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文章摘要
杨小莉,杨小丽,李小丹,邵鑫,杨梅.敞开酸溶-电感耦合等离子体质谱法同时测定钨矿石和锡矿石中14种微量元素[J].岩矿测试,2014,33(3):321-326
YANG Xiao-li,YANG Xiao-li,LI Xiao-dan,SHAO Xin,YANG Mei.Simultaneous Determination of 14 Trace Elements in and Tin Ore with Open Acid Digestion by Inductively Coupled Plasma-Mass Spectrometry[J].Rock and Mineral Analysis,2014,33(3):321-326.DOI:
敞开酸溶-电感耦合等离子体质谱法同时测定钨矿石和锡矿石中14种微量元素
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Simultaneous Determination of 14 Trace Elements in and Tin Ore with Open Acid Digestion by Inductively Coupled Plasma-Mass Spectrometry
投稿时间:2013-08-16  
DOI:
中文关键词: 钨矿石  锡矿石  微量元素  敞开酸溶  电感耦合等离子体质谱法
英文关键词: tungsten ore  tin ore  trace elements  open acid digestion  Inductively Coupled Plasma-Mass Spectrometry
基金项目:中国地质大调查项目(12120113014700)
作者单位
杨小莉 武汉地质矿产研究所, 湖北 武汉 430205 
杨小丽 武汉地质矿产研究所, 湖北 武汉 430205 
李小丹 武汉地质矿产研究所, 湖北 武汉 430205 
邵鑫 武汉地质矿产研究所, 湖北 武汉 430205 
杨梅 武汉地质矿产研究所, 湖北 武汉 430205 
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中文摘要:
      钨矿石和锡矿石成分复杂,具有丰富的共生或伴生元素。在国家标准方法中,对其中的微量共生或伴生元素含量多采用单元素测定,分析强度大,效率低。本文采用混合酸在敞开体系中消解样品,以 50%盐酸提取盐类,电感耦合等离子体质谱仪同时测定钨矿石和锡矿石中的锂钪铬钴镍铜铅锌铷钼铯锑铋钍等14种微量元素。通过比较碱熔法、盐酸+氢氟酸+硝酸+高氯酸四酸溶矿法、氢氟酸+硝酸+高氯酸三酸溶矿法这三种样品前处理方法,确定选择使用氢氟酸+硝酸+高氯酸三酸溶矿法溶解样品。ICP-MS测定过程中,选择铑和铼作为内标元素,有效监控分析信号的漂移。测定结果表明,各元素的检出限为0.003 ~1.64 μg/g,相对标准偏差在0.1%~3.1%,方法回收率在93.1%~104.3%。方法应用于实际钨矿石和锡矿石分析,测定结果与各元素标准测定值吻合较好。相对于传统处理方法,本法一次溶样,多元素同时测定,使分析效率得到了有效提高,更适合大批量多元素钨矿石和锡矿石样品的分析。
英文摘要:
      Tungsten and tin ores have abundant paragenesis or associated elements with complicated composition. At present, the contents of these trace elements are detected respectively by the national standard methods for tungsten ore and tin ore, which have a great labour intensity and low efficiency. The tungsten ore and tin ore samples were dissolved by mixed acid at normal pressure and extracted by hydrochloric acid (50% HCl), and 14 trace elements of Li, Sc, Cr, Co, Ni, Cu, Pb, Zn, Rb, Mo, Cs, Sb, Bi and Th were simultaneously measured by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). Three sample pre-treatment methods were compared among alkali fusion method, HCl-HNO3-HF-HClO4 method and HNO3-HF-HClO4 method. It was found that the HNO3-HF-HClO4 method is a simple operation and requires fewer reagents than traditional methods, which was chosen to dissolve the tungsten ore and tin ore samples. In the measurement, Rh and Re were selected as the internal standards to compensate for analytical signal drift. The results indicate that the detection limits of this method are 0.003-1.64 μg/g with a relative standard deviation (RSD, n=11) in the range of 0.1%-3.1%. The recovery rates were between 93.1%-104.3%. This method has been verified using practical tungsten and tin ore samples, and the results are in good agreement with the certified values. Comparing with the traditional treatment, this method has improved analysis efficiency, and is more suitable for analysis and detection of tungsten ore and tin ore samples in large batches.
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