A new approach of preparing monolithic silica column was founded by adopting an improved sol-gel technology with tetramethoxysilane and polyethylene glycol as the matrix materials. The reason of resulting in crack and deformation of monolithic column was explained. By using N,N-dimethylformamide and a heat treatment procedure, the problems of crack and deformation in preparing the column were solved and the drying time was shortened greatly. In addition, the methods of fabricating mesopore and the effects of porogen solvent of different concentrations on monolithic silica column were investigated. The results show that the column prepared possessed bimodal pores structures with micrometer-size co-continuous through-pores and silica skeletons which have nanometer-size mesopores, straight appearance, high porosity, good chemical and mechanical stability. The characteristics would favour the separation with a rapid speed and high efficiency for both small molecules and macromolecules.
