Acetylation of cellulose (Whatman cellulose powder CF-11 and Egyptian cotton fiber) by the use of the TFAA “impelling” method was examined, and the decrease in the degree of polymerization (DP) during the reaction was determined. Cellulose triacetate can be readily prepared by the TFAA method. When Whatman cellulose powder was used, the degradation of cellulose during acetylation was not observed in reaction times up to 5 hr, and a slight decrease in the degree of polymerization was detected in samples after reaction for more than 12 hr. The number of chain scissions per cellulose molecule for Egyptian cotton fiber was similar in magnitude to that for Whatman cellulose at the reaction time of 8 hr, but the value for Egyptian cotton fiber was considerably larger compared with that for Whatman cellulose after 12 hr.