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Characterization of crosslinked starch materials with spectroscopic techniques
Author(s) -
Delval Franck,
Crini Grégorio,
Bertini Sabrina,
MorinCrini Nadia,
Badot PierreMarie,
Vebrel Joël,
Torri Giangiacomo
Publication year - 2004
Publication title -
journal of applied polymer science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.575
H-Index - 166
eISSN - 1097-4628
pISSN - 0021-8995
DOI - 10.1002/app.20851
Subject(s) - magic angle spinning , fourier transform infrared spectroscopy , amorphous solid , materials science , spectroscopy , sorption , infrared spectroscopy , polymer , relaxation (psychology) , spinning , nuclear magnetic resonance spectroscopy , polymer chemistry , chemical engineering , analytical chemistry (journal) , chemistry , crystallography , organic chemistry , composite material , physics , psychology , social psychology , adsorption , quantum mechanics , engineering
Abstract The structure, mobility, and properties of crosslinked starch materials of various compositions were investigated with FTIR and NMR spectroscopy, and relaxation time measurements were taken with cross‐polarization/magic‐angle‐spinning (CP–MAS) and magic‐angle‐spinning (MAS) spectroscopy. Characterization by Fourier transform infrared spectroscopy confirmed the crosslinking reaction. The CP–MAS and MAS spectra allowed the assignment of the principal 13 C signals. The molecular mobility of these polysaccharides was analyzed in terms of the cross‐relaxation time between the protons and carbons, the 1 H spin–lattice relaxation time in the rotating frame, and the 1 H longitudinal spin–lattice relaxation time. Relaxation studies showed that increasing the crosslinking degree increased the amorphous content, and the material became rigid as an increasing number of covalent bonds in the polymer network reduced mobility. The values of the spin–lattice relaxation in the rotating frame reflected the homogeneous nature of the materials. The correlation between the crosslinking degree, structure, and mobility and the sorption properties of these sorbents was examined. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 93: 2650–2663, 2004