In this work we report on methodologies and procedures to obtain the doping profile of semiconductor homo‐ and heterostructure devices with ultra‐abrupt doping transitions at or near the surface of a device or test structure using capacitance–voltage measurement techniques. Novel methods to obtain the complete carrier distribution (or ‘‘spike’’) of structures containing single of multiple planar (also known as delta) doped layers will be addressed. Techniques to measure the true doping profile of abrupt step and staircase doped structures will also be discussed. Extensive numerical models and methods have been developed to accurately extract doping and carrier concentration profiles of traditional and two‐dimensional electron (or hole) gas devices. The analysis and acquisition techniques which have been developed are applicable to all group IV and III–V compound semiconductor devices containingp‐nhomojunctions or heterojunctions, Schottky or Mott barriers, or MOS or MIS barriers. General limitations imposed by Debye screening and specific considerations related to quantum mechanical carrier confinement will be discussed. Strategies to confirm the abruptness of the impurity doping or alloy composition transitions will also be addressed.