A new coupled cloud point extraction (CPE) was developed as prompt, easy and economical preconcentration technique for spectrophotometric determination of tiny amounts of Fe 3+ and Hg 2+ in real samples. A modern thiazolylazo ligand [methyl phenyl thiazolyl azo]-3-methyl-4-methoxy-2-naphthol (MPTAN) was done for the CPE method in the preconcentration of Fe 3+ and Hg 2+ as an earlier step to its characterization by UV-VIS spectrophotometry. The analytical manner includes the formation of under study metals complex with new ligand and quantitatively extracted to the Cloud point layer (CPL) of TritonX-100 after heating. The concentration of MPTAN, metals, pH, thermodynamic data and volume of surfactant was optimized. The investigation of stoichiometry has the ratio of metal to ligand of 1:1. Under finest settings and conditions, the calibration curve was found to be linear in the concentration range of two ions (0.05-10) ppm and the limit of detection for Fe 3+ and Hg 2+ are (0.016 and 0.041) ppm respectively. The suggested CPE has an excellent methodology for characterization of trace metal ions in surrounding samples with a complex matrix as in soils, water, vegetable, meats, and fruits.