Even though the hydrometallurgical residue of non-ferrous metals contains small amounts of gold and silver, the residue has been landfilled due to low economic feasibility. Nowadays pyrometallurgical processes were developed to recover valuable metals from the residue, and, in these processes, gold and silver could be concentrated to an amount comparable to the content of gold or silver concentrates. In the pyrometallurgical process, impurities such as Fe, SiO2, and Ca are separated into slag, while Cu, Pb, Au, Ag are reduced to a metal phase and then recovered by specific gravity separation in the molten state at a high temperature. When separation efficiency is low, slag is mixed into the speiss, which causes many problems in the process. n this study, the slag mixed with the speiss obtained from the process was separated by conducting the specific gravity separation methods. In the case of the simulated sample experiment using the conventional Knelson concentrator, the separation efficiency decreased as the centrifugal force increased from 20% to 30%, and the possibility of specific gravity separation was confirmed. In the case of speiss mixed with slag, the separation efficiency was low at about 17%, indicating that it was difficult to separate specific gravity the materials. A newly designed Vibrating ball bed method using zirconia balls was investigated to separate the speiss and slag. As the number of particles increased, a particle interfere with the sinking of other particles. The separation efficiency increased to 100% at 22Hz (shaking power) with 3 limestones and 3 speiss, respectively.