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2-(3-Ethylthioureido)benzoic acid was prepared and characterized by electronic spectrum, elemental analysis, Fourier transform infrared spectroscopy, ¹H nuclear magnetic resonance spectrum and mass spectrum. The produced ligand was applied for the preconcentrative of Fe³⁺, Co²⁺, Cu²⁺ and Zn²⁺ in aqueous samples by cloud point extraction methodology. Triton X-114 was used as extractant. Experimental parameters that may affect the extraction process were examined and optimized; such as pH, ligand and triton concentrations, type of diluting solvent, extraction temperature and ionic strength. The calibration curves were linear upto 500 μg L⁻¹ for Fe³⁺, Cu²⁺ and Zn²⁺ and upto 200 μg L⁻¹ for Co²⁺. The achieved detection limits were 1.5, 0.23, 0.71 and 0.35 μg L⁻¹ for Fe³⁺, Co²⁺, Cu²⁺ and Zn²⁺ respectively. The accuracy was established by analysis of certified reference materials (Seronorm whole …