Journal of Earth Science, Vol. 28, No. 4, p. 578–587, August 2017 ISSN 1674-487X Printed in DOI: 10.1007/s12583-017-0798-5 Invited Article

Typical Oxygen Isotope Profile of Altered Oceanic Crust Recorded in Continental Intraplate Basalts

Huan Chen 1, 2, 3, Qun-Ke Xia *1, Etienne Deloule4, Jannick Ingrin3 1. School of Earth Sciences, Zhejiang University, 310027, China 2. School of Earth and Space Sciences, University of Science and Technology of China, 230026, China 3. UMET, UMR CNRS 8207, Université de Lille1, 59655 Villeneuve d’Ascq, France 4. CRPG, UMR 7358, CNRS Université de Lorraine, 54501 Vandoeuvre-les Nancy, France Huan Chen: http://orcid.org/0000-0003-3524-4163; Qun-Ke Xia: http://orcid.org/0000-0003-1256-7568

ABSTRACT: Recycled oceanic crust (ROC) has long been suggested to be a candidate introducing en- riched geochemical signatures into the mantle source of intraplate basalts. The different parts of oceanic crust are characterized by variable oxygen isotope compositions (δ18O=3.7‰ to 13.6‰). To trace the sig- natures of ROC in the mantle source of intraplate basalts, we measured the δ18O values of clinopyroxene (cpx) phenocrysts in the Cenozoic basalts from the Shuangliao volcanic field, NE China using secondary ion mass spectrometer (SIMS). The δ18O values of the Shuangliao cpx phenocrysts in four basalts ranging from 4.10‰ to 6.73‰ (with average values 5.93‰±0.36‰, 5.95‰±0.30‰, 5.58‰±0.66‰, and 4.55‰± 0.38‰, respectively) apparently exceed those of normal mantle-derived cpx (5.6‰±0.2‰) and fall in the typical oxygen isotope range of altered oceanic crust. The δ18O values display the negative correlations with the Eu, Sr anomalies of whole rocks and erupted ages, demonstrating that (1) the ROC is the main enriched component in the mantle source of the Shuangliao basalts and (2) the contributions of ROC var- ied with time. The basalt with the lowest δ18O value is characterized by a significant K positive anomaly, 18 highest H2O/Ce and Ba/Th ratios, suggesting that the mantle source of basalts with low δ O can also in- clude a water-rich sediment component that may be the trigger for partial melting. Considering the continuous subduction of the Pacific slab, the temporal heterogeneity of the source components is likely to be caused by the Pacific slab subduction. KEY WORDS: continental basalt, oxygen isotope, recycled oceanic crust, Pacific slab, eastern China.

0 INTRODUCTION al., 2012; Huang and Zhao, 2006). Therefore, the recycled The small-volume continental intraplate basalts are widely oceanic crust (ROC) has increasingly been suggested to be one spread in each continent (e.g., eastern China, western Africa, of the major enriched components in their mantle sources western US, western/central Europe, southeastern Australia), and (Chen et al., 2017, 2015a, b; Liu et al., 2015a, b; Wang et al., the genesis of these basalts are hotly debated (Farmer, 2014). 2015; Xu et al., 2012; Kuritani et al., 2011). Especially in eastern China, the continental basalts extend from Oxygen isotope exchanges between oceanic crust and the northernmost to the southernmost, along the continental mar- seawater occurs during hydrothermal alteration (Muehlenbachs gin (Lei et al., 2013), which form an important part of the volcano and Clayton, 1976). Because the temperature of hydrothermal belt of the western circum-Pacific rim (Fig. 1). These basalts are alteration varied from the lower to the upper part of the oceanic characterized by typical ocean island basalt (OIB)-like trace ele- crust, different layers of altered oceanic crust acquired distinct ment patterns and Sr-Nd-Pb isotopic compositions, which indicate oxygen isotope compositions through hydrothermal exchange the presence of enriched components in the mantle sources (e.g., with seawater (Taylor, 1974). The general profile of oxygen Chen et al., 2007; Zhang et al., 2001; Jung and Hoernes, 2000; isotope compositions of altered oceanic crust exhibits δ18O Marzoli et al., 2000; Zou et al., 2000; Rogers et al., 1995; Zhou values higher than the normal mantle in the upper part and δ18O and Armstrong, 1982). Recently, seismic tomography studies have values lower than the normal mantle in the lower part (Fig. 2) revealed the presence of recycled oceanic slab in the Earth’s man- (Gao et al., 2006; Eiler, 2001; Hoffman et al., 1986; Gregory tle (e.g., Liu et al., 2017; Fichtner and Villaseñor, 2015; Wei et and Taylor, 1981). Therefore, oxygen isotope is a powerful tool to trace ROC component in the mantle source of continental *Corresponding author: [email protected] intraplate basalts (e.g., Chen et al., 2017; Liu et al., 2015a, b; © China University of Geosciences and Springer-Verlag Berlin Wang et al., 2015; Kokfelt et al., 2006; Eiler et al., 2000; Putlitz Heidelberg 2017 et al., 2000; Woodhead et al., 1993). The Shuangliao volcanic field is located in the south part Manuscript received May 24, 2017. of NE China, which consists of eight volcanoes. Xu et al. (2012) Manuscript accepted July 19, 2017. and Chen et al. (2015b) conducted detailed geochemical studies

