Laser probe Ar/Ar dating: History and development from a technical perspective

The ⁴⁰Ar/³⁹Ar method using a laser probe opened the door to microscale measurements and diffusion profiles frozen in samples. In the first decade since the initial application of a laser for ⁴⁰Ar/³⁹Ar dating in 1973, practical applications have been few. This is due not only to the fact that the laser and vacuum technologies were immature but that mass spectrometry was also in its infancy. In those days, the sensitivity of a mass spectrometer was generally insufficient to measure the small amount of argon degassed from a geological sample by a laser. These problems have subsequently been solved by new technologies. To understand their current status, a brief history of their development is outlined. This outline focuses on the required detection limit in micro scale measurement, practical approaches for accurate measurement are explained through examples in our laboratory specifically relating to the technical aspects of ⁴⁰Ar/³⁹Ar dating.     

激光显微探针~(40)Ar/~(39)Ar同位素定年

已有 5 0年历史的K Ar定年法 ,由于过剩Ar和Ar丢失的普遍发现 ,使其最广泛的应用面临着严重挑战。40 Ar/ 3 9Ar分步加热释氩法是常规K Ar定年法的发展 ,它克服了常规K Ar定年法的一些局限 ,又可以测定岩浆构造热事件。激光显微探针40 Ar/ 3 9Ar定年法是在 2 0世纪末把聚焦激光束应用在40 Ar/ 3 9Ar分步加热释氩法中而发展起来的一种定年方法。它既具有常规K Ar定年法和40Ar/ 3 9Ar分步加热释氩法的所有优越性 ,又把定年引入微观领域。特别是在 2 0世纪的最后几年 ,以激光显微探针40 Ar/ 3 9Ar定年方法的完善和精度的提高为标志 ,把K Ar年代学研究推向了一个新的里程碑。微区微量高精度高分辨定年 ,把定年时限扩展到人类历史范畴 ,精细的分析技术拓宽了年代学的应用范围 ,使之解决的地质问题更广泛和深入 ,并且开始冲击着地球科学中的某些热点和难点课题。     

Instrumentation Development for In Situ 40Ar/39Ar Planetary Geochronology

The chronology of the Solar System, particularly the timing of formation of extra‐terrestrial bodies and their features, is an outstanding problem in planetary science. Although various chronological methods for in situ geochronology have been proposed (e.g., Rb‐Sr, K‐Ar), and even applied (K‐Ar), the reliability, accuracy, and applicability of the ⁴⁰Ar/³⁹Ar method makes it by far the most desirable chronometer for dating extra‐terrestrial bodies. The method however relies on the neutron irradiation of samples, and thus a neutron source. Herein, we discuss the challenges and feasibility of deploying a passive neutron source to planetary surfaces for the in situ application of the ⁴⁰Ar/³⁹Ar chronometer. Requirements in generating and shielding neutrons, as well as analysing samples are described, along with an exploration of limitations such as mass, power and cost. Two potential solutions for the in situ extra‐terrestrial deployment of the ⁴⁰Ar/³⁹Ar method are presented. Although this represents a challenging task, developing the technology to apply the ⁴⁰Ar/³⁹Ar method on planetary surfaces would represent a major advance towards constraining the timescale of solar system formation and evolution.     

