The density evolution of HCN, NH3, H2O and CO molecules over time was monitored by laser absorption spectroscopy (LAS) in a low pressure DC pulsed discharge in N2-H2 gas mixtures with addition of CH4 or O2. The discharge was maintained in an industrial-scale, active screen plasma nitrocarburizing (ASPNC) reactor with a steel active screen (AS). The measured species densities were analysed using a simplified kinetic model that includes three characteristic times for chemical processes in the ASPNC reactor. The shortest time (1 to 4 min) was associated with the gas residence time in the reactor, the middle one (about 20 min) was assigned to surface reactions on the AS and workload, whereas the largest one (about 3 to 5 hours) was assigned to surface reactions on the cold reactor walls. The work highlights the importance of monitoring the gas composition during plasma nitrocarburizing processes in order to maintain defined treatment conditions and compensate for continuously changing chemical kinetics at the internal reactor surfaces.