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1.
作者在昆士兰大学利用多接收等离子质谱仪MicromassIsoprobe测定了7种USGS岩石参考标准AGV-1、AGV-2、BHVO-1、BHVO-2、BCR-2、BIR-1/1和W-2的Pb同位素组成,同时测定了标准物质NBS981的Pb同位素组成。采用~(203)Tl-~(205)Tl同位素作为内部标准进行同位素分馏校正。所获得达到NBS981和USGS岩石标准AGV-1、BHVO-1的同位素比值的精度可与热电离质谱双稀释剂法或三稀释剂法数据相媲美,甚至具有更高精度。而BHVO-2、AGV-2和BCR-2  相似文献   

2.
王林森  张利 《矿物岩石》2003,23(2):44-48
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   

3.
LA-MC-ICP-MS锆石微区原位U-Pb定年技术   总被引:297,自引:33,他引:264  
利用激光多接收等离子体质谱(LA-MC-ICP-MS)技术对30~1 065 Ma的系列锆石进行了详细的定年研究.包含离子计数器的多接收系统使得不同质量数的同位素信号可以同时静态接收,并且不同质量数的峰基本上都是平坦的,进而可以获得高精度的数据,均匀锆石颗粒207Pb/206Pb、206Pb/238U、207Pb/235U比值的测试精度(2σ)均为2%左右,对锆石标准的定年精度和准确度在1%(2σ)左右;不同质量数同位素信号的同时静态接收使得剥蚀时间缩短,剥蚀深度变浅,相比LA-ICP-MS方法,提高了激光剥蚀的空间分辨率.对5个锆石标准和2个实际样品的测试表明,206Pb/235U年龄测定误差在1%(2σ)以内,定年结果在误差范围内与前人报道值完全一致,测试精度达到国际同类实验室先进水平.  相似文献   

4.
MC-ICP-MS高精度测定Pb同位素比值   总被引:1,自引:1,他引:1  
多接收器等离子体质谱是近年发展起来的高精度同位素分析手段之一,通过用等离子体质谱测量Pb国际标准物质NBS981和NBS982,显示出多接收器等离子体质谱分析Pb同位素的优势。利用205Tl/203Tl进行作为内标,可以实现Pb同位素的质量分馏校正,极大地提高了Pb同位素分析的重现性。相比较热电离质谱,该方法精度更高,样品的用量更少,测试时间更短,多接收器等离子体质谱测定Pb同位素技术有良好的应用前景。  相似文献   

5.
刘建辉 《岩矿测试》2012,31(4):597-601
在SHRIMP锆石U-Pb同位素定年中,常用实测的204Pb校正普通铅,然后求得206Pb/238U、207Pb/206Pb等同位素比值及年龄。本文主要论述了普通铅204Pb校正的原理、来源、测定方法及其对实验结果的影响。通过实验得出普通铅204Pb测定结果不准确,会使数据在谐和图中的投影点偏离谐和线,使年龄结果偏离真实值。影响普通铅204Pb的因素有很多,主要有测试位置是否有包体或裂纹、锆石表面的清洁程度、普通铅204Pb的峰位置是否正确等;此外,一次离子束强度、密度均匀性、束斑形状、清洗时间也可能有影响。由于大多锆石样品中普通铅204Pb含量很低,在扫描普通铅204Pb峰中心时,最好在高铀锆石包体、裂隙处,或在长石等含普通铅204Pb较高的矿物上进行,同时为了避免受质量数204左侧峰拖尾叠加的影响,通常把204Pb峰位置设定在峰中心稍偏右处。  相似文献   

