吉林大学学报(理学版) ›› 2021, Vol. 59 ›› Issue (2): 427-434.

• • 上一篇    

ICP-MS法测定钼矿石中伴生锂、镓和稀土元素

梁亚丽, 杨珍, 阿丽莉, 贺攀红,  孙银生   

  1. 河南省核工业地质局, 郑州 450044;  河南省核工业放射性核素检测中心, 郑州 450044
  • 收稿日期:2020-10-23 出版日期:2021-03-26 发布日期:2021-03-26
  • 通讯作者: 阿丽莉 E-mail:lilia100200@126.com

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

LIANG Yali,  YANG Zhen,  A Lili, HE Panhong,  SUN Yinsheng   

  1. Henan Province Nuclear Geology,Zhengzhou 450044,China;Henan Nuclear Industry Radioactive Nuclide Test Centre,Zhengzhou 450044,China
  • Received:2020-10-23 Online:2021-03-26 Published:2021-03-26

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151Eu,157Gd,159Tb质谱干扰的校正系数. 结果表明,  20 μg/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0.001~0.113 μg/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.

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

Abstract: 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 151Eu,157Gd,159Tb mass spectrum interference was determined. The results show that the standard solution of 20 μg/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—0.113 μg/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.

Key words: inductively coupled plasma mass spectrometry; , closed , digestion; , molybdenum ore; , associated; , lithium; , gallium; , rare earth element

中图分类号: 

  • O655