激光显微探针40Ar/39Ar 定年方法研究

实验结果表明，在激光探针40Ar/36Ar年龄和常规40Ar/39Ar年龄之间有较好的吻合性，多次测定BSP-1角闪石国际标样年龄值大部分在2020-20900Ma之间，多次测定周口店花岗岩中ZBH-25国内标样年龄值大部分在130-135.9Ma。分析区域可小到30μm以下（激光束本身可被聚集到10μm以下）。研究表明，激光显微探针技术在下述工作中将是一个极有前途的工具①测定不易大量获取的样品年龄；②研究遭受多期地质历史事件作用因而有复杂Ar状态的岩石年代；③研究在岩石样品中填充在不同结构位置上的矿物年     

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.     

^40Ar／^39Ar测年中的冷却年龄和变形年龄

^40Ar／^39Ar法年龄数据的解释与Ar同位素在矿物中的封闭温度有关。冷却年龄只能限制变质——变形事件发生的时间区间,不能真正代表地质事件的发生时间。因此,必须想办法得到变形年龄。本文从封闭温度概念出发,探讨了压力、冷却速率、有效扩散范围和几何形态、颗粒大小、动力学参数等对矿物封闭温度的影响,介绍了新近提出的“封闭窗”概念,并讨论了在什么情况下可以获得变形年龄。     

激光Ar/Ar微区定年的应用及展望

40Ar/39Ar定年中,存在一些使用传统的大样逐步升温技术难以处理的难题,如变质及沉积岩样品常含有多期次矿物而难以获得理想结果,过剩Ar在样品中的分布以及来源问题一直难以有效解决,根据缓慢冷却钾长石的40Ar/39Ar年龄谱提出的热演化模型也因为Ar在矿物中扩散机制的不明确性而不断受到质疑。20世纪90年代将紫外激光（UV-laser）成功引入40Ar/39Ar年代学分析后,为解决这些难题提供了一种思路。借助激光微区     

40Ar-39Ar同位素测年方法及其应用

^40Ar—^39Ar测年法的出现，为同位素地质年代学开辟了一个新的领域；但过剩氩的存在、年龄谱的分析方法，又制约着地质事件的年龄解释。在介绍该方法的原理、校正、年龄谱的分析和应用及过剩氩问题等方面内容的基础上，结合阿尔金断裂研究实例，对该断裂中的新生矿物进行了^40Ar-^39Ar测年，进而确定了阿尔金断裂走滑活动的年龄。     

40Ar/39Ar dating of cleavage formation in tuffs during anchizonal metamorphism

⁴⁰Ar/³⁹Ar incremental-release analyses were carried out on whole-rock and constituent white mica (illite)-rich size fractions (0.63–1 to 6.3–20 m) within two very-low grade, penetratively cleaved metatuffs of contrasting anchizonal metamorphic grade (northeastern Rheinisches Schiefergebirge, Federal Republic of Germany). One sample from the upper anchizone displays internally concordant ⁴⁰Ar/³⁹Ar spectra with plateau ages ranging between ca. 316 and 325 Ma. These are similar to conventional K-Ar ages determined for the whole-rock and size fractions. Together the isotopic results suggest that cleavage formed at ca. 320 Ma during a concomitant very-low grade metamorphism. This is consistent with biostratigraphic controls which suggest that metamorphism and cleavage formation occurred during the Westphalian.A metatuff sample from the middle anchizone records more internally discordant ⁴⁰Ar/³⁹Ar age spectra with total-gas ages ranging from 366 to 372 Ma. These are ca. 35–45 Ma older than corresponding conventional K-Ar ages, indicating marked recoil-loss of ³⁹Ar occurred during irradiation. Transmission electron microscopy reveals that white mica grains within size fractions from the upper anchizone sample have clearly defined, straight edges whereas those within the middle anchizone samples are embayed and diffuse. This results in an increase in surface/volume ratio and therefore greater susceptibility for recoil-loss of ³⁹Ar in the middle anchizone sample. Grain-edge morphology appears to be a major factor in determining the extent of recoil-loss of ³⁹Ar during ⁴⁰Ar/³⁹Ar analysis of fine-grained size fractions.     

