A novel dispersive liquid-liquid microextraction (DLLME) procedure was developed using 3hydroxy-4-methy1-2(31-1)-thiazole- thione for the separation and preconcentration of Cu(II) prior to quantification by flame atomic absorption spectrometry (FAAS). Ethanol (0.5 mL) was used as the dispersion solvent, and a mixture of ethanol, carbon tetrachloride, and 3-hydroxy4methy1-2(3H)thiazolethione was rapidly injected with a syringe into a sample containing Cu(ll). Fine droplets formed, and then the mixture was centrifuged. The lower organic phase was isolated and dissolved in concentrated nitric acid to a total volume of 250 pL. A 25-4 aliquot of this solution was introduced into a FAAS using a microinjection system. The influence of parameters such as pH, volume, and type of the extraction solvent, the volume and type of the dispersion solvent, and the amount of 3hydroxy-4-methy1-2(3H)-thiazole- thione was examined. The relative standard deviation (%RSD), limit of detection (LOD), limit of quantification (LOQ), preconcentration factor (PF), and enhancement factor (EF) were 5.34%, 2.54iig/L, 8.48 pg/L, 60, and 42, respectively.