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In this paper, the evolution of structural, textural and surface properties of attapulgite after treatment with increasing concentrations of hydrochloric acid (0.5, 1, 3 and 5 M) is reported. The solids obtained were characterized by SEM, XRD, FTIR and BET analysis. The surface properties were also evaluated using inverse gas chromatography at infinite dilution (IGC-ID) and finite concentration (IGC-FC). The IGC analysis permitted us to reach several parameters such as: specific surface area, BET constant with organic probes and the distribution functions of the adsorption energy sites on the solid surface. At dilute concentrations of acid, carbonates are eliminated and the specific surface area increases. However, the morphology and crystal structure of attapulgite are preserved. At higher concentrations of acid, dissolution of octahedral sheets and at the same time formation of an amorphous silica from the tetrahedral sheets occur. However, the fibrous morphology is still preserved. The calculation of distribution functions reveals a clear evolution in the heterogeneity of the surface during the acid treatment, the appearance of shoulders is attributed to the development of strong specific interactions between the injected polar probe and silanol groups on the surface of amorphous silica formed during the acid treatment.