The radiometric ages of the returned samples are the cornerstone of lunar cratering chronology models. However, all the previous samples were from the lunar nearside and the radiometric ages of those samples that can be associated with particular surfaces are <4.0 billion years. On 25 June 2024, Chang'e-6 successfully returned 1.935-kilogram samples from the lunar farside. The samples included local basalts with an age of 2807 ± 3 million years and the norites with an age of 4247 ± 5 million years likely corresponding to the age of the South Pole-Aitken basin. With these radiometric ages, we refined the lunar chronology function (CF) and verified that it is still consistent with a combination of an exponential decrease and a linear rate. We further derived the impacting rate and found it supports a smooth decay instead of abrupt changes of the impactor flux at early times. The refined lunar CF can be used to obtain more reliable ages for unsampled lunar areas and provide critical constraint for the lunar early impact history.
Sedimentary pyrite constitutes an invaluable geological archive for reconstructing Earth's ancient environments, yet interpreting its origins within deep geological records is often complicated by subsequent diagenetic modification. Here, we examine four distinct pyrite morphologies (framboidal pyrites hosted in chert nodules and matrix, euhedral pyrites within calcite rims of nodules, and pyrite aggregates within surrounding matrix rocks) preserved in the Ediacaran Doushantuo Formation of South China, utilizing a combination of highresolution electron microscopy and in-situ secondary ion mass spectrometry sulfur isotope analysis. Our microscopic observations identify well-preserved framboidal pyrites, variably altered by post-depositional processes, alongside large euhedral pyrite crystals encapsulated by calcite, and irregular pyrite aggregates. Integrated nanoscale microscopic and in situ isotopic analyses consistently demonstrate that framboidal pyrites exhibit negative S34S values, indicative of microbial sulfate reduction within the water column or at the sediment-water interface during early diagenesis. Conversely, euhedral pyrites and irregular aggregates from nodule rims and surrounding matrix yield significantly positive S34S values, consistent with thermochemical sulfate reduction during late-stage burial diagenesis. This finding contrasts with previous interpretations that attribute positive S34S values to a diminished marine sulfate reservoir within a restricted paleoceanographic setting. Our results emphasize that post-depositional thermochemical sulfate reduction processes can significantly elevate S34S values of pyrites. This study underscores the critical necessity of deconvolving diagenetic overprinting from primary signatures by integrating in-situ isotopic and microscopic analyses, thereby refining paleoenvironmental reconstructions from pyrite archives.
Unraveling the origin of lunar farside-nearside asymmetry requires comparison of various lithologies from both hemispheres, a task long hindered by the absence of farside samples. Here, we present geochemical data for Chang'e 6 (CE6) lithologies from the farside, revealing systematic differences from their nearside counterparts. CE6 anorthosites are more magnesian, while CE6 Mg-suite samples contain lower potassium, rare earth element, and phosphorus (KREEP) contents. However, CE6 Mg-suite samples have Mg# values comparable to Apollo Mg-suite rocks. The mantle source of CE6 2.8-billion-year-old basalts is similar to that of Apollo low-Ti basalts. This systematic geochemical comparison of farside and nearside lithologies, which sample distinct lunar magma ocean (LMO) product layers, indicates that the mantle displays no clear compositional dichotomy. In contrast, the farside anorthositic crust is more magnesium-rich and thicker, while late-stage LMO products may be thinner on the farside. Therefore, we propose that the observed farside-nearside asymmetry originated from lateral thermal convection within a long-lived LMO on the tidally locked Moon.
