Skeletal iron catalysts were prepared by leaching Fe/Al intermetallics in large excess quantities of 6M aqueous NaOH at 10, 30 and 50°C. The precursor iron aluminides were produced by arc melting under a dry argon atmosphere and were comprised of the main phases FeAl, FeAl₂, Fe₂Al₅ and FeAl₃ along with intermediate compositions FeAl+FeAl₂, FeAl₂+Fe₂Al₅ and Fe₂Al₅+FeAl₃. It was shown that FeAl does not leach under these conditions, whereas all the other alloy samples leached to produce almost pure skeletal iron with BET surface areas in the range 14 - 71 m²g^-1. Kinetic modelling of hydrogen evolution curves of the iron aluminides showed that the Avrami-Erofeev nucleation-growth model (-ln(1-α)^1/n = kt) with exponents of either n = 1 or n = 1.5 was   able to fit the obtained data well. The apparent activation energies were in the range of 48.3-  57.4 kJmol^-1. Scanning electron microscopy images showed that the leached materials have a three-dimensional, porous nano-structure made from rods.