Article,

Compositional heterogeneity of heterogeneously deacetylated chitosans

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Carbohydr. Polym., 29 (1): 17 -- 24 (January 1996)

Abstract

Commercial chitosans prepared by heterogeneous alkaline deacetylation with different F-A values were fractionated into acid-soluble and acid-insoluble fractions. The amount of acid-soluble fractions increased with increasing time of deacetylation. The acid-soluble fractions were characterized with respect to fraction of acetylated units (F-A), diad frequencies, intrinsic viscosities, molecular weights and molecular weight distributions. F-A values for the acid-insoluble fractions were obtained using CPMAS C-13 NMR spectroscopy. As a control, the F-A values for the acid-soluble fractions determined from CPMAS C-13 NMR spectroscopy were compared and found to be consistent with the F-A values from H-1 NMR spectroscopy. The diad frequencies indicated that the acetyl groups in the acid-soluble fractions of the commercially heterogeneously deacetylated chitosans were randomly distributed. Determination of eta, M(w) and M(w)/M(n) indicated negligible depolymerization of the acid-soluble fractions when deacetylation was performed under a nitrogen purge at 75 degrees C. Chemical characterization revealed compositional heterogeneity in the chitosans, with chitin-like acid-insoluble fractions with F-A values between 0.88 and 0.95, and acid-soluble fractions with F-A values from 0.20 to 0.52. Copyright (C) 1996 Elsevier Science Ltd

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