6.
梁清玲  江思宏  刘翼飞 《地质论评》2013,59(6):1119-1130
本文对河北丰宁地区前人所定的东猴顶正长斑岩和石英正长斑岩进行了岩石学、锆石U Pb年代学、元素地球化学以及Sr—Nd—Pb—Hf同位素分析。LA MC ICP MS锆石U Pb测年和岩石学显示东猴顶岩体为早白垩世(~129Ma)钾长花岗斑岩,而非前人认为的侏罗纪—白垩纪正长斑岩和石英正长斑岩。东猴顶岩体具有高硅(6907%~7300%)、富碱(Na2O+K2O:900%~1056%)和FeO(全铁)/MgO比值大的特征,属高钾钙碱性系列;岩石富集轻稀土,负铕异常明显(δEu:025~041),相对富集K、Rb等大离子亲石元素和Zr、Hf、Th、U、Y等高场强元素,亏损Ca、Ba、Sr、P、Ti、Cr、Ni、Co等元素,Ga/Al比值高,具A型花岗岩特征,可能形成于伸展环境构造体制。岩体n(87Sr)/n(86Sr)i=070815~071197,εNd(t)值为-132~-168,对应的二阶段模式年龄(T2DM)为20~23Ga;全岩n(206Pb)/n(204Pb)i=16745~16765,n(207Pb)/n(204Pb)i=15372~15394,n(208Pb)/n(204Pb)i=37706~37794;锆石Hf同位素组成为εHf(t)值=-207 ~ -92,二阶段模式年龄(TDMC)为19~26 Ga。同位素特征表明岩体源岩可能主要来自壳源物质。考虑到华北克拉通东部地壳生长的主要时期为新太古代,因此,东猴顶岩体的岩浆来源于太古代地壳物质和部分亏损地幔物质的混合源区,是华北克拉通北缘中生代岩石圈强烈减薄、地壳伸展作用的结果。  相似文献   

7.
U—Pb同位素测年法及其应用   总被引:3,自引:0,他引:3  
宋忠宝 《西北地质》1998,19(1):68-71
本文介绍了U-Pb同位素体系测年的几种方法,并对各种方法的适用性和应用前景进行了讨论,认为高灵敏度高分辨率离子探针质谱法仍是当今世界上最先进的测年方法,单颗粒锆石Pb-Pb蒸发法和单颗粒锆石U-Ph同位素稀释法仍是目前和今后一段时期内广泛应用的测年方法。最后对U-Pb同位素测年的年龄数据的地质解释进行了探讨。  相似文献   

8.
采用双带测量方式,法拉第杯和离子计数器同时接收与跳峰接收相结合,建立了超微量钐同位素的热表面电离质谱的测量方法。优化了制样程序和质谱测量程序,研究了蒸发带电流对离子流强度的影响,考察了从纳克至微克不同样品用量的测量效果及其中Nd、Eu干扰核素的情况。对4 ng~2μg的天然丰度钐样品进行了同位素比值分析,相对标准偏差均小于1.1%。  相似文献   

9.
LA-MC-ICP-MS锆石Hf同位素的分析方法及地质应用   总被引:68,自引:111,他引:68  
本研究利用Thermo Finngan Neptune型多接收等离子质谱和Newwave UP213 激光剥蚀系统对两个国际锆石标准和一个实验室锆石标准进行了系统的测定.测得的TEMORA、GJ1和FM02锆石标准的176Hf/177Hf比值分别为0.282700±64(2SD,N=22),0.282008±25(2SD,N=26)和0.282967±44(2SD,N=27),该结果在误差范围内与文献报道值完全一致.采用不同的剥蚀直径对FM02锆石标准进行了对比测定,结果在误差范围内是一致的.从分析结果来看,GJ1和FM02的Hf同位素比值变化范围较小,是Hf同位素LA-MC-ICP-MS测试的理想标准锆石.文中还对四个不同地区的锆石Hf同位素进行了测定,结合前人研究,对其成因和物质来源进行了初步探讨.  相似文献   

10.
S型花岗岩中含有残留锆石并经历过后期Pb丢失事件是一个较普遍的现象,这使得其钻石U-Pb体系呈现出复杂的多阶段演化特征。虽然离子探针对各种复杂锆石U-Pb体系定年最为有效,但因其昂贵的成本使其应用受到限制,目前较为常用的仍是常规化学-质谱分析方法。在现有实验室Pb本底水平上恰当地选择单颗或多颗粒锆石进行分析,是获得高质量U-Pb年龄数据的关键。桂北三防岩体含有残留锆石并经历过后期Pb丢失事件,使其锆石U-Pb体系具有三阶段演化的特征。离子探讨和多颗粒锆石化学-质谱两种分析方法得出了一致的207Pb/206Pb年龄为820±9Ma,代表了岩体的形成年龄。而过去用常规微量锆石化学-质谱法得到的年龄(899Ma)实际上是一个无地质意义的“上交点年龄”。  相似文献   

