体质谱法(ICP-MS)的测定结果基本一致。经试验,通过更换GDMS的阳极帽、导流管、采样锥和透镜等4种耗材,可完全消除锡的记忆效应。
Abstract
Glow discharge mass spectrometry (GDMS) was applied to the determination of 24 impurity elements in pure tin, with quantification without reference standards. The pure tin sample should be washed with ethanol, water and ethanol again in succession to remove dust particles from its surface, and then be air-dried before used for analysis. The inter-relationship among the 3 key influential factors, i.e., the voltage, current and gas-flow of glow discharge, and their influences to the intensity of total ionization current during the process of glow discharge supttering and ionization were tested and discussed in this work. And the optimized conditions of glow discharge, under which the GDMS instrument behaved its best state, were found as follows:voltage of 590 V, current of 30 mA and gas flow of 450 mL·min-1. Mass numbers with higher relative abundance and with less interference under different resolution modes (middle or high) were selected for the analysis, to eliminate the influence of MS interferences in the determination of the impurity elements. Values of RSDs (n=5) found for the elements determined were all less than 15%. Detection limits (3s) found for the 24 elements were in the range of 0.003-0.174 μg·g-1. The analytical results of the elements determined by the present method were found in consistency basically with those found by ICP-AES or ICP-MS. It was shown by the testing result that the memory effect of tin was completely eliminated by renewing 4 of the easy-consumable spares of the instrument, i.e., the anode cap, the current duct, the sampling cone and the lens.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202003011
所属栏目 工作简报
基金项目 中国钢研科技集团有限公司青年创新专项基金(ZNCS098)
收稿日期 2019/7/10
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备注侯艳霞,博士研究生,主要从事金属材料测试方法的研究工作
引用该论文: HOU Yanxia,LIU Xiaobo,YANG Guowu,LI Xiaojia,HU Jingyu. Glow Discharge Mass Spectrometric Determination of 24 Impurity Elements in Pure Tin and Elimination of Memory Effect of Tin[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(3): 315~319
侯艳霞,刘晓波,杨国武,李小佳,胡净宇. 辉光放电质谱法测定纯锡中24种杂质元素和锡记忆效应的消除[J]. 理化检验-化学分册, 2020, 56(3): 315~319
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参考文献
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【3】王光灿,朱光辉,彭莉,等.ICP-AES同时测定高纯锡中的8种微量杂质元素[J].云南大学学报(自然科学版), 1999,21:96-97.
【4】金智宏.氯化分离-ICP-MS法测定高纯锡中的杂质元素Pb[J].湖南有色金属, 2008,24(5):59-61.
【5】魏建军,郎春燕,林龙飞,等.溴化分离-电感耦合等离子体质谱法测定高纯锡中的16种杂质元素[J].分析化学, 2013,41(6):927-930.
【6】王涛.石墨炉原子吸收法测定高纯锡中的杂质元素[J].山东冶金, 2000,22(5):58-59.
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【8】YU X, LI X J, WANG H Z. Interference correction in analysis of stainless steel and multi-element determination by glow discharge quadrupole mass spectrometry[J]. International Journal of Mass Spectrometry, 2007,262:25-32.
【9】VIETH, JOHN W, HUNEKE J C. Relative sensitivity factors in glow discharge mass spectrometry[J]. Spectrochimica Acta Part B:Atomic Spectroscopy, 1991,46(2):137-153.
【10】GANEEV A A, GUBAL A R, USKOV K N, et al. Analytical glow discharge mass spectrometry[J]. Russian Chemcial Bulletin, 2012,61(4):752-767.
【11】魏兴俭,王丽萍,秦震,等.辉光放电质谱法相对灵敏度因子影响因素研究[J].质谱学报, 2016,37(4):343-350.
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