摘要
试样以盐酸-硝酸溶解,建立了电感耦合等离子体质谱法(ICP-MS)测定镍铂合金中 17 个杂质元素的方法.采用标准模式测定Mg、Al、Ti、Cr、Mn、Co、Zn、Cu、Zr、Pd、Ag、Sn、Sm、和Pb,氨气反应模式测定Si和Fe(氨气流速分别为 0.2 和 0.25 mL/min);氦气反应模式测定V(氦气流速为 5 mL/min,考察了基体效应对测定结果的影响,采用内标校正提高分析的准确性,其中Mg、Al、Ti、Cr、V、Mn、Fe、Co、Zn和Si以Sc为内标,Cu、Zr、Pd、Ag和Sn以Y为内标,Sm和Pb以Re为内标.测定各元素的线性相关系数(r)不小于 0.9996,方法检出限为 0.0025～0.78 ng/mL.对NiPt5、NiPt15、NiPt60样品中 17个杂质元素进行测定,相对标准偏差(RSD)为 0.86%～13.07%,加标回收率 89.0%～116.5%,方法满足镍铂合金靶材的测定要求.
Abstract
After the sample of nickel-platinum alloy was digested in the mixture of hydrochloric acid and nitric acid,seventeen impurity elements were determined by inductively coupled plasma mass spectrometry(ICP-MS).The analysis of Mg,Al,Ti,Cr,Mn,Co,Zn,Cu,Zr,Pd,Ag,Sn,Sm and Pb was performed by using the normal mode whereas the measurement of Si and Fe were carried out by using NH3 as the reaction gas at a flow rate 0.2 and 25 mL/min,respectively.Finally,V content was analyzed by choosing He as the reaction gas at a flow rate of 5 mL/min.The effect of the matrix on the determination was investigated.Internal standard method was used to improve the accuracy.Sc was selected as an internal standard for correcting Mg,Al,Ti,Cr,V,Mn,Fe,Co,Zn,Si,and Y for Cu,Zr,Pd,Ag,Sn,and Re for Sm and Pb.The linear correlation coefficient(r)was larger than 0.9997.The detection limits were 0.0025～0.78 ng/mL,and the recoveries of standard addition were 89.0%～116.5%.The relative standard deviation(RSD)was found to be 0.86%～13.07%for all 17 elements.The method developed in this work can be applied to the analysis of Ni-Pt alloy target materials.
基金项目
国家标准制定任务项目(20213154-T-610)
NETL
NSTL
万方数据