This article describes a method for the preparation of (32)P patch for the treatment of skin cancer. It is based on the surface modification of a Nafion film by treatment with ZrOCl(2) solution, impregnation of a predicted quantity of (32)P into the film, and its subsequent immobilization into a nonleachable matrix by lamination. The effect of variations of critical parameters on the incorporation of (32)P into the membrane, such as solution pH, contact time, reaction volume, inactive carrier concentration of the feed, reaction temperature, and so on, was investigated to arrive at the conditions resulting in optimum retention of (32)P activity. The morphology of the membrane was evaluated by scanning electron microscope and energy dispersive spectral analyses. Quality control tests were carried out to ensure nonleachability, uniform distribution of activity, and stability of the patches.