Accurate isotope compositions of nanoparticles in planetary materials provide critical constraints on the evolution of the early solar system. Atom probe tomography (APT) can analyze isotopes in situ with the highest spatial resolution, making it ideal for nanoscale planetary materials. However, significant deviations between isotope ratios determined using APT and a traditional mass spectrometer have hindered the wide application of APT in isotope analysis. Here, we propose that these isotope ratio discrepancies arise from different uncounted rates of the isotopes in APT analysis. Theoretical assessment indicates that such discrepancies can be corrected using a suite of reference materials. Iron isotope analyses of Fe-Mn-Ni steels and meteoritic irons using APT and a multicollector inductively coupled plasma mass spectrometer (MC-ICP-MS) confirm a strong linear correlation between the two data sets, supporting the establishment of 56Fe/54Fe and 57Fe/54Fe calibration curves for APT data correction. The calibration curves were subsequently validated using four meteoritic irons with known Fe isotope ratios. Combining all of the errors, our corrected APT results achieve a 2σ uncertainty of <0.15‰ for δ56Fe. This precision demonstrates that our calibrated APT protocol enables accurate isotope determination, unlocking the potential of APT for precise isotope analysis of nanoscale planetary materials.
Palaeomagnetic data from Earth and planetary samples provide a crucial record for unraveling the evolution of planetary dynamos. However, these records are frequently compromised by secondary isothermal remanent magnetization (IRM) acquired under fields of several-to-tens of millitesla, especially in planetary palaeomagnetic investigations. Notably, such IRMs frequently exhibit “tail” components that resist equivalent alternating field demagnetization, thereby contaminating primary remanence. This phenomenon remains poorly understood, hindering physical insight and leading to the possible exclusion of potentially valuable extraterrestrial samples or inclusion of contaminated ones in palaeomagnetic investigations. Here, we conducted analyses on a Chang’e-5 returned sample, a lunar meteorite, and terrestrial basalts, including stepwise IRM contamination experiments, simulated IRM-contaminated palaeointensity analyses, rock magnetic measurements, and statistical simulations. The results confirm that the IRM tails are widespread, showing pronounced effects when contamination fields >∼20 mT. The IRM tails display distinct patterns in samples dominated by different magnetic grain sizes, which cannot be adequately explained by magnetic particle interactions. Instead, our simplified statistical model reveals that these tails can arise from domain state transitions in a subset of single-vortex and single-domain grains with multiple stable domain axis orientations. Finally, we evaluate the palaeomagnetic data of two lunar samples exhibiting moderate IRM contamination. While no reliable palaeointensity was obtained for the ∼2.9-Ga lunar meteorite, a convincing palaeointensity of ∼5 μT was retrieved from the ∼2.0-Ga Chang’e-5 basalt, supporting a persisting weak lunar dynamo. This study therefore provides a quantitative framework for assessing IRM-tail effects and recovering reliable palaeomagnetic records across terrestrial bodies.
Sulfur is closely associated with various types of ore deposits, particularly orogenic gold (Au) systems, where sulfur-bearing melts and fluids play a critical role in transporting ore-forming elements essential for ore formation. The widely accepted metamorphic devolatilization model suggests that compositionally fertile sedimentary rocks serve as potential gold sources. Therefore, understanding sulfur behavior during prograde metamorphism is essential for elucidating the mechanisms underlying metal activation and mobility. In this study, we conducted in-situ sulfur isotope (δ34S) analyses using secondary ion mass spectrometry (SIMS) on samples from the Hongshankou area, a representative Barrovian-type metamorphic sequence characterized by intermediate pressure-temperature (P-T) conditions. This sequence comprises the biotite, garnet, staurolite, and kyanite zones. Our results show a systematic increase in δ34S values (from 3.1‰ to 5.5‰) coupled with a progressive decrease in total sulfur content (from 320 ppm to 165 ppm) as metamorphic grade increases. The most pronounced sulfur mobilization occurs between the garnet and staurolite zones. In all analyzed samples, Au or Au-bearing minerals predominantly occur along the edges or within pyrite grains, highlighting the critical role of pyrite breakdown in controlling gold mobility. Thus, sulfur isotope fractionation provides robust constraints for quantitatively assessing sulfur mobility during metamorphism. These findings reinforce the concept that metasedimentary rocks and their metamorphic fluids represent fertile sources of Au and other metals enriched in orogenic gold deposits.
