Thin layer chromatographic method has been developed for the separation of metal ions such as Cr(VI), Cr(III), As(III), Cd(II), Tl(III) and Hg(II) from their two, three and four component mixtures. The separations were performed on thin layer of silica gel ‘G’ using aqueous l-Alanine as mobile phase. The effect of concentration and pH of mobile phase on the Rf values of individual metal ions were studied and the optimum conditions for separation of metal ions from their mixture were determined.