Hydrosilation of acetylene compounds for the preparation of a bonded phase in HPLC.

摘要

The goal of this thesis project was to prepare a bonded phase through hydrosilation of acetylenes that could be used as a stationary phase for high performance liquid chromatography (HPLC). HPLC is an important separation tool that is commonly used in many chemical analyses. The compounds selected were propiolic acid, 3,3-dimethyl-1-butyne, phenylacetylene, and 1-phenyl-2-propyn-1-ol. The latter two were packed into HPLC columns. These two were chosen for their different functional groups as well as their relatively short carbon chains.; One of the main focuses of this research was to determine if it is possible to attach two silicon atoms to the terminal carbon atom of each acetylene compound instead of just one silicon atom. This would allow for increased stability of the column as well as the possibility of giving better separations than the columns currently available. Cross Polarization-Magic Angle Spinning Nuclear Magnetic Resonance spectroscopy (CP-MAS NMR) and Diffuse Reflectance Infrared Fourier Transform spectroscopy (DRIFT) were used to verify the success of bonding.; Three classes of compounds were used to examine the viabilities of the phenylacetylene and 1-phenyl-2-propyn-1-ol columns: aromatic compounds, steroids, and benzodiazepines. These were selected in order to compare data from the new stationary phases with that in the literature. All HPLC testing was done in the normal phase mode.