The influence of clay preparation procedure on sorption and hydrolysis of carbaryl (1-naphthyl, A-methyl carbamate) by the reference smectite SWy-2 was examined. For research purposes, reference clays are sometimes used without purification, or more commonly, the <2 μm size fraction is obtained by gravity sedimentation or low-speed centrifugation. We determined that these common methods did not remove all the inorganic carbonate impurities present in SWy-2, and that these impurities caused alkaline conditions in aqueous clay suspensions leading to the alkaline hydrolysis of carbaryl to 1-naphthol. The hydrolytic activity of homoionic K-SWy-2 disappeared once carbonates were eliminated. Two methods were evaluated for preparing K-SWy-2 devoid of inorganic carbonates. In Method A, inorganic carbonates were first removed by incremental additions of a 0.5 M sodium acetate buffer (pH 5.0) until the clay suspension reached pH 6.8, followed by low-speed centrifugation to obtain the <2 μm size fraction; in Method B, the order of these steps was reversed. Carbaryl hydrolysis was used as a probe to determine the effectiveness of the two methods in terms of the removal of carbonate accessory minerals. Homoionic K-SWy-2 obtained by Methods A and B produced near neutral pH when suspended in water and hydrolysis of carbaryl in these suspensions was not evident. In this regard, both clay preparation methods were acceptable. However, there were procedural advantages with Method B, which is therefore recommended for the partial purification of reference clays, as detailed in this paper.