A simple and sensitive cloud point extraction method for the preconcentration of ultra-trace amounts of nickel as a prior step to its determination by graphite furnace atomic absorption spectrometry was proposed. It is based on the reaction of nickel with 2-(5-bromo-2-pyridylazo)-5-dimethylaminoaniline (5-Br-PADMA) in HAc-NaAc buffer media and mixed micelle-mediated extraction of the complex using the anionic surfactant sodium dodecyl sulfate sodium (SDS) and non-ionic surfactant (1,1,3,3-Tetramethylbutyl) phenyl-polyethylene (Triton X-114). The optimal reaction and extraction conditions such as pH, concentration of 5-Br-PADMA, SDS and Triton X-114, equilibrium temperature, incubation, and centrifuge time were evaluated and optimized. Under the optimal conditions, the calibration graph was linear over the range 0.1-5.5 ng/mL of nickel with a correlation coefficient of 0.9942. The detection limit obtained was 0.031 ng/mL, and the relative standard deviation was 2.1% for nickel (c = 2 ng/mL, n = 6). The proposed method was successfully applied to the determination of nickel in water samples.