Аннотация:A sulfur-functionalized silica xerogel (S – SiO2) was synthesized via a novel one-step precipitation method from sodium silicate by passing hydrogen sulfide gas and subsequently characterized to evaluate its potential for copper removal from aqueous media. The xerogel possesses a disordered mesoporous structure with a specific surface area of 19 m2/g and contains sodium and sulfur species incorporated into the silica matrix. The adsorption performance of S – SiO2 was assessed in Cu(II) solutions with initial concentrations ranging from 50 to 600 mg/L revealed a high adsorption capacity of 183 mg/g, consistent with the Langmuir isotherm model. The adsorption kinetics follow a pseudo-second-order model, indicating a chemisorption-controlled process. Thermodynamic parameters (𝛥G < 0, 𝛥H = 3.3 kJ∕mol, 𝛥S = 37.26 J∕mol ⋅ K) confirm that adsorption is spontaneous and endothermic. Nearly complete removal (≈ 99%) was achieved within 120 min at pH 4–6. Structural and spectroscopic analyses (HR-TEM, SAED, EDX, XPS, FTIR) reveal that Cu(II) removal proceeds via a combined mechanism involving surface complexation with silanol and sulfide groups and the formation of copper-containing phases, including CuS and CuO. The presence of residual sodium species in the unwashed xerogel promotes precipitation processes and enhances adsorption efficiency. These results demonstrate that the inorganically sulfur-modified silica xerogel is an efficient and low-cost material for copper removal, highlighting the potential of simple inorganic functionalization strategies for designing advanced adsorbents.