Chen, H., Xia, Q.-K., Deloule, E., et al., 2017. Typical Oxygen Isotope Profile of Altered Oceanic Crust Recorded in Continental Intraplate Basalts. Journal of Earth Science, 28(4): 578–587. doi:10.1007/s12583-017-0798-5. http://en.earth-science.net Typical Oxygen Isotope Profile of Altered Oceanic Crust Recorded in Continental Intraplate Basalts 579

120º 130ºE Cenozoic Marine sediments basalt Russia Pillow basalts 0 450 km Dikes

50ºN

Mongolia -

Tan-Lu fault Mishan fault

N-MORB Songliao Basin DTGL Shuangliao Gabbros NE China Changbaishan fold belts Sea of Japan Whole rock

40º North China 3456789102030 Craton δ18O (‰) (b) Figure 2. Typical oxygen isotope profile of an altered sediment-covered oce- Qinling-Dabie belt anic crust. The blue curve shows the average δ18O values of the altered oceanic Tan-Lu fault crust. The data for the oceanic crust are based on the Samail ophiolite (Taylor, 1974), the δ18O values of marine sediments are from Eiler (2001). Yangtze Craton East China Sea 18

30º Here, we measured the δ O values of the clinopyroxene (cpx) phenocrysts in Cenozoic basalts from the Shuangliao vol- Taibei canic field using secondary ion mass spectrometry (SIMS). The typical oxygen isotope profile of altered oceanic crust in the SE China fold system Shuangliao basalts clearly confirms that the recycled oceanic slab was present in the mantle source. The mass balance calculation South China Sea demonstrates that a water-rich sediment component may also be involved in the mantle source although the basalts display the

20º 18 18 (a) lowest δ O, in contrast with intuitively expected elevated δ O. Combined with the erupted ages, the changing source components 110º 120ºE is likely to be caused by the ongoing Pacific slab subduction. (b) N 1 GEOLOGICAL BACKGROUND AND SAMPLES Northeast China (NE China) lies in the Xing’an-Mongolia orogenic belt (XMOB), which belongs to the east part of the Pa- Xinkai River Songliao BasinChangling leozoic Central Asian orogenic belt (Fig. 1a). It is composed of several minor blocks (e.g., Erguna, Xing’an, Songliao, Jiamusi) Xiaohalabashan amalgamated during subduction and collision among the Siberian Bolishan Dahalabashan Craton, the North China Craton (NCC) and the Pacific Plate (Li, Tongliao Datuerjishan Shitoushan Bobotushan Dongliao 2006; Sengör and Natal’in, 1996; Sengör et al., 1993). The tectonic Xiaotuerjishan Shuangliao Aobaoshan River evolutions of NE China mainly include the closure of the Paleo- Yitong 050 km Asian Ocean, the amalgamation of several minor blocks and the

