M.Tech. / Studies on the removal of nickel and platinum are increasing due to the toxicities of these metals. Several methods are currently used to extract these metals however they present limitations. There is hence a need to develop an efficient method for the removal of nickel and platinum from aqueous solution. A study on the use of purified multiwalled carbon nanotubes (purified MWCNTs) and a phosphine derivatized multiwalled carbon nanotubes for the extraction of these metal ions from solution was therefore undertaken. Multiwalled carbon nanotubes (MWCNTs) were produced by nebulised spray pyrolysis, purified by a multi-step technique and functionalized. Phosphine moieties were attached to the bromoarylated- MWCNTs by metallated phosphide route leading to triphenylphoshine linked MWCNTs (Tpp-MWCNTs). As produced, purified and triphenylphosphine linked multiwalled carbon nanotubes were characterized by various techniques, including microscopic and spectroscopic techniques, thermal, elemental and surface analysis. Transmission and scanning electron microscopy used revealed purified MWCNTs had insignificant impurities. X-ray photoelectron spectroscopy (XPS) results showed that triphenylphosphine linked multiwalled carbon nanotubes had 2.6% phosphorus. Zeta potential results demonstrated that purified MWCNTs had positive surface charges at acidic pH. Triphenylphosphine linked multiwalled carbon nanotubes were negatively charged on the surface in acidic media. Batch adsorption experiments were carried out to investigate the removal of nickel and platinum from aqueous solutions. Several parameters which influence the adsorption process were studied, including the effect of pH, the contact time and the effect of initial concentration on adsorption. The adsorption models for the Freundlich and Langmuir isotherms were employed to fit the experimental data. Triphenylphosphine linked MWCNTs removed more nickel (84.68 mg/g) than purified MWCNTs (77.39 mg/g). In contrast, purified MWCNTs removed more platinum (10.5 mg/g) than triphenylphosphine linked MWCNTs (6.01 mg/g). Experimental data for nickel fitted both Freundlich and Langmuir models well whereas only Langmuir model fitted well for platinum. The adsorption of nickel and platinum was indeed found to be pH, time and initial concentration dependent. Metal species (nickel and platinum) in solution had also influenced the uptake of these metals using purified-and Tpp-MWCNTs.