Ultrahigh-temperature (UHT) metamorphism represents extremely hot crustal conditions, and is generally related to convergent plate margins during supercontinent assembly. However, the mechanisms to form Archean UHT metamorphism before supercontinent cycle are controversial. The Saglek-Hebron Complex (SHC) contains some of the oldest rocks on Earth that formed as early as ca 3.9 billion years ago and recorded polymetamorphism in Archean, although the exact metamorphic conditions and history are poorly understood. In this study, we investigate petrography, pressure-temperature (P-T) estimates, and zircon U-Pb geochronology of a metasedimentary rock from the SHC of northern Labrador, part of the North Atlantic Craton (NAC). The U-Pb age and trace element composition of zircon suggest zircon growth during melt crystallization and garnet resorption following an episode of ultrahigh-temperature (UHT) metamorphism at or before 2.72 Ga. Phase equilibrium modelling, two-felspar, and Zr-in-rutile thermometry together constrain UHT metamorphic P-T conditions to 7.2-9.2 kbar and 920-1000 degrees C. A rimward increase in the garnet grossular component, a change of garnet modes, and localized growth of matrix kyanite and rutile are consistent with a post-peak high-T retrograde stage within a P-T path associated with pressure increase and cooling (to similar to 11 kbar at similar to 850 degrees C). We propose that the UHT rocks formed previously in the lower crust of a hot and weak backarc region with elevated heat flow due to lithosphere extension and asthenosphere upwelling, which was closed by lateral thickening during subsequent multiple terrane convergence. Our findings are consistent with Hf isotopes in zircon from rocks of the NAC, the global record of metamorphism, and a period of cratonization of Earth's ancient crustal nuclei during the Neoarchean era that may be coincident with the operation of plate tectonics.
A natural rutile megacryst (JDX) was characterized as a reference material for in-situ microanalysis of trace elements. Validation experiments using electron probe microanalysis (EPMA) and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) in different laboratories demonstrated that the JDX rutile exhibits homogeneous distribution at mu m-mm scale with respect to Ti, Mg, Al, Sc, Fe, V, Cr, Zr, Nb, Sn, Hf, Ta, W, and U (RSD < 15%). Various techniques of bulk chemical analyses (XRF and solution ICP-MS) revealed good consistency with microbeam analytical results for most trace elements, suggesting that the studied rutile can serve as a reference material for in-situ microanalysis. Reference values and their uncertainties at the 95% confidence level for major and trace elements were presented in this study. The JDX rutile plays a significant role in improving analytical accuracy and ensuring quality control for trace element measurements, particularly in EPMA. It further enhances the geological applications of Zr-in-rutile geothermometry, V- and Fe-based oxybarometry, and quantitative provenance studies (e.g., Nb, Ta, and Cr).
Hainan Island in South China lies at the intersection of the Paleo-Tethyan and Paleo-Pacific tectonic regimes. The discovery of Carboniferous oceanic-type eclogites at Chaotanbi on northeastern Hainan Island offers a novel perspective for elucidating the early tectonic evolution of the Southeast Asian continent. Recently, new eclogite exposures have been recognized at Gongmiao and Yadunling, similar to similar to 70-100 km southwest of the Chaotanbi eclogites. These eclogites occur as kilometer-scale tectonic lenses in the Huangzhuling Complex, which predominantly comprises Late Devonian gneissic granites with subordinate Silurian clastic metasedimentary rocks. The Gongmiao eclogites generally preserve a primary mineral assemblage of garnet + omphacite + quartz + (rutile + ilmenite) +/- amphibole +/- zoisite or allanite, with rare kyanite or phengite. Peak pressure-temperature conditions during eclogite-facies metamorphism are estimated at 750-830 degrees degrees C and 18.5-21.2 kbar, followed by decompressional cooling through amphibolite-facies (690-740 degrees degrees C and 8.6-12.6 kbar) to greenschistand prehnite-pumpellyite-facies conditions. The Yadunling eclogites consist mainly of garnet + omphacite (completely symplectized in the matrix) + amphibole + quartz + (rutile + ilmenite) +/- epidote +/- calcite. They record a metamorphic history from prograde stage at 490-540 degrees degrees C and 10.7-14.0 kbar to peak stage at 620-700 