A fast-flow reactor technique is described by which Fe atoms can be produced in the gas phase in the afterglow of microwave-induced plasmas in hydrogen/argon and hydrogen/helium mixtures. When the iron salt FeCl3(s) was brought into the gas phase by thermal sublimation at temperatures between 360 and 405 K, it was partly converted to Fe atoms by reaction of the gaseous compounds FexCl3x(g) with hydrogen atoms. The Fe atoms were detected by atomic absorption spectroscopy (AAS). It was shown that sublimation of the salt is the rate-determining step of the overall plasma-afterglow atomisation process. Experimental conditions for the generation of Fe atoms suited to kinetic studies start at a temperature of 303 K. In the downstream region the concentration of Fe atoms decays due to diffusion to the reactor wall. Binary diffusion coefficients D-Fe/Ar and D-Fe/He of 231.5+/-6.6 and 370.0+/-15.5 cm(2) s(-1) Torr at 303 K, respectively, were determined.