In this work a newly semi polar extraction phase of carboxylated multiwalled carbon nanotube (MWCNTs) reinforced sol-gel immobilized polypropylene hollow fiber was prepared by low temperature hydrothermal process. It is coupled with flame atomic absorption spectroscopy was employed in the extraction and determination of cobalt and cadmium ions in wastewaters. The main factors influencing the pre-concentration and extraction of the metal ions have been examined in detail. Detection limits obtained in this way for Co(II) and Cd(II) ions were 0.0186 and 0.024 ng mL(-1), respectively.