The degree of acetylation (DA) of various samples has been evaluated by H-1 liquid-state NMR and C-13 and N-15 CP-MAS solid-state NMR over the whole range of DA. A good agreement has been found for all the experiments. The C-13 and N-15 CP-MAS experiments have permitted the evaluation of the chitin DA and content in the structural polysaccharides in a fungus named Aspergillus niger. The fungus structural carbohydrates mainly consist in pure chitin associated with glucans. Comparison of the C-13 CP-MAS spectra with standard (1-->3)-beta -D-glucans strongly suggests that chitin and glucans are linked via covalent bonds.