In this study, an alternative particle size measurement method, which can be used particularly in the production processes of materials like cement, gypsum, and polymer-modified cement used as binders in construction, has been developed. It has been observed that the developed piezo-acoustic size measurement method can mostly measure the sizes of powder particles smaller than 100 microns. In the study, cement, gypsum, and polymer-modified materials were sieved using 3 sieves of 33, 45, and 91 microns, and they were separated into 3 different size classes: 0-33, 33-45, and 45-91 microns. The materials were measured with the developed measurement setup, and the effect of material type and size class difference on the measurements was observed. According to the obtained results, it was seen that the size measurements of different powder particles below 100 microns can be performed with the developed piezo-acoustic technique.