Real-time evaluation of the concentration of impurities during organic solution crystallization

Abstract : ATR FTIR spectroscopy was previously presented as a promising technique for measuring supersaturation on-line during crystallization operations, without requiring complex hardware developments. The present paper reports new experimental results where, in addition to the determination of the concentration of the main dissolved product, the real-time measurement of the concentration of impurities is shown to be feasible before the onset of primary nucleation. Using spectral data obtained with both clear solutions and suspensions, the calibration of the in situ infrared sensor was performed to relate the time variations of the concentrations of the main product and of its main impurity, in the presence of both pH and temperature variations. As far as the on-line monitoring of crystallizing slurries is concerned, it is shown that measuring the concentration of impurities is very difficult to perform. However, the quantitative evaluation of impurities present in the clear solution feeding the crystallizer is valuable and expected to allow further design of monitoring and control policies leading to the reduction of batch-to-batch variations of the final quality of the solid produced.
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L Derdour, G Févotte, François Puel, P Carvin. Real-time evaluation of the concentration of impurities during organic solution crystallization. Powder Technology, Elsevier, 2003, 129 (1-3), pp.1-7. ⟨10.1016/S0032-5910(02)00283-8⟩. ⟨hal-01270735⟩

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