| This dissertation presents investigations into the use of single-bounce attenuated total internal reflection (ATR) infrared (IR) microspectroscopy as a detector for analytes in solution. The detection of analytes in nonmoving (static) solutions, flow injection, and separation systems are presented. Detection limits of succinylcholine chloride in water are shown to be as low as 21 ppm. A small sampling volume (180 fL) is important in reducing band broadening, and improving mass detection limits in low flow environments. Flow injection measurements demonstrate that the flow rate, injection volume, capillary diameter, and internal reflectance element (IRE) capillary separation distances are important. Improved analyte selectivity over traditional spectroscopic techniques is evaluated using high-performance liquid chromatography, capillary electrophoresis (CE), and polymermediated CE. Background electrolyte concentration has been found to play a large role in separation resolution and peak characteristics, which in turn affects infrared spectral quality. The choice of detector, and the preconcentration of analytes in solution using a reverse phase coating applied to a zirconia sol-gel, can have a large effect on detection limit. Future directions that reduce the detection limit, set-up time, and the creation of an infrared integrated cell are outlined. Finally, undergraduate analytical and physical chemistry labs are presented using modular spectrometers to construct UV/Vis, fluorescence, Raman, and atomic emission instruments. |
