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高速气相色谱法:各种概念概述

High-speed gas chromatography: an overview of various concepts.

作者信息

Cramers C A, Janssen H G, van Deursen M M, Leclercq P A

机构信息

Eindhoven University of Technology, Department of Chemical Engineering and Chemistry, The Netherlands.

出版信息

J Chromatogr A. 1999 Sep 24;856(1-2):315-29. doi: 10.1016/s0021-9673(99)00227-7.

Abstract

An overview is given of existing methods to minimise the analysis time in gas chromatography (GC) being the subject of many publications in the scientific literature. Packed and (multi-) capillary columns are compared with respect to their deployment in fast GC. It is assumed that the contribution of the stationary phase to peak broadening can be neglected (low liquid phase loading and thin film columns, respectively). The treatment is based on the minimisation of the analysis time required on both column types for the resolution of a critical pair of solutes (resolution normalised conditions). Theoretical relationships are given, describing analysis time and the related pressure drop. The equations are expressed in reduced parameters, making a comparison of column types considerably simpler than with the conventional equations. Reduction of the characteristic diameter, being the inside column diameter for open tubular columns and the particle size for packed columns, is the best approach to increase the separation speed in gas chromatography. Extremely fast analysis is only possible when the required number of plates to separate a critical pair of solutes is relatively low. Reducing the analysis time by reduction of the characteristic diameter is accompanied by a proportionally higher required inlet pressure. Due to the high resistance of flow of packed columns this seriously limits the use of packed columns for fast GC. For fast GC hydrogen has to be used as carrier gas and in some situations vacuum-outlet operation of capillary columns allows a further minimisation of the analysis time. For fast GC the columns should be operated near the conditions for minimum plate height. Linear temperature programmed fast GC requires high column temperature programming rates. Reduction of the characteristic diameter affects the sample capacity of the "fast columns". This effect is very pronounced for narrow-bore columns and in principle non-existing in packed columns. Multi-capillary columns (a parallel configuration of some 900 narrow-bore capillaries) take an intermediate position.

摘要

本文综述了气相色谱(GC)中现有的用于缩短分析时间的方法,这也是科学文献中众多出版物的主题。比较了填充柱和(多)毛细管柱在快速GC中的应用。假定固定相对峰展宽的贡献可忽略不计(分别为低液相负荷和薄膜柱)。该处理基于两种柱型在分离一对关键溶质时所需分析时间的最小化(分辨率归一化条件)。给出了描述分析时间和相关压降的理论关系。这些方程用简化参数表示,使得柱型之间的比较比传统方程简单得多。减小特征直径是提高气相色谱分离速度的最佳方法,特征直径对于开管柱是柱内径,对于填充柱是颗粒尺寸。只有当分离一对关键溶质所需的塔板数相对较低时,才可能实现极快速的分析。通过减小特征直径来缩短分析时间会相应地增加所需的入口压力。由于填充柱的高流动阻力,这严重限制了填充柱在快速GC中的应用。对于快速GC,必须使用氢气作为载气,在某些情况下,毛细管柱的真空出口操作可进一步缩短分析时间。对于快速GC,柱应在接近最小板高的条件下操作。线性程序升温快速GC需要高的柱温程序升温速率。特征直径的减小会影响“快速柱”的样品容量。这种影响在窄口径柱中非常明显,而在填充柱中原则上不存在。多毛细管柱(约900根窄口径毛细管的平行配置)处于中间位置。

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