A NAA-PIXE combined analysis has been applied to the precise measurement of the concentrations of Nb and Ti in Nb–Ti alloy ingot. The ingot is used in the production of superconductors and the concentration should be controlled very strictly. The ingot cross section could be analyzed with an accuracy of better than 1% by the use of NAA for the preparation of standard samples and PIXE for the nondestructive rapid scan of the surface. The radial and azimuthal concentration profiles of the ingot could be obtained.