The present invention relates to capillary columns including a monolith and a method for preparing a capillary column including a monolith. The monolith can be prepared by a sol gel method, and in the transformation from hydrosol to hydrogel, the monolith undergoes essentially no syneresis or volume shrinkage. Thus, deleterious effects of syneresis are avoided, such as the formation of channels having large dimensions that provide a pathway of least resistance for a mobile phase to effectively bypass portions of a stationary phase. The method for preparing a column having a monolith that undergoes essentially no syneresis involves a hydrogel solution that has a relatively low concentration of SiO2, i.e. less than about 5 g/100 mL.
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