A method is described for the determination of Hf, Sc and Y simultaneously with the REE in geological materials. An earlier method for REE separation from major elements was studied with the aim to apply it also to the determination of Hf, Sc and Y. Sample decomposition was carried out by melting with LiBO2. The method involves separation and concentration stages, using the cation-exchange resin DOWEX AG 50W-X8. Matrix elements were eluted with 2 mol/1 HCl, whereas 6 mol/1 HNO3 with oxalic acid and 8 mol/1 HNO3 were used to elute the elements to be determined. Some of the matrix elements could not be completely removed. This effect as well as the recovery rates of the determined elements were investigated. The measurements were performed by ICP-AES. Spectral interferences were also tested.