Zircon M257 ‐ a Homogeneous Natural Reference Material for the Ion Microprobe U‐Pb Analysis of Zircon     

Lutz Nasdala  Wolfgang Hofmeister  Nicholas Norberg  James M. Martinson  Fernando Corfu  Wolfgang Dörr  Sandra L. Kamo  Allen K. Kennedy  Andreas Kronz  Peter W. Reiners  Dirk Frei  Jan Kosler  Yusheng Wan  Jens Götze  Tobias Häger  Alfred Kröner  John W. Valley 《Geostandards and Geoanalytical Research》2008,32(3):247-265

We introduce and propose zircon M257 as a future reference material for the determination of zircon U‐Pb ages by means of secondary ion mass spectrometry. This light brownish, flawless, cut gemstone specimen from Sri Lanka weighed 5.14 g (25.7 carats). Zircon M257 has TIMS‐determined, mean isotopic ratios (2s uncertainties) of 0.09100 ± 0.00003 for ²⁰⁶pb/²³⁸U and 0.7392 ± 0.0003 for ²⁰⁷pb/²³⁵U. Its ²⁰⁶pb/²³⁸U age is 561.3 ± 0.3 Ma (unweighted mean, uncertainty quoted at the 95% confidence level); the U‐Pb system is concordant within uncertainty of decay constants. Zircon M257 contains ～ 840 μg g^?1 U (Th/U ～ 0.27). The material exhibits remarkably low heterogeneity, with a virtual absence of any internal textures even in cathodoluminescence images. The uniform, moderate degree of radiation damage (estimated from the expansion of unit‐cell parameters, broadening of Raman spectral parameters and density) corresponds well, within the “Sri Lankan trends”, with actinide concentrations, U‐Pb age, and the calculated alpha fluence of 1.66 × 10¹⁸ g^?1. This, and a (U+Th)/He age of 419 ± 9 Ma (2s), enables us to exclude any unusual thermal history or heat treatment, which could potentially have affected the retention of radiogenic Pb. The oxygen isotope ratio of this zircon is 13.9%o VSMOW suggesting a metamorphic genesis in a marble or calc‐silicate skarn.  相似文献   

Zircon M127 – A Homogeneous Reference Material for SIMS U–Pb Geochronology Combined with Hafnium,Oxygen and,Potentially, Lithium Isotope Analysis          下载免费PDF全文

Lutz Nasdala  Fernando Corfu  John W. Valley  Michael J. Spicuzza  Fu‐Yuan Wu  Qiu‐Li Li  Yue‐Heng Yang  Chris Fisher  Carsten Münker  Allen K. Kennedy  Peter W. Reiners  Andreas Kronz  Michael Wiedenbeck  Richard Wirth  Chutimun Chanmuang  Manuela Zeug  Tamás Váczi  Nicholas Norberg  Tobias Häger  Alfred Kröner  Wolfgang Hofmeister 《Geostandards and Geoanalytical Research》2016,40(4):457-475

In this article, we document a detailed analytical characterisation of zircon M127, a homogeneous 12.7 carat gemstone from Ratnapura, Sri Lanka. Zircon M127 has TIMS‐determined mean U–Pb radiogenic isotopic ratios of 0.084743 ± 0.000027 for ²⁰⁶Pb/²³⁸U and 0.67676 ± 0.00023 for ²⁰⁷Pb/²³⁵U (weighted means, 2s uncertainties). Its ²⁰⁶Pb/²³⁸U age of 524.36 ± 0.16 Ma (95% confidence uncertainty) is concordant within the uncertainties of decay constants. The δ¹⁸O value (determined by laser fluorination) is 8.26 ± 0.06‰ VSMOW (2s), and the mean ¹⁷⁶Hf/¹⁷⁷Hf ratio (determined by solution ICP‐MS) is 0.282396 ± 0.000004 (2s). The SIMS‐determined δ⁷Li value is ?0.6 ± 0.9‰ (2s), with a mean mass fraction of 1.0 ± 0.1 μg g^?1 Li (2s). Zircon M127 contains ~ 923 μg g^?1 U. The moderate degree of radiation damage corresponds well with the time‐integrated self‐irradiation dose of 1.82 × 10¹⁸ alpha events per gram. This observation, and the (U–Th)/He age of 426 ± 7 Ma (2s), which is typical of unheated Sri Lankan zircon, enable us to exclude any thermal treatment. Zircon M127 is proposed as a reference material for the determination of zircon U–Pb ages by means of SIMS in combination with hafnium and stable isotope (oxygen and potentially also lithium) determination.  相似文献   

