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1.
This study describes two methods (Procedures‐1 and ‐2) for the direct extraction of Au by an inorganic acid mixture (HClO4‐HBr‐HI‐aqua regia) from complex sample matrices. Standard PTFE jars at 200 °C were used to decompose test portions of 0.5–1 g, with subsequent precise and accurate analysis by ICP‐MS without any other preconcentration or separation. Procedure‐1 decomposed samples effectively without the necessity of leaching with HF and was developed for dust samples from e‐waste (electronic waste) processing; however, testing on geological reference materials showed very good results. The analyses of replicate decompositions (n = 5) from both procedures yielded very good precision (< 5% RSD) for most of the reference materials. The accuracy achieved was better than ± 10%, with the exception of NIST SRM 2782 data from Procedure‐1. Two unknown samples of dust from e‐waste processing (P‐1 and VM‐1) exhibited elevated concentrations of Au (21.31–61.64 μg g?1) with precision better than 10% (n = 5). The proposed techniques are simple, sensitive and sparing in the use of chemicals, and are designed for a variety of e‐waste dust samples. No significant influences were observed for the predicted spectral interferences on mass 197Au.  相似文献   

2.
A simple, rapid method for the determination of Re and Os concentrations and isotope compositions using isotope dilution multi‐collector inductively coupled plasma‐mass spectrometry (ID‐MC‐ICP‐MS) combined with Carius tube digestion and sparging introduction of Os was developed. For Os measurement, four channeltron ion counters to detect different Os isotopes were used simultaneously, which led to a drastic reduction in the measurement time. Rhenium isotopes were measured by means of eight Faraday cups with solution nebulisation and an ultrasonic membrane desolvator. The representative 188Os count rate of an Os standard solution containing 50 pg of total Os was approximately 110000–120000 cps at the onset of measurement; the Re intensity of our in‐house 10 pg g?1 standard solution reached 1820 V/μg g?1 with a sample uptake rate of 95–99 μl min?1. These values indicate that the sensitivity of the method was sufficient even for samples with low Re and Os concentrations, such as chert. As the temporal variations of the amplification efficiency of the ion counters differed from one another, we adopted a sample‐calibrator bracketing method to correct the measured Re and Os isotope ratios. The Re and Os concentrations via the isotope dilution method and the 187Os/188Os ratios of two sedimentary rock reference materials (JMS‐2 and JCh‐1) on the basis of the isotope ratios determined by the MC‐ICP‐MS and by negative thermal ionisation mass spectrometry (N‐TIMS) were comparable within their ranges. Based on Os isotope measurement of the IAG reference material [Durham Romil Os (DROsS)], the average difference from the recommended value and precision of Os isotope measurements by the sparging method in combination with multi‐ion‐counters were 0.72% and 0.76% [1RSD (%), n = 29], respectively. The precisions in the 187Os/188Os ratios [1RSD (%)] of JMS‐2, JCh‐1 and DROsS were 0.35–0.71, 1.56–3.31 and 0.99–1.28%, respectively, which depended on their Os ion intensities. No systematic difference was observed between the Re and Os geochemical compositions of JCh‐1 and JMS‐2 obtained by means of digestion with inverse aqua regia and CrO3‐H2SO4 solutions, suggesting that either acid solution can be used for the sparging method of sedimentary rock samples. As CrO3‐H2SO4 solution is believed to liberate predominantly the hydrogenous Re and Os fraction from organic‐rich sediment, the sparging method combined with CrO3‐H2SO4 digestion and multi‐ion‐counters in the mass spectrometry is expected to be a powerful tool for reconstructing the secular change in marine Os isotope compositions with high sample throughput.  相似文献   

