Articles | Volume 3, issue 1
https://doi.org/10.5194/gchron-3-35-2021
© Author(s) 2021. This work is distributed under
the Creative Commons Attribution 4.0 License.
the Creative Commons Attribution 4.0 License.
Special issue:
https://doi.org/10.5194/gchron-3-35-2021
© Author(s) 2021. This work is distributed under
the Creative Commons Attribution 4.0 License.
the Creative Commons Attribution 4.0 License.
Research article
| 
14 Jan 2021
Research article |
| 14 Jan 2021
| 14 Jan 2021
The use of ASH-15 flowstone as a matrix-matched reference material for laser-ablation U − Pb geochronology of calcite
Geological Survey of Israel, 32 Yeshayahu Leibowitz St., Jerusalem, 9692100, Israel
Jörn-Frederik Wotzlaw
Institute of Geochemistry and Petrology, ETH Zurich, Clausiusstrasse 25, 8092 Zurich, Switzerland
Maria Ovtcharova
Department of Earth Sciences, University of Geneva, Geneva, Switzerland
Anton Vaks
Geological Survey of Israel, 32 Yeshayahu Leibowitz St., Jerusalem, 9692100, Israel
Ciprian Stremtan
Teledyne Photon Machines, 384 Gallatin Park Drive, Bozeman, MT 59715, USA
Martin Šala
Department of Analytical Chemistry, National Institute of Chemistry, Hajdrihova 19, 1000 Ljubljana, Slovenia
Nick M. W. Roberts
Geochronology and Tracers Facility, British Geological Survey, Environmental Science Centre, Nottingham, NG12 5GG, UK
Andrew R. C. Kylander-Clark
Department of Earth Science, University of California, Santa Barbara, CA 93106, USA
Related authors
Bar Elisha, Perach Nuriel, Andrew Kylander-Clark, and Ram Weinberger
Geochronology, 3, 337–349, https://doi.org/10.5194/gchron-3-337-2021, https://doi.org/10.5194/gchron-3-337-2021, 2021
Short summary
Short summary
Distinguishing between different dolomitization processes is challenging yet critical for resolving some of the issues and ambiguities related to the formation of dolomitic rocks. Accurate U–Pb absolute dating of dolomite by LA-ICP-MS could contribute to a better understanding of the dolomitization process by placing syngenetic, early diagenetic, and/or epigenetic events in the proper geological context.
Stuart Umbo, Franziska Lechleitner, Thomas Opel, Sevasti Modestou, Tobias Braun, Anton Vaks, Gideon Henderson, Pete Scott, Alexander Osintzev, Alexandr Kononov, Irina Adrian, Yuri Dublyansky, Alena Giesche, and Sebastian F. M. Breitenbach
Clim. Past, 21, 1533–1551, https://doi.org/10.5194/cp-21-1533-2025, https://doi.org/10.5194/cp-21-1533-2025, 2025
Short summary
Short summary
We use cave rocks to reconstruct northern Siberian climate in 8.68 ± 0.09 Ma. We show that when the global average temperature was about 4.5 °C warmer than today (similar to what is expected in the coming decades should carbon emissions continue unabated), the Siberian Arctic temperature increased by more than 18 °C.
Dawid Szymanowski, Jörn-Frederik Wotzlaw, Maria Ovtcharova, Blair Schoene, Urs Schaltegger, Mark D. Schmitz, Ryan B. Ickert, Cyril Chelle-Michou, Kevin R. Chamberlain, James L. Crowley, Joshua H. F. L. Davies, Michael P. Eddy, Sean P. Gaynor, Alexandra Käßner, Michael T. Mohr, André N. Paul, Jahandar Ramezani, Simon Tapster, Marion Tichomirowa, Albrecht von Quadt, and Corey J. Wall
Geochronology, 7, 409–425, https://doi.org/10.5194/gchron-7-409-2025, https://doi.org/10.5194/gchron-7-409-2025, 2025
Short summary
Short summary
We present the first community-wide evaluation of the reproducibility of U–Pb zircon geochronology by isotope dilution thermal ionisation mass spectrometry (ID-TIMS). Eleven labs analysed aliquots of the same, homogenised, pre-spiked solution of natural zircon, which removed geological bias inherent to using heterogeneous natural zircon grain populations. We discuss remaining sources of inter-lab bias and propose areas of improvement to analytical procedures.
