A QEXAFS (quick-scanning EXAFS) technique has been devised to follow t
he local atomic coordination changes about selected reactants in a cla
ss of highly exothermic solid combustion reactions. Real-time EXAFS me
asurements during the combustion were made in the time frame of a few
seconds. By tuning the monochromator to a specific energy, at which ma
ximum changes occur in an EXAFS feature of an element transforming fro
m the reactant to the product phase, a time resolution of 20 ms was ac
hieved. The Ni + Al -> NiAl reaction has been investigated in some det
ail in light of a possible intermediate phase in the so-called after-b
urn region. The present QEXAFS findings together with the recent time-
resolved diffraction data on the same system lends, for the first time
, experimental insights into the structural macrokinetics of this clas
s of combustion systems.