Rapid online calibration for ATR-FTIR spectroscopy during batch crystallization of ammonium sulphate in a semi-industrial scale crystallizer

The knowledge of solute concentration throughout a batch crystallization process is essential from process control perspective. Despite the progress in process analytical technology (PAT), there still exist several challenges for online measurement of solute concentration at industrial scale. In this study, concentration monitoring was realized using attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy at lab as well as semi-industrial scale. Applications of the calibration model developed at lab scale for the measurements at the semi-industrial scale however resulted into strongly biased concentration predictions, caused by the differences in the curvature of fiber optics and the uneven thermal expansion of the probe. Therefore an alternative rapid online calibration method was developed during the start-up phase of the process. With this method, the time required for developing a working calibration model for concentration monitoring during crystallization of ammonium sulphate in a semi-industrial scale draft tube crystallizer has been reduced approximately by 90%. With the help of simultaneous concentration and crystal size distribution measurements at semi-industrial scale, the descriptive capability of the model was improved due to better kinetic parameters.

Research highlights▶ Calibration model developed at lab leads to biased measurements at pilot scale. ▶ Rapid online calibration possible at pilot scale. ▶ Rapid online calibration circumvents problems associated with calibration transfer. ▶ Simultaneous CSD and concentration measurements give better parameter estimates.