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

Show simple item record

dc.contributor.advisor Glennon, Jeremy D. en
dc.contributor.author Nagle, Amy P.
dc.date.accessioned 2015-08-20T09:09:43Z
dc.date.issued 2014
dc.date.submitted 2014
dc.identifier.citation Nagle, 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.uri http://hdl.handle.net/10468/1931
dc.description.abstract The 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.sponsorship Science Foundation Ireland (SFI Grant 08/SRC/B1412) en
dc.format.mimetype application/pdf en
dc.language.iso en en
dc.publisher University College Cork en
dc.rights © 2014, Amy P. Nagle. en
dc.rights.uri http://creativecommons.org/licenses/by-nc-nd/3.0/ en
dc.subject Silica en
dc.subject Stationary phase en
dc.subject Silica hydride en
dc.subject Supercritical carbon dioxide en
dc.subject Molecular recognition en
dc.title Silica bonded stationary phases: Innovative functionalization methods and novel chromatographic separations based on molecular recognition en
dc.type Doctoral thesis en
dc.type.qualificationlevel Doctoral en
dc.type.qualificationname PhD (Science) en
dc.internal.availability Full text not available en
dc.check.info Indefinite en
dc.check.date 10000-01-01
dc.description.version Accepted Version
dc.contributor.funder Science Foundation Ireland en
dc.description.status Not peer reviewed en
dc.internal.school Chemistry en
dc.check.type No Embargo Required
dc.check.reason Releasing this thesis would cause substantial prejudice to the commercial interests of University College Cork en
dc.check.opt-out Yes en
dc.thesis.opt-out true
dc.check.embargoformat Hard bound copy in Library only en
dc.internal.conferring Autumn Conferring 2014


Files in this item

Files Size Format View

There are no files associated with this item.

This item appears in the following Collection(s)

Show simple item record

© 2014, Amy P. Nagle. Except where otherwise noted, this item's license is described as © 2014, Amy P. Nagle.
This website uses cookies. By using this website, you consent to the use of cookies in accordance with the UCC Privacy and Cookies Statement. For more information about cookies and how you can disable them, visit our Privacy and Cookies statement