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Preparation of Monolithic Capillary Chromatographic Columns Using Supercritical Fluid as a Porogen Solvent

Szumski, Michał, Buszewski, Bogusław
Chromatographia 2014 v.77 no.15-16 pp. 1009-1017
carbon dioxide, ethylene glycol, liquid chromatography, permeability, porosity, proteins, silica, solvents, stainless steel, temperature
Monolithic polymeric beds were synthesized in fused silica capillaries using either trimethylolpropane trimethacrylate (TRIM) or a mixture of butyl methacrylate (BMA) with ethylene glycol dimethacrylate (EDMA) as monomers. Carbon dioxide at temperature and pressure conditions above its critical values was used as a porogen solvent. The purpose of using the supercritical carbon dioxide was to have the possibility of changing the solvation power (and thus the porosity of the resulting monolith) of the porogen by pressure and temperature changes instead of changing the porogen composition. The experiments were performed using a special setup consisting of a stainless steel high-pressure reactor to which the fused silica capillary was connected. The synthesized monoliths underwent liquid chromatographic evaluation. The polyTRIM capillary monoliths were characterized by different permeability, which depended on the pressure of the synthesis. BMA/EDMA columns were applied for separation of alkylbenzenes and a model mixture of proteins.