In the preformulation stage, there is a special need to determine the process behavior of materials with smaller amounts of samples. The purpose of this study was to assemble a novel automated multichamber microscale fluid bed module with a process air control unit for the characterization of fluidization behavior in variable conditions. The results were evaluated on the basis of two common computational methods, the minimum fluidization velocity, and the Geldart classification. The materials studied were different particle sizes of glass beads, microcrystalline cellulose, and silicified microcrystalline cellulose. During processing, the different characteristic fluidization phases (e.g., plugging, bubbling, slugging, and turbulent fluidization) of the materials were observed by the pressure difference over the bed. When the moisture content of the process air was increased, the amount of free charge carriers increased and the fine glass beads fluidized on the limited range of velocity. The silicification was demonstrated to improve the fluidization behavior with two different particle sizes of cellulose powders. Due to the interparticle (e.g., electrostatic) forces of the fine solids, the utilization of the computational predictions was restricted. The presented setup is a novel approach for studying process behavior with only a few grams of materials.