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Biodegradable and eco-friendly adsorbents composed of natural carbohydrates have been used to replace carbon-based materials. This study presents a natural carbohydrate-based chitosan/pectin (CS/Pec) hydrogel adsorbent to remove Pb(II) from aqueous solutions. The physical CS/Pec hydrogel was prepared by blending aqueous CS and Pec solutions at 65 °C, preventing the use of toxic chemistries (crosslinking agents). The thermosensitive CS/Pec hydrogel was quickly created by cooling CS/Pec blend at room temperature. The used strategy created stable CS/Pec hydrogel against disintegration and water dissolution. The as-prepared hydrogel was characterized by infrared spectroscopy (FTIR) and thermogravimetric analysis (TGA). The adsorbent had 1.688 mmol -COO− for each gram. These ionized sites bind Pb(II) ions, promoting their adsorption. The adsorption kinetic and equilibrium studies indicated that the Elovich and pseudo-second-order models adjusted well to the experimental data, respectively. The maximum removal capacities (qm) predicted by the Langmuir and Sips isotherms achieved 108.2 and 97.55 mg/g at 0.83 g/L adsorbent dosage (pH 4.0). The hydrogel/Pb(II) pair was characterized by scanning electron microscopy (SEM), X-ray dispersive energy (EDS), and differential scanning calorimetry (DSC). The chemisorption seems to play an essential role in the Pb(II) adsorption. Therefore, the adsorbent was not recovered, showing low potential for reusability.