The shape of gold is widely used in mineral exploration and in sedimentology to estimate the distance of transport from the source to the site of deposition. However, estimation of the morphology is based on qualitative observations or on the quantification of shape in 2D. The 3D analysis of grain shape is useful for accurate morphometric quantification and to evaluate its volume, which is related to particle size. This study compares X-ray 3D microscope and 3D SEM photogrammetry to reconstruct the shape of gold particles. These new methods are exploited to quantify the shape of gold grains 85 to 300 μm in size. The shape parameters, such as axial lengths, surface area, volume, diameter of curvature of all corners, and diameter of the largest inscribed sphere and smallest circumscribed sphere are measured on a particle in order to estimate shape factors such as flatness ratios, shape indices, sphericity, and roundness. Most shape parameters and shape factors estimated on the same gold grain with simple geometry are similar between the two approaches. This result validates these methods for the 3D description of gold particles with simple morphology, while providing a methodology for describing grains with more complex geometry.