An Acetic Acid‐Based Extraction Protocol for the Recovery of U,Th and Pb from Calcium Carbonates for U‐(Th)‐Pb Geochronology     

Andrew J. Mason  Gideon M. Henderson  Anton Vaks 《Geostandards and Geoanalytical Research》2013,37(3):261-275

A new method for the simultaneous recovery of U, Th and Pb from ca. 0.5 g calcium carbonate samples for the purpose of U‐(Th)‐Pb geochronometry is presented. The protocol employs ion‐exchange chromatography. Standard anion exchange resin (AG 1‐X8 100–200 mesh) was used as the static phase, and 90% acetic acid was used as the mobile phase to elute the unwanted matrix components; dilute nitric acid was used to elute the U, Th and Pb. Blanks of 1.8 pg Th, 6.4 pg Pb and 8.4 pg U were obtained. The protocol was evaluated by determining the isotopic composition of U‐Th‐Pb separates obtained from an in‐house reference material (prepared from a natural speleothem) by MC‐ICP‐MS. An independently dated speleothem was also reanalysed. Based on these tests, the extraction protocol had an acceptable blank and produced a Pb separate sufficiently free of matrix‐induced instrumental biases to be appropriate for U‐Th‐Pb chronology.  相似文献   

Middle Miocene peralkaline ignimbrites in the Hermosillo region (Sonora, Mexico): Geodynamic implications     

Jesús Vidal Solano  Francisco A. Paz Moreno  Alexander Iriondo  Alain Demant  Jean-Jacques Cochem 《Comptes Rendus Geoscience》2005,337(16):314

Scattered ignimbritic mesas crop out in the Hermosillo region (Sonora, Mexico). These rocks that have been dated at 12.5 Ma (Middle Miocene) have the petrography and chemical characteristics of comendites. Such a flare-up of peralkaline acidic volcanism, after a long period of subduction-related arc volcanism, emphasises an important change in the source of volcanism. It corresponds to the latest stage of continental extension prior to the marine invasion and the development of spreading centres in the Gulf of California. To cite this article: J. Vidal Solano et al., C. R. Geoscience 337 (2005).  相似文献   

Dating Micrometre‐Thin Rims Using a LA‐ICP‐MS Depth Profiling Technique on Zircon from an Archaean Metasediment: Comparison with the SIMS Depth Profiling Method     

Colter J. Kelly  Christopher R.M. McFarlane  David A. Schneider  Simon E. Jackson 《Geostandards and Geoanalytical Research》2014,38(4):389-407

Laser ablation‐inductively coupled plasma‐mass spectrometry (LA‐ICP‐MS) was examined as a tool for measuring isotopic variation as a function of ablation depth in unpolished zircon from an Archaean metasediment specimen. This technique was able to identify micrometre‐thin (> 3 μm) isotopically distinct mineral domains characterised by ca. 100 Myr younger ²⁰⁷Pb/²⁰⁶Pb ages associated with 2s age uncertainties as low ~ 0.2%, as well as elevated U content relative to grain interiors (up to an order of magnitude). Our calculated drilling rate suggests that each laser pulse excavated depths of ~ 0.06 μm. Ages resolved through the LA‐ICP‐MS methods overlap the 2s uncertainties of ²⁰⁷Pb/²⁰⁶Pb ages measured using SIMS depth profiling on the same zircon population. The rims were further evinced by the detection of relative enrichment (> 3 orders of magnitude) in REE in the outermost micrometres of the same zircon, measured using a different and independent LA‐ICP‐MS depth profiling technique. We propose a LA‐ICP‐MS U–Pb technique capable of quickly identifying and quantifying rims, which are indication of late, yet geologically significant, fluid events that are otherwise undefined.  相似文献   

CAMAM: A Miniature Laser Ablation Ionisation Mass Spectrometer and Microscope‐Camera System for In Situ Investigation of the Composition and Morphology of Extraterrestrial Materials     