桐柏——大别山主要构造热事件及40Ar/39Ar地质定年研究

桐柏——大别山是一条复合造山带。在其演化过程中曾经历了扬子旋回（1000Ma-761Ma）和加里东旋回（470Ma-401Ma）两个板块构造旋回的俯冲-碰撞造山作用，之后又经历了早、中华力西（357Ma-314Ma）的平移走滑和晚华力西（286Ma-261Ma）、印支期（224Ma-185Ma）、燕山期（130Ma-111Ma）逆掩或逆冲推覆的陆-陆叠覆造山作用。印支期的高压超高压变质岩系是在陆-陆叠覆造山作用下形成的。燕山期的造山不仅具显著的深层次构造岩浆作用特点，而且还伴随快速的隆升作用。     

Direct dating of folding events by 40Ar/39Ar analysis of synkinematic muscovite from flexural-slip planes

Timing of folding is usually dated indirectly, with limited isotopic dating studies reported in the literature. The present study investigated the timing of intracontinental, multi-stage folding in Upper Proterozoic sandstone, limestone, and marble near Beijing, North China, and adjacent regions. Detailed field investigations with microstructural, backscattered electron (BSE) images and electron microprobe analyses indicate that authigenic muscovite and sericite crystallized parallel to stretching lineations/striations or along thin flexural-slip surfaces, both developed during the complex deformation history of the study area, involving repeated compressional, extensional and strike-slip episodes. Muscovite/sericite separates from interlayer-slip surfaces along the limbs and from dilatant sites in the hinges of folded sandstones yield muscovite ⁴⁰Ar/³⁹Ar plateau ages of ∼158–159 Ma, whereas those from folded marble and limestone samples yield ages of 156 ± 1 Ma. Muscovite from thin flexural-slip planes on fold limbs and hinges yields ages within analytical error of ∼155–165 Ma. Further muscovite samples collected from extensionally folded limestone and strike-slip drag folds yield younger ages of 128–125 Ma with well-defined plateaus. To assess the potential influence of the detrital mica component of the host rock on the age data, two additional muscovite samples were investigated, one from a folded upper Proterozoic–Cambrian sandstone outside the Western Hills of Beijing and one from a folded sandstone sampled 20 cm from folding-related slip planes. Muscovite separates from these samples yield significantly older ages of 575 ± 2 Ma and 587 ± 2 Ma, suggesting that the timing of folding can be directly determined using the ⁴⁰Ar/³⁹Ar method. This approach enables the identification and dating of distinct deformation events that occur during multi-stage regional folding. ⁴⁰Ar/³⁹Ar dating can be used to constrain the timing of muscovite and sericite growth at moderate to low temperatures (<400 °C) during folding, yielding well-defined plateau ages and thereby the age of deformation in the upper crust.     

Calibration of GA1550 biotite standard for K/Ar and 40Ar/39Ar dating

The mineral separate GA1550 biotite has become an international standard for K/Ar and ⁴⁰Ar/³⁹Ar dating studies, although it was prepared as an intralaboratory standard at ANU to monitor tracer depletion from a gas pipette. It is one of a small number of samples that has been calibrated against ³⁸Ar tracers, some of which had been mixed with known amounts of atmospheric argon, so that a so-called primary calibration has been performed. By measuring GA1550 biotite against additional tracers from the same batch we have determined the radiogenic argon content of this sample as 1.342 (± 0.007) × 10^? 9 mol/g, and together with the measured K content of 7.645 (± 0.050) weight percent, we derive a best estimate for the K/Ar age as 98.5 ± 0.5 Ma, where the error is derived from averaging the ages determined relative to the ³⁸Ar tracer.     

