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1.
A new natural zircon reference material SA01 is introduced for U‐Pb geochronology as well as O and Hf isotope geochemistry by microbeam techniques. The zircon megacryst is homogeneous with respect to U‐Pb, O and Hf isotopes based on a large number of measurements by laser ablation‐inductively coupled plasma‐mass spectrometry (LA‐ICP‐MS) and secondary ion mass spectrometry (SIMS). Chemical abrasion isotope dilution thermal ionisation mass spectrometry (CA‐ID‐TIMS) U‐Pb isotopic analyses produced a mean 206Pb/238U age of 535.08 ± 0.32 Ma (2s, n = 10). Results of SIMS and LA‐ICP‐MS analyses on individual shards are consistent with the TIMS ages within uncertainty. The δ18O value determined by laser fluorination is 6.16 ± 0.26‰ (2s, n = 14), and the mean 176Hf/177Hf ratio determined by solution MC‐ICP‐MS is 0.282293 ± 0.000007 (2s, n = 30), which are in good agreement with the statistical mean of microbeam analyses. The megacryst is characterised by significant localised variations in Th/U ratio (0.328–4.269) and Li isotopic ratio (?5.5 to +7.9‰); the latter makes it unsuitable as a lithium isotope reference material.  相似文献   

2.
Two quartz samples of igneous origin, UNIL‐Q1 (Torres del Paine Intrusion, Chile) and BGI‐Q1 (Shandong province, China), were calibrated for their oxygen isotope composition for SIMS measurements. UNIL‐Q1 and BGI‐Q1 were evaluated for homogeneity using SIMS. Their reference δ18O values were determined by CO2 laser fluorination. The average δ18O value found for UNIL‐Q1 is 9.8 ± 0.06‰ and that for BGI‐Q1 is 7.7 ± 0.11‰ (1s). The intermediate measurement precision of SIMS oxygen isotope measurements was 0.32–0.41‰ (2s; UNIL‐Q1) and 0.40–0.48‰ (2s; BGI‐Q1), respectively. While less homogeneous in its oxygen isotope composition, BGI‐Q1 is also suitable for SIMS trace element measurements.  相似文献   

3.
We introduce and propose zircon M257 as a future reference material for the determination of zircon U‐Pb ages by means of secondary ion mass spectrometry. This light brownish, flawless, cut gemstone specimen from Sri Lanka weighed 5.14 g (25.7 carats). Zircon M257 has TIMS‐determined, mean isotopic ratios (2s uncertainties) of 0.09100 ± 0.00003 for 206pb/238U and 0.7392 ± 0.0003 for 207pb/235U. Its 206pb/238U age is 561.3 ± 0.3 Ma (unweighted mean, uncertainty quoted at the 95% confidence level); the U‐Pb system is concordant within uncertainty of decay constants. Zircon M257 contains ～ 840 μg g?1 U (Th/U ～ 0.27). The material exhibits remarkably low heterogeneity, with a virtual absence of any internal textures even in cathodoluminescence images. The uniform, moderate degree of radiation damage (estimated from the expansion of unit‐cell parameters, broadening of Raman spectral parameters and density) corresponds well, within the “Sri Lankan trends”, with actinide concentrations, U‐Pb age, and the calculated alpha fluence of 1.66 × 1018 g?1. This, and a (U+Th)/He age of 419 ± 9 Ma (2s), enables us to exclude any unusual thermal history or heat treatment, which could potentially have affected the retention of radiogenic Pb. The oxygen isotope ratio of this zircon is 13.9%o VSMOW suggesting a metamorphic genesis in a marble or calc‐silicate skarn.  相似文献   

