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1.
Various zircons of Proterozoic to Oligocene ages (1060-31 Ma) were analysed by laser ablation-inductively coupled plasma-mass spectrometry. Calibration was performed using Harvard reference zircon 91500 or Australian National University reference zircon TEMORA 1 as external calibrant. The results agree with those obtained by SIMS within 2s error. Twenty-four trace and rare earth elements (P, Ti, Cr, Y, Nb, fourteen REE, Hf, Ta, Pb, Th and U) were analysed on four fragments of zircon 91500. NIST SRM 610 was used as the reference material and 29Si was used as internal calibrant. Based on determinations of four fragments, this zircon shows significant intra-and inter-fragment variations in the range from 10% to 85% on a scale of 120 μm, with the variation of REE concentrations up to 38.7%, although the chondrite-normalised REE distributions are very similar. In contrast, the determined age values for zircon 91500 agree with TIMS data and are homogeneous within 8.7 Ma (2 s ). A two-stage ablation strategy was developed for optimising U-Pb age determinations with satisfactory trace element and REE results. The first cycle of ablation was used to collect data for age determination only, which was followed by continuous ablation on the same spot to determine REE and trace element concentrations. Based on this procedure, it was possible to measure zircon ages as low as 30.37 0.39 Ma (MSWD = 1.4; 2 s ). Other examples for older zircons are also given.  相似文献   

2.
胡志中  王坤阳  晏雄  杨波  杜谷 《岩矿测试》2020,39(6):804-815
激光剥蚀电感耦合等离子体质谱(LA-ICP-MS)是目前锆石研究常用方法之一,该法普遍采用环氧树脂靶为载体,对锆石环氧树脂靶表面形貌及平整度影响进行研究,有助于评估其制作工艺以及LA-ICP-MS锆石分析的准确性。本次研究采用原子力显微镜(AFM)对锆石环氧树脂靶表面进行形貌分析,并通过分析和对比193nm激光不同剥蚀模式和不同剥蚀条件下的锆石表面形貌,研究锆石表面形貌及平整度对LA-ICP-MS锆石分析的影响;同时实验采用氩离子抛光技术对锆石环氧树脂靶进行二次抛光,并探讨该技术对锆石环氧树脂靶影响。实验结果表明本次靶中表面总体平整性较好但存在细微的不平,锆石表面存在程度较小(几至几十纳米的不等)的擦痕,锆石颗粒边缘与靶面存在高差和间隙;而通过研究后认为锆石表面细微的不平对于分析的影响小于能量密度、频率、移动速率等其他激光参数的影响,对分析准确性的影响较小。实验分析并对比了锆石和玻璃标准等不同基体的线扫描形貌,发现其剥蚀深度以及剥蚀形貌存在差异,相同剥蚀条件下线扫描剥蚀深度:NIST610 > CGSG系列 > 锆石91500。经氩离子二次抛光后锆石样品表面擦痕不明显,但可能会对锆石造成损伤等影响。本次研究认为锆石环氧树脂靶表面总体平整性较好,锆石表面细微的不平对分析准确性的影响较小,不同基体的线扫描形貌研究则为LA-ICP-MS锆石及其他分析提供了参考,而氩离子抛光技术对LA-ICP-MS分析的影响及应用还有待进一步的研究。  相似文献   

3.
Zircon geochemistry can vary over micrometre scales; therefore, natural reference materials need to be well characterised before being used to calculate trace element mass fractions in unmeasured samples. Moreover, reference material homogeneity needs to be ensured with the accelerating rate of geoanalytical developments to map mineral chemistry at increasingly finer scales. Here, we investigate trace element zoning in four widely used zircon reference materials: 91500, Mud Tank, Temora and Plešovice, as well as zircon crystals from the Mount Dromedary/Gulaga Igneous Complex, Australia. Sub-micrometre resolution focused ion beam scanning electron microscope (FIB-SEM) based time-of-flight secondary ion mass spectrometry (ToF-SIMS) and 5 μm resolution LA-ICP-MS mapping show that trace elements are zoned in all reference materials, though 91500 exhibited the least zonation. We demonstrate that FIB-SEM-based ToF-SIMS can rapidly resolve variations in trace elements (e.g., U, Th, Sc, Y, Gd, Dy, Yb and Li) at sensitivities down to the μg g-1 level with a spatial resolution of 195 nm for areas 100 × 85 μm to 959 × 828 μm. Zircon 91500 is recommended for future quantitative analyses provided that (1) the spatial distribution of elements is imaged before analysis of unknown samples and (2) it is used in conjunction with a doped glass as the primary reference material.  相似文献   

