Towards single grain ESR dating of sedimentary quartz: first results

In optically stimulated luminescence dating, apparent ages of individual grains are thought to reflect a wide distribution of initial bleaching levels in hard to bleach sediments. Although having a larger age range (up to 1 Ma and beyond), this approach has not been used yet in electron spin resonance (ESR) dating. Here we report on the first results of ESR measurements on single sedimentary quartz grains. Initial bleaching levels are evaluated for two different River Meuse deposits in Limburg, NE Belgium. Measurements were done with a Q-band ESR spectrometer on transparent quartz grains of sufficiently large diameter (0.5–0.7 mm). Single crystal ESR properties were used to identify different ESR active centres. In about 50% of the selected grains an Al and/or Ti–Li signal was detected and the latter has been selected for further measurements. Artificial bleaching experiments show a strong signal decrease with UV light exposure. After gamma-ray irradiation, a number of different signal intensity vs. artificial dose curves could be observed: exponential growth, exponential saturation, linear, with inflexion points, and unclear ones. Many grains show increasing ESR signals with doses up to 1000 Gy, suggesting that the age range could be extended over 1 Ma, covering the Middle Pleistocene and part of the Early Pleistocene. Accumulated doses of individual grains were calculated using the additive dose method. The results show a large dose distribution of individual grains for both deposits. It is concluded that insufficiently bleached grains can be detected using single grain ESR measurements of sedimentary quartz in a fluvial environment.     

Single quartz grain electron spin resonance (ESR) dating of a contemporary desert surface deposit,Eastern Desert,Egypt

Signal resetting by sunlight prior to burial is a crucial assumption in electron spin resonance (ESR) dating of sediments. This resetting process is expected to be completed to a greater extent in arid than in fluvial environments. The present paper investigates the natural and artificially irradiated signal intensity of Ti related centres in single quartz grains collected from the desert surface (Eastern Desert, Egypt) in order to test this hypothesis. The results suggest that in most grains both the Ti–Li and Ti–H signal are completely reset to zero. Additive dose curves based on the sum of both Ti centres show an anomaly in the low dose region. Possible causes for this behaviour are briefly discussed. Three fitting procedures are conducted and each of them shows a different palaeodose distribution with a rather large spread in D_E values. It is concluded that similar fossil deposits would be datable by single grain ESR using Q-band measurements of the Ti–Li or Ti–H signals in quartz.     

石英电子自旋共振（ESR）的地学研究现状与展望

电子自旋共振（ESR）是一种对断层物质、燧石、火山灰和沉积物（水系、风成、冰川）定年的重要方法,它广为接受的测年范围为第四纪。对断层泥和沉积物样品,石英ESR信号的不完全归零往往使ESR年龄偏老,多重ESR中心法和颗粒大小“平顶判据”是判断信号归零特征的两种有效方法。为将ESR测年范围拓展至前第四纪,通常采用石英氧空位在加热转化后极大增强的E’心作为测年信号,但由于石英氧空位形成转化机理不明确,加热后增强的ESR信号与地质年龄的相关性有待进一步验证。近期研究表明石英ESR的封闭温度为49 ℃～82 ℃,可在比磷灰石（U-Th）/He更低的温度区间内研究地球近地表的构造演化过程。释光技术热年代学研究发展迅速,与之测年原理接近的ESR在低温热年代学领域展现了良好的应用前景,它与释光及磷灰石（U-Th）/He可相互比对、共同提高地球近地表构造和地形演化问题的分析精度。     

Simultaneous determination of alteration and eruption ages of volcanic rocks by electron spin resonance

The alteration and eruption ages of Japanese welded tuffs were estimated by the method of ESR using Ge, OHC and Al centers in quartz whose stabilities are different. The ages obtained from the Ge and OHC centers were 1–2 Ma, however the ages from the Al center varied from 0.059 to 1.36 Ma. The comparison of these ages with thermoluminescence (TL) and fission track (FT) ages proves that the ESR age of the Al center, which agrees with the TL age, shows the thermal history and, in an ideal case, gives the alteration age: those of the Ge and OHC centers, which agree with FT age, indicate the eruption age. Therefore, this method enables us to describe the thermal history of a rock.     

