Abstract This paper describes an electrochemical method for the preparation of 55Fe sources, utilized in the calibration of low energy X-ray detectors. In this process, electrodeposition of 55Fe containing 185 MBq (∼5 mCi) of activity on a small circular cross sectional flat surface area (∼0.07 cm2) within a cylindrical Cu metal rod was carried out at a current density of 20 mA/cm2 at 18 ºC for 4 h using sulphate bath maintained at pH ∼ 2. The electrolytic cell, the experimental set up used and the process of 55Fe deposition were described. The effect of various experimental parameters influencing the electrodeposition of 55Fe were identified and optimized. The texture and morphology of the electrodeposited samples were examined by X-ray diffraction (XRD), SEM and EDS techniques. The quantity of deposited 55Fe activity was assayed in a calibrated ion chamber. Quality control tests were carried out to ensure nonleachability, uniform distribution of activity and stability of the sources.