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Oxygen isotopic ratios are largely homogenous in the bulk of Earth’s mantle but are strongly fractionated near the Earth’s surface, thus these are robust indicators of recycling of surface materials to the mantle. Here we document a subtle but significant ~0.2‰ temporal decrease in δ¹⁸O in the shallowest continental lithospheric mantle since the Archean, no change in Δ′¹⁷O is observed. Younger samples document a decrease and greater heterogeneity of δ¹⁸O due to the development and progression of plate tectonics and subduction. We posit that δ¹⁸O in the oldest Archean samples provides the best δ¹⁸O estimate for the Earth of 5.37‰ for olivine and 5.57‰ for bulk peridotite, values that are comparable to lunar rocks as the moon did not have plate tectonics. Given the large volume of the continental lithospheric mantle, even small decreases in its δ¹⁸O may explain the increasing δ¹⁸O of the continental crust since oxygen is progressively redistributed by fluids between these reservoirs via high-δ¹⁸O sediment accretion and low-δ¹⁸O mantle in subduction zones.

 

A synthetic laser ruby crystal (HD-LR1) is introduced as a new matrix-matched reference material for secondary ionization mass spectrometry (SIMS) analysis of oxygen isotopes in corundum. Laser fluorination isotope ratio mass spectrometry (LF-IRMS) bulk analyses of multiple mg-sized fragments are homogenous, averaging δ18O = +18.40 ± 0.14‰ (95% confidence interval, n = 23) and Δ′17O = −0.368 ± 0.005‰ (as deviation from slope 0.528 for δ′17O vs. δ′18O at 95% conf., n = 11) relative to Vienna Standard Mean Ocean Water (V-SMOW). SIMS spot analyses show homogeneous O-isotopic values at the ng-scale independent of the location in the HD-LR1 single crystal and in four different crystallographic orientations. However, sample surface topography as an artefact of polishing corundum embedded in epoxy creates excess variability in δ18O within ∼100 μm from the edges of the grains. HD-LR1 is a chemical pure crystal with only Cr as a trace component detected at 276 μg g−1 by EPMA, whereas Be, often introduced in artificial gem enhancement, is <0.002 μg g−1 based on SIMS analyses. Therefore, HD-LR1 can also be used as a reference material for Cr, or as a blank for other trace element analyses of corundum by SIMS or LA-ICP-MS.

 

Active felsic magmatism has been rarely probedin situby drilling but one recent exception is quenched rhyolite sampled during the 2009 Iceland Deep Drilling Project (IDDP). We report finding of rare zircons of up to ∼100 µm in size in rhyolite glasses from the IDDP-1 well products and the host 1724 AD Viti granophyres. The applied SHRIMP U-Th dating for both the IDDP and the Viti granophyre zircons gives zero-age (±2 kyr), and therefore suggests that the IDDP-1 zircons have crystallized from an active magma intrusion rather than due to the 20–80 ka post-caldera magmatic episodes recorded by nearby domes and ridges. Ti-in-zircon geothermometer for Viti granophyre reveals zircon crystallization temperatures ∼800°C–900°C, whereas IDDP-1 rhyolite zircon cores show Ti content higher than 100 ppm, corresponding to temperatures up to ∼1,100°C according to the Ti-in-zircon thermometer. According to our thermochemical model at such elevated temperatures as 1,100°C, rhyolitic magma cannot be saturated with zircon and zircon crystallization is not possible. We explain this controversy by either kinetic effects or non-ideal Ti incorporation into growing zircons at low pressures that start to grow from nucleus at temperatures ∼930°C. High temperatures recorded by IDDP-1 zircon together with an occurrence of baddeleyite require that the rhyolite magma formed by partial melting of the host granophyre due to basaltic magma intrusion. Zr concentration profiles in glass around zircons are flat, suggesting residence in rhyolitic melt for >4 years. In our thermochemical modeling, three scenarios are considered. The host felsite rocks are intruded by: 1) a basaltic sill, 2) rhyolite magma 3) rhyolite sill connected to a deeper magmatic system. Based on the solution of the heat conduction equation accounting for the release of latent heat and effective thermal conductivity, these data confirm that the rhyolite magma could be produced by felsic crust melting as a result of injection of a basaltic or rhyolite sill during the Krafla Fires eruption (1975 AD).

 

There is abundant evidence for significant H2O in evolved melts from the platinum-rich UG2 chromitite and the Merensky Reef of the Bushveld Complex (South Africa), but there is no consensus about the source of H2O. We report triple-oxygen and hydrogen isotope ratios of interstitial, late-magmatic phlogopite from three localities of the UG2 layer. The phlogopite yielded δD values of –43‰ to –23‰, which is >30‰ higher than previously known from Bushveld rocks and far above the mantle values of ~–75‰. The phlogopite triple-oxygen isotope ratios are the first to be reported for Bushveld rocks, with values of Δ′17O0.5305 (17O excess relative to the reference line 0.5305) from –0.069‰ to –0.044‰ (δ18O 5.2‰–6.2‰). The oxygen data support existing models of as much as 30%–40% contamination of mantle-derived magmas in the lower to middle crust. However, the high δD values require a second step of contamination, which we attribute to brines from the marine sediments in the Transvaal Basin at the emplacement level.