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Chitin isolated enzymatically from Antarctic krill shells was dissolved in aqueous NaOH by freezing and thawing to create homogeneous conditions. Deacetylation was performed at room temperature or under heating. The degree of deacetylation, molecular weight, and dynamic viscosity of solutions were estimated in chitosan samples. Deacetylation of chitin under homogeneous conditions was optimized. Chitosans with molecular weights of 180–220 and 250–300 kDa were obtained from the chitins of Antarctic krill and northern shrimp, respectively.