Crystallization of Monohydrate Citric Acid. 1. In Situ Monitoring through the Joint Use of Raman Spectroscopy and Image Analysis

Abstract

Seeded batch crystallizations of monohydrate citric acid were performed under isothermal conditions (15 °C). Continuous monitoring of the overall solid concentration during the crystallization process was developed using in situ Raman spectroscopy. Quantitative estimation of the crystal size distribution (CSD) was made possible thanks to in situ image acquisition: off-line CSD measurements were further computed from the recorded pictures. The growth rate of monohydrate citric acid was estimated from solid concentration. Through in situ particle size visualization and quantitative analysis of the pictures, activated surface secondary nucleation was also shown to significantly impact the final CSD. It is underlined that, in addition to continuous Raman in situ spectroscopic concentration measurements, image acquisition yields highly valuable data on the dispersed phase. Advantages and drawbacks of the technique for the monitoring of solution crystallization are discussed.