Acloud point extraction (CPE) method for preconcentration of Pb(II), Fe(III) and Cr(III) has been established. This is based on the complexation of the metal ions with p-nitrophenylazoresorcinol (Magneson I) at pH 6.5 in the presence of non-ionic surfactant of octylphenoxy polyethoxyethanol (Triton X-114), prior to their determination by flame atomic absorption spectrometry (FAAS). The main factors affecting CPE efficiency, such as sample pH, complexing agent concentration, Triton X-114 concentration, temperature and incubation time were investigated. Under the optimized conditions, the detection limits (3s, n = 10) of Pb(II), Cr(III) and Fe(III) were 2.5, 2.3 and 1.9 μg L-1, respectively. The relative standard deviation for ten replicate determinations of the analytes was less than 2.4%. The validation of the procedure was carried out by analysis of certified reference materials. The proposed method has been applied to the determination of lead, chromium and iron in tap water and some food samples.