(极)年轻火山岩激光熔蚀40Ar/39Ar定年

对中国大量年轻或/和极年轻火山岩的定年实践研究表明,(极)年轻火山岩的激光熔蚀40Ar/39 Ar定年具有不同于第四纪以前喷发火山岩定年的显著特点.激光熔蚀40Ar/39Ar定年技术因为本底低、样品用量小以及与现代惰性气体同位素质谱设备在灵敏度、高精度方面的相一致,在年轻火山岩的定年中得到深入运用.借助激光在年轻或/和极年轻火山岩的40 Ar/39 Ar定年中,实践证明,样品形成时限越年轻(特别是相当于第四纪时期的样品),Nier值与样品中初始氩比值的偏离会引起K-Ar和40Ar/39 Ar表观年龄的偏差越大.对于小于0.2Ma的样品,Nier值与样品中初始氩比值的偏离对K-Ar和40Ar/39Ar表观年龄的偏差影响呈指数增长;当样品年龄相对较老(老于第四纪)时,Nier值和初始氩比值的偏离对K-Ar和40Ar/39 Ar表观年龄的影响较小.以40Ar/ArAr定年为出发点,定量给出界定年轻与极年轻火山岩的年龄:2～0.2Ma的火山岩界定为年轻火山岩,0.2Ma以来的火山岩称为极年轻火山岩.实验结果还证实,测定(极)年轻火山岩基质年龄时要尽量剔除非同源分馏的斑晶,以便去除斑晶可能带来的过剩氩影响;年轻火山岩样品的测年,应根据岩石结构和粒度特征选取合适的粒度,通常情况下,推荐0.2mm颗粒直径(60～80目)为理想粒径;年轻火山岩样品在快中子辐照后冷却放置时间不宜过长,否则造成37 Ar测不准,影响数据结果,带来较大偏差;激光40Ar/39Ar精细定年对标准样品的均一性有很高的要求,通过标定常用的国内外监测标样发现,标样SB-778-Bi,Bem4M,BT-1均一性很好,适合用作激光熔蚀40Ar/39Ar定年监测;测试数据的处理中,火山岩喷发后冷却结晶中同时形成的斑晶和基质的等时线处理能够帮助获得客观真实和精细的年龄结果.在此基础上,北京大学惰性气体同位素实验室建成了专用于(极)年轻火山岩精细定年的激光熔蚀40Ar/39Ar定年实验流程.     

Eruption of the Continental Flood Basalts at -259 Ma in the Emeishan Large Igneous Province, SW China： Evidence from Laser Microprobe ^40Ar/^39Ar Dating

A suite of continental flood basalts sampled over a vast exposure and stratigraphic thickness in the Emeishan large igneous province (LIP), SW China was investigated for laser microprobe 40Ar/39Ar dating. There are two 40Ar/39Ar age groups for these basalts, corresponding to 259-246 Ma and 177-137 Ma, respectively. A well-defined isochron gives an eruption age of huge quantities of mafic magmas at 258.9±3.4 Ma, which is identical to previous dating and paleontological data. Much younger 40Ar/39Ar ages for some basalts with low-greenschist metamorphic facies probably recorded a late thermo-tectonic event caused by collision between the Yangtze and Qiangtang continental blocks during the Mesozoic, which resulted in the reset of argon isotope system. The 40Ar/39Ar age data, we present here, combined with previous dating and paleontological data, suggest relatively short duration (about 3 Ma) of mafic volcanism, which have important implication on mantle plume genesis of the Emeishan continental flood basalts in the LIP.     

An 40Ar/39Ar investigation of the contact effects of a dyke intrusion,Kapuskasing Structural Zone,Ontario

An ⁴⁰Ar/³⁹Ar study on biotite and hornblende from baked tonalite gneiss adjacent to a 14-m-wide Kapuskasing dyke in the Chapleau Block of the Kapuskasing Structural Zone employed resistance-furnace step-heating, of bulk-mineral separates, single-grain laser step-heating, and laser spot dating of individual grains in thick section. All three methods yielded concordant results for the biotite, indicating that it has been uniformly overprinted at ca. 2.05 Ga. This date is probably a close estimate of the age of the dyke intrusion. The argon data from the hornblende are more difficult to interpret. All three methods suggest that the hornblende was partially overprinted and then affected by a later influx of excess argon from the external environment. Laser spot dates record an apparent age gradient, extending radially outward from 2.25 Ga in the grain cores to 2.4–2.7 Ga in the grain rims. Corresponding ³⁷Ar/³⁹Ar values show no systematic variation across the hornblende, although ³⁸Ar/³⁹Ar ratios display a similar pattern to the age distribution, with lower values in the cores than in the rims. The bulk separate and single grain step-heating spectra mimic a volume diffusion Ar-loss profile that would appear to be inconsistent with the laser-spot dates. Three possible interpretations to explain this apparent discrepancy may involve either experimental difficulties, an effective radius of diffusion which is much smaller than the actual grain radius, or an effective radius of diffusion that is of the order of the grain radius. It is clear that for the ⁴⁰Ar/³⁹Ar dating of samples that have experienced complex geologic histories, it is important to utilize both resistance-furnace and laser techniques.     

