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Response surface methodology (RSM) based on central rotatable experimental design was used to investigate the effect of ultrasound assisted simultaneous adsorption process variables on Cu: ZnS-NPs-AC from aqueous solution. Cu: ZnS-NPs-AC was characterized using field emission scanning electron microscopy (FE-SEM), Energy Dispersive X-ray Spectroscopy (EDX) and X-ray diffraction (XRD). To overcome the severe methylene blue (MB) and brilliant green (BG) dyes spectral overlapping, derivative spectrophotometric method were successfully applied for the simultaneous determination of dyes in their binary solutions. Simultaneous determination of the dyes can be carried out using the first-order and second order derivative signal at 664 and 663 nm for BG and MB, respectively. The factors investigated were pH (2.5–8.5), adsorbent mass (0.006–0.030 g), sonication time (1–5 min) and initial MB and BG …