Process gas control for plasma (ion) nitriding is a matter of estimating the flows necessary to accomplish the required surface metallurgy. This chapter reviews several studies aimed at better understanding process gas control in plasma nitriding and its influence on compound zone formation. Emphasis is placed on the effect of sputtering on the kinetics of compound zone formation. The discussion covers the processes involved in process gas control analysis by photo spectrometry and mass spectrometry and the difficulties associated with gas analysis.