Nucleophilic substitution in preparation and surface modification of hypercrosslinked stationary phases

Journal of Chromatography. a
Simona JankůJiří Urban

Abstract

Four linear diaminoalkanes (1,2-diaminoethane, 1,4-diaminobutane, 1,6-diaminohexane, and 1,8-diaminooctane) have been used to hypercrosslink poly(styrene-co-vinylbenzyl chloride-co-divinylbenzene) monolithic stationary phases by nucleophilic substitution reaction. The column efficiency of polymer monoliths improved with longer diaminoalkane with 1,8-diaminoctane providing the highest efficiency. The concentration of 1,8-diaminoctane, together with hypercrosslinking time and temperature has been optimized. To improve the permeability of prepared columns, the hypercrosslinking modification has been combined with an early termination of polymerization reaction and decrease in polymerization temperature. The optimal column has been prepared by a polymerization reaction for 2h at 65°C and hypercrosslinked in the presence of 3% 1,8-diaminooctane for 2h at 95°C. The repeatability study of the presented protocol provided relative standard deviation for nine columns prepared independently out of three individual polymerization mixtures in between 2.0-12.0% for retention factors and 1.5-6.5% for plate heights, respectively. Further, we have modified residual chloromethyl groups with 2-aminoethanesulfonic acid (taurine) to prepare monolit...Continue Reading

References

Sep 19, 2002·Journal of Chromatography. a·V DavankovL Pavlova
Jul 21, 2007·Journal of Chromatography. a·Georges Guiochon
May 3, 2011·Journal of Chromatography. a·Harun KokuAbraham M Lenhoff
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Apr 3, 2012·Journal of Chromatography. a·Harun KokuAbraham M Lenhoff
Nov 28, 2012·Langmuir : the ACS Journal of Surfaces and Colloids·Tibor MüllnerUlrich Tallarek
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Jul 31, 2014·Journal of Chromatography. a·Tim J Causon, Ivo Nischang
Aug 13, 2014·Journal of Separation Science·Jiří Urban, Veronika Škeříková
Sep 3, 2014·Journal of Chromatography. a·Fabrice Gritti, Georges Guiochon

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Citations

Apr 22, 2015·Journal of Chromatography. a·Jiří Urban
Dec 24, 2018·Journal of Separation Science·Martina KomendováJiří Urban
Feb 17, 2019·Journal of Separation Science·Fernando Maya, Brett Paull
Mar 19, 2020·Molecules : a Journal of Synthetic Chemistry and Natural Product Chemistry·Sarah Alharthi, Ziad El Rassi

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