3.
A method for the determination of total sulfur in geological materials by inductively coupled plasma‐optical emission spectrometry (ICP‐OES) is described. We show that good results were obtained using this method even for sample types with very low (< 20 μg g?1) sulfur concentration (e.g., peridotite). Sulfur was determined in fifteen geological reference materials with different sulfur contents. For reference materials with certified sulfur contents, the ICP‐OES method gave results in excellent agreement with certified values, and uncertainties better than 4% RSD. ICP‐OES results for sulfur in other reference materials yielded RSDs better than 10%, where S concentrations were > 100 μg g?1 (except for diabase W‐2a, 16% RSD). Reference materials with lower sulfur contents (< 40 μg g?1) showed much higher RSDs (17–18%). Except for RMs with certified values for sulfur, most data obtained by the combustion infrared detection method generally showed higher concentrations than those measured by ICP‐OES and a better RSD (≤ 8% for all materials except DTS‐2b).  相似文献   

4.
We report homogeneity tests on large natural apatite crystals to evaluate their potential as U reference materials for apatite fission‐track (AFT) thermochronology by laser ablation‐inductively coupled plasma‐mass spectrometry (LA‐ICP‐MS). The homogeneity tests include the measurements of major element concentrations by electron probe microanalysis (EPMA), whereas for U concentration, isotope dilution (ID) ICP‐MS and laser ablation (LA) ICP‐MS were employed. Two apatite crystals are potential reference materials for LA‐ICP‐MS analysis: a 1 cm3 fraction of a Durango crystal (7.5 μg g?1 U) and a 1 cm3 Mud Tank crystal (6.9 μg g?1 U). The relative standard deviation (1 RSD) of the U concentration determined by ID‐ICP‐MS of both apatite crystals was ≤ 1.5%, whereas 1 RSD for the LA‐ICP‐MS results was better than 4%, providing sufficient homogeneity for fission‐track dating. The results on the U homogeneity for two different apatite samples are an important step towards establishing in situ dating routines for AFT analysis by LA‐ICP‐MS.  相似文献   

5.
A specific method for the determination of bromine and iodine species in drinking water was developed by using high performance liquid chromatography‐ICP‐MS. An ICS‐A23 ion chromatography column was chosen for the separation of species, with the mobile phase being 0.03 mol l?1 ammonium carbonate at a flow rate of 0.8 ml min?1. The detection limits for BrO3?, Br?, IO3? and I? were 0.032, 0.063, 0.008 and 0.012 μg l?1, respectively. Spectroscopic interferences were only observed in blank samples and mainly resulted from the argon‐potassium polyatomic ion (40Ar39K+). However, this interference was negligible because of the elution and complete separation from that of iodinate under optimised conditions. The method developed was successfully applied to twenty‐two samples of drinking water obtained from a supermarket. Results indicated that 36.4% of the samples had BrO3? concentrations exceeding the Chinese national limit for drinking water of 10 μg l?1.  相似文献   

6.
A HF‐free sample preparation method was used to purify silicon in twelve geological RMs. Silicon isotope compositions were determined using a Neptune instrument multi‐collector‐ICP‐MS in high‐resolution mode, which allowed separation of the silicon isotope plateaus from their interferences. A 1 μg g‐1 Mg spike was added to each sample and standard solution for online mass bias drift correction. δ30Si and δ29Si values are expressed in per mil (‰), relative to the NIST SRM 8546 (NBS‐28) international isotopic RM. The total variation of δ30Si in the geological reference samples analysed in this study ranged from ‐0.13‰ to ‐0.29‰. Comparison with δ29Si values shows that these isotopic fractionations were mass dependent. IRMM‐17 yielded a δ30Si value of ‐1.41 ± 0.07‰ (2s, n = 12) in agreement with previous data. The long‐term reproducibility for natural samples obtained on BHVO‐2 yielded δ30Si = ‐0.27 ± 0.08‰ (2s, n = 42) on a 12 month time scale. An in‐house Si reference sample was produced to check for the long‐term reproducibility of a mono‐elemental sample solution; this yielded a comparable uncertainty of ± 0.07‰ (2s, n = 24) over 5 months.  相似文献   

