Trace element composition, texture, cathodoluminescence, Raman scattering, LA–ICP–MS U–Pb dating, and Lu–Hf isotopic composition of zircon Bai-1-2023 from sands of the Peschanaya Bay complex of Lake Baikal as a potential Early Proterozoic age standard
https://doi.org/10.24930/2500-302X-2026-26-1-81-99
EDN: KPCDNL
Abstract
The search for and substantiation of geochronological standards, as well as their interlaboratory testing, are current tasks in the field of analytical geochemistry. Zircon Bai-1-2023 from the sands of the bays of Lake Baikal (“Peschanaya Bay”), a product of the destruction of rapakivi granites of the Primorsky Complex of the Western Cis-Baikal region, has been proposed by the Institute of the Earth’s Crust SB RAS as a U–Pb geochronological standard. Results. This paper presents the results of an interlaboratory, “blind” U–Pb and Lu–Hf isotope study of more than 100 Bai-1-2023 zircon grains. Grain composition, texture, and homogeneity were analyzed by the methods of microprobe and LA–ICP–MS analysis, local Raman and cathodoluminescence spectroscopy. The results were compared with those obtained for international reference materials of zircon Mud Tank, 91500, Temora-2, GJ–1, and Plesovice. For 25 grains (37 LA–ICP– MS determination rounds), two statistically isolated, concordant age populations of 1871 ± 8.1 and 1781 ± 5.7 Ma were identified; for most points, the discordance parameter for 207Pb/206Pb and 206Pb/238U ages was less than 5–6%; for single ones – 10–17%. One population showed an age close to IR-TIMS dating (1859 ± 16 and 1853.6 ± 6.5 Ma). The presence of two populations is not accompanied by clearly distinguishable changes in the composition of zircon grains and their texture, cores, shells, and cracks. LA–ICP–MS data were obtained for 176Hf/177Hf and 176Lu/177Hf isotope ratios. The parameter εHf(t) and the model age of the source TDM were calculated as follows εHf(t)= –13.7 ÷ –6.5 and TDM = 2.5– 2.7 Ga. For zircon grains, significant variations in the position of the vibrational mode ν3(SiO4) (1003.4– 1006.6 cm-1) and its width FWHM (4.8–9.8 cm-1), as well as the values of accumulated autoradiation and equivalent doses – (0.64–2.47) and (0.20– 0.52)·1018 α-decay/g, respectively, were established. Bai-1-2023 zircon was shown to correspond to II–III stages of the mineral disorder. Cathodoluminescence brightness of zircon grains varied by more than an order of magnitude. In the spectra, a number of broad bands Ai, Bi, Ci in the near UV, blue–green, and yellow regions were distinguished. The position of points for Bai-1-2023 zircon on the triple Ai–Bi–Ci discrimination diagram was analyzed. Spectroscopic properties of Bai-1-2023 zircon and the degree of its radiation damage were shown to overlap the properties of the reference materials 91500 → Temora-2→ GJ–1 → Plesovice. Conclusions. Zircon Bai-1-2023 can be recommended as a secondary age reference material for verifying the accuracy of LA–ICP–MS analysis.
About the Authors
S. L. VotyakovRussian Federation
Sergey L. Votyakov
15 Academician Vonsovsky st., Ekaterinburg 620110
M. V. Chervyakovskaya
Russian Federation
Maria V. Chervyakovskaya
15 Academician Vonsovsky st., Ekaterinburg 620110
V. S. Chervyakovskiy
Russian Federation
Vasiliy S. Chervyakovskiy
15 Academician Vonsovsky st., Ekaterinburg 620110
E. A. Pankrushina
Russian Federation
Elizaveta A. Pankrushina
15 Academician Vonsovsky st., Ekaterinburg 620110
V. A. Bulatov
Russian Federation
Vladislav A. Bulatov
15 Academician Vonsovsky st., Ekaterinburg 620110
N. S. Chebykin
Russian Federation
Nikolai S. Chebykin
15 Academician Vonsovsky st., Ekaterinburg 620110
D. A. Mandrygina
Russian Federation
Daria A. Mandrygina
15 Academician Vonsovsky st., Ekaterinburg 620110
A. V. Ivanov
Russian Federation
Alexei V. Ivanov
128 Lermontov st., Irkutsk 664033
References
1. Andersen, T. (2008) Appendix A3: COMPBCORR – Software for common lead correction of UThAndersen, T. (2008) Appendix A3: ComPbCorr – Software for common lead correction of UTh-Pb analyses that do not report 204Pb. Mineralogical Association of Canada. V. 40: Laser Ablation ICP-MS in the Earth Sciences: Current Practices and Outstanding Issues (Ed. by P. Sylvester). Ottawa, Mineral. Assoc. Can, 312-314. https://doi.org/10.3749/9780921294801.app03
2. Black L.P., Gulson B.L. (1978) The age of the Mud Tank carbonatite, Strangways Range, Northern Territory. J. Aust. Geol. Geophys., 3, 227-232.
