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Tailor-made multi-component fuels are currently being developed for advanced Diesel engines. Accordingly, there is renewed interest in the detailed evaporation characteristics of such multi-component fuels, in particular because soot formation in reacting Diesel sprays generally depends on the mixture formation upstream of the lift-off location. It is also well established that fuel components with different volatility are generally not coevaporative due to fractional distillation in the mixture formation process of spark-ignition engines, but it is not clear if this holds for Diesel-like sprays, in which evaporation and mixing are expected to be more rapid. Unfortunately, little work has been done in this field, and some of the previous results appear to be contradictory. This paper presents a new laser diagnostic approach, which yields the vapor-phase concentrations of two fuel components simultaneously in Diesel-like sprays.