豫西南银洞沟铅锌银矿蚀变岩白云母~(40)Ar/~(39)Ar年龄及地质意义

通过对豫西南银洞沟矿床Y1矿脉的近矿蚀变岩中选取白云母进行40 Ar/39 Ar年龄测定,获得坪年龄为(284.5±2.0)Ma,相应的等时线年龄为(287.1±4.9)Ma。同时,选取本矿脉的白云母和闪锌矿颗粒进行Rb-Sr同位素年龄测试和方铅矿的铅模式年龄计算,得出与白云母40 Ar/39 Ar年龄测定相近的年龄范围,可见,银洞沟铅锌银矿的成矿年龄为成矿早阶段的蚀变年龄,成矿时代应该不早于284Ma。     

武当地块基性岩墙群^40Ar—^39Ar定年及其地质意义

通过对南秦岭武当地块内变形变质基性岩墙群中的角闪石、黑云母矿物的４０Ａｒ－３９Ａｒ定年,获得角闪石三组年龄,分别为高温坪年龄６９４．４±２１Ｍａ,中温坪年龄３８４．４±３Ｍａ（相应等时线年龄为３８３．３±１０Ｍａ）和低温视年龄２４０～１８０Ｍａ。黑云母单一坪年龄为２３５．３±２Ｍａ（相应等时年龄为２３６．７±６Ｍａ）。结合本区基性岩墙已获得的Ｓｍ－Ｎｄ全岩等时年龄（７８２±１６４Ｍａ）分析,７８２±１６４Ｍａ～６９４．４±２１Ｍａ代表岩墙侵位、冷却过程的时间,提供了武当地块裂解的构造事件年龄;３８４．４±３Ｍａ和约２４０Ｍａ则代表岩墙群侵位后两期重要构造－热事件的改造年龄。上述为武当地块的构造作用过程和南秦岭构造带的形成、演化提供了重要证据。     

自动化~(40)Ar/~(39)Ar定年设备研制

自主研发的小型高效气体纯化系统、二氧化碳激光熔样系统、流体包裹体提取系统和空气氩标定系统,与新一代小型高灵敏度多接收稀有气体质谱仪Argus VI联机,建立了激光阶段加热40Ar/39Ar定年、真空击碎流体包裹体40Ar/39Ar定年和空气氩标定等分析测试方法。开放式Qtegra Noble Gas软件和外部设备控制器Peri Con,使用户能够方便地自主增减和控制外部设备,实现计算机自动控制。通过"触点闭合"方式,Qtegra软件触发国产二氧化碳激光加热熔样软件启动,两者协调工作,实现激光阶段加热40Ar/39Ar定年分析的实验流程全自动化。空气氩分析获得了非常稳定的40Ar/36Ar比值,展示了自制空气氩标定系统和小型纯化系统的卓越性能,可资借鉴。新建40Ar/39Ar实验室为开展油气成藏年代学研究提供了一个高精度的测试平台。     

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.     

宁芜盆地凹山和东山铁矿床中阳起石的激光39Ar-40Ar年代学研究

文章通过对凹山和东山铁矿床中特征的组合矿物之一伟晶状阳起石进行激光39Ar-40Ar法定年,精确测定了玢岩铁矿的成矿时代。其中东山铁矿中新鲜阳起石(黑绿色)的39Ar-40Ar等时线年龄在126～129Ma之间,与赋矿围岩大王山组火山岩中角闪石的等时线年龄(127Ma)一致,证明成矿与成岩密切相关,成矿与成岩是同时期的产物。而凹山铁矿中蚀变阳起石(灰绿色)的39Ar-40Ar等时线年龄为(114±16)Ma。2种阳起石分别形成于成矿作用的不同阶段,黑绿色新鲜阳起石与磷灰石、磁铁矿同期形成,形成于岩浆向热液演化的高温阶段,在成岩和成矿之后的冷却过程中,矿体和潜火山岩体具有相同的闪石封闭温度(500℃±);而灰绿色蚀变阳起石形成于中期阳起石(透辉石)-钠长石-磷灰石-磁铁矿化矿体围岩蚀变阶段。     

海绿石 K-Ar、40Ar/39Ar 年代学研究

海绿石是与沉积岩同时形成的高钾层状硅酸盐自生矿物，其 K-Ar、40Ar/39Ar 年龄存在失真现象。笔者认为，引起年龄失真的主要原因是由于该矿物结构中含有可膨胀层。通过测量可膨胀层含量及中子活化过程中39Ar的丢失率，使可对海绿石常规 K-Ar、40Ar/39Ar 年龄进行校正，得到其年龄校正公式。     

