Revisiting molecular weight distribution of polystyrenes using adsorption high-performance thin-layer chromatography

A repeatable separation of polystyrenes according to MW, from 1920 to 520000 u.m.a, has been obtained under adsorption conditions using a method that comprises the use of Lichrospher HPTLC plates, and a controlled, isocratic elution with a 78:22 (v/v) mixture of cyclohexane (Cy)-tetrahydrofuran (THF). Likewise, UV-densitometric quantification of polystyrenes in mixtures can be achieved, by an intra-plate or an inter-plate procedure, using the corresponding polystyrene calibration curve. In the case or overlapped, unresolved peaks, an average curve of the corresponding polystyrenes can be used. Migration of polystyrenes strongly varies with slight variations in the relative proportion of Cy and THF in the mobile phase. This allows different ranges of MW to be separated as a function of mobile phase composition. Other factors influencing repeatability have been identified. Some reasons have been advanced to explain the current lack of activity in the research on polymer characterization by HPTLC. Old literature results concerning polystyrene separation have also been discussed in the light of modern HPTLC instrumentation. Developed method provides similar information on Molecular Weight Distribution (MWD) to that obtained using Gel Permeation Chromatography (GPC). Advantages and limitations of HPTLC for obtaining polymer MWD have also been discussed.
Authors thank the Spanish Ministerio de Ciencia e Innovación (MICINN) and FEDER (UE) for financial support (Plan Nacional de I+D+I, project CTQ2008-00959)