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1.
Refinements have been made to achieve over 99% yield in the conversion of CO to CO2 in order to improve the reproducibility and accuracy of δ18 O measurements in sulfates. BaSO4 (10-15 mg) was mixed with an identical amount of spectrographic-grade graphite and loaded into a Pt boat. The mixture was gradually heated to 1100 °C to reduce sulfate to CO and CO2; the former gas was simultaneously converted to CO2 by a glow discharge between Pt electrodes immersed in a magnetic field (produced by a pair of external neodymium magnets). A small memory effect was noticed during the analysis (less than 0.3‰ per 10‰ difference in δ18 O between two subsequently analysed samples). The memory effect, however, was suppressed by repetitive preparation of the same specimen. CO2 produced in this way from sulfate reference samples was analysed on a dual inlet and triple collector mass spectrometer along with CO2 equilibrated with VSMOW, GISP and SLAP water reference samples. To avoid large departures of measured isotope ratios from 18O/16O of the working calibrator we used CO2 gas prepared from ocean water sulfate for this purpose. The calibrated δ18 O values (in ‰) obtained in this way for NBS-127, IAEA SO-5 and IAEA SO-6 reference materials were 8.73 ± 0.05, 12.20 ± 0.07 and -10.43 ± 0.12, respectively.  相似文献   

2.
Diffusion modelling is applied to layered garnet–pyroxene–quartz coronas, formed by a pressure-induced reaction between plagioclase and primary pyroxene in a metabasic granulite. The reconstructed reaction involves some change in composition of reactant minerals. The distribution of minerals between layers is satisfactorily explained by diffusion-controlled reaction with local equilibrium, in which the diffusion coefficient for Al was smaller than those for Fe, Mg and Ca by a factor of approximately four. Diffusion of Mg towards plagioclase implies a chemical-potential gradient for MgO component in a direction opposite to the changing Mg content of garnet; this is explained by the influence of Al2O3 on the chemical potential of the pyrope end-member. Grain-boundary diffusion is suggested to have operated, possibly with composition gradients different from those in the bulk minerals. Chemical-potential differences across the corona are estimated from the variation in garnet composition, enabling affinity (the free energy change driving the reaction) to be estimated as 6.9±1.8  kJ per 24-oxygen mole of garnet produced. This implies that the pressure for equilibrium among the minerals was overstepped by 1.4±0.4  kbar. The probable P–T conditions of reaction were in the range 650–790  °C, 8–10  kbar. Assuming a timescale of reaction between 106 and 108 years, estimated diffusion coefficients for Fe, Mg and Ca are in the range 9×10−23 to 5×10−20 m2 s−1. These are consistent with experimental values in the literature for solid-state diffusion, including grain-boundary diffusion.  相似文献   

3.
This paper presents an adapted anion exchange column chemistry protocol which allowed separation of high-purity fractions of Cu and Zn from geological materials. Isobaric and non-spectral interferences were virtually eliminated for consequent multiple-collector ICP-MS analysis of the isotopic composition of these metals. The procedure achieved ∼ 100% recoveries, thus ensuring the absence of column-induced isotopic fractionation. By employing these techniques, we report isotopic analyses for Cu and Zn from five geological reference materials: BCR-027 blende ore (BCR), δ65Cu = 0.52 ± 0.15‰ (n = 10) and δ66Zn = 0.33 ± 0.07‰ (n = 8); BCR-030 calcined calamine ore (BCR), δ66Zn = -0.06 ± 0.09‰ (n = 8); BCR-1 basalt (USGS), δ66Zn = 0.29 ± 0.12‰ (n = 8); NOD-P-1 manganese nodule (USGS), δ65Cu = 0.46 ± 0.08‰ (n = 10) and δ66Zn = 0.78 ± 0.09‰ (n = 9); SU-1 Cu-Co ore (CCRMP), δ65Cu = -0.018 ± 0.08‰ (n = 10) and δ66Zn = 0.13 ± 0.17‰ (n = 6). All uncertainties are ± 2s; copper isotope ratios are reported relative to NIST SRM-976, and zinc isotope ratios relative to the Lyon-group Johnson Matthey metal (batch 3-0749 L) solution, JMC Zn. These values agree well with the limited data previously published, and with results reported for similar natural sample types. Samples were measured using a GVi IsoProbe MC-ICP-MS, based at the Natural History Museum, London. Long-term measurement reproducibility has been assessed by repeat analyses of both single element and complex matrix samples, and was commonly better than ± 0.07‰ for both δ66Zn and δ65Cu.  相似文献   

