共查询到18条相似文献，搜索用时 609 毫秒
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随着超净化实验室条件的完善以及多接收同位素质谱技术的成熟，铅同位素双稀释法倍受关注。用双稀释法测定铅同位素比值的方法原理，以及^204Pb—^207Pb双稀释剂的配制和标定方法。通过对标准物质NBS981和地质样品的分析测定，表明用双稀释法测定铅同位素比值，可以有效校正由质谱分析造成的同位素分馏效应，从而提高分析结果的精度和准确度。 相似文献
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多接收器等离子体质谱精确测定铼含量及其同位素丰度 总被引：5，自引：2，他引：5
利用多接收器等离子体质谱建立了快速精确测定铼含量及其同位素丰度的方法。溶液中加入铱元素进行铼同位素的质量分馏校正,在常规的溶液雾化进样条件下,采用同位素稀释法可准确测定纳克级的铼含量。铼标样A的自然同位素丰度的测量结果为185Re(37.437±0.008)%、187Re(62.563±0.008)%(2σ,n=5);铼稀释剂的同位素丰度测量结果为185Re(5.576±0.018)%、187Re(94.424±0.018)%(2σ,n=7);与未进行分馏校正的同位素组成的测量结果相比,精度和准确度均有提高。利用同位素稀释法测得铼标样A的浓度为(516.48±0.35)ng/g(2σ,n=5);测量精度和准确度均优于0.10%;利用反同位素稀释法对铼稀释剂B进行了详细的测量,平均测量结果为(62.74±0.26)ng/g(2σ,n=15),在分析误差范围内与其标定值完全一致;与未进行分馏校正的浓度测量结果相比,铼同位素丰度及铼含量的测量准确度均明显提高。 相似文献
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Re-Os同位素定年方法进展及ICP-MS精确定年测试关键技术 总被引：8，自引：0，他引：8
本文介绍了Re-Os同位素定年的基本原理、技术发展及应用现状;综述了样品分解和Re-Os分离富集的主要方法,重点对ICP-MS法进行Re-Os同位素定年做了较详尽的介绍,包括质量分馏校正、干扰校正、含量初测、取样量的确定、稀释剂的稀释比及稀释剂加入量等,以确保高精度测试;评述了ICP-MS最常见的测定对象-辉钼矿中Re-Os的失耦现象及降低其对Re-Os同位素定年影响的对策,文中描述了由测定同位素比值计算含量时的误差传递公式并重申了最佳稀释比。最后,指出了Re-Os同位素定年方法研究中应该关注的工作方向。 相似文献
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《地球化学》2017,(1)
为了更好地实现Re-Os同位素实验室之间数据比对,本实验室在了解国内外部分实验室的数据处理方法的基础上,提出了本实验室的N-TIMS Re、Os同位素计算方法。本文所涉及到的Re、Os同位素计算方法包括氧同位素干扰校正、Re同位素比值和含量计算、Os同位素测定质量分馏校正方法、三峰法和全峰法Os同位素比值和含量计算、测定结果的不确定度、Isoplot作图基本参数介绍和相关系数Rho的计算。对于辉钼矿和普通Os信号弱(~(187)Os/~(188)Os2000)的样品适合采用三峰法计算Os同位素比值,普通Os信号强(~(187)Os/~(188)Os2000)的样品应该采用全峰法计算同位素比值。在全峰法计算中,按照指数分馏规律以迭代计算方式校正Os同位素比值的质量分馏,采用5iso方法进行样品中Os和稀释剂中Os的摩尔比(N_(5iso)/S)_(Os)的计算。 相似文献
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《矿物岩石地球化学通报》2016,(1)
随着MC-ICP-MS的推广使用,同位素双稀释剂法在国际上已被广泛用于非传统稳定同位素领域中低浓度元素同位素组成的高精度分析,其可有效校正化学纯化和质谱测定过程中的同位素质量分馏,但该方法在国内还未得到全面应用。制约该方法使用的关键在于难以掌握两单稀释剂间(λ)以及双稀释剂与样品之间(p)的最优配比值。本文以Siebert等(2001)的几何迭代算法为例,详细说明了双稀释剂法的计算流程,提出了定性和定量双稀释剂的选择原则,并以硒同位素为例,说明了两单稀释剂间和双稀释剂与样品间最佳配比值的优化步骤,最后简要说明了双稀释剂组成的标定方法、双稀释剂法的优缺点,以及可用于同位素非质量分馏研究的发展趋势。 相似文献
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用Rb-Sr法测定地质年龄,对地质样品中的锶往往要进行两种同位素分析:非稀释分析以测定87Sr/86Sr比值;稀释分析以测定样品中86Sr的含量。随着稀释剂84Sr丰度的提高,Wasserburg et al.(1964),Van schmus(1965),Wetherill与Bickford(1965)采用了以一代二的办法——用稀释分析既测定含量又测87Sr/86Sr比值。由于稀释剂中84Sr高度富集,87Sr/86Sr受到的影响小,在当时的技术条件下,这些作者没有对一些数据处理进行讨论。但随着计算技术的应用,大大提高了测量精度,稀释剂对87Sr/87Sr的影响则必须加以考虑。 相似文献
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利用MC-ICPMS精确测定143Nd/144Nd和Sm/Nd比值 总被引：43，自引：14，他引：43
多收集器等离子体质谱(MCICPMS)用于分析SmNd同位素时,质量分馏系数(β)与同位素的质量数呈线性关系.可以采用两种方法进行质量分馏校正:双分馏系数内部校正法(DFIC)和单分馏系数外部校正法(SFEC).采用DFIC法,对国际标样ShinEtsuJNdi1和实验室标样NdGIG进行了为期五个月的143Nd/144Nd比值测量统计,结果分别为0.512120±0.000012(2σSD)、0.511532±0.000013(2σSD).采用SFEC法,对NdGIG标样的测量统计结果为0.511525±0.000015(2σSD).两种方法的测量结果在分析误差范围内与其推荐值或TIMS测量值完全一致.对加Ce和Sm的NdGIG混合溶液分别进行了Ce和Sm对143Nd/144Nd比值分析的干扰校正研究和Sm/Nd比值测量,结果显示,143Nd/144Nd比值分别与Ce/Nd、Sm/Nd测量值呈线性关系,Sm/Nd测量值与其质量比值亦呈很好的线性关系.这表明利用MCICPMS可以快速精确地测定存在Ce、Sm干扰的样品的143Nd/144Nd比值,同时可获得精确的Sm/Nd比值,而无需加入稀释剂.这就使直接测定地质样品的SmNd等时线年龄成为可能. 相似文献