7.
An in situ, medium‐resolution LA‐ICP‐MS method was developed to measure the abundances of the first‐row transition metals, Ga and Ge in a suite of geological materials, namely the MPI‐DING reference glasses. The analytical protocol established here hinged on maximising the ablation rate of the ultraviolet (UV) laser system and the sensitivity of the ICP‐MS, as well minimising the production of diatomic oxides and argides, which serve as the dominant sources of isobaric interferences. Non‐spectral matrix effects were accounted for by using multiple external calibrators, including NIST SRM 610 and the USGS basaltic glasses BHVO‐2G, BIR‐1G and BCR‐2G, and utilising 43Ca as an internal standard. Analyses of the MPI‐DING reference glasses, which represent geological matrices ranging from basaltic to rhyolitic in composition, included measurements of concentrations as low as < 100 μg g?1 and as high as > 104 μg g?1. The new data reported here were found to statistically correlate with the ‘preferred’ reference values for these materials at the 95% confidence level, though with significantly better precision, typically on the order of ≤ 3% (2sm). This analytical method may be extended to any matrix‐matched geological sample, particularly oceanic basalts, silicate minerals and meteoritic materials.  相似文献   

8.
The low‐Sr content (generally < 100 μg g?1) in clinopyroxene from peridotite makes accurate Sr isotopic determination by LA‐MC‐ICP‐MS a challenge. The effects of adding N2 to the sample gas and using a guard electrode (GE) on instrumental sensitivity for Sr isotopic determination by LA‐MC‐ICP‐MS were investigated. Results revealed no significant sensitivity enhancement of Sr by adding N2 to the ICP. Although using a GE led to a two‐fold sensitivity enhancement, it significantly increased the yield of polyatomic ion interferences of Ca‐related ions and TiAr+ on Sr isotopes. Applying the method established in this work, 87Sr/86Sr ratios (Rb/Sr < 0.14) of natural clinopyroxene from mantle and silicate glasses were accurately measured with similar measurement repeatability (0.0009–0.00006, 2SE) to previous studies but using a smaller spot size of 120 μm and low‐to‐moderate Sr content (30–518 μg g?1). The measurement reproducibility was 0.0004 (2s, n = 33) for a sample with 100 μg g?1 Sr. Destruction of the crystal structure by sample fusion showed no effect on Sr isotopic determination. Synthesised glasses with major element compositions similar to natural clinopyroxene have the potential to be adopted as reference materials for Sr isotopic determination by LA‐MC‐ICP‐MS.  相似文献   

9.
Concentrations of halogens (fluorine, chlorine, bromine and iodine) were determined in six geochemical reference materials (BHVO‐2, GS‐N, JG‐1, JR‐1, JB‐1b, JB‐2). Halogens were first extracted from powdered samples using a pyrohydrolysis technique, then hydrolysis solutions were analysed by ion chromatography for F and Cl and inductively coupled plasma‐mass spectrometry for Br and I. The detection limits in solutions were 100 μg l?1 for both F and Cl and 10 ng l?1 for Br and I. Considering the extraction procedure, performed on a maximum of 500 mg of sample and producing 100 ml of pyrohydrolysis solution, detection limits in rock samples were 20 mg kg?1 for F and Cl and 2 μg kg?1 for Br and I. The mean analytical errors on the studied composition ranges were estimated at 10 mg kg?1 for F and Cl, 100 μg kg?1 for Br and 25 μg kg?1 for I. The concentration values, based on repeated (generally > 10) sample analysis, were in good agreement generally with published values and narrowed the mean dispersion around mean values. Large dispersions are discussed in terms of samples heterogeneity and contaminations during sample preparation. Basaltic RMs were found to be more suitable for studies of halogen compositions than differentiated rock material, especially granites – the powders of which were heterogeneous in halogens at the 500 mg level.  相似文献   