Research Advances in ESR Provenance Tracing Methods of Quartz in Sediments

The ESR (Electron Spin Resonance) signals of quartz is a newly developed sediment provenance tracing method. In this paper, the various ESR signals in quartz, historical development of quartz ESR signals in sediment provenance tracing, thermal stability characteristics of heat treated E’ center, the potential use of quartz nature E’ center and the irradiated Al/Ti center, as well as successful applications in aeolian sediments, river sediments and marine sediments provenance tracing, were briefly reviewed. The most useful ESR centers of quartz include the heat treated E’ center, the nature E’ center, the Al center and the Ti center. According to recent application researches, the heat-treated E’ center is the most commonly practiced among them while the significance of provenance tracing by Al and Ti centers are still in experimental and theoretical stage. Moreover, nature signal intensities of quartz E’ center not only show a significant dependence on lithology both in bedrocks and deposits, but also can reflect the mixture ratio of deposits with different types of sourced bedrocks. As for the study objects, this method has been successfully used in the studies of provenance area of East Asian dust, the temporal and spatial changes of Loess Plateau provenance, the provenance change of aeolian sediment over time and space on Japanese Islands, as well as sediment provenance tracing of Japan Sea sediments. In addition, the ESR provenance tracing of quartz has promising application prospect in quantitative and semi-quantitative analysis of fluvial sediment provenance tracing. Along with the development of ESR dating, this method can significantly reflect and reconstruct the relationship among regional tectonic movements, geomorphic evolution, and climate evolution. In future work, the combination of trace elements provenance tracing and ESR signals provenance tracing in quartz will help improve and promote the development of sediments provenance tracing methods.     

Electron spin resonance dating of burned flint from Kebara Cave,Israel

Electron spin resonance (ESR) measurements of heated flint from Kebara cave show the presence of two radiation sensitive signals: E' and Al. Both are strongly interfered with by organic signals produced during heating of the flint. The signal subtraction method of Porat and Schwarcz (1991) was used to determine equivalent doses for flint samples from levels VII-XII, for which thermoluminescence (TL) ages on the same samples are known. Ages were determined using dose rates based on analyses of the flint and TLD measurements of external dose rates. The average E' age of 48.5 ± 5.1 ka is much less than the average TL age (62.2 ± 4.3 ka), whereas the average age of 64.6 ± 12 ka given by the Al signal is in good agreement with the TL age, but with much larger dispersion. © 1994 John Wiley & Sons, Inc.     

断层电子自旋共振定年中石英信号强度的影响因素分析

电子自旋共振(ESR)是一种利用矿物在地质环境中的累计辐射能进行测年的技术方法,它采用的测年矿物石英广泛分布,并具有记录断层作用良好的计时零点,是同位素测年的重要补充。ESR信号强度是决定ESR年龄精确度的关键因素,但是各种参数条件对测量结果的影响方式及其程度缺乏系统研究。本文以取自断层带石英的一种顺磁中心——E’心为研究对象,运用单因素重复性实验方法,分析石英ESR定年中5种影响因素与ESR信号强度的相关关系。结果表明,微波功率、调制幅度、扫描宽度是影响ESR信号强度的主控因素,样品管方位及直径对测量结果影响不大。微波功率0.02~0.1 m W、调制幅度0.25~0.4 Gs可作为精确测量断层泥石英E’心普适性的参数区间,过大或过小的扫描宽度均不利于ESR测量,可利用在大扫描宽度条件下先预扫描再精细扫描的方法确定合适的扫描宽度,重复测量后求取平均值可有效降低测量误差。利用本文提出的参数区间及其确定的方法测量断层泥石英的E’心信号强度,能显著提高ESR测量精度。     

Applicability of ESR dating using multiple centres to fault movement — The case of the Itoigawa-Shizuoka tectonic line, a major fault in Japan

No direct method for dating the fault movement has been hitherto established, except ESR dating whose applicability is disputed however. The most serious question in ESR dating is whether accumulated ESR signals are completely reset at the time of fault movement. When the defect centres are partially preserved at the time of previous faulting, the date obtained is uncertain. We have shown (Fukuchi et al., 1985, 1986), however, that we can judge correctly whether ESR signals were completely reset or not when the ESR signal counting is done for multiple ESR centres of different stabilities for resetting. From the data for completely reset centres, actual date of fault movement can be calculated.This multiple centre method was tested with samples whose ESR signal intensities are judged to be about zero at the time of fault movement. The result, which confirms the applicability for the fault movement dated back to 100 ka BP, is presented in this paper.     

