色谱

色谱

• “多维色谱”专栏 • 上一篇    下一篇

全二维气相色谱第二维死时间的测定

孔宏伟,叶芬,路鑫,董明荃,郭蕾,许国旺   

  1. National Chromatographic R. &A. Center, Dalian Institute of Chemical Physics, The Chinese Academy of Sciences, Dalian 116011, China
  • 收稿日期:2004-05-13 修回日期:1900-01-01 出版日期:2005-01-30 发布日期:1989-03-25
  • 通讯作者: 许国旺
  • 基金资助:

Dead Time Determination of the Second Dimension in a Com-prehensive Two-Dimensional Gas Chromatography

KONG Hongwei, YE Fen, LU Xin, DONG Mingquan, GUO Lei, XU Guowang   

  1. National Chromatographic R. &A. Center, Dalian Institute of Chemical Physics, The Chinese Academy of Sciences, Dalian 116011, China
  • Received:2004-05-13 Revised:1900-01-01 Online:2005-01-30 Published:1989-03-25
  • Contact: Guowang xu

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摘要： 建立了两种恒压模式下全二维气相色谱第二维死时间的测定方法。一种方法是利用不同压力下的相对保留时间差规律,计算非同步调制的全二维气相色谱第二维的保留时间,再利用正构烷烃同系物的保留规律线性拟合计算第二维的死时间;测定的第二维的死时间与温度的线性相关系数大于0.997。另一种方法是在已知化合物保留因子和温度关系的条件下,在一次程序升温中测定此化合物的3个以上不同流出温度条件下的表观保留时间,再根据该表观保留时间计算出死时间与温度的关系。实验结果表明,两种方法对死时间测定的偏差小于0.05 s。这两种方法适合于各种类型的全二维气相色谱,无论其调制方式是同步还是非同步。

关键词: 第二维死时间, 全二维气相色谱, 正构烷烃

Abstract: Comprehensive two-dimensional gas chromatography (GC×GC) is rapidly gaining importance for the analysis of complex samples. In order to predict chromatogram and optimize the operational conditions, the dead time of each dimension should be obtained exactly. Two methods to calculate the dead time of the second dimension were introduced. In the first method, based on the relationship between the time differences of a series of n-alkanes substances and the apparent retention times under different pressures, the true retention time can be calculated for non-synchronous GC×GC. The retention times of homologous series were used to calculate the dead time. Another rapid method to calculate the dead time of the second dimension is based on three or more apparent retention times in a single temperature programmed chromatographic run. The results show that the dead time of the second dimension can be calculated successfully by using the proposed methods and the deviation between the two methods is less than 0.05 s.

Key words: dead time of the second dimension, n-alkanes , comprehensive two-dimensional gas chromatography