A new ion exchanger has been prepared from syrian petroleum coke (S. P. C) of high sulphur content. Preparation of this ion exchanger was carried out by simple treatment of S. P. C with oleum at room temperature followed with statical ion exchange in aqueous sodium chloride solutions. The First, SPC ion exchanger with granular structure resulted from reacting 20 gr of the SPC granules with 20 ml of oleum. Where as a friable ion exchanger was produced when 40 ml of oleum were used in the process. The adsorption capacity of the two SPC ion exchangers was found out to be 100 mgeq and 170 mgeq respectively.