Recebido em 27/3/12; aceito em 20/10/12; publicado na web em 21/2/13 A simple, sensitive and selective cloud point extraction procedure is described for the preconcentration and atomic absorption spectrometric determination of Zn 2+ and Cd 2+ ions in water and biological samples, after complexation with 3,3',3",3'"-tetraindolyl (terephthaloyl) dimethane (TTDM) in basic medium, using Triton X-114 as nonionic surfactant. Detection limits of 3.0 and 2.0 μg L -1 and quantification limits 10.0 and 7.0 μg L -1were obtained for Zn 2+ and Cd 2+ ions, respectively. Relative standard deviation was 2.9 and 3.3, and enrichment factors 23.9 and 25.6, for Zn 2+ and Cd 2+ ions, respectively. The method enabled determination of low levels of Zn 2+ and Cd 2+ ions in urine, blood serum and water samples.