Preparation and characterization of long alkyl chain methacrylate-based monolithic column for capillary chromatography

Abstract

This paper describes the fabrication of long alkyl chain methacrylate monolithic materials for using as stationary phases in capillary liquid chromatography. Following deactivation of the capillary surface with 3-(trimethoxysilyl)propyl methacrylate (γ-MAPS), monoliths were formed by co-polymerisation of stearyl methacrylate (SMA) with ethylene glycol dimethacrylate (EDMA) in the presence of the initiator AIBN and a mixture of porogens including iso-amyl alcohol and 1,4-butanediol. The monoliths were prepared in 100 μm i.d. capillaries and the composition of the polymerisation mixtures were optimised in terms of the ratio of SMA/EDMA, the porogen composition and ratio of porogen to monomers. As the porogen weight fraction decreased, the microglobules became smaller and as expected, the total porosity decreased. In order to determine the usability of such materials, the column permeability K was measured by pumping water through the columns at different linear flow rates. Good results were obtained when these capillaries were used to separate mixtures of weak acids, neutral and basic compounds.