Doctoral Dissertations

Date of Award

3-1987

Degree Type

Dissertation

Degree Name

Doctor of Philosophy

Major

Chemistry

Major Professor

Michael J. Sepaniak

Abstract

The experimental parameters affecting efficiency and selectivity in micellar electrokinetic capillary chromatography (MECC) were investigated. The use of the technique to separate the metabolites of vitamin B6 and the quantitation of pyridoxic acid in urine are also presented.

The observed efficiency in a chromatographic technique is dependent upon many experimental factors. The effect of the injection procedures on the observed efficiency was evaluated. The operational parameters of injection voltage and duration of the injection process for electroinjection procedures were examined. Recommendations for injection procedures are discussed for the minimization of injection contributions to band broadening. The effects on the observed efficiency of column parameters were evaluated. Van Deemter type plots were constructed to examine the individual contributions to band broadening in MECC. Column diameter, buffer concentration, applied voltage, and surfactant concentration were studied to elucidate their role in the separation process.

The diversity of available stationary and mobile phases increases the versatility of any chromatographic technique. In MECC the micelles in the mobile phase perform the function of a stationary phase in conventional liquid chromatography. The applicability of four surfactant systems was examined. Test solutes were used to gauge the performance of each micellar system.

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