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Porous structure of the monolithic sorbent and separation properties of monolithic capillary columns in gas and liquid chromatography

机译:气相色谱和液相色谱中整体吸附剂的多孔结构和整体毛细管柱的分离特性

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Macroporous polymer based on polydivinylbenzene was used for the preparation of monolithic capillary columns with the diameter from 0.01 to 0.53 mm for separations by gas and liquid chromatography. The separation properties of the columns were studied by analysis of model systems of aromatic (in liquid chromatography) and light (in gas chromatography) hydrocarbons. The permeability was determined and the C parameter of the Van-Deemter equation was found for each column. The permeability of the majority of columns determined by gas chromatography is independent of the column diameter. The permeability of the same columns in liquid chromatography is also almost constant for the columns 0.53-0.1 mm in diameter; however, the permeability decreases sharply on going to columns of smaller diameter. In gas chromatography the value of the C parameter reflecting the effect of the mass transfer of the sorbate between the mobile and stationary phases on the smearing of a chromatographic peak in the column approximately the same for all columns. In liquid chromatography the value of the C coefficient in the Van-Deemter equation for the same capillary columns changes with a change in the column diameter and reaches a minimum for the columns 0.1 mm in diameter. The differences observed for the characteristics of the columns in gas and liquid chromatography are due to different structures of the macroporous monolith formed in columns of different diameter and to the effect of solvation of the monolith by the mobile phase under the conditions of liquid chromatography.
机译:基于聚二乙烯基苯的大孔聚合物被用于制备直径为0.01至0.53 mm的整体式毛细管柱,以通过气相色谱和液相色谱分离。通过分析芳烃(液相色谱)和轻质(气相色谱)烃的模型系统,研究了色谱柱的分离性能。确定渗透率,并为每列找到Van-Deemter方程的C参数。通过气相色谱法测定的大多数色谱柱的渗透率与色谱柱直径无关。对于直径为0.53-0.1 mm的色谱柱,液相色谱中相同色谱柱的渗透率也几乎恒定;然而,渗透率在进入直径较小的色谱柱时会急剧下降。在气相色谱中,C参数的值反映了在流动相和固定相之间山梨酸酯的传质对色谱图中色谱峰涂片的影响,所有色谱柱的色谱图大致相同。在液相色谱中,相同毛细管色谱柱的Van-Deemter方程中的C系数值随色谱柱直径的变化而变化,并且对于直径为0.1 mm的色谱柱达到最小值。在气相色谱和液相色谱中观察到的色谱柱特性差异是由于在不同直径的色谱柱中形成的大孔整料结构不同以及液相色谱条件下流动相对整料的溶剂化作用所致。

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