铜陵地区中酸性侵入岩年代学研究

本文选择了铜陵地区主要岩石类型的代表性岩体中黑云母为测定对象，准确地测定了侵入岩的４０Ａｒ／３９Ａｒ同位素年龄。测定结果表明，区内侵入岩的年龄均小于１４０Ｍａ，属燕山晚期的产物，后期热事件为成矿时代，晚于岩浆侵入时代，在此基础上，分析了ＫＡｒ法、ＲｂＳｒ法同位素年龄产生偏差的原因     

Ar and Ar recoil loss during neutron irradiation of sanidine and plagioclase

The ⁴⁰Ar/³⁹Ar dating technique requires the activation of ³⁹Ar via neutron irradiation. The energy produced by the reaction is transferred to the daughter atom as kinetic energy and triggers its displacement, known as the recoil effect. Significant amounts of ³⁹Ar and ³⁷Ar can be lost from minerals leading to spurious ages and biased age spectra. Through two experiments, we present direct measurement of the recoil-induced ³⁹Ar and ³⁷Ar losses on Fish Canyon sanidine and plagioclase. We use multi-grain populations with discrete sizes ranging from 210 to <5 μm. One population consists of a mixture between sanidine and plagioclase, and the other includes pure sanidine.We show that ³⁹Ar loss (depletion factor) for sanidine is ∼3% for the smallest fraction. Age spectra of fractions smaller than ∼50 μm show slight departure from flat plateau-age spectrum usually observed for large sanidine. This departure is roughly proportional to the size of the grain but does not show typical ³⁹Ar loss age spectra. The calculated thickness of the total depletion layer d₀(sanidine) is 0.035 ± 0.012 (2σ). This is equivalent to a mean depth of the partial depletion layer (x₀) of 0.070 ± 0.024 μm. The latter value is indistinguishable from previous values of ∼0.07-0.09 μm obtained by argon implantation experiments and simulation results.We show that it is possible to adequately correct ages from ³⁹Ar ejection loss provided that the d₀-value and the size range of the minerals are sufficiently constrained. As exemplified by similar calculations performed on results obtained in a similar study of GA1550 biotite [Paine J. H., Nomade S., and Renne P. R. (2006) Quantification of ³⁹Ar recoil ejection from GA1550 biotite during neutron irradiation as a function of grain dimensions. Geochim. Cosmochim. Acta70, 1507-1517.], the d₀(biotite) is 0.46 ± 0.06 μm. The significant difference between empirical results on biotite and sanidine, along with different simulation results, suggests that for biotite, crystal structures and lattice defects of the stopping medium and possibly subsequent thermal degassing (due to ∼150-200 °C temperature in the reactor or extraction line bake out) must play an important role in ³⁹Ar loss.The second experiment suggests that ³⁷Ar recoil can substantially affect the age via the interference corrections with results that suggest up to ∼98% of ³⁷Ar can be ejected from the ∼5 μm grain dimension.Further investigation of silicates of various compositions and structures are required to better understand (and correct) the recoil and recoil-induced effects on both ³⁹Ar and ³⁷Ar and their influences on ⁴⁰Ar/³⁹Ar dating.     

Formation and exhumation of blueschists and eclogites from NE Oman: new perspectives from Rb–Sr and 40Ar/39Ar dating

