A concentrate obtained from mining tailings containing mainly cassiterite and columbotantalite was reduced for the production of tin metal. The compounds CaCO₃, Na₂CO₃, K₂CO₃, and borax were used as fluxes in the pyrometallurgical reduction smelting process, and graphite was employed as the reducing agent. The greatest recovery of Sn (>95%) was obtained when using CaCO₃ as the flux; the purity of Sn was 96%. A slag equivalent to 25% of the mass of the initial concentrate was produced during the recovery of the Sn. This contained 45% Nb₂O₅ and Ta₂O₅, adding extra value to the mine tailings. The tin metal ingot was purified by electrorefining involving a tin and H₂SO₄ electrolyte solution and a 101.9 A/m² current applied for 148 h. Under these conditions, 90 wt % of the Sn in the ingot was recovered at a purity of 99.97%.

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.