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M.Sc. (Chemistry) / Please refer to full text to view abstract

Thesis (Ph. D.)--University of Wisconsin--Madison, 1981. / Typescript. Vita. eContent provider-neutral record in process. Description based on print version record. Includes bibliographical references (leaves 380-394).

Thesis (Ph. D.)--University of Wisconsin--Madison, 1984. / Typescript. Vita. eContent provider-neutral record in process. Description based on print version record. Includes bibliographical references (leaves 320-336).

Thesis (Ph. D.)--Florida State University, 2005. / Advisor: Dr. John G. Dorsey, Florida State University, College of Arts and Sciences, Dept. of Chemistry and Biochemistry. Title and description from dissertation home page (viewed Sept. 19, 2005). Document formatted into pages; contains xxii, 154 pages. Includes bibliographical references.

Thesis (Ph. D.)--Florida State University, 2005. / Advisor: John G. Dorsey, Florida State University, College of Arts and Sciences, Dept. of Chemistry and Biochemistry. Title and description from dissertation home page (viewed Jan. 25, 2006). Document formatted into pages; contains xxiii, 132 pages. Includes bibliographical references.

The physical and chemical nature of chemically bonded phases used in high performance liquid chromatography have been studied. These bonded phases were characterized by a variety of chromotographic and non-chromatographic experiments. The non-chromatographic techniques included ¹³C NMR and batch extraction methods. The role played by the bonded phase as well as the mobile phase in determining the retention characteristics of the "stationary phase" were determined. The retention of solute molecules on bonded phases was found to be a function of the chain length of the bonded phase, the chemical nature of the bonded molecule, and the type of organic modifier used in the mobile phase. The energetics of the solute-stationary phase interactions was determined by the differential enthalpy and was found to be indicative of a partitioning process between two liquid phases. The retention process was also affected by the surface coverage of the bonded molecule. Optimum retention and separation characteristics were obtained with a hydrocarbon bonded phase of high surface coverage when used with a mobile phase containing a very polar organic modifier. The efficiency of these bonded phases was found to be independent of chain length as well as surface coverage of the bonded molecule. Some bonded phases which have specific functionalities incorporated into the bonded molecule are not true reversed phases. The selectivity of the bonded phases towards polar solute molecules was found to be affected by the type of organic modifier used in the mobile phase. The major accomplishment of this work shows that the stationary phase consists of the bonded molecule as well as trapped mobile phase. The composition of this ternary mixture is a function of the type and amount of bonded material and the type and amount of organic modifier used in the mobile phase.

The use of a new styrene-divinylbenzene copolymer bead, Showdex Polymerpak D-814, as a stationary phase in high-performance liquid chromatography is investigated. Unlike conventional silica-based stationary phases, copolymer beads may be used with both aqueous and organic mobile phases. The effect of the mobile phase on solute retention with the copolymer beads is described. Although the copolymer beads exhibit characteristics of both solid and liquid stationary phases, it is shown that the beads act primarily as a liquid when used with the mobile phases chosen for this work. It is further shown that solute retention on the beads results from dispersion interactions between the solute and the stationary phase. Batch extraction distribution constants are determined to confirm the validity of the distribution model proposed. The chromatographic behavior of a variety of aromatic compounds is described. These range from polycyclic aromatic hydrocarbons to substituted benzenes to phthalate esters. A quantitative measure of the effect of a substituent group on retention is developed from an analysis of the experimental results. This measure is then used to successfully predict the retention behavior of some disubstituted benzene compounds. Some model separations are developed to illustrate the usefulness of this measure. Finally, the implications of this work for gradient elution chromatography are discussed.

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