石油学报(石油加工) ›› 2018, Vol. 34 ›› Issue (2): 373-379.doi: 10.3969/j.issn.1001-8719.2018.02.020

• 研究报道 • 上一篇    下一篇

石脑油中杂质元素的快速质谱分析

聂西度1,谢华林2   

  1. 1. 湖南工学院 材料与化学工程系,湖南 衡阳 421002;
    2. 长江师范学院 化学化工学院,重庆 涪陵 408100
  • 收稿日期:2017-05-08 修回日期:2017-06-21 出版日期:2018-03-25 发布日期:2018-05-24
  • 通讯作者: 谢华林,男,教授,博士,主要从事材料化学的研究与应用;E-mail:hualinxie@vip.163.com E-mail:hualinxie@vip.163.com
  • 作者简介:第一作者:聂西度,男,教授,博士,主要从事质谱分析方法的研究与应用
  • 基金资助:
    国家自然科学基金项目(21271187)、;重庆市高校优秀成果转化项目(KJZH17131)、湖南省自然科学基金资助项目(14JJ5032)和湖南省教育厅重点科研项目(14A035)资助

Rapid Determination of Impurity Elements in Naphtha by Inductively Coupled Plasma Tandem Mass Spectrometry

NIE Xidu1, XIE Hualin2   

  1. 1. Department of Material and Chemical Engineering, Hunan Institute of Technology, Hengyang 421002, China;
    2. College of Chemistry and Chemical Engineering, Yangtze Normal University, Fuling 408100, China
  • Received:2017-05-08 Revised:2017-06-21 Online:2018-03-25 Published:2018-05-24

摘要: 研究建立了石脑油中杂质元素的快速分析方法。石脑油样品经无水乙醇简单稀释后,直接采用电感耦合等离子体串联质谱(ICPMS/MS)法测定其中的Si、P、S、Cl。针对复杂基质测定过程中存在的多原子离子干扰,采用MS/MS模式,通过向碰撞反应池(CRC)中加入O2为反应气,使28Si+、31P+、32S+分别与O2发生质量转移反应生成28Si16O+2、31P16O+、32S16O+,从而消除多原子质谱干扰;通过向碰撞反应池(CRC)中加入H2,使35Cl+与H2发生质量转移反应生成H352Cl+消除干扰。28Si16O+2、31P16O+、32S16O+、H352Cl+的检出限分别为015、0058、026和396 μg/L。为验证方法的准确性,分析了国际标准参考物质润滑油(NIST SRM 1848)中Si、P、S、Cl的含量,所测定的结果与标准参考物质所提供的标准值无显著性差异,相对标准偏差(RSD)小于37%,表明所建立的分析方法准确可靠,适合于石脑油中Si、P、S、Cl 4个杂质元素的快速测定。

关键词: 石脑油, 电感耦合等离子体串联质谱, 杂质元素, 碰撞反应池, 质量转移

Abstract: Rapid analysis method has been established for the determination of impurity elements in naphtha. Firstly, the sample is diluted with absolute ethyl alcohol, and then Si, P, S and Cl elements are analyzed by inductively coupled plasma tandem mass spectrometry (ICPMS/MS). It suggests that 28Si16O+2, 31P16O+ and 32S16O+ species are generated via the reaction among 28Si+, 31P+ and 32S+ with O2, respectively, in the MS/MS mode by adding O2 as reaction gas to the collision reaction cell (CRC). Thus, to eliminate the existence and interference of the complex matrix polyatomic interferences, H2 is added to the CRC as the reaction gas, with the generation of H352Cl+ species via the mass shift reaction between 35Cl+ and H2. The detection limits of 28Si16O+2, 31P16O+, 32S16O+ and H352Cl+ are 015 μg/L, 0058 μg/L, 026 μg/L, 396 μg/L, respectively. The accuracy of the analytical method is assessed by the analysis of the standard reference materials NIST SRM 1848 (trace elements in lubricating oil), which shows no significant difference between the measured values and the certified values. The relative standard deviation (RSD) is less than 37%. The measurement procedure is suitable for analyzing Si, P, S and Cl elements in naphtha.

Key words: naphtha, inductively coupled plasma tandem mass spectrometry, impurity elements, collision reaction cell, mass shift