11.
The development of the MC-ICP-MS method, which was launched about one decade ago and was largely stimulated by the need to solve geological problems, has opened a new avenue in isotope mass spectrometry. One of the advantages of this method is the possibility of applying a newly developed approach to the correction of analytical results for the effect of mass discrimination by normalizing the measured isotope ratios of an element to a reference (standard) isotope ratio of another element. This makes it possible to overcome the main disadvantage of conventional thermal ionization mass spectrometry (TIMS), in which the effect of mass discrimination cannot be fully taken into account during isotope analysis, and thus to implement a highly accurate method for the analysis of Pb-isotope composition. In application to the capability of the NEPTUNE MC-ICP mass spectrometer, we optimized and calibrated a method for high-accuracy Pb isotope analysis in solutions spiked with Tl, with all currently measured Pb-isotope ratios normalized to the standard 205Tl/203Tl ratio (TLN-MC-ICP-MS). The factors affecting the random and systematic analytical errors were examined, and the optimal operating regime and analytical conditions were determined. Much attention was paid to the correlation of the measurement results and the mass discrimination effect determined from the 205Tl/203Tl ratio. The value of the 205Tl/203Tl normalizing ratio was analytically determined through isotope analyses of the NIST SRM 981, and SRM 982 standard samples of Pb-isotope composition. The data obtained for two mixtures Tl + Pb (SRM 982) and Tl + Pb (SRM 981) in ten replicate analyses were 2.38898 ± 12 and 2.38883 ± 20, respectively. These results are in good mutual agreement, and their general mean 205Tl/203Tl = 2.3889 ± 1 coincides (within the error) with the recently published values of 2.3887 ± 7 [Collerson et al., 2002] and 2.3889 ± 1 [Thirlwall, 2002]. The precision of the method (±2SD), which was assayed by the long-term reproducibility of the results of replicate analyses of SRM 981 and seven galena samples (90 analyses) was 0.016–0.018% for the 206Pb/204Pb, 207Pb/204Pb, and 208Pb/204Pb ratios and 0.005 and 0.009% for the 207Pb/206Pb and 208Pb/206Pb ratios, respectively. The precision of the isotope analysis of common Pb was significantly improved (by factors of 6–10 for various isotope ratios) compared with the precision of TIMS techniques acceptable in isotope studies during three decades. The described method was applied to examine the Pb-isotope composition of approximately 250 samples of galena, scheelite, and pyrite from a number of well known (including large) gold, sulfied, and base-metal deposits. The precision of the method (0.01–0.02%) makes it possible to study small inter-and intra-phase differences in Pb-isotope ratios in hydrothermal and magmatic rocks, to assay the scale of regional and variations in the isotope composition of ore Pb, and to correlate the Pb-isotope composition of rocks and ores and reveal its evolutionary trends.  相似文献   

12.
The authors measured Pb isotope compositions of seven USGS rock reference standards, i.e. AGV-1, AGV-2, BHVO-1, BHVO-2, BCR-2, BER-1/1 and W-2, together with NBS 981 using a micromass isoprobe multi-collector inductively-coupled plasma mass spectrometer (MC-ICP-MS) at the University of Queensland. 203Tl-205Tl isotopes were used as an internal standard to correct for mass-dependant isotopic fractionation. The results for both NBS 981 and USGS rock standards AGV-1 and BHVO-1 are comparable to or better than double- and triple-spike TIMS (thermal ionization mass spectrometry) data in precision. The data for BHVO-2 and, to a lesser extent, AGV-2 and BCR-2 are reproducibly higher for 206Pb/204Pb, 207Pb/204Pb and 208Pb/204Pb than double-spike TIMS data in the literature. The authors also obtained the Pb isotope data for BIR-1/1 and W-2, which may be used as reference values in future studies. It is found that linear correction for Pb isotopic fractionation is adequate with the results identical to those corre  相似文献   