Jade Margerum, Julia Homann, Stuart Umbo, Gernot Nehrke, Thorsten Hoffmann, Anton Vaks, Aleksandr Kononov, Alexander Osintsev, Alena Giesche, Andrew Mason, Franziska A. Lechleitner, Gideon M. Henderson, Ola Kwiecien, and Sebastian F. M. Breitenbach
Clim. Past, 21, 661–677, https://doi.org/10.5194/cp-21-661-2025, https://doi.org/10.5194/cp-21-661-2025, 2025
Short summary
Short summary
We analyse a southern Siberian stalagmite to reconstruct soil respiration, wildfire, and vegetation trends during the Last Interglacial (LIG) (124.1–118.8 ka) and the Holocene (10–0 ka). Wildfires were more prevalent during the LIG than the Holocene and were supported by fire-prone species, low soil respiration, and a greater difference between summer and winter temperature. We show that vegetation type and summer/winter temperature contrast are strong drivers of Siberian wildfires.
Pieter Vermeesch, Noah McLean, Anton Vaks, Tzahi Golan, Sebastian F. M. Breitenbach, and Randall Parris
EGUsphere, https://doi.org/10.5194/egusphere-2025-432, https://doi.org/10.5194/egusphere-2025-432, 2025
Short summary
Short summary
U-Pb dating of cave sediments has provided important new time constraints on the evolution of cave-dwelling organisms (including early humans), and of Earth's climate during the past 5 million years. This paper shows that the most common type of U-Pb dating, which uses 238U and 206Pb, can be inaccurate beyond 2 million years ago. It proposes an alternative type of U-Pb dating, using 235U and 207Pb, as a more accurate alternative.
Sava Markovic, Jörn-Frederik Wotzlaw, Dawid Szymanowski, Joakim Reuteler, Peng Zeng, and Cyril Chelle-Michou
Geochronology, 6, 621–638, https://doi.org/10.5194/gchron-6-621-2024, https://doi.org/10.5194/gchron-6-621-2024, 2024
Short summary
Short summary
We present a pioneering method for high-precision U–Pb dating of individual growth zones in zircon. These micrometer zones in single grains can record key geological processes from magma priming prior to eruptions to planetary formation, yet dating them at high precision has so far been technically challenging. Our method employs two cutting-edge microbeam techniques to microsample these growth zones for high-precision dating, allowing us to tackle a number of outstanding research questions.
Marcel Guillong, Elias Samankassou, Inigo A. Müller, Dawid Szymanowski, Nathan Looser, Lorenzo Tavazzani, Óscar Merino-Tomé, Juan R. Bahamonde, Yannick Buret, and Maria Ovtcharova
Geochronology, 6, 465–474, https://doi.org/10.5194/gchron-6-465-2024, https://doi.org/10.5194/gchron-6-465-2024, 2024
Short summary
Short summary
RA138 is a new reference material for U–Pb dating of carbonate samples via laser ablation inductively coupled plasma mass spectrometry. RA138 exhibits variable U–Pb ratios and consistent U content, resulting in a precise isochron with low uncertainty. Isotope dilution thermal ionization mass spectrometry analyses fix a reference age of 321.99 ± 0.65 Ma. This research advances our ability to date carbonate samples accurately, providing insights into geological processes and historical timelines.
Henning Lorenz, Jan-Erik Rosberg, Christopher Juhlin, Iwona Klonowska, Rodolphe Lescoutre, George Westmeijer, Bjarne S. G. Almqvist, Mark Anderson, Stefan Bertilsson, Mark Dopson, Jens Kallmeyer, Jochem Kück, Oliver Lehnert, Luca Menegon, Christophe Pascal, Simon Rejkjær, and Nick N. W. Roberts
Sci. Dril., 30, 43–57, https://doi.org/10.5194/sd-30-43-2022, https://doi.org/10.5194/sd-30-43-2022, 2022
Short summary
Short summary
The Collisional Orogeny in the Scandinavian Caledonides project provides insights into the deep structure and bedrock of a ca. 400 Ma old major orogen to study deformation processes that are hidden at depth from direct access in modern mountain belts. This paper describes the successful operations at the second site. It provides an overview of the retrieved geological section that differs from the expected and summarises the scientific potential of the accomplished data sets and drill core.
