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Modelling of Overloaded Gradient Elution in Reversed-Phase Liquid Chromatography
Karlstads universitet, Fakulteten för teknik- och naturvetenskap, Avdelningen för kemi och biomedicinsk vetenskap.ORCID-id: 0000-0001-8561-6872
Karlstads universitet, Fakulteten för teknik- och naturvetenskap, Avdelningen för kemi och biomedicinsk vetenskap.ORCID-id: 0000-0002-8943-6286
Karlstads universitet, Fakulteten för teknik- och naturvetenskap, Avdelningen för kemi och biomedicinsk vetenskap.ORCID-id: 0000-0003-1819-1709
Karlstads universitet, Fakulteten för teknik- och naturvetenskap, Avdelningen för kemi och biomedicinsk vetenskap.ORCID-id: 0000-0002-7123-2066
2012 (Engelska)Konferensbidrag, Enbart muntlig presentation (Refereegranskat)
Abstract [en]

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 thus 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 can be modelled under gradient elution conditions. Our aim is to make it possible to use modelling tools for a more reliable computer-assisted optimization, accounting for 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 presentation we will discuss how to obtain the adsorption isotherm data experimentally for two substances using the perturbation peak method. The substances investigated are cyclohexanone and cycloheptanone on a system comprising of a Kromasil C18-column and methanol-water as 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

Ort, förlag, år, upplaga, sidor
2012.
Nationell ämneskategori
Analytisk kemi
Identifikatorer
URN: urn:nbn:se:kau:diva-15258OAI: oai:DiVA.org:kau-15258DiVA, id: diva2:562035
Konferens
21st Analysdagarna (Analytical days). Uppsala, Sweden, June 11-13, 2012
Tillgänglig från: 2012-10-23 Skapad: 2012-10-23 Senast uppdaterad: 2019-07-12Bibliografiskt granskad

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Ņsberg, DennisEnmark, MartinSamuelsson, JörgenFornstedt, Torgny

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Ņsberg, DennisEnmark, MartinSamuelsson, JörgenFornstedt, Torgny
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Analytisk kemi

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