thermoluminiscence dating – Science@Bleßberghöhle

Thermoluminiscence Dating of speleothemes

Posted on 24. September 202424. September 2024 by Norbert in Results

Zhang, Junjie; Klose, Jennifer; Scholz, Denis; Marwan, Norbert; Breitenbach, Sebastian F. M.; Katzschmann, Lutz; Kraemer, Dennis; Tsukamoto, Sumiko

Isothermal thermoluminescence dating of speleothem growth – A case study from Bleßberg cave 2, Journal Article

In: Quaternary Geochronology, vol. 85, pp. 101628, 2024.

Abstract | Links | BibTeX

@article{zhang2024,

title = {Isothermal thermoluminescence dating of speleothem growth – A case study from Bleßberg cave 2,},

author = {Junjie Zhang and Jennifer Klose and Denis Scholz and Norbert Marwan and Sebastian F. M. Breitenbach and Lutz Katzschmann and Dennis Kraemer and Sumiko Tsukamoto},

doi = {10.1016/j.quageo.2024.101628},

year  = {2024},

date = {2024-09-21},

urldate = {2024-09-21},

journal = {Quaternary Geochronology},

volume = {85},

pages = {101628},

abstract = {Speleothems are a key archive of past climatic and environmental changes. 230Th/U dating is the most commonly used method to determine speleothem ages. However, incorporation of non-radiogenic thorium may hamper 230Th/U dating, and samples older than 600 ka also remain out-of-reach. Calcite exhibits a thermoluminescence (TL) signal at 280 °C with a high characteristic saturation dose, and provides significant potential to date carbonate samples over several million years. Hitherto, the application of TL dating for calcite has mainly been hindered by two factors: 1) a spurious TL signal occurring in the high temperature range, and 2) non-uniform dose rate due to U-series disequilibrium. Here we test an isothermal TL (ITL) dating method on a speleothem sample from Bleßberg cave 2, Germany. We show that the ITL signal measured at 240 °C can completely remove the 280 °C TL peak with a negligible TL contribution from the higher temperature range, thus reducing the influence from the spurious signal. The time-dependent dose rate variation can be simulated using the initial radioactivity of 238U, 234U, 230Th and their decay constants. We use the 230Th/U dating method to provide precise and accurate radiometric ages documenting that the speleothem grew between 425.5 ± 5.4 and 320.5 ± 9.7 ka. The ITL ages (421 ± 23 to 311 ± 23 ka) of four subsamples from the speleothem are consistent with the 230Th/U ages at isochronous sampling positions, showing the general reliability of the ITL dating method. ITL dating provides a pathway to construct chronologies for palaeoclimate reconstructions for speleothems beyond the range of the 230Th/U-method and for samples that are unsuitable for U-series dating methods.},

