镀金液中杂质元素的电感耦合等离子体质谱法测定

Determination of Impurity Elements in Gold Plating Bath by Inductively Coupled Plasma-Mass Spectrometry

电感耦合等离子体质谱(ICP-MS)法具有很多优点,但其测定镀金液中杂质元素时基体元素Au对测定有干扰和抑制。用甲基异丁基酮(MIBK)萃取分离镀金液中基体Au,通过加入内标混合溶液校正残余Au对待测元素的干扰,再用ICP-MS测定镀金液中的杂质元素Mn,Fe,Cu,Co,Ni,Cd,Pb,讨论了萃取条件、仪器工作参数、同位素及内标元素、质谱干扰、基体效应等对测量的影响,确定了最佳测定条件。结果表明:该方法的检出限为0.015～0.180μg/L,加标回收率为93.22%～107.78%,相对标准偏差为1.6%～4.1%;该方法准确、快速、简便,完全满足镀金液中杂质元素的测定要求。

Methyl isobutyl ketone (MIBK) was used to extract and separate Au in gold plating bath.Mixed solu-tion as an internal standard was then introduced to get rid of inter-ference from residual Au in measurement of metallic impurities.Impurity elements including Mn,Fe,Cu,Co,Ni,Cd and Pb in the gold plating bath were finally determined by using inductively coupled plasma-mass spectrometry(ICP-MS).The effects of ex-traction condition,instrument parameters,isotopes and internal standards,interference with mass spectrometry and matrix interfer-ence on the measurement were investigated,and the optimized conditions for determination were established.Results indicate that detection limit,recovery ratio and relative standard error for the title method are 0.015 ～0.180 μg/L,93.22%～107.78% and 1.6% ～4.1 % respectively.The method was accurate,expeditious and convenient,and could be satisfactorily applied for determina-tion of impurity elements in gold plating bath.