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This research is focused on the ultrasound-assisted removal of Auramine-O (AO) dye from aqueous solutions using ZnS:Cu nanoparticles loaded on activated carbon (ZnS:Cu-NP-AC) as an adsorbent. ZnS:Cu nanoparticles were synthesized and characterized using FESEM (Field-Emission Scanning Electron Microscopy) and XRD (X-Ray Diffraction) analysis. The experiments were designed by response surface methodology. A quadratic model was used to predict the variables. Analysis of variance was used for investigation of variables and interaction between them. High F-value (48.91), very low P-value (<0.00001), non-significant lack of fit, and the determination coefficient (R2 = 0.977) demonstrate good correlation between experimental and predicted values of the response. The highest removal percent attained was 99.76%, and the optimum parameters achieved are: adsorbent amount (0.02 g), initial dye …