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Brian L. Gulson Allen L. Meier Stanley E. Church Karen J. Mizon 《Journal of Geochemical Exploration》1989,32(1-3)
Thermal ionization mass spectrometry (TI-MS) has long been the method of choice for Pb-isotope determinations. More recently, however, inductively coupled plasma mass spectrometry (ICP-MS) has been used to determine Pb-isotope ratios for mineral exploration. The ICP-MS technique, although not as precise as TI-MS, may promote a wider application of Ph-isotope ratio methods because it allows individual isotopes to be determined more rapidly, generally without need for chemical separation (e.g., Smith et al., 1984; Hinners et al., 1987). To demonstrate the utility of the ICP-MS method, we have conducted a series of Pb-isotope measurements on several suites of samples using both TI-MS and ICP-MS. 相似文献
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Global change has become a hot spot in Quaternary geology,and high-precision,high-sensitivity dating is also an urgent problem which needs to be solved.This paper presents some achievements in U-servies dating of marine corals by thermal ionization mass spectrometry (TIMS) and its application to the study of paleo-environments.Recently,coral samples were determined for their ages on a MAT-262 mass spectrometer and satisfactory results have been obtained. 相似文献
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应用同位素稀释法热电离质谱(TIMS)技术测定珊瑚礁的高精度铀系年龄。通过对BarbadosⅢ、Ⅳ阶地等样品分析,RendezvousHil和Curacao+6m的TIMS年龄分别为129.2±1.2kaB.P.和125.4±1.1kaB.P.,对应深海沉积物氧同位素第5期5e段的高海面;Kendal山阶地为208.1±1.9kaB.P.,可能代表7c间冰期高海平面的时代。该结果与Edwards等测定同一阶地的年龄一致,与α谱法数据在误差范围内吻合。另外,探讨了初始铀同位素比值的变化,并对TIMS年龄的可靠性做了评价。 相似文献
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In situ U-series dating by laser-ablation multi-collector ICPMS: new prospects for Quaternary geochronology 总被引：2，自引：0，他引：2
Stephen M. Eggins Rainer Grün Malcolm T. McCulloch Alistair W.G. Pike John Chappell Les Kinsley Graham Mortimer Michael Shelley Colin V. Murray-Wallace Christoph Sptl Lois Taylor 《Quaternary Science Reviews》2005,24(23-24):2523-2538
The capabilities and potential applications of in situ dating of Quaternary materials using laser ablation-MC-ICPMS are explored. 234U/238U and 230Th/234U can be measured with precision sufficient for dating at a spatial resolution of 100 μm or better in samples that contain as a little as 1 ppm uranium. Moreover, U and Th concentrations and U-series isotope ratios can be continuously profiled to determine changes in age that occur with sample growth (e.g. in speleothems). These capabilities additionally permit the dating of bones, teeth and possibly molluscs, which are subject to post-mortem open-system behaviour of U-series isotopes, and can be employed to elucidate processes of U-series migration during weathering and diagenesis. A drawback of laser ablation-MC-ICPMS is that it cannot in general provide U-series age estimates with the high precision and accuracy of conventional TIMS or solution MC-ICPMS methods. However, sample preparation is straightforward, the amount of sample consumed negligible, and it can be used to rapidly characterise or screen and select samples from which more precise and accurate dates can be obtained using conventional methods. Given further instrumental developments and the establishment of suitable matrix-matched standards for carbonates and other materials, we foresee that laser ablation-MC-ICPMS will play an increasingly important role in Quaternary dating research. 相似文献
