A new podand-type dioxaoctanediamide-based chemosensor having two pyrene moieties was prepared, and its fluoroionophoric behaviorstoward transition-metal ions were investigated. Pyrene-appended dioxaoctanediamide
1 showed a selective fluorescence quenching towardHg
2+ ions over other transition-metal ions in an aqueous methanol solution. Unique responses in pyrene monomer and excimer emissionsallowed selective ratiometric determination of Hg
2+ ions in aqueous environments, and the detection limit was found to be 1.6 × 10
-6 M.