Both H3PO4 activation procedures develop activated carbons having suitable activation yields and porosity developments, giving the Activation after Incipient Wetness Impregnation method better results than the Activation after Hydrothermal Impregnation. Both natural bio-fibers are good precursors, rendering the coconut fiber matting better results than the banana pseudostem. The variables studied affect the porosity development, being precursor and H3PO4/precursor ratio the variables that most affect. By a suitable selection of these variables, activated carbons having high adsorption capacities (BET above 2500 m2 g鈭? and micropore volume above 1.00 cm3 g鈭?) and well developed mesoporosity (reaching 1.41 cm3 g鈭?), can be prepared. Most of the samples prepared perform very well for adsorbing gasoline vapors, showing a linear relationship with their resulting volumes.