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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.
激光剥蚀-电感耦合等离子体质谱(LA-ICP-MS)技术是目前最常用的锆石U-Pb同位素年龄测定方法之一。该方法能够对单颗粒锆石内部年龄差异实现快速、准确的原位微区分析。文章总结了近年来激光剥蚀系统、ICP-MS技术以及LA-ICP-MS锆石U-Pb定年方法、相关应用实例研究的进展和现状。系统评述了激光发生器,剥蚀池,剥蚀参数(激光波长、脉冲宽度、剥蚀气体、孔径大小)以及四极杆和扇形磁场质谱仪对锆石U-Pb年龄数据的精度和准确度的影响。详细介绍了基于锆石年龄标准样品、标准溶液及其他标样的外标定量校准方法,单个U/Pb比值计算方法,普通铅校正方法以及同位素年龄与微量元素同时测定的方法。目前LA-ICP-MS锆石U-Pb定年技术主要应用于碎屑锆石的沉积物源区示踪和岩浆事件的年代学约束研究。  相似文献   

3.
4.
A direct method for the determination of lead isotopic ratios by laser ablation-inductively coupled plasma-quadrupole mass spectrometry (LA-ICP-QMS) is presented. Samples of lake sediments were ground and pressed as pellets before being analysed. Mass bias was corrected by analysing an external calibration sample manufactured with pure silica doped with NIST SRM 981 solution. The efficiency of the mass bias correction was checked by comparing the ICP-MS data with lead isotopic ratios determined by thermal ionisation mass spectrometry (TIMS). The average long term reproducibilities were 0.40%, 0.40%, 0.20% and 0.30% (RSD) respectively for the 206Pb/204Pb, 207Pb/204Pb, 206Pb/207Pb and 208Pb/206Pb ratios. The method was applied to the study of lake sediment samples, in order to determine the amount and origin of historical contamination by lead.  相似文献   

5.
Using a state‐of‐the‐art 193 nm‐LA‐MC‐ICP‐MS system and with careful control of analytical procedures, the long term external reproducibility and accuracy of the ages Phanerozoic zircons measured over a period of months using calibrator bracketing for the 206Pb/238U and 207Pb/206Pb ages were ca. 1% (2 RSD) if a single reference zircon was used for the matrix‐matched calibration. When different reference zircons were used for the calibration, suspicious systematic shifts in the obtained ages were observed and thus a reduction in the overall accuracy of the dating method became obvious. Such shifts were within a few percent range of the U‐Pb and Pb/Pb ages and seemed to vary independently of zircon age and composition. A “test of accuracy” experiment was conducted reducing instrumental effects as far as possible by analysing five different reference zircons mounted on a single mount eight times during the same session. An identical protocol was used for all analyses, with unchanged instrument parameters and with ion beam intensities kept as identical as possible. For data reduction, every zircon served consecutively as the reference zircon for calibration, with the others in the batch treated as unknowns. The known reference age and the four calculated ages obtained using the four other RMs for calibration were then compared. Even using such a strict analytical protocol, shifts in 206Pb/238U, 207Pb/235U and 207Pb/206Pb ratios were still present. They varied non‐systematically and ranged from ?4.35% to 3.08% for the investigated age range (1065 Ma to 226 Ma). Assuming the absence of instrumental effects (i.e., memory, dead‐time correction, non‐linearity of ion counters and interdetector calibration, crystallographic orientation, ablation cell geometry and setup, gas flows), the observed shifts were attributed to matrix and/or ablation related effects. It is proposed that non‐spectral matrix effects in the Ar plasma torch resulted in non‐uniform signal enhancement (or depression?) leading to shifts both in elemental and Pb isotopic ratios. Additionally, the ablated particle size distribution could be an important factor controlling plasma conditions and thus mass bias and fractionation. Until such effects are well understood and controlled, it would seem that any LA‐ICP‐MS zircon U‐Pb and 207Pb/206Pb age determination cannot be meaningfully interpreted at below a ca. 3% to 4% (2 RSD) confidence level.  相似文献   