3. Chervyakovskaya M.V., Votyakov S.L., Chervyakovskiy V.S. (2021) Study of the Lu/Hf Isotopic Composition of Zircons Using a Neptune Plus Multicollector Inductively Coupled Plasma Mass Spectrometer and an NWR 213 Laser Ablation Attachment. Analitika i kontrol’, 25(3), 212-221. (In Russ.)
4. Corfu F., Hanchar J.M., Hoskin P.W.O., Kinny P. (2003) Atlas of zircon textures. Reviews in Mineralogy and Geochemistry. V. 53: Zircon. (Ed. by J.M. Hanchar, P.W.O. Hoskin). Washington, Mineral. Soc. Amer., 469-500. https://doi.org/10.2113/0530469
5. Dawson P., Hargreave M.M., Wilkinson G.R. (1971) The vibrational spectrum of zircon (ZrSiO4). J. Phys. C: Solid State Phys., 4(2), 240-256.
6. Donskaya T.V., Bibikova E.V., Mazukabzov A.M., Kozakov I.K., Gladkochub D.P., Kirnozova T.I., Plotkina Yu.V., Reznitsky L.Z. (2003) Primorsky granitoid complex of the Western Cis-Baikal region: geochronology and geodynamic typification. Geologiya i geofizika, 44(10), 1006-1016. (In Russ.)
7. Giovanardi T., Lugli F. (2017) The Hf-INATOR: A free data reduction spreadsheet for Lu/Hf isotope analysis. Earth Science Informatics, 10(3-4), 517-523. https://doi.org/10.1007/s12145-017-0303-9
8. Horn I., Rudnick R.L., McDonough W.F. (2000) Precise elemental and isotope ratio determination by simultaneous solution nebulization and laser ablation-ICP-MS: application to U-Pb geochronology. Chem. Geol., 164(3-4), 281-301.
9. Inductively coupled plasma mass spectrometry handbook (2005). (Ed. by S.M. Nelms). Oxford, Blackwell Publishing Ltd., 485 р.
10. Ivanov A.V., Bryansky N.V., Efremova U.S., Gladkochub E.A., Karimov A.A., Mikheeva E.A., Demonterova E.I., Dubensky A.S., Erofeeva K.G., Khubanov V.B., Semenova D.V., Karpov A.V., Rodionov N.V., Davydov V.G., Larionov A.N., Votyakov S.L., Chervyakovskaya M.V., Chervyakovsky V.S., Pankrushina E.A., Mandrygina D.A., Kulikova A.V., Minnebaev K.R., Zhang L.-L. (2025) Russian interlaboratory experience of U-Pb local dating of a zircon sample with a known age. Relationships between the Formation Times of Igneous Formations and Ore Deposits in the Metallogenic Provinces of Eurasia. Proceedings of the IX Russian Conference on Isotope Geochronology. Moscow, IGEM RAN, 66-68 p. (In Russ.)
11. Ivanov A.V., Bryansky N.V., Efremova U.S., Gladkochub E.A., Karimov A.A., Demonterova E.I., Mikheeva E.A., Shcherbakov Yu.D., Dubensky A.S., Sheshukov V.S., Yerofeeva K.G., Okina O.I., Hubanov V.B., Semenova D.V., Karpov A.V., Rodionov N.V., Davydov V.G., Larionov A.N., Votyakov S.L., Chervyakovskaya M.V., Chervyakovsky V.S., Pankrushina E.A., Mandrygina D.A., Kulikova A.V., Minnebaev K.R., Zhang L.-L., Kudryashov N.M. (2026) Potential standard BAI-1-2023 of Early Proterozoic zircon for U-Pb dating by local methods. Geodinamika i tektonofizika. In print. (In Russ.)
