This study reports on the impregnation of bi-metallic adsorbents based on commercial coconut activated carbon (CAC), surface-modified with metal acetate (ZnAc2), metal oxide (ZnO and TiO2), and the basic compound potassium hydroxide (KOH). The morphology of the adsorbents was then characterized with SEM-EDX, the microporosity was determined using Brunauer–Emmett–Teller (BET) analysis, the thermal stability was investigated via thermogravity analysis (TGA), and functional group analysis was undertaken with Fourier-transform infrared (FTIR) spectroscopy. These modified adsorbents were subjected to a real adsorption test for H2S capture using a 1 L adsorber with 5000 ppm H2S balanced for N2, with temperature and pressure maintained at an ambient condition. Adsorption–desorption was carried out in three cycles with the blower temperature varied from 50 °C to 150 °C as the desorption condition. Characterization results revealed that the impregnated solution homogeneously covered the adsorbent surface, effecting the morphology and properties. Based on this study, it was found that ZnAc2/TiO2/CAC_DCM showed a significant increase in adsorption capacity with the different temperatures applied for the desorption in the second cycle: 1.67 mg H2S/g at 50 °C, 1.84 mg H2S/g at 100 °C, and 1.96 mg H2S/g at 150 °C. ZnAc2/ZnO/CAC_DCM seemed to produce the lowest percentage of degradation in the three cycles for all the temperatures used in the adsorption–desorption process. Therefore, ZnAc2/ZnO/CAC_DCM has the potential to be used and commercialized for biogas purification for H2S removal.