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Assessing the macroporous structure of monolithic columns by transmission electron microscopy
Umeå University, Faculty of Science and Technology, Department of Chemistry.
Umeå University, Faculty of Science and Technology, Department of Chemistry.
Umeå University, Faculty of Science and Technology, Department of Computing Science.
Umeå University, Faculty of Science and Technology, Department of Chemistry.
2007 (English)In: Analytical Chemistry, ISSN 0003-2700, E-ISSN 1520-6882, Vol. 79, no 1, 335-344 p.Article in journal (Refereed) Published
Abstract [en]

A set of monolithic stationary phases representing a broad span of monomers and porogens have been characterized directly in their capillary chromatographic format by computational assessment of their pore structure from transmission electron micrographs obtained after in situ embedment of the monoliths in contrast resin, followed by dissolution of the fused-silica tubing, further encasement of the resin-embedded monolith, and microtomy. This technique has been compared to mercury intrusion, a more conventional technique for macroporosity estimation. Supplementing the embedding resin by lead methacrylate gave a negative staining, and the resulting micrographs showed a good contrast between the polymeric monoliths and the embedding resin that allowed studies on the pore formation and polymer development. The technique was also applied to a commercial monolithic silica column.

Place, publisher, year, edition, pages
Columbus, OH: American Chemical Society , 2007. Vol. 79, no 1, 335-344 p.
Keyword [en]
pore-size distributions, mercury intrusion porosimetry, cement-based materials, organic polymer monoliths, capillary electrochromatography, stationary phases, inappropriate method, liquid-chromatography, avoid compression, ion-exchange
URN: urn:nbn:se:umu:diva-12980DOI: 10.1021/ac0614902OAI: diva2:152651
Available from: 2007-06-11 Created: 2007-06-11 Last updated: 2011-03-17Bibliographically approved
In thesis
1. Monolithic separation media synthesized in capillaries and their applications for molecularly imprinted networks
Open this publication in new window or tab >>Monolithic separation media synthesized in capillaries and their applications for molecularly imprinted networks
2006 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

The thesis describes the synthesis of chromatographic media using several different approaches, their characterizations and applications in liquid chromatography. The steps to achieve a separation column for a specific analyte are presented. The main focus of the study was the design of novel molecularly imprinted polymers.

Attachment of monolithic polymeric substrates to the walls of fused silica capillaries was studied in Paper I. With a broad literature survey, a set of common methods were tested by four techniques and ranked by their ability to improve anchoring of polymers. The best procedure was thus used for all further studies.

Synthesis of monoliths in capillary columns was studied in Paper II. With the goal of separating proteins without denaturation, various monoliths were polymerized in situ using a set of common monomers and cross-linkers mixed with poly(ethylene glycol) as porogen. The resulting network was expected to present “protein-friendly pores”. Chemometrics were used to find and describe a set of co-porogens added to the polymerization cocktails in order to get good porosity and flow-through properties.

Assessment of the macroporous structure of a monolith was described in Paper III. An alternative method to mercury intrusion porosimetry was proposed. The capillaries were embedded in a stained resin and observed under transmission electron microscope. Images were then computed to determine the pore sizes.

Synthesis of molecularly imprinted polymers grafted to a core mono-lith in a capillary was described in Paper IV. The resulting material, imprinted with local anaesthetics, was tested for its chromatographic performance. Similar imprinted polymers were characterized by microcalorimetry in Paper V. Finally, imprinted monoliths were also synthesized in a glass tube and further introduced in a NMR rotor to describe the interactions between stationary phase and template in Paper VI.

Place, publisher, year, edition, pages
Umeå: Kemi, 2006. 50 p.
bupivacaine, etching, phosphorylated tyrosine, poly(ethylene glycol), silanization, transmission electron microscopy, fused silica capillaries, isothermal titration calorimetry, local anæsthetic, molecularly imprinted polymer, monolith, nuclear magnetic resonance
National Category
Analytical Chemistry
urn:nbn:se:umu:diva-923 (URN)91-7264-207-6 (ISBN)
Public defence
2006-12-01, Lilla Hörsallen KB3A9, KBC-Huset, Umeå University, Umeå, Sweden, 10:00
Available from: 2006-11-10 Created: 2006-11-10 Last updated: 2011-04-15Bibliographically approved

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Courtois, JulienSzumski, MichalGeorgsson, FredrikIrgum, Knut
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