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Ultrasonic speckle velocimetry (USV) is a non-invasive technique that allows the measurement of fluid velocity in flow and also that of powders under sedimentation. To improve the USV method, we studied the sedimentation of polymethyl methacrylate and silica particles in water. Then, we built a sedimentation cell and characterized the diameter distribution of the particles. Subsequently, we carried out a specific study to optimize the USV procedure, the signal processing and data analysis. Space and temporal resolution and USV dynamics are also discussed with regard to the optimization conditions. We found that USV is a useful technique to measure velocities between 10−5 and 1 m s−1, using appropriate ultrasonic transducers. The space resolution is fixed by the length and the percentage of overlapping of the analyzed speckle windows and varies between 48 and 536 µm for the different studied particle families. Furthermore, we found that a 0.1 ns temporal resolution could be obtained after a zero padding signal processing. In the context of our sedimentation experiments, we showed that the velocities measured by USV are in close agreement with those measured by particle image velocimetry and theory.