keywords = {},

pubstate = {published},

tppubtype = {article}

}

Close

Speleothems are a key archive of past climatic and environmental changes. 230Th/UU/Th-Datierung Die U/Th-Datierung ist eine sehr präzise radiometrische Altersbestimmung auf Basis der Uran-Thorium-Zerfallsreihe. Das Uran zerfällt mit bekannten Halbwertszeiten (245.500 Jahre) zum Tochterelement Thorium. Stalagmiten bauen bei ihrem Wachstum (fast) nur das wasserlösliche Uran ein, während das schlecht bewegliche Thorium zum größten Teil im Boden und Epikarst über der Höhle verbleibt. Das kann man nutzen, um die Zeit zu berechnen, die seit der Ausfällung der untersuchten Karbonatprobe vergangen ist. Moderne massenspektrometrische Verfahren erlauben Altersbestimmungen mit der U/Th-Methode bis zu 700.000 Jahren vor Heute. dating is the most commonly used method to determine speleothem ages. However, incorporation of non-radiogenic thorium may hamper 230Th/U dating, and samples older than 600 kaka BP Mit "ka BP" sind "Tausend Jahre vor 1950" gemeint. Das "BP" steht für "before present", was in der Paläoklima-Wissenschaft als 1950 festgelegt wurde. "11.000 ka BP" bedeuted also 11 Tausend Jahre vor 1950, oder unter Verwendung unseres gewohnten Kalenders: 9050 v. Chr. also remain out-of-reach. Calcite exhibits a thermoluminescence (TL) signal at 280 °C with a high characteristic saturation dose, and provides significant potential to date carbonate samples over several million years. Hitherto, the application of TL dating for calcite has mainly been hindered by two factors: 1) a spurious TL signal occurring in the high temperature range, and 2) non-uniform dose rate due to U-series disequilibrium. Here we test an isothermal TL (ITL) dating method on a speleothem sample from Bleßberg cave 2, Germany. We show that the ITL signal measured at 240 °C can completely remove the 280 °C TL peak with a negligible TL contribution from the higher temperature range, thus reducing the influence from the spurious signal. The time-dependent dose rate variation can be simulated using the initial radioactivity of 238U, 234U, 230Th and their decay constants. We use the 230Th/U dating method to provide precise and accurate radiometric ages documenting that the speleothem grew between 425.5 ± 5.4 and 320.5 ± 9.7 ka. The ITL ages (421 ± 23 to 311 ± 23 ka) of four subsamples from the speleothem are consistent with the 230Th/U ages at isochronous sampling positions, showing the general reliability of the ITL dating method. ITL dating provides a pathway to construct chronologies for palaeoclimate reconstructions for speleothems beyond the range of the 230Th/U-method and for samples that are unsuitable for U-series dating methods.

Close

Zhang, J.; Klose, J.; Sierralta, M.; Tsukamoto, S.; Scholz, D.; Marwan, N.; Breitenbach, S.

Isothermal thermoluminescence (ITL) dating of a speleothem from Bleßberg Cave Presentation

29.06.2023, (17th International Luminescence and Electron Spin Resonance Dating conference (LED2023), Copenhagen (Denmark)).

Abstract | BibTeX

@misc{zhang2023,

title = {Isothermal thermoluminescence (ITL) dating of a speleothem from Bleßberg Cave},

author = {J. Zhang and J. Klose and M. Sierralta and S. Tsukamoto and D. Scholz and N. Marwan and S. Breitenbach},

editor = {17th International Luminescence and Electron Spin Resonance Dating conference (LED2023), Copenhagen (Denmark)},

year  = {2023},

date = {2023-06-29},

urldate = {2023-06-29},

abstract = {The calcite thermoluminescence (TL) signal (280 °C peak) saturates at much higher doses (saturation dose up to 5000 Gy) compared to quartz and feldspar, which shows great potential to extend the dating limit. However, spurious TL signal occurred at the high temperature range hindered its application. The conventional multiple-aliquot additive-dose (MAAD) protocol used for TL dating applies extrapolation for equivalent dose (De) estimation, which also has large error. Isothermal TL (ITL) dating with the single-aliquot regenerative-dose (SAR) protocol might be a promising way as it reduces the influence of the spurious TL signal, and it applies interpolation to obtain the De. However, this protocol has not been tested on samples with independent age control.



This study tests the ITL SAR dating protocol on a speleothem sample from Bleßberg cave, which has been accurately dated with 230Th/U (ca. 320–425 ka). ITL measurement at 235 °C for 200 °C can remove the 280 °C TL peak completely without TL contribution from higher temperature range. ITL De shows a plateau when the ITL temperature varies between 230 °C and 240 °C. Peak shifting and isothermal annealing tests indicate the 280 °C TL peak has a lifetime of tens of millions years at 10 °C, which is stable enough for the age range of this speleothem sample. The accurate alpha efficiency (α-value) and the U, Th distribution within the sample are measured to estimate the dose rate. The dose rate variation with time due to U-series disequilibrium is corrected for. The ITL ages are compared with the 230Th/U ages to evaluate the performance of the ITL dating protocol.},

note = {17th International Luminescence and Electron Spin Resonance Dating conference (LED2023), Copenhagen (Denmark)},

