© 2019 Published under licence by IOP Publishing Ltd.This research highlights the chemical modification of one of the carbon nanostructures (multi-walled carbon nanotubes-COOH) with an artificial sweetener (saccharine) to synthesize a highly efficient absorbent material (MWCNTs-CO-Sac). This material was thereafter used to the packing column in solid phase extraction of cadmium and copper divalent ions from real samples. This nano-adsorbent was diagnosed with different techniques: Infrared spectroscopy (FTIR), Thermogravimetry (TG), Differential thermal analysis (DTA), powder X-ray diffraction (PXRD), energy-dispersive X-ray spectroscopy (EDX), Particle size distribution (PSD) and scanning electron microscopy (SEM). The effect of pH, sample and eluent flow rates, volume, type and concentration of eluent, volume of sample and interfering ions were studied to achieve the optimal conditions for solid phase extraction of Cd(II) and Cu(II) based on the inductively coupled plasma-optical emission spectrometry (ICP-OES). Moreover, the preconcentration factors were calculated to be 75. The results of a limit of detection (LOD) 0.07 μgL-1 and 0.09 μgL-1 for Cd(II) and Cu(II) respectively. The relative standard deviation (RSD %) of this study was 0.45% for Cd(II) and 0.51% for Cu(II). The optimized method was applied to soil and environmental water samples.