Borosilicate crimp top vials (Agilent Technologies, 10 mL, 23 × 46 mm) were charged with 5 mg of the photocatalyst and transferred to a Chemspeed Accelerator SWING platform for liquid transfer. Degassed aqueous ascorbic acid solution (0.1 mL) and degassed stock solution of H2PtCl6 were loaded into the system and the whole system was flushed with nitrogen for 4 hours. Liquids were automatically dispensed into the vials and the vials were capped under inert conditions by the system. The vials were then ultrasonicated for 10 minutes before illumination with an Oriel Solar Simulator 94123A (1 Sun, classification IEC 60904-9 2007 spectral match A, uniformity classification A, temporal stability A, 1600 W Xenon lamp, 12 × 12 in. output beam, Air ass 1.5G filter, 350-1000 nm) and continuous dispersion of the photocatalyst on a Stuart roller bar SRT9.. After photocatalysis, the samples were measured on a Shimadzu GC-2010 plus equipped with a BID detector using a HS-20 headspace auto-sampler and sampling from the headspace of the vial. Helium was used as the carrier-gas and the gases were separated on a 5 Å Molseive capillary column. The gas amounts were calculated by referencing against standard gases with known concentrations of hydrogen and CO. Hydrogen and CO dissolved in the reaction mixture was not measured and the pressure increase generated by the evolved hydrogen and CO was neglected in the calculations.