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This article describes how a fiber-optic turbidity probe may be used as an inferential sensor to aid in the control of commercial-scale batch crystallizations. The discussion focuses on several unseeded crystallization examples involving cooling or cooling plus addition of antisolvent. In a typical control scheme, the fiber-optic probe is used to detect an initial nucleation event, to control a subsequent digestion step for fines dissolution with the potential for modification of nuclei size, number, and purity, and then to monitor a growth period. During the digestion step, temperature is increased and adjusted to achieve a desired reduction in the fiber-optic signal in order to control the extent of digestion. Within Dow, this approach has proven to be robust and cost-effective for numerous commercial-scale batch crystallizations including those with highly fouling or corrosive environments.

in Wiley InterScience (www.interscience.wiley.com).High-speed, in situ video microscopy is a promising technology for measuring critical solid-phase properties in suspension crystallization processes. This paper demonstrates the feasibility of high-resolution, video-imaging-based particle size distribution (PSD) measurement by applying image analysis and statistical estimation tools to images from a simulated batch crystallization of an industrial photochemical. The results also demonstrate the ability to monitor important quality parameters, such as the ratio of nuclei mass to seed mass, that cannot be monitored by conventional technologies. General recommendations are given for achieving appropriate sampling conditions to enable effective imaging-based PSD measurement.