An experimental heat treatment chamber and control system were developed to perform in-situ X-ray diffraction experiments during low-pressure carburizing (LPC) processes. Results from the experimental chamber and industrial furnace were compared, and it was proven that the built system is reliable for LPC experiments. In-situ X-ray diffraction investigations during LPC treatment were conducted at the German Electron Synchrotron Facility in Hamburg Germany. During the boost steps, carbon accumulation and carbide formation was observed at the surface. These accumulation and carbide formation decelerated the further carbon diffusion from atmosphere to the sample. In the early minutes of the diffusion steps, it is observed that cementite content continue to increase although there is no presence of gas. This effect is attributed to the high carbon accumulation at the surface during boost steps which acts as a carbon supply. During quenching, martensite at higher temperature had a lower c/a ratio than later formed ones. This difference is credited to the early transformation of austenite regions having lower carbon content. Also, it was noticed that the final carbon content dissolved in martensite reduced compared to carbon in austenite before quenching. ... mehrThis reduction was attributed to the auto-tempering effect.