This paper presents a new method for separating Rhenium, Molybdenum, Vanadium and Tungsten ions on a thin layer of Perlite using the thin layer -electro-chromatography method. This method is based on the combination between chromatographic forces and electric forces by applying different voltages on the separation plate for different times using several electrolytes as different mobile phase concentrations, at different applying field duarations on the process. This method also shows the possibility of using Perlite as a thin layer in this kind of separation process, which can apply in the separation of other types of biochemistry and inorganic ions This relatively simple method is cost effective.