Two new azo-azomethine receptors, H2L1 and H2L2, containing hydrazine, naphthalene and different electron withdrawing groups, Cl and NO2, have been designed and synthesized for qualitative and quantitative detection of Cu2+ and Co2+ in aqueous media. The crystal structure of H2L1is reported. The H2L1was used as a chemosensor for selective detection of trace amount of Cu2+ in aqueous media. H2L2 was also applied to naked-eye distinction of Cu2+ and Co2+ from other transition metal ions in aqueous media. Detection limit of Cu2+ is 0.07 ppm and 0.08 ppm, in water, for H2L1 and H2L2, respectively, which are lower than the World Health Organization (WHO) recommended level. The binuclear Cu(II) and Co(II) complexes of the receptors have been also prepared and characterized using spectroscopic methods and MALDI-TOF Mass analysis. Furthermore, the binding stoichiometry between the receptors upon the addition Cu2+ and Co2+ has been investigated using Job's plot. Moreover, the fluorescence emission spectra of the receptors and their metal complexes are also reported.