| Summary: | Soot is characterized by a multiscale structural organization; the only diagnostic tool that can give access to it is the transmission electron microscope (TEM). However, as it is a diffraction-based technique, TEM images only conjugate aromatic systems and, thus, it is particularly useful to combine it with electron energy-loss spectroscopy (EELS), which is able to provide quantitative information about the relative abundance of sp<sup>3</sup> and sp<sup>2</sup> hybridized carbon. In this paper, a method for the EELS spectrum analysis of carbonaceous materials, recently developed for electron-irradiated graphite and glassy carbon composition analysis, has been applied for the first time on soot samples, in order to test its performance in soot nanostructure study in combination with TEM and high-resolution TEM (HRTEM). Soot samples analyzed were collected in the soot inception region of premixed flames of different hydrocarbon fuels. EELS, in agreement with TEM and HRTEM, showed a quite disordered and heterogeneous structure for young soot, with a relatively low sp<sup>2</sup> content and slight presence of fullerene-like structures, more evident in the case of methane soot hinting to the effect of more saturated aliphatic fuels on soot characteristics at soot inception.
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