Langmuir, Vol.27, No.1, 187-195, 2011
Evaluations of the BET, I-Point, and alpha-Plot Procedures for the Routine Determination of External Specific Surface Areas of Highly Dispersed and Porous Silicas
Nitrogen adsorption isotherms of silicas and other oxidic materials are distorted by the presence of micropore adsorption and capillary condensation. This distortion affects the determination of the specific area of the material, depending on the chosen calculation procedure. Correction of the initial (total) isotherm for micropore capacity decreases or eliminates this source of error to give a useful estimate of the external surface area. In the present work, 26 silica-based adsorbent materials were studied to obtain total and external specific surface areas by the Brunauer-Emmett-Teller (BET), I-point, and a-plot procedures, using the micropore capacities from the alpha-plots to obtain the corrected (external) isotherms. Errors in the specific surface areas due to the presence of micropores are given by the equation Delta sA = 3.267 (m(2)/cm(3) STP) sV(mic), where sA is the specific surface area in m(2)/g and sV(mic) is the micropore capacity in cm(3) STP/g. A consistent set of conversion factors was obtained by which the external specific surface area obtained using one of these procedures can be converted, with part-per-thousand precision, to either of the others. Although the I-point procedure presents the advantage of not requiring a defined p/p(0) range, the alpha-plot procedure is recommended for routine determinations of external specific areas of silicas and other oxidic materials, except for cases in which the shapes of the adsorption isotherms of the sample and the reference differ significantly from one another in the p/p(0) range used for the determination.