This method is devised for the determination of hafnium in zirconium oxide as reactor material.The“sifter electrode-spark excitation technique ” employed by C.Feldman and J.Y.Ellenburg is utilized and the sensitivity is extended to 100 ppm hafnium.In this technique, samples, finely ground and mixed with equal amount of graphite powder, are put into the “ sifter electrode ” used as the upper electrode, and are excited in ARL Multisoure oscillating spark.A marked improvement is made in signal to noise ratio of hafnium spectral line but the sensitivity is not sufficient.