Marek Tulej  Andreas Riedo  Maike B. Neuland  Stefan Meyer  Peter Wurz  Nicolas Thomas  Valentine Grimaudo  Pavel Moreno‐García  Peter Broekmann  Anna Neubeck  Magnus Ivarsson 《Geostandards and Geoanalytical Research》2014,38(4):441-466

Performance studies of a microscope‐camera system (MCS) and a laser ablation/ionisation mass spectrometer (LIMS) instrument (referred to here as a laser mass spectrometer or LMS) are presented. These two instruments were designed independently for in situ analysis of solids on planetary surfaces and will be combined to a single miniature instrument suite for in situ chemical and morphological analysis of surface materials on planetary bodies. LMS can perform sensitive chemical (elemental, isotope and molecular) analyses with spatial resolution close to micrometre‐sized grains. It allows for studies with mass resolution (M/ΔM) up to 800 in ablation mode (elemental composition) and up to 1500 in desorption mode (molecular analysis). With an effective dynamic range of at least eight orders of magnitude, sensitive and quantitative measurements can be conducted of almost all elements and isotopes with a concentration larger than a few ppb atoms. Hence, in addition to the major element composition, which is important for the determination of mineralogical constituents of surface materials, trace elements can also be measured to provide information on mineral formation processes. Highly accurate isotope ratio measurements can be used to determine in situ geochronology of sample material and for investigations of various isotope fractionation processes. MCS can conduct optical imagery of mm‐sized objects at several wavelengths with micrometre spatial resolution for the characterisation of morphological surface details and to provide insight into surface mineralogy. Furthermore, MCS can help in the selection of sample surface areas for further mass spectrometric analysis of the chemical composition. Surface auto‐fluorescence measurements and images in polarised light are additional capabilities of the MCS, to identify either fluorescing minerals or organic materials, if present on the analysed surface, for further investigation by LMS. The results obtained by investigations of NIST reference materials, amino acid films and a natural graphite sample embedded in silicate rock are presented to illustrate the performance of the instruments and their potential to deliver chemical information for mineral and organic phases in their geological context.  相似文献   

Preliminary optical and radiocarbon age determinations for Upper Pleistocene alluvial sediments in the southern Anti Atlas Mountains,MoroccoDatation des sédiments alluviaux du Pléistocène supérieur du versant sud de l'Anti-Atlas,Maroc     

Martin Thorp  Peter Glanville  Stephen Stokes  Richard Bailey 《Comptes Rendus Geoscience》2002,334(12):903-908

This paper presents the first results of a ¹⁴C and optical luminescence dating project on extensive alluvial silt formations in the southern Anti Atlas Mountains in southern Morocco. The silts comprise three members: basal silts, an inter-silt fluvial gravel member and a top silt member and are incised by the rivers. Top silt dates are: 11 340–11 940, 12 670–13 130 cal. yr BP, and 10.6±0.7 ka (OSL). OSL dates for the inter-silt gravels are 29.6±2.0 ka and for the bottom silts is 45.0±3.7 ka. The sediments correlate with Soltanian stratigraphies known elsewhere in Morocco. To cite this article: M. Thorp et al., C. R. Geoscience 334 (2002) 903–908.  相似文献   

U‐Th Zircon Dating by Laser Ablation Single Collector Inductively Coupled Plasma‐Mass Spectrometry (LA‐ICP‐MS)          下载免费PDF全文

Marcel Guillong  Jakub T. Sliwinski  Axel Schmitt  Francesca Forni  Olivier Bachmann 《Geostandards and Geoanalytical Research》2016,40(3):377-387