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Gang Yang Aaron Zimmerman Nicole C. Hurtig Svetoslav V. Georgiev Vineet Goswami Judith L. Hannah Holly J. Stein 《Geostandards and Geoanalytical Research》2020,44(2):231-242
Rhenium–osmium geochronometry for samples with low Re and complex matrices requires improved Re extraction methods. Here, we investigate plausible controls on efficiency and efficacy of Re extraction during our anion resin bead purification. Four different protocols are compared, each isolating a single variable to test. Rhenium concentrations for solutions at each step of each protocol document differences in chemical recovery/yield. The negative‐thermal ionisation mass spectrometry (N‐TIMS) signal intensity serves as a proxy for Re yield and purity. These data document correlations between the N‐TIMS signal intensity and (a) the duration of anion resin bead conditioning prior to loading with Re‐bearing solution, and (b) both duration and strength of nitric acid used during rinsing of the Re‐loaded anion resin bead. The optimal protocol improved Re signal intensity around fourteen times compared with our current Re extraction protocol, an aggregate of 2.4 times improvement in chemical recovery (yield) and 5.8 times improvement in emission efficiency (purity). Repeated N‐TIMS isotopic measurements on our in‐house Re standard solution (1407) verify that our optimal protocol‐3 does not fractionate Re isotopes. The improved anion resin bead method considerably lowers the Re detection limit and allows Re‐Os isotopic analysis of picogram‐level Re hosted in geological samples with complex matrices. 相似文献
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近10年来国际上用热电离质谱代替α谱仪测定不平衡铀系样品的年龄，在造礁珊瑚、洞穴堆积物、年轻火山岩和湖泊沉积物等领域已取得了显著的成果。该技术有明显的优点，如样品用量少，测试时间短，测量精度高，测年范围宽，是中更新世至全新世以来有效的测年方法之一，可为全球变化研究提供高精度和高灵敏度的年龄谱，展示了热电离质谱技术如同加速器质谱技术一样，有广阔的应用前景。我们曾用MAT－262质谱仪对国内石笋标样(GBW04412，GBW04413)和国际珊瑚标样(RKM－4)进行过测试，取得了与标准值一致的结果。 相似文献
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海洋有孔虫的硼同位素能够反映海水酸碱度值的变化,为研究大气CO2浓度在长时间尺度上的变化提供了一种新的手段,甚至可能超出冰芯所能企及的范围。天然样品中硼同位素的测定方法最为常用的是热电离质谱法,分为正热电离质谱法与负热电离质谱法。目前海洋有孔虫硼同位素分析主要应用负热电离质谱法,该方法最大的优点是所需要的样品量比较小（＜1ng B),实验精度却相对比较高(0.6‰～2.0‰; 2sd.)。近年来,基于常规负热电离质谱法发展的全蒸发负热电离质谱法通过分析完所有样品而有效降低分析过程中所发生的分馏效应所带来的影响,并使样品的信号最大化,该方法精度能够达到0.7‰(2s.d.)。本文详细介绍了常规负热电离质谱法和全蒸发负热电离质谱法的各个分析步骤,包括样品前处理、涂样、质谱分析、同质异位素干扰以及实验分析精度等方面。随着实验分析技术的进展,海洋有孔虫硼同位素已被用来重建长时间尺度(百万年和千万年)和短时间尺度(冰期-间冰期)的大气CO2浓度变化。现有的研究证实利用海洋浮游有孔虫硼同位素重建的大气CO2浓度变化与Vostok冰芯记录的大气CO2浓度变化吻合地很好。 相似文献
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《Quaternary Science Reviews》2003,22(10-13):1373-1382
U and Th concentration profiles in fossil hominid and faunal teeth have been measured by laser ablation ICPMS. These profiles record diverse modes of U and Th uptake, particularly within enamel, that can be broadly related to the state of sample preservation. Observed U profiles are in general inconsistent with existing diffusion–adsorption models developed for U-uptake in bone and teeth. Where the models appear applicable, calculated diffusion rates are several orders of magnitude smaller than previous estimates. Laser ablation ICPMS offers a means of rapidly characterizing U and Th distributions in the enamel and dentine components of teeth as a precursor to ESR and U-series dating. In particular, it should allow the identification of teeth (and also bone) samples that have simple U-uptake histories and are amenable to precise dating by time-consuming and expensive Th–U and Pa–U TIMS techniques. We also demonstrated the use of laser ablation ICPMS to measure U-series isotopes in dentine and enamel samples with relatively high U concentrations (>20 ppm). These results, obtained using a quadrupole ICPMS, illustrate significant promise for in situ U-series isotope analysis, particularly when combined with the greater sensitivity and multi-collection capabilities of new sector ICPMS instrumentation. The latter may permit precise isotope ratio measurements on samples containing only a few ppm of U. 相似文献
