This paper describes a rapid method for the separation and determination of microgram amounts of scandium and thorium.5,7-Dichloro-8-quinolinol in chloroform is used to extract thorium from aqueous solution of pH 3.2-3.4, from which no scandium is extracted.Xylenol Orange ethanolic solution is added directly to the organic layer, after washing once with water, and the absorbance is measured at 540 mμ.Then the aqueous layer containing scandium is adjusted to pH 5-5.5 with urotropin and extract again with dichloroquinolinol in chloroform solution.The scandium in organic layer is also determined directly by adding Xylenol Orange ethanolic solution and measuring the absorbance at 530 mμ.