Abstract: The suitable condition and operation step are obtained for the determination of Zr by spectrophotometry and X ray fluorescence spectrometry. It is found that spectrophotometry using xylenol orange or arsenazo Ⅲ as developing reagent is not applied to determine Zr concentration in the aqueous samples extracted by TBP or stripping from TBP. It is suggested X ray fluorescence spectrometry should be used for the determination of Zr in the above samples.