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Article Dans Une Revue Macromolecules Année : 2007

Characterization of Amphiphilic Diblock Copolymers Synthesized by MADIX Polymerization Process

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We combined several analytical techniques (NMR, matrix assisted laser desorption ionization - time-of-flight mass spectroscopy MALDI−TOF MS, GPC, functional analysis on the first block, liquid chromatography at the point of exclusion adsorption transition LC-PEAT, and capillary electrophoresis CE) to analyze and quantify the characteristics of homopolymer precursors and amphiphilic diblocks synthesized by controlled radical polymerization process (CRP). We present here a detailed quantitative characterization of amphiphilic diblock copolymers (poly(butyl acrylate)−poly(acrylic acid) or PBA-b-PAA, and poly(di(ethylene glycol) ethyl ether acrylate)−poly(acrylic acid) or PDEGA-b-PAA). The samples were synthesized in ethanol by macromolecular design via inter-exchange of xanthate (MADIX), a reversible addition fragmentation transfer (RAFT) polymerization process using xanthates as control agents. The analytical results have permitted a determination of the transfer constant of xanthate CXa (≈ 2.7 and 1.5 for respectively PBA and PDEGA) and the transfer constant to solvent Cs (≈ 6 × 10-4). In the final diblock products, homopolymer side products were characterized. The amount of hydrophobic homopolymer was quantified by a specially developed LCPEAT technique in critical conditions for PBA. The hydrophilic homopolymer h-PAA amount was determined by quantitative capillary electrophoresis CE experiments. These analytical approaches allowed the quantification of the side products in a CRP system as well as the improvement of the reaction conditions via a thorough knowledge of the reaction mechanism.

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hal-00202246 , version 1 (04-04-2024)

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Marc Jacquin, Pierre Muller, Gilda Lizarraga, Corinne Bauer, Hervé Cottet, et al.. Characterization of Amphiphilic Diblock Copolymers Synthesized by MADIX Polymerization Process. Macromolecules, 2007, 40 (8), pp.2672-2682. ⟨10.1021/ma062600+⟩. ⟨hal-00202246⟩
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