Optic microscopy, X-ray diffraction (XRD), Mö ssbauer spectroscopy (MS), Electron microprobe analysis (EPMA) and secondary ions mass spectroscopy (SIMS) were used to study Colombian auriferous soils. The auriferous samples, collected from El Diamante mine, located in Guachavez-Nariñ o (Colombia), were prepared by means of polished thin sections and polished sections for EPMA and SIMS. Petrography analysis was made using an optical microscope with a vision camera, registering the presence, in different percentages, of the following phases: pyrite, quartz, arsenopyrite, sphalerite, chalcopyrite and galena. By XRD analysis, the same phases were detected and their respective cell parameters calculated. By MS, the presence of two types of pyrite was detected and the hyperfine parameters are: d 1 = 0.280 T 0.01 mm/s and DQ 1 = 0.642 T 0.01 mm/s, d 2 = 0.379 T 0.01 mm/s and DQ 2 = 0.613 T 0.01 mm/s. For two of the samples MS detected also the arsenopyrite and chalcopyrite presence. The mean composition of the detected gold regions, established by EPMA, indicated 73% Au and 27% Ag (electrum type). Multiple regions of approximately 200 Â 200 mm of area in each mineral sample were analyzed by SIMS registering the presence of Binvisible gold^associated mainly with the pyrite and occasionally with the arsenopyrite. Key words invisible gold . Mö ssbauer spectroscopy . X-rays diffraction . secondary ions mass spectroscopy SIMS . pyrite . quartz . arsenopyrite Hyperfine Interact (2005) 166:605-611