Doctoral Degrees (Chemistry and Polymer Science)

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Browsing Doctoral Degrees (Chemistry and Polymer Science) by browse.metadata.advisor "Crouch, Endrew"

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    Panaceas and pitfalls in electrodriven chromatographic techniques
    (Stellenbosch : University of Stellenbosch, 2007-12) Buica, Astrid Sorina; Sandra, Pat; Crouch, Endrew; University of Stellenbosch. Faculty of Science. Dept. of Chemistry and Polymer Science.
    In this thesis the main capillary electrodriven chromatographic techniques (i.e. Capillary Electrochromatography CEC, Micellar Electrokinetic Chromatography MEKC and Microemulsion Electrokinetic Chromatography MEEKC) were compared in terms of column manufacturing, fundamental chromatographic performance, and some applications were developed. The first stage of this thesis aimed at developing improved packed and open tubular CEC columns. For the manufacturing of packed CEC columns, the frit-burning step proved of critical importance, together with the slow build-up of the packed bed. The making of open tubular columns is a relatively simple, "one pot" sol-gel reaction taking place in mild conditions. The nature of the gel and the resulting selectivity of the column could easily be changed by changing the precursors. In a second stage of this thesis the packed and open tubular CEC columns were evaluated chromatographically and compared with the results obtained by MEKC and MEEKC. All electrodriven separation techniques showed high efficiencies. The selectivity proved easier to tune with sol-gel chemistry for the making of open tubular columns. Resolution is acceptable for packed CEC, MEKC and MEEKC. For peak capacity, CEC has the advantage of a practically non-limited elution time, while MEKC and MEEKC suffer of the drawback of the existence of an elution window which is limited in time by the elution of the micelles. Some applications were developed in this study on open tubular CEC columns and for the packed CEC columns. Various sugars derivatized with 9- aminopyrene-1,4,6-trisulfonic acid (APTS) could be separated with open tubular CEC, using an octyl, amino or cyano stationary phase. Open tubular columns containing α, β and γ cyclodextrins attached to the stationary phase were developed. This approach proved promising for the separation of positional isomers. A method was developed for the analyses of a mixture of carbamates and for several steroids with packed column CEC directly coupled with MS.