Abstract:In the context of self-driving laboratories (SDLs), ensuring automated and error-free capping is crucial, as it is a ubiquitous step in sample preparation. Automated capping in SDLs can occur in both large and small workspaces (e.g., inside a fume hood). However, most commercial capping machines are designed primarily for large spaces and are often too bulky for confined environments. Moreover, many commercial products are closed-source, which can make their integration into fully autonomous workflows difficult. This paper introduces an open-source capping machine suitable for compact spaces, which also integrates a vision system that recognises capping failure. The capping and uncapping processes are repeated 100 times each to validate the machine's design and performance. As a result, the capping machine reached a 100 % success rate for capping and uncapping. Furthermore, the machine sealing capacities are evaluated by capping 12 vials filled with solvents of different vapour pressures: water, ethanol and acetone. The vials are then weighed every 3 hours for three days. The machine's performance is benchmarked against an industrial capping machine (a Chemspeed station) and manual capping. The vials capped with the prototype lost 0.54 % of their content weight on average per day, while the ones capped with the Chemspeed and manually lost 0.0078 % and 0.013 %, respectively. The results show that the capping machine is a reasonable alternative to industrial and manual capping, especially when space and budget are limitations in SDLs.
Abstract:Powder X-ray diffraction (PXRD) is a key technique for the structural characterisation of solid-state materials, but compared with tasks such as liquid handling, its end-to-end automation is highly challenging. This is because coupling PXRD experiments with crystallisation comprises multiple solid handling steps that include sample recovery, sample preparation by grinding, sample mounting and, finally, collection of X-ray diffraction data. Each of these steps has individual technical challenges from an automation perspective, and hence no commercial instrument exists that can grow crystals, process them into a powder, mount them in a diffractometer, and collect PXRD data in an autonomous, closed-loop way. Here we present an automated robotic workflow to carry out autonomous PXRD experiments. The PXRD data collected for polymorphs of small organic compounds is comparable to that collected under the same conditions manually. Beyond accelerating PXRD experiments, this workflow involves 13 component steps and integrates three different types of robots, each from a separate supplier, illustrating the power of flexible, modular automation in complex, multitask laboratories.