subduction of the Pacific Plate since Late Mesozoic (Maruyama et Figure 1. (a) Simplified tectonic divisions and the distribution of the Ceno- al., 1997; Sengör and Natal’in, 1996; Sengör et al., 1993). zoic intraplate basalts in eastern China as well as the location of the The Shuangliao volcanic field is located in the southeast of Shuangliao volcanic field (modified from Xu et al., 2012); (b) the distribu- the Songliao Basin, which consists of eight volcanoes: Ao- tion and sample locations (red stars) of the Shuangliao basalts. DTGL. baoshan (ABS), Bobotushan (BBT), Bolishan (BLS), Shitoushan Daxin’anling-Taihangshan Gravity Lineament. (STS), Dahalabashan (DHLB), Xiaohalabashan (XHLB), Da- tuerjishan (DTEJ) and Xiaotuerjishan (XTEJ) (Fig. 1b). Seismic including Ar-Ar erupted ages, major and trace elements, tomography has shown the presence of a stagnant subducted Sr-Nd-Pb isotopes and H2O content on these basalts. The Pacific slab in the mantle transition zone beneath the Shuangliao Shuangliao basalts are characterized by high Fe2O3, HIMU volcanic field (Liu et al., 2017; Wei et al., 2012; Huang and Zhao, (high µ)-type trace element patterns and significant correlations 2006). The Shuangliao basalts vary from basanite, alkaline oli- between Ba/Th, Ce/Pb and H2O/Ce ratios, which suggested that vine basalt, and transitional basalts to dolerites (Chen et al., the recycled oceanic slab component may be involved in the 2015b; Xu et al., 2012). Abundant peridotite xenoliths were car- mantle source and the contributions of these source components ried out by the eruption of these volcanoes (Yu et al., 2009). The changed with time. Hence, this area is an appropriate place to Ar-Ar dating results have shown that all volcanoes erupted be- trace oxygen isotopic signatures of ROC in continental basalts. tween 51.0 and 41.6 Ma (Xu et al., 2012). Volcanic cones with

580 Huan Chen, Qun-Ke Xia, Etienne Deloule and Jannick Ingrin high alkalinity erupted between 51 and 48.5 Ma, while transi- 2010; Valley and Kita, 2009; Eiler et al., 1997). tional or subalkaline cones erupted between 43.0 and 41.6 Ma, For the deviation caused by transport and detection proc- indicating that the alkalinity of the Shuangliao volcanic rocks esses, the fractionation factor (δ18O*) could be calculated from 18 decreased with time (Xu et al., 2012). the measured value of NSH9 (δ Oraw) and the “true” value 18 Our samples were collected from BBT, BLS, DHLB and (δ Otrue), using the following equation (Kita et al., 2009) XTEJ (red stars in Fig. 1b). According to Chen et al. (2015b) and δ18O*=bias =δ18ONSH9 –δ18ONSH9 (1) Xu et al. (2012), these rocks can be classified into three types: (1) (raw) (true) basanite (BBT and BLS), alkali olivine basalt (DHLB) and tran- For sessions with a linearly time-dependent bias drift, a sitional basalt (XTEJ). The basanites from BBT and BLS contain linear correlation between this bias and time is used to correct. 20% of olivine (ol) and cpx phenocrysts. Meanwhile, in alkali For the deviation caused by the mineral type and composi- olivine basalts and transitional basalts, the phenocrysts are com- tion during production of secondary ions (matrix effect), the posed of olivine, clinopyroxene and plagioclase (pl). The mantle correlation between the relative IMF and the Mg# of a group of xenoliths are mainly spinel lherzolites with minor spinel harzbur- cpx standards was estimated (Fig. 3; Gurenko et al., 2001). A gites. The Ar-Ar plateau ages of BBT, BLS, DHLB and XTEJ linear function correlation between IMF and cpx’s Mg# for each basalt are 50.1±0.8, 49.7±0.2, 51.0±0.5, and 43.0±0.4 Ma, re- session was obtained spectively (Xu et al., 2012). IMF  f (Mg# )  A Mg#  B (2)

