Abstract: In this paper,the ammonium ferrous sulfate titrimetric method for the determination of vanadium in V-Al alloy has been established,which used HCl+HNO₃ to decompose the sample,used ammonium persulfate oxidate the vanadium to pentavalent in the 6~7 mol/L sulfuric acid.The determination conditions,such as sample quantity,concentration of ammonium ferrous sulfate standard solution,sulfuric acidity,ammonium persulfate solution dosage,were selected and optimized to determine the best experimental conditions.The method was used to measure the content of Vanadium in the V-Al alloy,and the determination of relative standard deviation（RSD,n = 8） ＜0.2%.The recoveries was 99.8%~100.7%,which fully meet the analysis and quick analysis requirement.