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电感耦合等离子体质谱法测量铼和锇同位素比值的质量分馏校正 总被引：3，自引：0，他引：3
用Re标准溶液测定出X Series-7电感耦合等离子体质谱(ICP-MS)检测器的死时间为43ns。由于Re和Ir的对数分馏系数线性相关,可以用Ir对Re进行在线分馏校正。利用配制的Re同位素比值标准溶液检验该方法,大多数校正值对标准值的相对偏差在±0.1%以下。ICP-MS测量时,Os的分馏系数与中位质量数成正比,采用由迭代方法得到的样品和稀释剂混合物的同位素比值(192Os/188Os)mix作为标准化值对其他Os同位素比值进行分馏校正。用已知Os同位素比值的标准溶液对该方法进行检验,结果表明,经校正后,大多数校正值与标准值的相对偏差在±0.3%以下。上述Re-Os同位素分馏校正方法将改善用ICP-MS进行Re-Os定年时的精密度和准确度。 相似文献
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Analysis of noble gases in water using a quadrupole mass spectrometer in static mode 总被引：1，自引：0，他引：1
Jason C. Poole Gavin W. McNeill Stephen R. Langman Frank Dennis 《Applied Geochemistry》1997,12(6):707-714
A quadrupole-based mass spectrometer used in static mode has been employed to determine noble gas concentrations of water samples by isotope dilution. Water samples are degassed and spiked with minor isotopes of each noble gas. After separation of the various gas components, the isotopic ratios are measured in the mass spectrometer. Because a spike is added to each sample, the recovery of each gas component does not have to be quantitative. Equilibration temperatures are calculated from the gas concentrations, based on noble gas solubility data. An accuracy of ±1°C, from the air equilibration temperature, is attainable for air-saturated water samples prepared under controlled conditions in the laboratory. The method has been applied to groundwaters from the London Basin Chalk aquifer. The noble-gas-derived temperatures are consistent with climatic conditions prevailing at the periods of recharge. 相似文献
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Accurate Isotopic and Concentration Analyses of Small Amounts of Pb Using Isotope Dilution Coupled with the Double Spike Technique 总被引：1，自引：0，他引：1
Takeshi Kuritani Tomohiro Usui Tetsuya Yokoyama Eizo Nakamura 《Geostandards and Geoanalytical Research》2006,30(3):209-220
A new method has been developed for the simultaneous determination of Pb abundance and Pb isotopic composition with high precision and accuracy for small test portion masses by thermal ionisation mass spectrometry. In this method, a 205 pb-204 pb double spike is added to samples prior to the chemical separation of Pb, and the isotopic composition of the spike-sample mixture is determined rigorously by the double spike technique using a 207 Pb-204 Pb spike. The isotopic composition and concentration of Pb in the sample are then obtained by utilising the principle of isotope dilution. Using this technique, replicate determinations of Pb from NIST SRM 981 and GSJ JP-1 (peridotite; 0.07 μg g−1 Pb) were performed. The measured concentration and isotopic data were identical, within uncertainty, to published data or to data that were determined independently in this study. The application of this method to U-Pb dating and the determination of the "initial" Pb isotopic composition was also tested. Lead isotopic compositions and the concentrations of Pb, Th and U were determined for a single batch of samples, through the addition of 205 pb-204 pb, 230 Th and 235 U spikes to samples prior to chemical separation. Also in these experiments, we confirmed that this routine gives accurate data for Pb, Th and U concentrations and Pb isotopic compositions. 相似文献
