An experimental system for separation of gas and solid two phases in supersonic gas flow was established. Separation efficiencies of hollow glass beads were measured under room temperature and different nozzle inlet total pressures from 482 kPa to 537 kPa. The experimental results show that the 57.83% - 67.28% particles with a Sauter average diameter of 9.84 μm can be separated by the experimental device. the 75.73% - 80.52% particles with diameters above 8.31 μm and the 96% - 100% particles with diameters above 15 μm can also be separated. Bigger particles correspond to higher separation efficiency. The present method for separation of gas and solid two phases in supersonic gas flow is successful and feasible.