By means of electrolysis with a mercury cathode, microgram quantities of copper, lead, cadmium, zinc, iron, cobalt, and nickel can be separated from at least 0.51V[ vanadium solutions. Quantitative recovery of all these traces of metals except cadmium from the mercury by distillation is satisfactory, and their subsequent estimation by either polarographie or spectrophotometrie methods is adequate.Electrolytic stripping of dilute amalgams at controlled potentials shows that the electrodeposited metals could not only be separated into the two major groups of passive (Fe, Co, and Ni) and nonpassive (Cu, Pb, Cd, and Cu) metals, but that separations within the nonpsssive group are also possible.