6.
Application of Laser Ablation ICP-MS to U-Th-Pb Dating of Monazite   总被引:2,自引:1,他引:2  
Recent advances in laser ablation ICP-MS techniques allow accurate U-Th-Pb age dating of monazites that are as young as several tens of million years to a precision better than 2%. Accuracy of the age determinations has been improved by true real-time mass bias correction via nebulisation of a solution containing enriched 233U and natural Tl isotopes. The Tl-U tracer solution eliminates possible effects of variable sample matrices on the precision and accuracy of measured isotopic ratios. Mass bias corrections based on measured 205Tl/233U ratios in the tracer solution allow direct measurement of 235U in monazite. Combined with high-sensitivity laser ablation ICP-MS measurements, direct measurement of 235U particularly improves the precision of U-Pb dating of young monazites. Correction for laser-induced Pb/U and Pb/Th elemental fractionation is based on a mathematical treatment of time resolved count-rate data that is independent of laser ablation characteristics, does not require external standardisation and allows variable laser pit size or raster patterns for each measurement. The new procedures make the LA ICP-MS technique more flexible for in situ U-Th-Pb analysis.  相似文献   

7.
The analytical capabilities of laser ablation (LA)-ICP-MS in determining Li, Be and B at trace levels in geological samples have been tested on a series of glass reference materials and natural samples. The LA-ICP-MS instrument used consisted of a sector-field ICP-MS coupled with a laser ablation microprobe operating at either 266 or 213 nm wavelength. Reference glasses from NIST (SRM 612, 614 and 616) and MPI-DING (KL2-G, ML3B-G, StHs6/80-G, GOR128-G, GOR132-G, T1-G and ATHO-G) were selected to develop the analytical method and to assess the best instrumental configuration. A series of calcic amphiboles with different Li, Be and B concentrations were also analysed using both LA-ICP-MS and SIMS to test the applicability of the method to natural minerals. Results indicated that with a spot size of 40 μm the agreement between measured and reference values of Li, Be and B is generally better than 10% for NIST SRM 612 and 20% for NIST SRM 614. Average reproducibility at the 2s level was 10% for Li, 20% for Be and 15% for B. Limits of detection were approximately 100 ng g-1 for Be and B and 200 ng g-1 for Li. These results were confirmed by analyses carried out on natural amphiboles and compared well in terms of precision and accuracy with those commonly achieved by SIMS.  相似文献   

8.
同位素地质年代学是探索地质体时空演化及地球动力学等问题的基础学科,应用最为广泛的当属含铀副矿物的U-Pb定年技术。榍石具有相对较低的U-Pb体系封闭温度,并广泛发育于岩浆岩、各类变质岩、热液成因岩石以及少量沉积岩中,是一种理想的中高温地质事件定年矿物。利用电感耦合等离子体质谱法(ICP-MS)测定榍石U-Pb年龄时,不可避免地要解决高普通铅以及元素分馏效应对测试的影响。本文对榍石LA-ICP-MS实验过程中的元素分馏行为进行研究,采用相同基体的标准样品与未知样品对比,发现了榍石不同颗粒之间元素分馏行为不一致的现象;同时采用不同的元素分馏校正方法,分别应用于锆石、独居石和榍石进行对比研究,认为分馏行为一致的副矿物定年可以采用"指数法"和"均值法"对数据进行校正,但是对于榍石这种分馏行为不一致的副矿物,定年时只有采用"截距法"对数据进行校正才可以获得正确的年龄。进而将此结论应用于秦岭造山带老牛山地区岩浆成因榍石样品,得到的结果与锆石年龄一致,表明"截距法"可以避免分馏行为不一致导致的校正不准确的问题。本研究成果为榍石LA-ICP-MS U-Pb定年方法的完善提供了一种思路。  相似文献   

9.
LA-MC-ICP-MS独居石微区原位U-Pb同位素年龄测定   总被引:7,自引:0,他引:7  
独居石富含U、Th,同时具有较低的初始普通Pb含量,是U-Pb和Th-Pb同位素定年的理想对象.由于普遍存在于多种岩石中,独居石的U-Th-Pb定年具有广阔的应用前景.本文报道利用193 nm ArF准分子激光剥蚀系统和NEPUNE多接收器电感耦合等离子体质谱仪,对独居石进行微区原位U-Pb同位素年龄测定的新方法.运用这一新方法对独居石样品AL01、BL02和CL03进行微区原位U-Pb同位素年龄测定,获得AL01和BL02号样品的206Pb/238U年龄加权平均值分别为(288.3±1.1) Ma (n=19)和(446.8±2.3) Ma (n=41);CL03号样品的U-Pb等时线年龄为(396.8±8.8) Ma (n=55),取得了令人满意的结果.  相似文献   

