Abstract: A method for the simultaneous spectrophotometric determination of iron (Ⅲ) and titanium (Ⅳ) in mixtures based on the formation of diantipyrilmethane (DAM) complexes with absorbance maxima of 390 and 460nm has been developed, and its application for their determination in aluminum alloy has been proved to be feasible.In general, photometric determination of iron and titanium in aluminum alloys is separately performed because the presence of one ion interfers with the determination of the other. In addition, although authors have earlier described the individual determination of iron (Ⅲ) and titanium (Ⅳ), no one has hitherto suggested a method of simultaneous spectrophotometric determination of iron ( Ⅲ ) and titanium (Ⅳ) with DAM.In the present paper, the eight variations described (including the solution of simultaneous equations, experimental coefficient method, dualwavelength spectrophotometry, identical molar absorptivity point method, and modified curves method) are all so simple that separations and methods for avoiding the interference of other ions are not necessary, and two ions can be determined with a single operation in the same aliquot.The experimental results showed that the method is applicable for the simultaneous spectrophotometric determination of 10-120μg of titanium and of 10-250μg of iron in aluminum alloys. Such a method generally gave a variation coefficient of 3-5% and a recovery of 90-108%. The method is simple, fast, accurate and reproducible.Future use of the technique is briefly discussed.