The cellulose triacetate，which was made by the vapour phase method by ZnCL2 catalyser，was fractionated using CH2Cl2－CH3OH as extracting solvent in a form of film，flake，or fiber． The fractionation of the fiber form was the best， but in every case，owing to heterogeneous contact of the triacetate solid and the extracting Iiquid，the results were unsatisfactory． Secondly，the fractionation of Spencer method was carried out using phenol - methanol－water（60 : 16 : 24）as solvent，methanol－water（16：24）as precipitant． Its results were almost satistactory compared with the solution extraction method reported elsewhere．