2 ANALYTICAL METHODS where A and B are the parameters in the linear regression. The 2.1 In-Situ Oxygen Isotope Measurement bias caused by the matrix effect between the unknown samples In-situ oxygen isotope measurement of cpx phenocryst was and the NSH9 was corrected using the following equation carried on a Cameca IMS-1270 at the Centre de Recherches bias =IMF–IMF =f(Mg#)–IMF (3) Pétrographiques et Géochimiques, Centre National de la Re- (2) (NSH9) (NSH9) 18 sample cherche Scientifique (CRPG-CNRS, Nancy), following the ana- Overall, the “true” value (δ Ocorrected ) for unknown samples lytical procedures described in Liu et al. (2015b) and Chen et al. was estimated by removing the effect of the bias (1) and bias(2) (2017). The sample coated with Au was compensated for the δ18 Osample charging by an electron gun. The Cs+ primary ion beam was corrected 18 sample focused into 20 μm in diameter on the sample surface at ~5.3 nA α Oraw  bias(1)  bias(2) (4) and 10 kV. Secondary negative ions were extracted at 10 kV and 18 sample 18 NSH9 18 NSH9 α Oraw  (δ Oraw δ O true )  17 18 the OH and O ions were distinguished by the 3000 mass ( f (Mg # )  IMF ) resolution power. Two off-axis Faraday cups (L’2 and H1) were (NSH9) 16 18 used to detect the O and O of the samples in multi-collection The standards were analyzed every day before measuring mode. The oxygen isotope values of the cpx phenocrysts were the unknown samples. The correlation between Mg# and IMF 18 reported in δ O relative to the reference standards (Vienna Mean of standards in each day (each session) was estimated. The Standard Ocean Water, VSMOW). The internal precision of analytical results of each session for the standards are listed in single analysis was typically less than 0.1‰ (2σ). Fig. 3 and Table 1.

2.2 Corrections of Instrumental Mass Fractionation 2.3 Precision and Accuracy The correlation between instrumental mass fractionation The error includes the internal precision of the instrument, # 2+ 2+ 2+ (IMF) and the Mg (=100×Mg /(Mg +Fe )) of cpx can be used the reproducibility or repeatability during measurement and the for the matrix effect during the measurement of oxygen isotopes additional error caused by IMF corrections. by SIMS (Gurenko et al., 2001). Thus, the Nüshan cpx The internal precision of Cameca IMS 1270 at megacrysts (NSH2, NSH5, NSH8, NSH9, NSH10, and NSH14) CRPG-Nancy is typically in the range of ±0.08‰–0.14‰ (in from eastern China, with homogeneous oxygen isotope composi- most cases <0.1‰) (2SE). The reproducibility or repeatability tions and the similar chemical compositions as those of cpx during measurement can be calculated from a standard devia- phenocrysts in this study (Xia et al., 2004), were selected for the tion of N measurements (Kita et al., 2009; Valley and Kita, correction of the matrix effect. The IMF can be generally defined 2009; Fitzsimons et al., 2000). During the measurement, sev- as the deviation between the measured and true values and can eral analyses are conducted (generally 3 times) on each cpx occur at the production, transport and detection of secondary ions. grain. The standard deviation of the mean (SE) is typically less The transport and detection of secondary ions are primarily con- than ±0.3‰. The additional error caused by IMF corrections trolled by the state of the instrument, which can be monitored by usually contain three portions: 1) the uncertainty regarding the periodically measuring the standard (NSH9). The main propor- standards’ oxygen isotopic composition (less than ±0.2‰, 2SD, tion of mass fractionation occurs at the production of secondary Xia et al., 2004); 2) the uncertainty regarding the chemical ions, which depends on type and composition of the mineral composition of cpx (the error of Mg# is near 1 unit for EPMA (commonly referred to as the “matrix effect”). For this portion, a analysis, Chen et al., 2015b); and 3) the uncertainty from “ma- group of standards (NSH2, NSH5, NSH8, NSH9, NSH10, trix effect” line calibrated by the linear least-square (Eq. 2). NSH14), with chemical compositions bracketing the unknown Based on Eq. 2, the uncertainty of oxygen isotopes introduced samples was used to correct the “matrix effect” (Deegan et al., by the error of Mg# is less than ±0.1‰. The uncertainty caused 2016; Hartley et al., 2012; Kita et al., 2010, 2009; Page et al., by the least-square regression line (Eq. 2) can be calculated by

Typical Oxygen Isotope Profile of Altered Oceanic Crust Recorded in Continental Intraplate Basalts 581

5.0 5.0 Session 1 (a) Session 2 (b) 4.0 4.0

3.0 3.0

IMF

IMF yx= -0.154 +14.998 yx= -0.124 2 +12.643 2.0 R²=0.939 2.0 R²=0.736 7

1.0 1.0 70 72 74 76 78 80 82 70 72 74 76 78 80 82 Cpx Mg# Cpx Mg# 2.5 2.5 ( c) (d) 2.0 Session 3 2.0 Session 4 1.5 1.5

IMF IMF 1.0 1.0 yx= -0.091 5 +7.993 9 yx= -0.099 4 +8.893 0.5 R²=0.840 3 0.5 R²=0.888 2 0.0 0.0 70 72 74 76 78 80 82 84 70 72 74 76 78 80 82 84 # # Cpx Mg Cpx Mg

Figure 3. The correlation between Mg# and IMF of clinopyroxene standards in each session.