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Bruno Hamelin Gérard Manhes Francis Albarede Claude J. Allègre 《Geochimica et cosmochimica acta》1985,49(1):173-182
A reappraisal of the “Double Spike Method” for correction of the mass discrimination in lead isotope analysis is presented in view of the possible efficiency of this method, especially as related to the improved performance of the new multi-collector mass spectrometers.First, the effects of mass discrimination during lead isotope analysis, using the silica-gel phosphoric acid method, are discussed in order to verify the validity of the linear discrimination law. In this discussion, we give evidence of a slight bias of the isotopic composition of the SRM 981 NBS lead standard, commonly used for mass discrimination calibrations.A rigorous way to deal with the propagation of the within-run statistical errors on the precision of the double spike correction is then presented. This allows the optimization of the parameters of the method (spike isotopic composition and precision, spiking proportion) and the calculation of the respective error associated with each corrected isotopic ratio. The perturbation of the double spike correction due to analytical contamination, which has caused previous failure in the application of the method, is avoided by preparation of the mixture between the spike and the sample at the very end of the chemical separation procedure.Using a single collector mass spectrometer, examples of application on lead standards and on a set of samples suggest a possible improvement in the precision by a factor of 3 compared to the usual method of fractionation normalization and confirm the usefulness of the method with the new generation of mass spectrometers. 相似文献
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The geochemistry of Re-Os and the recent use of Re as a non-traditional stable isotope both need accurate and precise quantification of 187 Re/185 Re ratios. This paper reports rhenium isotopic data obtained from the analysis of a standard solution and geological samples by MC-ICP-MS. We show that measured isotopic ratios are modified by matrix effects that cannot be accounted for by the standard solution bracketing technique. The bias resulting from measurements on a spiked (185 Re-enriched) sample is shown to alter the apparent Re concentration by several percent. When spiking samples and calibrators with tungsten, simultaneous measurement of tungsten and rhenium isotopes compensates for the matrix-induced modification of mass bias. Rhenium and tungsten are shown to have different fractionation factors. This may be due to the fact that the two elements fractionate in a different but systematic way, or that the reference isotopic ratios used for elemental Re and W are incoherent with one another. The consistency of fractionation through time can be used to obtain an empirical relationship between W and Re measured ratios from a standard solution to obtain a sample's fractionation-corrected 187 Re/185 Re spiked ratio on samples containing pg g−1 levels of Re, even if some matrix capable of affecting mass bias remains in the final solution. 