Metal-containing aluminophosphate molecular sieves (MeAPOs) were observed to exhibit remarkable catalytic activity in partial oxidation of hydrocarbons under mild condition. in this paper we review the spectroscopic characterization of framework incorporation and redox behavior of vanadium and cobalt in MeAPOs. EXAFS/XANES and XPS studies of the oxidation state and coordination of V and Co in as-prepared MeAPOs and after odor treatments will also be presented. These studies show that fourfold coordinated Co2+ Of CoAPO-11 was only partially oxidized to Co3+, while grafted V4+ Of VAPO-5 was almost completely oxidized to V5+ after calcination. All Co and V species remain in the AlPO4 framework during redox treatments.