Development of a stereo imaging system for three-dimensional shape measurement of crystals

Despite the availability of various Process Analytical Technologies (PAT) for measuring other particle properties, their inherit limitations for the measurement of crystal shape have been restricted. This has impacted, in turn, on the development and implementation of optimisation, monitoring and control of crystal shape and size distributions within particle formulation and processing systems In recent years, imaging systems have shown to be a very promising PAT technique for the measurement of crystal growth, but still essentially limited as a technique only to provide two-dimensional information. The idea of using two synchronized cameras to obtain 3D crystal shape was mentioned previously (Chem Eng Sci 63(5) 1171-1184, 2008) but no quantitative results were reported. In this paper, a methodology which can directly image the full three-dimensional shape of crystals has been developed. It is based on the mathematical principle that if the two-dimensional images of an object are obtained from two different angles, the full three-dimensional crystal shape can be reconstructed. A proof of concept study has been carried out to demonstrate the potentials in using the system for the three-dimensional measurement of crystals

Measurement, modelling, and closed-loop control of crystal shape distribution: Literature review and future perspectives

Crystal morphology is known to be of great importance to the end-use properties of crystal products, and to affect down-stream processing such as filtration and drying. However, it has been previously regarded as too challenging to achieve automatic closed-loop control. Previous work has focused on controlling the crystal size distribution, where the size of a crystal is often defined as the diameter of a sphere that has the same volume as the crystal. This paper reviews the new advances in morphological population balance models for modelling and simulating the crystal shape distribution (CShD), measuring and estimating crystal facet growth kinetics, and two- and three-dimensional imaging for on-line characterisation of the crystal morphology and CShD. A framework is presented that integrates the various components to achieve the ultimate objective of model-based closed-loop control of the CShD. The knowledge gaps and challenges that require further research are also identified

Stereo Imaging Camera Model for 3D Shape Reconstruction of Complex Crystals and Estimation of Facet Growth Kinetics

The principle that the 3D shape of crystals that grow from a solution can be characterised in real-time using stereo imaging has been demonstrated previously. It uses the 2D images of a crystal that are obtained from two or more cameras arranged in defined angles as well as a mathematical reconstruction algorithm. Here attention is given to the development of a new and more robust 3D shape reconstruction method for complicated crystal structures. The proposed stereo imaging camera model for 3D crystal shape reconstruction firstly rotates a digitised crystal in the three-dimensional space and varies the size dimensions in all face directions. At each size and orientation, 2D projections of the crystal, according to the angles between the 2D cameras, are recorded. The contour information of the 2D images is processed to calculate Fourier descriptors and radius-based signature that are stored in a database. When the stereo imaging instrument mounted on a crystalliser captures 2D images, the images are segmented to obtain the contour information and processed to obtain Fourier descriptors and radius-based information. The calculated Fourier descriptors and radius-based signature are used to find the best matching in the database. The corresponding 3D crystal shape is thus found. Potash alum crystals that each has 26 habit faces were used as a case study. The result shows that the new approach for 3D shape reconstruction is more accurate and significantly robust than previous methods. In addition, the growth rates of {111}, {110} and {100} faces were correlated with relative supersaturation to derive models of facet growth kinetics

Development of an X-ray real-time stereo imaging technique using synchrotron radiation

An X-ray stereo imaging system with synchrotron radiation was developed to perform real-time stereo imaging and stereo angiography

Magnetic tests for magnetosome chains in Martian meteorite ALH84001

Transmission electron microscopy studies have been used to argue that magnetite crystals in carbonate from Martian meteorite ALH84001 have a composition and morphology indistinguishable from that of magnetotactic bacteria. It has even been claimed from scanning electron microscopy imaging that some ALH84001 magnetite crystals are aligned in chains. Alignment of magnetosomes in chains is perhaps the most distinctive of the six crystallographic properties thought to be collectively unique to magnetofossils. Here we use three rock magnetic techniques, low-temperature cycling, the Moskowitz test, and ferromagnetic resonance, to sense the bulk composition and crystallography of millions of ALH84001 magnetite crystals. The magnetic data demonstrate that although the magnetite is unusually pure and fine-grained in a manner similar to terrestrial magnetofossils, most or all of the crystals are not arranged in chains

Phips-halo: The airborne particle habit imaging and polar scattering probe-part 3: Single-particle phase discrimination and particle size distribution based on the angular-scattering function

A major challenge for in situ observations in mixed-phase clouds remains the phase discrimination and sizing of cloud hydrometeors. In this work, we present a new method for determining the phase of individual cloud hydrometeors based on their angular-light-scattering behavior employed by the PHIPS (Particle Habit Imaging and Polar Scattering) airborne cloud probe. The phase discrimination algorithm is based on the difference of distinct features in the angular-scattering function of spherical and aspherical particles. The algorithm is calibrated and evaluated using a large data set gathered during two in situ aircraft campaigns in the Arctic and Southern Ocean. Comparison of the algorithm with manually classified particles showed that we can confidently discriminate between spherical and aspherical particles with a 98 % accuracy. Furthermore, we present a method for deriving particle size distributions based on single-particle angular-scattering data for particles in a size range from 100 µm ≤ D ≤ 700 µm and 20 µm ≤ D ≤ 700 µm for droplets and ice particles, respectively. The functionality of these methods is demonstrated in three representative case studies

Application of ultraviolet, visible, and infrared light imaging in protein-based biopharmaceutical formulation characterization and development studies

Imaging is increasingly more utilized as analytical technology in biopharmaceutical formulation research, with applications ranging from subvisible particle characterization to thermal stability screening and residual moisture analysis. This review offers a comprehensive overview of analytical imaging for scientists active in biopharmaceutical formulation research and development, where it presents the unique information provided by the ultraviolet (UV), visible (Vis), and infrared (IR) sections in the electromagnetic spectrum. The main body of this review consists of an outline of UV, Vis, and IR imaging techniques for several (bio)physical properties that are commonly determined during protein-based biopharmaceutical formulation characterization and development studies. The review concludes with a future perspective of applied imaging within the field of biopharmaceutical formulation research

In Situ Measurement of 3D Crystal Size Distribution by Double-View Image Analysis with Case Study on l-Glutamic Acid Crystallization

An in situ measurement method is proposed for monitoring three-dimensional (3D) crystal size distribution (CSD) during a crystallization process, based on a binocular microvision system. The stereo particle shape is reconstructed from double-view images captured by two microscopic cameras fixed at different angles outside the crystallizer. To overcome the influence from solution turbulence and uneven illumination background involved with in situ imaging, a microscopic double-view image analysis method is established to identify the key corners of each particle shape in the captured images, including corner detection and corner matching. Two fast algorithms are therefore given for online detection of two typical crystal morphologies of prismatic and needle-like shapes, such as α- and β-forms of l-glutamic acid (LGA) crystals, respectively. On the basis of the identified key corners for different particle shapes, a 3D geometry model is established to approximately reconstruct the 3D shape for each imaged particle, such that 3D sizes of each particle could be quantitatively estimated, along with the particle volume. Experiments on the LGA cooling crystallization are performed to demonstrate the effectiveness of the proposed method