BET–SURFACE AREA ANALYSIS

2.1 INTRODUCTION
Specific surface area of the samples was determined with the classic BET
method (the Brunauer–Emmett–Teller isotherm). The BET isotherm is the basis for
determining the extent of nitrogen adsorption on a given surface.

2.2 PRINCIPLE
Representative samples were pre-dried at room temperature (22±1 °C) in a
vacuum desiccator and degassed at 90 °C for 1 h and then at 200 °C for 4 h. The iron
sample was contained within a glass sample tube cooled to cryogenic
temperature, then exposed to nitrogen gas at a series of precisely controlled
pressures. With each incremental pressure increase, the number of nitrogen
molecules on the surface increased. The pressure at which adsorption equilibrium
occurs was measured and the universal gas law was applied to determine the
quantity of gas molecules adsorbed. As adsorption proceeded, the thickness of the
adsorbed nitrogen film increased with surface microspores being filled before
macrospores. The process continued until the point of bulk condensation of the nitrogen
and then the reverse sequence of desorption occurred. The systematic sorption and
desorption of nitrogen provided the fundamental information on the surface
characteristics the total surface area.