Structural changes in carbon fibers at each stage of, especially, preoxidation process are well known to play a great role in achieving the ultimate product quality. Differential scanning calorimetry (DSC), scanning electron microscope (SEM), density method and optical microscope were used to characterize the preoxidation extent. A conventional pproach, e.g., density aim, to evaluate the extent of preoxidation is not very exact. A DSC curve of a PAN precursor only can provide general information, major in the temperature regime of preoxidation reaction. However,the evaluation of a preoxidation extent, especially from conventional preoxidation temperature with a great span egime of 200～400℃, is put forward in this paper, in which the evolution of core/shell morphological structure is a kind of straightforward evidence.