degrees degrees C and 16.2-17.9 kbar, followed by near-isothermal decompression (620-670 degrees degrees C and 8.7-12.7 kbar) and subsequent cooling to greenschistfacies conditions. Ion microprobe zircon U-Pb ages constrain eclogite protoliths to 359 +/- 2 Ma (Gongmiao) and metamorphism to 310-295 Ma, with rutile cooling ages of 295-285 Ma. Trace element geochemical analyses indicate that the Gongmiao eclogites have an island arc geochemical signature, with bulk-rock initial pound Nd pound values of--1.0 to + +2.7 and an average zircon initial pound Hf pound value of + +11.1, whereas the Yadunling eclogites display affinities consistent with normal mid-ocean-ridge basalt, with initial pound Nd pound values of + +5.5 to + +6.2. These data suggest that their protoliths correspond to arc-type gabbros and oceanic basalts, respectively, formed in a backarc basin environment. Minor siliceous rocks (with terrigenous detritus) within or adjacent to the Yadunling eclogites likely experienced synchronous metamorphism and deformation along with the eclogites. However, the widespread gneissic granites and clastic metasedimentary rocks underwent only low-grade metamorphism at ca. 285 Ma. This implies that the eclogites were tectonically juxtaposed with these country rocks during their exhumation. The coeval Gongmiao, Yadunling, and Chaotanbi eclogites define a > >100 km NE-SW-trending medium-to high-temperature eclogite belt on eastern Hainan Island. The formation of this eclogite belt is inferred to be related to the opening and closure of a backarc basin and subsequent arc-continent collision, which are induced by the retreating to advancing subduction of the western Paleo-Pacific oceanic lithosphere during the late Paleozoic.
The Qinling-Tongbai-Hong'an-Dabie orogenic belt records complex tectonic evolution history from the Paleozoic to the Mesozoic. However, the Paleozoic magmatism and metamorphism of the Dabie orogen remain poorly constrained. This study presents an integrated geochemical, geochronological, and isotopic investigation of mylonitized monzonite and granite in the Beihuaiyang zone. Zircon U-Pb dating and Hf isotopic analysis reveal that the granite from the Tiechong pluton formed at ca. 451 Ma with positive epsilon Hf(t) values (10.3-14.4), whereas the monzonite from the Gongdian outcrop crystallized at 481 +/- 4 Ma with negative epsilon Hf(t) values (-7.2 to-0.7). Geochemical signature and zircon Hf isotopic composition of monzonite provided clear evidence for its genesis in a continental arc setting with significant crustal materials. Metamorphic zircon and titanite U-Pb ages documented multiple Carboniferous-Permian tectonic-thermal metamorphism at ca. 340 Ma, 313 Ma, and 283 Ma. The high-temperature metamorphism in the eastern Dabie orogen shows a clear contrast to the high-pressure/low-temperature metamorphism in the Hong'an orogen, indicating tectonic variations within the oceanic subduction system. These new data provide critical petrological and geochemical evidence for the eastward extension of the Paleozoic Qinling orogen and the Shangdan Ocean into the Dabie orogen, offering new constraints on the lateral tectonic correlation and evolution history of the Qinling-Tongbai-Hong'an-Dabie orogenic belt.
The aragonite shells of giant clam (Tridacna spp.) with clear daily growth bands have been demonstrated to be an ideal paleoweather archive. However, the current paleoweather proxies of Tridacna spp. are still limited in variety and require further expansion. 518O, one of the most commonly used geochemical proxies in paleoclimate research, has been widely used for monthly paleoclimate reconstruction in Tridacna spp., which usually reflects sea surface temperature (SST) and seawater 518O. However, its implication in paleoweather reconstruction is seldomly discussed due to the limitation of data resolution. Here, the daily to weekly resolved Tridacna 518O profiles from northern South China Sea (SCS) were analyzed using secondary ion mass spectrometer (SIMS). The results show that the daily to weekly resolved 518O profiles have distinct seasonal cycles, but the derived SST seasonality cannot rule out the possibility of influence from high-frequency fluctuations. More importantly, the daily to weekly resolved 518O profiles show significant intraseasonal oscillation (ISO). Together with the contemporaneous instrumental data, it is suggested that the ultrahigh resolution Tridacna 518O has the potential to record the ISO via hydrological and thermal processes.
