A systematic study has been described on the laser diffraction (LD) and static image analysis (SIA) of rectangular particles [1]. To rule out powder sampling, sample dispersion and particle orientation as a possible root cause for differences in size distribution profile, powder samples were initially immobilized by means of a dry disperser onto a glass plate. For a defined region of the glass plate the diffraction pattern as induced by the dispersed particles, and the 2D dimensions of the individual particles were measured by LD and optical microscopy, respectively. Correlation between LD and SIA could be demonstrated considering the scattering intensity of the individual particles as the most dominating factor. For both spherical and rectangular particles, theory explains the latter to relate to the square of their projected area. In traditional LD, the size distribution profile is dominated by the maximum projected area of the particles (A), and the diffraction diameters of a rectangular particle with length L and breadth B are perceived by the LD instrument to correspond by approximation with spheres having a diameter of ∅ L and ∅ B , respectively. Weighting for differences in scattering intensity between spherical and Page 3 of 56 rectangular particles exlains each rectangular particle to contribute to the overall LD volume probability distribution proportional to A 2 /L and A 2 /B. Accordingly, for rectangular particles this scattering intensity weighted diffraction diameter (SIWDD) concept explains an overestimation of their shortest dimension and an underestimation of their longest dimension. For this study various samples have been analysed with the longest dimension of the particles ranging from ca. 10 to 1000 µm. For a variety of pharmaceutical powders all with a different rectangular particle size and shape, the demonstrated correlation between LD and SIA aims to facilitate the user in a better validation of LD methods based on SIA data.