Andrew J. Mason, Anton Vaks, Sebastian F. M. Breitenbach, John N. Hooker, and Gideon M. Henderson
Geochronology, 4, 33–54, https://doi.org/10.5194/gchron-4-33-2022, https://doi.org/10.5194/gchron-4-33-2022, 2022
Short summary
Short summary
A novel technique for the uranium–lead dating of geologically young carbonates is described and tested. The technique expands our ability to date geological events such as fault movements and past climate records.
Pascal Bohleber, Marco Roman, Martin Šala, Barbara Delmonte, Barbara Stenni, and Carlo Barbante
The Cryosphere, 15, 3523–3538, https://doi.org/10.5194/tc-15-3523-2021, https://doi.org/10.5194/tc-15-3523-2021, 2021
Short summary
Short summary
Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) offers micro-destructive, micrometer-scale impurity analysis of ice cores. For improved understanding of the LA-ICP-MS signals, novel 2D impurity imaging is applied to selected glacial and interglacial samples of Antarctic deep ice cores. This allows evaluating the 2D impurity distribution in relation to ice crystal features and assessing implications for investigating highly thinned climate proxy signals in deep polar ice.
Bar Elisha, Perach Nuriel, Andrew Kylander-Clark, and Ram Weinberger
Geochronology, 3, 337–349, https://doi.org/10.5194/gchron-3-337-2021, https://doi.org/10.5194/gchron-3-337-2021, 2021
Short summary
Short summary
Distinguishing between different dolomitization processes is challenging yet critical for resolving some of the issues and ambiguities related to the formation of dolomitic rocks. Accurate U–Pb absolute dating of dolomite by LA-ICP-MS could contribute to a better understanding of the dolomitization process by placing syngenetic, early diagenetic, and/or epigenetic events in the proper geological context.
José Manuel Benítez-Pérez, Pedro Castiñeiras, Juan Gómez-Barreiro, José R. Martínez Catalán, Andrew Kylander-Clark, and Robert Holdsworth
Solid Earth, 11, 2303–2325, https://doi.org/10.5194/se-11-2303-2020, https://doi.org/10.5194/se-11-2303-2020, 2020
Short summary
Short summary
The Sobrado unit represents an allochthonous tectonic slice of exhumed high-grade metamorphic rocks formed during a complex sequence of orogenic processes in the middle to lower crust. We have combined U–Pb geochronology and REE analyses (LASS-ICP-MS) of accessory minerals in migmatitic paragneiss (monazite, zircon) and mylonitic amphibolites (titanite) to constrain the evolution. A Middle Devonian minimum age for HP metamorphism has been obtained.
Andrew R. C. Kylander-Clark
Geochronology, 2, 343–354, https://doi.org/10.5194/gchron-2-343-2020, https://doi.org/10.5194/gchron-2-343-2020, 2020
Short summary
Short summary
This paper serves as a guide to those interested in dating calcite by laser ablation. Within it are theoretical and practical limits of U and Pb concentrations (and U / Pb ratios), which would allow viable extraction of ages from calcite (and other minerals with moderate U / Pb ratios), and which type of instrumentation would be appropriate for any given sample. The method described uses a new detector array, allowing for lower detection limits and thereby expanding the range of viable samples.
Nick M. W. Roberts, Jack K. Lee, Robert E. Holdsworth, Christopher Jeans, Andrew R. Farrant, and Richard Haslam
Solid Earth, 11, 1931–1945, https://doi.org/10.5194/se-11-1931-2020, https://doi.org/10.5194/se-11-1931-2020, 2020
Short summary
Short summary
We characterise a well-known fractured and faulted exposure of Cretaceous chalk in NE England, combining field observations with novel U–Pb calcite dating. We show that the faulting and associated fluid flow occurred during the interval of ca. 64–56 Ma, predating earlier estimates of Alpine-related tectonic inversion. We demonstrate that the main extensional fault zone acted as a conduit linking voluminous fluid flow and linking deeper sedimentary layers with the shallow subsurface.
