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Present work is focused on the preparation of mustard stalk activated carbon (MSAC) using chemical activation with H3PO4 and exploring its properties for its use in dye removal from wastewater. Adsorption variable (dosage, contact time, and solution pH), pore structure, morphology, surface functional groups, equilibrium kinetics, and isotherm study for removal of methylene blue (MB) using MSAC were investigated. The present study showed that an adsorption dosage of 0.2 g L-1 and pH 8 can be considered as optimum for the MB removal. SEM result showed that pore of MSAC was larger than the pore of the mustard stalk (MS). BET surface area and total pore volume of MSAC were found as 510 m2 g-1 and 0.33 cm3 g-1, respectively. Equilibrium adsorption data were examined by Langmuir and Freundlich isotherm models. Better correspondence to the Langmuir model with a maximum adsorption capacity of 212.76 mg g-1 (MB onto MSAC) was obtained. Dimensionless factor, RL revealed favourable nature of the sorption in the MSAC - MB system. Adsorption rates were found to conform to the pseudo-second-order kinetics with good correlation. These results show that the MSAC could be used as a renewable and economical alternative to commercial AC in the removal of MB dye from wastewater.