直流辉光放电质谱法半定量分析金属镝中73种杂质元素  

Semi-Quantitative Analysis of 73 Impurity Elements in Dysprosium Metal by Direct Current-Glow Discharge Mass Spectrometry

作　　者：李爱嫦 墨淑敏 潘元海 邱长丹 祝利红 董超波 LI Aichang;MO Shumin;PAN Yuanhai;QIU Changdan;ZHU Lihong;DONG Chaobo(Guobiao(Beijing)Testing&Certification Limited Company,Beijifig 101407,China)

机构地区：[1]国标(北京)检验认证有限公司,北京101407

出　　处：《理化检验（化学分册）》2021年第12期1067-1073,共7页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：建立了直流辉光放电质谱法(DC-GDMS)半定量分析金属镝中73种杂质元素的方法。取金属镝样品(25 mm×10 mm)分析,采用合适的质量数和分辨率将待测元素峰和干扰峰完全分离,从而消除质谱干扰,在放电气体流量为450 mL·min^(-1),放电电流为45 mA,预溅射时间为15 min的条件下,利用仪器自带"典型相对灵敏度因子(RSF)"校正结果,测定金属镝中73种杂质元素。结果表明:在没有标准物质的情况下,可实现对金属镝中73种杂质元素的半定量分析;重复测定样品11次,测定值的相对标准偏差(RSD)均小于2.0%;将该方法与国家标准方法(GB/T 12690.5-2017中的电感耦合等离子体原子发射光谱法和GB/T 18115.9-2006中的电感耦合等离子体质谱法)进行比对,所得结果基本一致。A method for semi-quantitative analysis of the 73 impurity elements in dysprosium metal by direct current-glow discharge mass spectrometry(DC-GDMS)was established.The dysprosium metal sample(25 mm×10 mm)was taken to analyze,and the element peaks and interference peaks were completely separated with appropriate mass number and resolution,so as to eliminate the interference of mass spectrum.Under the conditions of discharge gas flow of 450 mL·min^(-1) and discharge current of 45 mA,the 73 impurity elements in dysprosium metal were determined by using the correction results of"typical relative sensitivity factor(RSF)"provided by the instrument.It was showed that the semi-quantitative analysis of the 73 impurity elements in dysprosium metal could be achieved without standard materials.The sample was determined 11 times repeatedly,with RSDs of the determined values less than 2.0%.The proposed method was compared with the national standard method(ICP-AES in GB/T 12690.5-2017 and ICP-MS in GB/T 18115.9-2006),and the results were basically consistent.

关 键 词：直流辉光放电质谱法 金属镝 半定量分析 杂质元素 

分 类 号：O657.63[理学—分析化学]