Columbite-(Fe) is a post-magmatic accessory mineral occurring within syenogranites and greisens from the Desemborque Pluton. The petrographic (SEM) and geochemical (EPMA and LA-ICPMS) examination of this mineral shows two distinct textural types within both the rocks, named columbite-1 and columbite-2. The columbite-1 type is characterized by zoned crystals with two stages of crystallization: i) An early Nb-rich cores with low Ta/(Ta + Nb) and Mn/(Mn + Fe) ratios (0.02–0.08 and 0.17 to 0.21 apfu, respectively), and ii) a later Ta-rich rims with higher Ta/(Ta + Nb) ratios (0.11–0.26) and similar Mn/(Mn + Fe) ratios (from 0.14 to 0.22) relative to the former cores. On the other hand, the columbite-2 type is defined by irregular crystals with patchy textures and very low Ta/(Ta + Nb) ratios (0.008–0.038) and moderate Mn/(Mn + Fe) ratios between 0.20 and 0.38. Trace element compositions of all columbite-(Fe) crystals are relatively enriched in HREEs and HFSEs; however, the columbite-2 presents higher abundances of REEs, Y, Th, U, Pb, Sc, and Sn relative to the columbite-1. This study highlights a unique hydrothermal origin for both the columbite types, but the textural relations of the columbite-2 crystals indicated that its formation is related to fluid-induced alterations of post-magmatic fluorite and/or cassiterite crystals at the final stage of the post-magmatic evolution.

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Amphibole and biotite were the principal mafic minerals precipitated during the magmatic and post-magmatic (including hydrothermal) crystallisation stages of coeval metaluminous to slightly peraluminous syenogranites and peralkaline alkali-feldspar granites of the Mandira Granite Massif, in the post-collisional A-type Graciosa Province, S-SE Brazil. Magmatic calcic (ferro-ferri-hornblende and hastingsite) amphiboles occur in the metaluminous syenogranites, whereas calcic (ferro-edenite), sodic–calcic (ferro-ferri-winchite) and sodic (arfvedsonite and riebeckite) amphiboles occur in peralkaline alkali-feldspar granites. Rare earth element (REE) contents decrease from hornblende to winchite and riebeckite, and the partition coefficients indicate increasing compatibility from light rare earth elements (LREE) to heavy rare earth elements (HREE), with a marked preference for the HREE over the LREE in the sodic–calcic and, particularly, the sodic amphiboles. Post-magmatic calcic- (ferro-actinolite) and sodic- (riebeckite) amphiboles are also present in the peralkaline granites. Magmatic biotite (annite) is dominant in syenogranites, whereas post-magmatic annite and late-to post-magmatic annite evolving to siderophyllite occurs in the peralkaline granites. Typical hydrothermal phyllosilicates are chlorite (chamosite) in syenogranites and related greisens, and ferri-stilpnomelane which is present in both peralkaline granites and metaluminous syenogranites. Lithostatic pressure estimates suggest that the main granites were emplaced under pressures of ~93–230 MPa, with close-to-liquidus temperatures varying from ~830°C for syenogranites to ~900°C for the peralkaline granites. The original magmas crystallised mainly under relatively reduced (buffered at ~ –1 ≤ QFM ≤ 0), and more oxidising (somewhat above QFM) environments, respectively. Chlorite, replacing biotite in syenogranites and as the main mineral in the related greisens, permits the temperature of the main hydrothermal event to have taken place between 250 and 272°C. Estimated log (fHF/fHCl) values from biotite compositions vary from ~ –2 to –1 (syenogranites) and ~ –3.5 to –2 (peralkaline granites) and indicate F preference over Cl in the hydrothermal fluid phase.