Apatite is a ubiquitous accessory mineral in different types of rocks and mineral deposits,demonstrating remarkable persistence throughout the entire magmatic-hydrothermal process.The variability of sulfur concentration and the valence state occupying the crystal lattice could be influenced by relatively oxidizing conditions.The concentration of sulfur in apatite was initially applied in constraining the oxygen fugacity of magma and estimating the sulfur content of the parental magma.In recent years,with the development of in situ microanalysis techniques for sulfur isotopic ratios in apatite using Secondary Ion Mass Spectrometry(SIMS)and Laser Ablation Multi-Collector Inductively Coupled Plasma Mass Spectrometry(LA-MC-ICP-MS),rapid analysis of apatite sulfur isotopes with high spatial resolution has become feasible.Compared to the traditional bulk analysis,the in situ analytical method eliminates the need for lengthy purification process and improves the efficiency of analyses.The in situ microanalysis of S isotopes in apatite has revealed the inter-and intra-crystalline isotopic variations of mineral grains on the scale of tens of microns,providing critical evidence for addressing geological problems such as formation and mineralization of rocks.This study reviewed recent advancements in methods for in situ microanalysis of S isotopic ratios in apatite using SIMS and LA-MC-ICP-MS,along with their geological applications.
Investigations in collisional orogens involved in polyphase deformation, high-grade metamorphism, partial melting of rocks and fluid-flow regimes have constraints on data interpretation, particularly regarding the time of primary magmatism and later melting. Zircon geochronological investigations were carried out on granites and granitic gneisses of the Central Indian Tectonic Zone (CITZ) of India to resolve the problem regarding the timing of the collisional events. A granite gneiss previously mapped as the basement for the Sausar Group or as a syn-tectonic (syn-orogenic) intrusion in the Sausar Group provided U-Pb age of 1296 +/- 6 Ma, and results from another post-tectonic (post-orogenic) granite emplacement in the Sausar Group gave U-Pb age of 933 +/- 7 Ma. While the age of the latter defines a bench-mark point for the time limit of compressional tectonics in the region, the age of the former is much older than the previously identified time of amalgamation between the North and South Indian Blocks along CITZ at similar to 1040 Ma. The discrepancy for time of emplacement of the granite gneiss was scrutinised by analysing the map pattern of the gneiss and the metasedimentary rocks bordering it, available P-T path for CITZ, high-precision zircon geochronological data from CITZ and about 94 geochemical analyses of granite gneisses in CITZ along with the data generated for the analysed granites. These multi-pronged approaches provided additional bench-mark points in the tectonic evolution of CITZ. The geochronological results from the granite gneiss do not support the previous suggestion regarding amalgamation of blocks along CITZ during the "Grenvillean Orogeny" at similar to 1040 Ma.
As the largest and oldest well-preserved impact structure on the Moon, the South Pole-Aitken (SPA) basin on the lunar farside is critical for understanding early solar system dynamics and lunar history, but accurately determining its age remains challenging. Crater-counting chronology and Apollo sample studies propose various SPA-forming ages, which require validation by in situ sampling of the SPA basin. Here, we present the petrology, geochemistry and chronology of norite clasts from the SPA basin that were returned by Chang'e-6. These norites have highly anorthite-rich, rare-earth element-poor plagioclase and magnesium-rich pyroxene, in contrast to Mg-suite norites that were returned from the lunar nearside. Abundant Fe-Ni metals with meteoritic Ni/Co ratios, depletion of volatile elements and variable grain sizes and cooling rates strongly indicate that the norites were crystallized from an impact melt sheet. Precise Pb-Pb ages of zirconium-bearing minerals in the norites yield two distinct impact events at 3.87 and 4.25 Ga. The former represents an impact-resetting event within the basin. The latter finding is most consistent with the age of the SPA impact, providing an initial 4.25-Ga anchor for the older end of the lunar crater chronology and refining the timeline for early lunar evolution.
