Skip to main content


Front. Earth Sci., 02 November 2021
Sec. Petrology

New Detrital Zircon Age of the Paleo-Mesoproterozoic Xiong’er Group, Southern North China Craton

  • 1Southern Marine Science and Engineering Guangdong Laboratory (Zhuhai), School of Earth Sciences and Engineering, Sun Yat-sen University, Zhuhai, China
  • 2Guangdong Provincial Key Lab of Geodynamics and Geohazards, School of Earth Sciences and Engineering, Sun Yat-Sen University, Guangzhou, China


The tectonic setting of the southern margin of the North China Craton (NCC) during Paleo-Mesoproterozoic is still under debate (Zhao et al., 2004; He et al., 2009; Zhao et al., 2009; Zhai et al., 2015). One of the controversies regarding this issue is the duration of the Xiong’er volcanism. The Xiong’er Group is mainly composed of basaltic andesite, andesite, dacite, and rhyolite with intercalated siliciclastic rocks. One suggestion is that the Xiong’er volcanism spans a very short period within 1.78–1.75 Ga, typical of an igneous event in a continental rift setting (Zhao et al., 2004; Zhai et al., 2015). By contrast, other researchers consider the duration of the Xiong’er volcanism lasted from ca. 1.78 Ga until 1.45 Ga and suggest a prolonged subduction in the southern NCC during that time (He et al., 2009; Zhao et al., 2009). Here, we present new geochronological data for the interlayered siliciclastic rocks from the Majiahe Formation in the upper Xiong’er Group. Our results show unexpected young zircons at ca. 1400 Ma, possibly suggesting the long-term duration of the Xiong’er volcanism.

Methods and Analytical Process

Sample Preparation

The Paleo-Mesoproterozoic succession in the southern NCC is distributed in three sub-regions, namely, the Song-Ji, Mianchi-Queshan, and Xiaoqinling-Luanchuan areas (Figure 1). In the Mianchi-Queshan area, the Xiong’er Group is thought to be the earliest deposition during the breakup of the supercontinent Nuna/Columbia. Our sample site is located in the Mianchi-Queshan area. The sample NOD-139-1 was collected from a layer intercalated in volcanic rocks of the Majiahe Formation in the upper Xiong’er Group (Figure 1).


FIGURE 1. The distribution of the Xiong’er Group and the sample site.

The tuffaceous siltstone, which is mainly composed of clay matrix, ilmenite, quartz, and plagioclase, was sampled for zircon geochronological analysis. The separation of the zircons was accomplished at the Langfang (Yuneng) Yuheng Mineral and Rock Service Ltd. and is consistent with the guidelines described in Liu et al. (2018). The sample was crushed into 40–100 mesh after removing inclusions and veins. Then, rock powder was elutriated and separated into the light and heavy segments, which the latter segments were processed with the strong magnetic selection. The less magnetic portion was then filtered by the electromagnetic filter, in which the non-magnetic minerals will be detained for the heavy liquid filter. The metal sulfide in the products was further removed by the high-frequency dielectric separator, leaving the portion that contains mostly zircon. Last, the zircons were hand-picked and purified by a binocular microscope.

Two hundred randomly hand-picked zircon grains were mounted in epoxy and polished to approximately half of the average zircon grain thickness. The morphological structure was examined by transmission and reflection light microscopy. The internal structure of zircons was examined using cathodoluminescence (CL) images. Zircon CL images were obtained using an Analytical Scanning Electron Microscope (JSM IT100) connected to a GATAN MINICL system. The imaging condition was 10.0–13.0 kV voltage of electric field and 80–85 µA current of the tungsten filament.

