Abstract

Although the airbath oven is a reliable heating method for gas chromatography (GC), resistive heating is needed for higher analytical throughput and on-site chemical analysis because of size, heating rate and power requirements. In the last thirty years, a variety of resistive heating methods were developed and implemented for both benchtop and portable GC systems. Although fast heating rates and low power consumption have been achieved, losses in column efficiency and resolution, complex construction processes and difficulties experienced in recovering damaged columns have also become problematic for routine use of resistively heated columns. To solve these problems, a new resistively heated column technique, which uses metal columns and self-insulated heating wires, was developed for capillary gas chromatography. With this method, the total thermal mass was significantly less than in commercial column assemblies. Temperature-programming using resistive heating was at least 10 times faster than with a conventional oven, while only consuming 1—5% of the power that an oven would use. Cooling a column from 350 °C to 25 °C with an air fan only required 1.5 min. Losses in column efficiency and peak capacity were negligible when compared to oven heating. The major trade-off was slightly worse run-to-run retention time deviations, which were still acceptable for most GC analyses. The resistively heated column bundle is highly suitable for fast GC separations and portable GC instruments. Fabrication technologies for microelectromechanical systems (MEMS) allow miniaturization of conventional benchtop GC to portable, microfabricated GC (µGC) devices, which have great potential for on-site chemical analysis and remote sensing. The separation performance of µGC systems, however, has not been on par with conventional GC. Column efficiency, peak symmetry and resolution are often compromised by column defects and non-ideal injections. The relatively low performance of µGC devices has impeded their further commercialization and broader application. This problem can be resolved by incorporating thermal gradient GC (TGGC) into microcolumns. Negative thermal gradients reduce the on-column peak width when compared to temperature-programmed GC (TPGC) separations. This unique focusing effect can overcome many of the shortcomings inherent in µGC analyses. In this dissertation research, the separation performance of µGC columns was improved by using thermal gradient heating with simple set-ups. The analysis time was ~20% shorter for TGGC separations than for TPGC when wide injections were performed. Up to 50% reduction in peak tailing was observed for polar analytes, which significantly improved their resolution. The signal-to-noise ratios (S/N) of late-eluting peaks were increased by 3 to 4 fold. These results indicate that TGGC is a useful tool for bridging the performance gap between µGC and benchtop GC.

Degree

PhD

College and Department

Physical and Mathematical Sciences; Chemistry and Biochemistry

Rights

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