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A cloud point extraction procedure was presented for the preconcentration of copper, nickel and cobalt ions in various samples. After complexation with methyl-2-pyridylketone oxime (MPKO) in basic medium, analyte ions are quantitatively extracted to the phase rich in Triton X-114 following centrifugation. 1.0molL⁻¹ HNO₃ nitric acid in methanol was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The adopted concentrations for MPKO, Triton X-114 and HNO₃, bath temperature, centrifuge rate and time were optimized. Detection limits (3SDb/m) of 1.6, 2.1 and 1.9ngmL⁻¹ for Cu²⁺, Co²⁺ and Ni²⁺ along with preconcentration factors of 30 and for these ions and enrichment factor of 65, 58 and 67 for Cu²⁺, Ni²⁺ and Co²⁺, respectively. The high efficiency of cloud point extraction to carry out the determination of analytes in complex matrices was demonstrated …