AbstractThe aim of this study was to utilize processed orange peel waste (TOP) as an adsorbent to remove Cu(II) and Ni(II) ions from aqueous solutions. As a result of systematic experiments to determine the optimal conditions, it was determined that the most suitable conditions for the effective removal of Cu(II) ions were 400 mg/L initial concentration, 100 min contact time, 0.2 g adsorbent dosage, and a solution pH of 5.92. Similarly, the optimal conditions for the removal of Ni(II) ions were determined by systematic experiments to be 300 mg/L initial concentration, 0.2 g adsorbent dosage, 100 min contact time, and a solution pH of 6.19. The systematic experiments also included further investigation of the surface properties of TOP, and promising results were obtained by tests at three different temperatures (298, 308, and 318 K). The adsorption capacities for Cu(II), Ni(II), and Ni(II) were determined as 72.99, 75.18, and 76.33 mg/g, 42.55, 44.44, and 46.29 mg/g, respectively. Further analysis of the adsorption kinetics revealed that the pseudo‐second‐order model accurately represented the experimental data for both ions. Thermodynamic investigations provided strong evidence that the adsorption process of these noble metal ions on TOP is endothermic and spontaneous. The results of this study emphasize that TOP, with its low cost, easy‐to‐use nature, and high adsorption capacity, can be considered a long‐term solution for environmental remediation and water treatment in sustainable engineering applications.