电感耦合等离子体质谱(ICP-MS)法测定金绿宝石中16种痕量稀土元素  

Determination of Sixteen Trace Rare Earth Elements in Chrysoberyl by Inductively Coupled Plasma Mass Spectrometry with Alkaline Fusion

作　　者：刘闫 姚明星[1,2,3] 樊蕾 孙启亮 毛香菊 张丽萍[1,2,3] LIU Yan;YAO Mingxing;FAN Lei;SUN Qiliang;MAO Xiangju;ZHANG Liping(Zhengzhou Institute of Multipurpose Utilization of Mineral Resources,CAGS,Zhengzhou,Henan 450006,China;Key Laboratory for Polymetallic Ores’Evaluation and Utilization,MNR,Zhengzhou,Henan 450006,China;Key Laboratory of Comprehensive Utilization of Gold Resource in Henan Province,Zhengzhou,Henan 450006,China)

机构地区：[1]中国地质科学院郑州矿产综合利用研究所,郑州450006 [2]国家非金属矿资源综合利用工程技术研究中心,郑州450006 [3]河南省黄金资源综合利用重点实验室,郑州450006

出　　处：《中国无机分析化学》2023年第3期234-239,共6页Chinese Journal of Inorganic Analytical Chemistry

基　　金：国家自然科学基金资助项目(22106148)。

摘　　要：金绿宝石结构稳定,常规敞开酸溶、密闭酸溶、微波消解三种前处理方法并不能将其完全分解,使得测定结果偏低。采用碳酸钠-硼酸混合熔剂进行熔融,样品分解完全,通过优化熔融温度与时间、熔剂用量与配比,建立了电感耦合等离子体质谱(ICP-MS)法测定金绿宝石中16种痕量稀土元素的分析方法。选择丰度高、干扰小的同位素、动能歧视碰撞池(KED)模式及干扰系数校正法消除质谱干扰,以185Re为内标元素及样品稀释降低基体干扰。实验表明,各稀土元素的校准曲线相关系数r值在0.999 1~0.999 8,方法检出限为0.000 1~0.013μg/g,定量限为0.000 5~0.067μg/g。采用国家标准物质GBW07151验证方法的精密度,计算出相对标准偏差(RSD,n=7)在1.3%~4.6%,并将方法用于金绿宝石实际样品中稀土元素的测定,RSD为0.90%~3.2%,加标回收率为94.0%~104%,符合国家地质矿产行业标准允许范围,结果稳定、可靠。Chrysoberyl is stable in structure and cannot be completely decomposed by conventional three pretreatment methods of the open acid solution, closed acid solution, and microwave digestion.The determination result is lower than actual value.In this paper, sodium carbonate-boric acid mixed flux is used to decompose chrysoberyl completely.The melting temperature and time, flux dosage, and ratio are optimized.A method for the determination of sixteen trace rare earth elements in chrysoberyl by inductively coupled plasma mass spectrometry(ICP-MS) is established.Isotopes with high abundance and low disturbance, kinetic energy discriminate against collision pool mode(KED) and interference coefficient correction method are selected to eliminate the interference of mass spectrometry.Standard internal method based on185Re and sample dilution is used to reduce the matrix interference.The results show that the correlation coefficient of calibration curves of rare earth elements ranges from 0.999 1 to 0.999 8.The method detection limit is between 0.000 1 and 0.013 μg/g, and the quantitative limit is between 0.000 5 and 0.067 μg/g.The national standard substance GBW07151 is used to verify the precision of the method.The calculated relative standard deviation(RSD,n=7) is between 1.3% and 4.6%.Moreover, the method is applied to the determination of rare earth elements in chrysoberyl actual samples.RSD is from 0.90% to 3.2% and the recoveries are 94.0%—104%.It is in line with the allowable range of the national geological and mineral industry standard, and the result is stable and reliable.

关 键 词：金绿宝石 稀土元素 碳酸钠 硼酸 电感耦合等离子体质谱法 动能歧视碰撞池模式 

分 类 号：O657.63[理学—分析化学] TH843[理学—化学]