Copper has been successfully separated from cadmium, zinc, and lead by TLC on silica gel layers; 1.0 M sodium formate -1.0 M potassium iodide (1 + 9) was used as mobile phase. After this separation the copper was quantitatively determined by titration and by atomic absorption spectrometry. Standard deviation, relative error, limits of detection and amount recovered were calculated, The method was applied to the separation and identification of metal ions in industrial wastewater.