A systematic study of the comparative extraction behavior of some divalent metals has been carried out with the high molecular weight carboxylic acid, namely SRS-100. Benzene is used as diluent. The study includes the extraction behavior as a function of pH, effect of diluent, metal ion concentration, solvent concentration, and finally interference of the associated elements. In almost all cases nearly quantitative extraction has been achieved. The proposed method is very simple, rapid, and is applicable both at micro and macro levels. The. method is applicable to extraction of metal ions in the presence of other commonly interfering ions present at the milligram level.