Silica bonded stationary phases: Innovative functionalization methods and novel chromatographic separations based on molecular recognition

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dc.check.date10000-01-01
dc.check.embargoformatHard bound copy in Library onlyen
dc.check.infoIndefiniteen
dc.check.opt-outYesen
dc.check.reasonReleasing this thesis would cause substantial prejudice to the commercial interests of University College Corken
dc.check.typeNo Embargo Required
dc.contributor.advisorGlennon, Jeremy D.en
dc.contributor.authorNagle, Amy P.
dc.contributor.funderScience Foundation Irelanden
dc.date.accessioned2015-08-20T09:09:43Z
dc.date.issued2014
dc.date.submitted2014
dc.description.abstractThe research work included in this thesis examines the synthesis, characterization and chromatographic evaluation of novel bonded silica stationary phases. Innovative methods of preparation of silica hydride intermediates and octadecylsilica using a “green chemistry” approach eliminate the use of toxic organic solvents and exploit the solvating power and enhanced diffusivity of supercritical carbon dioxide to produce phases with a surface coverage of bonded ligands which is comparable to, or exceeds, that achieved using traditional organic solvent-based methods. A new stationary phase is also discussed which displays chromatographic selectivity based on molecular recognition. Chapter 1 introduces the chemistry of silica stationary phases, the retention mechanisms and theories on which reversed-phase liquid chromatography and hydrophilic interaction chromatograpy are based, the art and science of achieving a well packed liquid chromatography column, the properties of supercritical carbon dioxide and molecular recognition chemistry. Chapter 2 compares the properties of silica hydride materials prepared using supercritical carbon dioxide as the reaction medium with those synthesized in an organic solvent. A higher coverage of hydride groups on the silica surface is seen when a monofunctional silane is reacted in supercritical carbon dioxide while trifunctional silanes result in a phase which exhibits different properties depending on the reaction medium used. The differing chromatographic behaviour of these silica hydride materials prepared using supercritical carbon dioxide and using organic solvent are explored in chapter 3. Chapter 4 focusses on the preparation of octadecylsilica using mono-, di- and trifunctional alkoxysilanes in supercritical carbon dioxide and in anhydrous toluene. The surface coverage of octadecyl groups, as calculated using thermogravimetric analysis and elemental analysis, is highest when a trifunctional alkoxysilane is reacted with silica in supercritical carbon dioxide. A novel silica stationary phase is discussed in chapter 5 which displays selectivity for analytes based on their hydrogen bonding capabilities. The phase is also highly selective for barbituric acid and may have a future application in the solid phase extraction of barbiturates from biological samples.en
dc.description.sponsorshipScience Foundation Ireland (SFI Grant 08/SRC/B1412)en
dc.description.statusNot peer revieweden
dc.description.versionAccepted Version
dc.format.mimetypeapplication/pdfen
dc.identifier.citationNagle, A. P. 2014. Silica bonded stationary phases: Innovative functionalization methods and novel chromatographic separations based on molecular recognition. PhD Thesis, University College Cork.en
dc.identifier.urihttps://hdl.handle.net/10468/1931
dc.language.isoenen
dc.publisherUniversity College Corken
dc.rights© 2014, Amy P. Nagle.en
dc.rights.urihttp://creativecommons.org/licenses/by-nc-nd/3.0/en
dc.subjectSilicaen
dc.subjectStationary phaseen
dc.subjectSilica hydrideen
dc.subjectSupercritical carbon dioxideen
dc.subjectMolecular recognitionen
dc.thesis.opt-outtrue
dc.titleSilica bonded stationary phases: Innovative functionalization methods and novel chromatographic separations based on molecular recognitionen
dc.typeDoctoral thesisen
dc.type.qualificationlevelDoctoralen
dc.type.qualificationnamePhD (Science)en
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