The sol-gel method is applied to prepare Cu+ or Ag+ containing alumina adsorbents which have potential application in purification or separation of carbon monoxide or olefins containing gases. Wet impregnation and sol-solution mixing methods are used to incorporate the active species into the sol-gel derived gamma-alumina support. These alumina adsorbents have the characteristics of large specific surface area, high dispersion of active species on the grain surface, and mesopore size with a uniform pore size distribution. The gas chromatographic technique determines the carbon monoxide adsorption properties on these alumina adsorbents. Adsorption equilibrium constants, adsorption rate constants, axial dispersion coefficients, heat of adsorption, and adsorption activation energy are determined from GC response peaks by using the moment method The alumina adsorbents prepared by the sol-gel method appear to be superior to the similar adsorbents prepared by other methods.