A simple, sensitive, and greener method for green extraction and preconcentration of lead from aqueous media and further assay by UV-Vis spectrophotometer has been developed using 1,5 diphenylthiocarbazone (dithizone). Several factors of dispersive liquid-liquid microextraction (DLLME) including the type and volume of extraction and dispersive solvents, shaking time, the concentration of dithizone as a complexing agent, and pH were optimized. Under optimum selected conditions, the limit of detection (LOD), the limit of quantification (LOQ), the linearity range, the relative standard deviation (RSD), and the Enrichment factor (EF) of the proposed method were obtained at 0.007 ppm, 0.025 ppm, 0.01-0.1 ppm, 4.3% (n = 3) and 40, respectively. This proposed method was successfully applied in the analysis of three synthetic water samples and good spiked recoveries over the range of 96.0–98.5% were obtained.