Measurement of the particle temperature and velocity in detonation spraying is significantly complicated by the pulsed character of the process. In the present study, these parameters are measured for powders with strongly different nature and properties such as WC/Co, Inox and Ti. Experiments are performed using an original computer-controlled detonation spraying (CCDS) installation developed by the authors. The system is distinguished by the mode of powder feeding into the gun barrel which is pulsed in time and localized in space. Evolution of the particle-in-flight velocity and size is examined by an original CCD-camera-based diagnostic tool developed by the authors. A significant spatial separation of the particles along the detonation plume is observed during their acceleration: 15 μm fine particles overtake 45 μm coarse particles by more than 10 plume diameters. For this reason, distributed scanning over the plume length is applied in order to obtain adequate results. A previously developed mathematical model of the process is experimentally validated. Calculations are found to be in a qualitative agreement with the experimental results. As far as particle-in-flight velocity is concerned, the agreement is even quantitative.