The hydrogen evolution reaction (HER) plays a crucial role in clean energy production in hydrogen fuel cells. In order to utilise this process effectively, new catalysts are required that are cheap, non-toxic and efficient. In this context, 2D materials such as transition metal dichalcogenides (e.g. MoS 2 ) should offer the desired properties but have so far proven difficult to manufacture into useful devices. In this work, liquid|liquid interfaces are used for the assembly and testing of the catalytic efficiency of a number of 2D materials and their composites, exploiting the ability of the materials to self-assemble at these interfaces and be tested electrochemically in situ. MoS 2 , WS 2 , and graphene were developed for hydrogen evolution at the water|1,2-dichlorobenzene (DCB) interface. The exfoliation process was carried out in DCB and resulted in multi-layer MoS 2 , few layer WS 2 and graphene: when assembled at the water|DCB interface, these materials acted as efficient HER catalysts. HER was investigated using voltammetry, with bulk reaction kinetics monitored by in-situ UVvisible spectroscopy at a constant potential. MoS 2 exhibited the highest performance of the catalysts examined, with an average rate constant of 0.0132 ± 0.063 min -1 at an applied Galvani potential of +0.5 V. This is ascribed to the sulphur edge sites of MoS 2 , which are known to be active for hydrogen evolution predominantly.