10.
Thirty‐three samples, including 22 eclogites, collected from the Dabie ultrahigh‐pressure (UHP) metamorphic belt in eastern China, have been studied for seismic properties. Compressional (Vp) and shear wave (Vs) velocities in three mutually perpendicular directions under hydrostatic pressures up to 1.0 GPa were measured for each sample. At 1.0 GPa, Vp (7.5–8.4 km s?1), Vs (4.2–4.8 km s?1), and densities (3.2–3.6 g cm?3) in the UHP eclogites are higher than those of UHP orthopyroxenite (7.3–7.5 km s?1, 4.1–4.3 km s?1, 3.2–3.3 g cm?3, respectively) and HP eclogites (7.1–7.9 km s?1, 4.0–4.5 km s?1, 3.1–3.5 g cm?3, respectively). Kyanitites (with 99.5% kyanite) show extremely high velocities and density (9.37 km s?1, 5.437 km s?1, 3.581 g cm?3, respectively). The eclogites show variation of Vp‐ and Vs‐anisotropy up to 9.70% and 9.17%, respectively. Poisson’s ratio (σ) ranges from 0.218 to 0.278 (with a mean of 0.255) for eclogites, 0.281–0.298 for granulites and 0.248 to 0.255 for amphibolites. The σ values for serpentinite (0.341) and marble (0.321) are higher than for other lithologies. The elastic moduli K, G, E of kyanitite were obtained as 163, 102 and 253 GPa, respectively. The Vp and density of representative UHP metamorphic rocks (eclogite & kyanitite) were extrapolated to mantle depth (15 GPa) following a reasonable geotherm, and compared to the one dimension mantle velocity and density model. The comparison shows that Vp and density in eclogite and kyanitite are greater than those of the ambient mantle, with differences of up to ΔVp > 0.3 km s?1 and Δρ > 0.3–0.4 g cm?3, respectively. This result favours the density‐induced delamination model and also provides evidence in support of distinguishing subducted high velocity materials in the upper mantle by means of seismic tomography. Such ultra‐deep subduction and delamination processes have been recognized by seismic tomography and geochemical tracing in the postcollisional magmatism in the Dabie region.  相似文献   

11.
This article presents new boron concentrations for nine geochemical reference materials (GS‐N, FK‐N, GL‐O, BX‐N, DT‐N, AN‐G, GH, Mica‐Fe, Mica‐Mg). After extraction by a modified pyrohydrolysis technique, boron concentrations were measured by ICP‐MS. The blank levels for the whole procedure were 0.091 ± 0.020 ng ml?1 or 14 ± 5 ng of boron in total. The method was first validated by measuring nine reference materials with known boron concentrations. The determined boron concentrations are all within the range of recommended or published values, which means that the yields were 100%, and show precisions below 10% for samples containing over 2 μg g?1 of boron.  相似文献   

12.
N(187Os)/N(188Os) ratios of six geological reference materials were measured using static Faraday cups (FCs) with 1013 Ω amplifiers by N‐TIMS. Our results show that the repeatability precision was 2–3‰ (2 RSD, n = 3), when taking ~ 1 g of BHVO‐2 with 76 pg g?1 of Os mass fraction and ~ 2 g of BCR‐2 with 21 pg g?1 of Os mass fraction for each sample, whether measured by FCs or by secondary electron multiplier. The repeatability precision measured by FCs was 1–0.2‰ (2 RSD, n = 3) when taking ~ 1 g of BIR‐2 with 350 pg g?1 of Os mass fraction, ~ 1 g of WGB‐1 with 493 pg g?1 of Os mass fraction or ~ 0.5 g of WPR‐1 with 13.3 ng g?1 of Os mass fraction for each sample, which is much better than those measured by secondary electron multiplier. Instead, when taking ~ 2 g of AGV‐2 with 4 pg g?1 Os mass fraction, the repeatability precision measured by secondary electron multiplier is 3–4‰ (RSD, n = 3), which is better than those measured by FCs. Of the six reference materials analysed, WPR‐1 and BIR‐1a are the most homogeneous with regard to Os isotopic composition (2 RSD of 0.08% and 0.23%, respectively) when test portion masses are 0.5–1 g.  相似文献   

