Zirconium and hafnium have opposite nuclear properties and are used very differently in the nuclear industry. However, hafnium is a common metal impurity in zirconium, and the chemical properties of the two are very similar except for nuclear properties, and it is difficult to separate and detect them. At present, the detection of hafnium content in zirconium is usually achieved by using an inductively coupled plasma (ICP) spectrometer, but ICP equipment is expensive, and the detection cost is high. Therefore, it is necessary to develop a simple and low-cost method for the determination of hafnium content in zirconium. Based on this, this paper takes the spectrophotometric method as a starting point. Through a series of experiments on the influence of pH and concentrations of the color-developing agent xylenol orange sodium salt on the absorbance of zirconium and hafnium ions, the appropriate variables are selected to detect the content of hafnium in zirconium. Finally, according to the measured absorbance and total ion concentration, by comparing the working curve of zirconium and hafnium ions, the content of hafnium in zirconium is calculated based on the lever principle.