钕铁硼合金中13种元素辉光放电质谱法定量分析研究  

Quantitative Analysis for 13 Elements in NdFeB Alloy by Glow Discharge Mass Spectrometry

作　　者：聂帅[1] 刘鹏宇[1] 李宝城[1] 田佳[1] 鲍叶琳 刘兵[1] 

机构地区：[1]北京有色金属研究总院分析测试研究所,北京100088

出　　处：《稀有金属》2016年第8期756-762,共7页Chinese Journal of Rare Metals

基　　金：国家科技部创新方法工作专项项目(2012IM030500)资助

摘　　要：为了探索辉光放电质谱法(GD-MS)定量分析稀土材料中微量元素含量,建立了GD-MS法测定钕铁硼(NdFeB)合金中13种常微量元素的方法。因Nd Fe B合金尚无标准样品,制备了6块控制样品并进行均匀性检验与定值;优化了GD-MS仪器条件(放电电流、放电气体流量、离子源温度和透镜电参数)来获得足够且稳定的灵敏度与分辨率以及适宜且稳定的离子流强度。测定控制样品并建立工作曲线,测定了2块钕铁硼合金试样中的Al,V,Cr,Mn,Co,Ni,Cu,Ga,Zr,Nb,Mo,Tb,Dy共13种常微量元素的含量。结果表明:GD-MS法与电感耦合等离子体发射光谱法(ICP-AES)的测定结果相吻合,各元素的相对标准偏差(RSD)都小于3%,该准确度与精密度良好,能够对稀土材料中稀土和非稀土元素的准确测定。In order to investigate quantitative analysis for 13 elements in rare earth materials by glow discharge mass spectrometry（ GD-MS）,a method for determination of 13 elements in NdFeB alloy was established. 6 control samples of NdFeB alloy were prepared,then the test for the homogeneity and certified results of determined elements were achieved,and instrument conditions such as the discharge current,the discharge gas flow rate,ion source temperature,and lenses electronic parameters were optimized to get satisfying sensitivity and resolution,appropriate and stable ion flow. Six control samples were analyzed and working curve for each elements was established,and 13 elements including Al,V,Cr,Mn,Co,Ni,Cu,Ga,Zr,Nb,Mo,Tb and Dy of two NdFeB alloy samples were determined using GD-MS. The results coincided with inductively coupled plasma atomic emission spectrometry（ ICPAES） and the relative standard deviations（ RSD） of 13 elements were less than 3. 5 %,which concluded satisfactory accuracy and precision of this method,so GD-MS could determine the rare earth and non-rare earths elements in rare earth materials accurately.

关 键 词：辉光放电质谱法(GD-MS) 钕铁硼合金 控制样品 工作曲线 定量分析 

分 类 号：O657.63[理学—分析化学]