keywords = {},

pubstate = {published},

tppubtype = {presentation}

}

Close

This study examines the method of isothermal thermoluminescence dating to determine the age of speleothems. Traditional methods for dating cave formations, such as U/ThU/Th-Datierung Die U/Th-Datierung ist eine sehr präzise radiometrische Altersbestimmung auf Basis der Uran-Thorium-Zerfallsreihe. Das Uran zerfällt mit bekannten Halbwertszeiten (245.500 Jahre) zum Tochterelement Thorium. Stalagmiten bauen bei ihrem Wachstum (fast) nur das wasserlösliche Uran ein, während das schlecht bewegliche Thorium zum größten Teil im Boden und Epikarst über der Höhle verbleibt. Das kann man nutzen, um die Zeit zu berechnen, die seit der Ausfällung der untersuchten Karbonatprobe vergangen ist. Moderne massenspektrometrische Verfahren erlauben Altersbestimmungen mit der U/Th-Methode bis zu 700.000 Jahren vor Heute. dating, are challenging for very old samples. At LIAG, the stalagmite BB2-1 was used to investigate how thermoluminescence dating can be adjusted to provide accurate ages. Since light exposure on the stalagmite can affect the dating results, part of the material was removed using a special acid to minimize this effect. Additionally, it was tested how light might still influence the results. The age estimates were compared with U/Th ages measured at the University of Mainz, and they are in good agreement within the margin of error. This study thus demonstrates that thermoluminescence dating can provide reliable age estimates for particularly old speleothems.

Correlation of dating points — Comparison of dating results of BB2-1 using U/Th dating and TL dating

Development and application of alternative dating methods

Posted on 28. April 202124. September 2024 by Norbert in Project

Project Lead

Leibniz Institute for Applied Geophysics Hannover (LIAG) – Section 3: Geochronology

Content

Development and application of dating methods based on luminescence and electron spin resonance (ESRElektronenspinresonanz-Datierung Eine physikalische Datierungsmethode, die darauf beruht, daß die Menge magnetischer Anomalien im Probenmaterial proportional zur Lagerungszeit im Sediment ist.) methods. Using samples from the Blessberg Cave, thermoluminescence (TL) dating of speleothems is being tested, which has the potential to date calcite up to ~2 million years.

Furthermore, it is planned to date cave sediments.

Leibniz Institute for Applied Geophysics Hannover (LIAG) – Section 3: Geochronology

Posted on 12. April 202124. September 2024 by Norbert in Group

The LIAG is a non-university research institute in Hanover, which is concerned with the exploration of the usable subsurface as well as the development of geophysical measurement and evaluation methods. The institute looks back on more than 50 years of experience in geophysical research.

The section Geochronology is specialised in Quaternary geochronology using luminescence and electron spin resonance (ESRElektronenspinresonanz-Datierung Eine physikalische Datierungsmethode, die darauf beruht, daß die Menge magnetischer Anomalien im Probenmaterial proportional zur Lagerungszeit im Sediment ist.) methods. For Blessberg Cave the group is testing thermoluminescence (TL) dating of speleothems, which has a potential to date calcite up to ~2 million years. It is also planned to contribute in dating cave sediments.

Contact

Dr. Sumiko Tsukamoto

Web Site

https://www.leibniz-liag.de

Publications

Zhang, Junjie; Klose, Jennifer; Scholz, Denis; Marwan, Norbert; Breitenbach, Sebastian F. M.; Katzschmann, Lutz; Kraemer, Dennis; Tsukamoto, Sumiko

Isothermal thermoluminescence dating of speleothem growth – A case study from Bleßberg cave 2, Journal Article

In: Quaternary Geochronology, vol. 85, pp. 101628, 2024.

Abstract | Links | BibTeX

@article{zhang2024,

title = {Isothermal thermoluminescence dating of speleothem growth – A case study from Bleßberg cave 2,},

author = {Junjie Zhang and Jennifer Klose and Denis Scholz and Norbert Marwan and Sebastian F. M. Breitenbach and Lutz Katzschmann and Dennis Kraemer and Sumiko Tsukamoto},

