An experimental study, using size measurements, X-ray diffraction (XRD), scanning electron microscopy (SEM) and inverse gas chromatography at infinite dilution (IGC-ID) and finite concentration (IGC-FC) conditions, has been carried out to evaluate, respectively, the changes of particles size, crystalline phases, morphology and surface properties evolution of attapulgite powder after grinding in wet media. The particles size decreases significantly after grinding in ball mill in different liquid media. The SEM analysis shows that the fibers are preserved during grinding in aqueous media. With IGC-ID, after grinding using wet ball milling in hydrochloric acid, the values of gamma(d)(s) determined by injection of alkane probes decrease significantly because of the disappearance of the insertion sites able to retain the probes. In the same grinding conditions, with IGC-FC, the specific surface area obtained with octane probe increases significantly from 114 m(2)/g to 156 m(2)/g. (C) 2020 Elsevier B.V. All rights reserved.