10.
The Zhashui-Shanyang district is one of the most important sulfide deposits in the Qinling Orogen where the formation of porphyry-skarn Cu-Mo deposits has a close genetic link with the Yanshannian magmatism. Laser Ablation-Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) U-Pb zircon dating of two granodiorite intrusions (Xiaohekou and Lengshuigou deposits) was investigated in the Zhashui-Shanyang district and the rock-forming ages obtained from 148.3±2.8?to 152.6±1.2?Ma, averaging 150.5 Ma, accompanied by a younger disturbance age of 144.3±1.7?Ma in the Lengshuigou intrusion, which is in excellent agreement with published sensitive high resolution ion micro-probe (SHRIMP) zircon date on the later monzodiorite porphyry phase in the Lenshuigou deposit. Two samples were selected for molybdenite ICP-MS Re-Os isotopic analyses from the Lengshuigou granodiorite porphyry, yielding Re-Os model ages from 149.2±2.7 Ma to 150.6±3.4 Ma, with a weighted mean age of 149.7±2.1 Ma. These mineralization ages overlap rock-forming ages of the host intrusions within the error range. This implies that the mineralization occurred in the Late Jurassic, which belongs to the tectonic phase B event of the Yanshan Movement, not Cretaceous as previously thought. Therefore, the Late Jurassic mineralization of the Zhashui-Shanyang district could be connected to the large-scale Yanshan molybdenum metallogenic period, the geodynamic regime of which is attributable to the far field response of convergence of surrounding plates, perhaps the approximately westward subduction of the Izanagi plate beneath the Eurasian continent.  相似文献   

11.
对安徽月山岩体开展了锆石原位U-Pb测年及Lu-Hf同位素研究.锆石的LA-ICP-MS年代学研究表明,月山闪长岩的U-Pb年龄为(139.3 ±1.5)Ma,与长江中下游成矿带早白垩世成铜岩体的年龄一致.月山闪长岩中的锆石具有均一的Hf同位素初始比值,介于0.282 430~0.282 491间.这些锆石的ε(Hf)(t)介于-9.05~-6.90间,亏损地幔模式年龄介于1.06~1.17 Ga间.结合长江中下游地区岩浆岩其他地球化学特征,认为月山岩体可能是在俯冲体系下由幔源岩浆经结晶分异作用且局部伴有一定程度的同化混染作用所形成.  相似文献   

12.
外标物质及内标元素的选择是激光剥蚀-电感耦合等离子体质谱(LA-ICP-MS)准确测定元素含量的关键因素之一。文章选用玻璃标准参考物质NIST 610、GSE-1G、BHVO-2G、BCR-2G、ATHO-G、KL2-G和T1-G作为外标,Si或Zr作为内标,对锆石M257中的Ti进行LA-ICP-MS微区原位测定。结果显示,选择Si或Zr作内标,采用BCR-2G、ATHO-G、KL2-G和T1-G作外标时,Ti含量测定值与参考值之间差异均较大,因此它们不适合作外标物质。采用BHVO-2G作外标和Si作内标,NIST 610作外标和Zr作内标,Ti含量测定值与参考值之间的差异均小于4%,因此BHVO-2G和NIST 610可有条件地作为外标物质。选择Si还是Zr作内标,GSE-1G作外标时,Ti含量的测定值与参考值之间的差异均小于3%,说明GSE-1G是较为合适的外标物质。选用GSE-1G作为外标,Si作内标,对5个标准锆石中的Ti含量进行了测定,结果显示,Ti元素在锆石91500中分布不均匀,而在锆石GJ-1、M257、PENGLAI和MUDTANK中分布均匀。在Ti元素分布均匀的GJ-1、M257、PENGLAI和MUDTANK等4个锆石中,由于Ti的含量均小于5μg/g,不适合作为锆石中Ti元素测定用的外标物质,但可作为测定时的质量监控样品。  相似文献   