Direct 40Ar/39Ar K‐feldspar dating of Late Permian—Early Triassic brittle faulting in northern Norway

While the offshore post‐Caledonian extensional history of the north Norwegian passive margin is well constrained, the tectonic relationship between onshore and offshore regions is less clear because of limited age constraints on the timing of rifting onshore. ⁴⁰Ar/³⁹Ar dating of K‐feldspar from hydrothermally altered fault rocks in a Precambrian gneiss complex in northern Norway was used to study the timing of extensional faulting onshore. In addition, ⁴⁰Ar/³⁹Ar dating of K‐feldspar from the host rock provided insight into the regional rock cooling history prior to brittle deformation. Results indicated a dominant Late Permian–Early Triassic (~265–244 Ma) faulting event and found no evidence for later reactivation, which has been documented offshore. The region cooled to below the closure temperature for ⁴⁰Ar/³⁹Ar K‐feldspar in the Carboniferous to Early Permian, prior to the main brittle faulting event. ⁴⁰Ar/³⁹Ar dating of fault zone K‐feldspar products provided a means to date brittle faulting events.     

40Ar-39Ar同位素定年方法研究进展

^40Ar-^39Ar同位素定年法是由K-Ar法发展而来,通过将39K利用快中子辐照衰变成^39Ar,测量40Ar^＊/^39Ar来获得年龄值.经过长期发展,该方法的测试技术逐渐成熟,其中气体提取发展为常规阶段升温法、激光显微探针法以及真空压碎流体包裹体法;气体纯化主要有冷阱去除法、钛泵吸附法、锆铝泵吸附法;气体测试的质谱仪也在灵敏度、分辨率、背景值等技术指标上有很大提高.^40Ar-^39Ar同位素定年法在石油、固体矿产等方面应用广泛,尤其在油气成藏时间、成岩成矿作用时间的热年代学研究等领域.     

40Ar/39Ar Dating of Xuebaoding Granite in the Songpan-Garzê Orogenic Belt, Southwest China, and its Geological Significance

<正>Thus far,our understanding of the emplacement of Xuebaoding granite and the occurrence and evolution of the Songpan-Garze Orogenic Belt has been complicated by differing age spectra results.Therefore,in this study,the ~(40)Ar/~(39)Ar and sensitive high resolution ion micro-probe(SHRIMP) U-Pb dating methods were both used and the results compared,particularly with respect to dating data for Pankou and Pukouling granites from Xuebaoding,to establish ages that are close to the real emplacements.The results of SHRIMP U-Pb dating for zircon showed a high amount of U,but a very low value for Th/U.The high U amount,coupled with characteristics of inclusions in zircons,indicates that Xuebaoding granites are not suitable for U-Pb dating.Therefore,muscovite in the same granite samples was selected for ~(40)Ar/~(39)Ar dating.The ~(40)Ar/~(39)Ar age spectrum obtained on bulk muscovite from Pukouling granite in the Xuebaoding,gave a plateau age of 200.1±1.2 Ma and an inverse isochron age of 200.6±1.2 Ma.The ~(40)Ar/~(39)Ar age spectrum obtained on bulk muscovite from Pankou granite in the Xuebaoding gave another plateau age of 193.4±1.1 Ma and an inverse isochron age of 193.7±1.1 Ma. The ~(40)Ar/~(36)Ar intercept of 277.0±23.4(2σ) was very close to the air ratio,indicating that no apparent excess argon contamination was present.These age dating spectra indicate that both granites were emplaced at 200.6±1.3 Ma and 193.7±1.1 Ma,respectively.Through comparison of both dating methods and their results,we can conclude that it is feasible that the muscovite in the granite bearing high U could be used for ~(40)Ar/~(39)Ar dating without extra Ar.Based on this evidence,as well as the geological characteristics of the Xuebaoding W-Sn-Be deposit and petrology of granites,it can be concluded that the material origin of the Xuebaoding W-Sn-Be deposit might partially originate from the Xuebaoding granite group emplacement at about 200 Ma.Moreover,compared with other granites and deposits distributed in various positions in the Songpan-Garze Orogenic Belt,the Xuebaoding emplacement ages further show that the main rare metal deposits and granites in peripheral regions occurred earlier than those in the inner Songpan-Garze.Therefore,~(40)Ar/~(39)Ar dating of Xuebaoding granite will lay a solid foundation for studying the occurrence and evolution of granite and rare earth element deposits in the Songpan-Garze Orogenic Belt.     

