When the determination of titanium in titanium-vanadium alloy samples with vanadium content more than 0.60 % is carried out by ammonium ferric sulfate titration method,vanadium was seriously interfered with the determination of titanium.Therefore,the titanium-vanadium alloy was dissolved by hydrochloric acid,hydrofluoric acid and nitric acid,and the titanium was precipitated into sodium trititanate in sodium hydroxide,which was separated from the interfering elements such as vanadium and tin.The precipitation was dissolved in hydrochloric acid,reduced by adding aluminum flake,and finally,the titanium was determined by ferric ammonium sulfate titration.The influence of sample decomposition,interference elements,dosage of the precipitant,precipitation dissolution,selection of reducing agent,selection of protective device and time before titration on determination was studied.The relative standard deviation of titanium in titanium-vanadium alloy was 0.12 %-0.17 % with this method,and the determination results are consistent with the given value.The method can be applied to the analysis of titanium in the titanium-vanadium alloy.