4.
This study is Part II of a series that documents the development of a suite of calibration reference materials for in situ SIMS analysis of stable isotope ratios in Ca‐Mg‐Fe carbonates. Part I explored the effects of Fe2+ substitution on SIMS δ18O bias measured from the dolomite–ankerite solid solution series [CaMg(CO3)2–CaFe(CO3)2], whereas this complementary work explores the compositional dependence of SIMS δ13C bias (calibrated range: Fe# = 0.004–0.789, where Fe# = molar Fe/(Mg+Fe)). Under routine operating conditions for carbonate δ13C analysis at WiscSIMS (CAMECA IMS 1280), the magnitude of instrumental bias increased exponentially by 2.5–5.5‰ (session‐specific) with increasing Fe‐content in the dolomite structure, but appeared insensitive to minor Mn substitution [< 2.6 mole % Mn/(Ca+Mg+Fe+Mn)]. The compositional dependence of bias (i.e., the matrix effect) was expressed using the Hill equation, yielding calibration residual values ≤ 0.3‰ relative to CRM NBS‐19 for eleven carbonate reference materials (6‐μm‐diameter spot size measurements). Based on the spot‐to‐spot repeatability of a drift monitor material that ‘bracketed’ each set of ten sample‐spot analyses, the analytical precision was ± 0.6–1.2‰ (2s, standard deviations). The analytical uncertainty for individual sample analyses was approximated by combining the precision and calibration residual values (propagated in quadrature), suggesting an uncertainty of ± 1.0–1.5‰ (2s).  相似文献   

5.
We introduce a potential new working reference material – natural zircon megacrysts from an Early Pliocene alkaline basalt (from Penglai, northern Hainan Island, southern China) – for the microbeam determination of O and Hf isotopes, and U–Pb age dating. The Penglai zircon megacrysts were found to be fairly homogeneous in Hf and O isotopes based on large numbers of measurements by LA-multiple collector (MC)-ICP-MS and SIMS, respectively. Precise determinations of O isotopes by isotope ratio mass spectrometry (IRMS) and Hf isotopes by solution MC-ICP-MS were in good agreement with the statistical mean of microbeam measurements. The mean δ18O value of 5.31 ± 0.10‰ (2s) by IRMS and the mean 176Hf/177Hf value of 0.282906 ± 0.0000010 (2s) by solution MC-ICP-MS are the best reference values for the Penglai zircons. SIMS and isotope dilution-TIMS measurements yielded consistent 206Pb/238U ages within analytical uncertainties, and the preferred 206Pb/238U age was found to be 4.4 ± 0.1 Ma (95% confidence interval). The young age and variably high common Pb content make the Penglai zircons unsuitable as a primary U–Pb age reference material for calibration of unknown samples by microbeam analysis; however, they can be used as a secondary working reference material for quality control of U–Pb age determination for young (particularly < 10 Ma) zircon samples.  相似文献   

6.
Precision and accuracy in SIMS zircon geochronology strongly depend on the method of determination of the interelement ion ratios (e.g., 206Pb/238U) from the measured secondary ion ratios (206Pb+/238U+). Six possible U–Pb calibrations (Pb/U–UO2/U, Pb/U–UO/U, Pb/U–UO2/UO, Pb/UO–UO2/U, Pb/UO–UO/U, Pb/UO–UO2/UO) based on simple power law relationships, and Pb/UO2‐related one‐ and two‐ (a power law) dimensional ones were compared using data acquired on the 91500 zircon reference material from one hundred measurement sessions, to determine the most statistically reliable scheme. Taking advantage of U oxide species (UO and UO2) over atomic U, due to their similar energy distribution to Pb and higher intensities, the data calibrated with Pb/UO–UO2/UO showed the smallest mean uncertainties and dispersions, and provided the best‐fit calibration curve consistently. Although it was demonstrated with Temora 2 that the unknown zircon age was not changed significantly by different calibrations, its precision could be improved using the Pb/UO–UO2/UO calibration in zircon geochronology.  相似文献   

