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

• Published in: Journal of Chromatography A Vol. 1163; no. 1; pp. 128 - 137
• Main Authors: Petit, Christelle, Luneau, Benoît, Beaudoin, Emmanuel, Gigmes, Didier, Bertin, Denis
• Format: Journal Article
• Language: English
• Published: Amsterdam Elsevier B.V 07.09.2007; Elsevier
• Subjects: Analytical chemistry; Applied sciences; Chemistry; Chromatographic methods and physical methods associated with chromatography; Chromatography, Liquid - methods; Effective interaction parameter; Exact sciences and technology; Functional polymer; Liquid chromatography at critical conditions; Molecular Structure; Organic polymers; Other chromatographic methods; Physicochemistry of polymers; Polymerization; Polymers - chemistry; Polystyrenes - chemistry; Preparation, kinetics, thermodynamics, mechanism and catalysts; Pure eluent; Spectrometry, Mass, Matrix-Assisted Laser Desorption-Ionization; Temperature; Liquid chromatography at critical conditions; Temperature; Functional polymer; Pure eluent; Effective interaction parameter; Polymer blends; Living polymer; HPLC chromatography; Mobile phase; Styrene derivative polymer; Characterization; Critical conditions; Organic solvent; Free radical polymerization; N,N-Dimethylformamide; Preparation; Styrene polymer; Interaction parameter
• ISSN: 0021-9673
• DOI: 10.1016/j.chroma.2007.06.039

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 °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.