Phlogopite40Ar/39Ar geochronology of mantle xenoliths from the North China Craton: Constraints on the eruption ages of Cenozoic basalts

Mantle xenoliths provide direct information about lithospheric evolution and asthenosphere–lithosphere interaction, and therefore precise dating of the host basalts which carried the xenoliths is important. Here we report ⁴⁰Ar/³⁹Ar geochronology of phlogopite separates from five spinel lherzolite xenoliths collected from the North China Craton (Hannuoba of Hebei Province, Sanyitang of Inner Mongolia Autonomous Region and Hebi of Henan Province), as well as the groundmass of the host basalts. Argon extraction was performed by conventional step heating technique and ultra-violet laser ablation microprobe (UVLAMP) technique. ⁴⁰Ar/³⁹Ar incremental heating results on groundmass yielded geologically meaningless ages. However, conventional step heating on phlogopites produced Miocene cooling ages, identical to the eruption ages obtained from the K–Ar dating methods of the Hannuoba and Sanyitang basalts. Adopting procedures to exclude potential influence of excess radiogenic Ar from a deep fluid source on a phlogopite separate from lherzolite yielded results with a good agreement of ages suggesting that the argon isotopes are distributed homogenously in this mineral, with no influence of excess argon. Phlogopites from Hebi yield ages between 6.43 and 6.44 Ma which are slightly older than those obtained from K–Ar method on whole-rocks. The discrepancy in the K–Ar ages obtained from the altered whole-rock samples suggests partial loss of ⁴⁰Ar. As a consequence, phlogopite Ar–Ar ages are considered more accurate than that of the whole-rocks. These results suggest that ⁴⁰Ar/³⁹Ar chronology of phlogopite provides reliable and precise ⁴⁰Ar/³⁹Ar ages of host basalts.     

Development of high precision Rb-Sr phlogopite and biotite geochronology; an alternative to Ar/Ar tri-octahedral mica dating

Potassium-Ar and Rb-Sr dating of minerals was fundamental in early efforts to date magmatic and metamorphic processes and paved the way for geochronology to become an important discipline within the earth sciences. Although K-Ar and, in particular, ⁴⁰Ar/³⁹Ar dating of micas is still widely applied, Rb-Sr dating of micas has declined in use, even though numerous studies demonstrated that tri-octahedral mica yields geologically realistic, and more reliable and reproducible Rb-Sr ages than the K-Ar or ⁴⁰Ar/³⁹Ar system. Moreover, a reduction of uncertainties typically reported for Rb-Sr ages (ca. 1%) can now be achieved by application of multi-collector inductively coupled plasma mass spectrometry (MC-ICPMS) rubidium isotope dilution measurements (<0.3%). Replicate Rb-Sr biotite ages from the Oslo rift, Norway, yield an external reproducibility of ±0.3% (n=4) and an analytical error of ±0.8 Ma for individual ages that vary between 276.9 and 275.5 Ma. Conventional thermal ionisation mass spectrometry (TIMS) Rb analysis on the same mineral separates yields ages between 276.1 and 271.7 Ma, three times the spread compared to Rb MC-ICPMS data. Biotite and phlogopite from the central Nagssugtoqidian orogen, West Greenland, yield ⁴⁰Ar/³⁹Ar plateau ages (ca. 1700 Ma) with a spread of ±150 Ma, while Rb-Sr ages on either biotite or phlogopite separates have a much narrower range of ±10 Ma. This comparison of Rb-Sr and ⁴⁰Ar/³⁹Ar ages demonstrates the robustness of the Rb-Sr system in tri-octahedral micas and cautions against the sole use of ⁴⁰Ar/³⁹Ar tri-octahedral mica ages to date geological events. Analytical errors of 16 Ma for these Rb-Sr mica ages determined by TIMS are reduced to <±5 Ma when the Rb concentration is determined by MC-ICPMS. All the TIMS and MC-ICPMS data from the Nagssugtoqidian orogen agree within assigned analytical uncertainties. However, high precision Rb-Sr dating by MC-ICPMS can resolve geological information obscured by TIMS age determinations. TIMS data for seven phlogopite samples form an isochron age of 1645±6 Ma, and thus, no differentiation in age between the different samples can be made. In contrast, MC-ICPMS Rb measurements on the same samples reveal two distinct populations with ages of 1633±3 or 1652±5 Ma.Combining the mica Rb-Sr geochronological data with the well-constrained thermal history of this ancient orogen, we estimate the closure temperature of the Rb-Sr system in 1-2 mm slowly cooled phlogopite crystals, occurring in a matrix of calcite and plagioclase to be ∼435 °C, and at least 50 °C above that of biotite.     

