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The purpose of the current study was to examine the potential of raw and calcined alluvium, prepared from water streams in agricultural land, as a novel adsorbent for removing methylene blue (MB) and methyl violet (MV) from the aqueous media. Central composite design (CCD) was used to optimize the adsorption process as well as the interaction between parameters (adsorbent dose, initial pH, ultrasonic time and initial dye concentration). The physicochemical properties and surface changes of raw and calcined alluvium were investigated using scanning and transmission electron microscopy (SEM and TEM), X-ray diffraction (XRD), Brunauer–Emmett–Teller (BET), and Fourier transform infrared spectroscopy (FTIR). The BET surface and pore diameter of the calcined alluvium was obtained 68.13 m²/g and 16.58 nm, respectively. Langmuir, Freundlich, and Tamkin equations were used to model the adsorption …