Measurements of accurate particle size distribution and chemical composition are important to understand the influence of human health and indoor environment. In this research, volatile particles generated from a pod-type Heated Tobacco Product (HTP) were measured by Aerodyne Aerosol Mass Spectrometer (AMS) and Scanning Mobility Particle Sizer (SMPS) using various aerosol fixation agents to reduce the volatility of particles. A simple method of aerosol fixation was applied, and the effective fixation agents and the primary factor of fixation were elucidated. The effective fixation agent was determined in from the view point of the solubility between aerosol substrates and fixation agents. We found that nonadecanoic acid had a higher effect on the fixation for propylene glycol and glycerin; however, it did not work for aerosol substrates with a low polarity. In particles without fixation, the organic mass concentration (derived by AMS) was significantly reduced due to volatilization in the measurement apparatus. In contrast, the fixed volatile particles showed a higher organic mass concentration due to suppression of volatilization. The number peak diameter of the volatile particles without fixation derived by SMPS was observed to be below 100 nm, whereas that of the fixed volatile particles was about 200 nm. The particle concentration of SMPS with fixation was in agreement with that of a light scattering method (welas®). The elemental and surface compositions of fixed volatile particles were analyzed by Scanning Electron Microscope-Energy Dispersive X-ray spectrometry (SEM-EDX) and Time-of-Flight Secondary Ion Mass Spectrometry (TOF-SIMS) under a vacuum condition. The results revealed that the fixation agent was localized on the surface of the particles, reducing the volatility of particles.