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Caractérisation par spectrométrie de masse MALDI–TOF de poly(isosorbide-éther)s cycliques et linéaires obtenus sous irradiation microondes
Institution:1. Institut national de recherche et d''analyse physico-chimique (INRAP), pôle technologique de Sidi Thabet, 2020 Sidi Thabet, Tunisie;2. Groupe de spectrométrie de masse de l''UMR 7613 « Synthèse, structure et fonction des molécules bioactives », université Pierre-et-Marie-Curie, bât. F, 7e étage, porte 738, boîte courrier 45, 4, place Jussieu, 75252 Paris cedex 05, France;3. Laboratoire des réactions sélectives sur support, ICMMO, université Paris-Sud, Orsay, bât. 420, 91405 Orsay cedex, France
Abstract:Characterisation of cyclic and linear poly(isosorbide-ether)s obtained under microwave irradiation by MALDI–TOF mass spectrometry. We studied the influence of the alkyl chain length and of the leaving group on the fraction of cyclic or linear poly(isosorbide-ether)s. A survey by MALDI–TOF MS showed that cyclic chains (C) are predominant when some short aliphatic chains are used (m = 4 or 6), whereas with longer chains (m = 8, 10 or 12), we noted that cyclic products were in a minority, whatever the leaving group (bromide or mesyl). Important non-thermal microwave effects have been demonstrated, notably a methanol-insoluble fraction of polyether considerably larger than the one obtained by conventional heating. These poly(isosorbide-ether)s have been characterized by RMN, MALDI–TOF, SEC, elementary analysis, and DSC. The survey of the thermal behaviour by DSC showed that the temperatures of fusion increase with the aliphatic chain's length (m = 12; Tf = 37 °C).
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