7.
A potential zircon reference material (BB zircon) for laser ablation‐inductively coupled plasma‐mass spectrometry (LA‐ICP‐MS) U‐Pb geochronology and Hf isotope geochemistry is described. A batch of twenty zircon megacrysts (0.5–1.5 cm3) from Sri Lanka was studied. Within‐grain rare earth element (REE) compositions are largely homogeneous, albeit with some variation seen between fractured and homogeneous domains. Excluding fractured cathodoluminescence bright domains, the variation in U content for all analysed crystals ranged from 227 to 368 μg g?1 and the average Th/U ratios were between 0.20 and 0.47. The Hf isotope composition (0.56–0.84 g/100 g Hf) is homogeneous within and between the grains – mean 176Hf/177Hf of 0.281674 ± 0.000018 (2s). The calculated alpha dose of 0.59 × 1018 g?1 for a number of BB grains falls within the trend of previously studied, untreated zircon samples from Sri Lanka. Aliquots of the same crystal (analysed by ID‐TIMS in four different laboratories) gave consistent U‐Pb ages with excellent measurement reproducibility (0.1–0.4% RSD). Interlaboratory assessment (by LA‐ICP‐MS) from individual crystals returned results that are within uncertainty equivalent to the TIMS ages. Finally, we report on within‐ and between‐grain homogeneity of the oxygen isotope systematic of four BB crystals (13.16‰ VSMOW).  相似文献   

8.
We present multitechnique U‐Pb geochronology and Hf isotopic data from zircon separated from rapakivi biotite granite within the Eocene Golden Horn batholith in Washington, USA. A weighted mean of twenty‐five Th‐corrected 206Pb/238U zircon dates produced at two independent laboratories using chemical abrasion‐isotope dilution‐thermal ionisation mass spectrometry (CA‐ID‐TIMS) is 48.106 ± 0.023 Ma (2s analytical including tracer uncertainties, MSWD = 1.53) and is our recommended date for GHR1 zircon. Microbeam 206Pb/238U dates from laser ablation‐inductively coupled plasma‐mass spectrometry (LA‐ICP‐MS) and secondary ion mass spectrometry (SIMS) laboratories are reproducible and in agreement with the CA‐ID‐TIMS date to within < 1.5%. Solution multi‐collector ICP‐MS (MC‐ICP‐MS) measurements of Hf isotopes from chemically purified aliquots of GHR1 yield a mean 176Hf/177Hf of 0.283050 ± 17 (2s, n = 10), corresponding to a εHf0 of +9.3. Hafnium isotopic measurements from two LA‐ICP‐MS laboratories are in agreement with the solution MC‐ICP‐MS value. The reproducibility of 206Pb/238U and 176Hf/177Hf ratios from GHR1 zircon across a variety of measurement techniques demonstrates their homogeneity in most grains. Additionally, the effectively limitless reserves of GHR1 material from an accessible exposure suggest that GHR1 can provide a useful reference material for U‐Pb geochronology of Cenozoic zircon and Hf isotopic measurements of zircon with radiogenic 176Hf/177Hf.  相似文献   

