Determination of copper,nickel,lead,antimony and bismuth in methanesulfonate electroplating tin slurry by inductively coupled plasma atomic emission spectrometry after microwave digestion
DONG Linan, ZHOU Lili, ZHAO Xiwen, ZHU Chunyao
Institute of Research of Iron and Steel, Jiangsu Province and Sha Steel, Zhangjiagang 215625, China
Abstract：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).
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