13.
A method was developed for the determination of platinum‐group elements (PGE) in geological samples by isotope dilution‐inductively coupled plasma‐mass spectrometry combined with sulfide fire assay preconcentration. Samples were fused and PGE analytes were concentrated in sulfide buttons. The buttons were dissolved using HCl leaving PGE analytes in insoluble residues, which were digested in HNO3 and simultaneously processed for the distillation of Os. The remaining solutions were further prepared for the purification of Ru, Rh, Pd, Ir and Pt using a tandem assembly of cation and Ln resin columns. The eluents were directly analysed by membrane desolvation‐ICP‐MS. Ruthenium, Pd, Os, Ir and Pt were determined by isotope dilution, whereas Rh was determined by conventional reference material calibration combined with 193Ir as the internal standard element. The method was validated using a series of PGE reference materials, and the measurement data were consistent with the recommended and the literature values. The measurement precision was better than 10% RSD. The procedural blanks were 0.121 ng for Ru, 0.204 for Rh, 0.960 ng for Pd, 0.111 ng for Os, 0.045 ng for Ir and 0.661 ng for Pt, and the limits of detection (3s) were 0.011 ng g?1 for Ru, 0.008 ng g?1 for Rh, 0.045 ng g?1 for Pd, 0.009 ng g?1 for Os, 0.006 ng g?1 for Ir and 0.016 ng g?1 for Pt when a test portion mass of 10 g was used. This indicates that the proposed method can be used for the determination of trace amounts of PGE in geological samples.  相似文献   

14.
The Lamont‐Doherty Earth Observatory radiogenic isotope group has been systematically measuring Sr‐Nd‐Pb‐Hf isotopes of USGS reference material BCR‐2 (Columbia River Basalt 2), as a chemical processing and instrumental quality control monitor for isotopic measurements. BCR‐2 is now a widely used geochemical inter‐laboratory reference material (RM), with its predecessor BCR‐1 no longer available. Recognising that precise and accurate data on RMs is important for ensuring analytical quality and for comparing data between different laboratories, we present a compilation of multiple digestions and analyses made on BCR‐2 during the first author's dissertation research. The best estimates of Sr, Nd and Hf isotope ratios and measurement reproducibilities, after filtering at the 2s level for outliers, were 87Sr/86Sr = 0.705000 ± 11 (2s, 16 ppm, n = 21, sixteen digestions, one outlier), 143Nd/144Nd = 0.512637 ± 13 (2s, 25 ppm, n = 27, thirteen digestions, one outlier) and 176Hf/177Hf = 0.282866 ± 11 (2s, 39 ppm, n = 25, thirteen digestions, no outliers). Mean Nd and Hf values were within error of those reported by Weis et al. (2006, 2007) in their studies of RMs; mean Sr values were just outside the 2s uncertainty range of both laboratories. Moreover, a survey of published Sr‐Nd‐Hf data shows that our results fall within the range of reported values, but with a smaller variability. Our Pb isotope results on acid leached BCR‐2 aliquots (n = 26, twelve digestions, two outliers) were 206Pb/204Pb = 18.8029 ± 10 (2s, 55 ppm), 207Pb/204Pb = 15.6239 ± 8 (2s, 52 ppm), 208Pb/204Pb = 38.8287 ± 25 (2s, 63 ppm). We confirm that unleached BCR‐2 powder is contaminated with Pb, and that sufficient leaching prior to digestion is required to achieve accurate values for the uncontaminated Pb isotopic compositions.  相似文献   

