电感耦合等离子体质谱法测定高纯铌中20种痕量杂质元素  

Determination of 20 Trace Impurity Elements in High-Purity Niobium by Inductively Coupled Plasma Mass Spectrometry

作　　者：刘洁[1] 陈忠颖[1] 刘巍[1] 郭颖[1] LIU Jie;CHEN Zhongying;LIU Wei;GUO Ying(Testing Center,Shanghai Research Institute of Materials,Shanghai 200437,China)

机构地区：[1]上海材料研究所检测中心,上海200437

出　　处：《理化检验（化学分册）》2018年第10期1158-1162,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：上海材料研究所技术创新项目(17SG-06)

摘　　要：高纯铌样品0.050 0g中加入适量的水,缓慢加入1mL氢氟酸和2mL硝酸,低温加热使其溶解,冷却至室温,用水定容至100mL。采用电感耦合等离子体质谱法测定所得溶液中20种痕量杂质元素,以内标法定量。结果表明:20种元素的检出限(3s)为0.005～0.20μg·g-1,回收率为95.0%～110%。按所提出方法分析铌锭样品,所得结果与辉光放电质谱法所得结果相符。The high-purity niobium sample （0.050 0 g） was dissolved in the mixture of some water, 1 mL of HF and 2 mL of HNO3, which were added slowly, by heating at low temperature, and then the solution was cooled to room temperature, and made its volume up to 100 mL. The 20 trace impurity elements in above solution were determined by inductively coupled plasma mass spectrometry （ICP-MS）, and internal standard method was used for quantitative analysis. As shown by the results, the detection limits （3s） of 20 elements were found in the range of 0.005-0.20 μg · g^-l. Values of recovery were found in the range of 95.0%- 110%. A niobium ingot sample was analyzed by the proposed method, giving results in consistency with the results found by glow discharge mass spectrometry.

关 键 词：电感耦合等离子体质谱法 高纯铌 痕量杂质元素 

分 类 号：O657.63[理学—分析化学]