We present an approach for the estimation of ore processing residue volumes in historical mine waste dumps by the use of different geophysical methods in combination with mineralogical investigations. The stamp mill dump in the Harz mountains, Germany was examined with the methods electrical resistivity tomography (ERT), ground penetrating radar (GPR) and spectral induced polarization (SIP) flanked by mineralogical studies at many drilling points. The mineralogical results were used to calibrate the geophysical results and to distinguish between valuable and non-valuable waste material. With SIP we investigated individual profiles and took lab samples. These lab results emphasize the differences between the fine-grained tailings of clayey silt to silty sand in the top layer and the sandy tailings underneath in both resistivity and phase. From the GPR results we can distinguish between different layers and various backfillings in the first two meters due to the much higher resolution than the other methods. From ERT we achieved an overview about the dimension and inner structure of the dump and the boundary between the sandy residual material and the host rock. To estimate the volume of the residual body we carried out 2D inversion of all ERT profiles followed interpolation between the inverted profiles. From the drilling interpretation, the SIP lab results and the ERT field measurements we defined a resistivity threshold of 350 ohm-m for the ore processing residues to achieve a 3-dimensional body of the dump. The volume of this body was then corrected by a factor due to consideration of uncertainties, e.g., forest areas, inaccessible dump sections, small-scale anomalies (geological or different anthropogenic nature) and inversion coverage. As a result, we were able to calculate the volume of the ore processing residues which can be used further for the determination of the economic potential (remaining metal content).