Table 1 The SIMS analysis results of standards for matrix effect correction where A and B are same as in Eq. 2. The calculated results show that the uncertainty caused by Mg#a δ18O a δ18O IMF SE true measured the least-square regression line is less than ±0.1‰ for sessions Session 1 NSH2 72.9 5.46 9.15 3.69 0.31 1, 3 and 4 and less than ±0.2‰ for Session 2 (Fig. 4). NSH8 77.8 5.99 8.77 2.78 0.2 Overall, the total errors on δ18O are generally about ±0.5‰. NSH9 80 5.33 8.15 2.82 0.15 NSH14 71.6 5.07 9.17 4.1 0.12 3 RESULTS NSH5 80.3 5.88 8.55 2.67 0.3 The chemical compositions of the cpx phenocrysts selected Session 2 NSH2 72.9 5.46 8.7 3.24 0.06 for SIMS analyses have been determined by Chen et al. (2015b). NSH8 77.8 5.99 8.84 2.85 0.05 The BSE (backscattered electron) images show that most of the NSH14 71.6 5.07 9.16 4.09 0.1 cpx phenocrysts are euhedral and homogeneous (Fig. 5), and only NSH5 80.3 5.88 8.7 2.82 0.06 a few of them have an inherited core. These cpx phenocrysts ex- Session 3 NSH2 72.9 5.46 6.67 1.21 0.07 hibit chemical homogeneity within individual grains (Chen et al., NSH8 77.8 5.99 6.61 0.62 0.13 2015b). They are augitic to diopsidic cpx and have relatively # NSH14 71.6 5.07 6.72 1.65 0.16 lower Mg (68.2–82.2) and Cr2O3 (<0.8 wt.%), higher TiO2 (0.7 wt.%–4 wt.%) compared to cpx in the peridotite xenoliths carried NSH5 80.3 5.88 6.58 0.7 0.22 by the Shuangliao basalts (91.5–92.8 Mg#, 0.72 wt.%–1.42 wt.% NSH10 82.5 5.77 6.34 0.57 0.11 Cr2O3, 0.16 wt.%–0.32 wt.% TiO2). Most of the studied cpx has Session 4 NSH2 72.9 5.46 6.86 1.4 0.15

NSH8 77.8 5.99 7.15 1.16 0.01 0.30 NSH14 71.6 5.07 7.06 1.99 0.14 NSH5 80.3 5.88 6.84 0.96 0.16 0.25 NSH10 82.5 5.77 6.46 0.69 0.21 a. Data from Xia et al. (2004). 0.20 Session 2 the equation

perdicted 0.15 #* # 2 1 (Mg  Mg ) SE (5) Session 4 SEδ pred  SEδ std  n n (Mg#  Mg# )2 i1 i 0.10 Session 3 Session 1 where Mg#* is the Mg number of cpx, n is the number of stan- dards involved in the regression line, Mg# is the average Mg# 0.05 # # of all of the standards, Mg i is the Mg of the i-th standard, and the SEδ std is the standard deviation of the data points regarding 0.00 60 65 70 75 80 85 90 the regression line, which is calculated as follows # Cpx Mg 2 n (y  Ax  B) SE i i (6) Figure 4. The relationship between the errors caused by matrix effect re- δ std i1 n  2 gression line and the Mg# of clinopyroxene, calculated by Eqs. (5) and (6).

