This paper reports an environmentally friendly analytical technique by extraction and pre-concentration of metal ions in cloud point for increased sensitivity and replacement of toxic solvents. The cloud point extraction (CPE) proved to be an easy, cheap, efficient and safe method for pre-concentrate trace metals. Cadmium and nickel were extracted simultaneously using complexes of dithiocarbamate in acidic medium, and quantitatively extracted with surfactant Triton X-114 and determined by atomic absorption spectrophotometry (AAS). Under optimal conditions, the limits of quantification (LQ) were 4,92 µg L-1 for Cd and 17,4 µg L-1 for Ni. The proposed method was applied to the quantification of cadmium and nickel in water sample, with satisfactory results.