Abstract: The U-Nb-Zr alloy sample is dissolved by HNO3, H2O2 and HF, and the contents of Nb and Zr in the sample are determined on the JY-70 n type ICP-AES by using the internal standard synchronous dilution method. The range of determination is 1%-10% and 0. 33%-3. 33% respectively for Nb and Zr. The relative standard deviation is better than 3. 2% for Nb, and 2. 5% for Zr. The method is rapid and convenienty for determing Nb and Zr in U-Nb-Zr alloy sample.