Simultaneous in-situ determination of U-Pb age and trace elements in zircon by LA-ICP-MS in 20 μm spot size

Simultaneous in-situ determination of U-Pb ages and 20 trace elements of three international zircon standards （91500, GJ1 and TEMORA 1） and one laboratory zircon standard （SK10-2） separated from Cenozoic fine-grained gabbro was carried out on quadrupole ICP-MS equipped with 193 nm excimer laser in 20 μm spot size. The weighted mean ^206Pb/^238U ages of 91500, GJ1 and TEMORA 1 are 1064.4±4.8 Ma （2σ）, 603.2±2.4 Ma （2σ） and 418.2±2.4 Ma （2σ）, respectively. The relative standard deviations （RSDs） of ^206Pb/^238U ages （2σ） are less than 2.2% for single measurements and 0.6% for weighted means. The obtained weighted mean ^206Pb/^238U ages of three standard zircons agree with the recommended values within 2σrerror. The weighted mean ^206Pb/^238U age of SK10-2 is 31.42=0.25 Ma （2σ） and the RSDs of ^206Pb/^238U ages （2σ） are between 2.4% and 5.7% for single measurements and less than 0.8% for weighted mean. The obtained weighted mean ^206Pb/^238U age is in good agreement with the age obtained by Yuan （2004）. Trace element concentrations of NIST612 and NIST614 obtained under the same LA-ICP-MS operating conditions agree with the recommended values within analytical error. The results indicate that it is possible to measure U-Pb age and trace elements simultaneously by LA-ICP-MS in a small spot size of 20μm.     

陕南铜厂闪长岩体的成岩、成矿时代及其地质意义

铜厂闪长岩体位于扬子地台北缘勉县-略阳-阳平关三角地块区域内, 主要由闪长岩、石英闪长岩和花岗闪长岩组成。LA-ICPMS 和 SHRIMP 锆石U-Pb 同位素定年结果表明铜厂闪长岩体存在 3 个侵位结晶阶段: 早期阶段的闪长岩形成于 879 ±7 Ma; 中期阶段的石英闪长岩形成于 848±5 ～840±7 Ma, 含矿钠长岩脉于 834±7 Ma侵位结晶, 与中期阶段石英闪长岩侵位时代在误差范围内一致; 晚期阶段花岗闪长岩形成于 824±5 Ma。这些新的年代学数据表明铜厂闪长岩体及其相伴生的大型铜厂铜矿形成于晋宁期, 而不是古生代, 揭示了扬子地台北缘存在重要的新元古代早期岩浆活动, 与 Rodinia 超大陆的裂解事件在时间上( 860 ～750 Ma) 基本一致, 是Rodinia 超大陆事件在扬子地台北缘的重要响应。     

广西大宁岩体和初洞岩体锆石U-Pb年代学 及Hf同位素研究

利用锆石LA-ICP-MS U-Pb定年,获得大宁岩体形成年龄为441.1±3.0 Ma,其包体年龄为439.5±3.6 Ma,初洞岩体形成年龄为423.5~434.2 Ma。结果表明,大宁岩体及其包体几乎同期形成,而初洞岩体是后期的侵入体。Lu-Hf同位素研究结果表明,大宁岩体及其暗色包体与初洞岩体具有相似的Hf同位素组成,在εHf(t)-年龄图上落在1440~1960 Ma的老地壳区间,表明三者的岩浆源区均是早元古代到中元古代地壳,暗色包体是岩浆早期分离结晶的产物,而初洞岩体是岩浆结晶分异晚期的产物。     

西藏洞中拉铅锌矿床石英斑岩锆石U-Pb年代学研究

探讨西藏洞中拉铅锌矿区的石英斑岩岩体归属.通过详细的地质填图,并采用LAICPMS锆石U-Pb法年龄测定技术,对石英斑岩进行年代学研究.通过石英斑岩样品中单颗粒锆石22个样品点的分析,得到其206 Pb/238U的加权平均年龄为126.9±1.1 Ma,MSWD=0.96.这一结果否认了这套岩石单元属于始新世林子宗群帕...     