Zircon crystals in the age range of ca. 10–300 ka can be dated by ²³⁰Th/²³⁸U (U‐Th) disequilibrium methods because of the strong fractionation between Th and U during crystallisation of zircon from melts. Laser ablation inductively coupled plasma‐mass spectrometry (LA‐ICP‐MS) analysis of nine commonly used reference zircons (at secular equilibrium) and a synthetic zircon indicates that corrections for abundance sensitivity and dizirconium trioxide molecular ions (Zr₂O₃⁺) are critical for reliable determination of ²³⁰Th abundances in zircon. When corrected for abundance sensitivity and interferences, mean activity ratios of (²³⁰Th)/(²³⁸U) for nine reference zircons analysed on five different days averaged 0.995 ± 0.023 (95% confidence weighted by data‐point uncertainty only, MSWD = 1.6; n = 9), consistent with their U‐Pb ages > 4 Ma that imply equilibrium for all intermediate daughter isotopes (including ²³⁰Th) within the ²³⁸U decay chain. U‐Th zircon ages generated by LA‐ICP‐MS without mitigating (e.g., by high mass resolution) or correcting for abundance sensitivity and molecular interferences on ²³⁰Th are potentially unreliable. To validate the applicability of LA‐ICP‐MS to this dating method, we acquired data from three late Quaternary volcanic units: the 41 ka Campanian Ignimbrite (plutonic clasts), the 161 ka Kos Plateau Tuff (juvenile clasts) and the 12 ka Puy de Dôme trachyte lava (all eruption ages by Ar/Ar, with zircon U‐Th ages being of equal or slightly older). A comparison of the corrected LA‐ICP‐MS results with previously published secondary ion mass spectrometry (SIMS) data for these rocks shows comparable ages with equivalent precision for LA‐ICP‐MS and SIMS, but much shorter analysis durations (~ 2 min vs. ~ 15 min) per spot with LA‐ICP‐MS and much simpler sample preparation. Previously undated zircons from the Yali eruption (Kos‐Nisyros volcanic centre, Greece) were analysed using this method. This yielded a large age spread (~ 45 to > 300 ka), suggesting significant antecryst recycling. The youngest zircon age (~ 45 ± 10 ka) provides a reasonable maximum estimate for the eruption age, in agreement with the previously published age using oxygen isotope stratigraphy (~ 31 ka).  相似文献   

The Potassium‐Argon Laser Experiment (KArLE): In Situ Geochronology for Planetary Robotic Missions     

Barbara A. Cohen  J. Scott Miller  Zheng‐Hua Li  Timothy D. Swindle  Renee A. French 《Geostandards and Geoanalytical Research》2014,38(4):421-439

Geochronology is a fundamental measurement for planetary samples, providing global and solar system context for the conditions prevailing on the planet at the time of major geological events. The potassium (K)‐Argon (Ar) laser experiment (KArLE) will make in situ noble gas geochronology measurements aboard planetary robotic missions such as rovers and landers. Laser‐induced breakdown spectroscopy (LIBS) is used to measure the K abundance in a sample and to release its noble gases; the evolved Ar is measured by mass spectrometry, and relative K content is related to absolute Ar abundance by sample mass, determined by optical measurement of the ablated volume. This approach allows K and Ar to be measured on identical volumes multiple times to create an isochron, which improves the age determination and reveals irregularities in the rock if they exist. The KArLE technique measures a whole‐rock K‐Ar age with 10% uncertainty or better for rocks 2 Ga or older, sufficient to resolve the absolute age of many planetary samples. The LIBS–mass spectrometry approach is attractive because the analytical components have been flight‐proven, do not require further technical development and provide essential measurements (complete elemental abundance, evolved volatile analysis, micro‐imaging) as well as in situ geochronology.  相似文献   

A Critical Evaluation of U–Pb Calibration Schemes Used in SIMS Zircon Geochronology          下载免费PDF全文

Heejin Jeon  Martin J. Whitehouse 《Geostandards and Geoanalytical Research》2015,39(4):443-452

Precision and accuracy in SIMS zircon geochronology strongly depend on the method of determination of the interelement ion ratios (e.g., ²⁰⁶Pb/²³⁸U) from the measured secondary ion ratios (²⁰⁶Pb⁺/²³⁸U⁺). Six possible U–Pb calibrations (Pb/U–UO₂/U, Pb/U–UO/U, Pb/U–UO₂/UO, Pb/UO–UO₂/U, Pb/UO–UO/U, Pb/UO–UO₂/UO) based on simple power law relationships, and Pb/UO₂‐related one‐ and two‐ (a power law) dimensional ones were compared using data acquired on the 91500 zircon reference material from one hundred measurement sessions, to determine the most statistically reliable scheme. Taking advantage of U oxide species (UO and UO₂) over atomic U, due to their similar energy distribution to Pb and higher intensities, the data calibrated with Pb/UO–UO₂/UO showed the smallest mean uncertainties and dispersions, and provided the best‐fit calibration curve consistently. Although it was demonstrated with Temora 2 that the unknown zircon age was not changed significantly by different calibrations, its precision could be improved using the Pb/UO–UO₂/UO calibration in zircon geochronology.  相似文献