超高效液相色谱法测定甲基磺酸电镀锡液中硫酸根  

Determination of SO_(4)^(2-) in MSA Tin Electroplate Solution by UPLC

作　　者：周桂海[1] 王德智[1] ZHOU Guihai;WANG Dezhi(Technology center,Shanghai Meishan Iron and steel Co.,Ltd.,Nanjing 210039,China)

机构地区：[1]上海梅山钢铁股份有限公司技术中心,江苏南京210039

出　　处：《电镀与精饰》2021年第4期39-43,共5页Plating & Finishing

摘　　要：采用亚乙基桥杂化颗粒色谱柱,柱温设定45℃,以乙腈和水(体积比80∶20)为流动相,流速为0.3 mL/min,并与蒸发光散射检测器联用,建立超高效液相色谱法(UPLC)测定甲基磺酸(MSA)电镀锡液中硫酸根含量。实验对样品前处理、色谱分离条件和检测器检测参数进行了优化。方法应用到实际样品检测,相对标准偏差为0.74%~1.3%,检出限为15.2 mg/L,加标回收实验回收率为99.0%~101.1%。该方法与硫酸根钡重量法比对,检测结果无显著性差异,应用到电镀锡液合成样品测定,测定值与理论值相符。A determination method of SO_(4)^(2-) in methyl sulfonic acid(MSA)tin electroplate solution was established by ultra-performance liquid chromatography(UPLC)combined with BEH amide chromatographic column and evaporative light-scattering detector(ELSD)method.The column temperature was 45℃and the mobile phase was acetonitrile and water(volume ratio of 80∶20).The sample pretreatment,chromatographic separation condition and detector detection parameters were optimized.The proposed method was applied to the determination of SO_(4)^(2-) in actual sample.The relative standard deviation was 0.74%~1.3%,and the recoveries were between 99.0%~101.0%.Compared with barium sulfate gravimetric method,there was no significant difference.The synthetic sample was determiner by the method.The results were consistent with the theoretical values.

关 键 词：超高效液相色谱法 电镀锡液 硫酸根 

分 类 号：O657.7[理学—分析化学]