In the analysis of solid samples, there are two distinct advantages to performing direct analysis on the solid: (1) minimal sample preparation and (2) avoids potential sample contamination from the reagents used in the dissolution process. The two most common optical techniques for direct solids analysis are arc and spark emission spectroscopy. The most important drawback associated with arc and spark spectroscopy is in the acquistion and interpretation of the spectrum. The development of a custom echelle spectrometer with Charge Injection Device (CID) array detection carried out in these laboratories should be particularly well suited for arc and spark emission spectroscopy. CIDs exhibit many of the best characteristics of photographic film and PMT detection while providing the added advantage of nondestructive readout and Random Access Integration (RAI). This thesis describes the work coupling a spark source to a CID/echelle spectrometer. When properly shielded, the sensitive electronics of the CID function normally in the presence of the spark discharge. The potential for this system to be able to handle the wide variety of spectroscopic situations resulting from the complex spectra typically obtained with this type of excitation is attributed to the flexibility of the instrument which allows the use of alternate line for analysis and internal standard calibration. Additionally, the use of multiple lines has been applied to comparative analysis, monitoring the background for changes in excitation, and determination of the optimum lines to be used for quantification. Effective utilization of the large database of spectral information has lead to the development of sophisticated expert systems such as automated qualitative and semiquantitative analysis routines. Preliminary work with an astigmatism free imaging spectrograph and a Charge Coupled Device (CCD) array detector has shown the ease with which spatial and spectral maps of emission source can be generated. Observation of the spark discharge process in a hope of gaining a clearer picture of the mechanisms of sample excitation seems to be the most rational approach to ultimately obtaining control over the spark process and alleviating the problems associated with sparks excitation.
| Identifer | oai:union.ndltd.org:arizona.edu/oai:arizona.openrepository.com:10150/185942 |
| Date | January 1992 |
| Creators | Pomeroy, Robert S. |
| Contributors | Denton, M. Bonner, Fernando, Quintus, Burke, Michael F., Miller, Walter B., Forster, Leslie |
| Publisher | The University of Arizona. |
| Source Sets | University of Arizona |
| Language | English |
| Detected Language | English |
| Type | text, Dissertation-Reproduction (electronic) |
| Rights | Copyright © is held by the author. Digital access to this material is made possible by the University Libraries, University of Arizona. Further transmission, reproduction or presentation (such as public display or performance) of protected items is prohibited except with permission of the author. |
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