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Mechanical alloying processes are carried out usually with addition of some lubricants, referred to also as a process control agents (PCA). About 1-2 wt% of a PCA (usually stearic acid) is normally added to prevent excessive cold welding amongst the powder particles, especially when powders of ductile metals are milled. However, lubricants (maybe disintegrated after MA process) must be removed in the early stages of heating during the sintering process. The aim of the present study was to determine the effect of the MA process especially (i) milling time and (ii) influence of lubricant addition on thermal effects during heating of iron powder (Astaloy CrM) with the addition of 1 wt% stearic acid measured by differential scanning calorimeter (DSC) and thermogravimetry (TG) techniques. Removal of the lubricants during heating of the blended powders and exhaust gases from the furnace were monitored by quadruple mass spectrometry (QMS). Determination of the physical and technological properties of the powder mixture obtained from MA was performed with a laser particle sizer. Distribution of particle sizes, flow and apparent density were also measured. Furthermore, the shape and morphology of the powders were characterised by a light optical microscope (LOM) and scanning electron microscope (SEM).