Abstract: Hollow glass microspheres are widely used in aerospace, military industry and other fields, whose heat transfer performance is determined by internal gas pressure. At present, there is no report on residual gas analysis at home and abroad. According to the characteristics of hollow glass microspheres, a sample crushing mechanism is designed. Based on the pressure rise method and throughput method, combined with the crushing rate, the calculation formulae of the internal pressure are deduced. The residual gas is decompressed by a small hole and analyzed by the quadrupole mass spectrometer. Compared with the first reading method, the gas composition analysis result of the integration method has a better consistency. The results show that the sampling mechanism can obtain more than 40% microspheres crushing rate. The internal pressure of hollow glass microspheres prepared by the glass powder method is about 27000 Pa, and the residual gas components mainly include SO₂, N₂, CO, CO₂ and O₂.