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An experimental fuel surrogate validation approach is proposed for a compression ignition application, and applied to validate a Jet-A POSF 4658 fuel surrogate. The approach examines the agreement of both physical and chemical properties of surrogate and target fuels during validation within a real compression-ignition engine environment during four sequential but distinct combustion phases. In-cylinder Mie Scattering measurements are applied to evaporating sprays to compare the behavior of the surrogate, its target fuel, and for reference, n-heptane. Early mixture formation and low temperature reaction behavior were investigated using 2-D broadband chemiluminescence imaging, while high temperature ignition and combustion chemistry were studied using OH chemiluminescence imaging. The optical measurements were combined with cylinder pressure-based combustion analysis, including ignition delay and premixed burn duration, to validate the global behavior of the surrogate.