Photogrammetric three-dimensional (3D) reconstruction is an image processing technique used to develop digital 3D models from a series of two-dimensional images. This technique is commonly applied to optical photography though it can also be applied to microscopic imaging techniques such as scanning electron microscopy (SEM). The authors propose a method for the application of photogrammetry techniques to SEM micrographs in order to develop 3D models suitable for volumetric analysis. SEM operating parameters for image acquisition are explored and the relative effects discussed. This study considered a variety of microscopic samples, differing in size, geometry and composition, and found that optimal operating parameters vary with sample geometry. Evaluation of reconstructed 3D models suggests that the quality of the models strongly determines the accuracy of the volumetric measurements obtainable. In particular, they report on volumetric results achieved from a laser ablation pit and discuss considerations for data acquisition routines.