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热电离质谱铀系法测定碳酸盐标样 总被引：5，自引：0，他引：5
用高精度热电离质谱（ＴＩＭＳ）铀系法测定碳酸盐标样的年龄,测定结果与α谱仪铀系法进行比较,铀含量和年龄值均吻合。方法对Ｕ的回收率可达９５％,Ｔｈ为９２％。ＴＩＭＳ铀系法具有样品用量少、测试时间短、精度高的优点。 相似文献
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Elizabeth Keegan Stephan Richter Ian Kelly Henri Wong Patricia Gadd Heinz Kuehn Adolfo Alonso-Munoz 《Applied Geochemistry》2008
Elemental and isotopic ratio analyses of U ore concentrate samples, from the 3 operating U mining facilities in Australia, were carried out to determine if significant variations exist between their products, thereby allowing the U ore concentrate’s origin to be identified. Elemental analyses were conducted using inductively coupled plasma mass spectrometry (ICP-MS) and X-ray fluorescence spectrometry (XRF). Lead isotope ratios were measured using ICP-MS and U isotope analyses were conducted using thermal ionisation mass spectrometry (TIMS). Minute quantities of sample, such as that obtained from a swipe, were also examined for elemental concentrations using secondary ion mass spectrometry (SIMS). The results of multivariate statistical analysis show clear patterns in the trace elemental composition of the processed U ores, indicating that it is possible to use this feature as a unique identifier of an Australian U ore concentrate’s source. Secondary ion mass spectrometry analyses also allow individual particles to be differentiated using this ‘fingerprinting’ technique. Isotope ratios determined using TIMS reveal that there is a significant difference in the n(234U)/n(238U) isotope ratio between the U ore concentrate from each mine. 相似文献
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高精度ICP-MS 230Th测年新技术及其在贵州衙门洞Y1石笋测年研究中的应用 总被引：5，自引：0，他引：5
在系统介绍洞穴石笋高精度ICP-M S铀系年代学原理与方法的基础上,对贵州荔波县衙门洞Y1石笋进行了IC P-M S 230 Th测年研究。综合分析认为精确时标的建立对于利用石笋进行古气候重建具有重要的实际意义;采用ICP-M S 230 Th测年方法进行石笋样品定年准确可靠,并且比TIM S方法具有更高的效率,所需样品更微量。通过生长速率变化分析表明,石笋生长速率记录了过去冷暖突变事件,因此可以用它作为一个有意义的环境记录替代指标来研究古降水及古气候变化。 相似文献
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珊瑚的B同位素组成是海水pH值记录的良好替代指标。对传统的高精度的B同位素组成分析的方法正离子热电离质谱（PTIMS）和负离子热电离质谱（NTIMS）方法进行了对比研究。结果显示,NTIMS分析方法具有极高的灵敏度,可以分析微小样品量,但由于其分馏较明显,并且我们的实验结果表明前人建议的使用O同位素进行分馏校正的方法仅在某些特定情况下适用,而对大多数的测定缺乏有效分馏校正,同时有机质或者激发剂带来的CNO-干扰难以完全排除,因此NTIMS的结果重现性稍差,δ11B外部精度约为±1．0‰（2σ）左右。PTIMS则分馏不明显,Cs2CNO^＋干扰可以有效监控并排除,可以获得很好的结果：δ11B内部精度和外部精度均优于±0．2‰（2σ）,可以满足高精度pH值重建的要求。然而PTIMS方法的灵敏度低,难以对微小样品量进行分析。因此PTIMS和NTIMS方法是相互补充的,相互无法完全取代。 相似文献
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Jon D. Woodhead 《Geostandards and Geoanalytical Research》2005,29(1):26-36
This annual review documents developments and applications in the field of isotope ratio determination, as reflected in the literature for the Earth and environmental sciences for the year 2003. Particular emphasis is placed upon the relationship between the two dominant analytical techniques-thermal ionisation mass spectrometry (TIMS) and multi-collector inductively coupled plasma-mass spectrometry (MC-ICP-MS)-and the rapidly changing nature of their roles in isotope analysis. Additionally, the review covers developments in single-collector ICP-MS and TOF technologies, new sample preparation procedures and the characterisation of isotopic reference materials, together with fundamental investigations of mass spectrometer performance. 相似文献