Reappraisement and refinement of zircon U-Pb isotope and trace element analyses by LA-ICP-MS

A protocol was established for simultaneous measurements of zircon U-Pb ages and trace elements by LA-ICP-MS at spot sizes of 16 32 μm.This was accomplished by introducing N 2 into ICP to increase the sensitivity.The obtained U-Pb ages for zircon standards GJ-1,TEMORA and SK10-2 are consistent with the preferred values within about 1% uncertainty (2σ) by simple external calibration against zircon standard 91500.Different data reduction softwares could yield different uncertainties for calculation of U-Pb ag...     

Zircon LA-ICPMS study and petrogenesis simulation of Dahuabei pluton in the Wulashan area,Inner Mongolia

Dahuabei pluton in the Wulashan area,Inner Mongolia,is an alkaline and peraluminous granitic pluton.LA-ICPMS U-Pb dating of zircons indicates that this pluton crystallized at 330±10 Myr.The pluton did not experience apparent zircon fractionation.The consistent temperatures between Zr saturation (765℃) and the average zircon-rutile Ti equilibrium (780℃),together with zircon ages and their CL images,indicated that there were no inherited zircons in this pluton.Through the simulation of the dry-system crystallization process of magma cooling at 200 MPa and 1100-709℃,the phase diagram and composition evolution tendency of different phases were obtained.The magma reached its liquidus at 1069℃.Sanidine was the first crystallized phase;at 709℃ the residual magma was less than 4%,and the range of 1069-719℃ should be the most suitable approach to the real condition.It is shown that at least some part of the pluton underwent such isobaric equilibrium crystallization processes during its crystallization.     

藏北羌塘南缘早白垩世青草山强过铝质S型花岗岩的成因: 来自地球化学和锆石U-Pb年代学的约束

藏北羌塘南缘扎普?多不杂岩浆弧内的青草山花岗岩体由花岗斑岩和石英二长斑岩组成, 目前缺乏地球化学和年代学数据来约束其成因和形成时代。用 LA-ICP-MS 方法测得石英二长斑岩锆石 206Pb/238U 年龄加权平均值为122±1 Ma (MSWD=3.9), 花岗斑岩的锆石SHRIMP U-Pb 年龄为114.6±1.2 Ma (MSWD=1.1), 表明岩体形成于早白垩世。岩体含白云母、堇青石, 无角闪石, 具有富铝(A1₂O₃ 含量: 14.81%~15.86%)、贫钙(CaO 含量: 1.10%~2.44%)、总碱含量高(K₂O+Na₂O 含量: 6.86%~8.80%)的特征, 铝饱和指数 A/CNK 为1.06~1.20, 在 CIPW 标准矿物计算中出现刚玉分子(1.20%~2.86%), 未出现透辉石, 表明该岩体为一套强过铝质亚碱性 S 型花岗岩。(La/Yb)N=3.24~16.20, LREE/HREE=4.37~12.4, 在配分曲线上显示左高右低的特征, 富集Rb, Th, U, K, La, Ce 等大离子亲石元素, 亏损Ta, Nb, P, Ti, Y 等高场强元素, 具有较典型的岛弧岩浆岩地球化学特征。研究结果揭示, 青草山花岗岩为班公湖?怒江洋壳北向俯冲背景下, 上地壳杂砂岩质成分发生部分熔融作用的产物。     

Determination of U-Pb age and rare earth element concentrations of zircons from Cenozoic intrusions in northeastern China by laser ablation ICP-MS

Using the in situ zircon U-Pb dating method of LA-ICPMS, we analyzed the 31 Ma old SHRIMP U-Pb age of the Yongsheng nepheline syenite from southern Jilin Province under different spot sizes. The obtained ages are comparable with that of SHRIMP in both accuracy and precision. The age is also identical to that of the Yinmawanshan gabbro from the Liaodong Peninsula within error. Both the Yongsheng nepheline syenite and the Yinmawanshan gabbro represent the youngest known exposed intrusions in northeastern and even eastern China. The results indicate the Eocene mantle-derived magmatic underplating, and the rapid crustal uplifting of this region since 30 Ma. The analyses also document extremely high LREE concentrations and relatively fiat REE patterns for the zircons from the Yongsheng nepheline syenite, which represent a new type of zircon REE pattern.     

