Dilute solution viscometry method is used for studying viscosity behavior of newly prepared N , O -carboxymethyl chitosan (NOCC), cellulose acetate (CA), and their blends at different compositions (0/10, 2/8, 4/6, 5/5, 6/4, 8/2, 10/0). In this method, reduced viscosity ( η sp / c ) and inherent viscosity (ln η rel / c ) of the given polymer sample have been determined by measuring the fl ow time of the polymer sample in acetone solvent. Huggins ( k ) and Kraemer coeffi cients ( k ′ ) for given polymer-solvent system are calculated from the extrapolation of plots ( η sp / c ) versus ( c ) and (ln η rel / c ) versus ( c ). The miscibility of this polymer system is determined using different criteria such as ∆ b , ∆ b ′ , b 12 exp , interaction parameter ∆ [ η ], thermodynamic parameter α , and modifi ed thermodynamic parameter β . Based on the positive or negative sign of this criteria, miscibility of the polymer system is investigated. The results of the dilute solution viscometry method suggested that the NOCC/CA blends are miscible at the compositions range of 4/6, 5/5, 6/4, and 8/2 and completely immiscible at the 2/8 composition. The results are also supported by Fourier transform infrared analyses of all the compositions.