Laser probe 40Ar/39Ar 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.     

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。     

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。     

(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.     

多宝山斑岩铜矿区水热蚀变矿物的激光显微探针40Ar/39Ar定年

在利用脉冲显微激光探针⁴⁰Ar/³⁹Ar定年技术测定标准样品的J值和年龄适用范围的基础上,研究了黑龙江省嫩江县北部多宝山斑岩铜矿区水热成因矿物的年代学。结果表明,高钾含量的水热蚀变矿物适合于激光探针的表面微区测定,并且可以克服水热蚀变矿物中的³⁹Ar “反冲”丢失对年龄结果的影响。矿区的岩浆-水热事件主要有两期,分别为253-220Ma和184-162Ma,前者代表了成矿时代,后者反映出由成矿期后岩浆活动所引起的水热叠加事件。     

40Ar/39Ar age of the onset of high-Ti phase of the Emeishan volcanism strengthens the link with the end-Guadalupian mass extinction

Precise time constraints of the main extrusive phase of the Emeishan large igneous province (ELIP) remain unresolved because basalts commonly do not contain suitable minerals for U–Pb dating, whereas previous ⁴⁰Ar/³⁹Ar studies on basalts yielded tectonothermal overprint ages. The timing for the ELIP was deduced from indirect dating of minor intrusions of ultramafic/mafic and felsic compositions by geochronological methods and geological correlations. The extrusive part of the ELIP consists of an older low-Ti and younger high-Ti basalt phases. We have found fresh samples of plagioclase-phyric rocks at the lower Qiaojia extrusive section (the Yunnan province of China), which belong to the ELIP unit of the high-Ti basalt series. ⁴⁰Ar/³⁹Ar dating on plagioclase from two samples conducted at two different laboratories using different age standards yielded statistically indistinguishable results with the weighted mean age of 260.1 ± 1.2 Ma for five individual measurements. This provides the direct constraints on the onset of the ELIP high-Ti basalt extrusive phase. The obtained age is within the error or slightly older than the age of the Guadalupian–Lopingian boundary and felsic ignimbrite capping the ELIP lava succession (both dated at 259.1 ± 0.5 Ma). Our new data are strengthening the short duration of the, at least, high-Ti phase of the ELIP volcanism and its temporal link with the end-Guadalupian mass extinction. Estimation of the total duration of the ELIP volcanism awaits finding of suitable for dating low-Ti basalts.     

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.     

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.     

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。     

Dating deformation using crushed alkali feldspar: 40Ar/39Ar geochronology of shear zones in the Wyangala Batholith,NSW, Australia

Diffusion parameters have been estimated for K-feldspar in and adjacent to mylonite shear zones in the Wyangala Batholith. The parameters obtained suggest that deformation during mylonitisation would have caused argon systematics to reset because diffusion distances were reduced by cataclasis, deformation and/or recrystallisation. However, the mineral lattice remained sufficiently retentive to allow subsequently produced radiogenic argon to be retained. ⁴⁰Ar/³⁹Ar geochronology is thus able to constrain operation of these biotite-grade ductile shear zones to the period from ca 380 Ma to ca 360 Ma, at the end of the Tabberabberan Orogeny.     

雷州半岛第四纪火山岩激光40Ar/39Ar等时线定年研究

雷州半岛是我国新生代火山岩最重要的分布地区之一,火山活动主要集中在中晚更新世。前人对雷州火山岩的年代学研究以K-Ar法为主。研究表明,雷州火山岩测年结果大致分布在0.38～3.04Ma范围内。根据地层和火山岩层的叠置关系,雷州第四纪火山岩由于覆盖在被确定是1.87Ma和0.76Ma沉积的地层之上,故火山岩年龄应小于该地层年龄。K-Ar法定年结果与雷州地区地层叠置关系存在矛盾。本文通过对雷州半岛第四纪火山岩进行野外考察及采样,利用激光40Ar/39Ar年代学方法进行了精细定年。结果表明,雷州火山岩的喷发主要集中18万年前后。定年结果还表明,对于年轻样品,基于尼尔值计算的K-Ar年龄及40Ar/39Ar表观年龄偏老,等时线年龄相对较为可靠。对同一样品的斑晶、基质作斑晶-基质等时线计算,只有在斑晶基质满足同源条件时才有意义。本文首次提出,通过对比未照射样品的初始36Ar/38Ar值的均一性,以检验样品是否同源,确认斑晶-基质等时线年龄的可信度。据此,等时线的处理方法可以推广应用于特定区域内全部同源同时样品。     

New U-Pb zircon and Ar/Ar muscovite age constraints on the emplacement of the Lizio syn-tectonic granite (Armorican Massif, France)

