- A novel shadowgraphic inline probe to measure crystal size distributions (CSD),
based on acquired greyscale images, is evaluated in terms of elevated temperatures and fragile
crystals, and compared to well-established, alternative online and offline measurement techniques,
i.e., sieving analysis and online microscopy. Additionally, the operation limits, with respect to
temperature, supersaturation, suspension, and optical density, are investigated. Two different
substance systems, potassium dihydrogen phosphate (prisms) and thiamine hydrochloride (needles),
are crystallized for this purpose at 25 L scale. Crystal phases of the well-known KH2PO4/H2O system
are measured continuously by the inline probe and in a bypass by the online microscope during
cooling crystallizations. Both measurement techniques show similar results with respect to the crystal
size distribution, except for higher temperatures, where the bypass variant tends to fail due to
blockage. Thiamine hydrochloride, a substance forming long and fragile needles in aqueous solutions,
is solidified with an anti-solvent crystallization with ethanol. The novel inline probe could identify
a new field of application for image-based crystal size distribution measurements, with respect
to difficult particle shapes (needles) and elevated temperatures, which cannot be evaluated with
common techniques.