吕梁地区宁家湾岩体锆石 U-Pb 年代学、地球化学特征及地质意义

对呈小规模岩株状产出的宁家湾岩体进行野外地质、岩石学、岩石地球化学、锆石U-Pb同位素年代学和Hf同位素组成研究, 目的是确定其岩石成因及地球动力学意义。两件样品的LA-ICP-MS锆石U-Pb定年结果分别为2364±6 Ma (MSWD=0.13)和2360±23 Ma (MSWD =4.0), 属古元古代岩浆活动的产物。研究结果表明, 宁家湾岩体富碱、高K和Si, 具有高FeO^T/MgO 比值和高的高场强元素(HFSE)含量, 富集Rb, Ba, Th和U等元素, 具有低的Ca和Mg含量, 明显亏损P和Ti, 具弱轻重稀土分异和强Eu负异常(δEu=0.13~0.36)的海鸥型稀土分配模式, 显示高分异I型花岗岩的特征。较高的Y/Nb值(1.2~2.8)、锆石的ε_Hf(t)均为正值(+1.6~+6.4)以及单阶段模式年龄t_DM1(Hf)和二阶段模式年龄t_DM2(Hf)分别为2449~2629 Ma和2474~2711 Ma的特点, 表明源区可能为壳幔混合。明显的Nb, P 和 Ti负异常及Ce, Nd和Zr正异常, 反映出大陆边缘弧岩浆岩的特征。结合区域地质背景, 认为宁家湾岩体很可能形成于岛弧构造环境。     

Garnet Sm-Nd and U-Pb systems: A case study of a granulite from the European Variscan belt

This study presents zircon and garnet ages of a mafic granulite from the high-grade Variscan basement of the Black Forest, Germany and discuss isotope closure temperature of garnet Sm-Nd and U-Pb systems. Zircon grains yield 207Pb/206Pb ages between ～340 and ～414 Ma by the U-Pb and evaporation methods. In contract, garnet dating gives Sm-Nd and Pb-Pb isochron ages of (398±3) Ma and (411±14) Ma, respectively, which are older than most of zircon ages. These data imply that most of zircons lost radiogenic Pb, probably due to metamictization or recrystallisation during the granulite-facies metamorphism (～800℃) at ～340 Ma. Garnet Sm-Nd and U-Pb systems preserve chronological information of pro-grade metamorphism, probably profiting from a fluid-absence metamorphic environment. These results demonstrate that garnet mineral can be a better candidate than zircon mineral to date high-grade metamorphism by the U-Pb and Sm-Nd methods in some cases.     

吕梁地区近周营组蚀变火山岩 U-Pb-Hf同位素特征及其地质意义

选择吕梁群中原岔上群北部地层的蚀变火山岩进行锆石U-Pb年代学和Hf同位素研究。锆石U-Pb测试获得两组年龄结果, 较年轻的谐和年龄为1813±6 Ma (n=7), 较老的²⁰⁷Pb/²⁰⁶Pb加权平均年龄为2516±31 Ma(n=2), 前者为火山岩喷发时代, 后者代表捕获锆石年龄。年轻锆石的ε_Hf(t)值为-10.8~-2.3, T_DM1值为2308~2655 Ma; 捕获锆石的ε_Hf(t)值为+10.0~+13.1。年龄约为2.5 Ga锆石的ε_Hf(t)值高于亏损地幔演化线, 考虑到UPb同位素和Hf同位素测点位置不完全相同, 说明所获得的Hf同位素组成为无地质意义的混合数值; 年龄约为1.8 Ga锆石的Hf同位素特征反映其可能源于富集地幔或受地壳物质混染的亏损地幔。结合前人的研究成果, 推断岩浆作用事件发生在约1.81 Ga 的碰撞后阶段。     

