学术论文

      电感耦合等离子体质谱法测定地质样品中钪镓锗铟镉铊时的干扰及其消除方法

      Elimination of Interferences in ICP-MS Determination of Sc, Ga,Ge,In,Cd and Tl in Geological Samples

      摘要:
      地质样品经硝酸-氢氟酸-高氯酸密闭分解。适当稀释样品(稀释因子 DF=1000),控制试液中的含盐量,并结合内标(Rh、Ir)校正消除基体效应和物理效应。28 Si16 O1 H、29 Si16 O 干扰45 Sc的测定,在样品处理时除硅以消除其干扰。142 Ce2+、142 Nd2+干扰71 Ga 的测定,58 Ni16 O、148 Sm2+、148 Nd2+干扰74 Ge 的测定,114 Sn、98 Mo16 O、97 Mo16 O1 H 干扰114 Cd 的测定,115 Sn、98 Mo16 O1 H、98 Mo17 O干扰115 In 的测定,采用数学校正法消除它们的干扰。高含量的204 Pb 和206 Pb 分别干扰203 Tl 和205 Tl的测定,在样品处理时采用沉淀分离铅以消除其干扰。应用此方法测定了国家一级标准物质中的钪、镓、锗、铟、镉和铊的含量,测定值与认定值相符。
      Abstract:
      Geological sample was decomposed with a mixed acid of nitric acid,hydrofluoric acid and perchloric acid under hermetic condition.The salt content of the sample solution was carefully controlled by appropriate dilution with value of DF of 1 000.Elimination of matrix and physical effects were attained by correction with Rh and Ir as internal standards.Interferences of 28 Si16 O1 H and 29 Si16 O on the determination of 45 Sc were eliminated by removal of Si in sample pre-treatment.Furthermore,some other interferences,such as 142 Ce2+ and 142 Nd2+ on the determination of 71 Ga,58 Ni16 O,148 Sm2+ and 148 Nd2+ on the determination of 74 Ge,114 Sn,98 Mo16 O and 97 Mo16 O1 H on the determination of 114 Cd,115 Sn,98 Mo16 O1 H and 98 Mo17 O on the determination of 115 In,were eliminated by mathematical corrections.The interferences of 204 Pb and 206 Pb (with high concentration)on the determination of 203 Tl and 205 Tl were eliminated by separation with precipitation of Pb from the sample solution in the pre-treatment. The proposed method was tested by analyzing a CRM for its corrtents of Sc,Ga,Ge,In,Cd and Tl,giving results in consistency with the certified values.
      Author: SUN Chao-yang DONG Li-ming HE Ying-ting YANG Li-hua ZHENG Cun-jiang
      作者单位: 浙江省地质矿产研究所,杭州,310007
      刊 名: 理化检验-化学分册 ISTICPKU
      年,卷(期): 2016, 52(9)
      分类号: O657.63
      机标分类号: O65 R28
      在线出版日期: 2016年11月21日
      基金项目: 国家重大科学仪器设备开发专项资助