The Fourier Transform Infrared spectrometer (FTIR) has been used increasingly as a detector for various forms of chromatography. Clearly the most established marriage has been that of the Gas Chromatograph (GC) with the FTIR. GC-FTIR has been developed well beyond other forms. The main objective of this thesis, however, is to extend the FTIR as a detector to previously untested forms of chromatography using a flow cell interface. These forms of chromatography include High Performance Liquid Chromatography (HPLC), both normal-phase and reversed-phase, and packed-column Supercritical Fluid Chromatography (SFC).
Normal phase HPLC-FTIR was demonstrated on not only analytical scale columns, but semi-preparative and microbore scales as well. Significant advantages, particularly with respect to the low solvent consumption, were found in the microbore HPLC-FTIR experiment. This led to the development of a chromatographically improved flow cell, the Zero Dead Volume (ZDV) HPLC-FTIR interface. The ZDV cell shows superior chromatographic characteristics and has unique spectrometric characteristics because of its unusual cross-section. Detection limits as low as 40 ng were observed.
Extension to reversed-phase HPLC-FTIR required incorporation of the Flow Injection Analysis (FIA) technique of low-dispersion flowing extraction. The compounds separated by HPLC are extracted into an infrared-transparent solvent, and the extracted compounds are detected by similar means to normal-phase HPLC-FTIR.
Investigation of SFC-FTIR incorporated a high-pressure, gold-lined lightpipe flow cell to detect the components separated by the supercritical C0₂/packed-column chromatograph. Several unusual spectrometric characteristics were noted. Detection limits as low as 50 ng were observed with SFC-FTIR. / Ph. D.
Identifer | oai:union.ndltd.org:VTETD/oai:vtechworks.lib.vt.edu:10919/54450 |
Date | January 1985 |
Creators | Johnson, Charles Clifford |
Contributors | Chemistry, Taylor, Larry T., Dorn, Harry C., Bell, Harold M., Graybeal, Jack D., Dillard, John G., McNair, Harold M. |
Publisher | Virginia Polytechnic Institute and State University |
Source Sets | Virginia Tech Theses and Dissertation |
Language | en_US |
Detected Language | English |
Type | Dissertation, Text |
Format | xii, 123 leaves, application/pdf, application/pdf |
Rights | In Copyright, http://rightsstatements.org/vocab/InC/1.0/ |
Relation | OCLC# 12607230 |
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