The ionic gelation technique is widely used in the encapsulation of different types of substances, with applications in different segments, including food. This technique has many advantages such as mild production conditions that help maintain the characteristics of the encapsulated substances. The technique has some limitations such as the retention of hydrophilic substances, which can be overcome by using a double emulsion. This chapter presents the ionic gelation technique for encapsulating substances. The most commonly used wall materials, pectin and alginate, and the main salts to promote polymer cross-linking are described. Practical procedures for obtaining laboratory-scale particles are described. The main analyses for this type of particles are mentioned. Some problems that may occur during the procedure are listed. Various applications of particles obtained in the study are described.