Thin layer chromatographic method has been developed for the separation of metal ions such as Cr (VI), Cr (III), Ni (II), Co (II), Cu(II), Fe(III), Zn(II) and Mo(VI) from their two, three and four component mixtures. The separations were performed on thin layer of silica gel ‘G’ using aqueous Humic acid as mobile phase. Thin layer of Silica Gel-G was used to study the chromatographic behavior of metal ions in surfactant mixed solvents. Effect of presence of humic acid at various concentrations, presence of strong and weak electrolytes, and effect of concentration of surfactant, effect of acidity and basicity of aqueous surfactant on mobility of metal cations were also studied. By using surfactant and with various additives mixed in mobile phase, metal ions such as Cu2+, Hg2 +, W6+ and Ni2+ were separated from their binary mixture. Semi-quantitative determination of Ni2+ by measurement of spot area was attempted.