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In recent years, high demands for Se and Te in the solar panels and semiconductors industry have encouraged its extraction from primary and secondary sources. However, the two elements’ similar chemical and physical properties make pure element production, Se or Te, arduous. This work is aimed to investigate the significant factors of Se and/or Te recovery in the copper cementation process using the response surface methodology. The test was carried out in two series, for Te and Se, so that H₂SO₄, CuSO₄, Te(or Se) concentration, and temperature are the factors of experimentation. According to response surface methodology (RSM) results for both test series (i. e. Se and Te), 50 g/L H₂SO₄, 15 g/L Cu, and 35 °C, 3000 mg/L Se (or 750 mg/L Te) was specified for higher Se recovery (97%), and the lowest Te extraction (2%) as an optimum condition, so that could make a suitable separation process. Hence, the cementation test was conducted in the simultaneous presence of Se and Te, so the separation index became 5291. Moreover, the cementation test was carried out in the pregnant leach solution of copper anode slime, and the separation factor was measured to be 606. On the other hand, the thermodynamic evaluation and XRD patterns of the process’s sediments confirm that Se is precipitated as Cu₂Se and Cu_1.8Se, whereas no Te components are detected in the sediments.