Real-Time Characterization of Crystal Shape and Size Distribution Based on Moving Window and 3D Imaging in a Stirred Tank

Abstract

Crystal shape distribution, i.e. the multidimensional size distribution of crystals, is of great importance to their down-stream processing such as in filtration as well as to the end-use properties including the dissolution rate and bioavailability for crystalline pharmaceuticals. Engineering crystal shape and shape distribution requires knowledge about the growth behavior of different crystal facets under varied operational conditions e.g. supersaturations. Measurement of the facet growth rates and growth kinetics of static crystals in a crystallizer without stirring has been reported previously. Here attention is given to study on real-time characterization of the 3D facet growth behavior of crystals in a stirred tank where crystals are constantly moving and rotating. The measurement technique is stereo imaging and the crystal shape reconstruction is based on a stereo imaging camera model. By reference to a case study on potash alum crystallization, it is demonstrated that the crystal size and shape distributions (CSSD) of moving and rotating potash alum crystals in the solution can be reconstructed. The moving window approach was used to correlate 3D face growth kinetics with supersaturation (in the range 0.04 - 0.12) given by an ATR FTIR probe. It revealed that {100} is the fastest growing face, leading to a rapid reduction of its area, while the {111} face has the slowest growth rate, reflected in its area continuously getting larger.