Polystyrene nanofiber ion exchangers (PSNIE) were prepared by electrospinning from solutions of dissolved polystyrene followed by sulfortation processes. Coating and sulfonation have been used to modify glass fiber surfaces with polystyrene to produce cation exchange fibers (CEF). In this paper, new experimental results investigating the performance of PSNIE and CEF are presented in relation to the relevant parameters (ion exchange capacity (IEC), water uptake, and surface morphology). The IEC and water uptake of the PSNIE and CEF is depended upon the sullonation time. The PSNIE sample with 30 min sulfonation time showed the maximum IEC of 3.74 mmol/g-dry-PSNIE and water uptake of 0.77 g H2O/g-dryPSNIE. ne IEC and water uptake of CEF reached up to 3.61 mmol/g-CEF and 0.25 g H2O/g-dry-CEF.