微波消解-电感耦合等离子体原子发射光谱法测定甲基磺酸盐(MSA)电镀锡泥中铜镍铅锑铋

甲基磺酸盐(MSA)体系电镀锡板在生产过程中,电镀液中的锡发生氧化会在阳极形成锡泥,这种固废产物中的重金属元素如果处理不当,将危害环境,因此准确测定电镀锡泥中金属元素的含量有利于指导其后续处理。实验采用硝酸-盐酸-氢氟酸并采用微波消解法对样品进行消解,可有效除去锡泥中有机物且不会造成待测元素的损失;采用基体匹配法消除基体效应的影响,选择Cu 324.754 nm、Ni 231.604 nm、Pb 220.353 nm、Sb 206.833 nm、Bi 190.241 nm为分析谱线,建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定MSA电镀锡泥中铜、镍、铅、锑、铋的方法。结果表明:在仪器最佳工作条件下,各元素校准曲线的线性相关系数均大于0.999 5,各元素检出限为0.000 2%~0.000 6%。按照实验方法测定MSA电镀锡泥中铜、镍、铅、锑、铋,结果的相对标准偏差(RSD,n=8)均小于3%,加标回收率为97%~104%。按照实验方法测定MSA电镀锡泥样品中铜、镍、铅、锑、铋,结果与火焰原子吸收光谱法测定铜、镍、铅,硫酸铈滴定法测定锑,EDTA滴定法测定铋的对比结果一致性较好。

Determination of copper,nickel,lead,antimony and bismuth in methanesulfonate electroplating tin slurry by inductively coupled plasma atomic emission spectrometry after microwave digestion

During the production process of methanesulfonate(MSA) electrolytic tinplate, tin in the electroplate liquid will be oxidized to form tin slurry in anode. The improper handling of heavy metal elements in such waste solid products is harmful to the environment. Therefore, the accurate determination of metal contents in electroplating tin slurry is helpful to guide its subsequent treatment. The sample was decomposed by microwave digestion in nitric acid-hydrochloric acid-hydrofluoric acid system. The organic materials in tin slurry could be effectively removed without loss of testing elements. The influence of matrix effect was eliminated by the matrix matching method. Cu 324.754 nm, Ni 231.604 nm, Pb 220.353 nm,Sb 206.833 nm and Bi 190.241 nm were selected as the analytical lines. The determination method of copper, nickel, lead, antimony and bismuth in MSA electroplating tin slurry by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The results showed that: under the optimal working conditions of instrument, the linear correlation coefficients of calibration curves of testing elements were all higher than 0.999 5. The limits of detection of testing elements were between 0.000 2% and 0.000 6%. The contents of copper, nickel, lead, antimony and bismuth in electroplating tin slurry were determined according to the experimental method, and the relative standard deviations (RSD, n=8) of determination results were all less than 3%. The recoveries were between 97% and 104%. The proposed method was applied for the determination of copper, nickel, lead, antimony and bismuth in MSA electroplating tin slurry samples, and the found results were consistent with those obtained by other methods (flame atomic absorption spectrometry for the determination of copper, nickel and lead; ceric sulfate titration for the determination of antimony; EDTA titration for the determination of bismuth).