Date of Award

5-2016

Degree Type

Dissertation

Degree Name

Doctor of Philosophy

Major

Chemistry

Major Professor

Michael J. Sepaniak

Committee Members

Bhavya Sharma, Jimmy W. Mays, Dawnie W. Steadman

Abstract

The purpose of this dissertation is to develop analytical methods that aid in the detection of forensic analytes. Forensic analytes require methods with increased sensitivity and low limit of detection capabilities. Improvements in separation techniques, surface enhanced Raman spectroscopic techniques, and wire-less gas sensing can each assist in the detection of trace evidence.

When surface enhanced Raman is coupled with thin-layer chromatography a mixture of compounds can be separated and transferred to a metal substrate to be detected using Raman spectroscopy. Surface enhanced Raman scattering enhances the Raman signal intensity by placing a metal substrate in close proximity to an analyte. The new method gives a chemically specific intensified signal along with a chromatographic separation. A traditional separation is performed on a TLC plate, allowed to dry, wetted with a solvent, placed in contact with a metal substrate, and detected using Raman. More efficient chromatographic platforms can be implemented with this method.

New efficient chromatographic platforms are also beneficial to the detection of forensic analytes. Recently, photolithographically nanofabricated open system pillar arrays have proved to be more efficient separation platforms when compared to traditional TLC. These platforms are a form of ultra-thin layer chromatography. This dissertation describes the effects of manipulation on the inter-pillar gap distances with respect to band dispersion. The studies herein manipulate the pillar arrays in order to optimize the separation platform.

The third method developed involved gas sensing of volatile organic compounds. An amorphous ferromagnetic micro-wire was coated with a polymer, where the polymer swelled in response to the gas introduced. When the gas caused the polymer to swell a differential stress response was applied on the micro-wire. The fabricated sensor was tested on simple organic gases but has capabilities to detect low concentrations of low vapor pressure forensic analytes.

All three projects were significant advancements in analytical method development. The analytes used were either fluorescent dyes or volatile organic compounds to test feasibility of each method. More efficient chromatographic platforms were fabricated, surface enhanced Raman was coupled to TLC, and a micro-wire gas sensor was calibrated for the studies performed in this dissertation.

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