The Gibbsian Surface Excesses (GSE) are the true experimental variables for
measurement of equilibria and kinetics for pure and multicomponent gas-sol
id adsorption. The gravimetric and volumetric methods, which are the most c
ommonly used experimental procedures, are revisited. The common practice of
ignoring helium adsorption during measurement of adsorbent density by heli
um pycnometry and measurement of void volumes in adsorption apparatus by he
lium expansion can lead to large errors in estimating GSE at high pressures
and for less selectivity adsorbed components of a gas mixture. Methods to
overcome these problems are described.