超高效液相色谱法测定甲基磺酸锡电镀液中甲基磺酸

发布时间：2018-02-28 10:08

本文关键词： 超高效液相色谱蒸发光散射法锡电镀液甲基磺酸　出处：《冶金分析》2017年06期 　论文类型：期刊论文

【摘要】：准确测定甲基磺酸锡电镀液中甲基磺酸的含量对镀锡板稳定生产和电镀液老化评价有着重要意义。采用BEH Amide色谱柱(3.0×150mm,1.7μm),以0.010mol/L乙酸铵乙腈溶液-0.010mol/L乙酸铵水溶液(体积比为80∶20)为流动相,控制流速为0.40mL/min,建立了超高效液相色谱法测定甲基磺酸锡电镀液中甲基磺酸含量的方法。干扰试验表明:甲基磺酸锡电镀液中其他共存组分对甲基磺酸的测定均没有干扰。在甲基磺酸质量浓度为1.00~10.00mL/L范围内,甲基磺酸质量浓度的对数与其峰面积的对数呈线性关系,线性相关系数为0.999 6。将实验方法应用于甲基磺酸锡电镀液实际样品中甲基磺酸的测定,测得结果的相对标准偏差(RSD,n=11)为0.79%~1.2%,加标回收率为99%~102%。按照甲基磺酸锡电镀液配方体系配制甲基磺酸锡电镀液合成样品,并采用实验方法进行测定,测定值与理论值相符。
[Abstract]:Accurate determination of methanesulfonic acid in tin methanesulfonate electroplating solution is of great significance for the stable production of tin plating plate and the evaluation of ageing of plating solution. The BEH Amide column is used to determine the content of methanesulfonic acid in the electroplating solution of 3.0 脳 150mm ~ 1.7 渭 m ~ (-1) 渭 m 路m ~ (-1) with 0.010 mol / L ammonium acetate acetonitrile solution -0.010 mol / L ammonium acetate aqueous solution (volume). Than 80: 20) as the mobile phase, A method for the determination of methanesulfonic acid in tin methanesulfonate electroplating solution by ultra-high performance liquid chromatography was established at a flow rate of 0.40 mL / min. The interference test showed that none of the other coexisting components in tin methanesulfonate electroplating solution was determined for p-methylsulfonic acid. Interference. In the range of 1.00 渭 m L / L of methyl sulfonic acid, The logarithm of mass concentration of methyl sulfonic acid is linear with the logarithm of its peak area, and the linear correlation coefficient is 0.999 6. The method has been applied to the determination of methyl sulfonic acid in practical samples of tin methanesulfonate electroplating solution. The relative standard deviation (RSD) of the measured results is 0.79 ~ 1.2and the recovery rate is 99 ~ 102.The synthetic sample of tin methanesulfonate electroplating solution is prepared according to the formula system of tin methanesulfonate electroplating solution, and the measured value is in agreement with the theoretical value.
【作者单位】：上海梅山钢铁股份有限公司技术中心;
【分类号】：O657.72;TQ153.13

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