The newly developed method is based upon the well known phosphate method for the separation of zirconium and the determination of zirconium as oxyquinolate. It is explained how zirconium oxyquinolate is separated from an oxalatecontaining solution after the phosphate precipitation was dissolved in oxalic acid. The conditions are given for the separation of zirconium from titanium and thorium in the phosphate precipitation and from niobium and tantalum in the oxyquinolate precipitation. By means of this method it is possible to determine small quantities of zirconium (2 to 5 mg) with an accuracy of up to plus or minus 2 to 4%. (TCO)