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dc.contributor.advisorWilson, Lee D.en_US
dc.creatorMahmud, Sarker Tareken_US
dc.date.accessioned2007-09-17T15:39:58Zen_US
dc.date.accessioned2013-01-04T04:58:51Z
dc.date.available2008-09-19T08:00:00Zen_US
dc.date.available2013-01-04T04:58:51Z
dc.date.created2007-09en_US
dc.date.issued2007-09-19en_US
dc.date.submittedSeptember 2007en_US
dc.identifier.urihttp://hdl.handle.net/10388/etd-09172007-153958en_US
dc.description.abstractMesoporous silica materials containing microporous cavities provided by covalently bound ¦Â-cyclodextrin (CD ICS) were synthesized by co-condensation of a ¦Â-CD functionalized triethoxy silane (CD ICL) with tetraethyl orthosilicate (TEOS) by using neutral amine surfactants as structure directing agents (SDA). CD ICL was prepared by reacting ¦Â-CD with 3-isocyanatopropyltriethoxysilane. IR spectroscopy of CD ICL showed complete disappearance of isocyanato group at 2270 cm-1. 1H NMR results indicate an average of four isocyanate linkers covalently attached to random hydroxyl substituents of each molecule of ¦Â-CD. Nine different CD ICS materials were synthesized using dodecylamine, tetradecylamine or hexadecylamine with ¦Â-CD (2, 4, and 6 mol %) with respect to TEOS. The incorporation of ¦Â-CD within the mesoporous framework was supported by IR, Raman, MALDI TOF MS, solid state 13C NMR CP-MAS and TGA results. Small angle X-ray diffraction results showed a peak at 2¦È ¡Ö 2.20, supporting the presence of an ordered silica mesostructure framework. For materials with same CD loading, the surface area and pore volume doubled as the surfactant from dodecylamine to hexadecylamine. However, as the CD loading increased from 2% to 6%, the surface area decreases by a factor of ~ 1.5. MALDI TOF mass spectrometry showed two peaks at m/z 1157 a.m.u. and 1173 a.m.u. for [¦Â-CD + Na]+ and [¦Â-CD + K]+ respectively due to desorption of ¦Â-CD from the walls of the silica matrix. The 13C NMR CP MAS results showed 13C signals in the region ¦Ä=60-110 ppm due to the nuclei of ¦Â-CD. CD ICS materials were found to be effective as a sorbent in both gas and aqueous phases, respectively. The sorption capacity (mmol/g) of p-nitrophenol increased from 61% to 84% with an increase of CD loading from 2% to 6% and as the alkyl chain length of the SDA increases from dodecylamine to hexadecylamine. The adsorption isotherm of CH3Cl in the gas phase and that of p-nitrophenol in the aqueous phase at ambient temperature adopts a multilayer model of adsorption.en_US
dc.language.isoen_USen_US
dc.subjectMethyl Chloride gas and p-nitrophenol sorptionen_US
dc.subjectPMOen_US
dc.subjectTGAen_US
dc.subjectNitrogen Porosimetryen_US
dc.subjectHexagonal Mesoporous silicaen_US
dc.subjectSAXDen_US
dc.subjectRamanen_US
dc.subjectCyclodextrinen_US
dc.titleStudies of cyclodextrin functionalised silica materialsen_US
thesis.degree.departmentChemistryen_US
thesis.degree.disciplineChemistryen_US
thesis.degree.grantorUniversity of Saskatchewanen_US
thesis.degree.levelMastersen_US
thesis.degree.nameMaster of Science (M.Sc.)en_US
dc.type.materialtexten_US
dc.type.genreThesisen_US
dc.contributor.committeeMemberWard, Dale E.en_US
dc.contributor.committeeMemberScott, Roberten_US
dc.contributor.committeeMemberOguocha, Ikechukwuka N.en_US


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