Abstract
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.Electronic supplementary materialThe online version of this article (doi:10.1007/s10337-014-2651-7) contains supplementary material, which is available to authorized users.
Highlights
During last two decades, monolithic macroporous materials have become very popular in analytical chemistry and in separation science because of several advantages they provide
According to the reports of Cooper et al [37,38,39], such monomers or their mixtures as TRIM, ethylene glycol dimethacrylate (EDMA) and TRIM/MAA dissolve in SC-CO2 and can polymerize to form a monolith if the monomer concentration is higher than 40 %
We did not observe any differences in the morphology of the polymers if only the initial pressure exceeded 10.3 MPa at 60 °C
Summary
Monolithic macroporous materials have become very popular in analytical chemistry and in separation science because of several advantages they provide. Monoliths can be synthesized in different formats—from classical columns through capillaries to channels of chip devices. In comparison to particulate-based stationary phases beds, they provide much higher mass transfer [1,2,3,4,5]. A serious advantage of the monolithic supports over particulate materials is their easy (in general) way of preparation which relies on a chemical process (polymerization or polycondensation) induced in a liquid solution, which is introduced into a tube or a chip channel [6]. There have been elaborated several types of monolithic stationary phases, namely silica, polymer-based and those of mixed inorganic–organic nature [7,8,9,10,11]
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