琼北火山岩激光40Ar/39Ar定年研究

新生代以来,雷琼地区多次、大量地喷发了一系列火山岩。前人主要基于K-Ar法对此划分了期次。本文采用激光40Ar/39Ar年代学方法,对琼北火山岩区进行了精细定年研究。低本底激光40Ar/39Ar法能够对低钾含量,极少量样品(毫克级)进行精细测定,非常适合极年轻火山岩的定年工作。结果显示的火山岩激光40Ar/39Ar法高质量数据表明琼北火山喷发活动时限跨越1.3～0.052Ma。在比较了表观年龄与等时线年龄差异之后,本文给出了年龄推荐值。正如测试数据所显示,本地区新生代火山岩普遍存在40Ar和36Ar过剩的问题,此时只有等时线年龄才代表喷发的真实年龄。     

Cassiterite LA-MC-ICP-MS U/Pb and muscovite 40Ar/39Ar dating of tin deposits in the Tengchong-Lianghe tin district,NW Yunnan,China

The Tengchong-Lianghe tin district in northwestern Yunnan, China, is an important tin mineralization area in the Sanjiang Tethyan Metallogenic Domain. There are three N–S trending granite belts in the Tengchong-Lianghe area, with emplacement ages ranging from Early Cretaceous to Late Cretaceous and Early Cenozoic. Tin mineralization is spatially associated with these granitic rocks. However, the petrogenetic link between the tin deposits and the host granites is not clear because of the lack of age data for the tin mineralization. We investigate the possibility of direct dating of cassiterite from three typical tin deposits in the Tengchong-Lianghe tin district, using laser ablation multicollector inductively coupled plasma mass spectrometry (LA-MC-ICP-MS). In situ LA-MC-ICP-MS dating of seven cassiterite samples from the Lailishan (LLS-1 and LLS-2), Xiaolonghe (XLH, WDS, DSP, and HJS), and Tieyaoshan (TYS) tin deposits yielded well-defined ²⁰⁶Pb/²⁰⁷Pb–²³⁸U/²⁰⁷Pb isochron ages. To assess the accuracy of the in situ U/Pb dating of cassiterite, ⁴⁰Ar/³⁹Ar dating of coexisting muscovite (in samples LLS-1, DSP, and TYS) was also performed. The cassiterite in situ U/Pb ages (47.4?±?2.0, 71.9?±?2.3, and 119.3?±?1.7 Ma, respectively) are in excellent agreement with the coexisting muscovite ⁴⁰Ar/³⁹Ar ages (48.4?±?0.3, 71.9?±?1.4, and 122.4?±?0.7 Ma, respectively). The U/Pb ages of cassiterite combined with the ⁴⁰Ar/³⁹Ar ages of muscovite indicate that there are three tin mineralization events in this district: the Lailishan tin deposit at 47.4?±?2.0 to 52?±?2.7 Ma, the Xiaolonghe tin deposit at 71.6?±?2.4 to 3.9?±?2.0 Ma, and the Tieyaoshan tin deposit at 119.3?±?1.7 to 122.5?±?0.7 Ma. These ages are highly consistent with the zircon U/Pb ages of the host granites. It is su.ggested that the Cretaceous tin mineralization might have taken place in a subduction environment, while the Early Tertiary tin metallogenesis was in a postcollisional geodynamic setting.     

