The extraction of Zr(IV) and Nb(V) from aqueous solutions of mineral acids with 1 % l-phenyl-3-methyl-4-benzoyl-pyrazole-5-one and 5 % tri-iso-octylamine solutions in chloroform has been investigated respectively. The mechanism of extraction and the composition of the extracted species have been suggested and the effect of complexing and salting-out agents also determined. Separation factors of various metals with respect to niobium have been estimated and separation from zirconium and many other elements has been achieved. Procedures are recommended for the separation of 9! Nb from 9 5 Zr 5 Nb mixture as well as from the fission products.