4.
Thirteen geochemical reference standards have been analysed for lithium by a technique originally developed for assay of lithium in biological materials. The technique consists of thermal neutron irradiation, then measurement of 3He from decay of 3H produced via the reaction 6Li(n, α)3H. The results are compared with literature values.  相似文献   

5.
The CRPG (Nancy, France) has prepared secondary reference materials for Li isotope measurements by mixing 7Li or 6Li spikes and either L-SVEC or IRMM-016 certified reference materials to produce solutions having a known Li concentration and isotopic composition. The Li7-N and Li6-N solution samples (1.5 mol l−1 HNO3) have nominal δ7Li isotopic compositions of 30.1‰ and -9.7‰ respectively relative to L-SVEC and concentrations of 100 mg l−1. Repeated measurement of these samples using the QUAD-ICP-MS at the CRPG yielded δ7Li of 30.4 ± 1.1‰ (n = 13) and -8.9 ± 0.9‰ (n = 9) at the 2s level of confidence. An additional LiCl-N solution was measured and yielded a delta value of 9.5 ± 0.6‰ (n = 3). Identical results were obtained at the BRGM (Orléans, France) from determinations performed with a Neptune MC-ICP-MS (30.2 ± 0.3‰, n = 89 for the Li7-N, -8.0 ± 0.3‰, n = 38 for the Li6-N and 10.1 ± 0.2‰, n = 46 for LiCl-N at the 2s level of confidence). The deviation of measured composition relative to the nominal value for the Li6-N solution might be explained by either contamination during preparation or an error during sample weighing. These secondary reference materials, previously passed through ion exchange resin or directly analysed, may be used for checking the accuracy of Li isotopic measurements over a range of almost 40‰ and will be available to the scientific community upon request to J. Carignan or N. Vigier, CRPG.  相似文献   

6.
Thermoluminescence dating of Dimlington Stadial deposits in eastern England   总被引：2，自引：0，他引：2  
The loess component of a solifluction deposit of the Dimlington Stadial exposed at the inland site of Eppleworth in eastern England gave a thermoluminescence date of 17.5 ± 1.6 × 103 years. The solifluction deposit is overlain by a slightly weathered till correlated with the Skipsea Till of coastal exposures. which lies between organic horizons with radiocarbon dates of 18,500–18,240 B.P. and 13,045 B.P. Although the till must have been deposited during the Dimlington Stadial (after 18,240 B.P. at Dimlington and after 17,500 B.P. at Epplcworth), it gave apparent TL dates of 42.1 ± 3.6 × 103 years at Eppleworth and 102 ± 9 × 103 years at Dimlington, indicating that the components of the till were not exposed to light immediately before deposition.  相似文献   

7.
An extraordinarily large and geographically extensive 3D dataset has allowed us to relate permeability to detailed geological features. Permeability data derived from several thousand pumptests in Quaternary sediments (thickness < 120 m) of the Upper Rhine valley vary from K = 4.5 × 10−7 m s−1 to K = 2.7 × 10−1 m s−1. The geometric mean of the data is K = 2.25 × 10−3 m s−1. The permeability distribution maps for four different stratigraphic levels show that the highest values are found in sections beneath recent and historic fluvial systems. Fossil fans of small rivers from the Black Forest can be identified in the Rhine valley on the basis of the permeability pattern. The average hydraulic conductivity decreases S–N along the flow direction which corresponds to a decrease in grain-size of the fluvial sediments.  相似文献   

8.
Abstract. Primary fluid inclusions in quartz and carbonates from the Kanggur gold deposit are dominated by aqueous inclusions, with subsidiary CO2-H2O inclusions that have a constant range in CO2 content (10–20 vol %). Microthermometric results indicate that total homogenization temperatures have a wide but similar range for both aqueous inclusions (120 to 310C) and CO2-H2O inclusions (140 to 340C). Estimates of fluid salinity for CO2-H2O inclusions are quite restricted (5.9∼10.3 equiv. wt% NaCl), whereas aqueous inclusions show much wider salinity ranging from 2.2 to 15.6 equivalent wt %NaCl.
The 6D values of fluid inclusions in carbonates vary from -45 to -61 %, in well accord with the published δD values of fluid inclusions in quartz (-46 to -66 %). Most of the δ18O and δD values of the ore-forming fluids can be achieved by exchanged meteoric water after isotopic equilibration with wall rock by fluid/rock interaction at a low water/rock ratio. However, the exchanged meteoric water alone cannot explain the full range of δ18O and δD values, magmatic and/or meta-morphic water should also be involved. The wide salinity in aqueous inclusions may also result from mixing of meteoric water and magmatic and/or metamorphic water.  相似文献   

