The organo-clay used in this work was prepared from a Na-montmorillonite (Wyoming-USA deposit) by treatment with water solution of hexadecyltrimethylammonium cations. As organo-clays exhibit strong sorptive capabilities for organic molecules, 2-mercapto-5-amino-1,3,4-thiadiazole organofunctional groups, with potential usefulness in chemical analysis, were incorporated on its solid surface. The physically adsorbed reagent did not present any restrictions in coordinating with several metal ions on the surface. The resultant organo-clay complex exhibited strong sorptive capability for removing mercury ions from water in which other metals and ions were also present. The purpose of this work is to study the selective separation of mercury(II) from aqueous solution using the organo-clay complex, measured by batch and chromatographic column techniques, and its application as preconcentration agent in a chemically modified carbon paste electrode for determination of mercury(II) in aqueous solution.