华北北缘大青山小井沟岩体年代学、地球化学和Hf同位素特征及其地质意义

为了加深对华北北缘晚古生代构造背景以及古亚洲洋闭合时限的认识, 对华北北缘大青山地区小井沟花岗岩开展了年代学、地球化学和同位素研究。分别利用LA-MC-ICP-MS, ICP-AES和ICP-MS等方法进行锆石U-Pb测年, 主、微量和稀土元素分析以及锆石Hf同位素测试。结果表明, 小井沟岩体侵位于二叠纪, 侵位年龄为275±1 Ma (MSWD=0.93)。该花岗岩具有高硅(SiO₂=70.72%~72.64%)、高钾(K₂O=4.19%~4.23%)的特点, A/CNK均约为1.1, 属于弱过铝质的高钾钙碱性系列, 稀土元素总量(ΣREE)为87.67~101.51 μg/g, 配分曲线呈右倾型, 具有微弱的Eu负异常, 富集大离子亲石元素(LILE, 如Rb, Ba, K, Sr等), 亏损高场强元素(HFSEs, 如Nb, Ta, Y, Yb, Lu等), 应该是由下地壳部分熔融形成。该花岗岩的锆石具有负的ε_Hf(t)值(-9.56~-5.00), 模式年龄(T_DM2)在1.91~1.61 Ga之间, 表明华北陆块古元古代的地壳岩石应该是其主要物源, 可能有幔源物质的参与。结合整个华北北缘二叠纪花岗岩的岩浆演变特征, 小井沟岩体应形成于由俯冲向碰撞-后碰撞转变的过渡时期, 古亚洲洋可能在晚二叠世之前已闭合。     

Hf isotopic compositions of the standard zircons for U-Pb dating

Zircon, a common accessory mineral in various kindsof rocks, is an important subject for U-Pb isotopic dating.With requirements for high spatial resolution with highprecision and accuracy, SHRIMP (Sensitive High Resolu-tion Ion Micro Probe) and LA-ICPMS (Laser AblationInductively Coupled Plasma Mass Spectrometry) nowserve as the important tools in zircon U-Pb dating. Sinceboth methods need standard zircon for external age cali-bration, an ideal standard zircon is critical for obtai…     

In situ simultaneous determination of trace elements, U-Pb and Lu-Hf isotopes in zircon and baddeleyite

This paper describes a combined method of simultaneously measuring U-Pb and Lu-Hf isotopes as well as trace elements in Phalaborwa baddeleyite and 91500, GJ-1, TEMORA-1 and SK10-2 zircons by means of Neptune MC-ICPMS and Agilent Q-ICPMS connected to a 193 nm excimer laser ablation system. Material ablated by laser was carried in different proportions into Q-ICPMS for U-Pb isotopic and trace elemental and MC-ICPMS for Lu-Hf isotopic compositions. Experiments indicate that different proportions of ablated material for the Q-ICPMS and MC-ICPMS （6：4, 5：5 and 4：6 respectively） do not show any bias for the zircon/baddeleyite U-Pb age, Lu-Hf isotope and trace elemental compositions within analytical errors. Using 40-60 μm spot size, the obtained U-Pb ages of Phalaborwa baddeleyite, 91500, GJ-1, TEMORA and SK10-2 zircons are 2065±15 （2σ, n=20）, 1063±6 （2σ, n=-19）, 613±6 （2σ, n=20）, 416±5 （2σ, n=20） and 32.6±0.5 （2σ, n=20） Ma, respectively. The ^176Hf/^177Hf ratios are 0.281231±24 （2SD, n=20）, 0.282310±35 （2SD, n=19）, 0.282028±34 （2SD, n=20）, 0.282687±34 （2SD, n=20） and 0.282752±53 （2SD, n=20）, respectively. The obtained trace elemental compositions are identical to the reference values. Therefore, this kind of technique makes it possible to simultaneously obtain the U-Pb age, Lu-Hf isotopes and trace elemental compositions of zircon and baddeleyite, which could be an important tool in solving problems in earth sciences.     

