Date of Award
10-1982
Document Type
Dissertation - Restricted
Degree Name
Doctor of Philosophy (PhD)
Department
Chemistry
First Advisor
Daniel Haworth
Second Advisor
Bruce Pollard
Third Advisor
Karen Fallgatter
Fourth Advisor
Michael D. Ryan
Fifth Advisor
David Schrader
Abstract
A continuum source atomic fluorescence spectrometer (CSAFS) has been constructed for use in high performance liquid chromatography (HPLC). The design is described in detail, and analytical figures of merit such as reproducibility and limits of detection are presented for the spectrometer.
The CSAF spectrometer was interfaced to a high performance liquid chromatograph for metal specific detection. Details of this interface are presented, as well as performance characteristics of the interfaced system. The HPLC-CSAFS system was used to speciate cadmium ion from cadmium complexed to soil fulvic a new method for determining the stability constant of that reaction based on this separation is presented.
The peak shapes of the system are described in terms of two models. These models examine the physical and chemical processes of the detector and how these processes affect the peak shape. Computer simulations are used to fit experimental data to the models.
A theoretical framework is described which extends present signal-to-noise theory for static systems to dynamic, time-dependent methods. These equations define dynamic figures of merit, particularly signal-to-noise ratio and limit of detection, in terms of their static system counterparts. The postulations are verified by experimentation on the HPLC-CSAFS system and by computer simulation of noise processes.