Vergleich der Eigenschaften von PS/DVB-basierten Copolymeren unterschiedlicher Morphologie im Hinblick auf ihre Einsatzfähigkeit als stationäre Phasen in der Ionenaustauschchromatographie

Ein breites Feld an analytischen Fragestellungen erfordert in der Flüssigchromatographie immer effizientere Trennsäulen und immer schnellere Trennungen. Die Effizienz von chromatographischen Trennsäulen ist dabei neben der Packungsgüte und der Funktionali-sierung insbesondere von den Eigenschaften d...

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Bibliographic Details
Main Author: Gröticke, Katrin Ursula Ada
Contributors: Seubert, Andreas (Prof. Dr.) (Thesis advisor)
Format: Doctoral Thesis
Published: Philipps-Universität Marburg 2013
Online Access:PDF Full Text
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A broad field of analytical issues demands increasingly efficient separation columns and faster separations in liquid chromatography. Efficiency of chromatographic separation columns not only depends on the quality of the column packing and on the functionalisation but also especially on the properties of the used substrate. Two current trends to improve the separation efficiency are the reduction of the particle diameter of spherical phases and the development of monolithic phases. Both of these approaches are not pervasive in ion exchange chromatography (IC) yet. Therefore the emphasis of this work is a systematic investigation concerning the influence of variation in the particle diameters of macroporous, heavily crosslinked, spherical polystyrene/divinylbenzene(PS/DVB)-phases on the separation efficiency in IC. The polymeric particles are generated by a two-step swelling procedure using polystyrene seed latices, which are prepared via the Goodwin procedure. The synthesis of those seed latices is varied in a specific manner to gain and characterise batches with different particle diameters in the range of 0.5 µm to 1.3 µm. These batches are used for the production of spherical PS/DVB batches by swelling and crosslinking in a process referring to Ugelstad. The control of the resulting particle diameters is gained by using three different strategies whereby the synthesis parameters are varied in a systematical way. Thus it becomes possible to generate PS/DVB-batches in the range of 1.7 µm to 5.5 µm. The produced batches are investigated systematically concerning their properties and their capability to being used as stationary phases. A closer look is taken to the influence of the chosen synthesis parameters on the porosity of the materials and also on their behaviour as stationary phases. The particular phases are deployed under reversed phase conditions as well as under IC conditions. When comparing the results it is evident that on separation columns with similar packing quality plate height and particle diameter behave proportional. Monolithic phases based on styrene and divinylbenzene are prepared and investigated. Different synthesis strategies are used and the resulting products are compared. For the use in IC develops the covalent attachment of the monolith to the column wall made of polyetheretherketone (PEEK) the biggest problem.