In order to make a supermicrofiber fabric with PET/co-PET sea-island type filament fiber, the optimum conditions of dissolution of co-PET composite filament fiber was examined. The data set was made at various organic acid concentration and steam temperature with treated time as a main variable. At the same time, the microstructure changes by organic acid treatment of sea-island type PET supermicrofibers were monitored by thermal analysis morphology, DSC thermgrams and SEM images. Weight reduction behavior of supermicrofibers by caustic treatment was investigated in a comparative method. The termination of dissolution was also confirmed using DSC thermgrams and SEM images.