A spectrophotometric method for the determination of traces of aluminium in titanium oxide has been described. The method was based on selective extraction of titanium as TiCI,.2TBP (TBP = tri-obutyl phosphate) with TBP in CCI, in llN HCI medium. Aluminium was then determined at pH 5.3 with xylenol orange in presence of tartiuic acid in aqueous medium by measuring the extinction at 530 om. The deleterious effect of traces of titanium left unextracted in the aqueous medium has been taken care of and removed by masking with H,0 2 • The method obeyed Beer's Law up to 2 fLg Al 2 0 3 /ml and yielded satisfactory results in its application to different titania samples.