582 Huan Chen, Qun-Ke Xia, Etienne Deloule and Jannick Ingrin

TiO2 higher than 0.7 wt.% and the concentration of TiO2 show a gen isotope profile of altered oceanic crust (Gao et al., 2006; negative correlation with the MgO (Fig. 6), which suggests that Eiler, 2001; Hoffman et al., 1986; Gregory and Taylor, 1981); these cpx are igneous phenocrysts. The inherited core of some cpx and (2) the δ18O values within individual samples also display has a relatively lower TiO2 concentration (<0.7 wt.%), which is considerable variations from 1.04‰ to 1.75‰. consistent with the chemical composition of the cpx from the During the magma formation and evolution, the oxygen lower continental crust in eastern China (Zhang and Zhang, 2007 isotope compositions of magma can be affected by many factors, and the references therein). Moreover, the highest Mg# values of including partial melting of the mantle source, fractional crystal- the cpx phenocrysts are similar to those of the coexisting ol lization, crustal contamination (or assimilation-fractional crystal- phenocrysts (~84.3), suggesting that these cpx phenocrysts were lization [AFC] process), devolatilization and water-melt interac- syn-crystallized with the ol phenocrysts. tion during ascent to the surface and alteration on the surface. The oxygen isotope compositions of the Shuangliao cpx With MgO between 8 wt.% and 3 wt.%, the fractionation of phenocrysts are reported in Table 2 and plotted in Fig. 7. The δ18O oxygen isotopes caused by partial melting, fractional crystalliza- values vary widely, ranging from 4.10‰ to 6.73‰, and the aver- tion and/or devolatilization will be less than 0.1‰ for δ18O of the age δ18O value of the cpx phenocrysts in BBT, BLS, DHLB and basaltic melt (Eiler, 2001). Therefore, partial melting, fractional XTEJ is 5.93‰±0.36‰, 5.95‰±0.30‰, 5.58‰±0.66‰, and crystallization and devolatilization are unlikely to be the primary 4.55‰±0.38‰, exceeding the value of cpx in typical mid-ocean cause of δ18O variations in our samples. In addition, the previous ridge basalt (MORB) and mantle peridotites (5.4‰–5.8‰) (Eiler studies have shown that crustal contamination for the Shuangliao et al., 1997; Mattey et al., 1994). Interestingly, this variation is basalts is limited (Chen et al., 2015b; Xu et al., 2012), thus ex- time-dependent. From 51 to 43 Ma, the δ18O of the Shuangliao cluding the effect of crustal contamination on the observed oxy- basalts varied from the values higher than those of the normal gen isotopic variations. Theoretically, an AFC process would mantle to the values lower than those of the normal mantle, which significantly affect the oxygen isotopic compositions of melts if displayed an oxygen isotope profile similar to that of the altered they underwent during ascent (Taylor, 1974). According to the oceanic crust (Gao et al., 2006; Eiler, 2001; Hoffman et al., 1986; equation in Taylor (1974), to increase the δ18O value, high degree Gregory and Taylor, 1981). of fractional crystallization and crustal contamination is required. However, the sample (BBT2) with the highest δ18O value is 4 DISCUSSION characterized by highest Mg# (66.9), highest Ni (525.6 ppm) 4.1 Heterogeneity of Oxygen Isotope Compositions and Cr (373 ppm) contents, highest Nb/U (38.4) and Ce/Pb The δ18O values of the cpx phenocrysts in the Shuangliao (24.9) ratios (Chen et al., 2015b), which is not consistent with basalts have two primary features: (1) the average δ18O values this AFC process. Although the high-temperature water-melt vary widely, from 4.55‰ to 5.95‰, falling in the typical oxy- interaction during crystallization (Wang and Eiler, 2008) can

Figure 5. The BSE images of the cpx phenocrysts in the Shuangliao basalts. Abbreviation cpx. clinopyroxene.

Typical Oxygen Isotope Profile of Altered Oceanic Crust Recorded in Continental Intraplate Basalts 583

Table 2 The oxygen isotope composition of the cpx phenocrysts in the Shuangliao basalts

