A method has studied to determine niobium of niobium oxalate.The technological parameters have been optimized by orthogonal experiment.Niobium oxalate is burned to niobium pentoxide.Niobium content of niobium oxalate is determined by loss of mass.The method RSD is less than 0.4%.It shows good accuracy and exactitude compared with other methods.The method is very quick and easy tooperate.It satisfies demand of production technology.