Development and applications of an inexpensive and modular medium-throughput microcrystalliser for the preparation and characterisation of solid phases

Identification, isolation, and control of solid form are important for process and product control of specialty chemicals and pharmaceutical compounds. Solid forms are commonly isolated by crystallisation from solution and as a consequence acquisition of both phase equilibrium and kinetic information is vital. In these cases, control of solid form requires a complete assessment of the relationship between crystallisation conditions and both structural and physical aspects of solid form through a number of experiments which may run into many hundreds for complex systems. Traditionally such experiments have been completed sequentially. To fully characterise complex systems in this manner often takes years and so to accelerate this process and characterise a wider phase space, tools for studying multiple samples have been developed to increase throughput. These high-throughput synthetic and analytical techniques are often prohibitively expensive for smaller-scale research laboratories. As a solution to this problem, we have developed a low cost (<4000 GBP) and modular medium-throughput microcrystalliser and optical tomography system for acquisition of phase equilibria, crystallisation kinetic, and solid-form data on organic materials. The design and typical applications of this equipment are presented here.