9.
Garnet–clinopyroxene ultra‐high‐pressure (UHP) rocks from the northern Bohemian Massif contain zircon with micro‐diamond inclusions. Trace element concentrations, oxygen and hafnium isotopic composition and U–Pb age of distinct textural domains in zircon characterize their growth conditions and temporal evolution. Diamond‐bearing zircon mantle domains with relicts of oscillatory zoning have uniform Th/U ratios (~0.1–0.2), high‐Ti contents (110–190 ppm, corresponding to temperatures of at least 1100 °C), and some (two of 17 mantle analyses) preserve steep heavy rare earth element (HREE) patterns with YbN/GdN = 10–11, with a weak negative Eu anomaly. These signatures are consistent with crystallization from a melt under UHP/ultra‐high‐temperature (UHT) conditions. Some of the bright‐cathodoluminscence (CL) rims preserve Th/U and Ti values characteristic of the zircon mantles, but others show elevated Th/U ratios of ~0.3–0.4 and lower Ti contents (20–40 ppm; only 13 ppm in a rare low‐CL outer rim). As they feature flat HREE patterns and negative Eu anomalies and commonly make embayments and truncate the mantle zoning, we suggest that they have formed through recrystallization in the solid state during exhumation of the rock, when both garnet and plagioclase were stable. The three zircon domains, that is, cores, mantles and rims, yield U–Pb concordia ages of 340.9 ± 1.5, 340.3 ± 1.5 and 341.2 ± 3.4 Ma respectively. When linked to the previously reconstructed P–T path of the rock, the error limits of the zircon mantle and rim ages constrain the exhumation of the rocks from depth of ~140 km (UHP) to ~80 km (HP) to a minimum rate of 1.5 cm yr?1. The zircon cores are heterogeneous in terms of Th/U ratio (below 0.1 but also above 0.2) and REE characteristics, and their εHf values scatter between ?15.7 and +4.8 with similar values for individual domains within a single zircon grain suggesting a very localized control on hafnium isotope composition on a grain scale. The non‐equilibrated εHf values as well as a large range of the Hf‐depleted mantle model ages possibly reflect the presence of a heterogeneous population of old zircon. Consequently, the uniform and young 238U/206Pb ages may represent (near‐)complete resetting of the U–Pb geochronometer during the UHP–UHT event at c. 340 Ma through dissolution–reprecipitation process. In contrast to Hf, the oxygen isotope composition of zircon is homogeneous, ranging between 7.8‰ and 9.6‰ VSMOW, reflecting a source containing upper crustal material and homogenization at UHP–UHT conditions. Our study documents that continental crust was subducted to mantle depths at c. 340 Ma during the Variscan orogeny and was subsequently very rapidly exhumed, implying that the sequence of events was faster than can be resolved by the secondary ion mass spectrometry technique.  相似文献   

10.
Inter‐laboratory comparison of laser ablation ICP‐MS and SIMS U‐Pb dating of synthetic detrital zircon samples provides an insight into the state‐of‐the art of sedimentary provenance studies. Here, we report results obtained from ten laboratories that routinely perform this type of work. The achieved level of bias was mostly within ± 2% relative to the ID‐TIMS U‐Pb ages of zircons in the detrital sample, and the variation is likely to be attributed to variable Pb/U elemental fractionation due to zircon matrix differences between the samples and the reference materials used for standardisation. It has been determined that ~ 5% age difference between adjacent age peaks is currently at the limit of what can be routinely resolved by the in situ dating of detrital zircon samples. Precision of individual zircon age determination mostly reflects the data reduction and procedures of measurement uncertainty propagation, and it is largely independent of the instrumentation, analytical technique and reference samples used for standardisation. All laboratories showed a bias towards selection of larger zircon grains for analysis. The experiment confirms the previously published estimates of the minimum number of grains that have to be analysed in order to detect minor zircon age populations in detrital samples.  相似文献   

11.
Most monazite reference materials (RMs) for in situ U‐Pb geochronology are rich in Th; however, many hydrothermal ore deposits contain monazite that is low in trace element contents, including Th, U and Pb. Because of potential problems with matrix effects and the lack of appropriate matrix‐matched RMs, such variations can bias dating of hydrothermal deposits. In this paper, we describe a polycrystalline low‐U and low‐Th Diamantina monazite from the Espinhaço Range, SE Brazil. It has a U‐Pb ID‐TIMS weighted mean 207Pb*/235U ratio of 0.62913 ± 0.00079, 206Pb*/238U of 0.079861 ± 0.000088 and 207Pb*/206Pb* of 0.057130 ± 0.000031, yielding a weighted mean 206Pb*/238U date of 495.26 ± 0.54 Ma (95% c.l.). In situ dates acquired with different methods (LA‐(Q, SF, MC)‐ICP‐MS and SIMS) are within uncertainty of the ID‐TIMS data. U‐Pb LA‐(Q, MC)‐ICP‐MS runs, using Diamantina as a primary RM, reproduced the ages of other established RMs within < 1% deviation. The LA‐MC‐ICP‐MS analyses yielded homogeneous Sm‐Nd isotopic compositions (143Nd/144Nd = 0.511427 ± 23, 2s; 147Sm/144Nd = 0.1177 ± 13, 2s) and εNd(495 Ma) of ?18.7 ± 0.5 (2s). SIMS oxygen isotope determinations showed measurement reproducibility better than ± 0.3‰ (2s), confirming Diamantina's relative homogeneity at test portion masses below 1 ng.  相似文献   

