A simple and rapid electrochemical technique for the preparation of uniform and adherent metal deposits on thin metallized plastic films has been developed. It is based on the use of an electrolytic cell, characterized by the separation of the anode and cathode compartments by a fritted glass disc. Furthermore, electrodeposition is achieved from a solution having a volume of only 0.15 ml. The technique and the conditions used to realize the electrodeposition on thin metallized plastic films is described. The cell has been used to electrodeposit many metals, mostly by spontaneous electrodeposition using a magnesium anode and also by application of an external voltage using a platinum anode. In this paper, we describe the experimental conditions and report the results dealing with the electrodeposition of Co, Ni, Ag, Hg, and Zn. Deposits of less than a microgram to several hundred micrograms per square centimeter were obtained with high yields in 10 to 40 min. The use of the technique for the preparation of radioactive sources of Co-60, Ni-63, Ag-llOm, and Hg-203 for absolute rate determinations is reviewed.