LA-ICP-MS U-Pb analyses performed on zircon grains from the Lizio granite yielded an emplacement age of 316 ± 6 Ma. Typical S-C structures show that the Lizio granite was emplaced contemporaneously with dextral shearing along the northern branch of the South Armorican Shear Zone and that it was therefore active at that time. ⁴⁰Ar/³⁹Ar analyses performed on muscovite grains yielded plateau dates ranging between 311.5 and 308.2 Ma. Muscovite chemistry is typical of primary magmatic muscovite, which precludes a late fluids-induced resetting of the K-Ar isotopic system. ⁴⁰Ar/³⁹Ar dates thus likely correspond to the cooling ages below the argon closure temperature. Considering the uncertainties on the measured ages, we can propose that either the Lizio granite cooled down quickly in less than a million of years or that it remained in a hot environment for several millions of years after its emplacement. This latter scenario could have been sustained by shear heating during dextral shearing along the northern branch of the South Armorican Shear Zone.     

年轻火山岩的定年:进展与问题

年轻火山岩定年对人类的起源与进化、地质年表建立、古环境演化、火山灾害、岩浆演化及地球动力学等研究非常重要。由于年轻样品放射性成因子体积累较少、大气氩含量高,微量的过剩氩极难识别,使得年轻火山岩及其沉积地层高精度定年一直是地质年代学中最具挑战性的课题之一。过去几年,年轻火山岩定年在技术上的进展主要体现在定年精度和准确度不断提升,尤其是利用新型多接收稀有气体质谱对单颗粒样品进行逐步升温~(40)Ar/~(39)Ar定年,是方法学上最重要的进展之一。本文总结了年轻火山岩~(40)Ar/~(39)Ar定年的现状、影响因素和相关定年技术及应用,以引起大家的关注和思考,共同提高我国年轻火山岩定年的技术水平。利用新型多接收质谱和创新的实验方法,通过对全球重要火山喷发事件和年轻国际标准样的研究,广泛开展实验室间的对比是提高国内~(40)Ar/~(39)Ar年代学水平并在年轻火山岩定年中取得突破的重要途径,也是当前~(40)Ar/~(39)Ar年代学研究的重要方向。     

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.     

Intercalibration of the Hb3gr Ar/Ar dating standard

The ⁴⁰Ar/³⁹Ar dating technique is based on the knowledge of the age of neutron fluence monitors (standards). Recent investigations have improved the accuracy and precision of the ages of most of the Phanerozoic-aged standards (e.g. Fish Canyon Tuff sanidine (FCs), Alder Creek sanidine, GA1550 biotite and LP-6 biotite); however, no specific study has been undertaken on the older standards (i.e. Hb3gr hornblende and NL-25 hornblende) generally used to date Precambrian, high Ca/K, and/or meteoritic rocks.In this study, we show that Hb3gr hornblende is relatively homogenous in age, composition (Ca/K) and atmospheric contamination at the single grain level. The mean standard deviation of the ⁴⁰Ar^?/³⁹Ar_K (F-value) derived from this study is 0.49%, comparable to the most homogeneous standards. The intercalibration factor (which allows direct comparison between standards) between Hb3gr and FCs is R_FCs^Hb3gr = 51.945 ± 0.167. Using an age of 28.02 Ma for FCs, the age of Hb3gr derived from the R-value is 1073.6 ± 5.3 Ma (1σ; internal error only) and ± 8.8 Ma (including all sources of error). This age is indistinguishable within uncertainty from the K/Ar age previously reported at 1072 ± 11 Ma [Turner G., Huneke, J.C., Podosek, F.A., Wasserburg, G.J., 1971. ⁴⁰Ar-³⁹Ar ages and cosmic ray exposure ages of Apollo 14 samples. Earth Planet. Sci. Lett. 12, 19-35].The R-value determined in this study can also be used to intercalibrate FCs if we consider the K/Ar date of 1072 Ma as a reference age for Hb3gr. We derive an age of 27.95 ± 0.19 Ma (1σ; internal error only) for FCs which is in agreement with the previous determinations. Altogether, this shows that Hb3gr is a suitable standard for ⁴⁰Ar/³⁹Ar geochronology.     

Amphibole Ar/Ar Geochronology from the Okcheon Metamorphic Belt, South Korea and its Tectonic Implications

