The use of infrared spectroscopy for characterization of the composition of chitin and chitosan covering the entire range of degree of acetylation (DA) and a wide variety of raw materials is examined further. The ratio of absorbance bands selected was calibrated using 1H liquid and 13C CP-MAS solid-state NMR as absolute techniques. IR spectra of the structural units of these polymers validated the choice of baselines and characteristic bands. The bands at 1650 and 1320cm−1 were chosen to measure the DA. As internal reference, the intensities at 3450 and 1420cm−1 were evaluated. The absorption band ratios involving the reference at 3450cm−1 had poorer fit.. The absorption ratio A1320/A1420 shows superior agreement between the absolute and estimated DA-values (DA%=31.92A1320/A1420−12.20;r=0.990).