Abstract
Photochemical synthesis and photocatalysis in droplet microreactors represent promising approaches to relieve the global energy and environmental crises. Here, we describe a protocol for studying microdroplet photoreaction at an individual droplet level based on in situ micro-Raman spectroscopy. We provide details of superhydrophobic substrate preparation, microdroplets generation, photoreactions performing, and data analyses. In addition, we show the operational details of preliminary scale-up tests of microdroplet photoreaction for practical application. For complete details on the use and execution of this protocol, please refer to Li et al. (2022).