9.
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10.
In the Boreal Chalk of northwestern Europe the base of the Maastrichtian Stage is defined by entry of the belemnite Belemnella . In the Kronsmoor section, in northwestern Germany, which is a standard section for the European Chalk, 87Sr/86Sr at the Campanian/ Maastrichtian (C/M) boundary is 0.707723±9 (10). An isotopic correlation of this boundary to the US Western Interior, for which a highly refined cephalopod biostratigraphy exists, suggests that this boundary, as defined at Kronsmoor, occurs within the Baculites jenseni zone. This correlationagrees with the latest placement based on biostratigraphic criteria. On87Sr/86Srcriteria the boundary at Kronsmoor correlates to the English Chalk at Trunch, Norfolk, UK, at a level 3.5 m lower than its position based on biostratigraphic criteria.
At Kronsmoor, 87Sr/86Sr increases in a quasi-linear manner through much of the section, suggesting that, averaged over intervals of 1 Myr, the gross sedimentation rate and temporal rate of change of 87Sr/86Sr were approximately constant through the section. For US samples, zonally-plotted values of 87Sr/86Sr define a quasi-linear trend, which suggests a moderate uniformity of zonal duration from the Baculites compressus zone (73.2±0.7 Ma, 10) to the Baculites grandis zone (70.1±0.7 Ma, 10).  相似文献   

11.
An igneous zircon reference material (OG1) was characterised for U-Pb isotopes by ID-TIMS, and utilised to evaluate SIMS (SHRIMP) instrumental mass fractionation (IMF) of radiogenic Pb isotopes (207Pb*/206Pb*). The TIMS 207Pb*/206Pb* reference value for OG1 was 0.29907 ± 0.00011 (95% confidence limit), 3465.4 ± 0.6 Ma. The high 207Pb* (∼ 30 μg g−1), negligible common Pb, and isotopic homogeneity permitted precise (± 1–2‰) 207Pb*/206Pb* measurements within the analytical sessions. External reproducibility of mean 207Pb*/206Pb* ratios between sessions was demonstrated for one instrument, yielding a mean IMF of +0.87 ± 0.49‰. The mean 207Pb*/206Pb* ratios between instruments were dispersed beyond uncertainties, with session IMF values from +3.6 ± 1.7‰ to −2.4 ± 1.3‰, and a grand mean IMF value (twenty-six sessions) of +0.70 ± 0.52‰, indicating a tendency towards elevated 207Pb*/206Pb*. The specific causes of variability in IMF are unclear, but generally reflect subtle differences in analytical conditions. The common practice in SIMS of assuming that IMF for Pb+ is insignificant could result in systematic age biases and underestimated uncertainties, of critical importance for precise correlation of Precambrian events. Nevertheless, a zircon RM such as OG1 can be readily incorporated into routine dating to improve 207Pb*/206Pb* accuracy and external reproducibility.  相似文献   

12.
A well-preserved moraine on the northern coast of County Donegal, Ireland, has played a critical role in our understanding of the glacial history of this sector of the Irish Ice Sheet (IIS). Because of a lack of numerical dating of the moraine, however, previous interpretations of its age and significance to the glacial history of this region have varied widely. Here we report eight in situ cosmogenic 10Be ages on boulders sampled from the moraine. Two of these ages are outliers, with the remaining six ranging from 18.8±1.0 10Be kyr to 20.9±1.3 10Be kyr, with an uncertainty-weighted mean age of 19.4±0.3 10Be kyr (19.4±1.2 kyr accounting for production rate uncertainty). Our results confirm one previous 10Be age obtained from the moraine, with the combined data ( n =7) constraining the age of initial deglaciation of the IIS from its LGM position on the continental shelf to be 19.3±0.3 10Be kyr (19.3±1.2 kyr accounting for production rate uncertainty). These ages are in excellent agreement with calibrated 14C ages that constrain retreat of the IIS margin from the continental shelf elsewhere in northwestern and western Ireland and the Irish Sea Basin associated with the start of the Cooley Point Interstadial (≥20–≤18.2 cal. kyr BP), suggesting widespread deglaciation of the IIS ∼19.5–20 kyr ago.  相似文献   

