Peroxydisulfuric acid is one of the oxidants which is produced on site and on demand by electrolysis in an undivided cell. In this report we provide the optimization of process parameters for the production of peroxydisulfuric acid in an undivided electrolytic cell taking BDD anode with various cathodes such as Ti, DSA, Pt, Zr etc. When current is passed the anodic oxidation produce a mixture of peroxymonosulfuric acid (H₂SO₅), hydrogen peroxide (H₂O₂) and peroxydisulfuric acid (H₂S₂O₈). The effects of varying cathode electrode material, area of the cathode, applied current densities on the production rate was estimated. It is found that the nature of the cathode influences the percentage of formation of peroxydisulfuric acid to some extent. Also, the smaller cathode area made found to improve the yield of oxidants.