The production of activated carbon from coconut shell treated with phosphoric acid (H3PO4) was optimized using the response surface methodology (RSM). Fifteen combinations of the three variables namely; impregnation ratio (1, 1.5, and 2); activation time (10, 20, and 30 min); and activation temperature (400, 450, and 500 °C) were optimized based on the responses evaluated (yield, bulk density, average pore diameter, small pore diameter, and number of pores in a unit area). Pore diameters were directly measured from scanning electron microscope (SEM) images. Individual second-order response surface models were developed and contour plots were generated for the optimization analysis. The optimum range identified for impregnation ratio was from 1.345 to 2, while for the activation time was from 14.9 to 23.9 min. For the activation temperature it was from 394 to 416 °C. The optimum points are 1.725, 19.5 min, and 416 °C, respectively. The models were able to predict well the values of the responses when the optimum variable parameters were validated as proven by the generally acceptable values of the residual percentages. Direct characterization of the pores using the SEM was found to be a good technique to actually see the pores and get actual measurements. Additionally, RSM has also proven to be a good tool in optimization analysis to get not only optimum production condition points but ranges, which are crucial for the flexibility of the production process, as well.