A new type of preparation employing153Sm metallic-hydroxide macroaggregates (153Sm-MHM) for radiation synovectomy was developed. The radiopharmaceutical was prepared by reacting the aqueous solution of153SmCl3 with sodium borohydride solution in 0.5N NaOH. Microscopic analysis showed that153Sm-MHM mean particle size was 4 m (range 1–15 m) avoiding the formation of fine particles (<1 m) which were153Sm-hydroxide macroaggregates preparations (153Sm-HM). Also, suspension properties as sedimentation rate, were better for153Sm-MHM than for153Sm-hydroxyapatite and153Sm-HM. Biological studies in normal rabbits demonstrated high retention into de Knee joint space even at 48 h after administration of153Sm-MHM (>99%).