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This paper describes how the analytical methodology for fuels and exhaust gases was selected and developed for the experimental sectors of the EPEFE study. It covers the selection of standard test methods for fuels analysis and addresses how round-robin exercises in non-standard areas of fuels analysis were designed, organised, monitored and reviewed, and then used to define the approach to (and the scope of) the speciated fuel analyses. The paper also addresses how the exhaust gas analysis was designed in relation to emissions testing methodology. The means used to evaluate and, where necessary, optimise the exhaust gas speciation capabilities of participating laboratories, and in which round-robin activities were a key element, are also explained.