ZHOU Guihai,WANG Dezhi.Determination of SO42- in MSA Tin Electroplate Solution by UPLC[J].Plating & Finishing,2021,(4):39-43.[doi:10.3969/j.issn.1001-3849.2021.04.009]
超高效液相色谱法测定甲基磺酸电镀锡液中硫酸根
- Title:
- Determination of SO42- in MSA Tin Electroplate Solution by UPLC
- Keywords:
- UPLC tin electroplating solution SO42-
- 文献标志码:
- A
- 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。
- Abstract:
- A determination method of SO42- 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 SO42- 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.
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备注/Memo
收稿日期：2019-08-28；修回日期：2019-10-24
作者简介：周桂海(1979-)，男，本科，高级工程师，从事冶金分析测试技术研究工作，E-mail：zhouguihai@baosteel.com