Aluminium diffusion coatings are often prepared by using a pack aluminization technique, which is a specific variety of the CVD method. The coating process takes place in a bed containing a master alloy (MA) that serves as a source of the coating forming element (CFE). The phase composition of the diffusion layer obtained depends on the activity of the CFE during the pack aluminization processing. One of the methods to control the activity is a variation in the chemical composition of the MA. In this method the MA of the needed CFE concentration is also prepared by using the pack aluminization technique. So the pack aluminization technique is used twice during the processing cycle: once for MA preparation and once for coating. The method was applied to coating of iron with a layer of FeAl.