电感耦合等离子体串联质谱法测定高纯钼中痕量钛  

Determination of trace titanium in high purity molybdenum by inductively coupled plasma tandem mass spectrometry

作　　者：苏丹丹 胡净宇[1,2] 刘晓波 侯艳霞 沈学静[1,2] SU Dandan;HU Jingyu;LIU Xiaobo;HOU Yanxia;SHEN Xuejing(Central Iron and Steel Research Institute,Beijing 100081,China;NCS Testing Technology Co.,Ltd,Beijing 100081,China)

机构地区：[1]钢铁研究总院有限公司,北京100081 [2]钢研纳克检测技术股份有限公司,北京100081

出　　处：《分析试验室》2024年第11期1545-1549,共5页Chinese Journal of Analysis Laboratory

基　　金：国家重点研发计划(2021YFF0700100)资助。

摘　　要：针对高纯钼中痕量钛分析中较难克服的双电荷干扰问题,采取氧气质量转移模式对其进行消除。根据待测元素钛的性质分析了可能的干扰情况,并在不同测定模式下考察待测物质的背景等效浓度(BEC),确定最佳干扰消除方法。设置一级质量过滤器Q_(1)的质荷比(m/z)为48,二级质量过滤器Q_(2)的m/z为64,钛经过碰撞/反应池的氧气作用后产生^(48)Ti^(16)O^(+),避免了^(96)Mo^(++)对^(48)Ti^(+)检测结果的干扰。氧气做反应气时的气体流速为0.225 mL/min;钪为内标校正相应信号。方法线性范围为0.5~100 ng/mL,线性相关系数为0.9999,检出限为0.098 ng/mL,定量限为0.296 ng/mL。加标回收率在94.7%~106.6%之间,测定结果与参考数值吻合较好。Oxygen mass transfer mode was adopted to eliminate the double charge interference problem which is difficult to overcome in the analysis of trace titanium in high purity molybdenum.The possible interference was analyzed according to the properties of titanium,and the background equivalent concentration (BEC) of the substance was investigated under different measurement modes to determine the best interference elimination method.The mass-charge ratios (m/z) of the primary mass filter Q_(1) and the secondary mass filter Q_(2) were set as 48 and 64,respectively.After the oxygen action in the collision/reaction cell,titanium turned into ^(48)Ti^(16)O^(+),avoiding the interference of ^(96)Mo^(++)on the detection results of ^(48)Ti^(+).The gas flow rate of oxygen as the reaction gas was 0.225 mL/min.Scandium was selected as the internal standard to correct the corresponding signal.The linear range was 0.5-100 ng/mL,the linear correlation coefficient was 0.9999,the limit of detection (LOD) was 0.098 ng/mL,and the limit of quantification (LOQ) was 0.296 ng/mL.The spiked recoveries were between 94.7%and 106.6%,and the results were in good agreement with the reference.

关 键 词：电感耦合等离子体质谱(ICP-MS) 串联质谱(MS/MS) 高纯钼 痕量钛 

分 类 号：O657.31[理学—分析化学] X832[理学—化学]