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This paper aims to evaluate the ability of VNIR proximal soil spectroscopy to determine post-fire soil chemical properties and discriminate fire severity based on soil spectra. A total of 120 topsoil samples (0–3 cm) were taken from 6 ha of unburned (control (CON)) and burned areas (moderate fire severity (MS) and high fire severity (HS)) in Mediterranean Croatia within one year after the wildfire. Partial least squares regression (PLSR) and an artificial neural network (ANN) were used to build calibration models of soil pH, electrical conductivity (EC), CaCO₃, plant-available phosphorus (P₂O₅) and potassium (K₂O), soil organic carbon (SOC), exchangeable calcium (^exCa), magnesium (^exMg), potassium (^exK), sodium (^exNa), and cation exchange capacity (CEC), based on soil reflectance data. In terms of fire severity, CON samples exhibited higher average reflectance than MS and HS samples due to their lower SOC content. The PCA results pointed to the significance of the NIR part of the spectrum for extracting the variance in reflectance data and differentiation between the CON and burned area (MS and HS). DA generated 74.2% correctly classified soil spectral samples according to the fire severity. Both PLSR and ANN calibration techniques showed sensitivity to extract information from soil features based on hyperspectral reflectance, most successfully for the prediction of SOC, P₂O₅, ^exCa, ^exK, and CEC. This study confirms the usefulness of soil spectroscopy for fast screening and a better understanding of soil chemical properties in post-fire periods.