The partition curve is an important tool to evaluate the separation performance of mineral separators like dense medium cyclones (DMCs). This curve is constructed by float-and-sink (FaS) analysis which involves the use of heavy liquids and suspensions. This traditional technique is hazardous to the environment, laborious, and time-consuming. Here, a new technique using X-ray computed tomography (XCT) scanning was successfully developed and applied for describing the partition curve of a DMC at an Australia-based lead–zinc mineral processing plant. The DMC feed, concentrate and reject streams were sampled and sieved into several size classes. The chemical assays and averaged densities according to each class were analysed by X-ray fluorescence spectrometry and gas pycnometry, respectively. The partition behaviour was investigated by XCT analysis. A model was proposed to determine the mass yield value – an important parameter to define partition curves – by mass balance and reconciliation, which is generally unknown during the sampling of continuous separation processes. From the reconstructed XCT images, we obtained detailed information on individual particles such as volume, surface area, mass, and density. Cumulative mass distribution curves and partition curves of the DMC for different size classes were then constructed and agreed with the FaS analysis. Using the XCT technology can help overcome the issues of the traditional FaS analysis. Moreover, this technology would allow for evaluating DMC separation efficiency with continuous, online, and real-time monitoring and control.