Ar-40/ Ar-39 stepwise crushing technique has become more important for dating hydrothermal fluids trapped in mineralhosted fluid inclusions. However, understanding the gas release patterns and interpreting the Ar-40/ Ar-39 dating results have remained challenging. Here we use Ar-40/ Ar-39 analyses coupled with quadrupole mass spectrometer (QMS) analyses of gases released by stepwise crushing to reconstruct the hydrothermal activities recorded by fluid inclusions hosted by wolframite, cassiterite, and quartz from the Yaogangxian tungsten deposit in South China. Microscopic observations and laser Raman spectroscopic studies reveal two main groups of fluid inclusions hosted in hydrothermal minerals: small, isolated and CH4 rich primary fluid inclusions (PFIs), and larger, mostly CO2 -rich secondary fluid inclusions (SFIs) that distribute along micro-cracks. Formamide and alkane in the vapor phases of large aqueous SFIs are also found. The QMS analyses reveal systematic compositional features for gases released during different crushing stages: (1) gases from the initial crushing stage are H2O-poor, CO2 -rich with CO2/CH4 > 1, likely dominated by gases from large vapor-rich SFIs; (2) gases from the final crushing stage are CH4-dominated gas mixtures with CO2 /CH4 < 1, likely dominated by gases from small PFIs; while (3) gases from the intermediate stage are rich in H2O, formamide, and ethane, which resemble gases from large liquid-rich SFIs. Combined results from microscopic observations, and Raman and QMS analyses suggest that stepwise crushing extracts gases progressively from large vapor-rich SFIs, large aqueous SFIs to small PFIs. Similarly, gases released during each crushing stage have distinct Ar-40/ Ar-39 compositions and corresponding ages. Gases released during the initial crushing stage show high and correlated Ar-40* and and Ar-38(ci) signals with abnormally old( 40)Ar/ Ar-39 ages, which could be related to the vapor-rich SFIs. Gases released during the final crushing stage yield Ar-40/ Ar-39 ages of 159-154 Ma, which agree well with stepwise heating Ar-40/ Ar-39 age (156 +/- 0.9 Ma) of intergrown muscovite and published ore-forming ages. We propose that the Ar-40/ Ar-39 ages of gases released during the final crushing stage are reasonable age estimates for the PFIs. Gases released during the intermediate stage yield Ar-40/Ar- 39 ages of 128-127 Ma, which agree well with stepwise heating Ar-40/Ar- 39 age (129 +/- 2.1 Ma) of the cross-cutting K-feldspar vein. This result likely suggests that intermediate stage gases mainly derived from aqueous SFIs that formed during late-stage hydrothermal events. In this study, we demonstrate that gas release patterns revealed by Ar-40/ Ar-39 epwise crushing are consistent with those revealed by Raman and QMS analyses. Therefore, combining these techniques provides a better picture of the timing and nature of hydrothermal geofluids in general. (C) 2019 Elsevier Ltd. All rights reserved. Publication name | GEOCHIMICA ET COSMOCHIMICA ACTA, 251 36-55; 10.1016/j.gca.2019.02.016 APR 15 2019 | Author(s) | Xiao, Ming; Qiu, Hua-Ning; Jiang, Ying-De; Cai, Yue; Bai, Xiu-Juan; Zhang, Wan-Feng; Liu, Man; Qin, Chao-Jian | Corresponding author(s) | JIANG Yingde jiangyd@gig.ac.cn Chinese Acad Sci, Guangzhou Inst Geochem, State Key Lab Isotope Geochronol & Geochem, Guangzhou 510640, Guangdong, Peoples R China. QIU Huaning huaningqiu@cug.edu.cn China Univ Geosci Wuhan, Key Lab Tecton & Petr Resources, Minist Educ, Wuhan 430074, Hubei, Peoples R China. | Author(s) from IGCAS | QIN Chaojian | View here for the details
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