The Penouta Sn-Ta deposit, in the northwest of Spain, is a greisenized granitic cupola where Ta minerals occur mainly as disseminations in a leucogranite body intruded in Precambrian–Lower Cambrian gneisses and mica-schists. This leucogranite is a medium- to fine-grained inequigranular rock consisting mainly of quartz, albite, K-feldspar and muscovite. Accessory minerals are mainly of spessartine, zircon, cassiterite, Nb-Ta oxides, monazite, xenotime, native bismuth and pyrite. The alteration processes were mainly albitization, muscovitization and kaolinitization.This leucogranite is peraluminous and P-poor, with 0.03–0.07 wt.% P₂O₅, 900–1500 ppm Rb, 30–65 ppm Cs, 120–533 ppm Li, 80–140 ppm Ta, 51–81 ppm Nb and up to 569 ppm of Sn.Mineralogical characterization of Nb-Ta oxide minerals was determined by X-ray diffraction, scanning electron microscopy, electron microprobe analysis and mineral liberation analysis. Mn-rich members of the columbite-group minerals (CGM) are the most common Ta-bearing phases, but microlite, wodginite, tapiolite and Ta-rich cassiterite occur also. CGM crystals are commonly zoned concentrically, with a Nb-rich core surrounded by a Ta-rich rim, with a sharp boundary between them. Convoluted zoning occurs also. Dissolution textures resulting from the corrosion of columbite and tantalite rims, in particular, are common. The Mn/(Mn + Fe) ratio varies between 0.33 and 0.97 and the Ta/(Ta + Nb) ratio between 0.07 and 0.93. Wodginite and microlite formed as late replacements of CGM and occur associated with tantalite and cassiterite. Subhedral to anhedral cassiterite crystals, usually up to 200 μm across, occur in two generations: the earlier one is Nb,Ta-poor whereas in the later generation, the Ta content can reach >9 wt.% of Ta₂O₅and 1.7 wt.% of Nb. The presence of a fluid phase in the apical zone of the granite, probably related to the separation of a fluid/vapour of the melt, could explain the sponge-like textures, the Ta enrichment associated with these textures, the occurrence of Ta-enriched mineral phases (microlite and wodginite) and their common interstitial character.

The modelling of high pressure grinding rolls is described by the population balance model, a mass balance which includes several functions that are related to the mineral characteristics, material kinetics and operative conditions of the device. The breakage distribution function is one of these functions and refers to the way in which the daughter particles are generated by the process of comminution. The piston-die press is presented as a methodology to determine the breakage distribution function of two different materials, from the mechanical response point of view: altered granite and a cal-silicate material. The aim is to determine the relation between the operative conditions and the mineral characteristics in order to explain and predict the breakage function parameters. The materials were characterised using XRD and single compression strength tests. The altered granite is a brittle material, which generates more fines under single compression conditions compared to bed compression conditions, mainly due to the mineral composition and the response of the material to the breakage action. The cal-silicate material shows a normal trend in its breakage behaviour. As is expected, the mineralogical characterisation is a useful tool to predict the values of the parameters of the breakage distribution function.

The mineralogy and liberation characteristics of the comminuted Penouta leucogranite host of the Sn-Ta ore were determined. Grinding developed by a combination of high-pressure grinding rolls (HPGR) followed by a ball mill (BM) was compared with a single ball mill process. The mineral characteristics of the grinding products were analyzed using a Tescan Integrated Mineralogical Analyzer (TIMA-X) and X-ray powder diffraction (XRD). The ore contains 103 ppm of Ta and is mainly composed of quartz, albite, microcline, muscovite, and kaolinite. Nb, Ta-rich minerals are columbite-(Mn) and tantalite-(Mn), as well as minor microlite and wodginite. The liberation in the product is high in the size fraction of less than 250 µm (51–52 wt % for columbite-group minerals (CGM) and 74–80 wt % for cassiterite) and reduced in larger particles (8.8–17 wt % for CGM and 28–37 wt % for cassiterite). The recovery in the −250 µm fraction was high, while in the larger fraction it is limited, remaining up to 80 ppm in some tailings. The combined use of HPGR and a BM reduces the particle size distribution of the product and, thus, increases the liberation of the ores. Smaller fractions can be treated directly using gravity methods; however, particles of a size greater than +250 µm should be ground more.

