A new pyrene appended diaza-18-crown-6 ether derivative 1 has been prepared and its fluoroionophoric properties toward transition metal ions were investigated. Compound 1 exhibited a high Hg2+-selectivity over other transition metal ions as well as alkali and alkaline earth metal ions in aqueous acetonitrile solution. The ratiometric analysis of the monomer and excimer emissions of pyrene successfully signals the presence of Hg2+ ions. The detection limit for Hg2+ ions was found to be 3.1 ´ 10-6 M in 50% aqueous acetonitrile solution at pH 8.1. Competition experiments also suggest that the compound could be utilized as a selective and sensitive fluorescent chemosensor for the analysis of micromolar Hg2+ ions in physiological and environmental samples.