This work presents a novel technique with fast response for Residence Time Distribution (RTD) measurements in gas-solid unit operations (e.g., fluidized bed reactors). This technique is based on an optical method which eliminates the requirement of knowing the velocity and concentration profiles at the exit section of the system. Experiments were carried out with SiC particles and a phosphorescent pigment used as a tracer. A concentration measurement system was developed to measure the tracer concentration in SiC/pigment mixtures. The corresponding pigment concentrations were evaluated at the bottom of this system using a photomultiplier. The pigment concentration was derived from the integral of the signal intensity received by the photomultiplier. Then, a calibration curve was established which provided the empirical relationship between the integral and pigment concentration. In order to validate this RTD measurement technique, a series of experiments was performed in a bubbling fluidized bed and the effect of the bed height was studied. It was shown that the experimental RTD curves were in good agreement with the theoretical RTD of bubbling fluidized beds. This solids RTD measurement technique can be used to provide a better understanding of the hydrodynamics of complex solids unit operations.