Document Detail

Towards a solution for viscous heating in ultra-high pressure liquid chromatography using intermediate cooling.
MedLine Citation:
PMID:  20181348     Owner:  NLM     Status:  MEDLINE    
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.
K Broeckhoven; J Billen; M Verstraeten; K Choikhet; M Dittmann; G Rozing; G Desmet
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Publication Detail:
Type:  Journal Article; Research Support, Non-U.S. Gov't     Date:  2010-01-29
Journal Detail:
Title:  Journal of chromatography. A     Volume:  1217     ISSN:  1873-3778     ISO Abbreviation:  J Chromatogr A     Publication Date:  2010 Mar 
Date Detail:
Created Date:  2010-03-08     Completed Date:  2010-05-14     Revised Date:  -    
Medline Journal Info:
Nlm Unique ID:  9318488     Medline TA:  J Chromatogr A     Country:  Netherlands    
Other Details:
Languages:  eng     Pagination:  2022-31     Citation Subset:  IM    
Copyright Information:
2010 Elsevier B.V. All rights reserved.
Vrije Universiteit Brussel, Department of Chemical Engineering (CHIS-IR), Pleinlaan 2, 1050 Brussels, Belgium.
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MeSH Terms
Chromatography, High Pressure Liquid / instrumentation*
Resins, Synthetic / chemistry
Reg. No./Substance:
0/Resins, Synthetic

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