We present a novel application of Raman microtomography for quantitative characterisation of glass inclusion-hosted bubbles, which allows for the simultaneous identification and volumetric quantification of mineral and fluid phases filling the bubble. The combination of Raman microtomography with synchrotron XRF mapping and scanning electron microscopy provides a complete compositional and textural characterisation of the bubble. In the studied samples, minerals are systematically present on the walls of the bubbles: dominantly carbonates in samples from continental intraplate and hotspot volcanic provinces, and sulfates in the sample from subductionrelated settings. Along with fluid CO 2 , carbonates sequester 65 to 84 % of the CO 2 originally dissolved in the melt, while 18 to 60 % of the sulfur contained in the inclusion is stored in sulfides and/or sulfates. Thus, the total melt inclusion CO 2 and S contents can be underestimated (by up to ∼ 40 % and 60 %, respectively) if minerals in the bubbles are neglected. This study highlights the importance of 3D mapping of shrinkage bubbles hosted in glass inclusions for a better assessment of the bulk pre-eruptive contents of volatiles in magmas.
Abstract. Experimental homogenization of olivine-hosted melt inclusions representative of near-primary basic and ultrabasic magmas is a powerful approach to investigate the nature of their source regions and the melting conditions in Earth's mantle. There is growing evidence that the total CO2 contents of olivine-hosted melt inclusions may reach values of the order of a single to several weight percent, especially in intraplate continental basalts. To be able to homogenize melt inclusions with such high CO2 contents, we developed a technique allowing for heat treating of the melt inclusions under hydrostatic pressures up to 3–4 GPa in a piston cylinder, using thick-walled Au80–Pd20 containers and molten NaCl as the surrounding medium for the inclusion-bearing olivines. We applied this technique to olivine phenocrysts from Thueyts basanite, Bas-Vivarais volcanic province, French Massif Central. Thueyts melt inclusions were chosen because of their high CO2 contents, as indicated by up to 1.19 wt % dissolved CO2 in the glasses and by the presence of shrinkage bubbles containing abundant carbonate microcrystals in addition to a CO2 fluid phase. The homogenization experiments were conducted at pressures of 1.5 to 2.5 GPa, temperatures of 1275 and 1300 ∘C, and run durations of 30 min. In all the melt inclusions treated at 2.5 GPa–1300 ∘C and half of those treated at 2 GPa–1300 ∘C, we were able to completely homogenize the inclusions, as indicated by the disappearance of the starting bubbles, and we obtained total CO2 contents ranging from 3.2 wt % to 4.3 wt % (3.7 wt % on average). In all the other melt inclusions (equilibrated at 1.5 or 2 GPa and 1300 ∘C or at 2.5 GPa–1275 ∘C), we obtained lower and more variable total CO2 contents (1.4 wt % to 2.9 wt %). In the inclusions with the highest total CO2 contents, the size of the shrinkage bubble was in most cases small (<5 vol %) to medium (<10 vol %): this is a strong argument in favor of an origin of these melt inclusions by homogeneous entrapment of very CO2-rich basanitic liquids (∼ 4 wt %) at pressures of 2 to 2.5 GPa. The lower total CO2 contents measured in some inclusions could reflect a natural variability in the initial CO2 contents, due for instance to melt entrapment at different pressures, or CO2 loss by decrepitation. An alternative scenario is heterogeneous entrapment of basanitic liquid plus dense CO2 fluid at lower pressures but still at least on the order of 1 GPa as indicated by dissolved CO2 contents up to 1.19 wt % in the glasses of unheated melt inclusions. Whatever the scenario, the basanites from the Bas-Vivarais volcanic province were generated in a mantle environment extremely rich in carbon dioxide.
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