Analytical Process

The zircon U-Pb isotope was analyzed by laser-ablation-inductively coupled plasma-mass spectrometry (LA-ICPMS) using an Agilent 7,500a mass spectrometer equipped with GeoLas 200 M laser-ablation system consisting of ComPex102 (193 nm ArF-excimer laser, Lambda Physik) and an optical system (MicroLas) at the National Key Laboratory of Continental Dynamics in the Northwest University, China. The spot size was 25 μm, and the carrier gas helium was transported into the ablation cell. All the experimental procedures are referred to Liu et al. (2007) and Liu et al. (2018). In this study, the U-Pb isotopic ages and the instrumental mass deviation were calibrated by using the standard zircon 91,500 and GJ-1, respectively. The analysis on the standard reference zircon 91,500 was conducted in every six spots while the GJ-1 was in every twelve spots. The weighted mean ages of the 91,500 and GJ-1 during this process were presented in the supplementary materials (Supplementary Figure S1). The widely used 91,500 reference zircon was dated with the isotope-dilution thermal-ionization (ID-TIMS) 206Pb/238U age of 1,065.4 ± 0.6 Ma (Wiedenbeck et al., 1995). In the National Key Laboratory of Continental Dynamics in the Northwest University, previous studies yielded the LA-ICP-MS 206Pb/238U age of 1,062.2 ± 6.0 Ma (Yuan et al., 2008). In this study, the weighted mean 206Pb/238U age of the 91,500 is 1,062.6 ± 4.2 Ma, within the 2σ error of the ID-TIMS age. The reference zircon GJ-1 was first analyzed with the ID-TIMS 207Pb/206Pb and 206Pb/238U ages at 608.5 ± 0.4 Ma and 599.8 ± 4.5 Ma, respectively (Jackson et al., 2004). The previous study in this laboratory yielded a slightly older 206Pb/238U age of 604.6 ± 2.9 Ma (Yuan et al., 2008). Our analysis yields an intercept age of 607 ± 6.3 Ma and a weighted mean 206Pb/238U age of 608.6 ± 6.9 Ma, respectively (Supplementary Figure S1).

To reduce the probability of missing age components, 84 zircon grains were randomly selected for analysis in this study (Dodson et al., 1988; Fedo et al., 2003). The concentration ratios and the apparent ages were calculated using ICPMSDataCal (Liu et al., 2008; Liu et al., 2010). The common lead calibration was also applied according to Andersen (2002). Detrital zircon age spectra were calculated and presented using ISOPLOT (version 3.23) (Ludwig, 2003) and the DensityPlotter (Vermeesch, 2012).


The 84 spots yield 73 single-grain data that are less than 10% discordant. The external morphology of the zircons is variable from anhedral with a nearly rounded shape to euhedral with a clear pyramid face while most are subhedral. Some of the grains are the fragments of intact ones (e.g., the No.10 gain in Supplementary Figure S2). From the cathodoluminescence intensities, the zircon grains of this sample can be divided into two groups (Supplementary Figure S2). One group with dark and strong CL emission showed homogeneous or patchy internal texture whereas another group with weak to intermediate intensities showed distinct oscillatory zones which indicated the igneous origin (Supplementary Figure S2). Meanwhile, the former group generally yields older age which corresponds with high U content and lower Th/U ratio (Supplementary Figure S2; Supplementary Table). These zircons are possibly from the metamorphic basement or the recycled sedimentary rocks. The zircons with more white color and oscillatory zones show relatively younger ages. The three youngest zircon grains showed distinct euhedral external morphology and blurred internal oscillatory zones (Figure 2). The probability density distribution of the obtained zircon ages shows two prominent peaks at 2,100 Ma and 1850 Ma (Figure 2). The former is possibly sourced from the Taihua (tonalite-trondhjemite-granodiorite) 2000–2,200 Ma TTG assemblages in the southern NCC while the latter is consistent with the ca. 1850 Ma granitic pluton in the central NCC (Huang et al., 2010; Zhao and Zhai, 2013). There are a considerable number of zircon grains that yield ages younger than the previous geochronological reports for the Xiong’er Group, among which the three youngest 206Pb/238U ages are 1,349 ± 32 Ma, 1,478 ± 21 Ma, and 1,646 ± 36 Ma (Figure 2). Our new detrital zircon age report from the Majiahe Formation in the upper Xiong’er Group provides a new constraint on the duration of the Xiong’er volcanism in the southern NCC. According to previous studies, if the Xiong’er volcanism occurred in a short duration from 1.78 Ga to 1.75 Ga, it is impossible to get younger age from the interval of the Xiong’er Group. Therefore, our data in this study contradicted the opinion above whereas supported the model proposed by He et al. (2009) and Zhao et al. (2009), in which the Xiong’er volcanism probably can last to 1,450 Ma or even younger.


FIGURE 2. The cumulative frequency and Concordia diagrams of the zircon age of the sandstone from the Majiahe Formation (NOD-139-1).