doi = {10.1016/j.quageo.2024.101628},

year  = {2024},

date = {2024-09-21},

urldate = {2024-09-21},

journal = {Quaternary Geochronology},

volume = {85},

pages = {101628},

abstract = {Speleothems are a key archive of past climatic and environmental changes. 230Th/U dating is the most commonly used method to determine speleothem ages. However, incorporation of non-radiogenic thorium may hamper 230Th/U dating, and samples older than 600 ka also remain out-of-reach. Calcite exhibits a thermoluminescence (TL) signal at 280 °C with a high characteristic saturation dose, and provides significant potential to date carbonate samples over several million years. Hitherto, the application of TL dating for calcite has mainly been hindered by two factors: 1) a spurious TL signal occurring in the high temperature range, and 2) non-uniform dose rate due to U-series disequilibrium. Here we test an isothermal TL (ITL) dating method on a speleothem sample from Bleßberg cave 2, Germany. We show that the ITL signal measured at 240 °C can completely remove the 280 °C TL peak with a negligible TL contribution from the higher temperature range, thus reducing the influence from the spurious signal. The time-dependent dose rate variation can be simulated using the initial radioactivity of 238U, 234U, 230Th and their decay constants. We use the 230Th/U dating method to provide precise and accurate radiometric ages documenting that the speleothem grew between 425.5 ± 5.4 and 320.5 ± 9.7 ka. The ITL ages (421 ± 23 to 311 ± 23 ka) of four subsamples from the speleothem are consistent with the 230Th/U ages at isochronous sampling positions, showing the general reliability of the ITL dating method. ITL dating provides a pathway to construct chronologies for palaeoclimate reconstructions for speleothems beyond the range of the 230Th/U-method and for samples that are unsuitable for U-series dating methods.},

keywords = {},

pubstate = {published},

tppubtype = {article}

}

Close

Speleothems are a key archive of past climatic and environmental changes. 230Th/UU/Th-Datierung Die U/Th-Datierung ist eine sehr präzise radiometrische Altersbestimmung auf Basis der Uran-Thorium-Zerfallsreihe. Das Uran zerfällt mit bekannten Halbwertszeiten (245.500 Jahre) zum Tochterelement Thorium. Stalagmiten bauen bei ihrem Wachstum (fast) nur das wasserlösliche Uran ein, während das schlecht bewegliche Thorium zum größten Teil im Boden und Epikarst über der Höhle verbleibt. Das kann man nutzen, um die Zeit zu berechnen, die seit der Ausfällung der untersuchten Karbonatprobe vergangen ist. Moderne massenspektrometrische Verfahren erlauben Altersbestimmungen mit der U/Th-Methode bis zu 700.000 Jahren vor Heute. dating is the most commonly used method to determine speleothem ages. However, incorporation of non-radiogenic thorium may hamper 230Th/U dating, and samples older than 600 kaka BP Mit "ka BP" sind "Tausend Jahre vor 1950" gemeint. Das "BP" steht für "before present", was in der Paläoklima-Wissenschaft als 1950 festgelegt wurde. "11.000 ka BP" bedeuted also 11 Tausend Jahre vor 1950, oder unter Verwendung unseres gewohnten Kalenders: 9050 v. Chr. also remain out-of-reach. Calcite exhibits a thermoluminescence (TL) signal at 280 °C with a high characteristic saturation dose, and provides significant potential to date carbonate samples over several million years. Hitherto, the application of TL dating for calcite has mainly been hindered by two factors: 1) a spurious TL signal occurring in the high temperature range, and 2) non-uniform dose rate due to U-series disequilibrium. Here we test an isothermal TL (ITL) dating method on a speleothem sample from Bleßberg cave 2, Germany. We show that the ITL signal measured at 240 °C can completely remove the 280 °C TL peak with a negligible TL contribution from the higher temperature range, thus reducing the influence from the spurious signal. The time-dependent dose rate variation can be simulated using the initial radioactivity of 238U, 234U, 230Th and their decay constants. We use the 230Th/U dating method to provide precise and accurate radiometric ages documenting that the speleothem grew between 425.5 ± 5.4 and 320.5 ± 9.7 ka. The ITL ages (421 ± 23 to 311 ± 23 ka) of four subsamples from the speleothem are consistent with the 230Th/U ages at isochronous sampling positions, showing the general reliability of the ITL dating method. ITL dating provides a pathway to construct chronologies for palaeoclimate reconstructions for speleothems beyond the range of the 230Th/U-method and for samples that are unsuitable for U-series dating methods.

