高效液相色谱串联质谱法测定酸铜电镀液中硫代丙烷磺酸钠  

Determination of sodium thiopropane sulfonate in acid copper plating solution by high performance liquid chromatography-tandem mass spectrometry

作　　者：孙文慧 秦宇媚 罗富智 蒋军 SUN Wenhui;QIN Yumei;LUO Fuzhi;JIANG Jun(GRG Metrology&Test Group Co.,Ltd.,Guangzhou510656,China)

机构地区：[1]广电计量检测集团股份有限公司,广州510656

出　　处：《化学分析计量》2023年第9期58-62,共5页Chemical Analysis And Meterage

摘　　要：基于高效液相色谱串联质谱建立了酸铜电镀液中硫代丙烷磺酸钠光亮剂的定性定量分析方法。以聚二硫二丙烷磺酸钠(SPS)和3-巯基-1-丙烷磺酸钠(MPS)为标准样品,以配置喷射流电喷雾离子源三重四级杆的高效液相色谱质谱联用仪为测试仪器,采用C_(18)反相色谱柱,乙酸铵水溶液-乙腈为流动相。采用硫酸水溶液配制不同浓度梯度的SPS和MPS混合标准溶液,以标准样品的母离子和子离子作为定性定量离子,分别建立SPS和MPS的标准工作曲线,两者的质量浓度在0.05~2 mg/L范围内,标准工作曲线的线性相关系数均大于0.9999,样品的加标回收率为96.8%~106.7%,测定结果的相对标准偏差小于2.0%(n=6),聚二硫二丙烷磺酸钠和3-巯基-1-丙烷磺酸钠的检出限分别为0.0030、0.0036 mg/L,定量限分别为0.0100、0.0120 mg/L。该方法可应用于电镀工厂对电镀液中微量硫代丙烷磺酸钠光亮剂的检测分析。A qualitative and quantitative analysis method was established to determine sodium thiopropane sulfonate brightener in acid copper electroplating solution by liquid chromatography-mass spectrometry/mass spectrometry(HPLCMS/MS).Bis-(sodium sulfopropyl)-disulfide(SPS)and sodium 3-mercaptopropanesulphonate(MPS)were analyzed on a high performance liquid chromatograph-triple quadrupole mass spectrometry equipped with electron spray ionization and C18 reversed phase column,and mixed solution of ammonium acetate aqueous solution and acetonitrile was used as mobile phase.A series of mixed standard solutions concentration of SPS and MPS were obtained through sulfuric acid aqueous solutions,then standard curves of SPS and MPS were established through their parent ion and daughter ion acted as qualitative and quantitative ions.In the mass concentrations ranged from 0.05 to 2 mg/L,the linear correlation coefficient of the standard curve was greater than 0.9999.The recoveries of SPS and MPS were 96.8%-106.7%with the relative standard deviation less than 2.0%(n=6).The detection limited of SPS and MPS were 0.0030 mg/L and 0.0036 mg/L,respectively,and quantification limits were 0.0100 mg/L and 0.0120 mg/L,respectively.This analysis method can be applied to the monitoring and analysis of trace sodium thiopropane sulfonate brightener of electroplate liquid in electroplate factory.

关 键 词：酸铜电镀液 高效液相色谱串联质谱法 聚二硫二丙烷磺酸钠 3-巯基-1-丙烷磺酸钠 

分 类 号：O657.6[理学—分析化学]