超高效液相色谱法测定甲基磺酸盐镀锡电镀液中对苯二酚

Determination of Hydroquinone in Tin Electroplating Solution with Methanesulfonae by Ultra-High Performance Liquid Chromatography

移取25.00mL样品,用水定容至100mL,用0.2μm水系滤膜过滤后制得样品溶液,采用BEH Amide色谱柱(3.0mm×150mm,1.7μm)分离,以0.010mol·L-1乙酸铵乙腈溶液-0.010mol·L-1乙酸铵水溶液(体积比为70∶30)为流动相,流量为0.40mL·min-1,采用蒸发光散射检测器。干扰试验表明:甲基磺酸盐镀锡电镀液中其他共存组分对对苯二酚的测定均没有干扰。对苯二酚质量浓度在10.0~100.0mg·L-1内,其质量浓度的对数与其峰面积的对数呈线性关系,检出限(3S/N)为2.21mg·L-1。方法用于测定甲基磺酸盐镀锡电镀液样品中的对苯二酚,测定值的相对标准偏差(n=11)为0.79%~1.2%,加标回收率为99.2%~102%,。按照甲基磺酸盐镀锡电镀液配方配制合成样品,采用试验方法对对苯二酚进行测定,测定值与理论值相符。

The sample（25.00 mL）was diluted to 100 mL with deionized water,and the solution was filtered with a 0.2μm aqueous filter to prepare the sample solution.BEH Amide chromatographic column（3.0 mm×150 mm,1.7μm）was used for seperation,with 0.010 mol· L-1 ammonium acetate acetonitrile solution-0.010 mol·L-1 ammonium acetate aqueous solution（volume ratio of 70∶30）as the mobile phase at the flow rate of 0.40 mL· min-1.Evaporatire light scattering detector was used.The interference tests showed that the determination of hydroquinone was not affected by other coexisting components in the tin electroplating solution with methanesulfonate.When the mass concentration of hydroquinone was in range of 10.0-100.0 mg·L-1,the logarithm of its mass concentration was linear to the logarithm of its corresponding peak area,with detection limit（3 S/N）of 2.21 mg·L-1.The proposed method was applied to the determination of hydroquinone in actual samples,giving relative standard deviations（n=11）were in the range of 0.79%-1.2%,and the values of recovery obtained by standard addition method ranged from 99.2% to 102%.The synthetic sample of tin electroplating solution with methanesulfonate was prepared according to its formula and determined by the proposed method.The results were consistent with the theoretical values.