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This work compared the surface functional group (SFG) types and concentrations and sp 3 /sp 2 hybridization ratios of in-cylinder soot samples generated by a heavy-duty diesel engine when employing n -heptane and a toluene/ n -heptane mixture (20% toluene by volume) as the fuels. In-cylinder soot samples were obtained from a total cylinder sampling system, and the SFGs and sp 3 /sp 2 hybridization ratios were analyzed using Fourier transform infrared and X-ray photoelectron spectroscopy. Despite the differences in fuel formulation, both n -heptane and n -heptane/toluene soot exhibited similar trends in terms of changes in the SFGs concentrations and sp 3 /sp 2 hybridization ratios during the combustion process. However, the addition of toluene to the n -heptane was found to increase the concentrations of all SFGs as well as the sp 3 /sp 2 hybridization ratio. The C OH and C O group concentrations exhibited a bimodal distribution for both the n -heptane and n -heptane/toluene soot throughout the combustion process, with the concentrations peaking in the premixed and diffusion combustion phases, respectively. In contrast, the relative amounts of aliphatic C H groups decreased in the premixed combustion phase, increased in the early diffusion combustion phase, and then decreased in the subsequent combustion phase. The sp 3 /sp 2 hybridization ratios obtained from both fuel soot were observed to initially decrease, then to increase before a decrease during the combustion process. There was a definite correlation between the sp 3 /sp 2 hybridization ratio and the relative concentration of aliphatic C H groups. [ABSTRACT FROM AUTHOR]