12. Ivanov A.V., Efremova U.S., Bryansky N.V., Karimov A.A., Mikheeva E.A., Demonterova E.I., Gladkochub E.A., Dubensky A.S., Erofeeva K.G., Khubanov V.B., Semenova D.V., Karpov A.V., Rodionov N.V., Lepekhina E.N., Larionov A.N., Votyakov S.L., Chervyakovskaya M.V., Chervyakovsky V.S., Pankrushina E.A., Bulatov V.A., Chebykin N.S., Mandrygina D.A. (2024) Zircon from Early Proterozoic rapakivi granites of the Primorsky complex, western Baikal region: a potential standard for U-Pb dating by local methods. Minerals: structure, properties, and research methods. Proceedings of the XIV All-Russian Scientific Conference. Yekaterinburg, IGG UrO RAN, 58. (In Russ.)
13. Jackson S.E., Norman J.P., William L.G., Belousova E.A. (2004) The application of laser ablation-inductively coupled plasma-mass spectrometry to in situ U-Pb zircon geochronology. Chem. Geol., 211(1-2), 47-69. https://doi.org/10.1016/j.chemgeo.2004.06.017
14. Kolesov B.A., Geiger C.A., Armbruster T. (2001) The dynamic properties of zircon studied by single-crystal X-ray diffraction and Raman spectroscopy. Europ. J. Mineral., 13(5), 939-948. https://doi.org/10.1127/0935-1221/2001/0013-0939
15. Kooijman E., Berndt J., Mezger K. (2012) U-Pb dating of zircon by laser ablation ICP-MS: recent improvements and new insights. Eur. J. Miner., 24, 5-21.
16. Krasnobaev A.A., Votyakov S.L., Krokhalev V.Ya. (1988) Spectroscopy of zircons (properties, geological applications). Moscow, Nauka Publ., 150 p. (In Russ.)
17. Lloyd G. (1987) Atomic number and crystallographic contrast images with the SEM: a review of backscattered electron techniques. Miner. Mag., 51(359), 3-19.
18. Machado N., Simonetti A. (2001) U-Pb dating and Hf isotopic composition of zircon by laser-ablation-MC-ICP-MS. Laser ablation-ICPMS in the Earth sciences: Principles and applications, 29, 121-146.
19. Marsellos A.E., Garver J.I. (2010) Radiation damage and uranium concentration in zircon as assessed by Raman spectroscopy and neutron irradiation. Amer. Miner., 95, 1192-1201.
20. Messerly J.D. (2008) Current developments in laser ablation-inductively coupled plasma-mass spectrometry for use in geology, forensics, and nuclear nonproliferation research. Thes. Diss. Iowa, 121. https://doi.org/10.2172/964364
21. Murakami T., Chakoumakos B.C., Ewing R.C., Lumpkin G.R., Weber W.J. (1991) Alpha-decay event damage in zircon. Amer. Miner., 76(9-10), 1510-1532.
22. Nasdala L., Smith D.C., Kaindl R., Ziemann M.A. (2004) Raman spectroscopy: Analytical perspectives in mineralogical research. EMU Notes Miner., 6(9), 1-63.
23. Palenik C.S., Nasdala L., Ewing R.C. (2003) Radiation damage in zircon. Amer. Miner., 88(5), 770-781. https://doi.org/10.2138/am-2003-5-606
24. Patent 2022119509. Method for Selecting Reference Samples for External Standardization in LA-ICP-MS Analysis of U-Pb and Lu-Hf Isotopic Composition of Zircon. (Votyakov S.L., Chervyakovskaya M.V., Pankrushina E.A., Shchapova Yu.V., Mikhalevsky G.B.). 14.03.2023. (In Russ.)
25. Patent CN112649492A. Zircon U-Pb rapid dating method of LA-ICP-MS. (Inventors Zhang Wen, Hu Zhaochu, Luo Tao, Feng Yantong Liu Hong). 06.01.2021.
26. Patent СN106908510A; CN106908510B. Method for determining U-Pb age of zircon sample. (Inventors Huang Chao, Liu Jingbo, Xie Liewen, Yang Jinhui, Yang Yueheng). 30.06.2017.