准噶尔盆地周边硅质岩激光40Ar/39Ar法定年

由于较低的钾元素含量以及过剩氩的存在,长期以来对硅质岩的40Ar/39Ar定年一直存在较大难度。近年来,由于仪器水平的不断提高,新实验技术和方法的应用,特别是激光全熔40Ar/39Ar定年技术的应用,40Ar/39Ar定年方法具有了足够高的测试精度和稳定的低本底水平,可以满足测试极低钾元素含量的硅质岩样品的要求。利用多组矿物颗粒测试数据计算等时线年龄的方法可以很好地去除过剩氩对硅质岩年龄的影响。本文利用激光全熔40Ar/39Ar定年方法对新疆准噶尔盆地边缘的两个硅质岩样品进行了定年研究。采自白碱滩地区的08BJT-3样品的年龄测试结果为294±14Ma,该年龄结果与硅质岩样品所处的晚石炭世地层沉积年代基本一致。采自卡拉麦里地区的KML-2样品的年龄测试结果为266±14Ma,该年龄结果与强烈变形改造硅质岩样品的卡拉麦里构造变形带活动年代十分一致,表明激光全熔40Ar/39Ar定年方法可以准确地对硅质岩进行定年。     

Age calibration of the Fish Canyon sanidine Ar/Ar dating standard using primary K-Ar standards

The ⁴⁰Ar/³⁹Ar dating technique requires the use of neutron fluence monitors (standards). Precise calibrations of these standards are crucial to decrease the uncertainties associated with ⁴⁰Ar/³⁹Ar dates. Optimal calibration of ⁴⁰Ar/³⁹Ar standards should be based on K/Ar standards having independent isotope dilution measurements of ⁴⁰K and ⁴⁰Ar*, based on independent isotope tracers (spikes) because this offers the possibility to eliminate random interlaboratory errors. In this study, we calibrate the widely used Fish Canyon sanidine (FCs) standard based on four primary K/Ar standards (GA-1550, Hb3gr, NL-25, and GHC-305) on which K and Ar* concentrations have been determined in different labs with independently calibrated tracers. We obtained a mean age of 28.03 ± 0.08 Ma (1σ; neglecting uncertainties of the ⁴⁰K decay constants) for FCs, based on the decay constant recommended by Steiger and Jäger [Steiger R.H., Jäger. E. 1977. Subcommission on geochronology: convention of the use of decay constants in geo- and cosmochronology. Earth Planet. Sci. Lett.36, 359-362.]. This age corresponds to a mean ⁴⁰Ar*/⁴⁰K value of (1.6407 ± 0.0047) × 10⁻³. We also discuss several criteria that prevent the use of previous calibrations of FCs based on other primary standards (LP-6, SB-3 and MMhb-1). The age of FCs obtained in this study is based on the ⁴⁰K decay constants of Steiger and Jäger (1977) but we anticipate the imminent need for revision of the value and precision of the ⁴⁰K decay constants (representing the main source of uncertainties in ⁴⁰Ar/³⁹Ar dating). The ⁴⁰Ar*/⁴⁰K result of FCs obtained in this study allows therefore a rapid calibration of the age of FCs with uncertainties at the 0.29% level but perhaps more importantly this value is independent of any particular value of the ⁴⁰K decay constants and may be used in the future in conjunction with revised decay constants.     

