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1.
1 IntroductionAnicecoreobtainedfrom polarglaciersoricesheetsisoneofthemostimportantarchivestoreconstructpaleoclimaticandpaleoatmosphericcondition .Informationonpale o environmentcanbeextractedfromicecoresaschemicaland/orphysicalsignals.Amongthechemicalsignals,heavymetalsarenotedassignalsofterrestrialenvironmentalchangeandanthropogenicpollution (e.g .Murozumietal.1 969;NgandPatterson 1 981 ;Hongetal.1 994) .SinceconcentrationsofmostofthemetalsinpolarsnowincentralGreen landareatorbelowthepptl… 相似文献
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Paul R. Craddock Olivier J. Rouxel Lary A. Ball Wolfgang Bach 《Chemical Geology》2008,253(3-4):102-113
We have developed a technique for the accurate and precise determination of 34S/32S isotope ratios (δ34S) in sulfur-bearing minerals using solution and laser ablation multiple-collector inductively coupled plasma mass spectrometry (MC-ICP-MS). We have examined and determined rigorous corrections for analytical difficulties such as instrumental mass bias, unresolved isobaric interferences, blanks, and laser ablation- and matrix-induced isotopic fractionation. Use of high resolution sector-field mass spectrometry removes major isobaric interferences from O2+. Standard-sample bracketing is used to correct for the instrumental mass bias of unknown samples. Background on sulfur masses arising from memory effects and residual oxygen-tailing are typically minor (< 0.2‰, within analytical error), and are mathematically removed by on-peak zero subtraction and by bracketing of samples with standards determined at the same signal intensity (within 20%). Matrix effects are significant (up to 0.7‰) for matrix compositions relevant to many natural sulfur-bearing minerals. For solution analysis, sulfur isotope compositions are best determined using purified (matrix-clean) sulfur standards and sample solutions using the chemical purification protocol we present. For in situ analysis, where the complex matrix cannot be removed prior to analysis, appropriately matrix-matching standards and samples removes matrix artifacts and yields sulfur isotope ratios consistent with conventional techniques using matrix-clean analytes. Our method enables solid samples to be calibrated against aqueous standards; a consideration that is important when certified, isotopically-homogeneous and appropriately matrix-matched solid standards do not exist. Further, bulk and in situ analyses can be performed interchangeably in a single analytical session because the instrumental setup is identical for both. We validated the robustness of our analytical method through multiple isotope analyses of a range of reference materials and have compared these with isotope ratios determined using independent techniques. Long-term reproducibility of S isotope compositions is typically 0.20‰ and 0.45‰ (2σ) for solution and laser analysis, respectively. Our method affords the opportunity to make accurate and relatively precise S isotope measurement for a wide range of sulfur-bearing materials, and is particularly appropriate for geologic samples with complex matrix and for which high-resolution in situ analysis is critical. 相似文献
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建立了HF—HN03密封酸溶以及Na2O2熔融处理样品,乙醇增强灵敏度,电感耦合等离子体质谱直接测定地质样品中微量和超痕量碲的方法。样品溶液中加入乙醇(φ=4%),在0.85L/min的载气流速下,碲信号可增强2.5倍以上。碲的方法检出限(100,DF=1000)为0.02μg/g。用土壤和水系沉积物国家一级标准物质验证了方法的准确度,标准物质的绝大多数分析结果与标准值的误差在允许范围内。分析了大洋多金属结核样品及深海沉积物样品中的微量碲,结果与其他方法相符,精密度试验RSD(n=3)<10%。 相似文献
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本文提出了用ICP-AES法直接同时测定高纯氧化钇中14个稀土和16个非稀土杂质元素的分析方法,对被测元素的 谱线、氧化钇基本及背景影响进行了研究,用标准加入法测出氧化钇基准中的微量杂质元素,消除了由于忽略基准中的杂质元素含量给高纯氧化钇分析测定带来的误差,同时对工作条件进行了优化。方法中各被测元素的检出限为0.003~1.31ug/g,能够满足生产过程中的质量控制及进出口商品检验 相似文献
7.