13.
New analyses have been performed in order to enhance the data-set on the independent ages of four glasses that have been proposed as reference materials for fission-track dating. The results are as follows. Moldavite - repeated 40Ar/39Ar age determinations on samples from deposits from Bohemia and Moravia yielded an average of 14.34 ± 0.08 Ma. This datum agrees with other recent determinations and is significantly younger than the 40Ar/39Ar age of 15.21 ± 0.15 Ma determined in the early 1980s. Macusanite (Peru) -four K-Ar ages ranging from 5.44 ± 0.06 to 5.72 ± 0.12 Ma have been published previously. New 40Ar/39Ar ages gave an average of 5.12 ± 0.04 Ma. Plateau fission-track ages determined using the IRMM-540 certified glass and U and Th thin films for neutron fluence measurements agree better with these new 40Ar/39Ar ages than the previously published ages. Roccastrada glass (Italy) - a new 40Ar/39Ar age, 2.45 ± 0.04 Ma, is consistent with previous determinations. The Quiron obsidian (Argentina) is a recently discovered glass that has been proposed as an additional reference material for its high spontaneous track density (around 100 000 cm-2). Defects that might produce "spurious" tracks are virtually absent. An independent 40Ar/39Ar age of 8.77 ± 0.09 Ma was determined and is recommended for this glass. We believe that these materials, which will be distributed upon request to fission-track groups, will be very useful for testing system calibrations and experimental procedures.  相似文献   

14.
Abstract. Silica scales containing large amounts of smectite were recently found in the pipelines for geothermal water at a geothermal power plant. To elucidate the mechanism of smectite formation, seven silica scale samples were characterized by powder X-ray diffraction, chemical analysis and 27A1 MAS NMR. Smectite was present in samples with MgO levels above 10 wt% and Al2O3 levels below 10 wt%. In 27A1 MAS NMR spectra, peaks assigned to both tetrahedrally and octahedrally coordinated aluminum (Al(4) and Al(6)) were observed for Mg-rich samples, whereas a peak due to Al(4) alone appeared in Mg-poor samples. From these observation and comparison between 27A1 MAS NMR spectra for synthesized precipitates of Al2O3-SiO2 containing MgO and not containing MgO, it is concluded that magnesium plays an important role in the stabilization of Al(6), and results in the formation of smectite  相似文献   

15.
We report silicon isotopic determinations for USGS rock reference materials BHVO-1 and BHVO-2 using a Nu Plasma multi-collector (MC)-ICP-MS, upgraded with a new adjustable entrance slit, to obtain medium resolution, as well as a stronger primary pump and newly designed sampler and skimmer cones ("B" cones). These settings, combined with the use of collector slits, allowed a resolution to be reached that was sufficient to overcome the 14N16O and 14N2 interferences overlying the 30Si and the 28Si peaks, respectively, in an earlier set-up. This enabled accurate measurement of both δ30Si and δ29Si. The δ value is expressed in per mil variation relative to the NBS 28 quartz reference material. Based on data acquired from numerous sessions spread over a period of six months, we propose a recommended average δ30Si of −0.33 ± 0.05‰ and −0.29 ± 0.11‰ (2se) for BHVO-1 and BHVO-2, respectively. Our BHVO grand mean silicon isotope composition (δ30Si =−0.31 ± 0.06‰) is significantly more negative than the only published value for BHVO-2, but is in very good agreement with the recently established average value of ocean island basalts (OIB), confirming the conclusion that the OIB reservoir has a distinct isotopic composition from the solar reservoir as sampled by chondrites.  相似文献   

16.
解洪晶  武广  朱明田  钟伟  刘军  糜梅 《地质科学》2013,48(3):827-846
西北天山莱历斯高尔岩体主要由花岗闪长斑岩和二长花岗斑岩组成,二者具有相似的地球化学特征,可能为同源岩浆分异演化的产物。锆石SHRIMP U-Pb年龄显示岩体形成于晚泥盆世(374±4 Ma)。莱历斯高尔岩体具有较高的SiO2(67.75% ～74.71%)含量和K2O/Na2O(1.24～2.20)比值,属于高钾钙碱性系列。稀土元素配分曲线为轻稀土富集型(La/Yb)N(5.25～10.57),具有中等-弱的Eu负异常δEu(0.55～0.92)。微量元素特征显示富集大离子亲石元素(LILE),而亏损高场强元素(HFSE),具有较低的Sr(122×10-6～356×10-6)含量、较高的Y(17.19×10-6～21.82×10-6)和Yb(1.78×10-6～2.57×10-6)含量。岩体的Sr-Nd同位素特征为ISr=0.707 867～0.709 654,εNd(t)=-2.79～-1.46。铅同位素特征为206Pb/204 Pb=18.423～19.915,207 Pb/204Pb=15.576～15.685,208 Pb/204Pb=38.344～39.305。元素和同位素地球化学特征表明,莱历斯高尔岩体岩浆源区主要为中元古代下地壳的部分熔融,并有部分地幔物质的加入。岩体形成于晚泥盆世准噶尔洋向伊犁-中天山微板块陡角度俯冲的大陆弧构造环境。  相似文献   

