ICP-MS/MS分析高温合金中痕量镉的质谱干扰消除研究  

Study on the interference elimination of trace cadmium in superalloy by ICP-MS/MS

作　　者：侯艳霞[1,2] 杨国武 李小佳[1,2] 刘庆斌 HOU Yanxia;YANG Guowu;LI Xiaojia;LIU Qingbin(Central Iron&Steel Research Institute,Beijing 100081;NCS Testing Technology Co.,Ltd.,Beijing 100081)

机构地区：[1]钢铁研究总院,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》2022年第3期330-334,共5页Chinese Journal of Analysis Laboratory

摘　　要：建立了三重四极杆-电感耦合等离子体质谱(ICP-MS/MS)分析高温合金中痕量Cd的方法,研究了单四极杆模式(SQ)和双四极杆模式(QQQ)中分别通入不同的碰撞/反应气体(He,O_(2)和NH_(3))的干扰消除效果。结果表明,采用双四极杆加氧模式(QQQ-O_(2))和加氨模式(QQQ-NH_(3)),干扰消除效果显著优于其他模式;O_(2)和NH_(3)的最佳流速分别为0.75 mL/min和0.50 mL/min;考察0.10~100 mg/g Mo溶液中加入0.1μg/g Cd后的回收率、高温合金标准物质测定结果和实际样品测定结果,Cd的回收率在95.5%~116.2%之间,标准物质测定值在标准值范围内,实际样品测定值与氢化物发生原子荧光法测试结果吻合。所建立方法可以消除Mo的多原子离子对痕量Cd的质谱干扰。A triple quadrupole inductively coupled plasma mass spectrometry(ICP-MS/MS)method was developed for the determination of trace Cd in superalloys.Meanwhile,the interference elimination effects of different collision/reaction gases(He,O_(2)and NH_(3))in single quadrupole mode(SQ)and double quadrupole mode(QQQ)were investigated.The results indicated that the modes of QQQ-O_(2)and QQQ-NH_(3)possessed satisfactory interference elimination effect than the others.The optimal flow rates of O_(2)and NH_(3)were 0.75 mL/min and 0.50 mL/min,respectively.In order to verify the interference elimination effect,the recovery rate of 0.1μg/g Cd in 0.10 mg/g to 100 mg/g Mo content solutions,as well as the determination results of superalloy standard substance and the actual sample were investigated.The measured value was within the range of the standard value,and the measured value of the actual sample was consistent with that of the hydride generation atomic fluorescence method.Therefore,the proposed method can eliminate the polyatomic ions interference of Mo on trace Cd.

关 键 词：ICP-MS/MS 高温合金 痕量镉 质谱干扰消除 

分 类 号：O657.63[理学—分析化学]