Cited articles
Anjiang, S., Anping, H., Cheng, T., Liang, F., Wenqing, P., Yuexing, F., and Zhao, J.: Laser ablation in situ U-Pb dating and its application to diagenesis-porosity evolution of carbonate reservoirs, Petroleum Exploration and Development, 46, 1127–1140, 2019.
Black, L. P. and Gulson, B. L.: The age of the Mud Tank carbonatite, Strangways Range, Northern Territory, B.M.R.J. Austral. Geol. Geophys., 3, 227–232, 1978.
Condon, D., Schoene, B., McLean, N., Bowring, S., and Parrish, R.: Metrology and traceability of U–Pb isotope dilution geochronology (EARTHTIME Tracer Calibration Part I), Geoch. Cosmoch. A., 164, 464–480, 2015.
Coogan, L. A., Parrish, R. R., and Roberts, N. M.: Early hydrothermal carbon uptake by the upper oceanic crust: Insight from in situ U-Pb dating, Geology, 44, 147–150, 2016.
Crouvi, O., Amit, R., Enzel, Y., and Gillespie, A. R.: Active sand seas and the formation of desert loess, Quat. Sci. Rev., 29, 2087–2098, 2010.
Elisha, B., Nuriel, P., Kylander-Clark, A., and Weinberger, R.: Towards in-situ U–Pb dating of dolomites, Geochronology Discuss. [preprint], https://doi.org/10.5194/gchron-2020-19, in review, 2020.
Godeau, N., Deschamps, P., Guihou, A., Leonide, P., Tendil, A., Gerdes, A., Hamelin, B., and Girard, J.-P. J. G.: U-Pb dating of calcite cement and diagenetic history in microporous carbonate reservoirs: Case of the Urgonian Limestone, France, Geology, 46, 247–250, 2018.
Goodfellow, B. W., Viola, G., Bingen, B., Nuriel, P., and Kylander-Clark, A. R. C.: Palaeocene faulting in SE Sweden from U–Pb dating of slickenfibre calcite, T. Nova, 29, 321–328, https://doi.org/10.1111/ter.12280, 2017.
Guillong, M., Wotzlaw, J.-F., Looser, N., and Laurent, O.: Evaluating the reliability of U–Pb laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) carbonate geochronology: matrix issues and a potential calcite validation reference material, Geochronology, 2, 155–167, https://doi.org/10.5194/gchron-2-155-2020, 2020.
Hansman, R. J., Albert, R., Gerdes, A., and Ring, U.: Absolute ages of multiple generations of brittle structures by U-Pb dating of calcite, Geology, 46, 207–210, 2018.
Hiess, J., Condon, D. J., McLean, N., and Noble, S. R.: 238U/235U systematics in terrestrial uranium-bearing minerals, Science, 335, 1610–1614, 2012.
Hill, C. A., Polyak, V. J., Asmerom, Y., and Provencio, P.: Constraints on a Late Cretaceous uplift, denudation, and incision of the Grand Canyon region, southwestern Colorado Plateau, USA, from U‐Pb dating of lacustrine limestone, Tectonics, 35, 896–906, 2016.
Hoareau, G., Claverie, F., Pecheyran, C., Paroissin, C., Grignard, P.-A., Motte, G., Chailan, O., and Girard, J.-P.: Direct U-Pb dating of carbonates from micron scale fsLA-ICPMS images using robust regression, Geochronology Discuss. [preprint], https://doi.org/10.5194/gchron-2020-10, in review, 2020.
Holdsworth, R., McCaffrey, K., Dempsey, E., Roberts, N., Hardman, K., Morton, A., Feely, M., Hunt, J., Conway, A., and Robertson, A.: Natural fracture propping and earthquake-induced oil migration in fractured basement reservoirs, Geology, 47, 700–704, 2019.