12.
We document the development of a suite of carbonate mineral reference materials for calibrating SIMS determinations of δ18O in samples with compositions along the dolomite–ankerite solid solution series [CaMg(CO3)2–CaFe(CO3)2]. Under routine operating conditions for the analysis of carbonates for δ18O with a CAMECA IMS 1280 instrument (at WiscSIMS, University of Wisconsin‐Madison), the magnitude of instrumental bias along the dolomite–ankerite series decreased exponentially by ~ 10‰ with increasing Fe content in the dolomite structure, but appeared insensitive to minor Mn substitution [< 2.6 mol% Mn/(Ca+Mg+Fe+Mn)]. The compositional dependence of bias (i.e., the sample matrix effect) was calibrated using the Hill equation, which relates bias to the Fe# of dolomite–ankerite [i.e., molar Fe/(Mg+Fe)] for thirteen reference materials (Fe# = 0.004–0.789); for calibrations employing either 10 or 3 μm diameter spot size measurements, this yielded residual values ≤ 0.3–0.4‰ relative to CRM NBS 19 for most reference materials in the suite. Analytical precision was ± 0.3‰ (2s, standard deviations) for 10‐μm spots and ± 0.7‰ (2s) for 3‐μm spots, based on the spot‐to‐spot repeatability of a drift monitor material that ‘bracketed’ each set of ten sample‐spot analyses. Analytical uncertainty for individual sample analyses was approximated by a combination of precision and calibration residual values (propagated in quadrature), suggesting an uncertainty of ± 0.5‰ (2s) for 10‐μm spots and ± 1‰ (2s) for 3‐μm spots.  相似文献   

13.
Hornblende from the Lone Grove Pluton, Llano Uplift, Texas, has served as an irradiation reference material in 40Ar/39Ar studies for decades. In order to evaluate the apparent age bias that currently exists between the U‐Pb and 40Ar/39Ar systems, zircon and titanite were dated by isotope dilution‐thermal ionisation mass spectrometry (ID‐TIMS) from the same rock from which the hornblende 40Ar/39Ar reference material HB3gr is derived. Zircon U‐Pb data indicate initial crystallisation at 1090.10 ± 0.16 Ma (2s), a date that is 1.7% older than the accepted K‐Ar date (1072 ± 14 Ma, 2s) for HB3gr; an offset that exceeds the typical 0.5–1% bias between the two systems, though remaining within uncertainty due to the large uncertainties in the 40K decay constant. Zircon data are presented using both EARTHTIME tracers ET535 and ET2535 and are statistically indistinguishable. Single grain titanite analyses range between 1082 ± 0.75 and 1086 ± 0.81 Ma (2s) and are interpreted to record the subsequent cooling following crystallisation at rates between 30 and 50 °C Ma?1. This is supported by the observation that hornblende 40Ar/39Ar dates corrected for decay constant bias are resolvably younger than the zircon U‐Pb date and in good agreement with titanite U‐Pb dates, permitting the conclusion that both titanite U‐Pb and hornblende 40Ar/39Ar systems provide a record of cooling.  相似文献   

