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Abstract: Nanoscale crystals are becoming increasingly recognised in the products of volcanic eruptions, spanning a range of magma compositions. The crystallisation of nanolites impacts magma rheology, ascent dynamics, and eruptive style. Their impact can be enhanced due to their capacity to aggregate and develop neighbouring chemically differentiated boundary layers. However, their 3D interaction, spatial distribution, and morphology is not currently understood. Here we present a cutting-edge, 3D nanometre-scale visualisation and quantification of nanolites in scoriae of the Las Sierras-Masaya basaltic Plinian eruptions, acquired using X-ray ptychography. We find that Ti-magnetite nanolites aggregate, forming elongate, irregular structures in 3D. Their crystallisation extracts Fe and Ti from the melt, resulting in differentiated boundary layers with higher viscosity. Syn-eruptive crystallisation of nanolites and their interaction is estimated to have increased magma viscosity by 2–3 orders of magnitude, therefore, they likely had a strong control on magma rheology, increasing the potential of magma fragmentation.

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Abstract: The explosivity of a volcanic eruption is controlled by several interdependent processes during magma ascent, such as crystallisation, gas exsolution and outgassing. Syn-eruptive crystallisation can increase the potential of magma fragmentation. Whilst the degree of coupling between the gas and melt phases during ascent can influence eruptive style. Quantitative textural analysis of vesicles and crystals in erupted products can provide insight into syn-eruptive conduit processes and the conditions leading to magma fragmentation. Synchrotron-based imaging techniques such as X-ray computed micro-tomography can provide information on vesicle and crystal size, shape and their spatial distribution in 3D. Furthermore, X-ray ptychography, an X-ray microscopy technique with nanoscale resolution, can be used to expand this 3D textural analysis to nanoscale crystals in volcanic rocks. Here, we present a 3D reconstruction and quantification of vesicle and crystal textures in pyroclasts of the Masaya Triple Layer eruption, a highly explosive Plinian eruption of Masaya caldera, Nicaragua. Images and observations of vesicle textures at the micro-scale were acquired using X-ray computed micro-tomography and used to reconstruct the geometrical properties of the connected pore network, including connectivity, tortuosity and the throat-pore size ratio. X-ray ptychography was used to perform a 3D textural analysis of nanoscale crystals within the groundmass of clasts. These data were used to reconstruct conduit processes and evaluate the impact of syn-eruptive crystallisation, vesiculation and outgassing on magma rheology and fragmentation. Our results provide insight into the driving mechanisms of highly explosive, basaltic Plinian activity, and also highlight the potential of using multi-scale 3D imaging techniques to analyse textural features in pyroclasts and investigate controls on eruptive style.

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Abstract: The mobility and the rheological behaviour of magma within the Earth’s crust is controlled by magma viscosity. Crystallization and crystal morphology strongly affect viscosity, and thus mobility and eruptibility of magma, by locking it at depth or enabling its ascent towards the surface. However, the relationships between crystallinity, rheology and eruptibility remain uncertain because it is difficult to observe dynamic magma crystallization in real time. Here we show the results of in situ 3D time-dependent, high temperature, moderate pressure experiments performed under water-saturated conditions to investigate crystallization kinetics in a basaltic magma. 4D crystallization experiments with in situ view were performed using synchrotron X-ray microtomography, which provides unique quantitative information on the growth kinetics and textural evolution of pyroxene crystallization in basaltic magmas. Crystallization kinetics obtained with 4D experiments were combined with a numerical model to investigate the impact of rapid dendritic crystallization on basaltic dike propagation, and demonstrate its dramatic effect on magma mobility and eruptibility. We observe dendritic growth of pyroxene on initially euhedral cores, and a sur- prisingly rapid increase in crystal fraction and aspect ratio at undercooling ≥30 °C. Rapid dendritic crystallization favours a rheological transition from Newtonian to non-Newtonian behaviour within minutes. Modelling results show that dendritic crystallization at moderate undercooling (30-50 °C) can strongly affect magma rheology during magma ascent within a dike with important implications for the mobility of basaltic magmas within the crust. Our results provide insights into the processes that control whether magma ascent within the crust leads to eruption or not.

