In this study, 10 cellulose samples of various origins were subjected to heat annealing in 0.1 N NaOH at 260 "C. The initial and annealed samples were analyzed by electron diffraction experiments. It was confirmed that the initial samples contained various proportions of Ia (triclinic) and ID (monoclinic) phases. They could be classified into two families: a family I where the amount of the phase Ia was either small or below detection and a family I1 where this phase was the major component. The annealing treatment revealed that the Ia phase was metastable as it could be converted totally to the stable ID phase. The conversion Ia near 3240 and 750 cm-l were assigned to the Ia phase whereas bands near 3270 and 710 cm-l corresponded to the ID phase.
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