title: Characterization of an amylose-graft-poly(n-butyl methacrylate) copolymer obtained by click chemistry by EPR and SS-NMR spectroscopies.
abstract: We present an investigation of the main chemical and physico-chemical properties of a graft copolymer of amylose and poly(n-butyl methacrylate), Am-g-PBMA, amphiphilic and able to self-assemble in water, prepared by coupling end azide-functionalized PBMA and alkyne-functionalized amylose under convenient click conditions. A deep knowledge of these properties is necessary in the perspective of real applications of the copolymer. To this aim we combined a basic characterization through FT-IR, TGA, ICP-OES and SEM with an extensive EPR and Solid State NMR investigation. It was possible to characterize the main structural and dynamic properties of Am-g-PBMA and highlight the presence of residual copper (Cu(II)) from the catalyst, even after an extensive purification procedure. We could identify two main species of Cu(II): Cu(II) complexes coordinated to the N,N,N',N'',N''-pentamethyldiethylenetriamine (PMDETA) ligand from the catalyst and to the copolymer triazole nitrogens and multi-nuclear or clustered Cu(II) species likely coordinated to amylose hydroxyl groups.
authors.affiliation: Dipartimento di Chimica e Chimica Industriale, Università di Pisa, Via Risorgimento 35, 56126 Pisa, Italy; INSTM, Consorzio Interuniversitario per la Scienza e Tecnologia dei Materiali, via Giusti 9, 50121 Firenze, Italy. Electronic address: silvi@dcci.unipi.it.
authors.forename: Silvia
authors.initials: S
authors.lastname: Borsacchi
authors.affiliation: Istituto di Chimica dei Composti Organometallici del Consiglio Nazionale delle Ricerche, Area della Ricerca di Pisa-S. Cataldo, Via G. Moruzzi 1, 56124 Pisa, Italy. Electronic address: lucia.calucci@pi.iccom.cnr.it.
authors.forename: Lucia
authors.initials: L
authors.lastname: Calucci
authors.affiliation: Dipartimento di Chimica e Chimica Industriale, Università di Pisa, Via Risorgimento 35, 56126 Pisa, Italy; INSTM, Consorzio Interuniversitario per la Scienza e Tecnologia dei Materiali, via Giusti 9, 50121 Firenze, Italy. Electronic address: marco.geppi@unipi.it.
authors.forename: Marco
authors.initials: M
authors.lastname: Geppi
authors.affiliation: Dipartimento di Chimica e Chimica Industriale, Università di Pisa, Via Risorgimento 35, 56126 Pisa, Italy. Electronic address: federicolt@libero.it.
authors.forename: Federico
authors.initials: F
authors.lastname: La Terra
authors.affiliation: Istituto di Chimica dei Composti Organometallici del Consiglio Nazionale delle Ricerche, Area della Ricerca di Pisa-S. Cataldo, Via G. Moruzzi 1, 56124 Pisa, Italy. Electronic address: calogero.pinzino@pi.iccom.cnr.it.
authors.forename: Calogero
authors.initials: C
authors.lastname: Pinzino
authors.affiliation: Istituto per i Processi Chimico-Fisici del Consiglio Nazionale delle Ricerche, Area della Ricerca di Pisa-S. Cataldo, Via G. Moruzzi 1, 56124 Pisa, Italy. Electronic address: monica.bertoldo@ipcf.cnr.it.
authors.forename: Monica
authors.initials: M
authors.lastname: Bertoldo
mesh_terms: D000688:Amylose / Q000737:chemistry*; D002384:Catalysis; D057930:Click Chemistry / Q000379:methods*; D056831:Coordination Complexes / Q000737:chemistry; D003300:Copper / Q000737:chemistry / Q000378:metabolism; D004578:Electron Spin Resonance Spectroscopy / Q000379:methods; D009682:Magnetic Resonance Spectroscopy / Q000379:methods; D008689:Methacrylates / Q000737:chemistry*; D009584:Nitrogen / Q000737:chemistry; D058105:Polymerization; D011108:Polymers / Q000138:chemical synthesis / Q000737:chemistry*; D014230:Triazoles / Q000737:chemistry
chemical_list: D056831:Coordination Complexes; D008689:Methacrylates; D011108:Polymers; D014230:Triazoles; C116863:poly(butyl methacrylate); D003300:Copper; D000688:Amylose; D009584:Nitrogen
keywords: Amylose; Click chemistry; Graft copolymers; MAS NMR; Nuclear relaxation times; PBMA