Horstwood, M. S., Košler, J., Gehrels, G., Jackson, S. E., McLean, N. M., Paton, C., Pearson, N. J., Sircombe, K., Sylvester, P., and Vermeesch, P.: Community-derived standards for LA-ICP-MS U-(Th-) Pb geochronology–Uncertainty propagation, age interpretation and data reporting, Geostand. Geoanal. Res., 40, 311–332, 2016.
Li, Q., Parrish, R., Horstwood, M., and McArthur, J.: U–Pb dating of cements in Mesozoic ammonites, Chem. Geol., 376, 76–83, 2014.
Ludwig, K. R.: Using Isoplot/Ex: Age of Chronological Toolkit for Microsoft Excel, version 1.00, Berkeley Geochronnology Center Special Publication, 1, 1-4, 1998.
MacDonald, J. M., Faithfull, J. W., Roberts, N. M. W., Davies, A. J., Holdsworth, C. M., Newton, M., Williamson, S., Boyce, A., and John, C. M.: Clumped-isotope palaeothermometry and LA-ICP-MS U–Pb dating of lava-pile hydrothermal calcite veins, Contrib. Mineral. Petr., 174, 63, https://doi.org/10.1007/s00410-019-1599-x, 2019.
Mason, A. J., Henderson, G. M., and Vaks, A.: An Acetic Acid-Based Extraction Protocol for the Recovery of U, Th and Pb from Calcium Carbonates for U-(Th)-Pb Geochronology, Geostand. Geoanal. Res., 37, 261–275, https://doi.org/10.1111/j.1751-908X.2013.00219.x, 2013.
Nuriel, P., Weinberger, R., Kylander-Clark, A. R. C., Hacker, B. R., and Craddock, J. P.: The onset of the Dead Sea transform based on calcite age-strain analyses, Geology, 45, 587–590, https://doi.org/10.1130/g38903.1, 2017.
Nuriel, P., Craddock, J., Kylander-Clark, A. R., Uysal, I. T., Karabacak, V., Dirik, R. K., Hacker, B. R., and Weinberger, R. J. G.: Reactivation history of the North Anatolian fault zone based on calcite age-strain analyses, Geology, 47, 465–469, 2019.
Parrish, R. R., Parrish, C. M., and Lasalle, S.: Vein calcite dating reveals Pyrenean orogen as cause of Paleogene deformation in southern England, J. Geol. Soc., https://doi.org/10.1144/jgs2017-107, 2018.
Paton, C., Woodhead, J. D., Hellstrom, J. C., Hergt, J. M., Greig, A., and Maas, R.: Improved laser ablation U‐Pb zircon geochronology through robust downhole fractionation correction. Geochemistry, Geophysics, Geosystems, Geochem. Geophys. Geosyst., 11, Q0AA06, https://doi.org/10.1029/2009GC002618, 2010.
Piccione, G., Rasbury, E. T., Elliott, B. A., Kyle, J. R., Jaret, S. J., Acerbo, A. S., Lanzirotti, A., Northrup, P., Wooton, K., and Parrish, R. R.: Vein fluorite U-Pb dating demonstrates post–6.2 Ma rare-earth element mobilization associated with Rio Grande rifting, Geosphere, 15, 1958–1972, 2019.
Ring, U. and Gerdes, A.: Kinematics of the Alpenrhein-Bodensee graben system in the Central Alps: Oligocene/Miocene transtension due to formation of the Western Alps arc, Tectonics, 35, 1367–1391, 2016.
Roberts, N. M. and Walker, R. J.: U-Pb geochronology of calcite-mineralized faults: Absolute timing of rift-related fault events on the northeast Atlantic margin, Geology, 44, 531–534, 2016.
Roberts, N. M., Rasbury, E. T., Parrish, R. R., Smith, C. J., Horstwood, M. S., and Condon, D. J.: A calcite reference material for LA-ICP-MS U-Pb geochronology, Geochem. Geophy. Geosy., 18, 2807–2814, 2017.