Seven eclogite facies samples from lithologically different units which structurally underlie the Semail ophiolite were dated by the ⁴⁰Ar/³⁹Ar and Rb–Sr methods. Despite extensive efforts, phengite dated by the ⁴⁰Ar/³⁹Ar method yielded saddle, hump or irregularly shaped spectra with uninterpretable isochrons. The total gas ages for the phengite ranged from 136 to 85 Ma. Clinopyroxene–phengite, epidote–phengite and whole‐rock–phengite Rb–Sr isochrons for the same samples yielded ages of 78 ± 2 Ma. We therefore conclude that the eclogite facies rocks cooled through 500 °C at c. 78 ± 2 Ma, and that the ⁴⁰Ar/³⁹Ar dates can only constrain maximum ages due to the occurrence of excess Ar inhomogeneously distributed in different sites. Our new results lead us to conclude that high‐pressure metamorphism of the Oman margin took place in the Late Cretaceous, contemporaneous with ophiolite emplacement. Previously published structural and petrological data lead us to suggest that this metamorphism resulted from intracontinental subduction and crustal thickening along a NE‐dipping zone. Choking of this subduction zone followed by ductile thinning of a crustal mass wedged between deeply subducted continental material and overthrust shelf and slope units facilitated the exhumation of the eclogite facies rocks from depths of c. 50 km to 10–15 km within c. 10 Ma, and led to their juxtaposition against overlying lower grade rocks. Final exhumation of all high‐pressure rocks was driven primarily by erosion and assisted by normal faulting in the upper plate.     

Provenance of Cape Supergroup sediments and timing of Cape Fold Belt orogenesis: Constraints from high-precision 40Ar/39Ar dating of muscovite

The Permian Cape Fold Belt (CFB) of South Africa forms part of a major orogenic belt that originally extended from Argentina, across southern Africa and into Antarctica. The CFB is dominated by complexly folded and faulted rocks of the siliciclastic Cape Supergroup that were deposited in the Cape Basin. The provenance of the Cape Supergroup, timing of deformation and tectonic setting are poorly constrained. U-Pb detrital zircon provenance studies suggest that the Cape Basin received sedimentary detritus from the African Mesoproterozoic Namaqua-Natal Metamorphic Belt, Neoproterozoic-Cambrian Pan-African Belts and the Brasiliano orogenic belts of South America, Africa and Antarctica. However, as zircon is able to survive multiple orogenic and sedimentary transport cycles, complementary provenance tools are required to confirm Cape Supergroup provenance. Previous studies have suggested both uni-modal and multi-modal models for the timing of CFB orogenesis. In the current study, structurally controlled, muscovite-bearing samples were collected along several north-south traverses across the CFB. Detailed textural and mineral chemistry analyses identified multiple muscovite populations, commonly with complex intergrowth features. High precision ⁴⁰Ar/³⁹Ar analyses reveal a dominant 490–465 Ma detrital muscovite population, lending support to a largely South American provenance for the Cape Supergroup. Lesser detrital muscovite populations in the range 650–500 Ma and >730 Ma, corroborate previous zircon provenance studies suggesting Pan-African/Brasiliano terranes and the Namaqua-Natal Metamorphic Belt as significant sediment sources, respectively. Detailed ⁴⁰Ar/³⁹Ar analyses of multiple neo-crystallised muscovite samples are consistent with a single major phase of CFB deformation occurring between 253.4 and 249.6 Ma. This age is interpreted to represent either the peak or final dominant phase of CFB deformation.     

大别山碧溪岭榴辉岩450 Ma年龄信息:石榴子石流体包裹体40Ar-39Ar定年初步结果

高压-超高压变质岩常含有过剩40Ar,排除过剩40Ar的干扰是获得可靠40Ar-39Ar年龄的关键.本文试图从流体包裹体40Ar-39Ar定年的角度,探讨榴辉岩40Ar-39Ar定年技术与过剩40Ar问题.采用真空击碎法提取流体包裹体,对碧溪岭浅色榴辉岩石榴子石进行40Ar-39Ar定年,获得了下降型年龄谱:最初9个阶段年龄谱总体上呈逐渐下降,表观年龄从2 226 Ma下降到753 Ma,这是次生包裹体(含过剩40Ar)与原生包裹体(不含过剩40Ar)混合的结果;第10阶段至第22阶段(末阶段),年龄谱呈平缓波动,表观年龄变化小,对应坪年龄为(449±18)Ma(2σ,39Ar占59.5%),这是微小的原生流体包裹体的贡献,此13个数据点在36Ar/40Ar-39Ar/40Ar图上构成线性关系很好的反等时线,对应的等时线年龄(448±34)Ma代表了石榴子石的结晶年龄,40Ar/36Ar初始比值(292±5)表明原生包裹体不含过剩40Ar.