N-'Hydroxy-N ,N' -diphenylbenzamidine (HDPBA)" arnbidentate chelating agent, reacts with cobalt(III) andrnironeIII) in the p,resence of azide to give a pinkishrnred and red-violet coloured mixed ligand complexes,rnwhich are quantitatively extractable into chloroformrnfrom the aqueous phase at pH 7.4-7.8 and 2-5 respectively,.rnallowing spectropJiotometric determinations of the metalrnions. The cobalt(III) and iron(III) mixed ligandrncomplexes have wavelengths of maximum absorption atrn520 and 520-540 run with their respective molar absorptivitiesrnof 1980 lit. mole-l cm-l and 4895 lit. mole-Irncm-l • Beer's Law obeys from 3.6 to 24 ppm for cobalt(III)rnand from 1.6 to 11.2 ppm for iron(III). The effect ofrnforeign ions and several other experimental variablesrnhave been studied., The composition of the cobalt(III)rnand iron(rII) mixed ligand complexes have been determinedrnby spectrophotometric methods- and ilre found to be 1:1:2rn(Co: HDPBA:N:3) and 1:2:2 (Fe:HDPBA:l{'3) respectively.rnOn the basis of the differences in the pH of thernreact'ion media for irone III) and cobal t( III), a separationrnprocedure for the two metals in a solution has beenrnestablished folloHed by spectrophotometric determinations.rnThe method has allowed the separntion and determinationrnof varied proportions of ironeIII) and cobalt(III) in a solution of the two metal ions. ,Moreover, the methods have been applied successfully for the separation andrndetermination of cobalt and iron in synthetic samples.a solution of the two metal ions. Moreover, the methods have been apr;lied successfully for the separation andrndetermination of cobalt and iron in synthetic samples