14.
Fluid plays a key role in metamorphism and magmatism in subduction zones. Veins in high‐pressure (HP) to ultrahigh‐pressure (UHP) rocks are the products of fluid‐rock interaction, and can thus provide important constraints on fluid processes in subduction zones. This contribution is an integrated study of zircon U–Pb and O–Hf, as well as whole‐rock Nd–Sr isotopic compositions for a quartz vein, a complex vein, and their host eclogite in the Sulu UHP terrane to decipher the timing and source of fluid flow under HP‐UHP metamorphic conditions. The inherited magmatic zircon cores from the host eclogite constrain the protolith age at c. 750 Ma. Their variable εHf(t) values from ?1.11 to 2.54 and low δ18O values of 0.32–3.40‰ reflect a protolith that formed in a rift setting due to the breakup of the supercontinent Rodinia. The hydrothermal zircon from the quartz and the complex veins shows euhedral shapes, relatively flat HREE pattern, slight or no negative Eu anomaly, low 176Lu/177Hf ratios, and low formation temperatures of 660–690 °C, indicating they precipitated from fluids under HP eclogite facies conditions. This zircon yielded similar U–Pb ages of 217 ± 2 and 213 ± 3 Ma within analytical uncertainty, recording the timing of fluid flow during the exhumation of the UHP rock. It is inferred that the fluids might be of internal origin based on the homogeneity of δ18O values of the hydrothermal zircon from the quartz (?2.41 ± 0.13‰) and complex veins (?2.35 ± 0.12‰), and the metamorphic grown zircon of the host eclogite (?2.23 ± 0.16‰). The similar εNd(t) values of the whole rocks also support such a point. Zircon O and whole‐rock Nd isotopic compositions are therefore useful to identify the source of fluid, for they are major and trace components in minerals involved in metamorphic reactions during HP‐UHP conditions. On the other hand, the hydrothermal zircon from the veins and the metamorphic zircon from the host eclogite exhibit variable εHf(t) values. Model calculation suggests that the Hf was derived from the breakdown of major rock‐forming minerals and recycling of the inherited magmatic zircon. The variable whole‐rock initial 87Sr/86Sr ratios might be caused by subsequent retrograde metamorphism after the formation of the veins.  相似文献   

15.
In situ U-Pb geochronology and hafnium, oxygen and zirconium isotope measurements in zircons using laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) and ion microprobe techniques can provide essential isotopic data to constrain geological evolutionary histories. Developing reliable zircon reference materials is the cornerstone for in situ zircon chronology and isotopic studies. In this study, the homogeneity of U-Pb ages and Hf-O-Zr isotope ratios in three Sri Lankan zircon megacrysts (SLZA, SLZB and SLZC) were investigated using multiple analytical methods. The obtained U, Th, Pb and Hf mass fractions of the SLZA zircon were 839 ± 56 μg g-1 (1s), 151 ± 15 μg g-1 (1s), 198 ± 28 μg g-1 (1s) and 8635 ± 286 μg g-1 (1s), respectively. The mass fractions of U, Th, Pb and Hf in the SLZB zircon were 1106 ± 106 μg g-1 (1s), 331 ± 61 μg g-1 (1s), 376 ± 57 μg g-1 (1s) and 9673 ± 976 μg g-1 (1s), respectively. The U, Th, Pb and Hf mass fractions determined in the SLZC zircon were 551 ± 35 μg g-1 (1s), 111 ± 8 μg g-1 (1s), 129 ± 18 μg g-1 (1s) and 7881 ± 393 μg g-1 (1s), respectively. The chemical abrasion isotope dilution thermal ionisation mass-spectrometry (CA-ID-TIMS) method yielded a Th-corrected weighted mean 206Pb/238U age of 556.94 ± 1.29 Ma (95% conf., n = 5) for the SLZA zircon, 552.90 ± 1.29 Ma (95% conf., n = 7) for the SLZB zircon and 560.83 ± 1.29 Ma (95% conf., n = 7) for the SLZC zircon. The obtained Hf isotopic compositions of the SLZA, SLZB and SLZC zircons determined with the solution MC-ICP-MS method were 0.281651 ± 0.000014 (2s, n = 10), 0.281704 ± 0.000008 (2s, n = 10) and 0.281676 ± 0.000006 (2s, n = 10), respectively. The obtained O isotopes of the SLZA and SLZB zircons measured with the laser fluorination method were 12.14 ± 0.56‰ (2s, n = 4) and 11.91 ± 0.30‰ (2s, n = 4), respectively. The Zr isotopes of the SLZA, SLZB and SLZC zircons determined with double spike TIMS analysis yielded mean δ94/90ZrSRM3169 values of -0.03 ± 0.06‰ (2s, n = 10), -0.03 ± 0.04‰ (2s, n = 10) and 0.00 ± 0.07‰ (2s, n = 8), respectively. The SLZA zircon can be used as a primary reference or quality control material for microbeam U-Pb, Hf and Zr isotope measurements because of its slight heterogeneity. The U-Pb, Hf and Zr isotopic compositions of the SLZB and SLZC megacrysts were homogeneous. The O isotopic compositions in the SLZA and SLZB zircon were slightly dispersed, indicating that these two megacrysts can only serve as secondary reference materials for microbeam O isotope measurements.  相似文献   

