Calcium sulphate static phase thin layer chromatography (TLC) has been performed in eight pure and mixed solvent systems containing acetonitrile and dioxane. Separations of Ph2+ from Hg2+, Bi3+ and UO22+; UO22+ from VO2+; Ni2+; from Cr3+; Ag+ from Bi3+; Ce4+ from Ce3+; Hg2+ from Cd2+; Zn2+ from Hg2+ have been achieved successfully. Rapid quantitative separation of mercury (2-20 mug) from binary, ternary and multicomponent mixtures containing several metal ions has also been successfully achieved.