The spectrophotometric determination of cerium can be carried out by several methods, which involve either the formation of complexes of cerium(III) and cerium(IV) or the oxidation of suitable reagents by cerium(IV) and further measuring the intensity of the colour of the oxidised matter. The latter methods show a lack of selectivity and low sensitivity owing to the nature of the redox reaction. The methods that involve the formation of complexes have also been shown to have low selectivity and sensitivity. However, the most useful methods are those based on the complexes of cerium(III) with Xylenol Orange and Methylthymol Blue (MTB), but they are affected by many interferences. In this work the reaction of cerium(III) with MTB in the presence of oxalate and cyanide ions was studied at pH 10.2, which improves the sensitivity and the selectivity of the determination of cerium.