13.
为探讨内蒙古中部地区镁铁质-超镁铁质岩形成时代及地球化学特征,完善区域成岩成矿年代学格架,本文对克布、黄花滩和小南山岩体进行了锆石U-Pb年代学及全岩地球化学分析。LA-ICP-MS锆石U-Pb测年获得克布和黄花滩镁铁质-超镁铁质岩结晶年龄分别为258±2 Ma(MSWD=2.3)和262±1 Ma(MSWD=0.51),属于中-晚二叠世,小南山辉长岩应形成于中-晚二叠世(~273 Ma)。全岩地球化学分析表明,三个岩体样品m/f值介于0.96~3.54之间,主要为镁铁质-超镁铁质岩,其稀土和微量元素曲线基本表现为轻稀土元素(LREE)和大离子亲石元素(LILE)相对富集,高场强元素(HFSE)相对亏损的相似性特征,但也有明显的区别,显示各岩体岩浆演化或分异程度可能不尽相同。综合区域研究资料表明,内蒙古中部地区晚古生代镁铁质-超镁铁质岩浆活动可能至少始于早二叠世(294Ma),持续至中-晚二叠世(273~258Ma),且二叠纪时期中亚造山带南缘较大范围内均发育较为活跃的幔源岩浆活动。克布、黄花滩和小南山岩体应形成于后碰撞伸展环境,其岩浆源区可能混染了俯冲流体交代改造的地幔楔物质,使3个岩体的岩石样品均显示具有富含大离子亲石元素和轻稀土元素,贫高场强元素等部分岛弧岩浆特征的信号。  相似文献   

14.
LA-ICP-MS锆石U-Pb同位素年龄测定表明,组成广西姑婆山花岗岩的东、西岩体和里松岩体的年龄分别为160.8±1.6Ma、165.0±1.9Ma、163.0±1.3Ma,在误差范围内基本一致,说明整个姑婆山岩体是同一时代的产物,是燕山中期第一阶段华南大规模陆壳重熔型花岗岩浆活动的产物。姑婆山花岗岩中的各个岩体虽然形成于同一时代,但它们之间在岩石学、地球化学特征方面有一定的差异。除了主微量元素、稀土元素特征有所不同外,Rb-Sr、Sm-Nd同位素特征研究表明姑婆山西岩体的粗粒花岗岩、东岩体、里松岩体及其包体的平均(87Sr/86Sr)i=0.7064、εNd(t)平均为-3.03,反映它们的源区有较多地幔物质组分参与;而姑婆山西岩体的细粒花岗岩的(87Sr/86Sr)i=0.7173、εNd(t)平均为-5.00,具强烈的Eu亏损、高Rb/Sr值等特征,它的源区可能是由一个相对古老地壳组分和年轻地幔组分组成的混合源区。此外,姑婆山东岩体(GP-1)中发现的继承锆石的206Pb/238U年龄为806.4Ma,与杭州—诸广山—花山花岗岩带(HZH)上的赣北九岭堇青石花岗岩、广西英桥混合花岗岩的年龄相似,为HZH带新元古代的岩浆活动提供了锆石年代学方面的依据。  相似文献   

15.
研究区位于南岭成矿带西段湘—桂交界处,该区中生代岩浆活动频繁,成岩成矿作用显著,尤以燕山期最为强烈.为厘定桂东北贺州开山镇孔子庙英安岩的成岩时代和探讨其岩浆源区,文章对其进行了LA-ICP-MS锆石U-Pb定年和锆石Lu-Hf同位素研究.锆石U-Pb定年结果限定了英安岩的侵位年龄为157.1±0.9 Ma.锆石Lu-H...  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.
同位素稀释热电离质谱法测定锡石U-Pb年龄探索   总被引:1,自引:0,他引:1  
针对我国锡多金属矿床的定年问题,建立一种采用同位素稀释热电离质谱(ID-TIMS)法进行锡石U-Pb同位素定年的方法,并与激光烧蚀电感耦合等离子体质谱(LA-ICP-MS)法进行对比验证。由于采用化学处理技术分别纯化了U和Pb,减少了普通铅的影响,大大提高了分析测定精度。将该方法应用于某地区石英-锡石-黑钨矿脉的锡石样品分析,获得了精确的U-Pb年龄值。  相似文献   

