The factorial experimental design technique has been used to investigate the adsorption of Bismarck Brown-Y (BBY) from wastewater onto agricultural waste Areca Husk Carbon Fibre (AHCF). The Factorial Design (23) is adopted for optimizing variable parameters from these studies. The interaction between three process parameters for the adsorption of dye is optimized. Batch mode of experiments is carried out for the adsorption studies. The adsorption parameters pH, temperature and particle size of the adsorption capacity are analysed and optimized as pH 4-9, particle size 100-250 BSS and temperature 300-320 K. The statistical tools t-test, ANOVA, F-test are tested to verify the fitness of adsorption and the results are validated by this design of experimental model. All these values revealed with the normal probability plots, main & interaction plots, Pareto charts and contour plots. The regression values are evolved with Design of Experiment software and prove the fitness on experimental data. Physico-Chemical characteristics and adsorption efficiency of AHCF of the wastewater are also determined and the results revealed AHCF is a good adsorbent. The structural and morphological features of activated carbon are characterized by FTIR, XRD, SEM and EDAX studies.