A bonded polyoxyethylene phase for gas and liquid chromatography

Abstract

Bonded phases were produced by reacting 2,4,7,9-tetramethyl-5-decyne-4,7-bis(polyethyleneoxide 30 mol) ether (Surf[Formula: see text]nol® 485) with silicic supports of high and low surface area. There is circumstantial evidence (a) that the nonextractable layer is held by multiple hydrogen bonding and (b) that the synthesis of these packings involves a reaction at the crosslinking site of the surfactant. The bonded phases, with layer thicknesses between 10 and 30 Å, were tested with three chromatographic techniques. In gas–solid chromatography, the phase proved well deactivated and yielded a reduced plate height of 2.5 (using a silica gel support). In gel permeation chromatography, polyethyleneglycols eluted within the mobile-phase volume. In liquid–solid (normal-phase adsorption) chromatography, the elution pattern differed significantly from that of unmodified silica gel. In each case, high-efficiency separations were obtained. The chromatographic experiments thus demonstrated the potential usefulness of the new phase for both gas and liquid chromatography. However, it was not tested in direct comparison with conventional phases nor was its utility established by subjecting it to routine analytical use.