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A closer study of methanol adsorption and its impact on solute retentions in supercritical fluid chromatography
Karlstad University, Faculty of Health, Science and Technology (starting 2013), Department of Engineering and Chemical Sciences. (INTERACT)
AstraZeneca R&D, Innovat Med, Resp Inflammat & Autoimmun, S-43183 Molndal, Sweden..
AstraZeneca R&D, Innovat Med, Resp Inflammat & Autoimmun, S-43183 Molndal, Sweden..
AstraZeneca R&D, Innovat Med, Resp Inflammat & Autoimmun, S-43183 Molndal, Sweden..
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2016 (English)In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1442, p. 129-139Article in journal (Refereed) Published
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Abstract [en]

Surface excess adsorption isotherms of methanol on a diol silica adsorbent were measured in supercritical fluid chromatography (SFC) using a mixture of methanol and carbon dioxide as mobile phase. The tracer pulse method was used with deuterium labeled methanol as solute and the tracer peaks were detected using APCI-MS over the whole composition range from neat carbon dioxide to neat methanol. The results indicate that a monolayer (4 angstrom) of methanol is formed on the stationary phase. Moreover, the importance of using the set or the actual methanol fractions and volumetric flows in SFC was investigated by measuring the mass flow respective pressure and by calculations of the actual volume fraction of methanol. The result revealed a significant difference between the value set and the actually delivered volumetric methanol flow rate, especially at low modifier fractions. If relying only on the set methanol fraction in the calculations, the Methanol layer thickness should in this system be highly overestimated. Finally, retention times for a set of solutes were measured and related to the findings summarized above concerning methanol adsorption. A strongly non-linear relationship between the logarithms of the retention factors and the modifier fraction in the mobile phase was revealed, prior to the established monolayer. At modifier fractions above that required for establishment of the methanol monolayer, this relationship turns linear which explains why the solute retention factors are less sensitive to changes in modifier content in this region.

Place, publisher, year, edition, pages
2016. Vol. 1442, p. 129-139
Keywords [en]
Supercritical fluid chromatography, SFC, Excess adsorption, Solvent adsorption, Tracer-pulse method, Solute retention
National Category
Chemical Engineering
Research subject
Chemical Engineering
Identifiers
URN: urn:nbn:se:kau:diva-42028DOI: 10.1016/j.chroma.2016.03.006ISI: 000374083100014PubMedID: 26979267OAI: oai:DiVA.org:kau-42028DiVA, id: diva2:927968
Available from: 2016-05-13 Created: 2016-05-13 Last updated: 2017-11-30Bibliographically approved

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Glenne, EmelieSamuelsson, JorgenFornstedt, Torgny

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