Novel monolithic columns for microscale liquid chromatography and capillary electrochromatography Public Deposited

http://ir.library.oregonstate.edu/concern/graduate_thesis_or_dissertations/bn999b00f

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  • The challenges prompted by miniaturization of chromatographic systems have led scientists to explore new avenues in the synthesis of stationary phases. Packed capillary columns have found limited application in routine analysis due to a number of technical difficulties, most of which are attributable to the frits. New column designs insure the use of stationary phases with high surface area in columns that do not require fits. This dissertation describes novel designs of fritless capillary columns prepared for capillary electrochromatography (CEC) and micro liquid chromatography (micro LC). Designed especially for CEC, the first class of monolithic colunm presented here comprises the entrapped columns. These are made by trapping particles of chromatographic packing material in a fine network of a silicate or organic based polymer. Due to the simple composition of the entrapment matrix, straightforward manufacturing procedure and modest equipment requirement, the method can readily be transferred to any laboratory and easily automated. Elimination of frits, stabilization of the packed bed and on-the-fly customization of column length render mechanically robust columns that are remarkably stable over time, from which manufacturing imperfections can be easily removed. As the water glass entrapment matrix initially studied was replaced by so! gel derived polymers or organic based polymers, the entrapment procedure was gradually improved, demonstrating minimal influence on the structure and chromatographic properties of the original reverse phase sorbent. High efficiency separations were obtained in both CEC and micro LC formats. This immobilization method was also used to prepare chiral CEC columns by entrapping a molecular imprinted polymeric (MIP) packing having minimal surface charge density, thus being unable to support electroosmotic flow (EOF) without the entrapment matrix. A new type of monolithic stationary phase in which silica beads dictate the porosity of the polymer was also developed. The interstitial space of a chromatographic bed made of silica beads was filled with a mixture of monomers and crosslinker and polymerization was thermally initiated. Subsequent washing of the polymeric rod with an alkaline solution rendered a porous monolith that was used for both micro LC and CEC.
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