相似文献
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位于河南省舞阳县的贾湖遗址是一处著名的新石器时代遗址,距今7800～9000年。遗址中出土了大量的人和动物的骨骼与牙齿,这为研究史前时期中国中部地区人类的迁移情况提供了很好的材料。在本次研究中,共分析了26个人和动物样品,包括12个人体骨密质样品、9个人牙釉质样品和5个猪牙釉质样品。测定了每个样品的锶同位素浓度和87Sr/86Sr比值,结果表明猪牙釉质的锶同位素浓度（平均值为196±51ppm,n=5,1σ）高于人牙釉质的浓度（平均值为110±61ppm,n=9,1σ）,人骨骼的锶同位素浓度（平均值为444±173ppm,n=12,1σ）明显地高于人牙釉质的浓度。根据5个猪牙釉质样品87Sr/86Sr平均值±2倍的标准偏差确定的当地锶同位素比值范围（0.712205～0.712420）,发现14个人类个体中有5个是外来迁入的,并且从第1期到第3期人口的迁移率有增加的趋势。这是在国内首次利用锶位素分析方法对古人类的迁移现象进行研究,同时也表明此方法可以很好地判断古人类迁移行为。 相似文献
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辉钼矿Re-Os同位素定年方法的改进与应用 总被引：13，自引：9，他引：4
公认的Re-Os同位素定年代表物辉钼矿,目前已在金属硫化物矿床年代学研究领域获得了广泛的应用。本研究采用浓HNO3分解辉钼矿样品,大大地简化了Re和Os的化学制备过程,并根据辉钼矿中正常Os含量水平相对放射成因187Os可以忽略的特点,以正常Os标准为稀释剂,实现了仪器测量过程中Os同位素质量分馏的在线校正,改善了分析数据的质量。该方法经辉钼矿国家标准物质进行验证,获得了满意的Re、Os含量及Re-Os年龄数据,并且在南岭地区与连阳复式岩体相关的姓坪夕卡岩型钼矿床成矿年龄研究中获得了成功应用。在实际应用中,为了获得有意义的能反映真实地质事件的年龄数据,辉钼矿样品不仅要有足够的取样量,而且还要保证粒度细、混合均匀。 相似文献
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《Applied Geochemistry》2006,21(5):756-765
The continuous flow elemental analyzer-isotopic ratio mass spectrometer (EA-IRMS) technique provides a significant improvement over conventional extraction methods for the determination of C- and S-isotope ratios in geological materials. It is faster and requires much smaller quantities of material for analysis. Sample preparation is simple, with little or no need for chemical or complete mechanical mineral phase separation, and EA-IRMS sample introduction is rapid. However, because of its simplicity and the fact that data quality depends on the control of a variety of factors, the technique requires rigid adherence to a careful sample analysis protocol.The matching of sample and reference peak heights by sample weight adjustment minimizes non-linearity effects. An accurate calibration should be determined by using standards having a wide range of isotopic compositions, ideally bracketing the samples analysed to both low and high isotopic ratios, and a regular analysis of standards undertaken to maintain the accuracy of the calibration. The calibration equation must be monitored throughout the run by regular analysis of standards, and performance of the Cu-reduction reactor regularly checked to avoid O2 saturation. With this level of attention to analytical detail, measured precision on replicates of isotopic standards is in the order of ±0.1‰ for both C and S isotopic analyses. For S this is a significant improvement over conventional techniques, with 53% of natural samples analysed replicating to better than ±0.1‰. 相似文献