13.
为了明确内蒙古别鲁乌图铜多金属矿床的成矿年龄与矿床成因,对该矿床中与成矿关系密切的流纹岩进行了锆石U-Pb年龄以及主要金属硫化物的S、Pb同位素测试。其中流纹岩的锆石206Pb/238U加权平均年龄为(271.7±1.6)Ma(MSWD=1.02),显示成矿作用发生于二叠纪。金属硫化物的S同位素分析结果显示δ34SV-CDT值分布在-0.6‰~1.0‰之间,平均为0.49‰,变化范围较窄,显示S的来源单一;Pb同位素组成比较集中,206Pb/204Pb为18.207~18.674,207Pb/204Pb为15.620~15.699,208Pb/204Pb为38.144~38.790,具有壳幔混源的特征。S、Pb同位素特征均指示成矿物质主要来源于岩浆热液。结合区域地质、矿床地质、空间分带等特征以及S、Pb同位素组成可知,别鲁乌图铜多金属矿床为VHMS型矿床,形成于二叠纪陆缘弧裂谷中。  相似文献   

14.
We introduce a potential new working reference material – natural zircon megacrysts from an Early Pliocene alkaline basalt (from Penglai, northern Hainan Island, southern China) – for the microbeam determination of O and Hf isotopes, and U–Pb age dating. The Penglai zircon megacrysts were found to be fairly homogeneous in Hf and O isotopes based on large numbers of measurements by LA-multiple collector (MC)-ICP-MS and SIMS, respectively. Precise determinations of O isotopes by isotope ratio mass spectrometry (IRMS) and Hf isotopes by solution MC-ICP-MS were in good agreement with the statistical mean of microbeam measurements. The mean δ18O value of 5.31 ± 0.10‰ (2s) by IRMS and the mean 176Hf/177Hf value of 0.282906 ± 0.0000010 (2s) by solution MC-ICP-MS are the best reference values for the Penglai zircons. SIMS and isotope dilution-TIMS measurements yielded consistent 206Pb/238U ages within analytical uncertainties, and the preferred 206Pb/238U age was found to be 4.4 ± 0.1 Ma (95% confidence interval). The young age and variably high common Pb content make the Penglai zircons unsuitable as a primary U–Pb age reference material for calibration of unknown samples by microbeam analysis; however, they can be used as a secondary working reference material for quality control of U–Pb age determination for young (particularly < 10 Ma) zircon samples.  相似文献   

15.
The internal precision of Pb isotope analyses using single-zircon evaporation in a double-filament solid source mass spectrometer (Kober 1986) can be improved combining the evaporation of Pb directly from the single grain with a suitable Pb+ emitter-bedding technique. This is most easily done by step-wise evaporating the investigated grain at temperatures of 1700–1800 K generating on the ‘cold’ ionization filament a deposit of radiogenic Pb together with further elements and compounds derived directly from the crystal. The heating of the deposit on the ionization filament to 1400–1500 K results in long-lived and stable Pb+ ion beams. The ‘activating reagents’ in the deposit are HfO2 and SiO2. Their release from the zircon grain together with the radiogenic Pb, which presumably is sited in the crystalline zircon domains as Pb4+, is probably due to disintegration reactions of trace-element silicates hosted in the grain. In the bedding deposited on the ionization filament thermally stable Pb/Hf/SiO2 compounds are formed (PbHfSiO5(?)). They retain the Pb isotopes on the (Re) filament up to 1400 K–1500 K and are highly efficient Pb+ ion emitters similar to the ‘Si-gel’-method (Cameron et al. 1969). The combined evaporation/emitter-bedding technique has been applied to natural zircons of different genesis and to isotope standards. Routinely, a Pb+ ion yield of 2*10?4-1*10?3 and a relative standard deviation of the 207Pb/206Pb ratio in the order of 1% have been obtained for sub-ng- to ng-amounts of Pb from standards and samples. The method rapidly can yield Pb isotope information on the ‘concordant’ zircon phases with a standard deviation of ±15–20 Ma of the derived ages also in the case of Paleozoic zircon populations.  相似文献   

