In spray chilling microencapsulation, after sample atomization, part of the microparticles are retained in the equipment’s cooled chamber. The microparticles that are used in the product development are obtained in the collecting pot. Motivated by the full use of the microparticles produced, the physical-chemical characterization and comparison between microparticles in the cooled chamber and in the collecting pot were carried out. Microparticles were produced with 50% hibiscus extract and 50% of the lipid materials fully hydrogenated palm fat and refined palm oil. In addition, 4% of PGPR emulsifiers were used in relation to lipids. The emulsion was treated using assisted ultrasound with 0.288 kJ.cm-3 of energy density and submitted to a spray chiller. Total anthocyanins, anthocyanin retention and color of samples from the cooled chamber and collecting pot were analyzed. To determine the total anthocyanins by spectrophotometry, anthocyanins were extracted in acidified ethanol, submitted to ultrasonic bath and centrifuged. Color parameters (L*.a* and b*) were measured by a portable colorimeter. Results were statistically analyzed by Student's t test at p<0.05 showing significant differences in the physicochemical characteristics of microparticles in the cooled chamber and collecting pot. The microparticles from the collector pot presented higher content and retention of anthocyanins, 1439 mg/100g and 93.62%, compared to those from the chamber, 1366 mg/100g and 88.87%. These results are explained by the incomplete solidification process of the microparticles in the chamber, which may present larger sizes compared to the microparticles in the collector pot. Larger particles show smaller contact surfaces, impairing the extraction of anthocyanins. The color parameters indicated differences between the samples, with lower luminosity for the chamber samples and more intense colors in pink tones. Despite the differences between the microparticles in the cooled chamber and the collecting pot, both have good characteristics to be applied in foods, considering their particularities.