27. Pearson N.J., Griffin W.L., O’Reilly S.Y. (2008) Mass fractionation correction in laser ablation multiple-collector ICP-MS: implications for overlap corrections and precise and accurate in situ isotope ratio measurement. Mineralogical Association of Canada. V. 40: Laser Ablation ICP-MS in the Earth Sciences: Current Practices and Outstanding Issues. (Ed. by P. Sylvester). Ottawa, Mineral. Assoc. Can., 93-116. https://doi.org/10.3749/9780921294801.ch07
28. Pidgeon R.T., Wilde S.A. (1998) The interpretation of complex zircon U-Pb systems in Archaean granitoids and gneisses from the Jack Hills, Narryer Gneiss Terrane, Western Australia. Precamb. Res., 91(3-4), 309-332.
29. Rubatto D. (2017) Zircon: the metamorphic mineral. Rev. Miner. Geochem., 83(1), 261-295. https://doi.org/10.2138/rmg.2017.83.9
30. Shchapova Yu.V., Votyakov S.L., Zamyatin D.A., Chervyakovskaya M.V., Pankrushina E.A. (2020) Minerals Concentrating dand f-Elements: Local Spectroscopic and LA-ICP-MS Studies of Composition, Structure, and Properties, Geochronological Applications. Novosibirsk, SO RAN, 2020. 427 p. (In Russ.)
31. Siebel W., Shang C.K., Thern E., Danisık M., Rohrmuller J. (2012) Zircon response to high-grade metamorphism as revealed by U-Pb and cathodoluminescence studies. Int. J. Earth Sci. (Geol. Rundsch.), 101(8). https://doi.org/10.1007/s00531-012-0772-5
32. Slama J., Kosler J., Condon D.J., Crowley J.L., Gerdes A., Hanchar J.M., Horstwood M.S.A, Morris G.A., Nasdala L., Norberg N., Schaltegger U., Schoene B., Tubrett wM.N., Whitehouse M.J. (2008). Plesovice zircon – a new natural reference material for U-Pb and Hf-isotopic microanalysis. Chem. Geol., 239, 1-35.
33. Steiger R.H., Jäger E. (1977) Subcommission on geochronology: convention on the use of decay constants in geoand cosmochronology. Earth Planet. Sci. Lett. 36(3), 359-362. https://doi.org/10.1016/0012-821X(77)90060-7
34. Syme R.W.G., Lockwood D.J., Kerr H.J. (1977) Raman spectrum of synthetic zircon (ZrSiO4) and thorite (ThSiO)4. J. Phys. C: Solid State Phys., 10(8), 1335. https://doi.org/10.1088/0022-3719/10/8/036
35. Váczi T., Nasdala L. (2016) Electron-beam-induced annealing of natural zircon: a Raman spectroscopic study. Phys. Chem. Miner., 44(6), 389. https://doi.org/10.1007/s00269-016-0866-x
36. Votyakov S.L., Chervyakovskaya M.V., Shchapova Yu.V., Pankrushina E.A., Mikhalevsky G.B., Chervyakovsky V.S. (2022) Cathodoluminescence and Raman spectroscopy as a basis for selecting reference samples in LA-ICP-MS analysis of zircon. Geodinamika i tektonofizika, 13(2), 1-14. (In Russ.)
37. Wiedenbeck M., Hanchar J.M., Peck W.H., Sylvester P., Valley J., Whitehouse M., Franchi I. (2004) Further characterisation of the 91500 zircon crystal. Geostandards Geoanalytical Res., 28(1), 9-39.
Review
For citations:
Votyakov S.L., Chervyakovskaya M.V., Chervyakovskiy V.S., Pankrushina E.A., Bulatov V.A., Chebykin N.S., Mandrygina D.A., Ivanov A.V. Trace element composition, texture, cathodoluminescence, Raman scattering, LA–ICP–MS U–Pb dating, and Lu–Hf isotopic composition of zircon Bai-1-2023 from sands of the Peschanaya Bay complex of Lake Baikal as a potential Early Proterozoic age standard. LITHOSPHERE (Russia). 2026;26(1):81-99. (In Russ.) https://doi.org/10.24930/2500-302X-2026-26-1-81-99. EDN: KPCDNL
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