18.
锆石LA-ICP-MS原位微区U-Pb定年及微量元素的同时测定   总被引:7,自引:0,他引:7  
利用配有的 New Wave 213 nm 激光和 ThermoFisher X Series 2四极杆等离子体质谱,对年龄在158~1065 Ma之间的5个标准锆石进行了U-Pb同位素和微量元素的同时测定.测定结果显示,在激光频率为10 Hz,斑束直径为30μm 下,91500、GJ-1、TEMORA-1、Ple?ovice 和 Qinghu 标准锆石所获得的加权平均年龄分别为(1059±11) Ma (2σ, n=21),(604.4±4.7) Ma (2σ, n=25),(419.3±3.4) Ma (2σ, n=14),(338.7±2.4) Ma (2σ, n=23)和(158.9±1.7) Ma (2σ, n=18),年龄分析测定的单点相对偏差(2σ)均小于5.6%,加权平均年龄的相对偏差(2σ)均小于1.08%.5个标准锆石定年结果在误差范围内与前人报道的年龄值完全一致.在相同的测试条件下,以 NIST610为外标,对上述标准锆石的微量元素进行了同时测定, Ple?ovice 除了 Nb比文献给定的值偏高外,其余微量元素和91500微量元素的测定结果都落在文献报道的范围之内, GJ-1中的Pb、Th和U落在TIMS测定值的范围之内, TEMORA-1中的Th和U落在SHRIMP测定的值之内, Qinghu中的Th和U落在SIMS测定的值之内.从5个标准锆石的稀土元素球粒陨石标准化曲线可看出,所获得的稀土元素的相对含量也准确.  相似文献   

19.
Laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) is a microanalytical tool especially suitable for providing fast and precise U-Pb geochronological results on zircon grains. A new 193 nm excimer laser adapted to a micromachining workstation, equipped with a newly designed two-volume ablation cell and coupled with a quadrupole ICP-MS, is presented here. The system was tuned routinely to achieve sensitivities in the range of 3000 cps/μg g−1 for 238U (< 2% RSD), with a 34 μm spot size, at 5 Hz and ∼ 8 J cm−2, while ablating the NIST SRM 612 glass reference material. The system was capable of providing fast (< 1.5 minutes each analysis) and precise (generally < 1.5% 1s errors) 206Pb/238U zircon ages. The ages of widely used reference material zircons (Plesovice, 337 Ma; Temora, 416 Ma; R33, 418 Ma; Sri Lanka, 564 Ma; 91500, 1065 Ma) could be precisely matched, with an accuracy on isotopic ratios that ranged from ∼ 2 to ∼ 6%, depending on the homogeneity of the natural reference materials.  相似文献   

20.
对位于陕西汉中略阳县境内与铜厂铜矿关系密切的闪长岩体进行了地球化学、锆石U-Pb年代学及Lu-Hf同位素研究。地球化学研究表明,该岩体具有较高的Al2O3、Na2O和MgO含量,低K2O含量,属低钾钙碱性系列岩石。富集大离子亲石元素(Rb、Ba、Th、K、U),贫高场强元素(Ti、Nb、Ta、HREE),低Sr,显示壳源成因岩浆岩特征。依据锆石特征及锆石U-Pb同位素测年结果确定该岩体形成时代为(843.7±3.8)Ma,属新元古代岩浆作用的产物。锆石Hf同位素测试结果显示:εHf(t)介于-5.96~-30.17,二阶段模式年龄tDMC变化范围较大,介于1 816~3 344 Ma,存在1.81~1.95 Ga、2.13~2.65 Ga、2.72~2.78 Ga、2.97~3.09 Ga和~3.34 Ga 5组年龄峰值,暗示从新太古代到古元古代,扬子陆块曾发生过多期地壳增生事件。铜厂闪长岩是在Rodinia超大陆裂解过程中,由这些古老地壳物质部分熔融的结果。闪长岩体中2.72~2.78 Ga模式年龄峰值的出现,表明鱼洞子群的部分基性物质参与了铜厂闪长岩岩浆的形成。  相似文献   

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