Data Availability Statement

The original contributions presented in the study are included in the article/Supplementary Material, and further inquiries can be directed to the corresponding author.

Author Contributions

XL acquired and processed the data, wrote, and drawn the pictures.


This research was financially funded by the National Natural Science Foundation of China (No. 42002207, 42025204, 41772214) and Fundamental Research Funds for the Central Universities (No. 19lgpy71).

Conflict of Interest

The author declares that the research was conducted in the absence of any commercial or financial relationships that could be construed as a potential conflict of interest.

Publisher’s Note

All claims expressed in this article are solely those of the authors and do not necessarily represent those of their affiliated organizations, or those of the publisher, the editors and the reviewers. Any product that may be evaluated in this article, or claim that may be made by its manufacturer, is not guaranteed or endorsed by the publisher.


I am grateful to the two reviewers’ constructive comments which clarify my thoughts on the LA-ICP-MS methodology as well as the logical implication of the dataset.

Supplementary Material

The Supplementary Material for this article can be found online at:


Andersen, T. (2002). Correction of Common Lead in U-Pb Analyses That Do Not Report 204Pb. Chem. Geology. 192, 59–79. doi:10.1016/S0009-2541(02)00195-X

CrossRef Full Text | Google Scholar

Dodson, M. H., Compston, W., Williams, I. S., and Wilson, J. F. (1988). A Search for Ancient Detrital Zircons in Zimbabwean Sediments. J. Geol. Soc. 145 (6), 977–983. doi:10.1144/gsjgs.145.6.0977

CrossRef Full Text | Google Scholar

Fedo, C. M., Sircombe, K. N., and Rainbird, R. H. (2003). Detrital Zircon Analysis of the Sedimentary Record. Rev. Mineralogy Geochem. 53 (1), 277–303. doi:10.2113/0530277

CrossRef Full Text | Google Scholar

He, Y., Zhao, G., Sun, M., and Xia, X. (2009). SHRIMP and LA-ICP-MS Zircon Geochronology of the Xiong'er Volcanic Rocks: Implications for the Paleo-Mesoproterozoic Evolution of the Southern Margin of the North China Craton. Precambrian Res. 168, 213–222. doi:10.1016/j.precamres.2008.09.011

CrossRef Full Text | Google Scholar

Huang, X.-L., Niu, Y., Xu, Y.-G., Yang, Q.-J., and Zhong, J.-W. (2010). Geochemistry of TTG and TTG-like Gneisses From Lushan-Taihua Complex in the Southern North China Craton: Implications for Late Archean Crustal Accretion. Precambrian Res. 182, 43–56. doi:10.1016/j.precamres.2010.06.020

CrossRef Full Text | Google Scholar

Jackson, S. E., Pearson, N. J., Griffin, W. L., and Belousova, E. A. (2004). The Application of Laser Ablation-Inductively Coupled Plasma-Mass Spectrometry to In Situ U-Pb Zircon Geochronology. Chem. Geology. 211, 47–69. doi:10.1016/j.chemgeo.2004.06.017

CrossRef Full Text | Google Scholar

Liu, X., Gao, S., Diwu, C., Yuan, H., and Hu, Z. (2007). Simultaneous In-Situ Determination of U-Pb Age and Trace Elements in Zircon by LA-ICP-MS in 20 μm Spot Size. Chin. Sci Bull. 52, 1257–1264. doi:10.1007/s11434-007-0160-x

CrossRef Full Text | Google Scholar

Liu, X., Li, S., Li, X., Zhao, S., Wang, T., Yu, S., et al. (2018). Detrital Zircon U-Pb Geochronology and Provenance of the Sanxiatian Formation (Huade Group) in the North China Craton: Implications for the Breakup of the Columbia Supercontinent. Precambrian Res. 310, 305–319. doi:10.1016/j.precamres.2018.02.006

CrossRef Full Text | Google Scholar

Liu, Y., Gao, S., Hu, Z., Gao, C., Zong, K., and Wang, D. (2010). Continental and Oceanic Crust Recycling-Induced Melt-Peridotite Interactions in the Trans-North China Orogen: U-Pb Dating, Hf Isotopes and Trace Elements in Zircons from Mantle Xenoliths. J. Petrol. 51, 537–571. doi:10.1093/petrology/egp082