Close

Zhang, J.; Klose, J.; Sierralta, M.; Tsukamoto, S.; Scholz, D.; Marwan, N.; Breitenbach, S.

Isothermal thermoluminescence (ITL) dating of a speleothem from Bleßberg Cave Presentation

29.06.2023, (17th International Luminescence and Electron Spin Resonance Dating conference (LED2023), Copenhagen (Denmark)).

Abstract | BibTeX

@misc{zhang2023,

title = {Isothermal thermoluminescence (ITL) dating of a speleothem from Bleßberg Cave},

author = {J. Zhang and J. Klose and M. Sierralta and S. Tsukamoto and D. Scholz and N. Marwan and S. Breitenbach},

editor = {17th International Luminescence and Electron Spin Resonance Dating conference (LED2023), Copenhagen (Denmark)},

year  = {2023},

date = {2023-06-29},

urldate = {2023-06-29},

abstract = {The calcite thermoluminescence (TL) signal (280 °C peak) saturates at much higher doses (saturation dose up to 5000 Gy) compared to quartz and feldspar, which shows great potential to extend the dating limit. However, spurious TL signal occurred at the high temperature range hindered its application. The conventional multiple-aliquot additive-dose (MAAD) protocol used for TL dating applies extrapolation for equivalent dose (De) estimation, which also has large error. Isothermal TL (ITL) dating with the single-aliquot regenerative-dose (SAR) protocol might be a promising way as it reduces the influence of the spurious TL signal, and it applies interpolation to obtain the De. However, this protocol has not been tested on samples with independent age control.



This study tests the ITL SAR dating protocol on a speleothem sample from Bleßberg cave, which has been accurately dated with 230Th/U (ca. 320–425 ka). ITL measurement at 235 °C for 200 °C can remove the 280 °C TL peak completely without TL contribution from higher temperature range. ITL De shows a plateau when the ITL temperature varies between 230 °C and 240 °C. Peak shifting and isothermal annealing tests indicate the 280 °C TL peak has a lifetime of tens of millions years at 10 °C, which is stable enough for the age range of this speleothem sample. The accurate alpha efficiency (α-value) and the U, Th distribution within the sample are measured to estimate the dose rate. The dose rate variation with time due to U-series disequilibrium is corrected for. The ITL ages are compared with the 230Th/U ages to evaluate the performance of the ITL dating protocol.},

note = {17th International Luminescence and Electron Spin Resonance Dating conference (LED2023), Copenhagen (Denmark)},

keywords = {},

pubstate = {published},

tppubtype = {presentation}

}

Close

Sierralta, Melanie; Katzschmann, Lutz; Nikonow, Wilhelm; Rammlmair, Dieter

Insights in Bleßberg cave: Speleothem chronology and geochemical research Proceedings Article

In: 75. Jahrestagung der Deutsche Geophysikalische Gesellschaft in Hannover, 2015.

Abstract | BibTeX

@inproceedings{sierralta2015,

title = {Insights in Bleßberg cave: Speleothem chronology and geochemical research},

author = {Melanie Sierralta and Lutz Katzschmann and Wilhelm Nikonow and Dieter Rammlmair},

year  = {2015},

date = {2015-03-23},

booktitle = {75. Jahrestagung der Deutsche Geophysikalische Gesellschaft in Hannover},

abstract = {During construction works on the railway network between Ebensfeld and Erfurt a karst cave was found in the Bleßberg tunnel. The so called „Bleßberg Cave“ developed in limestone of the Lower Muschelkalk. The investigations by the Geological Survey of Thuringia (TLUG), the mining agency of Thuringia, and the incorporated society of cave explorer in Thuringia revealed impressing objects (stalagmites, stalactites, sinter, excentriques, cave lake, cave creek), which were partly sampled; furthermore the extent of the cave was measured. The more than 1000 m long cave had no natural entrance. Based on interdisciplinary studies on the sampled material information about the development and age of the cave will be obtained. Speleothem represent an impressive and unique archive for climate and palaeoenvironmental changes. The growth of stalagmites can be linked to warm climate phases of past. In these warm stages, the growth of stalagmites depends on the precipitation and the water supply; thus palaeoenvironmental conditions are preserved. The aim of this study is to decode the environmental condi- tions using high resolution techniques. Selected stalagmites and sinters were radiometrically dated by 230Th/U and analysed for their stable isotopic compositions. Furthermore, micro-energy dispersive X-ray fluorescence analyses were performed to evaluate trace element dis- tribution and identify growth phases of the speleothem. Most elements revealed the layered texture of the specimen while distribution of Al recorded the fractures. Some visibly identified hiatuses could be associated with changes in chemistry (Si, Fe). The determined 230Th/U ages on several speleothem samples range between 6 ka and 360 ka. In combination with high res- olution stable isotope investigation they provide insights into climatic changes from MIS 11 to the Holocene.},