Molybdenum Mass Fractions and Isotopic Compositions of International Geological Reference Materials
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Pei‐Pei Zhao Jie Li Le Zhang Zhi‐Bing Wang De‐Xin Kong Jin‐Long Ma Gang‐Jian Wei Ji‐Feng Xu 《Geostandards and Geoanalytical Research》2016,40(2):217-226
The double‐spike method with multi‐collector inductively coupled plasma‐mass spectrometry was used to measure the Mo mass fractions and isotopic compositions of a set of geological reference materials including the mineral molybdenite, seawater, coral, as well as igneous and sedimentary rocks. The long‐term reproducibility of the Mo isotopic measurements, based on two‐year analyses of NIST SRM 3134 reference solutions and seawater samples, was ≤ 0.07‰ (two standard deviations, 2s, n = 167) for δ98/95Mo. Accuracy was evaluated by analyses of Atlantic seawater, which yielded a mean δ98/95Mo of 2.03 ± 0.06‰ (2s, n = 30, relative to NIST SRM 3134 = 0‰) and mass fraction of 0.0104 ± 0.0006 μg g?1 (2s, n = 30), which is indistinguishable from seawater samples taken world‐wide and measured in other laboratories. The comprehensive data set presented in this study serves as a reference for quality assurance and interlaboratory comparison of high‐precision Mo mass fractions and isotopic compositions. 相似文献
8.
Jason Jweda Louise Bolge Cornelia Class Steven L. Goldstein 《Geostandards and Geoanalytical Research》2016,40(1):101-115
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
9.
An Alternative Protocol for Single Zircon Dissolution with Application to (U‐Th‐Sm)/He Thermochronometry
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Bouchaïb Tibari Arnaud Vacherat Martin Stab Raphaël Pik Delphine Yeghicheyan Pascal Hild 《Geostandards and Geoanalytical Research》2016,40(3):365-375
Zircon (U‐Th‐Sm)/He (ZHe) thermochronometry is a powerful tool that has been widely used in geology to constrain the exhumation histories of orogens. In this study, we present an alternative protocol for dissolving zircon grains for determination of parent nuclides. This new alkali fusion procedure developed at the SARM (Service d'Analyse des Roches et des Minéraux) in Nancy, France, is fast (requiring only 2 d, including cleaning steps) and offers several advantages over conventional methods by avoiding: (i) use of HF pressure dissolution and (ii) complete removing of grains from the metal microvials. After dissolution, U, Th and Sm were measured using an ICP‐MS. We tested the new procedure on two different ZHe reference materials, the Fish Canyon Tuff and Buluk Tuff; these provided precision values for ZHe‐age estimations of 9 and 6% (1s), respectively. In addition, using this method, zircons from the Buluk Tuff are shown to be chemically more homogenous and more suitable for assessing the uncertainty of the entire integrated procedure. 相似文献
10.
Community‐Derived Standards for LA‐ICP‐MS U‐(Th‐)Pb Geochronology – Uncertainty Propagation,Age Interpretation and Data Reporting
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Matthew S. A. Horstwood George Gehrels Simon E. Jackson Noah M. McLean Chad Paton Norman J. Pearson Keith Sircombe Paul Sylvester Pieter Vermeesch James F. Bowring Daniel J. Condon Blair Schoene 《Geostandards and Geoanalytical Research》2016,40(3):311-332
The LA‐ICP‐MS U‐(Th‐)Pb geochronology international community has defined new standards for the determination of U‐(Th‐)Pb ages. A new workflow defines the appropriate propagation of uncertainties for these data, identifying random and systematic components. Only data with uncertainties relating to random error should be used in weighted mean calculations of population ages; uncertainty components for systematic errors are propagated after this stage, preventing their erroneous reduction. Following this improved uncertainty propagation protocol, data can be compared at different uncertainty levels to better resolve age differences. New reference values for commonly used zircon, monazite and titanite reference materials are defined (based on ID‐TIMS) after removing corrections for common lead and the effects of excess 230Th. These values more accurately reflect the material sampled during the determination of calibration factors by LA‐ICP‐MS analysis. Recommendations are made to graphically represent data only with uncertainty ellipses at 2s and to submit or cite validation data with sample data when submitting data for publication. New data‐reporting standards are defined to help improve the peer‐review process. With these improvements, LA‐ICP‐MS U‐(Th‐)Pb data can be considered more robust, accurate, better documented and quantified, directly contributing to their improved scientific interpretation. 相似文献