Nitrogen depth profile of plasma nitrided pure iron was measured and evaluated by accurate experimental techniques. Plasma nitriding cycles were carried out on high purity iron substrate in an atmosphere of 75% H 2 –25% N 2 . Nitrogen concentration depth profiles in the compound layer and the diffusion zone were characterized by glow discharge optical emission spectroscopy (GDOES) and secondary ion mass spectroscopy (SIMS), respectively. Nitrogen diffusion depths were measured accurately by optical and scanning electron microscopy as well as SIMS technique at different nitriding times. Experimental results indicated good agreement between SIMS data and microscopic evaluations for various nitriding cycles. The results of SIMS showed the nitrogen diffusion depth of about 2000μm in the diffusion zone for 10h plasma nitriding at 550°C. Such high depth had not been detected in previous investigations in which the conventional methods such as EDS, GDS, XPS, EPMA or ion probe techniques were used.