电感耦合等离子体质谱(ICP-MS)法在测定微量金属元素时存在质谱干扰和非质谱干扰.采用ICP-MS法结合碰撞/反应池(CRC)质谱校正技术和内标校正技术测定了碱性化学镀镍液中Ti,Cr,Mn,Fe,Co,Cu,Zn,Cd,Sb,Pb 10种微量金属元素含量.待测液用硝酸消解后采用ICP-MS法进行分析,利用碰撞/反应池和炬屏蔽系统校正了分析过程中的质谱干扰,采用多内标元素45Sc,72Ge,89Y,115In,209 Bi校正了质谱分析中的基体效应,优化了相关分析试验条件.结果表明:对于0 ～500 μg/L内的待测元素,工作曲线的相关系数均不小于0.999 6,方法的检出限为0.011 ～0.218 μ,g/L,加标回收率分别为89.89％～107.61％,相对标准偏差(RSD)为1.70％ ～4.81％.本方法可快速、灵敏、准确地测定碱性化学镀镍液中10种微量金属元素含量.
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