Both environmentalists and archaeologists are interested in the detection and quantification of the remains of mine slag heaps from ancient smelters: possible pollution of the slag heaps and information concerning the history of the smelter's mine. Although magnetic surveys can be used to detect subsurface slag accumulations, it is not possible to derive the total amount of material from such surveys or to accurately delineate the heaps through the use of this method. Conversely, ‘Induced Polarization’ (IP) surveying allows a relevant and robust assessment of the volume of slag concentrations to be determined. In the present study, we follow up on results obtained in a previous study, carried out at the 14 th Castel‐Minier mine (Ariège, France) site, where we have shown that the chargeability is proportional to the slag concentration in the ground and have used this property to perform 3D tomography of the heap. Based on a previous investigation using spectral induced polarization along a simple profile showing that the phase peak related to the slags is situated at approximately 1 Hz, in the present paper we extend our prospection to 3D by using a Terrameter SAS1000 and measuring temporal chargeability. The set of three‐dimensional data is recorded by means of classical transect measurements along parallel close profiles and is then interpreted using the RES3DINV code. Finally, archaeological and auger soundings confirmed the assessments derived from this geophysical investigation. We also briefly discuss the source of the IP signal, which we suspect to be induced by magnetite particles embedded in the slags.