An understanding of the Okcheon Metamorphic Belt (OMB) in South Korea is central to unraveling the tectono-metamorphic evolution of East Asia. Amphibole-bearing rocks in the OMB occur as calcsilicate layers and lenses in psammitic rocks, in the psammitic rocks themselves, and in the mafic volcanic layers and intrusives. Most amphiboles fail to show ⁴⁰Ar/³⁹Ar plateau ages; those that do have ages ranging from 132 to 975 Ma. The disturbed age pattern and wide variation in ⁴⁰Ar/³⁹Ar ages can be related to metamorphic grade, retrograde chemical reactions, excess Ar and amphibole composition. The oldest age (975 Ma) can be interpreted either as an old igneous or metamorphic age predating sedimentation or a false age caused by excess Ar. The youngest age of 132 Ma and the disturbed age pattern found in amphiboles from rocks located close to Jurassic granitoids are the result of retrograde thermal metamorphic effects accompanying intrusion of the granitoids. Some medium- or coarse-grained amphiboles in the calcsilicates are aggregates of fine-grained crystals. As a result, they are heterogeneous and prove to be readily affected by excess Ar. A disturbed age pattern in amphiboles from the calcsilicates occurring in the high-grade metamorphic zone may also be the product of excess Ar. On the other hand, the disturbed pattern of amphiboles present in the calcsilicates from the low-grade metamorphic zone could arise from both excess Ar and mixed ages. However, amphiboles from psammitic rocks and some calcsilicates in the high-grade metamorphic zone and in intrusive metabasites display real plateau ages of 237 to 261 Ma. The temperature conditions in the high-grade metamorphic zone were higher than the argon closing temperature for amphibole, and the amphiboles in this zone give plateau ages only when they are homogeneous in composition, lack excess Ar, and have not been thermally affected by intrusion of the granitoids. The unmodified ⁴⁰Ar/³⁹Ar ages prove rather younger than the age of the Late Paleozoic metamorphic event of 280 to 300 Ma, but they are close to muscovite K-Ar ages of 263 to 277 Ma. These ⁴⁰Ar/³⁹Ar amphibole ages are interpreted as the time of cooling that followed the main regional, intermediate-P/T metamorphic climax. The results demonstrate that interpretation of ⁴⁰Ar/³⁹Ar amphibole ages in an area subjected to several metamorphic events can be accomplished only by undertaking a thorough tectono-metamorphic study, accompanied by detailed chemical analysis of the amphiboles.     

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.     

Comparison of Conventional K–Ar and Ar/Ar Dating of Young Mafic Volcanic Rocks

K–Ar and ⁴⁰Ar/³⁹Ar ages have been measured on nine mafic volcanic rocks younger than 1 myr from the Snake River Plain (Idaho), Mount Adams (Washington), and Crater Lake (Oregon). The K–Ar ages were calculated from Ar measurements made by isotope dilution and K₂O measurements by flame photometry. The ⁴⁰Ar/³⁹Ar ages are incremental-heating experiments using a low-blank resistance-heated furnace. The results indicate that high-quality ages can be measured on young, mafic volcanic rocks using either the K–Ar or the ⁴⁰Ar/³⁹Ar technique. The precision of an ⁴⁰Ar/³⁹Ar plateau age generally is better than the precision of a K–Ar age because the plateau age is calculated by pooling the ages of several gas increments. The precision of a plateau age generally is better than the precision of an isotope correlation (isochron) age for the same sample. For one sample the intercept of the isochron yielded an ⁴⁰Ar/³⁶Ar value significantly different from the atmospheric value of 295.5. Recalculation of increment ages using the isochron intercept for the composition of nonradiogenic Ar in the sample resulted in much better agreement of ages for this sample. The results of this study also indicate that, given suitable material and modern equipment, precise K–Ar and ⁴⁰Ar/³⁹Ar ages can be measured on volcanic rocks as young as the latest Pleistocene, and perhaps even the Holocene.     

稀有气体同位素地球化学在矿床学研究中的应用进展

稀有气体因其化学惰性以及在不同来源地质体中的同位素组成差异很大,在研究成矿流体来源、演化和壳-幔相互作用过程中具有非常重要的意义。另外,由于~4He、⁴⁰Ar是放射成因子体同位素,具有年代积累效应,因此,它们常被用于同位素测年。本文简要回顾了流体包裹体中稀有气体同位素的后生影响和样品、分析方法选择注意事项,以及近年来稀有气体同位素在成矿流体示踪,⁴⁰K-⁴⁰Ar、⁴⁰Ar-39Ar定年及(U-Th)/He定年方面的研究进展。已有研究证实流体包裹体中的稀有气体可能受后期扩散丢失、后生叠加和同位素分馏的影响,要根据目的选择不同的分析方法;稀有气体同位素可以示踪不同类型矿床的流体来源、演化及壳-幔相互作用、稀有气体同位素与卤素联合运用可以用来指示流体和盐度来源、演化过程以及矿物沉淀机制等,~3He/热的研究可以追溯流体的热源及其运移方式;流体包裹体⁴⁰Ar-³⁹Ar可以用于矿床直接定年,表生含钾矿物的⁴⁰K-⁴⁰Ar、⁴⁰Ar-³⁹Ar定年以及锆石、磷灰石和铁氧化物(U-Th)/He定年可为矿床及氧化带的形成时间、矿床形成后的抬升、剥露历史、古气候演化等重大地质问题讨论提供大量有意义的信息。     

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.