The recombination of hydrogen and oxygen in technical gaseous waste of nuclear power plants has been studied. A highly efficient catalyst for reacting H2 with O2 to form water was prepared. Various operating conditions and factors affecting the recombination of H2 and O2 were tested and the best conditions were determined. Results show that the Pd–Al2O3 catalyst prepared had very good characteristics. The recombination rate of H2 and O2 was higher than 98.3% and 99.9%, respectively. After recombination, residual concentrations of H2 and O2 in waste gas were O2<3 ppm, H2<400 ppm. The Pd–Al2O3 catalyst and operating conditions determined for gaseous waste processing of nuclear power plants were satisfactory.