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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(3.0×150 mm,1.7 μm),以0.010 mol/L乙酸铵乙腈溶液-0.010 mol/L乙酸铵水溶液(体积比为80∶20)为流动相,控制流速为0.40 mL/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1.00~10.00 mL/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.

The accurate determination of methanesulfonic acid content in methanesulfonic acid tin electroplate liquid is of great significance for the stable production of tin plate and aging evaluation of electroplate liquid.BEH Amide chromatographic column (3.0×150 mm, 1.7 μm) was used.The mobile phase was 0.010 mol/L ammonium acetate acetonitrile solution-0.010 mol/L ammonium acetate aqueous solution (volume ratio of 80∶20).The flow rate was controlled at 0.40 mL/min.Thus, a determination method of methanesulfonic acid in methanesulfonic acid tin electroplate liquid was established by ultra-high performance liquid chromatography.The interference tests showed that the determination of methanesulfonic acid was not affected by other coexisting components in methanesulfonic acid tin electroplate liquid.When the mass concentration of methanesulfonic acid was in range of 1.00-10.00 mL/L, the logarithm of its mass concentration was linear to the logarithm of its corresponding peak area with linear correlation coefficient of 0.999 6.The proposed method was applied to the determination of methanesulfonic acid in actual sample of methanesulfonic acid tin electroplate liquid.The relative standard deviation (RSD, n=11) was 0.79%-1.2%, and the recoveries were between 99% and 102%.The synthetic sample of methanesulfonic acid tin electroplate liquid was prepared according to its formula system and determined by determined by the proposed method.The results were consistent with the theoretical values.