Adsorption isotherms have been determined for the intercalation of cadmium ions (Cd2+) into layered hydrophobized montmorillonite (HDP-M) and calumit (DBS-C) sheets dispersed in ethanol (1)-cyclohexane (2) mixtures. The amount of Cd2+ adsorbed depended strongly on the composition of the binary liquid; at an ethanol mole fraction of 0.05 (x(1) = 0.05), 95% of the added Cd2+ is located in the ethanolic nanoreactor at the HDP-M (or DBS-C) surface. CdS nanoparticles have been generated in situ in ethanolic nanoreactors at the HDP-M and DBS-C surfaces. Absorption spectrophotometric measurements provided information on the number of CdS nanoparticles formed and on their absorption edges, bandgaps, and mean diameters. Good correlations have been obtained between the adsorption isotherms and the size (and the amount) of the CdS formed. X-ray diffractometry established that CdS nanoparticles stretched the HDP-M and DBS-C lamellas unevenly upon intercalation.