An improved approach is presented to model the product particle size distribution resulting from grinding in high-pressure roll crusher with the aim to be used in standard high-pressure grinding rolls (HPGR). This approach uses different breakage distribution function parameter values for a single particle compression condition and a bed compression condition. Two materials were used for the experiments; altered Ta-bearing granite and a calc-silicate tungsten ore. A set of experiments was performed with constant operative conditions, while varying a selected condition to study the influence of the equipment set-up on the model. The material was comminuted using a previously determined specific pressing force, varying the feed particle size, roll speed and the static gap. A fourth group of experiments were performed varying the specific pressing force. Experimental results show the high performance of the comminution in a high-pressure environment. The static gap was the key in order to control the product particle size. A mathematical approach to predict the product particle size distribution is presented and it showed a good fit when compared to experimental data. This is the case when a narrow particle size fraction feed is used, but the fit became remarkably good with a multi-size feed distribution. However, when varying the specific pressing force in the case of the calc-silicate material, the results were not completely accurate. The hypothesis of simultaneous single particle compression and bed compression for different size ranges and with different parameters of the distribution function was probed and reinforced by various simulations that exchanged bed compression parameters over the single particle compression distribution function, and vice versa.

The strategic importance of tantalum and its scarcity in Europe makes its recovery from low grade deposits and tailings interesting. In Penouta, the contents of Ta and Sn in old tailings from an Sn mine are of economic interest. Due to the relatively low grade of Ta of around 100 ppm, a detailed study of the mineralogy and liberation conditions is necessary. In this study, the mineralogy and the liberation characteristics of Sn and Ta ores of the Penouta tailings were investigated and compared with the current leucogranite outcropping ores. The characterization was conducted through X-ray diffraction, scanning electron microscopy, and electron microprobe. In addition, automated mineralogy techniques were used to determine the mineral associations and liberation characteristics of ore minerals. The grade of the leucogranite outcropping was found to be about 80 ppm for Ta and 400 ppm for Sn, and in the tailings used for the liberation study, the concentrations of Ta and Sn were about 100 ppm Ta and 500 ppm Sn, respectively. In both, the leucogranite outcropping and tailings, the major minerals found were quartz, albite, K-feldspar, and white mica. Ore minerals identified were columbite-group minerals (CGM), microlite, and cassiterite. The majority of CGM examined were associated with cassiterite, quartz, and muscovite particle compositions and cassiterite was mainly associated with CGM, quartz, and muscovite. The liberation size was 180 µm for CGM.

In this paper, the modeling of the liberation of scheelite is presented. A pattern of concentration experiments was performed to investigate the scheelite liberation and distribution density calculation procedure. In this work, one sample from a Mittersill tungsten ore was studied. This work describes a method for determining the downstream milling energy requirements for rod mill products based on a Bond mill test performance. The grade distribution of particles at a given size fraction was calculated using a predictive liberation model. The concentration behavior of these particles in size fractions was evaluated using batch concentrate tests. The recovery of particles in size/grade classes, image analysis using mineral liberation analysis (MLA), and function calculations were implemented for the modeling of the liberation. By describing the size, grade, and recovery data of particles in size/grade classes, a technique for the measurement of distribution functions was developed that relates beta distribution, a model for the function based on the incomplete beta function, and a solution to produce liberation modeling. It was shown that the predicted results agreed well with the observed results. With a procedure for measuring the liberation, it was possible to carry out the first experimental measurement of the beta distribution. This liberation/concentrate model has wide potential applications for metallurgy and plant design, where the liberation modeling is to be determined with the distribution density solution to the predictive mineral liberation function equation, which includes the liberation of ore samples and their liberation characteristics.