A new technique for extraction of metal ions in water samples, combination of multiwalled carbon nanotubes and polypropylene hollow fiber as a solid-liquid microextraction technique Eshaghi, Z., Farzin, F., Ahmadpour, A., Ahmadi Golsefidi, M., Ghasemi, E., Saify, A., and Tanha, A.K. A novel, simple, cost-effective, and sensitive method was developed for the determination of metal ions in water samples using multi-walled carbon Nanotubes as solid-phase adsorbents coupled with hollow fiber liquid phase microextraction. In this research a simple microextraction method was applied for the pre-concentration and extraction of metal ions from water samples. We used of octanol, as a liquid phase, and multi-walled carbon Nanotubes (MWCNTs) as the solid phase which both were impregnated into the pores of polypropylene hollow fiber as a solid/liquid microextraction device for extraction of metal ions from water samples. For optimization of the method different parameters such as; kind of organic extractor solvent, extraction time, agitation speed and pH were monitored and controlled. The effect of oxidation on the structural integrity of multiwalled carbon nanotubes through different agents has been studied. For these purpose, multiwalled carbon Nanotubes (MWCNTs) were functionalized by different agents like; nitric acid, citric acid and KMnO4 (PP) solutions. Here also the functionalized MWCNTs were sonicated in octanol and then injected into the porous hollow fiber tube. The method was evaluated and finally applied to waste water sample and results were obtained. All microextraction experiments were carried out at room temperature, 25oC.