A methodological survey of coacervation/phase separation techniques employed for the preparation of microspheres and microcapsules is presented. Basic features of macromolecular coacervation are discussed, and a classification of different coacervation procedures (i.e., simple, complex, aqueous, and nonaqueous) is provided. Microsphere formation and microencapsulation techniques based on coacervation/phase separation of gelatin, gelatin‐acacia, and ethylcellulose are described, and those of a wide range of other polysaccharide derivatives and synthetic polymers are tabulated. The dependence of microsphere/microcapsule characteristics on manufacturing parameters and performance evaluation of microspherical/microcapsular products are also discussed.