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Traditionally catalysis research and development has been limited to large purpose-built labs, requiring years of planning and implementation before the first molecules were even examined. However, recent developments in microfluidics, robotics, system miniaturization and machine intelligence allow the decoupling of research from multi-million dollar purpose-built facilities. Additionally this scaling-down of research has significant benefits for the environment, development timelines and researcher workload. In this publication we demonstrate the construction of a microfluidic catalysis research platform contained within a standard hard-sided case measuring just 0.73 m 2 , consuming under 100 W of power, and generating 66.7 μL of chemical waste per min. The system integrates a purpose-built microreactor with hot-swappable chuck, vacuum enclosure, manifolds, pumps, robotic autosampling, open-source controls and thermographic performance analysis. The system was used to investigate nine chemically different activators for a zirconocene-catalyzed α-olefin polymerization through efficient experimentation and automated transfer learning ML-based data interpretation. The contributions of different chemical structures to catalytic productivity were analyzed. Conclusions made include those regarding co-catalyst chemistry and probable operating conditions. This work demonstrates that a compact flow-based microfluidic platform can screen exothermic catalytic reactions and interpret the results using machine intelligence. 

Microfluidic reactors with in situ spectroscopy have enabled many new directions of research over the last two decades. The miniature nature of these systems enables several key advantages in heterogeneous catalysis, which includes the reaction surface or interface accessible to spectroscopic equipment making the discovery of new catalytic materials possible. Devices fabricated with materials that are transparent to electromagnetic radiation enable in situ and in operando spectroscopy such as Raman, UV-Vis, and IR directly at the point of the reaction, and thus high fidelity, transient information on the reaction chemistry is available. Innovative designs with NMR, electrochemical impedance spectroscopy, x-ray techniques, or terahertz imaging have also advanced the field of heterogeneous catalysis. These methods have been successfully engineered to make major breakthroughs in the design of catalytic materials for important classes of chemical reactions. In this review, the authors provide an overview of recent advances in the design of microreactors with in situ spectroscopy for the study of heterogeneous catalysis to raise awareness among the vacuum science community on techniques, tools, existing challenges, and emerging trends and opportunities.