15.
Properly combining highly siderophile element (HSE: Re, Pd, Pt, Ru, Ir, Os) abundance data, obtained by isotope dilution, with corresponding 187Os/188Os and 186Os/188Os measurements of rocks requires efficient digestion of finely‐ground powders and complete spike‐sample equilibration. Yet, because of the nature of commonly used methods for separating Os from a rock matrix, hydrofluoric acid (HF) is typically not used in such digestions. Consequently, some silicates are not completely dissolved, and HSE residing within these silicates may not be fully accessed. Consistent with this, some recent studies of basaltic reference materials (RMs) have concluded that an HF‐desilicification procedure is required to fully access the HSE (Ishikawa et al. (2014) Chemical Geology, 384, 27–46; Li et al. (2015) Geostandards and Geoanalytical Research, 39, 17–30). Highly siderophile element abundance and Os isotope studies of intraplate basalts typically target samples with a range of MgO contents (< 8 to > 18% m/m, or as mass fractions, < 8 to > 18 g per 100 g), in contrast to the lower MgO mass fractions (< 10 g per 100 g) of basalt and diabase RMs (i.e., BIR‐1, BHVO‐2, TDB‐1). To investigate the effect of HF‐desilicification on intraplate basalts, experiments were performed on finely ground Azores basalts (8.1–17 g per 100 g MgO) using a ‘standard acid digestion’ (2:1 mixture of concentrated HNO3 and HCl), and a standard acid digestion, followed by HF‐desilicification. No systematic trends in HSE abundances were observed between data obtained by standard acid digestion and HF‐desilicification. Desilicification procedures using HF do not improve liberation of the HSE from Azores basalts, or some RMs (e.g., WPR‐1). We conclude that HF‐desilicification procedures are useful for obtaining total HSE contents of some young lavas, but this type of procedure is not recommended for studies where Re‐Pt‐Os chronological information is desired. The collateral effect of a standard acid digestion to liberate Os, followed by HF‐desilicification to obtain Re and Pt abundances in samples, is that the measured Re/Os and Pt/Os may not correspond with measured 187Os/188Os or 186Os/188Os.  相似文献   

16.
A rapid and inexpensive method was developed for the determination of trace silver in polymetallic ore samples by use of eggshell membrane (ESM), a natural biomaterial, as the solid‐phase extraction (SPE) adsorbent coupled with flame atomic absorption spectrometry (FAAS). The ESM was used for the separation/pre‐concentration of silver, and the parameters affecting sensitivity, such as pH, sample flow rate, eluent volume and eluent flow rate, were carefully investigated. ESM was found to be an effective solid phase extractant for the adsorption of trace silver over a wide range of acidity from 0.02 to 0.50 mol l?1 HNO3. The sample solution in 0.4 mol l?1 HNO3 was pumped through an ESM microcolumn at the rate of 1.0 ml min?1. Silver was absorbed, and then eluted with a solution of 1.0% m/v thiourea–0.5% v/v HCl. Under these optimal conditions, ESM exhibited a good enrichment efficiency for silver with a dynamic adsorption capacity of 1.7 mg g?1. The proposed method was applied to the FAAS determination of trace silver in polymetallic ores and geological reference materials, GSO‐2, 3 and 5, and GSD‐11, GSD‐12, and the determined values were in good agreement with certified values.  相似文献   

17.
We report high‐precision iron isotopic data for twenty‐two commercially available geological reference materials, including silicates, carbonatite, shale, carbonate and clay. Accuracy was checked by analyses of synthetic solutions with known Fe isotopic compositions but different matrices ranging from felsic to ultramafic igneous rocks, high Ca and low Fe limestone, to samples enriched in transition group elements (e.g., Cu, Co and Ni). Analyses over a 2‐year period of these synthetic samples and pure Fe solutions that were processed through the whole chemistry procedure yielded an average δ56Fe value of ?0.001 ± 0.025‰ (2s, n = 74), identical to the expected true value of 0. This demonstrates a long‐term reproducibility and accuracy of < 0.03‰ for determination of 56Fe/54Fe ratios. Reproducibility and accuracy were further confirmed by replicate measurements of the twenty‐two RMs, which yielded results that perfectly match the mean values of published data within quoted uncertainties. New recommended values and associated uncertainties are presented for interlaboratory calibration in the future.  相似文献   