CrossRef Full Text | Google Scholar

Liu, Y., Hu, Z., Gao, S., Günther, D., Xu, J., Gao, C., et al. (2008). In Situ analysis of Major and Trace Elements of Anhydrous Minerals by LA-ICP-MS Without Applying an Internal Standard. Chem. Geology. 257, 34–43. doi:10.1016/j.chemgeo.2008.08.004

CrossRef Full Text | Google Scholar

Ludwig, K. R. (2003). User's Mannual for Isoplot 3.00: A Geochronological Toolkit for Microsoft Excel. Berkeley, CA: Berkeley Geochronology Center.

Google Scholar

Vermeesch, P. (2012). On the Visualisation of Detrital Age Distributions. Chem. Geology. 312-313, 190–194. doi:10.1016/j.chemgeo.2012.04.021

CrossRef Full Text | Google Scholar

Wiedenbeck, M., Allé, P., Corfu, F., Griffin, W. L., Meier, M., Oberli, F., et al. (1995). Three Natural Zircon Standards for U-Th-Pb, Lu-Hf, Trace Element and Ree Analyses. Geostandards Newsl. 19, 1–23. doi:10.1111/j.1751-908X.1995.tb00147.x

CrossRef Full Text | Google Scholar

Yuan, H. L., Gao, S., Dai, M. N., Zong, C. L., Gunther, D., Fontaine, G. H., et al. (2008). Simultaneous Determination of U-Pb Age, Hf Isotopes and Trace Element Composition of Zircon by Excimer Laser-Ablation Quadrupole and Multiple-Collector ICP-MS. Chem. Geology. 247 (1), 100–118. doi:10.1016/j.chemgeo.2007.10.003

CrossRef Full Text | Google Scholar

Zhai, M., Hu, B., Zhao, T., Peng, P., and Meng, Q. (2015). Late Paleoproterozoic-Neoproterozoic Multi-Rifting Events in the North China Craton and Their Geological Significance: A Study advance and Review. Tectonophysics. 662, 153–166. doi:10.1016/j.tecto.2015.01.019

CrossRef Full Text | Google Scholar

Zhao, G., He, Y., and Sun, M. (2009). The Xiong'er Volcanic belt at the Southern Margin of the North China Craton: Petrographic and Geochemical Evidence for its Outboard Position in the Paleo-Mesoproterozoic Columbia Supercontinent. Gondwana Res. 16, 170–181. doi:10.1016/

CrossRef Full Text | Google Scholar

Zhao, G., and Zhai, M. (2013). Lithotectonic Elements of Precambrian Basement in the North China Craton: Review and Tectonic Implications. Gondwana Res. 23, 1207–1240. doi:10.1016/

CrossRef Full Text | Google Scholar

Zhao, T. P., Zhai, M. G., Xia, B., Li, H., Zhang, Y. X., and Wan, Y. S. (2004). The SHRIMP Geochronology on the Zircons of the Xiong'er Volcanics: Constraints on the Initial Time of the Cover for North China Craton. Chin. Sci. Bull. 22, 2342–2349. doi:10.1007/BF03183721

CrossRef Full Text | Google Scholar

Keywords: North China Craton, Xiong’er Group, detrital zircon, mesoproterozoic, geochronological constraints

Citation: Liu X (2021) New Detrital Zircon Age of the Paleo-Mesoproterozoic Xiong’er Group, Southern North China Craton. Front. Earth Sci. 9:732505. doi: 10.3389/feart.2021.732505

Received: 09 July 2021; Accepted: 30 September 2021;
Published: 02 November 2021.

Edited by:

Mei-Fu Zhou, The University of Hong Kong, SAR China

Reviewed by:

Jane Hannah Scarrow, University of Granada, Spain
Justin L, Payne, University of South Australia, Australia

Copyright © 2021 Liu. This is an open-access article distributed under the terms of the Creative Commons Attribution License (CC BY). The use, distribution or reproduction in other forums is permitted, provided the original author(s) and the copyright owner(s) are credited and that the original publication in this journal is cited, in accordance with accepted academic practice. No use, distribution or reproduction is permitted which does not comply with these terms.

*Correspondence: Xiaoguang Liu,