学术论文

      微波消解-电感耦合等离子体质谱法测定镍精矿中Ga、Ge、Se、Cd、In、Te、La和Tl

      Determination of Ga, Ge, Se, Cd, In, Te, La and Tl in Nickel Concentrates by ICP-MS Combined with Microwave Digestion

      摘要:
      样品经硝酸盐酸-氢氟酸-过氧化氢(3+1+1+1)混合液微波消解后,加入硝酸(1+1)溶液溶解盐类,定容后供电感耦合等离子体质谱分析.以103 Rh和232Th为内标,采用校正方程消除质谱干扰.Se的线性范围为0.500~500.0μg·L-1,其他7种元素的线性范围均为0.050~100.0μg·L-1,8种元素的检出限(3s)在0.01~0.8 mg·kg-1之间.加标回收率在90.9%~113%之间,测定值的相对标准偏差(n=4)在0.90%~7.7%之间.方法用于测定镍精矿标准物质中Cd,测定值与认定值相符.
      Abstract:
      The sample was digested by microwave with the mixed solution of HNO3、HC1、HF and H2O2 (3+1+1 +1),then HNO3 (1+1) solution was added to dissolve the salt and the solution was diluted for ICP-MS analysis with 103Rh and 232Th as internal standard.The calibration equation was used to eliminate mass spectral interference.The linearity range of Se and the other 7 elements were 0.500-500.0,0.050-100.0 μg · L 1,respectively.The detection limits (3s) of 8 elements were in the range of 0.01-0.8 mg · kg-1.Recovery rates obtained by standard addition method were in the range of 90.9%-113%,and RSDs (n=4) were in the range of 0.90%-7.7%.The proposed method was applied to the determination of Cd in nickel concentrate standard substances,giving results in agreement with the certified values.
      作者: 赵小龙 [1] 燕娜 [2] 侍金敏 [2] 赵生国 [2] 何艳 [3]
      Author: ZHAO Xiaolong [1] YAN Na [2] SHI Jinmin [2] ZHAO Shengguo [2] HE Yan [3]
      作者单位: 西北师范大学化学化工学院,兰州,730070 甘肃出入境检验检疫局,兰州,730010 西北师范大学地理与环境科学学院,兰州,730070
      刊 名: 理化检验-化学分册 ISTICPKU
      年,卷(期): 2017, 53(9)
      分类号: O657.63
      在线出版日期: 2017年12月6日
      基金项目: 国家自然科学基金,国家质检总局科研项目,甘肃检验检疫局科技计划项目