Behavior of short silica monolithic columns in high pressure gas chromatography

In order to analyze light hydrocarbons mixtures with silica monolithic columns, a conventional gas chromatograph was modified to work with carrier gas pressure as high as 60bar. To understand hydrodynamic flow and retention with short columns (less than 30cm), special attention was required due to the temperature difference between the oven area and the FID detector which contain a significant length of the column. Efficiency and selectivity using various carrier gases (helium, nitrogen and carbon dioxide) at different inlet pressure for different oven temperature were studied. Carrier gas nature was a very significant parameter: on one side, linked to adsorption mechanism for gases like nitrogen and carbon dioxide onto the stationary phase modifying retention and selectivity, on the other side in relation to the minimum theoretical plate height which was as low as 15μm (66 000 platem(-1)) using carbon dioxide as carrier gas. The chromatographic system was then used to separate methane, ethane, ethylene, acetylene, propane, cyclopropane, and butane in less than 30s.