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Development of new fuels and engine combustion strategies for future ultra-low emission engines requires a greater level of insight into the process of emissions formation than is afforded by the approach of engine exhaust measurement. The paper describes the development of an in-cylinder gas sampling system consisting of a fast-acting, percussion-based, poppet-type sampling valve, and a heated dilution tunnel; and the deployment of the system in a single cylinder engine. A control system was also developed for the sampling valve to allow gas samples to be extracted from the engine cylinder during combustion, at any desired crank angle in the engine cycle, while the valve motion was continuously monitored using a proximity sensor. The gas sampling system was utilised on a direct injection diesel engine co-combusting a range of hydrogen-diesel fuel and methane-diesel fuel mixtures.