云开地块印支期构造热事件叠加改造:来自片麻岩中多矿物U-Pb年代学的证据

云开地块显生宙的构造演化一直是华南板块的研究热点之一.通过对云开地块变质基底中片麻岩进行独居石、磷灰石和锆石LA-ICP-MS U-Pb定年,获得了434±6 Ma（MSWD=3.0）和437±12 Ma（MSWD=6.0）的岩浆锆石年龄,结合镜下观察,认为其代表的是片麻岩原岩（花岗质岩石）的形成时代,与区域上加里东期构造-岩浆-变质-深熔事件的时限基本一致,为武夷-云开加里东造山作用的产物;磷灰石经过普通铅校正后分别给出了241±13 Ma（MSWD=2.2）和242±6 Ma（MSWD=1.4）的变质年龄,独居石则分别获得了236.2±0.8 Ma（MSWD=0.66）和229.4±1.2 Ma（MSWD=2.4）的变质年龄,这些年龄结果与云开地块构造岩云母Ar-Ar年龄相一致,暗示云井地块经历了印支期（230~240 Ma）构造热事件的叠加改造.对片麻岩中黑云母电子探针数据分析显示其具有相对高的Al、Ti和Mg含量,X_Mg值为0.37~0.45,属于铁质黑云母,其Ti饱和温度计给出温度范围为650~700℃（±50℃）,与独居石估算温度580~640℃（±25℃）在误差范围内基本一致,暗示印支期构造热事件对云开地块的叠加改造温度达到了700℃.综上所述,认为云开地块现今的构造格局是在加里东期造山作用基础上叠加了印支期构造塑造而成,叠加温度可能达到了700℃;此外,在利用矿物对温压计恢复加里东期变质作用P-T轨迹时应着重考虑印支期构造热事件对矿物成分的再造作用.      

ESR dating of saline sediments using NaHCO3 and NaCl

Age estimates of NaCl and NaHCO₃ in the sediments at Searles Lake, California have been obtained using electron spin resonance (ESR). ESR signals are identified as H⁺Ca²⁺---CO₃³⁻ or H⁺---CO₂⁻ electron type and hole CO₃⁻ type centres, stabilized by impurities in NaHCO₃ and in NaCl. The total dose of natural radiation (TD) and the tentative ESR ages were determined using these signals based on U, Th and K analyses assuming uranium series disequilibrium for a simple infinite medium. Although ESR ages are concordant with the stratigraphy, radiation assessment considering the loss and incorporation of radioactive elements must be made to get reliable absolute ages.     

东秦岭—大别造山带南、北缘晚白垩世以来构造演化的石英ESR年代学研究

运用α石英热活化ESR定年法对东秦岭—大别造山带南、北缘58件样品进行了研究。结果显示,东秦岭—大别造山带南、北缘ESR年龄范围主要集中在晚白垩世以来(99.2～3.4 Ma)。结合区域地质事实分析,晚白垩世以来,东秦岭—大别造山带南缘的构造演化可划分为73.1～52.3 Ma伸展断陷期、39.1～27.2 Ma伸展-挤压的转换期和22.8～3.4 Ma挤压期;东秦岭—大别造山带北缘的构造演化可划分为89～70.1 Ma挤压隆升期、61.6～43.2 Ma伸展断陷期、37.2～22.6 Ma伸展-挤压的转换期和15.6～3.9 Ma挤压期。东秦岭—大别造山带南缘和北缘新生代构造演化特征基本相同,但是受多种因素控制,东秦岭—大别造山带南、北缘晚白垩世的构造演化存在较大差异。ESR测年结果与东秦岭—大别造山带南、北缘已有的地质事实相吻合,验证了ESR测年的可靠性。     

沉积物的ESR测年

对沉积物中石英ESR测年的特性进行了较为详细地研究，可用沉积物中石英的Ge心信号进行ESR测年；根据石英E心饱和功率较小这一特性，采用较大的微波功率可以测得较老海洋沉积物（大于0.5Ma）的ESR年龄；石英E心的异常较照剂量响应是判断海岸风成沙环境的一个标志。此外，还介绍了沉积物ESR测年在地质上的应用。     

秦岭地区城口—房县断裂带变形特征及ESR定年

秦岭城口—房县断裂带是秦岭造山带和扬子板块的分界断裂带, 平面上呈向南西突出的弧形, 构成大巴山弧。断裂带的宏观构造组合显示了断裂带由北向南强烈逆冲, 断层岩的宏观特征和显微构造特征表明断裂带以浅层脆性变形为特点, 对断层岩的有限应变测量得出岩石发生了中等到较弱的变形。由断裂带石英脉电子自旋共振 (ESR)定年,测得 11个石英脉的年龄集中在 3个年龄段(240~230Ma, 165~130Ma, 70~60Ma), 其中 7个样品的年龄集中在 165~130Ma之间, 由此推断断裂带活动于中晚侏罗世(165~130Ma)达到其构造变形最强烈时期。     

