| Towards a solution for viscous heating in ultra-high pressure liquid chromatography using intermediate cooling. | |
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MedLine Citation:
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PMID: 20181348 Owner: NLM Status: MEDLINE |
Abstract/OtherAbstract:
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A generic solution is proposed for the deleterious viscous heating effects in adiabatic or near-adiabatic systems that can be expected when trying to push the column operating pressures above the currently available range of ultra-high pressures (i.e., 1200 bar). A set of proof-of-principle experiments, mainly using existing commercial equipment, is presented. The solution is based on splitting up a column with given length L into n segments with length L/n, and providing an active cooling to the capillaries connecting the segments. In this way, the viscous heat is removed at a location where the radial heat removal does not lead to an efficiency loss (i.e., in the thin connection capillaries), while the column segments can be operated under near-adiabatic conditions without suffering from an unacceptable rise of the mobile phase temperature. Experimental results indicate that the column segmentation does not lead to a significant efficiency loss (comparing the performance of a 10 cm column with a 2 cm x 5 cm column system), whereas, as expected, the system displays a much improved temperature stability, both in time (because of the shortened temperature transient times) and in space (reduction of the average axial temperature rise by a factor n). The method also prevents a large backflow of heat along the column wall that would lead to large efficiency losses if one would attempt to operate columns at pressures of 1500 bar or more. A real-world pharmaceutical example is given where this improved temperature robustness could help in moderating the changes in selectivity during method transfer from a low to a high pressure operation, although the complex non-linear behavior of the viscous heating and high pressure effects result in lower than expected improvement. |
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Authors:
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K Broeckhoven; J Billen; M Verstraeten; K Choikhet; M Dittmann; G Rozing; G Desmet |
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Publication Detail:
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Type: Journal Article; Research Support, Non-U.S. Gov't Date: 2010-01-29 |
Journal Detail:
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Title: Journal of chromatography. A Volume: 1217 ISSN: 1873-3778 ISO Abbreviation: J Chromatogr A Publication Date: 2010 Mar |
Date Detail:
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Created Date: 2010-03-08 Completed Date: 2010-05-14 Revised Date: - |
Medline Journal Info:
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Nlm Unique ID: 9318488 Medline TA: J Chromatogr A Country: Netherlands |
Other Details:
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Languages: eng Pagination: 2022-31 Citation Subset: IM |
Copyright Information:
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2010 Elsevier B.V. All rights reserved. |
Affiliation:
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Vrije Universiteit Brussel, Department of Chemical Engineering (CHIS-IR), Pleinlaan 2, 1050 Brussels, Belgium. |
Export Citation:
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| MeSH Terms | |
Descriptor/Qualifier:
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Chromatography, High Pressure Liquid
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instrumentation* Pressure Resins, Synthetic / chemistry Temperature Viscosity |
| Chemical | |
Reg. No./Substance:
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0/Resins, Synthetic |
From MEDLINE®/PubMed®, a database of the U.S. National Library of Medicine
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