17.
Boron Isotopic Analysis of Proposed Borosilicate Mineral Reference Samples   总被引：2，自引：0，他引：2  
This brief contribution presents new boron isotopic data for a set of proposed borosilicate reference minerals, most of which are described in the companion paper by Dyar et al.2001. The results for a variety of minerals (tourmalines, danburite, prismatine, serendibite, ferroaxinite and a Li mica) show that it is generally possible to reproduce the 11 B/10 B ratio within ± 0.5 per mil with replicate chemistry and mass spectrometry over long time spans. Because the accuracy of boron isotopic analysis is commonly determined by reference to secondary standards, it is suggested that some of the samples used in this study be adopted for interlaboratory comparisons and for quality control on boron isotopic analyses produced by a variety of analytical methods.  相似文献   

18.
The accuracy of 231Pa-235U measurements can be readily assessed using a secular equilibrium reference material (RM), but a secular equilibrium RM is also required to calibrate the 233Pa spike used in 231Pa determinations. The only silicate RM commonly accepted to be in secular equilibrium is Table Mountain Latite (TML) and so an additional reference is required. Our measurements on the widely available USGS BCR-2 (Basalt Columbia River) rock powder yielded (231Pa/235U) = 0.997 ± 0.013 2s (n = 10), indicating its value as a secondary reference to test the fidelity of U-Pa determinations. Such a reference material additionally provides a useful check on data reduction, which our literature survey highlights can lead to discrepancies of up to 53% between reported (231Pa/235U) activity ratios and corresponding U and Pa concentration data.  相似文献   

19.
Oxygen bulk diffusion rates were experimentally determined in a natural ultramylonite sample ( c . 5   μ m grain size; 15–20% biotite, 20% quartz, 60–65% feldspars, and minor Fe-oxides) from the Gerrish Island shear zone, SE Maine, USA. The diffusion experiments were performed at 250–550  °C and 100  MPa water pressure. Oxygen bulk diffusion rates were determined both parallel and perpendicular to the strong foliation of the sample. The Arrhenius parameters for transport parallel to the foliation are: D bulk0=2.0×10−11 m2 s−1 and Q =30±6 kJ mol−1. The bulk diffusivity perpendicular to the foliation is about a factor of 3.5 less than that parallel to the foliation with the same activation energy. The values of bulk diffusivity and activation energy obtained are consistent with ionic diffusion through a static aqueous fluid, suggesting that an interconnected fluid exists in the ultramylonite even under hydrostatic conditions. The microstructure of the ultramylonite was characterized using transmission electron microscopy (TEM). The nature and distribution of the interconnected fluid cannot be completely resolved from the TEM analysis; however, the low percentage of three-grain channels and open grain/interphase boundaries suggests that the fluid resides as a thin film on the grain surfaces. The results of this study have direct applications in many important geological settings and provide valuable insights into the observed rapid diffusion rates, strong lithological control and pervasive nature of fluid transport in mica-bearing rocks.  相似文献   

20.
The Ca isotopic composition of modern seawater has been determined using a 43Ca-48Ca double spike, which was calibrated using a 42Ca/44Ca seawater ratio of 0.30587 ± 0.00026. This ratio was determined from a total evaporation experiment in which the ion beam was measured from the beginning to the end of the emission. With integration of the peak intensities, the fractionation effects can be minimised, since total evaporation of the reservoir cancels out the effect of vapour enrichment in the light isotopes. This experiment avoids the gravimetric uncertainty inherent in the double spike calibration. This calibration allows the precise redetermination of the seawater isotopic composition of Ca. A mean 40Ca/44Ca ratio for two Atlantic water samples of 45.143 (2smean= 0.003) was found. The good reproducibility of the Ca isotope ratios in present seawater and the very strong isotopic homogeneity of Ca in the oceans illustrate the advantage of using seawater as the common standard, with the advantage of decreasing interlaboratory bias.  相似文献   

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