The development and application of glow discharge (GD) devices and associated spectroscopy for chemical analysis began as early as the 1930s and 1940s. However, it is since the 1960s and 1970s that Glow Discharge (GD) became a major focus of research in many analytical chemistry laboratories. The research work has been directed towards glow discharge source development and the fundamental study of the physical characteristics of the analytical glow discharge, and towards the development and application of glow discharge spectroscopic techniques for various analytical applications ranging from plasma etching and deposition systems in the micro-electronics industry to lasers or even plasma monitors. Hence, GD devices have become well-known for their ability to directly analyse solid material. More precisely, GD devices have been used for more than bulk analysis and are proving to be diverse tools for the in-depth analysis of layered materials.