Genetic and ore-forming ages of the Fe–P–(Ti) oxide deposits associated with mafic–ultramafic–carbonatite complexes in the Kuluketage block,NW China

Abstract

During the past 50 years, many geological and ore-deposit investigations have led to the discovery of the Fe–P–(Ti)-oxide deposits associated with mafic–ultramafic–carbonatite complexes in the Kuluketage block, northeastern Tarim Craton. In this paper, we discuss the genetic and ore-forming ages, tectonic setting, and the genesis of these deposits (Kawuliuke, Qieganbulake and Duosike). LA-ICP-MS zircon U–Pb dating yielded a weighted mean ²⁰⁶Pb/²³⁸U ages of 811?±?5?Ma, 811?±?4?Ma, and 840?±?5?Ma for Kawuliuke ore-bearing pyroxenite, Qieganbulake gabbro and Duosike ore-bearing pyroxenite, respectively. The CL images of the Kawuliuke apatite grains show core–rim structure, suggesting multi-phase crystallisation, whereas the apatite grains from Qieganbulake and Dusike deposits do not show any core–rim texture, suggesting a single-stage crystallisation. LA-ICP-MS apatite ²⁰⁷Pb-corrected U–Pb dating provided weighted mean ²⁰⁶Pb/²³⁸U ages of 814?±?21?Ma and 771?±?8?Ma for the Kawuliuke ores, and 810?±?7?Ma and 841?±?7?Ma for Qieganbulake and Duosike ores, respectively. The core–rim texture in apatite by CL imaging as well as two different ore-forming ages in the core and rim of the apatite indicate two metallogenic events for the Kawuliuke deposit. The first metallogenic period was magmatic in origin, and the second period was hydrothermal in origin. The initial ore-forming age of the Kawuliuke Fe–P–Ti mineralisation was ca 814?Ma and the second one was ca 771?Ma. On the other hand, the ore-forming ages of the Qieganbulake and Duosike deposits were ca 810?Ma and ca 841?Ma, respectively. Qieganbulake and Duosike deposits were of magmatic origin. Combined with previous geochronological data and the research on the tectonic background, we infer that the Kawuliuke, Qieganbulake and Duosike Fe–P–(Ti)-oxide deposits were formed in a subduction-related tectonic setting and were the product of subduction-related magmatism.     

Geochemical characteristics,cooling history and mineralization significance of Zhangtiantang pluton in South Jiangxi Province,P.R. China

The zircon SHRIMP dating of the Zhangtiantang granite gave an age of 159±7 Ma., which shows that the granite was produced at the early Late Jurassic. The Ar-Ar plateau ages of biotite and K-feldspar from the Zhangtiantang pluton are 153.2±1.1 Ma and 135.8±1.2 Ma, respectively. The Ar-Ar anti-isochrone ages of biotite and K-feldspar are 152.5±1.7Ma and 135.4±2.7Ma, respectively. The ages represent the isotopic closure ages of minerals in the pluton. The Zhangtiantang granites are regarded as peraluminous crust-derived type granites to possess the typical geochemical characteristics of calc-alkaline rocks on continental margin, with enriched Si, K, Al (average value of A/CNK as 1.18), HREE, Rb, U, and Th, heavily depleted V, Cr, Co, Ni, Ti, Nb-Ta, Zr, Sr, P, and Ba, strongly negative Eu and common corundum normative (average value of C as 1.84). The εNd_(t) values of the Zhangtiantang granite are −5.84 to −7.79, and t _2DM values are 1.69 to 1.83 Ga, which indicates partial melting of continental-crust metamorphic sedimentary rocks during the Middle Proterozoic. The cooling history of the Zhangtiantang granitic pluton indicates that the cooling velocity of pluton was faster (about 67°C/Ma) from zircon (158 Ma) to biotite (152 Ma), and was slower (about12°C/Ma) from biotite (152.5 Ma) to K-feldspar (135.8 Ma). It can be deduced that the temporal gap (about 10 Ma) between the granite formmation and W-Sn mineralization in South China may be related to ordinary magma-hydrothermal processes by the variational cooling curve of the pluton. The Zhangtiantang pluton was formed in a compressive setting, with differentiation evolution and mineralization occurring in a relative relaxation setting.     

