The International Agency for Research on Cancer (IARC) stated that chromium in the form of Cr(VI) has been deemed to be a class-A human carcinogen. It has been a major contaminant associated with wastewater. Moreover, the existence of heavy metals in aquatic systems is a critical concern for the environment as well as industries that manufacture or consume these particular elements. In order to remove these particular toxic metals, several well-known conventional methods including ion-exchange, filtration and adsorption are used. Amongst these methods, adsorption offers significant advantages such as the low-cost materials, ease of operation and efficiency in comparison to the other conventional methods.

The aim of this work was to develop nanomaterials (particles and fibers) to address some critical issues for the treatment of heavy metals, especially chromium in aqueous systems. Furthermore, the use of nanomaterials and how they relate to nanoscale operations at the biological level has generated considerable concerns in spite of their novel properties.

The first part of this thesis deals with the synthesis and characterizations of Fe₃O₄, magnetite, as nanoparticles which were further coated with surfactants bis(2,4,4-trimethylpentyl)dithiophosphinic acid, Cyanex-301, and 3-Mercaptopropionic acid with the active compound being the thiol (SH) groups, that will suffice as a viable material for Cr(VI) removal from aqueous solutions. The proposed mechanism was the complexation between the thiol group on Cyanex-301 and 3-Mercaptopropionic acid, respectively. The effect of different parameters on the adsorption including contact time, initial and final Cr(VI) ion concentration and solution pH was investigated.

The second part of this thesis encompassed the fabrication of flexible nanocomposite materials, with a large surface area and architecture for the removal of Cr(VI) in batch and continuous flow mode. A technique known as electrospinning was used to produce the nanofibers. The flexible yet functional materials architecture has been achieved by growing ZnO nanorod arrays through chemical bath deposition on synthesized electrospun poly-L-lactide nanofibers. Moreover, polyacrylonitrile nanofibers (PAN) were synthesized and adapted by the addition of hydroxylamine hydrochloride to produce amidoxime polyacrylonitrile nanofibers (A-PAN). Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to identify the morphologies and particle sizes whereas Fourier-Transform Infrared spectroscopy (FT-IR) was used to identify either the presence or absence of functional groups for the formation of PAN and A-PAN nanofibers. The optimization of functionalized nanoadsorbents to adsorb Cr(VI) was also carried out to investigate the effect of experimental parameters: contact time, solution pH, initial, final and other metal ion concentration. Commercially manufactured pristine engineered (TiO₂, ZnO and SiO₂) nanoparticles and lab-made functionalized (Fe₃O₄ and CeO₂) nanoparticles were studied while the powders were suspended in appropriate media by Dynamic Light Scattering (DLS) to identify their cytotoxicity effects.