Evaluation of 40Ar/39Ar Geochronology of Authigenic Illites in Determining Hydrocarbon Charge Timing: A Case Study from the Silurian Bituminous Sandstone Reservoirs,Tarim Basin,China

The Silurian bituminous sandstones(SBS) in the Tarim Basin, China are important basinwide reservoirs with an estimated area of approximately 249000 km2. We investigated the ages of authigenic illites in the SBS reservoirs and constrained their formation timing by using the ~(40)Ar/~(39)Ar step wise heating method. The age spectra, ~(39)Ar recoil loss and their controlling factors were investigated systematically. The ~(40)Ar/~(39)Ar ages were compared with the conventional K/Ar ages of identical clay fractions. The clay in the SBS reservoirs is dominated by orderly mixed-layer illite/smectite(I/S) with 5%–30% smectite layers. The I/S minerals morphology comprises primarily honeycomb, short filamentous and curved-lath particles, characteristic of authigenic illites. The unencapsulated ~(40)Ar/~(39)Ar total gas ages(UTGA) of the authigenic illites range from 188.56 ± 6.20 Ma to 491.86 ± 27.68 Ma, which are 7% to 103% older than the corresponding K/Ar ages of 124.87 ± 1.11 Ma to 383.45 ± 2.80 Ma, respectively. The K-Ar ages indicate multistage accumulations with distinct distribution patterns in the Tarim Basin: older(late Caledonian-early Hercynian) around the basin margin, younger(late Hercynian) in the basin centre, and the youngest(middle to late Yanshanian) in the Ha-6 well-block, central area of the North Uplift. The age difference is believed to have been caused by the ~(39)Ar recoil loss during the irradiation process. Compared with the K/Ar ages, the estimated ~(39)Ar recoil losses in this study are in the range from 7% to 51%. The ~(39)Ar recoil loss appears to increase not only with the decreasing particle sizes of the I/S, but also with increasing percentage of smectite layers(IR) of the I/S, and smectite layer content(SLC) of the samples. We conclude that due to significant ~(39)Ar recoil losses, UTGA may not offer any meaningful geological ages of the authigenic illite formation in the SBS and thus can not be used to represent the hydrocarbon charge timing. ~(39)Ar recoil losses during ~(40)Ar/~(39)Ar dating can not be neglected when dating fine authigenic illite, especially when the ordered mixed-layer I/S containing small amount of smectite layers(IR30%) in the reservoir formations. Compared with the unencapsulated Ar-Ar method, the conventional K-Ar method is less complicated, more accurate and reliable in dating authigenic illites in petroleum reservoirs.     

Precise molybdenite Re–Os and mica Ar–Ar dating of the Mesozoic Yaogangxian tungsten deposit, central Nanling district, South China

The Yaogangxian deposit in the central Nanling region, South China consists of vein-type ore bodies hosted in Cambrian to Jurassic strata and Mesozoic granitic intrusions. Wolframite and molybdenite are the dominant ore minerals intergrown with gangue minerals of quartz, feldspar, phlogopite, and muscovite. We have carried out molybdenite Re–Os and phlogopite and muscovite ⁴⁰Ar/³⁹Ar dating to better understand the timing and genesis of mineralization. Re–Os dating of eight molybdenite samples yielded model ages ranging from 152.0±3.5 to 161.1±4.5 Ma, with an average of 156.0 Ma. The Re–Os analyses give a well-defined ¹⁸⁷Re/¹⁸⁷Os isochron with an age of 154.9±2.6 Ma (MSWD=2.4). Hydrothermal phlogopite and muscovite display extremely flat ⁴⁰Ar/³⁹Ar age spectra. Phlogopite yields a ⁴⁰Ar/³⁹Ar plateau age of 153.0±1.1 Ma, whereas muscovite yields a plateau age of 155.1±1.1 Ma. Both ⁴⁰Ar/³⁹Ar ages are in good agreement with the Re–Os ages, placing the timing of tungsten mineralization at about 154 Ma. This age is consistent with the field relationships. Our new data, when combined with published geochronological results from other major deposits in this region, suggest that large scale W–Sn mineralization occurred throughout the central Nanling region in the Late Jurassic.     

