The tremendous increase in the use of heavy metals over the past few decades has inevitably resulted in an increased flux of metallic substances in the environment. These metals are of special concern because they are non-degradable, which therefore increases their concentration continuously in the environment. Hence, it is essential to remove these elements from wastewater. Cobalt and nickel elements, for example, include higher chances of development of lung, nose, larynx, respiratory failure; birth defects; and they have been listed as carcinogenic. Hence, it is essential to remove these elements from wastewater. Sorption is one of the more popular methods for the removal of heavy metals from the aqueous solutions. In this thesis, Sorel's cement and four modified Sorel's cements; Sorel's cement- silica gel (SCSI), Sorel's cement- sodium dihydrogen orthophosphate, (SCPH), Sorel's cement modified by hydrothermal (SCHY) and microwave (SCMI) techniques were synthesized and used as sorbent materials for the removal of cobalt (II) and nickel (II) ions from wastewater. The synthesized sorbent materials were characterized using advanced analytical techniques such as: Differential Thermal Analysis (DTA), X-ray diffraction (XRD), Scanning Electron Microscope (SEM), Atomic Force Microscope (AFM) and Fourier Transform Infrared Spectroscopy (FTIR). Various parameters affecting the sorption of these metal ions from aqueous solution have been studied in terms of particle size, shaking time, metal ion concentrations, hydrogen ion concentration, as well as temperature...