锌酸盐镀锌液中杂质元素的质谱分析

Determination of Impurity Elements in Zincate Bath for Zinc Plating by Inductively Coupled Plasma-Mass Spectrometry

利用带八极杆碰撞/反应池(ORS)和屏蔽炬技术的电感耦合等离子体质谱(ICP-MS)可同时直接测定锌酸盐镀锌液中Mg,V,Cr,Mn,Co,Ni,Cu,Cd,Sb,Pb杂质元素。通过向碰撞池中引入氢气和氦气消除多元素分子、离子的干扰,以50μg/L Sc,Ge,In,Tb为内标元素校正基体干扰和漂移,确定了仪器的最佳工作参数。结果表明:各元素在0～500.0μg/L内均有良好的线性关系,相关系数均在0.999 5以上;10种杂质元素的检出限在0.001～0.034μg/L,回收率为95.2%～107.4%,相对标准偏差(RSD)小于2.90%。

An inductively coupled plasma-mass spectrometry facility equipped with an octopole collision/reaction cell and shield torch system was employed to simultaneously determine impurity elements Mg,V,Cr,Mn,Co,Ni,Cu,Cd,Sb and Pb in zincate bath for zinc electroplating.The interferences of multi-element molecules and ions were eliminated by introducing hydrogen gas and helium gas into the collision/reaction cell,and the matrix interference and drift were corrected by introducing 50 μg/L Sc,Ge,In and Tb as the internal standard to correct.Then the optimal working parameters of the facility were established accordingly.Results indicate that a good linear relationship is achieved when the mass fraction of each element is in the range of 0～500.0 μg/L,and corresponding relative coefficient is 0.999 5.Besides,the detection limits for the 10 kinds of to-be-tested elements are 0.001-0.034 μg/L,the recoveries of samples are in the range of 95.2%～107.4%,and the relative standard deviation is less than 2.90%.