AbstractCellulosic fibers from cotton fibers (CF), recycled writing papers (RWP), recycled newspapers (RN), and macerated woody fibers of Leucaena leucocephala (MWFL) were acetylated by heterogeneous reactions with glacial acetic acid, concentrated H2SO4, and acetic anhydride. The resultant cellulose triacetate (CTA) was characterized for yield and solubility as well as by using 1H-NMR spectroscopy and SEM. The acetylated product (AP) yields for CF, RWP, RN, and MWFL were 112, 94, 84, and 73%, respectively. After isolation of pure CTA from the AP, the CTA yields were 87, 80, 68, and 54%. The solubility test for the CTA’s showed a clear solubility in chloroform, as well as mixture of chloroform and methanol (9:1v/v) and vice versa for acetone. The degree of substitution (DS) values for the CTA’s produced were nearly identical and confirmed the presence of CTA. In addition, the pore diameter of the CTA skeleton ranged from 0.072 to 0.239 µm for RWP and RN, and within the dimension scale of the CTA pinholes confirm the synthesis of CTA. Accordingly, pouring of the AP liquor at 25 °C in distilled water at the end of the acetylation and filtration did not hydrolyze the CTA to cellulose diacetate.