In this study Fenton's oxidation of dicamba in aqueous medium was investigated by using the response surface methodology. dosage of 11.38 and 0.33 mM respectively. The whole oxidation process was monitored by high performance liquid chromatography (HPLC) along with liquid chromatography/mass spectrometry (LC/MS). It was found that 82% of dicamba was mineralized to oxalic acid, chloride ion, CO 2 and H 2 O, which was confirmed with COD removal of 81.53%. The regression analysis was performed, in which standard deviation (\4%), coefficient of variation (\8), F value (Fisher's Test) ([2.74), coefficient of correlation (R 2 = R 2 adj ) and adequate precision ([12) were in good agreement with model values. Finally, the treatment process was validated by performing the additional experiments.