A rapid, simple, selective, economical, and sensitive dispersive liquid-liquid microextraction methodology has been established for the preconcentration of copper (Cu) at trace levels. The Cu(II) was complexed with 1-(2-pyridylazo)-2-naphthol; ethanol and carbon tetrachloride were used as disperser and extraction solvents, respectively. To obtain quantitative recovery of Cu(II), the effects of parameters influencing its extraction efficiency and subsequent determinations, i.e., pH, amount of complexing reagent, extraction time, and type and volume of disperser and extraction solvents, were examined. LOD and LOQ were 0.06 and 0.20 mu g/L, respectively. The enrichment factor of the proposed method was 60, and the RSD <5%. TMDA 51.3 and TMDA 70 fortified water certified reference materials were analyzed for validation of the procedure. The developed microextraction procedure has been used for the preconcentration of Cu(II) in water samples with acceptable results.