18.
An organic solvent‐free two‐step column procedure is presented that provided robust, high yield and super clean separation of Li from silicate rock sample matrices. The measured δ7Li value for BHVO‐2 of +4.29 ± 0.23‰ (1s) is comparable with the reported values. The δ7Li values for GSJ JP‐1 (+3.14 ± 0.41‰, 1s) and USGS DTS‐2 (+4.91 ± 0.34‰, 1s) presented here provide new reference values for ultramafic rock reference materials.  相似文献   

19.
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   

20.
A section of the orogenic middle crust (Orlica‐?nie?nik Dome, Polish/Czech Central Sudetes) was examined to constrain the duration and significance of deformation (D) and intertectonic (I) phases. In the studied metasedimentary synform, three deformation events produced an initial subhorizontal foliation S1 (D1), a subsequent subvertical foliation S2 (D2) and a late subhorizontal axial planar cleavage S3 (D3). The synform was intruded by pre‐, syn‐ and post‐D2 granitoid sheets. Crystallization–deformation relationships in mica schist samples document I1–2 garnet–staurolite growth, syn‐D2 staurolite breakdown to garnet–biotite–sillimanite/andalusite, I2–3 cordierite blastesis and late‐D3 chlorite growth. Garnet porphyroblasts show a linear Mn–Ca decrease from the core to the inner rim, a zone of alternating Ca–Y‐ and P‐rich annuli in the inner rim, and a Ca‐poor outer rim. The Ca–Y‐rich annuli probably reflect the occurrence of the allanite‐to‐monazite transition at conditions of the staurolite isograd, whereas the Ca‐poor outer rim is ascribed to staurolite demise. The reconstructed P–T path, obtained by modelling the stability of parageneses and garnet zoning, documents near‐isobaric heating from ~4 kbar/485 °C to ~4.75 kbar/575 °C during I1–2. This was followed by a progression to 4–5 kbar/580–625 °C and a subsequent pressure decrease to 3–4 kbar during D2. Pressure decrease below 3 kbar is ascribed to I2–3, whereas cooling below ~500 °C occurred during D3. In the dated mica schist sample, garnet rims show strong Lu enrichment, oscillatory Lu zoning and a slight Ca increase. These features are also related to allanite breakdown coeval with staurolite appearance. As Lu‐rich garnet rims dominate the Lu–Hf budget, the 344 ± 3 Ma isochron age is ascribed to garnet crystallization at staurolite grade, near the end of I1–2. For the dated sample of amphibole–biotite granitoid sheet, a Pb–Pb single zircon evaporation age of 353 ± 1 Ma is related to the onset of plutonic activity. The results suggest a possible Devonian age for D1, and a Carboniferous burial‐exhumation cycle in mid‐crustal rocks that is broadly coeval with the exhumation of neighbouring HP rocks during D2. In the light of published ages, a succession of telescoping stages with time spans decreasing from c. 10 to 2–3 Ma is proposed. The initially long period of tectonic quiescence (I1–2 phase, c. 10 Ma) inferred in the middle crust contrasts with contemporaneous deformation at deeper levels and points to decoupled P–T–D histories within the orogenic wedge. An elevated gradient of ~30 °C km?1 and assumed high heating rates of c. 20 °C Ma?1 are explained by the protracted intrusion of granitoid sheets, with or without deformation, whereas fast vertical movements (2–3 Ma, D2 phase) in the crust require the activity of deformation phases.  相似文献   

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