In situ U-Pb dating of xenotime by laser ablation （LA）-ICP-MS

Xenotime is an ideal mineral for U-Th-Pb isotopic dating because of its relatively high U and Th contents, but typically low concentration of common Pb. These characteristics, and the fact that it is widespread throughout various types of rocks, suggest that the U-Th-Pb dating of xenotime has broad applications. Studies of U-Pb dating on xenotime by ion microprobe (such as SHRIMP) have increased in recent years, whereas studies by laser ablation (LA)-ICP-MS are still rare. In this study, we developed a technique for U-Pb dating of xenotime using the 193 nm ArF laser-ablation system and Agilent 7500a Q-ICP-MS. To evaluate the reliability of our method, a xenotime standard, BS-1, was analyzed and calibrated against another xenotime standard, MG-1. The weighted mean 206 Pb/ 238 U ages of 510.1 ± 5.2 Ma (2 n = 21), 509.8 ± 4.3 Ma (2 n = 21) and 510.0 ± 4.6 Ma (2 n = 21) were obtained using beam diameters of 16, 24 and 32 m, respectively. These ages are identical to those determined by ID-TIMS method (weighted mean 206 Pb/ 238 U age of 508.8 ± 1.4 Ma), which supports the reliability of our LA-ICP-MS method. We also analyzed xenotimes in leucogranites from South Tibet and granites from Xihuashan in southern China, and obtained accurate and precise ages. Nevertheless, we observed systematic differences in Pb/U fractionation among xenotime, monazite and zircon. The matrix-effect resulted in either under-correction or over-correction of fractionation, and thus led to inaccurate ages. Thus, a matrix-matched material is required for U-Pb dating of xenotime by LA-ICP-MS.     

伊春花岗质片麻岩锆石 U-Pb 年代学特征

通过1∶5万朱拉比拉河等图幅区域地质调查工作,在伊春地区发现了新元古代花岗质片麻岩。应用锆石 U-Pb 测龄方法对花岗质片麻岩进行了年代学研究,23个点的206 Pb／238 U表面谐和年龄均在850 Ma 左右,加权平均为850．2±2．1 Ma。该年龄代表花岗质片麻岩体的侵位时间为新元古代;而较新的499 Ma 年龄可能是后期构造事件改造的新生锆石,反映后期构造热事件的年龄;1518 Ma 的年龄应是本次岩浆作用过程中捕获的早期锆石的年龄,该锆石年龄可能代表本区花岗岩的继承性锆石年龄。伊春花岗质片麻岩所在的地区存在前寒武纪的古老微陆块。     

U-Pb zircon dating constraints on formation time of Qilian high-grade metamorphic rock and its tectonic implications

In order to constrain the formation time of high-grade metamorphic rocks in the Qilian Mountains, U-Pb zircon dating was carried out by using LA-ICPMS technique for a paragneiss of the Hualong Group in the Qilian Mountains basement series and a weakly foliated granite that intruds into the Hualong Group. Zircons from the paragneiss consist dominantly of detrital magma zircons with round or sub-round shape. They have 207Pb/206Pb ages mostly ranging from 880 to 900 Ma, with a weighted mean age of 891 ±9 Ma, which is interpreted as the magma crystallization age of its igneous provenance and can be taken as a lower age limit for the Hualong Group. Magma crystallization age for the weak-foliated granite is 875±8 Ma, which can be taken as an upper age limit for the Hualong Group. Accordingly, the formation time of the Hualong Group is constrained at sometime between 875 and 891 Ma. A few zir- cons from both paragneiss and weak-foliated granite display old inherited ages of 1000 to 1700 Ma and young metamorphic ages of Early Paleozoic. The zircon age distribution pattern confirms that the Qilian Mountains and the northern margin of Qaidam Basin had a united basement, with geotectonic affinity to the Yangtze Block. The results also reveal that sediments of the Hualong Group formed by rapid accumulation due to rapid crustal uplift-erosion. This process may result from intensive Neoproterozoic orogenesis due to assembly of the suppercontinent Rodinia.     

