Abstract: A method is disclosed for the preparation of ytterbium(III) beta-diketonates, the improvement consisting in that the reaction between an ytterbium(III) halide and a chelating agent (such as acetylacetone, dibenzoylmethane and dipivaloylmethane for example) is caused to take place in an anhydrous medium and in the presence of gaseous ammonia, the ytterbium(III) halide being also anhydrous.