Coarse comminution test-work and modeling are powerful tools in the design and optimization of mineral processing plants and provide information on energy consumption. Additional information on mineral liberation characteristics can be used for assessing the potential of pre-concentration stages or screens in the plant design. In ores of high-value metals (e.g., Ta, W), standard techniques—such as the mineralogical quantification of grain mounts by quantitative evaluation of minerals by scanning electron microscopy (QEMSCAN) or chemical analysis by X-ray fluorescence (XRF) can be challenging, due to the low relative abundance of such valuable minerals. The cost of QEMSCAN is also a limiting factor, especially considering the large number of samples required for the optimization of coarse comminution. In this study, we present an extended analytical protocol to a well-established mechanical test of interparticle breakage to improve the assessment of coarse mineral liberation characteristics. The liberation of ore minerals is a function of the rock texture and the difference in size and mechanical properties of the valuable minerals relative to gangue minerals and they may fraction in certain grain sizes if they behave differently during comminution. By analyzing the bulk-chemistry of the different grain size fractions produced after compressional testing, and by generating element by size diagrams, it is possible to understand the liberation characteristics of an ore. We show, based on a case study performed on a tantalum ore deposit, that element distribution can be used to study the influence of mechanical parameters on mineral liberation. This information can direct further mineralogical investigation and test work