16.
This paper evaluates the analytical precision, accuracy and long‐term reliability of the U‐Pb age data obtained using inductively coupled plasma–mass spectrometry (ICP‐MS) with a frequency quintupled Nd‐YAG (λ = 213nm) laser ablation system. The U‐Pb age data for seven standard zircons of various ages, from 28 Ma to 2400 Ma (FCT, SL13, 91500, AS3, FC1, QGNG and PMA7) were obtained with an ablation pit size of 30 μm diameter. For 207Pb/206Pb ratio measurement, the mean isotopic ratio obtained on National Institute of Standards and Technology (NIST) SRM610 over 4 months was 0.9105 ± 0.0014 (n = 280, 95% confidence), which agrees well with the published value of 0.9096. The time‐profile of Pb/U ratios during single spot ablation showed no significant difference in shape from NIST SRM610 and 91500 zircon standards. These results encouraged the use of the glass standard as a calibration standard for the Pb/U ratio determination for zircons with shorter wavelength (λ = 213 nm) laser ablation. But 206Pb/238U and 207Pb/235U ages obtained by this method for seven zircon standards are systematically younger than the published U‐Pb ages obtained by both isotope dilution–thermal ionization mass spectrometry (ID‐TIMS) and sensitive high‐resolution ion‐microprobe (SHRIMP). Greater discrepancies (3–4% younger ages) were found for the 206Pb/238U ages for SL13, AS3 and 91500 zircons. The origin of the differences could be heterogeneity in Pb/U ratio on SRM610 between the different disks, but a matrix effect accuracy either in the ICP ion source or in the ablation‐transport processes of the sample aerosols cannot be neglected. When the 206Pb/238U (= 0.2302) newly defined in the present study is used, the measured 206Pb/238U and 207Pb/235U ages for the seven zircon standards are in good agreement with those from ID‐TIMS and SHRIMP within ±2%. This suggests that SRM610 glass standard is suitable for ICP‐MS with laser ablation sampling (LA‐ICP‐MS) zircon analysis, but it is necessary to determine the correction factor for 206Pb/238U by measuring several zircon standards in individual laboratories.  相似文献   

17.
利用新型阴离子交换树脂分离沉积物中的重金属Pb,采用表面热电离质谱法(TIMS)测定了沉积物样品中的Pb同位素组成。新型树脂为大孔径阴离子树脂AG-MP-1M,淋洗液采用低浓度的盐酸,避免了使用难以纯化的氢溴酸,可有效地降低试剂空白。通过对铅同位素标准物质NIST NBS-981的重复测试,方法的精密度(<0.5%,2s)和准确度均达到了应用研究的要求。对5个实际沉积物样品中的铅同位素组成进行测定,获得了理想的分析效果。  相似文献   

18.
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 205pb-204pb 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 207Pb-204Pb 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 205pb-204pb, 230Th and 235U 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   

19.
Inductively coupled plasma-mass spectrometry (ICP-MS) is capable of measuring isotopic and elemental abundances in geologic materials easily and rapidly. Although the precision of isotope ratio data obtained by ICP-MS is inferior to that by thermal ionization mass spectrometry, it is adequate for application to a number of geochemical exploration problems.National Institute of Standards and Technology (NIST) Pb metal standard reference material 981 (NBS981), was used as the isotopic standard to correct the measured isotope intensities for mass discrimination. The mean relative standard deviation (RSD) of the determinations of the abundances of 206Pb, 207Pb, and 208Pb in the two other NIST Pb isotope reference materials, NBS981 and NBS982, was better than 0.3%, whereas the RSD for the determination of the less abundant 204Pb was 0.4%. Accuracy was demonstrated by repeated analysis of NBS981, NBS982, and NBS983. The Student t-statistic ranged between −1.75 and 2.04 for the abundances of the 4 Pb isotopes in the three NIST materials.Data from a suite of 13 uraninite-rich samples from Labrador demonstrate the ability of ICP-MS to determine age and geochemical information sufficient for regional interpretations. The determined radiogenic 207Pb/206Pb ratios of 12 of the samples give ages between 1697 and 1805 Ma with average uncertainties (one standard deviation) of 4 Ma, whereas one of the samples has an age of 495 ± 4 Ma. The average age of the 12 samples was 1752 ± 27 Ma. Along with the Pb isotope intensities, 232Th and 238U were measured and the U-Pb age determined from a fit of the 206Pb/238U vs. 207Pb/235U for 9 of the samples. The concordia intercept age of 1740 Ma for the best-fit line is in good agreement with the mean 207Pb/206Pb age of 1752 Ma.  相似文献   

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