RESUMO
We studied molar mass limits for the LC LCD separation of parent polystyrene (PS) and poly(ethylene oxide) (PEO) homopolymers from PEO/PS based block copolymers and we identified optimized chromatographic conditions. Time delays between barriers and sample injections were 0-2-3'10. Eluent was composed of dimethylformamide (DMF) 40 wt.% and 1-chlorobutane (CLB) 60 wt.%; Barrier 1 (B1), which retained block copolymer, was composed of 100 wt.% CLB and Barrier 2 (B2), which retained PEO, was a mixture of DMF and CLB, which proportions were adjusted to studied block copolymers. With B2 composed of DMF 23 wt.% and CLB 77 wt.%, we obtained successful separation of PS23K-b-PEO35K-b-PS23K (56.5 wt.% of PS, the subscripts indicate the molar mass in kg mol(-1) of each polymer part in the block copolymer) from its parent homopolymers. With B2 adjusted to DMF 30 wt.% and CLB 70 wt.%, PS2.3K-b-PEO3.1K (42.6 wt.% of PS) was also efficiently separated from its parent homopolymers.
Assuntos
Cromatografia Líquida/métodos , Polietilenoglicóis/química , Poliestirenos/química , Butanos , Dimetilformamida , Peso Molecular , SolventesRESUMO
Separation of parent homopolymers, polystyrene and poly(ethylene oxide), from the triblock copolymer polystyrene-b-poly(ethylene oxide)-b-polystyrene was investigated by means of liquid chromatography techniques. Overall suitability was evaluated and compared for size exclusion chromatography, (SEC), liquid chromatography under critical conditions of enthalpic interactions (LC CC), and liquid chromatography under limiting conditions of desorption (LC LCD). Among these techniques, LC LCD was the only one able to fully separate block copolymers from both their parent homopolymers in one single run. The efficiency of the separation was proven by (1)H NMR analysis of previously collected fractions.
