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J Chromatogr A. 2007 Sep 7;1163(1-2):128-37. Epub 2007 Jun 27.

Liquid chromatography at the critical conditions in pure eluent: an efficient tool for the characterization of functional polystyrenes.

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  • 1Laboratoire UMR 6517, Chimie Biologie et Radicaux Libres, Equipe CROPS, Universités d'Aix-Marseille I, II et III, CNRS, Site de Saint-Jérôme, Avenue Escadrille Normandie Niemen, 13397 Marseille Cedex, France.


Functional polymers are usually separated by liquid chromatography at critical conditions (LC-CC) using a desorli/adsorli mixture as eluent. In this paper, we describe LC-CC using dimethylformamide (DMF) as pure eluent at 72 degrees C and its application to the analysis of functional polystyrenes. The critical adsorption point is reached by tuning the temperature so that the lack of repeatability is no longer a problem. We analysed several batches of polystyrenes, exhibiting different molecular weights and functionalities. We were able to differentiate di-, mono- and non-functional polystyrenes, bearing carboxylic acid, hydroxyl or nitroxide moieties. The behaviour of these polystyrenes expressed by the experimental results was compared with their behaviour described by the LC-CC theory through the calculation of the effective interaction parameter of each end group. The technique also makes it possible to quantify the fractions of different functional polymers in a blend.

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