A new approach was developed for sensitive determination of Fe(III) and Cu(II) ions using SnO2 nanopowder in the micellar medium on the contrary conventional cloud point extraction studies. The presented method contains a combination of solid-phase extraction and cloud point extraction. According to this procedure, the metal ions were firstly retained on modified SnO2 nanopowder and then passed to the surfactant-rich phase. The effect of experimental variables including pH, concentration of reagents, eluting solution, incubation time, equilibration temperature, sample volume, and effects of interfering ions have been investigated and optimized systematically. The calibration graphs were linear in the range of 0.23-100.00g L-1 and 0.30-110.00g L-1 for Fe(III) and Cu(II), respectively. Under optimized conditions, the limits of detections were 0.07 and 0.09g L-1 for Fe(III) and 0.09g L-1 for Cu(II). The proposed method offers satisfactory analytical features by means of combining two different and efficient preconcentration techniques. In addition, the method can be evaluated as an alternative and fast method according to only-surfactant-mediated extractions. The validation of method was carried out by recovery tests and certified reference material (CRM) analysis. The acceptable and compatible results were obtained in the analysis of CRM and real samples.