Abstract: A method is provided for measuring at resolutions which are in some instances less than 20 nanometers the concentration densities within one or more diffusion regions within a semiconductor substrate. The diffusion regions are prepared for measurement by cleaving a cross-sectional surface and polishing that surface to a substantially flat, exposed profile. The profile is purposefully pre-etched to remove oxide abutting the implant area and thereafter dopant-selective etched in accordance with concentration densities within the substrate. Pre-etching of oxide and concentration density etching of doped silicon provides an exposed topological contour measurable by atomic force microscopy (AFM). AFM can detect the entire cross-sectional surface including conductors and dielectrics. The topological height of impurity region profiles of a calibration wafer are correlated to impurity concentrations to form a calibration curve.