Glow‐discharge mass spectrometry, in which an rf glow discharge is used both to sputter etch the sample undergoing analysis and to ionize the neutral sputtered species, is shown to be a promising new technique for the elemental analysis of thin solid layers or bulk solids. A description of the method is given followed by some examples of its application to composition profiling. The influence of some parameters is shown and opinions as to the advantages and disadvantages of the method are given.