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We present a new set of reference materials, the ND70‐series, forin situmeasurement of volatile elements (H₂O, CO₂, S, Cl, F) in silicate glass of basaltic composition. The materials were synthesised in piston cylinders at pressures of 1 to 1.5 GPa under volatile‐undersaturated conditions. They span mass fractions from 0 to 6%m/mH₂O, from 0 to 1.6%m/mCO₂and from 0 to 1%m/mS, Cl and F. The materials were characterised by elastic recoil detection analysis for H₂O, by nuclear reaction analysis for CO₂, by elemental analyser for CO₂, by Fourier transform infrared spectroscopy for H₂O and CO₂, by secondary ion mass spectrometry for H₂O, CO₂, S, Cl and F, and by electron probe microanalysis for CO₂, S, Cl and major elements. Comparison between expected and measured volatile amounts across techniques and institutions is excellent. It was found however that SIMS measurements of CO₂mass fractions using either Cs⁺or O⁻primary beams are strongly affected by the glass H₂O content. Reference materials have been made available to users at ion probe facilities in the US, Europe and Japan. Remaining reference materials are preserved at the Smithsonian National Museum of Natural History where they are freely available on loan to any researcher. 

Abstract Arc magmas are produced from the mantle wedge, with possible addition of fluids and melts derived from serpentinites and sediments in the subducting slab. Identification of various sources and their relevant contributions to such magmas is challenging; in particular, at continental arcs where crustal assimilation may overprint initial geochemical signatures. This study presents oxygen isotopic compositions of zoned olivine grains from post-caldera basalts and boron contents and isotopes of these basalts and glassy melt inclusions hosted in quartz and clinopyroxene of silicic tuffs in the Toba volcanic system, Indonesia. High-magnesian (≥87 mol% Fo [forsterite]) cores of olivine in the basalts have δ18O values ranging from 5.12‰ to 6.14‰, indicating that the mantle source underneath Toba is variably enriched in 18O. Olivine with <87 mol% Fo has highly variable (4.8–7.2‰), but overall increased, δ18O values, interpreted to reflect assimilation of high δ18O crustal materials during fractional crystallization. Mass balance calculations constrain the overall volume of crustal assimilation for the basalts as ≤13%. The processes responsible for the 18O-enriched basaltic melts are further constrained by boron data that indicate the addition of <0.1 wt% fluids to the mantle, >40% of the fluids being derived from serpentinites and others from altered oceanic crust and sediments. This amount of fluids can increase δ18O of the magma by only ~0.02‰. Approximately 6–9% sediment-derived melt hybridization in the mantle wedge is further needed to yield basaltic melts with δ18O values in equilibrium with those of the high-Fo olivine cores. The cogenetic silicic tuffs, on the other hand, seem to record a higher proportion of fluid addition dominated by sediment-derived fluids to the mantle source, in addition to crustal assimilation. Our reconnaissance study therefore demonstrates the application of combined B and O isotopes to differentiate between melts and fluids derived from serpentinites and sediments in the subducted slab—an application that can be applied to arc magmas worldwide. 

Raman spectroscopy has become the tool of choice for analyzing fluid inclusions and melt inclusion (MI) vapor bubbles as it allows the density of CO2-rich fluids to be quantified. Measurements are often made at ambient temperature (Tamb ~18-25 °C), resulting in reported bulk densities between 0.2 and 0.7 g/mL despite that single-phase CO2 under these conditions is thermodynamically unstable and instead consists of a liquid (~0.7 g/mL), and a vapor phase (~0.2 g/mL). Here, we present results from experiments conducted at Tamb and 37 °C (above the CO2 critical temperature) on 14 natural CO2-rich MI bubbles from Mount Morning, Antarctica. Here, we show that at Tamb, laser power strongly affects the CO2 Raman spectrum of MI bubbles with bulk densities within the miscibility gap. High-power laser heating and low spectral resolution explain why published measurements have reported such bulk densities at Tamb even when using an instrument-specific calibration. 

Daynes, O.*, Ustunisik, G., and Nielsen, R. L., and Betts, M.*, “Depth of Formation of Petrogenetic Processes: Evidence from Plagioclase-Hosted Melt Inclusions” Presentation at Goldschmidt Conference, Lyon, France (July 9-14, 2023). 

Recent geochemical evidence confirms the oxidized nature of arc magmas, but the underlying processes that regulate the redox state of the subarc mantle remain yet to be determined. We established a link between deep subduction-related fluids derived from dehydration of serpentinite ± altered oceanic crust (AOC) using B isotopes and B/Nb as fluid proxies, and the oxidized nature of arc magmas as indicated by Cu enrichment during magma evolution and V/Yb. Our results suggest that arc magmas derived from source regions influenced by a greater serpentinite (±AOC) fluid component record higher oxygen fugacity. The incorporation of this component into the subarc mantle is controlled by the subduction system’s thermodynamic conditions and geometry. Our results suggest that the redox state of the subarc mantle is not homogeneous globally: Primitive arc magmas associated with flat, warm subduction are less oxidized overall than those generated in steep, cold subduction zones. 

Inclusions of basaltic melt trapped inside of olivine phenocrysts during igneous crystallization provide a rich, crystal-scale record of magmatic processes ranging from mantle melting to ascent, eruption, and quenching of magma during volcanic eruptions. Melt inclusions are particularly valuable for retaining information on volatiles such as H 2 O and CO 2 that are normally lost by vesiculation and degassing as magma ascends and erupts. However, the record preserved in melt inclusions can be variably obscured by postentrapment processes, and thus melt inclusion research requires careful evaluation of the effects of such processes. Here we review processes by which melt inclusions are trapped and modified after trapping, describe new opportunities for studying the rates of magmatic and volcanic processes over a range of timescales using the kinetics of post-trapping processes, and describe recent developments in the use of volatile contents of melt inclusions to improve our understanding of how volcanoes work. ▪  Inclusions of silicate melt (magma) trapped inside of crystals formed by magma crystallization provide a rich, detailed record of what happens beneath volcanoes. ▪  These inclusions record information ranging from how magma forms deep inside Earth to its final hours as it ascends to the surface and erupts. ▪  The melt inclusion record, however, is complex and hazy because of many processes that modify the inclusions after they become trapped in crystals. ▪  Melt inclusions provide a primary archive of dissolved gases in magma, which are the key ingredients that make volcanoes erupt explosively.