X-ray diffraction (XRD), differential thermal analysis (DTA) and 27Al and 29Si solid state MAS-NMR techniques were used to monitor the fractionation steps of a brazilian smectite, previously crushed, from Campina Grande, Paraíba. The sand, silt and clay fractions were obtained by physical and chemical treatments. The XRD analysis of sand and silt fractions showed that both fractions had predominant quartz and feldspar, respectively. The XRD results of the K + saturated and heated clay fraction confirmed that the natural clay belongs to the 2:1 clay-mineral group, whereas the analysis of the Mg 2+ saturated and glycolated clay fraction confirmed the presence of a smectite group clay. The MAS-NMR results of 27Al and 29Si showed that the sand fraction contains 79% of quartz and the silt fraction contains 55% of quartz, while the clay fraction is rich in smectite with low isomorphic replacement of Si by Al, and contains 38 % of quartz.