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A setup combining a number of techniques (WAXS, XANES and UV–Vis) has been used to probe the stability of an iron molybdate catalyst during redox cycling. The catalyst was first reduced under anaerobic methanol/helium conditions, producing formaldehyde and then regenerated using air. Although in this test-case the catalyst and conditions differ from that of a commercial catalyst bed we demonstrate how such a setup can reveal new information on catalyst materials. In particular we observe the formation of two phases during reduction; one which we propose to be an oxygen deficient ‘pseudo-molybdate phase’, the other a molybdenum carbide-like phase, both produced as oxygen is removed from the catalyst. Standard in situ techniques could detect such transient phases, however, the information from multiple techniques, allows us to more accurately identify the nature of these materials and to carry out appropriate complementary ex situ measurements to aid in the analysis. This and similar setups therefore offer a way to more quickly and accurately observe reaction pathways within a catalyst, which may for example, result in the deactivation of the material by different routes to those observed previously. Additionally, the specific combination of these techniques with on-line mass spectrometry, allows us to monitor the activity of the catalyst surface and here observe that different catalytic mechanisms may occur during different stages of the redox process. Therefore this setup should allow for the observation of many novel variations in a catalyst’s reactivity, leading to the improvement of current and development of new materials.

A Combined Multi-Technique In Situ Approach Used to Probe the Stability of Iron Molybdate Catalysts During Redox Cycling