Crystallization is a widely used chemical process that finds applications in pharmaceutical industries. In an industrial crystallization process, it is not only important to produce pure crystals but also to control the shape and size of the crystals, as they affect the efficiency of downstream processes and the dissolution property of the drug. The effectiveness of control algorithms depend on the availability of on-line, real-time information about these critical properties. In this paper, we investigate the use of lens-less in-line digital holographic microscopy for size and shape measurements for crystallization processes. For this purpose, we use non-crystalline spherical microparticles and carbon fibers with known sizes present in a liquid suspension as test systems. We propose an algorithm to extract size and shape information for a population of microparticles from the experimentally recorded digital holograms. The measurements obtained from the proposed method show good agreement with the corresponding known size and shape of the particles.© (2008) COPYRIGHT SPIE--The International Society for Optical Engineering. Downloading of the abstract is permitted for personal use only.