He,Ne and Ar composition in a neutron activated sea-floor basalt glass

We have measured the composition of He, Ne and Ar in the glassy rim of a fresh oceanic basalt from the East Pacific Rise. Three splits of the sample were subjected to neutron irradiation prior to analysis to investigate the noble gas release as a function of different neutron doses. The shapes of the observed ³⁹Ar-⁴⁰Ar degassing profiles depend critically on the irradiation dose due to a severe redistribution of excess ⁴⁰Ar. This shows that the application of the ³⁹Ar-⁴⁰Ar method for dating of glassy samples requires the utmost care.Including the He and Ne results from the irradiated specimens, it was possible to determine the concentrations of Li and Mg and to estimate upper limits for Na and F in addition to the concentrations of K, Ca and Cl which are measured routinely as a byproduct of the ³⁹Ar-⁴⁰Ar dating method. This provides a useful extension of the ³⁹Ar-⁴⁰Ar technique since it may help to identify the outgassing sites during stepwise heating experiments. Furthermore it allows one to study the diffusion behavior of He and Ne isotopes artificially produced during irradiation. In our samples the activation energies of ³He and ²¹Ne tend to increase with growing neutron doses.     

Quantification of Ar recoil ejection from GA1550 biotite during neutron irradiation as a function of grain dimensions

This study presents the first measurement of ³⁹Ar recoil ejection loss from individual, dimensionally characterized mineral grains due to neutron irradiation, and reveals the extent to which this recoil loss is problematic for ⁴⁰Ar/³⁹Ar dating. Using the well-characterized biotite standard GA1550, known to have between grain reproducibility of ⁴⁰Ar*/³⁹Ar_K of order 0.1%, we measured the thicknesses (3-210 μm) and surface areas (0.07-0.90 mm²) of 159 grains selected to span the dimensional range represented in the aliquot. Thinner grains with high surface area/volume (SA/V) reveal elevated ⁴⁰Ar/³⁹Ar, as much as 26% higher than thicker grains expected to suffer proportionately negligible depletion. Although the thinner grains yield intrinsically less precise measurements due to small ³⁹Ar ion beams, a regular decrease in net recoil loss with increasing biotite grain thickness is clear for grains thinner than ca. 50 μm. Grains thicker than 50 μm reveal essentially no ³⁹Ar loss within analytical uncertainties. The measured ³⁹Ar loss spectrum is significantly higher than predicted by previous modeling approaches. These results suggest a practical threshold of ca. 50 μm grain thickness for biotites, and probably other phyllosilicates, irradiated with ²³⁵U fission spectrum neutrons in order to avoid recoil artifacts. Poor agreement between our data and simulation results indicates that recoil displacement models should be revisited in order to resolve the discrepancy. Further empirical work to determine the recoil loss of ³⁹Ar in other minerals is important not only for routine age measurements, but also to shed more light on the role of recoil in multi-diffusion domain theory and other thermochronologic applications exploiting variable diffusion radii and/or grain size effects.     

^40Ar／^39Ar Plateau Age Spectra of Feldspars and Their Geological Implications

The paragenic minerals plagioclase,perthite,biotite,hornblende and pyroxene in acid-granite alkali-granite,monzonite and volcanic rocks collected from seven areas different in thermal history have been determined.On the basis of 14 plateau age spectra and isochron ages of paragenic miner-als in conjunction with the observed mineral textures ,the suitability of plateau age spectra of plagioclase and perthite and their thermo-chronological significance are discussed in this paper.The results indicate that undisturbed feldspar gives satisfactory^40Ar-^39Ar plateau ages in consis-tence with those of paragenic minerals.This means that feldspars from the undisturbed area are suita-ble for ^40Ar-^39Ar dating .On the other hand,the age spectra of feldspars as well as of biotite,pyroxene and hornblende affected by tectonic or thermodynamic events appear unsmooth at varying temperatures,thus complicating their interpretation.Feldspars may give an emplacement age of a rock and /or that of the latest thermodynamic event,depending on the intensity of the event and the retentivity of Ar in the mineral.