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Nickel sulfide nanoparticle-loaded activated carbon (NiS-NP-AC) were synthesized as a novel adsorbent for simultaneous and rapid adsorption of Methylene blue (MB) and Safranin-O (SO), as most together compounds in wastewater. NiS-NP-AC was characterized using different techniques such as UV–visible, Fourier transform infrared spectroscopy (FTIR), energy-dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and Brunauer–Emmett–Teller (BET). The surface area of the adsorbent was found to be very high (1018 m²/g according BET). By using central composite design (CCD), the effects of variables such as pH, adsorbent dosage, MB concentration, SO concentration and contact time on binary dyes removal were examined and optimized values were found to be 8.1, 0.022 g, 17.8 mg/L, and 5 mg/L and 5.46 min, respectively. The very short …