In this study, new activated carbons (ACs) were synthesized from a mixture of lemon and orange seeds (LOS) for toxic metal removal from aqueous solutions. Adsorbents have been produced by chemical activation with different activation agents (with H 3 PO 4 , ZnCl 2 and KOH) and activation temperature (600°C, 700°C, 800°C). The elemental analysis, FT-IR, XRD and SEM analyses were performed to determine the characterization of the ACs. A series of batch adsorption experiments were done to research the influence of various parameters such as pH, adsorbent dosage, contact time, temperature, the complexing agents on the toxic metal ions (Cu(II), Cr(III) and Ni(II)) removal capacity of ACs. Adsorption equilibration time was 60 min, the adsorption capacity was 118.02 mg/g for Ni(II) ions, 146.03 mg/g for Cr(III) ions and 150.45 mg/g for Cu(II) ions. The adsorption of toxic metal ions was observed as a maximum at pH = 5 on AC-ZnCl 2 (600°C) produced under N 2 atmosphere. The adsorption process was fitted with a Langmuir isotherm model and a pseudo-second-order kinetic equation, showing the metal ions adsorption on AC was monolayer coverage. Thermodynamic studies show that the adsorption is endothermic and spontaneous in nature. AC produced from the LOS mixture has not been encountered in the literature. A simple, easy-to-apply method has been developed for a new adsorbent prepared from a mixture of LOS with environmentally friendly, easy to produce, reusable, cost-effective, non-toxic and with good adsorption-desorption capacity. Therefore, this study will contribute to the world economy in terms of environmental and wastewater cleaning.