Advances in instrumentation and the parallel development of proper analytical methodologies have fuelled an extraordinary growth of analytical applications with glow discharge (GD) techniques. In fact, GDs with detection by optical emission spectrometry (OES) and mass spectrometry (MS) have become today, fast, comparatively simple, and reliable tools for materials analytical characterization at the nanoscale. A critical description of latest advances and presently available GD-OES and GD-MS instrumentation (commercial, prototype and laboratory equipments) is carried out here. Analytical strategies developed for the analysis at the surface and for concentration depth profile analysis of thin and ultrathin layers with GDs are also discussed. Finally, selected representative applications and trends of GD-OES and GD-MS techniques for the nanometer range analysis (e.g. nanolayers, two-dimension nanostructured materials and molecular depth profiling of polymer-based coatings) are briefly described, confirming the increasing analytical value of GD-OES and GD-MS techniques in the nanotechnology field.
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