4.
There is a growing need for new zircon reference materials for in situ Hf-isotope analysis by laser ablation-multicollector inductively coupled plasma-mass spectrometry (LA-MC-ICP-MS). In this contribution we document the results of a preliminary investigation of seven natural zircons, conducted in order to test their suitability in this regard. Solution MC-ICP-MS data on separated Lu and Hf fractions provided reference compositional data while the results of ca. 750 in situ LA-MC-ICP-MS analyses allowed assessment of potential micrometre-scale heterogeneity. On the basis of these analyses and additional relevant considerations such as availability, size and (Lu)Yb/Hf ratio, we suggest that, of the currently available zircons, Temora-2 and Mud Tank are most likely to provide robust reference materials for Hf isotope determinations both at the present time and into the future. The former has the advantage of also being well-characterised for U-Th-Pb systematics and suitable for in situ age determination, while the latter is the most readily available and is of very large grain size. Additional materials such as BR266, and 91500, although limited in supply, show more consistent Lu/Hf ratios and are thus of use in monitoring elemental fractionation during ICP-MS analysis.  相似文献   

5.
Analytical protocols for SHRIMP‐SI oxygen isotope analysis (δ18O) of a suite of zircon reference materials (RMs) are presented. Data reduction involved a robust estimate of uncertainties associated with the individual spot as well as for groups where the spot data are combined. The repeatability of δ18O measurements is dependent on both the analytical conditions and the choice of the primary reference material. Under optimised conditions, repeatability was often better than 0.4‰ (2s) allowing sample uncertainties to be obtained to better than 0.2‰ (at 95% confidence limit). Single spot uncertainty combined the within‐spot precision with the scatter associated with repeated measurements of the primary zircon reference material during a measurement session. The uncertainty for individual spots measured under optimised conditions was between 0.3 and 0.4‰ (at 95% confidence). The analytical protocols described were used to assess a variety of zircon RMs that have been used for geochronology and for which laser fluorination oxygen isotope data are available (Temora 2, FC1, R33, QGNG and Ple?ovice), as well as zircons that have been used as RMs for trace element or other types of determination (Mud Tank, Monastery, 91500, AS57, AS3, KIM‐5, OG1, SL13, CZ3 and several other Sri Lankan zircons). Repeated analyses over nine sessions and seven different mounts show agreement within analytical uncertainty for Temora 2, FC1, R33, QGNG, Ple?ovice and 91500, when normalised to Mud Tank. For existing ion microprobe mounts with these materials, an appropriate δ18O can be determined. However, care should be taken when using zircons from the Duluth Complex (i.e., FC1, AS57 and AS3) as reference materials as our data indicated an excess scatter on δ18O values associated with low‐U zircon grains.  相似文献   

6.
《Chemical Geology》2002,182(2-4):179-194
A technique using isotope-ratio-monitoring gas chromatography-mass spectrometry (irmGCMS) and excimer laser fluorination for in situ oxygen isotope analysis of silicates is described. The irmGCMS and oxygen extraction line is connected by a newly developed interface, reducing the time for a single analysis to less than 10 min. The precision obtained for δ18O is similar to what has been reported for excimer laser fluorination using dual inlet systems. δ18O values of two olivine standards had 1σ precision of ±0.14‰ (n=19 and n=10) and that of Dörentrup quartz had ±0.17‰. Eleven analyses of a large zircon crystal had a precision of ±0.12‰. However, between 300 and 600 nmol oxygen was liberated for a single analysis, equivalent to cylindrical laser holes 250 to 350 μm in diameter and depth. In the future it will be feasible to measure the isotope ratio of cylindrical volumes 150 μm in diameter simply by reducing the volume of the extraction line. While this is still significantly larger than what is possible with ion probes, the ratios obtained by excimer laser-irmGCMS are highly accurate and precise without correction. The value of this technique for in situ oxygen isotope measurements is demonstrated with two rock slabs from metamorphic rocks of the Dabie–Sulu ultra-high-pressure belt, China.  相似文献   