内蒙古中部宝力高庙组长英质火山岩U-Pb-Hf同位素特征及其地质意义

锆石SHRIMP U-Pb定年结果显示: 内蒙古中部白音乌拉地区原宝力高庙组的流纹岩形成时代为300.0±2.9 Ma, 属晚石炭世; 青格勒宝拉格地区原宝力高庙组的凝灰岩结晶年龄为159.6±1.4 Ma, 并获得 3颗捕获锆石的年龄分别为291.8±3.4, 304.0±3.3和734.7±9.2 Ma, 应属于晚侏罗世满克头鄂博组。锆石LA-MC-ICP-MS Hf同位素分析显示: 流纹岩锆石ε_Hf(t) 值为+10.5~+12.9, T_DM^C值为493~645 Ma; 凝灰岩岩浆锆石ε_Hf(t)值为+10.1~+13.1, T_DM^C值为369~563 Ma。研究结果表明, 流纹岩源于晚古生代新生地壳的重熔并混入少量老地壳物质, 凝灰岩源于晚古生代地壳的熔融。Hf同位素特征显示晚古生代流纹岩和中生代凝灰岩源于相似的源区, 揭示了晚古生代的一次重要的增生事件, 并且在约160 Ma时期发生过地壳的再造。结合前人的研究成果表明, 兴蒙造山带在约300 Ma时处于古亚洲洋演化过程中岛弧向碰撞后伸展环境的转换时期, 在约160 Ma受到蒙古?鄂霍茨克构造域的影响。     

Indosinian isotope ages of plutons and deposits in southwestern Miaoershan-Yuechengling,northeastern Guangxi and implications on Indosinian mineralization in South China

The Miaoershan-Yuechengling complex pluton is the largest granitoid complex in the western Nanling metallogenic belt with a surface exposure of >3000 km2.The complex pluton is composed of an early stage granitoid batholith and late stage small intrusions.The early stage batholith contains mainly medium-grained porphyritic mica granite and porphyritic monzonite granite,whereas the late stage intrusions are composed of muscovite granite porphyry and muscovite monzonitic granite.There are many W-Sn-Mo-Pb-Zn-Cu ores in the contact zone between the batholith and strata,forming an ore-rich belt around the batholith.Based on zircon LA-ICP-MS U-Pb ages,the southwestern part of the early stage batholith formed at 228.7 ± 4.1 Ma(MSWD = 2.49),with slightly earlier magmatic activity at 243.0 ± 5.8 Ma(MSWD = 2.62).The Yuntoujie muscovite granite was associated with W-Mo mineralization and has a zircon LA-ICP-MS U-Pb age of 216.8 ± 4.9 Ma(MSWD = 1.44).The Re-Os isochron age of molybdenite from the Yuntoujie W-Mo ore was 216.8 ± 7.5 Ma(MSWD = 11.3).Our new isotope data suggest that the late stage intrusive stocks from the southwestern Miaoershan-Yuechengling batholith were closely associated with W-Mo mineralization from the Indosinian period.These new results together with previous isotope data,suggest that South China underwent not only the well-known Yanshanian mineralization event,but also a widespread Indosinian metallogenic event during the Mesozoic period.Therefore,South China has a greater potential for Indosinian mineralization than previously thought such that more attention should be given to the Indosinian ore prospecting in South China.     

辽北新宾?苇子峪地区太古宙花岗质岩石的形成年代、成因及其地质意义

辽北新宾?苇子峪地区的花岗质岩石主要由英云闪长质?奥长花岗质片麻岩和二长花岗岩?正长花岗岩岩体等组成。为确定其形成年代及成因, 对这些花岗质岩石进行锆石U-Pb-Hf同位素和全岩地球化学分析。锆石LA-ICP-MS U-Pb同位素定年结果表明这些花岗质岩石均形成于新太古代, 英云闪长质和奥长花岗质片麻岩的岩浆结晶年龄分别为2588±4 Ma (MSWD=1.3)和2587±6 Ma (MSWD=1.8), 二长花岗岩?正长花岗岩则侵位于2555±4 Ma (MSWD=0.51)。全岩地球化学和锆石Lu-Hf同位素研究表明, 英云闪长质?奥长花岗质片麻岩形成于俯冲板片的部分熔融, 其原始岩浆在上升过程中受到地幔楔岩石的交代; 而二长花岗岩?正长花岗岩中一部分岩浆起源于变质杂砂岩的部分熔融, 其余形成于以变质玄武岩与变质沉积岩为主要成分的混合源区的部分熔融。结合近年的研究成果, 认为新宾?苇子峪地区的新太古代花岗质岩石可能形成于活动大陆边缘的动力学背景。