keywords = {},

pubstate = {published},

tppubtype = {inproceedings}

}

Close

During construction works on the railway network between Ebensfeld and Erfurt a karst cave was found in the Bleßberg tunnel. The so called „Bleßberg Cave“ developed in limestone of the Lower Muschelkalk. The investigations by the Geological Survey of Thuringia (TLUG), the mining agency of Thuringia, and the incorporated society of cave explorer in Thuringia revealed impressing objects (stalagmites, stalactites, sinter, excentriques, cave lake, cave creek), which were partly sampled; furthermore the extent of the cave was measured. The more than 1000 m long cave had no natural entrance. Based on interdisciplinary studies on the sampled material information about the development and age of the cave will be obtained. Speleothem represent an impressive and unique archive for climate and palaeoenvironmental changes. The growth of stalagmites can be linked to warm climate phases of past. In these warm stages, the growth of stalagmites depends on the precipitation and the water supply; thus palaeoenvironmental conditions are preserved. The aim of this study is to decode the environmental condi- tions using high resolution techniques. Selected stalagmites and sinters were radiometrically dated by 230Th/U and analysed for their stable isotopic compositions. Furthermore, micro-energy dispersive X-ray fluorescence analyses were performed to evaluate trace element dis- tribution and identify growth phases of the speleothem. Most elements revealed the layered texture of the specimen while distribution of Al recorded the fractures. Some visibly identified hiatuses could be associated with changes in chemistry (Si, Fe). The determined 230Th/U ages on several speleothem samples range between 6 ka and 360 ka. In combination with high res- olution stable isotopeIsotop Chemische Elemente können aus verschieden aufgebauten Atomen gebildet sein. Die Anzahl Protonen im Atomkern ist zwar dabei gleich, aber die Anzahl der Neutronen kann variieren. Man spricht dann von Isotopen, deren Massen kleine, aber messbare Unterschiede aufweisen. Der Atomkern des Sauerstoffs besteht z. B. aus 8 Protonen und in der Regel aus 8 Neutronen. Es gibt aber auch Sauerstoff, dessen Kerne aus 8 Protonen und 9 oder 10 Neutronen bestehen (neben selteneren, instabilen Sauerstoffisotopen). Um das zu kennzeichnen, gibt man zusätzlich zum chemischen Symbol noch die Massenzahl (Summe aus Protonen und Neutronen) an, also 16O, 17O oder 18O. Die unterschiedlichen Isotope verhalten sich zwar chemisch identisch, physikalisch aber - aufgrund ihres unterschiedlichen Gewichtes - leicht unterschiedlich. Damit stellen sie äusserst wertvolle Marker dar, die uns wichtige Hinweise zur Änderung des Klimas, der Umgebungsvegetation, Bodenaktivität und vielem mehr geben. investigation they provide insights into climatic changes from MISMIS "MIS" ist die Abkürzung für "marine isotope stage", übersetzt also "Isotopenstadium mariner Sedimente". Da sich beim Wechsel von Warm- zu Kaltzeiten (und umgekehrt) die Isotopenverhältnisse in den Kalkschalen kleiner Einzeller (Foraminiferen) auf dem Meeresboden ändern, werden diese zur Datierung herangezogen und lassen sich zur Eingruppierung verschiedener Klimazustände in der Vergangenheit nutzen. Die MIS werden rückwärts nummeriert (also größere Zahl = älter) und ungerade Zahlen stehen für Warmzeiten, gerade für Kaltzeiten. 11 to the Holocene.

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