Fast transient infrared studies in material science: development of a novel low dead-volume, high temperature DRIFTS...

A prototype DRIFTS flow reaction chamber was designed and developed in order to find analytical application in the study of heterogeneous catalysts operating at high temperatures under fast transient gas feed conditions. Minimisation of dead-volumes allows gas replacement in 8-10s at 10mLmin(-1) total flow. To overcome problems related to the reactivity of the cell walls under alternating oxidizing/reducing gases, the cell was built with Inconel 600trade mark, which was tested to be very inert even at high temperatures. The sample holder, which was developed to closely resemble a micro plug-flow reactor, poses some problems in terms of heat transfer to the outer body of the cell (limiting then the maximum reachable temperature) and of the correct measurement of the actual sample temperature. These problems were solved with a careful re-design of the upper part of the cell. The second prototype thus derived is able to reach temperatures up to 803K and allows gas replacement in less than 4s at 10mLmin(-1). The cell is inserted in a MCT-FT-IR, which allows to collect high quality spectra with a 1s time-resolution. The downstream flow can be analysed by a quadrupole mass spectrometer equipped with an enclosed source and by a commercial GC. The performances of this prototype cell are presented showing some tests carried out with ceria-zirconia (Ce(x)Zr(1-x)O(2)) catalysts for CO abatement under real operando conditions.