Micron- and submicron-size hollow particles are being used in various and diverse applications, including fillers for syntactic foams (light weight composite materials that can be molded and machined), and as a means for controlled release of chemicals and/or drugs. Commonly, the application dictates the required properties of the particles (size, size distribution, thickness of the skin, mechanical and chemical properties, etc.). The challenge is to develop a process that produces hollow particles with the desired specified properties that can be applied for different raw materials. This paper describes a process to produce micron-size hollow polymeric particles. First, the basic principles of the process are reviewed, emphasizing the main parameters that affect the properties of the particles. Second, a lab-scale unit to produce the hollow particles is described. Third, an analysis of experimental results obtained on the lab-scale unit are presented and compared to the results of a mathematical model of the process. Lastly, the mathematical model is used to determine the sensitivity of the parameters that affect the process performance and the particle properties.