Oceanic arc and back-arc magmas are typically sourced from mantle metasomatized by subducted slab fluids/melts, but the role of the overriding plate is often ignored. Here we report the oxygen isotopic compositions of olivines in basalts erupted during arc, arc rifting, and back-arc spreading stages in the Mariana convergent margin. Rifting-stage olivines have high Forsterite (Fo = 85-90) and mantle-like delta O-18 (4.92 to 5.69 parts per thousand). The delta O-18 values of olivines in arc and back-arc basin lavas correlate with their Fo values; high-Fo (>83) olivines have mantle-like delta O-18 while those in low-Fo olivines are as low as 3.87 +/- 0.30 parts per thousand. This indicates that fractionating magmas assimilated low-delta O-18 oceanic crust in the hydrothermally-altered upper plate, rather than the injections of underlying subducted slab-derived melts. Considering the globally widespread distribution of low-delta O-18 evolved olivine, we propose that low-delta O-18 wall rock may be common in the shallow lithosphere and serves as an important contributor to erupted evolved magma.
The Chang'e-5 landing site provides an important window into the Moon's late Eratosthenian period of volcanism at similar to 2 Ga. Clarifying the Moon's history of volcanic activity using radioisotopic dating assists investigations of the evolution of the lunar surface as well as the Moon's internal dynamics. Recent chronological investigations of Chang'e-5 basalts produced ages spanning similar to 100 Ma, thereby inhibiting interpretation of the duration of volcanism recorded in the returned samples. We used microcomputed tomography and Back-Scatter Electron imaging to characterize the structure and morphology of nine Chang'e-5 basalt clasts. Several basalt clasts lack shock features and are interpreted to have not been significantly thermally disturbed. Ar-40/Ar-39 incremental heating produced well defined plateaus for four sub-split samples that give a weighted mean age of 2,021 +/- 17 Ma (2 sigma). These are among the youngest mare basalts to be dated thus far by the Ar-40/Ar-39 method and, when combined with most of the published Pb-Pb ages for Chang'e-5 basalts, define a single episode of mare volcanism at similar to 2,021 Ma.
Lunar volcanism provides critical insights into the Moon's thermochemical evolution. We present petrological and geochemical analyses of six very‐low‐Ti (VLT) basalt fragments from Chang'e‐6 (CE6) samples. These basalts yield a Pb‐Pb age of around 2.9 Ga, representing the youngest reported VLT volcanism. They are slightly older than the low‐Ti basalts from the same soils and exhibit distinct pyroxene compositions and 238 U/ 204 Pb ratios, indicating derivation from distinct mantle sources. Compared to Apollo and Luna VLT basalts, these samples share similarly depleted Sr‐Pb isotopes but display elevated rare earth element concentrations and TiO 2 contents. These basalts most likely derived from low‐degree melting of an olivine‐orthopyroxene source followed by 30%–40% fractional crystallization. Further diffusion chronometry reveals rapid magma ascent from magma chamber to surface, likely facilitated by the thin lunar crust resulting from the South Pole‐Aitken basin‐forming impact. Our results provide new insights into the petrogenesis of volcanic activity on the lunar farside.
Orogenic reconstructions typically assume lithostatic pressure, which can be converted into burial depth. Deviations from lithostatic conditions, such as fluid overpressure, are recognized but poorly understood in natural rocks. Here we integrate petrological analysis, radiometric dating, and diffusion chronology to explore the thermal overprinting on metapelites from a Precambrian orogen caused by ca. 110 Ma porphyritic intrusions in Northern Korea. The dissolution-reprecipitation textures of garnet and monazite from the metapelites reveal rapid heating, dehydration, and reworking within similar to 300 years, reaching 600-640 degrees C and 0.75-0.85 GPa at ca. 110 Ma. The barometric results indicate depths that, if lithostatic, sharply contrast with the shallow emplacement of the contemporaneous porphyries nearby, indicating dehydration-induced supralithostatic fluid overpressure. These findings challenge the lithostatic paradigm and suggest that rapid dehydration and deviation from lithostatic pressures may be more prevalent than previously recognized, with important implications for orogenic reconstructions and seismogenic behaviors at plate boundaries.
