A systematic study of the comparative extraction behavior of some transitional metals has been performed with the high molecular weight carboxylic acids, SRS-100 and Versatic-9, using benzene as diluent. The study includes the extraction behavior as a function of pH, effect of diluent, metal ion concentration, solvent concentration, salting-out agent, and finally interference of the associated elements. Exchange reaction for several systems are reported. In almost all cases nearly quantitative extraction has been achiaved. It has been found that the extraction is rapid and complete within 3–4 min but the optimum period of extraction is kept at 5 min. In some cases quantitative separations have also been carried out.