16.
Metatexite and diatexite migmatites are widely distributed within the upper amphibolite and granulite facies zones of the Higo low‐P/high‐T metamorphic terrane. Here, we report data from an outcrop in the highest grade part of the granulite facies zone, in which diatexite occurs as a 3 m thick layer between 2 m thick layers of stromatic‐structured metatexite within pelitic gneiss. The migmatites and gneiss contain the same peak mineral assemblage of biotite + plagioclase + quartz + garnet + K‐feldspar with retrograde chlorite ± muscovite and some accessory minerals of ilmenite ± rutile ± titanite + apatite + zircon + monazite ± pyrite ± zinc sulphide ± calcite. Calculated metamorphic P–T conditions are 800–900 °C and 9–12 kbar. Zircon in the diatexite forms elongate euhedral crystals with oscillatory zoning, but no core–rim structure. Zircon from the gneiss and metatexite forms euhedral–subhedral grains comprising inherited cores overgrown by thin rims. The overgrowth rims in the metatexite have lower Th/U ratios than zircon in the diatexite and yield a 206Pb/238U age of 116.0 ± 1.6 Ma, which is older than the 110.1 ± 0.6 Ma 206Pb/238U age derived from zircon in the diatexite. Zircon from the diatexite has variable REE contents with convex upward patterns and flat normalized HREE, whereas the overgrowth rims in the metatexite and gneiss have steep HREE‐enriched patterns; however, both types have similar positive Ce and negative Eu anomalies. 176Hf/177Hf ratios in the overgrowth rims from the metatexite are more variable and generally lower than values from zircon in the diatexite. Based on U–Pb ages, trace element and Hf isotope data, the zircon rims in the metatexite are interpreted to have crystallized from a locally derived melt, following partial dissolution of inherited protolith zircon during anatexis, whereas the zircon in the diatexite is interpreted to have crystallized from a melt that included an externally derived component. By integrating zircon and petrographic data for the migmatites and pelitic gneiss, the metatexite migmatite is interpreted to have formed by in situ partial melting in which the melt did not migrate from the source, whereas the diatexite migmatite included an externally derived juvenile component. The Cretaceous high‐temperature metamorphism of the Higo metamorphic terrane is interpreted to reflect emplacement of mantle‐derived basalts under a volcanic arc along the eastern margin of the Eurasian continent and advection of heat via hybrid silicic melts from the lower crust. Post‐peak crystallization of anatectic melts in a high‐T region at mid‐crustal depths occurred in the interval c. 116–110 Ma, as indicated by the difference in zircon ages from the metatexite and diatexite migmatites.  相似文献   

17.
We report technical and data treatment methods for making accurate, high‐precision measurements of 18O/16O in Ca–Mg–Fe garnet utilising the Cameca IMS 1280 multi‐collector ion microprobe. Matrix effects were similar to those shown by previous work, whereby Ca abundance is correlated with instrumental mass fractionation (IMF). After correction for this effect, there appeared to be no significant secondary effect associated with Mg/Fe2+ for routine operational conditions. In contrast, investigation of the IMF associated with Mn‐ or Cr‐rich garnet showed that these substitutions are significant and require a more complex calibration scheme. The Ca‐related calibration applied to low‐Cr, low‐Mn garnet was reproducible across different sample mounts and under a range of instrument settings and therefore should be applicable to similar instruments of this type. The repeatability of the measurements was often better than ± 0.2‰ (2s), a precision that is similar to the repeatability of bulk techniques. At this precision, the uncertainties due to spot‐to‐spot repeatability were at the same magnitude as those associated with matrix corrections (± 0.1–0.3‰) and the uncertainties in reference materials (± 0.1–0.2‰). Therefore, it is necessary to accurately estimate and propagate uncertainties associated with these parameters – in some cases, uncertainties in reference materials or matrix corrections dominate the uncertainty budget.  相似文献   

