Abstract: By a QDTA/T/EGA/GC on line coupled simultaneous device, a fast micro-methodfor screening how the calcination conditions of a catalyst would affect its activity andselectivity has been established. The caralyst Co-Fe-Bi-Mo-A-B-C-O for the oxidationof dilute propylene to acrolein was used. Experimental results indicated that in the com-plex selective catalytic oxidation reaction the DTA peak does not always correspond tothe conversion rate. Accordingly, DTA peak can not be used directly as a criterion toscreen the activity of carelysts. By intercepting the gas evolved during the reaction andanalyzing it with GC, the corresponding relationship between the activity and the selec-tivity of catalysts can thus be established from the DTA peak and the peak area of theacrolein. The optimal calcination conditions obtained were confirmed by experimentalresults.