Thermally stimulated discharge current (TSDC) in Pure and Ferrocene doped Polysulfone (PSF) has been performed to identify the optimum conditions for the charge storage capacity of PSF. TSDC study in pure and ferrocene doped Polysulfone was carried out as a function of the voltage (250, 400, 550 and 700 V), the temperature of polarization (40, 50, 60 and 70 °C) and the amount of ferrocene doping (10, 50 and 100 mg) respectively. From the study, it is identified that an increase in the value of TSD current is obtained with an increase in the doping amount of ferrocene in PSF. The Maximum value of TSD current has been obtained for PSF doped with 100 mg of ferrocene as compared to pure PSF. Improvement in the value of TSD current has been pointed out with an increase in polarizing voltage from 250 to 700 V. A Shift in the relaxation peak has been reported toward the lower temperature with an increase in the doping amount. Reduction in the Activation Energy and relaxation time has been observed with an increase in the doping amount of ferrocene in PSF. Reduction in activation energy and relaxation time shows the improvement in the fast discharging current capacity of PSF due to ferrocene doping. The study demonstrates that best charge storage capacity of PSF is obtained, when it is doped with 100 mg of ferrocene at the polarizing temperature of 70 °C and at the Polarizing voltage of 700 Volt. The EDX study has confirmed the availability of Carbon, Oxygen and Sulphur elements in required proportion in PSF. The EDX study has also authenticated the improvement in the proportion of Iron element with an increase in the amount of ferrocene dopant in PSF. The EDX results of pure and doped PSF demonstrates the possibility to exploit the X-ray signal produced by the co-irradiation with secondary electrons to identify the elements in the sample.