Synthesis and characterization of stationary phases for reversed-phase liquid chromatography

Reversed-phase liquid chromatography (RPLC) is a very important analytical separations technique. The role of the stationary phase in RPLC has been under investigation for several years. These previous studies have been very fundamental in nature in an attempt to understand the retention mechanism of RPLC. This current research involves the investigation of some of the more practical and applied aspects of reversed-phase packings, especially with regard to the bonding density of C{dollar}sb{lcub}18{rcub}{dollar} chains on the surface of silica-based packings.; Synthetic methods were evaluated in an attempt to increase the C{dollar}sb{lcub}18{rcub}{dollar} bonding density. Sub-ambient temperature ultrasonic reactions were previously developed in our laboratory. The use of a variable power ultrasonic probe and the use of the addition of a second solvent for these sub-ambient temperature reactions were investigated.; Some of the bonding reaction conditions for reversed-phase packings have not been exhaustively studied. The effect of the silica pore size on the bonding reaction was studied over a range of 80 A to 300 A. The effect of sub-ambient temperatures on the kinetics of the bonding reaction was also investigated.; The role of bonding density on chromatographic parameters has long been ignored in the literature. Columns of varying bonding densities were evaluated for the effect on chromatographic efficiency, selectivity, and resolution. Also investigated was the effect of bonding density on the pH stability of phases under alkaline conditions. Finally the role of the C{dollar}sb{lcub}18{rcub}{dollar} bonding density on the loading capacity of both small organic molecules and proteins was determined.