Date of Award

Winter 1994

Project Type

Dissertation

Program or Major

Chemistry

Degree Name

Doctor of Philosophy

First Advisor

Christopher F Bauer

Abstract

The scope of this dissertation covers the development and subsequent utilization of an Evolved Gas Analysis (EGA) instrument using atomic emission from a microwave induced plasma source (MIP) as a detector. The majority of the effort during the course of the project was directed toward the design of a new plasma source that has a capacitively-coupled resonance cavity and a sheathed torch, and resolving a number of technical and scientific problems. This discourse also includes an account of the devices developed for use with the instrumentation.

Three applications are demonstrated. The detection, quantitation, and speciation of 10$\sp{-4}$ to 10$\sp{-6}$ gram quantities of moisture within sedimentary rock by EGA was first addressed. This investigation led to the recognition of the limitations of an older design plasma resonance cavity. Despite the development of plasma source the capacitively-coupled cavity the quantitative analysis was still difficult.

The second EGA application was analysis of trace copper-doped carbonates using a dual-wavelength detection system. The purpose of this study was to try to gain a better understanding of the nature of the association of the copper with the carbonates. No evidence was found for surface precipitates of copper carbonate or copper hydroxide, whose presence was suggested by solubility calculations.

One last application, that did not incorporate the use of EGA, was the use of a dual wavelength detection system for the analysis of Freon$\circler$ refrigerants via the ratio of chlorine and fluorine atomic emission. The instrumentation was tested for the ability to provide selective identification of several Freons$\circler$ and the determination of Freon$\circler$ concentrations in binary mixtures. The results from this study demonstrated the feasibility of the method, although limited quantitative precision was observed.

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