This research study was designed with the aim to prepare plant extract-mediated iron oxide nanoparticles (IONPs) and different chemically modified carbon adsorbents from the Parthenium hysterophorus plant and then optimize the carbon adsorbents by evaluating their adsorption applications in wastewater for the selected metal ions like arsenic (As 3+ ), lead (Pb 2+ ), and cadmium (Cd 2+ ). The Fourier transform infrared spectroscopy (FTIR) technique was used to highlight functional groups in plant-mediated IONPs and chemically modified carbon adsorbents. A scanning electron microscopy study was conducted to explain the surface morphology of the adsorbents. Energy-dispersive X-rays was used for elemental analysis and X-ray diffraction for particle size and crystallinity of the adsorbents. From the study, it was found that the best optimum conditions were pH = 5−6, initial concentration of adsorbate of 10 mg/L, dose of adsorbent of 0.01 g, contact time of 90−120 min of adsorbent and adsorbate, and temperature of 25 °C. At optimum conditions, the adsorption capacities of IONPs for arsenic (As) 144.7 mg/g, lead (Pb) 128.01 mg/g, and cadmium (Cd) ions 122.1 mg/g were recorded. The activated carbon at optimum conditions showed adsorption capacities of 46.35 mg/g for As, 121.95 mg/g for Pb, and 113.25 mg/g for Cd ion. At equilibrium, Langmuir, Freundlich Temkin, and Dubinin−Radushkevich isotherms were applied on the experimental adsorption data having the best R 2 values (0.973−0.999) by the Langmuir isotherm. High-correlation coefficient R 2 values (0.996−0.999) were obtained from the pseudo-second-order for all cases, showing that the adsorption process proceeds through pseudo second-order kinetics. The apparent adsorption energy E value was in the range of 0.24−2.36 kJ/mol. The adsorption capacity of regenerated IONPs for As gradually decreased from 144.8 to 45.67 mg/g, for lead 128.15 to 41.65 mg/g, and cadmium from 122.10 to 31.20 mg/g in 5 consecutive cycles. The study showed that the synthesized IONPs and acid-activated carbon adsorbent were successfully used to remove selected metal ions from wastewater.