The interstitial filling, grinding media and feed particle size are vital parameters to be considered during ball mill operation. Experiments were conducted to ascertain whether there are possible interactions between the three variables and the fineness of the required product. The data obtained was analysed using the Attainable Region (AR) optimization method which is a model-free and equipment-independent tool. Experimental results indicate that there is a need to adjust or correlate powder filling with grinding media and feed particle size. It is of paramount importance to find optimal operational parameters for these variables during ball mill operations. The AR technique helps identify opportunities to save engineers significant time, reduce operation costs and consequently allow them to get closer to the objective of optimum plant operation that would result in achieving product requirements.