Abstract：The electrolytic detinning was performed in hydrochloric acid medium using calomel electrode as reference electrode, platinum wire as auxiliary electrode and sample as working electrode. The change of electrolytic curve between voltage and time was observed. The electric current density for stripping of tin plating layer was 5 mA/cm2. The heating temperature of 500 ℃ and concentration time of 45 min were obtained by solution concentration experiments. Pb 220.353 nm was selected as the analytical line. The influence of matrix effect could be eliminated by preparing the calibration curve using matrix matching method. The content of iron in detinning solution was determined, and the interference amount of iron on lead was deducted. Finally, the content of lead in plating layer was obtained by calculation. Consequently, the determination method of lead in tin plating layer by inductively coupled plasma atomic emission spectrometry (ICP-AES) after electrolytic detinning was established. In 50 mL hydrochloric acid solution, the mass of lead in range of 2.50-15.0 μg was linear to the emission intensity with correlation coefficient of 0.999 3. The detection limit of lead in this method was 0.24 μg/g. The proposed method was applied to the determination of lead in tin plating layer. The relative standard deviations (RSD, n=6) were less than 3.0%, and the recoveries of standard addition were between 97% and 104%.
何志明, 吴益青, 贺萍. 电解脱锡-电感耦合等离子体原子发射光谱法测定镀锡板镀层中铅[J]. 冶金分析, 2016, 36(5): 39-43.
HE Zhi-ming,WU Yi-qing,HE Ping. Determination of lead in tin plating layer by inductively coupled plasma atomic emission spectrometry after electrolytic detinning. , 2016, 36(5): 39-43.
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