In the environment sulphur containing compounds are present in the effluents of industries like dyeing & printing, pharmaceuticals etc. photo-Fenton process was used for treatment of these industrial effluents. Fenton sensitized photo-oxidation of Thioglycolic acid has been studied. The rate of photo-oxidation on different reaction parameters like substrate, H₂O₂, FeSO₄, H₂SO₄ and polarity of solvent were studied. Involvement of free radical has been confirmed. A probable mechanism has been proposed with overall reaction.