辉光放电质谱法测定高纯钛中痕量杂质元素及其相对灵敏度因子校正  

Determination of impurity elements in high-purity titanium by glow discharge mass spectrometry and evaluation of their relative sensitivity factors

作　　者：余琼 连危洁[2] 翟宇鑫 马兰 李明利[3] YU Qiong;LIAN Weijie;ZHAI Yuxin;MA Lan;LI Mingli(College of Traditional Chinese Medicine,Zhejiang Pharmaceutical University,Ningbo 315500,China;Ningbo Branch of China Academy of Ordnance Science,Ningbo 315103,China;College of Medical Devices,Zhejiang Pharmaceutical University,Ningbo 315500,China)

机构地区：[1]浙江药科职业大学中药学院,宁波315500 [2]中国兵器科学研究院宁波分院,宁波315103 [3]浙江药科职业大学医疗器械学院,宁波315500

出　　处：《分析试验室》2023年第5期659-664,共6页Chinese Journal of Analysis Laboratory

基　　金：宁波市关键核心技术应急攻关计划项目(2020G009)资助。

摘　　要：通过选择合适的同位素及分辨率,建立了辉光放电质谱法(GDMS)测定高纯Ti中57种痕量杂质元素的方法。辉光放电过程优化条件为Ar流量500 mL/min,放电电流2.2 mA,预溅射时间30 min。利用高纯Ti标准样品获得了与基体匹配的13种元素的相对灵敏度因子(RSF)值。用建立的方法对高纯Ti溅射靶材样品进行检测,主要杂质元素为Al, Si, S, Cl, V, Cr, Mn, Fe, Ni, Cu, Zr,含量在0.051~2.470μg/g之间,相对标准偏差(RSD)<23%,杂质总量<5μg/g。其中,Ca, Nb元素的检出限为0.5μg/g,其余元素的检出限低至10 ng/g级或1 ng/g级,而且Th, U元素的检出限达到0.1 ng/g。该方法能够满足5N级高纯金属Ti溅射靶材的检测要求。Glow discharge mass spectrometry(GDMS)method was used for the determination of 57 trace impurity elements in high-pure titanium sputtering targets by selecting appropriate isotopes and resolution.The optimized parameters in the glow discharge process were set as follows.The argon gas flow rate was 500 mL/min,the discharge current was 2.2 mA,and the pre-sputtering time was 30 min.The relative sensitivity factor(RSF)values of 13 elements matching the matrix were obtained using high-purity titanium standard samples.The contents of the main impurity elements of Al,Si,S,Cl,V,Cr,Mn,Fe,Ni,Cu and Zr in the high-purity titanium samples detected by the established method were 0.051-2.470μg/g.The relative standard deviations(RSDs)were less than 23%with good repeatability,and the total amount of impurities was less than 5μg/g.The limits of detection of Ca and Nb were 0.5μg/g,the other elements could reach 10 ng/g or 1 ng/g,while that of Th and U were as low as 0.1 ng/g.The method can fulfill the detection requirements of 5N grade high purity titanium sputtering target.

关 键 词：辉光质谱 高纯Ti 杂质元素 相对灵敏度因子 

分 类 号：O657.63[理学—分析化学]