7.
Secondary ion mass spectrometry (SIMS) requires matrix‐matched reference materials to calibrate mass fractionation during oxygen isotope measurement. Over one thousand SIMS oxygen isotope measurements were conducted on eleven natural mineral samples (five olivines, three clinopyroxenes and three orthopyroxenes) in nineteen sessions using CAMECA IMS 1280 SIMS instruments to evaluate their potential as SIMS reference materials. The obtained results reveal oxygen isotope homogeneity of these samples. No matrix effect was measured for the same variety of mineral samples with limited Mg‐number variations (89.6–94.2, 90–91.9 and 90.1–92.1 for olivine, clinopyroxene and orthopyroxene, respectively). The recommended oxygen isotope compositions of these samples were determined using laser fluorination. These samples are therefore suitable to be used as reference materials for in situ oxygen isotope microanalysis.  相似文献   

8.
UV Laser Ablation ICP-MS: Some Applications in the Earth Sciences   总被引:4,自引:0,他引:4  
This study reports a series of applications of UV laser ablation ICP-MS in the geological sciences. The advantages and disadvantages of the PQ "S" option and the use of nitrogen in the carrier gas are discussed. A general problem common to all ablation techniques is the calibration technique and experiments involving synthetic calibration samples are covered. Zircon geochemistry and geochronology by LA-ICP-MS are discussed and data are presented for REE, Hf and U for a standard zircon (91500) as well as a series of zircons from Zimbabwe. The potential of using Ce and Eu anomalies in petrologic studies is illustrated by zircons from a fractionated gabbroic-granite in the Urals. The potential of the LA-ICP-MS method to utilise standard X-ray fluorescence glass discs is demonstrated as a useful semi-quantitative tool in determining REE patterns. LA-ICP-MS is a powerful tool in the analysis of the platinum group elements (and Re) and some examples are given in the successful application of the technique to partitioning in iron meteorites.  相似文献   

9.
In this contribution we evaluate the capabilities of laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) using a 12 μm spot size. Precision, accuracy and detection limits were assessed on the USGS BCR-2G reference material. We demonstrate that the 12 μm LA-ICP-MS analyses of experimentally-grown amphibole and garnet are in excellent agreement with secondary ion mass spectrometry (SIMS) trace element determinations on the same crystals. The 12 μm spot size configuration was subsequently used to determine trace element crystal-melt partition coefficients (Dc/m) for a wide range of trace elements in amphibole in equilibrium with a basanitic melt. The following strategy to determine accurately and evaluate Dc/m is proposed. One or more major elements determined previously by electron probe microanalysis (EPMA) was used to ensure consistency between EPMA and the composition of the aerosol produced by the laser ablation. Measured Dc/m values were successively evaluated using the lattice strain model. The use of this strategy significantly improved the precision and accuracy of Dc/m determination when a LA-ICP-MS configuration with a high spatial resolution was employed.  相似文献   

10.
湖南锡田花岗岩锆石U-Pb年代学及钨锡成矿时代的探讨   总被引:3,自引:3,他引:0  
华南是世界上最大的花岗岩省之一,其中中生代花岗岩最为发育,与之相伴生的是大量钨锡多金属矿床,花岗岩的成因演化因与这些矿床的成矿作用密切相关而备受关注。湖南锡田花岗岩体是该区的一个典型岩体,主要由黑云母花岗岩、黑云母二长花岗岩和细粒花岗岩组成,并伴生有钨锡矿床。本文以湖南锡田花岗岩体为研究对象,对其中不同类型的岩石进行了详细的岩石学和锆石SIMS与LA-ICP-MS U-Pb定年工作。分析结果表明,锡田花岗岩体存在晚三叠世(227~233Ma)和晚侏罗世(150~154Ma)两期岩浆活动,早期的岩浆活动主要分布在岩体北部和中部,晚期岩浆活动仅在岩体中部及东部矿体附近可见,两期岩浆活动具有相同的岩性组合。另外,对含矿花岗岩的锆石U-Pb定年结果表明该地区可能存在晚三叠世的成矿作用,结合前人的工作推断锡田地区钨锡矿的形成受晚三叠世和晚侏罗世两期岩浆事件的影响。  相似文献   

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