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A cloud point extraction (CPE) procedure which was developed for the separation and preconcentration of trace amounts of cobalt is combined with flame atomic absorption spectrometry (FAAS) to determine trace amounts of cobalt in water and food samples. The procedure is based on the formation of the hydrophobic complex between Co(II) and 4-methoxy-2-sulfo-benzenediazoaminoazo-benzene (MOSDAA) followed by its extraction into a Triton X-114 surfactant-rich phase. The parameters such as pH of sample, concentrations of MOSDAA and Triton X-114, equilibrium temperature, and equilibrium time, which affect both complexation and extraction, are optimized. Under the selected optimum conditions, the preconcentration of 10.0 mL, 0.1 μg mL−1 Co(II) solution results in a limit of detection of 0.47 ng mL−1 (3σ) and an enrichment factor of 19. A relative standard deviation of 2.78% (,  μg mL−1) for the determination of Co(II) is obtained. The proposed method was applied for the determination of trace amounts of cobalt in river water and millet samples with satisfactory results.