The influence of the conditions of preparation of divinylbenzene-based polymer monoliths on the properties of monolithic capillary columns for use in gas adsorption chromatography was examined. It was found that the polymerization time and the temperature and composition of the polymerization mixture have an effect on the dynamic and chromatographic properties of the columns. The monolithic capillary columns prepared under the optimal synthesis conditions had the height equivalent of a theoretical plate at the level of 20–30 μm, which is an order of magnitude below that of conventional open tubular columns.

Chromatographing a model mixture of hydrocarbons with various carrier gases (helium, hydrogen, nitrogen, carbon dioxide, and nitrous oxide) was used to study the separation ability of monolithic silica capillary columns. It was revealed that the nature of the carrier gas strongly affects the retention time of the sorbates and the height equivalent to a theoretical plate (HETP) of the column, with the values of both these parameters decreasing in the series He > H₂ > N₂ > CO₂ ∼ N₂O. This effect was found to be more pronounced for normal hydrocarbons than for their isomers. For chromatographing with CO₂ or N₂O under optimum conditions, the HETP was 25–30 μm, a value indicative of a higher specific efficiency of monolithic capillary columns. Theoretical correlations between the HETP and the properties of the mobile phase were considered. As a result, it was concluded that elevated pressures of the carrier gas, which are required to ensure the optimum operation of monolithic capillary columns, may affect the properties of the chromatographic system.