18.
Ice core from Greenland was melted, filtered, homogenised, loaded into glass ampoules, sealed, autoclaved to eliminate biological activity, and calibrated by dual‐inlet isotope‐ratio mass spectrometry. This isotopic reference material (RM), USGS46, is intended as one of two secondary isotopic reference waters for daily normalisation of stable hydrogen (δ2H) and stable oxygen (δ18O) isotopic analysis of water with a mass spectrometer or a laser absorption spectrometer. The measured δ2H and δ18O values of this reference water were ?235.8 ± 0.7‰ and ?29.80 ± 0.03‰, respectively, relative to VSMOW on scales normalised such that the δ2H and δ18O values of SLAP reference water are, respectively, ?428 and ?55.5‰. Each uncertainty is an estimated expanded uncertainty (U = 2uc) about the reference value that provides an interval that has about a 95‐percent probability of encompassing the true value. This reference water is available in cases containing 144 glass ampoules that are filled with either 4 ml or 5 ml of water per ampoule.  相似文献   

19.
Laser ablation‐inductively coupled plasma‐mass spectrometry (LA‐ICP‐MS) was examined as a tool for measuring isotopic variation as a function of ablation depth in unpolished zircon from an Archaean metasediment specimen. This technique was able to identify micrometre‐thin (> 3 μm) isotopically distinct mineral domains characterised by ca. 100 Myr younger 207Pb/206Pb ages associated with 2s age uncertainties as low ~ 0.2%, as well as elevated U content relative to grain interiors (up to an order of magnitude). Our calculated drilling rate suggests that each laser pulse excavated depths of ~ 0.06 μm. Ages resolved through the LA‐ICP‐MS methods overlap the 2s uncertainties of 207Pb/206Pb ages measured using SIMS depth profiling on the same zircon population. The rims were further evinced by the detection of relative enrichment (> 3 orders of magnitude) in REE in the outermost micrometres of the same zircon, measured using a different and independent LA‐ICP‐MS depth profiling technique. We propose a LA‐ICP‐MS U–Pb technique capable of quickly identifying and quantifying rims, which are indication of late, yet geologically significant, fluid events that are otherwise undefined.  相似文献   

20.
We report Hf isotope data for 3467 Ma igneous zircons from the Owens Gully Diorite of the Pilbara Craton. These zircons, designated OG1 or OGC, have simple, well‐defined U‐Pb age systematics. Measurements obtained by single crystal dissolution yield a moderate range in 176Hf/177Hf (mean 0.280633 ± 34) and 176Lu/177Hf (mean 0.00119) that translate into initial (3467 Ma) 176Hf/177Hf values that are equivalent within measurement uncertainty (mean 0.280554 ± 7, εHf = +0.6 ± 0.2, 2s). Laser ablation analysis yielded clustered initial 176Hf/177Hf ratios (mean 0.280560 ± 20, 2s) indistinguishable from those obtained by solution analysis. The antiquity and moderately high 176Lu/177Hf of these zircons result in significant corrections for radiogenic ingrowth of 176Hf (to 6 εHf units). Depth profiling by concurrent Pb‐Hf isotope determination reveals trends to lower 207Pb/206Pb in several crystals, although these are not accompanied by shifts in 176Hf/177Hf. We conclude that zircons from the Owens Gully Diorite are homogeneous for Hf isotopes at the scale of sampling and within the uncertainty limits of the measurement techniques employed. Zircon OG1/OGC would appear to be an ideal quality monitor for laser ablation Hf isotope determination in ancient zircons, and for laser ablation techniques where Hf isotope and age information are determined concurrently or simultaneously.  相似文献   

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