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Abstract: The Fe–Mg exchange coefficient between olivine (ol) and melt (m), defined as KdFe𝑇−Mg Kd Fe T − Mg  = (Feol/Fem)·(Mgm/Mgol), with all FeT expressed as Fe2+, is one of the most widely used parameters in petrology. We explore the effect of redox conditions on KdFe𝑇−Mg Kd Fe T − Mg using experimental, olivine-saturated basaltic glasses with variable H2O (≤ 7 wt%) over a wide range of fO2 (iron-wüstite buffer to air), pressure (≤ 1.7 GPa), temperature (1025–1425 °C) and melt composition. The ratio of Fe3+ to total Fe (Fe3+/∑Fe), as determined by Fe K-edge µXANES and/or Synchrotron Mössbauer Source (SMS) spectroscopy, lies in the range 0–0.84. Measured Fe3+/∑Fe is consistent (± 0.05) with published algorithms and appears insensitive to dissolved H2O. Combining our new data with published experimental data having measured glass Fe3+/∑Fe, we show that for Fo65–98 olivine in equilibrium with basaltic and basaltic andesite melts, KdFe𝑇−Mg Kd Fe T − Mg decreases linearly with Fe3+/∑Fe with a slope and intercept of 0.3135 ± 0.0011. After accounting for non-ideal mixing of forsterite and fayalite in olivine, using a symmetrical regular solution model, the slope and intercept become 0.3642 ± 0.0011. This is the value at Fo50 olivine; at higher and lower Fo the value will be reduced by an amount related to olivine non-ideality. Our approach provides a straightforward means to determine Fe3+/∑Fe in olivine-bearing experimental melts, from which fO2 can be calculated. In contrast to KdFe𝑇−Mg Kd Fe T − Mg , the Mn–Mg exchange coefficient, KdMn−Mg Kd Mn − Mg , is relatively constant over a wide range of P–T–fO2 conditions. We present an expression for KdMn−Mg Kd Mn − Mg that incorporates the effects of temperature and olivine composition using the lattice strain model. By applying our experimentally-calibrated expressions for KdFe𝑇−Mg Kd Fe T − Mg and KdMn−Mg Kd Mn − Mg to olivine-hosted melt inclusions analysed by electron microprobe it is possible to correct simultaneously for post-entrapment crystallisation (or dissolution) and calculate melt Fe3+/∑Fe to a precision of ≤ 0.04.

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Abstract: Basaltic volcanism is strongly influenced by magmatic viscosity, which, in turn, is controlled by magma composition, crystallisation, oxygen fugacity and vesiculation. We developed an environmental cell to replicate the pressure and temperature during magma ascent from crustal storage to the surface, while capturing crystallisation using in-situ 4D X-ray computed microtomography. Crystallisation experiments were performed at Diamond Light Source, using monochromatic 53 keV X-rays, a pixel size of 3.2 μm, a sample to detector distance of 2000 mm, 1440 projections per 180 deg, an acquisition time of 0.04 s, and a rotation velocity of 3.125 deg.s-1. The redox conditions were controlled using an oxidised nickel disk for each experiment. Our starting materials were samples made of crystal-free glass cylinders (Ø 3 mm) from the 2001 Etna eruption with 0.9 and 0.8 wt. % water content. In the experiments, samples and crucibles were sealed initially by applying ~10 N loads. All samples were then heated up above glass transition (between 800 °C and 900 °C) in order to allow sample homogenisation while preventing volatiles exsolution. We then pressurised each sample by applying uniaxial loads (between 80 and 380 N), using high-degree alumina pistons, in order to generate enough internal pressure to maintain bubble-free samples when the desired high temperature was reached. Once at the initial high temperature, we began experiments via dropping the temperature to different target isothermal (from 1210 to 1130 °C or 1180 to 1110 °C) and isobaric conditions (8 and 10 MPa, respectively). For the whole duration of the experiments, we were able to observe directly and record pyroxene crystal nucleation and growth. Specifically, we were able to observe pyroxene nucleation on bubbles at small undercooling (∆T) and epitaxial growth of pyroxene at large ∆T. An increase of ∆T (up to 50 °C) can be associated with a decompression of a magma chamber or a decompression during magma ascent in the conduit. As ∆T = 30 - 50 °C can be reached in most of the basaltic volcanic systems on Earth, our results provide a feasible explanation of which mechanisms control nucleation and growth of pyroxene crystals in hydrous basaltic magmas. In addition, epitaxial growth promotes a faster increase of the crystal volume. As a larger crystal content translates into a higher viscosity, our results have important implications for magma rheology, and are extremely important to improve our understanding of magma ascent dynamics during volcanic eruptions, and our capacity to predict eruptions and mitigate volcanic hazards.