We have synthesized a series of ion exchange functionalized fibers (IXF) from polystyrene (PS) and polyacrylonitrile (PAN). To obtain strong-acid cation exchange fibers, polystyrene was sulfonated using specific sulfonation protocols. Micron sized fibers (average diameter of 100m) were then produced from the functionalized polystyrene using a single-screw extruder equipped with a 30 hole spinneret with orifice diameter of 0.5 mm with a precise screw speed of 5 rpm, pump speed of 15 rpm, and with a feed rate of 2.4 cc/min. The extruder zone temperature was kept at 250 – 270 °C. Fiber was drawn at 120 degree with a draw ratio of 2. Electrospinning of functionalized polystyrene was also carried out to produce ultrafine functionalized fibers of 100 nm in average diameter. We have also electrospun polystyrene and polyisoprene blended nanofibers to increase the strength of the resulting blend nanofibers compared to pure PS nanofibers. To synthesize weak-acid cation exchange fibers polyacrylonitrile (PAN) was electrospun and the nanofibers obtained were alkaline hydrolyzed with 2 N NaOH for 20 minutes at room temperature to convert nitrile bonds to carboxylate. Cation exchange capacity (CEC) of the microfibers and nanofibers was determined. Sulfonated PS microfibers show high CEC of 4.0 meq/gm compared to that of nanofibers with 2.5 meq/gm. CEC of blended nanofibers of PS and polyisoprene was 2.0 meq/gm. In case of PAN fibers, nanosized electrospun fibers were found to show a CEC of 1.5 meq/gm. Weak-base anion exchange fiber synthesis was undertaken using appropriate protocol and its CEC was measured. For all IXF synthesized, fiber diameter was measured using SEM, degree of functionalization was qualitatively determined using FTIR and ion exchange capacity was computed after mass balance on a binary exchange system after equilibrium.