Ten types of 13 wt% MoO3/Al2O3 catalysts were prepared by a conventional impregnation or equilibrium adsorption method using a common extrudate support. These catalysts were subjected to a comprehensive characterization and catalytic reactions to find important preparation parameters in practical preparations. It was demonstrated in the present group study that the formation of crystalline MoO3 was strongly correlated with the Mo segregation on the outer surface of the extrudate. When the amount of the impregnation solution was large (ca. 10 cm(3) g-Al2O3-1), a considerably homogeneous distribution and high dispersion of Mo oxide species were attained irrespective of the other preparation parameters. It is suggested that when a pore volume impregnation or incipient wetness technique is employed, drying processes strongly affect the dispersion and distribution of Mo oxide species. Drying at a reduced pressure is suggested to result in a segregation of Mo oxides on the outer surface of the extrudate, and accordingly a formation of crystalline MoO3.