Roberts, N. M. W., Drost, K., Horstwood, M. S. A., Condon, D. J., Chew, D., Drake, H., Milodowski, A. E., McLean, N. M., Smye, A. J., Walker, R. J., Haslam, R., Hodson, K., Imber, J., Beaudoin, N., and Lee, J. K.: Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) U–Pb carbonate geochronology: strategies, progress, and limitations, Geochronology, 2, 33–61, https://doi.org/10.5194/gchron-2-33-2020, 2020.
Schmitz, M. D. and Schoene, B.: Derivation of isotope ratios, errors, and error correlations for U–Pb geochronology using
Vaks, A., Bar-Matthews, M., Matthews, A., Ayalon, A., and Frumkin, A.: Middle-Late Quaternary paleoclimate of northern margins of the Saharan-Arabian Desert: reconstruction from speleothems of Negev Desert, Israel, Quat. Sci. Rev., 29, 2647–2662, 2010.
Vaks, A., Woodhead, J., Bar-Matthews, M., Ayalon, A., Cliff, R. A., Zilberman, T., Matthews, A., and Frumkin, A.: Pliocene–Pleistocene climate of the northern margin of Saharan–Arabian Desert recorded in speleothems from the Negev Desert, Israel, Earth Planet. Sci. Lett., 368, 88–100, https://doi.org/10.1016/j.epsl.2013.02.027, 2013.
Vaks, A., Bar-Matthews, M., Ayalon, A., Matthews, A., and Frumkin, A.: Pliocene–Pleistocene palaeoclimate reconstruction from Ashalim Cave speleothems, Negev Desert, Israel, Geological Society, London, Special Publications, 466, 201–216, 2018.
van Elteren, J. T., Šelih, V. S., Šala, M., Van Malderen, S. J., and Vanhaecke, F.: Imaging artifacts in continuous scanning 2D LA-ICPMS imaging due to nonsynchronization issues, Anal. Chem., 90, 2896–2901, 2018.
van Elteren, J. T., Šelih, V. S., and Šala, M.: Insights into the selection of 2D LA-ICP-MS (multi) elemental mapping conditions, J. Anal. At. Spectr., 34, 1919–1931, 2019.
van Malderen, S.: Optimization of methods based on laser ablation-ICP-mass spectrometry (LA-ICP-MS) for 2-D and 3-D elemental mapping, Doctoral dissertation, Ghent University, Ghent, Belgium, 2017.
Vermeesch, P.: IsoplotR: A free and open toolbox for geochronology, Geosci. Front., 9, 1479–1493, 2018.
von Quadt, A., Wotzlaw, J.-F., Buret, Y., Large, S. J., Peytcheva, I., and Trinquier, A.: High-precision zircon U/Pb geochronology by ID-TIMS using new 1013 ohm resistors, J. Anal. At. Spectr., 31, 658–665, 2016.
Woodhead, J. and Petrus, J.: Exploring the advantages and limitations of in situ U–Pb carbonate geochronology using speleothems, Geochronology, 1, 69–84, https://doi.org/10.5194/gchron-1-69-2019, 2019.
Woodhead, J. D. and Hergt, J. M.: Strontium, neodymium and lead isotope analyses of NIST glass certified reference materials: SRM 610, 612, 614, Geol. Newsl., 25, 261–266, 2001.
Wotzlaw, J.-F., Buret, Y., Large, S. J., Szymanowski, D., and von Quadt, A.: ID-TIMS U–Pb geochronology at the 0.1‰ level using 10 13 Ω resistors and simultaneous U and 18 O/16 O isotope ratio determination for accurate UO 2 interference correction, J. Anal. At. Spect., 32, 579–586, 2017.
Short summary
This contribution presents a new reference material, ASH-15 flowstone with an age of 2.965 ± 0.011 Ma (95 % CI), to be used for in situ U–Pb dating of carbonate material. The new age analyses include the use of the EARTHTIME isotopic tracers and a large number of sub-samples (n = 37) with small aliquots (1–7 mg) each that are more representative of laser-ablation spot analysis. The new results could improve the propagated uncertainties on the final age with a minimal value of 0.4 %.
This contribution presents a new reference material, ASH-15 flowstone with an age of...
Special issue