Niobium(TT)N has been found to react with. N-4-chlorophenylcinnamohydroxamicrnacid(CPCHA) and thiocyanate to formrna golden yellow mixed ligand complex which is quantitativelyrnextractable into chloroform from 5*5-6« 5^1 hydrochloric acidrnsolutions. The complex exhibited a wavelength of maximumrnabsorption at 568 nm with a molar absorptivity of 47500M~icmrnand the system obeyed Beer's lav/ in the concentrationrnrange of 0«177~2.73 ppm of Nb, The composition of the complexrnhas been established spectrophotometrically to bern1:1:2(Nb:SCN“:CFCHA). The effects of diverse ions and ofrnseveral other experimental variables have been studied tornestablish the optimum conditions for extraction and determinationrnof niobium. On the basis of these studies a simple,rnprecise, sensitive, and a highly selective method has beenrndeveloped for the , determination of niobium(V) by solventrnextraction and spectrophotometry,, The method has been nsuccessfully applied to the determination of niobium inrnseveral synthetic samples corresponding to niobium containrning Ores, minerals, and alloys