Synthese und Charakterisierung neuer zwitterionischer stationärer Phasen unterschiedlicher Ladungsarchitektur zur Untersuchung des ZIC-Retentionsmechanismus

Die vorliegende Arbeit befasst sich mit dem Einfluss der Ladungsarchitektur auf den ZIC-Retentionsmechanismus. Die Synthese der untersuchten Materialien erfolgte über eine kupferbasierte Funktionalisierungsmethode angelehnt an ein ATRP-Schema. Durch Modifikation der Synthesevorschrift hinsichtlich d...

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Bibliographic Details
Main Author: Nehles, Dorothee
Contributors: Seubert, Andreas (Prof. Dr.) (Thesis advisor)
Format: Doctoral Thesis
Published: Philipps-Universität Marburg 2021
Online Access:PDF Full Text
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Table of Contents: This work focuses on the influence of charge architecture on the ZIC-retention mechanism. The synthesis of the stationary phases investigated was carried out using a method based on ATRP. Through modification of the synthetic prescription concerning catalytic systems, macroinitiators and reaction conditions ion exchangers as well as zwitterionic exchangers of high capacity were created on basis of DVB/EVB and methacrylat polymers.The arrangement of the charges was preset through the structure of the monomers used. The synthesis of known sulfobetaines has been optimised and new sulfobetains of inverted charge structure were prepaired. The influence of the charge architecture on the amount of ion exchange within the ZIC retentionmechanism was investigated via variation of the eluention concentration. UV-active anions and cations of earthalkaline and alkaline elements were used as substrats. Furthermore the influence oft he base material as well as the capacity has been analyzed through variations of both. The application of the materials synthesized to seperate organic substrates under ZIC-HILIC-conditions using a LC-ESI-MS has been tested. The detection of anions was carried out through determination of conductivity and of UV/VIS absorbance. For anorganic cations LC-ICP-MS was used. Based on the arrangement of charges neither anion nor cation exchange occured preferentially. Increasing charge distances and the chemical surrounding of the charge carrying functionalities seem to further ion exchange.