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Synthesis and modifications of materials for separation science
Umeå University, Faculty of Science and Technology, Department of Chemistry.
2008 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

This thesis deals with the preparation of materials for use in separation science and their surface modification by grafting. The overall aim is the preparation of diverse materials by combination of a set of developed tools.

Included in the thesis is the synthesis of monolithic media using non-traditional crosslinkers, the characterization of their porous properties and initial testing in reversed-phase chromatographic separation of proteins. The preparation of a library of short polymer chains, telomers, with varied functionality and their characterization is reported. Included in the characterization is the gradient polymer elution chromatography of selected telomers on a monolithic column in capillary format. The technique shows promise as a tool for monitoring of polymerization processes and for the separation of telomers with similar size but different functionalities or characteristics.

Finally, the combination of polymeric support materials and the prepared telomer library is used in surface modification. Surface modification is performed onto activated surfaces via a “grafting to” approach. One example is shown, the surface modification of epoxy-modified divinylbenzene particles by attachment of telomer chains introducing ion-exchange functionality. The material is tested for the separation of proteins, in ion-exchange chromatography mode.

Place, publisher, year, edition, pages
Umeå: Kemi , 2008. , 43 p.
Keyword [en]
material synthesis, monolith, surface modification, telomer, “grafting to”, gradient polymer elution, chromatography
National Category
Other Basic Medicine
Identifiers
URN: urn:nbn:se:umu:diva-1572ISBN: 978-91-7264-528-8 (print)OAI: oai:DiVA.org:umu-1572DiVA: diva2:141414
Public defence
2008-03-28, N360, Naturvetarhuset, Umeå Universitet, Umeå, 10:00 (English)
Opponent
Supervisors
Available from: 2008-03-07 Created: 2008-03-07 Last updated: 2017-05-18Bibliographically approved
List of papers
1. Extending the array of crosslinkers suitable for the preparation of polymethacrylate-based monoliths
Open this publication in new window or tab >>Extending the array of crosslinkers suitable for the preparation of polymethacrylate-based monoliths
2005 (English)In: Journal of Separation Science, ISSN 1615-9306, E-ISSN 1615-9314, Vol. 28, no 17, 2401-2406 p.Article in journal (Refereed) Published
Abstract [en]

The in situ preparation of monolithic capillary columns comprising copolymers of butyl methacrylate with ethylene dimethacrylate, diethylene glycol dimethacrylate, triethylene glycol dimethacrylate, and pentaerythritol tetraacrylate using thermal polymerization within 250 mu m ID capillaries and their application for mu-HPLC separations of proteins has been studied. For all crosslinkers, optimization of the porogenic mixture consisting of 1-propanol and 1,4-butanediol yielded monoliths with pore sizes above 1 mu m suitable for rapid separations at low back pressure. Very good separations were achieved for a protein mixture consisting of ribonuclease A, cytochrome c, myoglobin, and ovalbumin with all tested columns.

Keyword
capillary, crosslinker, mu-HPLC, monolith, monolithic column, polymerization, pore size, protein separation, reverse phase
Identifiers
urn:nbn:se:umu:diva-13015 (URN)10.1002/jssc.200500222 (DOI)
Available from: 2007-04-27 Created: 2007-04-27 Last updated: 2017-12-14Bibliographically approved
2. A Library of Thiol-Terminated Methacrylate Telomers Prepared by Photo-Initiated Iniferter Mediated Ppolymerization for use in
Open this publication in new window or tab >>A Library of Thiol-Terminated Methacrylate Telomers Prepared by Photo-Initiated Iniferter Mediated Ppolymerization for use in
(English)Manuscript (preprint) (Other (popular science, discussion, etc.))
Identifiers
urn:nbn:se:umu:diva-2996 (URN)
Available from: 2008-03-07 Created: 2008-03-07 Last updated: 2010-01-14Bibliographically approved
3. Gradient polymer elution chromatography of methacrylate Telomers on monolithic capillary columns prepared by nitroxide-mediated polymerization
Open this publication in new window or tab >>Gradient polymer elution chromatography of methacrylate Telomers on monolithic capillary columns prepared by nitroxide-mediated polymerization
(English)Manuscript (preprint) (Other academic)
Abstract [en]

Linear methacrylate telomers prepared by isopropylxanthic disulfide photoiniferted polymerization of 2-hydroxyethyl methacrylate, methyl methacrylate, and ethyl methacrylate have been separated from their precursor monomers using gradient polymer elution chromatography (GPEC) on a monolithic capillary column. The capillary monoliths were prepared by thermally initiated radical polymerization of styrene and divinylbenzene controlled by 1-carboxy-PROXYL stable free radicals, and characterized by nitrogen adsorption and mercury intrusion porosimetry. The separations in GPEC mode were performed using a mobile phase gradient from water to methanol, where water is the non-solvent and methanol the good solvent with respect to the telomers. Successful separation of telomers from their monomer was achieved for all tested telomers. In addition, it was observed that the retention times of the intact telomers were different from those of telechelic oligomers produced by hydrolysing the isopropylxanthic terminals. The current set-up is therefore promising both for monitoring of the progress of photoiniferted polymerizations and to monitor the hydrolysis of resulting polymerized oligomers into thiol-terminated telechelics.

Keyword
Gradient polymer elution chromatography, telechelics, living polymerization, monoliths, separation of polymers
National Category
Analytical Chemistry Polymer Chemistry
Research subject
Analytical Chemistry
Identifiers
urn:nbn:se:umu:diva-30309 (URN)
Available from: 2009-12-16 Created: 2009-12-16 Last updated: 2017-05-18Bibliographically approved
4. A cation-exchange material for protein separations based on grafting of thiol-terminated sulfopropyl methacrylate telomers onto hydrophilized monodisperse divinylbenzene particles
Open this publication in new window or tab >>A cation-exchange material for protein separations based on grafting of thiol-terminated sulfopropyl methacrylate telomers onto hydrophilized monodisperse divinylbenzene particles
2008 (English)In: Journal of Separation Science, ISSN 1615-9306, E-ISSN 1615-9314, Vol. 31, no 12, 2143-2150 p.Article in journal (Refereed) Published
Abstract [en]

A strong cation-exchange separation material has been prepared from monodisperse divinylbenzene particles modified by a grafting to approach, utilizing as anchoring points epoxy groups introduced onto the surface of the particles via oxidation of residual vinyl groups. The grafted chains consisted of thiol-terminated telomers of sulfopropyl methacrylate prepared by iniferter mediated polymerization, and grafting was performed by reaction of the corresponding thiolate anion with the surface epoxy groups. Attachment through epoxy moieties that were subsequently converted into 2,3-propanediol groups increased the hydrophilicity of the polymeric particles and incubation experiments showed no signs of the proteins denaturing on the column during an extended contact time of 1 h at room temperature. The performance of the grafted material was demonstrated by the chromatographic separation of cytochrome C, lysozyme, myoglobin, and ribonuclease A, in a cation-exchange mode.

Keyword
Grafting to, Photoinitiation, Polymeric particles, Protein separation, Precipitation polymerization
Identifiers
urn:nbn:se:umu:diva-10270 (URN)doi:10.1002/jssc.200800180 (DOI)18615833 (PubMedID)
Available from: 2008-08-06 Created: 2008-08-06 Last updated: 2017-12-14Bibliographically approved

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