The fluorescence EXAFS (FLEXAFS) technique has been combined with an in sit
u cell and on-line gas analysis. For this purpose a seven-element silicon d
rift detector has been used, which has high count rate capabilities and can
be operated at room temperature. The potential of this technique is shown
by the study of the state of copper promoter atoms in Fe-Cr based high temp
erature shift (HTS) catalysts. The FLEXAFS measurements revealed that Cu (0
.17 - 1.5 wt%) is present in the metallic state under working conditions of
the catalysts but easily re-oxidizes upon air exposure. The reduction beha
viour of copper depends strongly on the copper concentration and the pre-tr
eatment, i.e. if the catalysts have been calcined or used in the HTS reacti
on. For used catalysts, a Cu(I) phase was detected as intermediate during r
eduction. Its stability was especially high at low copper concentration.