In this study, a new sorbent was synthesized based on the in-situ growth of the combined ZIF-67 and ZIF-8 on the surface of MIL101. Finally, the adsorbent was made into a thin film with the help of polyvinylidene difluoride polymer and was used in the TFME technique for the simultaneous measurement of cadmium(II) and lead(II) metal ions in aqueous and cosmetic samples using flame atomic absorption spectroscopy. In order to achieve maximum efficiency and sensitivity, parameters affecting the extraction and desorption processes were optimized. Under the optimized condition, the linearity of the method, the limit of detections (LODs), the limit of quantifications (LOQs), the relative standard deviations (RSDs%), and enrichment factors (EFs) were equal with 0.2-150.0 µg l-1, 0.059-0.159 µg l-1, 0.197- 0.530 µg l-1, 1.2 to 2.5% and 73-75, in water matrix, respectively. Then the optimal conditions for Pb and Cd were used in water and cosmetics samples by flame atomic absorption spectroscopy and acceptable results were obtained.
