Spectroscopy offers a rapid and non-destructive approach for characterizing carbon in fire-affected soils, particularly in the Cerrado biome. Distinguishing total carbon (TC) from pyrogenic carbon (PC) remains challenging because both exhibit similar spectral signatures. This study evaluates the performance of Vis–NIR, MIR, and XRF spectroscopy for estimating TC and PC in soils under prescribed fire (PRF) and no-fire management (NPRF), as well as in associated charred materials.Vis–NIR provided the best estimates of TC in PRF soils, reflecting its sensitivity to fire-induced changes in organic matter. In NPRF soils, MIR showed the highest performance for TC due to its responsiveness to functional groups in more heterogeneous, minimally disturbed matrices. For PC, combining Vis–NIR and MIR improved predictions in both management systems, with higher accuracy in NPRF soils. XRF, although highly sensitive to fire-derived elements such as Fe, Si, and Ca, showed limited performance for PC in soils; however, it achieved the best results for PC estimation in charred residues. Vis–NIR was most effective for TC in the same material.The results indicate clear differences in TC and PC behavior across fire regimes. PRF soils showed lower TC and greater thermal alteration, whereas NPRF soils preserved higher TC with less aromatic enrichment. Although PC prediction remained moderate across models, the complementary information from Vis–NIR, MIR, and XRF improved the interpretation of the physicochemical factors controlling carbon variability. Refining multispectral calibration strategies will strengthen TC and PC discrimination and support carbon monitoring and fire-management planning in tropical ecosystems.
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