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Rainer Grün Maxime Aubert Marie-Hélène Moncel 《Geochimica et cosmochimica acta》2008,72(21):5278-5290
We have mapped U (238U) and Th (232Th) elemental concentrations as well as U-series isotope distributions in a Neanderthal tooth from the Middle Palaeolithic site of Payre using laser ablation ICP-MS. The U-concentrations in an enamel section varied between 1 and 1500 ppb. The U-concentration maps show that U-migration through the external enamel surface is minute, the bulk of the uranium having migrated internally via the dentine into the enamel. The uranium migration and uptake is critically dependent on the mineralogical structure of the enamel. Increased U-concentrations are observed along lineaments, some of which are associated with cracks, and others may be related to intra-prismatic zones or structural weaknesses reaching from the dentine into the enamel. The uranium concentrations in the dentine vary between about 25,000 and 45,000 ppb. Our systematic mapping of U-concentration and U-series isotopes provides insight into the time domain of U-accumulation. Most of the uranium was accumulated in an early stage of burial, with some much later overprints. None of the uranium concentration and U-series profiles across the root of the tooth complied with a single stage diffusion-adsorption (D-A) model that is used for quality control in U-series dating of bones and teeth. Nevertheless, in the domains that yielded the oldest apparent U-series age estimates, U-leaching could be excluded. This means that the oldest apparent U-series ages of around 200 ka represent a minimum age for this Neanderthal specimen. This is in good agreement with independent age assessments (200-230 ka) for the archaeological layer, in which it was found.The Th elemental concentrations in the dental tissues were generally low (between about 1 and 20 ppb), and show little relationship with the nature of the tissue. 相似文献
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《Quaternary Science Reviews》2003,22(10-13):1367-1372
An additional method of coupled ESR/U-series dating is developed for teeth showing post-depositional U-loss. The fundamental parameter for the dose rate calculation is the present-day 230Th-activity because of the geochemical immobility of thorium. Uranium and thorium concentrations are measured by thermal ionization mass spectrometry (TIMS). Due to the unknown uranium history an average saturation uptake of uranium is assumed leading to an average development of U-series activities. Therewith an internal dose rate and the age T can be calculated on condition that the modelled 230Th-activity at time T corresponds with the measured value. Using this new method, teeth, found in archaeological sites in France (Gramat, Bramefond), could be dated even though they show U-loss after U-uptake. Two teeth from Gramat could be dated to 128.3±8.6 and 130.5±10 ka. Two teeth from Bramefond have ages of 104.4±8.4 and 115.1±10.2 ka. Both sites can be ascribed to oxygen isotope stage 5. 相似文献
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用热电离质谱仪检测负离子，因技术上的原因，一直是国际质谱界关注的热点问题之一。近几年来，在此领域的探索取得突破，发展迅速。新型号的质谱上已大量使用这一技术。国内也填补了这一领域的空白，并将这一技术成功运用于老质谱仪的升级改造。本文重点阐述了作者本人在探索过程中遇到的疑难问题及解决问题的有效方法。 相似文献