Summary: A solvent extraction method is presented for the separation of 95Nb in a carrier-free form from Zr. Nb is extracted into a chloroform solution of N-benzoyl-N-phenyl-hydroxylamine from an aqueous hydrochloric acid phase 0.05 M in hydrofluoric acid. By following the recommended procedure a decontamination factor of about 104 from Zr is achieved and up to 1 mg per ml of Zr in the aqueous phase does not impair the separation. The Nb may be back extracted into aqua regia, ammoniacal hydrogen peroxide, or aqueous ammonia, from all of which aqueous solutions of different chemical compositions can readily be prepared. The complete procedure need not take longer than 30 minutes.