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An Experimental and Theoretical investigation on Mobile PhaseEffects on Competitive Adsorption Isotherms in Preparative LC
Karlstad University, Faculty of Technology and Science, Department of Chemistry and Biomedical Sciences.
Karlstad University, Faculty of Technology and Science, Department of Chemistry and Biomedical Sciences.
Karlstad University, Faculty of Technology and Science, Department of Chemistry and Biomedical Sciences.ORCID iD: 0000-0003-1819-1709
Karlstad University, Faculty of Technology and Science, Department of Chemistry and Biomedical Sciences.
2012 (English)Conference paper, (Refereed)
Abstract [en]

This poster serves as background information to the corresponding lecture. Mobile phase gradients have been used in LC since the 1950s and are still an important programming technique in both analytical and preparative LC. Improving the resolution, and thereby making the separation of complex samples possible, and reducing the separation time, which increases the productivity, are the two main advantages of gradient elution. The modelling of band profiles and the optimization of preparative separations has largely been studied under isocratic conditions. The shape of the gradient and the behaviour of the solutes are often determined experimentally with scarce knowledge about the underlying physicochemical equations. This "trial and error" approach results in time consuming and, possibly, expensive experiments. The goal of this work is to investigate the dependence of the adsorption behaviour on the mobile phase composition in reversed phase LC. By knowing the adsorption isotherm as a function of the concentrations of both the solute and the strong organic modifier, the band profiles are modelled under gradient elution conditions.Our aim is to make it possible to use modelling tools so one can optimize a separation and especially the gradient shape. Recent studies have shown that a significant improvement in productivity can be achieved if the gradient shapes are designed carefully [1,2].In this study we discuss how to obtain the adsorption isotherm data experimentally for two substances using the perturbation peak method. The substances which are investigated are cyclohexanone and cycloheptanone on a Kromasil C18-column with methanol-water as the mobile phase. The fitting of the nonlinear experimental data to appropriate theoretical isotherm models will also be discussed.For practical reasons, we will also be looking at how different key parameters, e.g. the column hold-up time, the column efficiency, the retention factor and the equilibrium constant, change with the mobile phase composition.With the experimentally determined adsorption isotherm as a basis, we will simulate overloaded band profiles under gradient elution conditions and compare the simulated results with experimentally obtained band profiles.A contribution from the Fundamental Separation Science Group www.separationscience.se

Place, publisher, year, edition, pages
2012.
National Category
Analytical Chemistry
Identifiers
URN: urn:nbn:se:kau:diva-15265OAI: oai:DiVA.org:kau-15265DiVA: diva2:562046
Conference
21st Analysdagarna (Analytical days). Uppsala, Sweden, June 11-13, 2012
Available from: 2012-10-23 Created: 2012-10-23 Last updated: 2017-01-25Bibliographically approved

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