江南隆起带北缘新生代构造演化的石英ESR年代学研究

运用α石英热活化ESR定年法对江南隆起带北缘35件样品进行了研究。结果显示,江南隆起带北缘的石英脉ESR年龄范围在195.8~3.4 Ma之间,主要集中在喜山期(75~3.4 Ma)。结合其他地质证据,江南隆起带北缘新生代构造演化可以划分为伸展断陷期(75~61.5 Ma)和挤压隆升期(43.2~3.4 Ma)两个阶段。前者以发育正断层和断陷盆地为特征,后者以重力滑脱构造为特征。喜山期的构造作用对先存构造进行了强烈的改造,包括南华北、中下扬子和江南隆起带北缘的整个中国东部地区在喜山期都经历了显著的构造活动。ESR测年结果与江南隆起带已有地质事实相吻合,检验了ESR测年的可靠性。     

ESR谱仪低温杜瓦瓶的研制及其在矿物学研究中的应用

文章介绍了ＥＳＲ谱仪低温杜瓦差的研制原理和方法以及应用它在液氮温度下研究孔雀石中的Ｃｕ＾２＋和天然刚玉中Ｔｉ＾３＋存在形式的实验结果。     

Geochemical characterization of marker tephra layers from major Holocene eruptions,Kamchatka Peninsula,Russia

Kamchatka Peninsula is one of the most active volcanic regions in the world. Many Holocene explosive eruptions have resulted in widespread dispersal of tephra-fall deposits. The largest layers have been mapped and dated by the ¹⁴C method. The tephra provide valuable stratigraphic markers that constrain the age of many geological events (e.g. volcanic eruptions, palaeotsunamis, faulting, and so on). This is the first systematic attempt to use electron microprobe (EMP) analyses of glass to characterize individual tephra deposits in Kamchatka. Eighty-nine glass samples erupted from 11 volcanoes, representing 27 well-identified Holocene key-marker tephra layers, were analysed. The glass is rhyolitic in 21 tephra, dacitic in two, and multimodal in three. Two tephra are mixed with glass compositions ranging from andesite/dacite to rhyolite. Tephra from the 11 eruptive centres are distinguished by their glass K₂O, CaO, and FeO contents. In some cases, individual tephra from volcanoes with multiple eruptions cannot be differentiated. Trace element compositions of 64 representative bulk tephra samples erupted from 10 volcanoes were analysed by instrumental neutron activation analysis (INAA) as a pilot study to further refine the geochemical characteristics; tephra from these volcanoes can be characterized using Cr and Th contents and La/Yb ratios.

Unidentified tephra collected at the islands of Karaginsky (3), Bering (11), and Attu (5) as well as Uka Bay (1) were correlated to known eruptions. Glass compositions and trace element data from bulk tephra samples show that the Karaginsky Island and Uka Bay tephra were all erupted from the Shiveluch volcano. The 11 Bering Island tephra are correlated to Kamchatka eruptions. Five tephra from Attu Island in the Aleutians are tentatively correlated with eruptions from the Avachinsky and Shiveluch volcanoes.     

西天山昭苏东南部阿登套地区大哈拉军山组火山岩及花岗岩侵入体的地球化学特征、时代和构造环境

西天山昭苏东南部阿登套地区大哈拉军山组火山岩主要由玄武质安山岩组成,具有富集大离子亲石元素、亏损高场强元素(如Nb、Ta、Ti)、稀土元素高度分馏的特征。这些玄武安山岩被一些钾长花岗岩和花岗斑岩脉体侵入。钾长花岗岩脉为准铝质,含有较高的Na2O+K2O、轻稀土元素、Zr、Nb、Y含量和较高的FeOT/MgO及Ga/Al比值。两类花岗岩均亏损Ba、Sr、P、Ti和Eu。钾长花岗岩和花岗斑岩给出的Laser-ICPMS锆石U-Pb年龄分别为354.2±2.3Ma和339.5±2.3Ma,表明其围岩即大哈拉军山组火山岩的形成时代不晚于早石炭世早期。综合野外地质观察、区域地质构造以及上述岩石的地球化学特征和时代,我们认为西天山昭苏南部大哈拉军山组火山岩及侵入其中的早石炭世A型花岗岩脉可能形成于活动陆缘弧后拉张环境。     

直进演化抑或分支演化──中国的人类化石证据

和县、巢湖、周口店和金牛山的人类化石表明,直立人有可能延续到0．200MaB．P,智人至少可上溯到0．310MaB．P。考虑到郧县人类化石有可能是代表智人,而不是代表直立人,则智人的历史可提早到蓝田直立人的年代。直立人与智人在生存年代上的重叠,提示了人属成员的演化不是以“直进演化”的形式实现的,如果把直立人和智人看成是两个不同的种的话。