The determination of Zirconium and Hafnium in presence of each other in geological sample Plasma Optical Emission Spectrometry (ICP adjusted and the suitable zirconium and hafnium lines were selected to give the most accurate determination each line was tested by a solution of 20 ppm zirconium mixed with 1 ppm hafnium to obtain the most sensitive lines which were 339.198 nm for zirconium and 239.336 nm for hafnium.effect of the major elements of monazite as Uranium, Thorium, Rare earth elements, Iron and Aluminium on the determination of the elements under studying.T which was upgraded of about 97% purity; the sample was leached by concentrated sulfuric acid (H zircon which contains zirconium and hafnium as a residue decomposition and measured by ICP-OES (Nuclear Materials Authority, Egypt) on the selected lines.