Pt/Mg/Al metal oxide catalysts were prepared by impregnation and co-precipitation methods, respectively. These samples were characterized by BET, XRD and NO-TPD; their NOX storage property and adsorbing intermediate species were investigated with NSC and FTIR. The results showed that the prepared methods exert significant influence on the physical structure properties and the adsorption abilities of NO. (Pt)/Mg/Al samples prepared by impregnation (IM) have larger specific areas and higher NO (X) storage capacity than (Pt)/Mg/Al catalysts prepared by co-precipitation (CP). The intermediate species of NO adsorbing process indicated that NO was firstly adsorbed as bridged nitrites both on Pt/Mg/Al (IM) and on Pt/Mg/Al (CP), then on Pt/Mg/Al (IM) the nitrites transferred into monodentate and bidentate nitrate species while on Pt/Mg/Al (CP) the nitrites only transferred into monodentate nitrate species.