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Analysis using size exclusion chromatography of poly(N-isopropyl acrylamide) using methanol as an eluent.

ABSTRACT: Size Exclusion Chromatography is traditionally carried out in either aqueous or non-polar solvents. A system to present molar mass distributions of polymers using methanol as a mobile phase is presented. This is shown to be a suitable system for determining the molar mass distributions poly(N-isopropylacrylamide)s (PNIPAM); a polymer class that is often difficult to analyze by size exclusion chromatography. DOSY NMR was used to provide intrinsic viscosity data that was used in conjunction with a viscometric detector to provide absolute calibration. Then the utility of the system was shown by providing the absolute molar mass distributions of dispersed highly branched PNIPAM with biologically functional end groups.

SUBMITTER: Swift T

PROVIDER: S-EPMC5486375 | biostudies-literature | 2017 Jul

REPOSITORIES: biostudies-literature

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Analysis using size exclusion chromatography of poly(N-isopropyl acrylamide) using methanol as an eluent.

Swift Thomas T Hoskins Richard R Telford Richard R Plenderleith Richard R Pownall David D Rimmer Stephen S

Journal of chromatography. A 20170525

Size Exclusion Chromatography is traditionally carried out in either aqueous or non-polar solvents. A system to present molar mass distributions of polymers using methanol as a mobile phase is presented. This is shown to be a suitable system for determining the molar mass distributions poly(N-isopropylacrylamide)s (PNIPAM); a polymer class that is often difficult to analyze by size exclusion chromatography. DOSY NMR was used to provide intrinsic viscosity data that was used in conjunction with a ...[more]

PMID: 28602503

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Project description:Thermoresponsive poly((N,N-dimethyl acrylamide)-co-(N-isopropyl acrylamide)) (P(DMA-co-NIPAM)) copolymers were synthesized via reversible addition-fragmentation chain transfer (RAFT) polymerization. The monomer reactivity ratios were determined by the Kelen-Tüdős method to be rNIPAM = 0.83 and rDMA = 1.10. The thermoresponsive properties of these copo-lymers with varying molecular weights were characterized by visual turbidimetry and dynamic light scattering (DLS). The copolymers showed a lower critical solution temperature (LCST) in water with a dependence on the molar fraction of DMA in the copolymer. Chaotropic and kosmotropic salt anions of the Hofmeister series, known to affect the LCST of thermoresponsive polymers, were used as additives in the aqueous copolymer solutions and their influence on the LCST was demonstrated. Further on, in order to investigate the thermoresponsive behavior of P(DMA-co-NIPAM) in a confined state, P(DMA-co-NIPAM)-b-PS diblock copolymers were prepared via polymerization induced self-assembly (PISA) through surfactant-free RAFT mediated emulsion polymerization of styrene using P(DMA-co-NIPAM) as the macromolecular chain transfer agent (mCTA) of the polymerization. As confirmed by cryogenic transmission electron microscopy (cryoTEM), this approach yielded stabilized spherical micelles in aqueous dispersions where the PS block formed the hydrophobic core and the P(DMA-co-NIPAM) block formed the hydrophilic corona of the spherical micelle. The temperature-dependent behavior of the LCST-type diblock copolymers was further studied by examining the collapse of the P(DMA-co-NIPAM) minor block of the P(DMA-co-NIPAM)-b-PS diblock copolymers as a function of temperature in aqueous solution. The nanospheres were found to be thermosensitive by changing their hydrodynamic radii almost linearly as a function of temperature between 25 °C and 45 °C. The addition of kosmotropic salt anions, as a potentially useful tuning feature of micellar assemblies, was found to increase the hydrodynamic radius of the micelles and resulted in a faster collapse of the micelle corona upon heating.

Dataset Information

Analysis using size exclusion chromatography of poly(N-isopropyl acrylamide) using methanol as an eluent.

Publications

Analysis using size exclusion chromatography of poly(N-isopropyl acrylamide) using methanol as an eluent.

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