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Morphological characterization and quantification of gold particles by optical image analysis (OIA) and by compositional analysis of microprobes using scanning electron microscope and electron microprobe analysis techniques were carried out on gold grains from the Minvoul area (Archean greenstone belt in Gabon). Large grains of almost pure gold were found throughout a weathering profile, which consisted of saprolite, mottled clay zone, iron duricrust, pisolitic gravels and yellow latosol. In the deeper horizons, gold was dissolved as shown by corrosion features on the surface of particles with average sizes of 2.6Φ and 2.35Φ in the saprolite and mottled clay zones, respectively. The occurrence of secondary gold in the duricrust was indicated by the larger size of the nuggets (average, 1.8Φ), the high fineness (> 995 in average) and the close textural relationship between gold and neoformed iron oxyhydroxides. The uppermost horizons composed of yellow latosol and pisolitic gravels were interpreted as transported materials based on their size distribution (average 0.85Φ and 1.34Φ), sorting and shape parameters. The best morphological parameter to describe the whole weathering profile was found to be the perimeter/area ratio. The highest ratios were recorded in the saprolite (average 0.192 μm−1), and decreased towards the surface (average 0.057 μm−1). The combination of the OIA technique and the microchemical analysis of gold grains allowed us to define specific morphological and compositional characteristics of the gold particles for each horizon. Both methods proved to be of great utility to understand gold concentration, dissolution and dispersion processes in supergene environments.