The purpose of this study was to synthesis and characterized sulfonated chitosan using acetyl sulfate. Sulfonated chitosan has been successfully synthesized using an alternative sulfonating agent using acetyl sulfate. Sulfonated chitosan was prepared by varying the volume of acetyl sulfate against chitosan for 1 hour at 40 oC and then terminated and filtered to obtain sulfonated chitosan. The sulfonated chitosan was characterized using Fourier Transform Infrared (FTIR), thermal analysis, and cation exchange capacity (CEC). FTIR data showed that all variation of sulfonated chitosan have sulfonate groups attached to both amine and hydroxyl group from chitosan. Thermal analysis showed lower thermal stability of sulfonated chitosan than chitosan. CEC data shows that the highest value obtained 14,5 mmol/g for addition 25 mmol acetyl sulfate. Sulfonated chitosan shows a high value of CEC and it has a promising material for polymer electrolyte membrane in Fuel Cells technology.