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 05s。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。
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.
出处
《色谱》
CAS
CSCD
北大核心
2005年第1期37-40,共4页
Chinese Journal of Chromatography
基金
国家自然科学基金(No.20175028)
中科院知识创新基金(青年基金)资助.
关键词
全二维气相色谱
第二维死时间
正构烷烃
comprehensive two-dimensional gas chromatography
dead time of the second dimension
n-alkanes