A new gem‐quality zircon reference material, S513, was developed for in situ microbeam U‐Th‐Pb, (U‐Th)/He geochronology and Hf‐O isotope measurement. The well‐cut gem‐quality zircon weighed 51.3 carats. Its U, Th, Pb and Hf mass fractions were 924 ± 64.6 μg g −1 (2 s ), 89.6 ± 3.92 μg g −1 (2 s ), 119 ± 5.20 μg g −1 (2 s ) and 8259 ± 244 μg g −1 (2 s ), respectively. Imaging results from LA‐ICP‐ToF‐MS analysis showed homogeneous distribution of elements in S513. The Th‐corrected weighted mean 206 Pb/ 238 U, 207 Pb/ 235 U and 207 Pb/ 206 Pb ratios of S513 zircon from eight ID‐TIMS analyses are 0.090955 ± 0.000019 (2 s , MSWD = 0.22, n = 8), 0.73873 ± 0.00023 (2 s , MSWD = 0.19, n = 8) and 0.058934 ± 0.000008 (2 s , MSWD = 0.35, n = 8), respectively. The Th‐corrected weighted mean 206 Pb/ 238 U age obtained from chemical abrasion‐isotope dilution‐thermal ionisation mass spectrometry is 561.18 ± 0.63 Ma ( n = 8, 95% conf., MSWD = 0.9), which is recommended as the best age estimate of S513. The weighted mean 206 Pb/ 238 U ages obtained from in situ microbeam analysis (i.e., LA‐ICP‐MS and SIMS) were 560.8 ± 5.8/10.2 Ma (2 s , n = 260) and 562.4 ± 7.2/13.4 Ma (2 s , n = 198). The measured weighted mean 208 Pb/ 232 Th age of S513 from LA analyses was 561.3 ± 3.3/11.7 Ma (2 s , n = 86). The U‐Pb and Th‐Pb ages of S513 obtained with in situ methods showed good agreement with the CA‐ID‐TIMS results, respectively. The obtained (U‐Th)/He age of S513 from thirty‐seven aliquots analysed with U‐Th isotope dilution method was 420.3 ± 7.6 Ma (2 s , MSWD = 0.72). The recommended reference value of Hf isotope ratio was 0.281606 ± 0.000010 (2 s , MSWD = 1.4, n = 12) according to the mean 176 Hf/ 177 Hf ratio acquired with solution MC‐ICP‐MS analysis. All the LA analyses yielded a mean 176 Hf/ 177 Hf ratio of 0.281605 ± 0.000008 (2 s , MSWD = 0.53, n = 310), which was consistent with the reference value. Laser fluorination analyses yielded mean δ 18 O values of S513 were 11.71 ± 0.11‰ (2 s , MSWD = 0.25, n = 5). The results obtained with multiple analytical methods show that zircon S513 is homogeneous to 8% (1 s ) or better for contents of Y, Nb, Ce, Gd, heavy REE, Ta, U, Th, Pb and Hf. Additionally, the homogeneity is observed at 0.12‰ (2 s ) for U‐Pb ages, 1.8% (2 s ) for (U‐Th)/He ages, 0.0036% (2 s ) for Hf isotopes, and 0.11‰ (2 s ) for O isotope ratios. Zircon S513 is proposed as a new potential primary calibration or quality control reference material for microbeam U‐Th‐Pb geochronology and Hf‐O isotope measurement.
Jin-Hui Yang (杨进辉)合作论文数Institute of Geology and Geophysics, Chinese Academy of Sciences9