色谱

色谱 ›› 2015, Vol. 33 ›› Issue (2): 188-194.DOI: 10.3724/SP.J.1123.2014.10028

• 技术与应用 • 上一篇    下一篇

气相色谱-单光子电离飞行时间质谱的联用及在柴油组分表征中的应用

谢园园1,2, 花磊1, 陈平1, 侯可勇1, 蒋吉春1,2, 王艳1,2, 李海洋1   

  1. 1. 中国科学院分离分析化学重点实验室, 中国科学院大连化学物理研究所, 辽宁 大连 116023;
    2. 中国科学院大学, 北京 100049
  • 收稿日期:2014-10-29 修回日期:2014-11-14 出版日期:2015-02-08 发布日期:2015-01-24
  • 通讯作者: 李海洋
  • 基金资助:

    国家高新技术研究发展计划("863"计划)项目(2014AA06A501,2014AA06A507);国家自然科学基金项目(21275143,21207129).

Coupling of gas chromatography with single photon ionization time-of-flight mass spectrometry and its application to characterization of compounds in diesel

XIE Yuanyuan1,2, HUA Lei1, CHEN Ping1, HOU Keyong1, JIANG Jichun1,2, WANG Yan1,2, LI Haiyang1   

  1. 1. Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China;
    2. University of Chinese Academy of Sciences, Beijing 100049, China
  • Received:2014-10-29 Revised:2014-11-14 Online:2015-02-08 Published:2015-01-24

PDF

209

被引次数

6

摘要：

建立了一种气相色谱(GC)与单光子电离-飞行时间质谱(SPI-TOF MS)联用(GC/SPI-TOF MS)的分析方法。首先,设计了一种双层套管的传输管用于连接GC与SPI-TOF MS,实现了GC与单光子电离离子源的无缝连接。在此基础上,以n-十五烷标准品和苯/甲苯/二甲苯的标准气为对象,对电离源的重要电压参数进行了优化,得到了纯净的分子离子峰,实现了对各类有机物的快速和准确定性。最后,将该方法用于分析柴油中的挥发性与半挥发性有机物,获得了柴油组分的二维GC×SPI-TOF MS谱图。不需要复杂的谱图解析和数据处理,根据谱图中离子的质荷比(m/z)归纳了柴油的主要成分,包括脂肪烃、芳香烃和含量很低的苯并吡咯等含氮化合物;根据色谱的保留时间将柴油中的同分异构体区分开来。结果表明GC/SPI-TOF MS法是一种简单、有效的分析方法,非常适于柴油及复杂环境样品等的分析表征。

关键词: 柴油, 单光子电离, 飞行时间质谱, 复杂环境样品, 挥发性与半挥发性有机物, 气相色谱

Abstract:

A novel analytical method coupling gas chromatography (GC) with single photon ionization time-of-flight mass spectrometry (SPI-TOF MS) has been developed. First of all, a double-wall-tube transfer line was built to combine GC with SPI-TOF MS, which realized seamless connection between GC and SPI ion source. Based on this, standard n-pentadecane and benzene/toluene/xylene standard gas mixtures were used to study important voltage parameters of the ion source. After the optimization of the ion source voltages, pure molecular ion peaks of the analytes were obtained in the mass spectra and qualitative analysis of different kinds of organic compounds were eventually realized rapidly and accurately. At last, GC/SPI-TOF MS was applied to the characterization of volatile and semi-volatile organic compounds in diesel and two-dimensional spectra of GC×SPI-TOF MS were obtained. Without complicated spectra interpretation and data processing, volatile and semi-volatile organic compounds in diesel have been classified qualitatively by ion mass-to-charge ratio (m/z) in SPI mass spectra, including aliphatic compounds, aromatic compounds and nitrogen-containing compounds with low concentration such as benzopyrroles. Isomeric compounds in diesel were separated and identified by retention times of chromatographic peaks. The results indicate that the proposed analytical method of GC/SPI-TOF MS is suitable for the characterization of complicated samples such as diesel and environmental pollutants with easy operation and high efficiency.

Key words: complicated environmental pollutants, diesel, gas chromatography (GC), single photon ionization (SPI), time-of-flight mass spectrometry (TOF MS), volatile and semi-volatile organic compounds

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