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Fabrication and characterization of nano-agglomerated monolithic stationary phases for separation science

Alwy, Ali (2013) Fabrication and characterization of nano-agglomerated monolithic stationary phases for separation science. Master of Science thesis, Dublin City University.

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Abstract

The following thesis provides an extensive study into the fabrication, surface modification and physical characterisation of polymer monoliths in capillary formats. These polymer monoliths were subsequently immobilised with metal oxide nanoparticles for separation of phosphorylated compounds. The fabricated monolithic columns in capillary format, in all instances, were modified with diethylamine and subsequently immobilised with citrate stabilised iron oxide nanoparticles. The monolithic stationary phases were characterised using back pressure and sC4D measurements, which can provide information on the reproducibility and density of the stationary phase. Citrate stabilised iron oxide nanoparticles (Fe3O4 NP’s) with a particle size of 15.8 nm were electrostatically immobilised on a poly(butylmethacrylate-co-ethylene dimethacrylate) monolith bearing grafted functional polymer chains with quaternary amine groups resulting in homogeneous and high density coverage of iron oxide nanoparticles on the monolithic column demonstrated by FE-SEM images. The monolithic column immobilised with Fe3O4 nanoparticles was connected to a HPLC instrument and used in the separation of phosphorylated compounds such as adenosine, adenosine monophosphate, adenosine diphosphate and adenosine triphosphate using gradient elution. In a related study, commercially available centrifugally driven solid-phase extraction silica monoliths were immobilised with 15.8 nm citrate stabilised iron oxide nanoparticles with a dense coverage without detrimental blockage of the flow-through macropores. Since Fe3O4 is known to form reversible complexes with phosphorylated species, the silica monoliths were subsequently used for the enrichment of selected nucleotides and phosphorylated peptides.

Item Type:Thesis (Master of Science)
Date of Award:November 2013
Refereed:No
Supervisor(s):White, Blánaid and Connolly, Damian and Paull, Brett
Uncontrolled Keywords:stationary phase; HPLC; monolith
Subjects:Physical Sciences > Analytical chemistry
Physical Sciences > Nanotechnology
Physical Sciences > Chemistry
DCU Faculties and Centres:DCU Faculties and Schools > Faculty of Science and Health > School of Chemical Sciences
Use License:This item is licensed under a Creative Commons Attribution-NonCommercial-No Derivative Works 3.0 License. View License
ID Code:19032
Deposited On:25 Nov 2013 14:53 by Blanaid White. Last Modified 26 Apr 2017 16:20

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