A fast and highly sensitive Kalman Filter analysis with flow injection-chemiluminescence(FI-CL) method for simultaneously determining the trace amounts of niobium and tantalum without separating them were developed in this paper. After depositing-separation of most interference ions, 1% EDTA as the mask reagent was used to dispel the effect of residual interference elements. The mixed chemiluminescence kinetic curve of Nb and Ta(Ⅴ) was analyzed by Kalman Filter in this method to realize the simultaneous determination of niobium and tantalum in the national standard samples.