ICP-MS法测定钼矿石中伴生锂、镓和稀土元素  

Determination of Associated Lithium,Gallium and Rare Earth Elements in Molybdenum Ore by Inductively Coupled Plasma Mass Spectrometry Method

作　　者：梁亚丽 杨珍 阿丽莉[1,2] 贺攀红 孙银生[1,2] LIANG Yali;YANG Zhen;A Lili;HE Panhong;SUN Yinsheng(Henan Province Nuclear Geology,Zhengzhou 450044,China;Henan Nuclear Industry Radioactive Nuclide Test Centre,Zhengzhou 450044,China)

机构地区：[1]河南省核工业地质局,郑州450044 [2]河南省核工业放射性核素检测中心,郑州450044

出　　处：《吉林大学学报（理学版）》2021年第2期427-434,共8页Journal of Jilin University:Science Edition

基　　金：河南省国土资源厅两权价款地质科研项目(批准号:豫国土资函[2016]106号).

摘　　要：通过比较氢氟酸-硝酸高压罐密闭消解法、氢氟酸-硝酸-高氯酸-盐酸低压密闭消解法和氢氟酸-硝酸-高氯酸-盐酸敞口消解法对钼矿样品的分解效果,选用低压密闭消解法制备样品,用电感耦合等离子体质谱(ICP-MS)法测定伴生稀有元素Li,Ga和15种稀土元素的质量比.通过对干扰元素的分析,选择合适同位素,并确定^(151)Eu,^(157)Gd,^(159)Tb质谱干扰的校正系数.结果表明,20μg/L的铑(Rh)标准溶液作为内标可有效抑制溶液中的基体效应和信号动态漂移,方法检出限为0.001~0.113μg/g,相对标准偏差(RSD,n=7)为0.30%~3.92%.经标准物质和实际样品验证,该方法可靠,适合钼矿中伴生Li,Ga和稀土元素的测定.By comparing the digestion effects of hydrofluoric acid-nitric acid high pressure tank closed digestion method,hydrofluoric acid-nitric acid-perchloric acid-hydrochloric acid low pressure closed digestion method and hydrofluoric acid-nitric acid-perchloric acid-hydrochloric acid open digestion method on molybdenum ore samples,the low pressure closed digestion method was selected to prepare samples,the inductively coupled plasma mass spectrometry(ICP-MS)method was used to determine the mass ratio of associated rare elements lithium,gallium and other 15 rare earth elements in molybdenum ore.Through the analysis of interfering elements,the suitable isotope was selected and the correction coefficients of^(151)Eu,^(157)Gd,^(159)Tb mass spectrum interference was determined.The results show that the standard solution of 20μg/L rhodium is used as an internal standard solution can effectively inhibit matrix effect and signal dynamic drift in the solution,the detection limit of the method is 0.001—0.113μg/g,and the relative standard deviation(RSD,n=7)is 0.30%—3.92%,which is verified by standard materials and actual samples.The method is reliable and suitable for the determination of associated lithium,gallium and rare earth elements in molybdenum ore.

关 键 词：电感耦合等离子体质谱法 密闭消解 钼矿石 伴生 锂 镓 稀土元素 

分 类 号：O655[理学—分析化学]