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在线高效液相色谱-毛细管气相色谱联用方法的建立

Establishment of a Coupling Method of High Performance Liquid Chromatography and Capillary Gas Chromatography

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【作者】 陈吉平黄威东张乐沣田玉增

【Author】 Chen Jiping, Huang Weidong *, Zhang Lefeng and Tian Yuzeng (Dalian Institute of Chemical Physics, the Chinese Academy of Scienses, Dalian, 116012)

【机构】 中国科学院大连化学物理研究所

【摘要】 建立了一种以保留间隙柱技术和阀切换以及定量管样品转移为接口并具有早期溶剂蒸气出口的在线液相色谱与毛细管气相色谱联用方法。考察了主要实验条件,如溶剂蒸发温度、载气压力等对联机系统性能的影响,并用萘和联苯对该系统的线性范围进行了测定。利用联机系统对一种轻柴油样品进行了分析。

【Abstract】 An on line coupling system of normal phase microbore HPLC and capillary GC has been established, in which retention gap technique with on column injection and partially concurrent solvent evaporation with early vapor exit were used. The conditions suitable for the coupling system of HPLC and CGC must be determined experimentally since the factors have to be adjusted with respect to solvent evaporation temperature and column inlet pressure etc. The suitable solvent evaporation temprature for the mobile phase used for this system, n hexane, was about 70℃ A temperature much lower or higher than 70℃ will influence the GC analysis. In addition,solvent evaporation temperature and column inlet pressure are interacting, that is, higher solvent evaporation temperature needs higher inlet pressure. At the above evaporation temperature, the suitable inlet pressure for this system was about 0.2MPa. In order to minimize the extra column effect on the LC peaks, thin transfer line and connectors of zero dead volume between LC column and GC column must be used. The separation and analysis of aromatics in a light diesel fuel was performed by using this system with 15cm×2mm i.d. YGW(5μm) silica LC column and 60m×0 25mm i.d. OV 101 GC column under the above conditions. The analytical results show that the system of on line coupling of HPLC with CGC is a reliable analytical tool for microcomponents in complex mixtures, especially for those requiring sample preparation prior to GC.

【基金】 国家自然科学基金
  • 【文献出处】 色谱 ,CHINESE JOURNAL OF CHROMATOGRAPHY , 编辑部邮箱 ,1997年03期
  • 【分类号】O658/O621
  • 【被引频次】4
  • 【下载频次】97
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