In this paper a new analytical method for determination of titanium and vanadium in aluminum oxide is described. The chemical analysis involves alkaline fusion of the calcined alumina, dissolution of the fused mass in hydrochloric acid, and solvent extraction of titanium and vanadium complexes with the aid of a new ligand N-4 chlorophenyl-N-hydroxy benzamide or benzamide N-hydroxy-N-p-Cl-phenyl (BHCP). The two impurities are extracted from one solution in two consecutive but identical operations. Titanium forms golden yellow colored Ti(IV)-BHCP and vanadium forms violet colored V(V)-BHCP complexes. The color intensities of Ti and V complexes are measured at 380 and 530 nm, respectively, using a spectrophotometer.