Fourier transform infrared spectrometric detection of chromatographic effluents: instrumental and methodological improvements using a flow cell interface

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dc.contributor.authorJohnson, Charles Clifforden
dc.contributor.committeechairTaylor, Larry T.en
dc.contributor.committeememberDorn, Harry C.en
dc.contributor.committeememberBell, Harold M.en
dc.contributor.committeememberGraybeal, Jack D.en
dc.contributor.committeememberDillard, John G.en
dc.contributor.committeememberMcNair, Harold M.en
dc.contributor.departmentChemistryen
dc.date.accessioned2015-07-10T20:00:08Zen
dc.date.available2015-07-10T20:00:08Zen
dc.date.issued1985en
dc.description.abstractThe 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.en
dc.description.degreePh. D.en
dc.format.extentxii, 123 leavesen
dc.format.mimetypeapplication/pdfen
dc.identifier.urihttp://hdl.handle.net/10919/54450en
dc.language.isoen_USen
dc.publisherVirginia Polytechnic Institute and State Universityen
dc.relation.isformatofOCLC# 12607230en
dc.rightsIn Copyrighten
dc.rights.urihttp://rightsstatements.org/vocab/InC/1.0/en
dc.subject.lccLD5655.V856 1985.J632en
dc.subject.lcshFourier transform spectroscopy -- Experimentsen
dc.subject.lcshInfrared spectroscopy -- Experimentsen
dc.subject.lcshLiquid chromatography -- Experimentsen
dc.titleFourier transform infrared spectrometric detection of chromatographic effluents: instrumental and methodological improvements using a flow cell interfaceen
dc.typeDissertationen
dc.type.dcmitypeTexten
thesis.degree.disciplineChemistryen
thesis.degree.grantorVirginia Polytechnic Institute and State Universityen
thesis.degree.leveldoctoralen
thesis.degree.namePh. D.en

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