Cyclic temperature-programmed reduction (TPR) and reoxidation (TPO) experiments can mimic the redox mechanism suggested by Mars and van Krevelen when using a hydrocarbon as reductant. The redox cycles enable fast probing of the activity and selectivity of multi-component oxide catalysts applied in the selective oxidation of short hydrocarbons. The technique was applied to quantitatively assess the redox properties of active bismuth molybdates and inactive bismuth tungstates (Bi2MxO3x+3, M = Mo, W), which are components of industrial acrolein synthesis catalysts. The specific reducibility of the supporting complex oxide Fe3Co7Mo12O46 is found to be low due to its comparably high surface area.