# 18 * 18 ** *** Sample Mg δ Omeasured IMF δ O corrected by IMF 1SE Average 1SD BBT2-12a 77.8 8.21 2.04 6.16 0.21 BBT2-14a 71.4 7.96 2.27 5.69 0.17 BBT2-20 73.4 8.00 2.08 5.92 0.16 BBT2-25a 68.2 8.18 2.71 5.46 0.12 BBT2-25b 74.2 8.21 2.04 6.17 0.12 BBT2-34a 72.3 8.24 2.45 5.79 0.09 BBT2-26a 73.4 8.11 2.14 5.97 0.10 BBT2-37a 74.9 8.42 2.17 6.26 0.08 BBT2-09a 82.2 8.04 1.31 6.73 0.16 BBT2-07a 74.3 8.52 2.44 6.08 0.27 BBT2-1a 70.3 8.25 2.61 5.64 0.05 BBT2-3a 74.9 7.90 2.03 5.87 0.13 BBT2-5a 76.9 6.79 1.68 5.11 0.21 BBT2-22a 72.8 8.46 2.48 5.98 0.14 BBT2-30a 75.4 8.19 2.06 6.12 0.04 5.93 0.36 BLS7-24d 76.0 7.67 1.82 5.85 0.18 BLS7-24b 76.0 7.88 2.03 5.85 0.13 BLS7-19a 78.9 7.66 1.64 6.02 0.17 BLS7-04 76.7 7.97 2.19 5.78 0.28 BLS7-37 81.5 7.89 1.37 6.52 0.13 BLS7-27a 76.0 8.89 2.94 5.95 0.18 BLS7-28a 74.0 7.91 2.00 5.90 0.17 BLS7-36a 77.0 8.56 1.99 6.57 0.28 BLS7-11a 75.2 7.60 2.07 5.53 0.20 BLS7-14a 76.3 8.04 2.07 5.97 0.14 BLS7-18a 72.0 7.97 2.36 5.61 0.12 BLS7-34a 75.8 7.75 1.94 5.80 0.20 5.95 0.30 DHLB10-1-08b 77.2 9.56 4.91 4.65 0.15 DHLB10-1-10b 72.9 9.55 5.17 4.37 0.44 DHLB10-1-15d 79.7 9.07 2.67 6.40 0.16 DHLB10-1-15b 78.7 8.82 2.89 5.93 0.17 DHLB10-1-15a 80.1 8.75 2.75 6.00 0.21 DHLB10-1-15c 78.3 8.89 3.00 5.89 0.14 DHLB10-1-06a 73.9 9.31 3.62 5.70 0.31 DHLB10-1-06b 30.5 8.84 3.07 5.77 0.04 DHLB10-1-03b 71.7 8.82 3.94 4.87 0.09 DHLB10-1-03c 80.0 9.15 2.93 6.22 0.22 5.58 0.66 XTEJ4-5-02a 77.0 9.28 4.46 4.82 0.10 XTEJ4-5-02b 78.3 9.51 4.30 5.21 0.22 XTEJ4-5-02c 78.8 9.56 4.25 5.32 0.11 XTEJ4-1-04a 76.1 9.05 4.74 4.32 0.02 XTEJ4-4-02a 76.8 8.92 4.73 4.19 0.13 XTEJ4-1-05a 75.9 8.57 4.07 4.50 0.30 XTEJ4-4-05a 77.4 8.72 4.16 4.57 0.26 XTEJ4-1-10b 76.1 8.92 4.51 4.41 0.19 XTEJ4-1-10a 74.0 9.16 4.91 4.25 0.24 XTEJ4-1-01b 68.5 10.03 5.92 4.10 0.29 XTEJ4-1-01c 72.9 9.84 5.42 4.42 0.08 4.55 0.38

The Mg# of cpx phenocrysts in Shuangliao basalts are from Chen et al. (2015b); *. IMF is the instrumental mass fractionation; **. SE is the standard error of the mean for the group of measurements in a single cpx grain; ***. SD is the one standard deviation of the averaged δ18O values for each sample.

584 Huan Chen, Qun-Ke Xia, Etienne Deloule and Jannick Ingrin

5 BBT2 consistent with the results of other basalts from the Chaihe- BLS7 aershan and Taihang volcanoes in eastern China (Chen et al., 2017; 4 DHLB10 Liu et al., 2015b), Cannary Island (Gurenko et al., 2011) and Yel- XTEJ4 lowstone (Wotzlaw et al., 2015). 3 4.2 Recycled Oceanic Crust in the Mantle Source Cpx of lower crust Detailed geochemical studies have shown that the Shuan- 2 2 in eastern China gliao basalts are characterized by high Fe O , HIMU-like trace Crust-derived 2 3 TiO (wt.%) cpx of inherited core element pattern and Sr-Nd isotope composition, which indicate 1 that the recycled oceanic slab may have been involved in the mantle source (Xu et al., 2012). 0 Generally, the lower gabbroic oceanic crust is enriched in 10 11 12 13 14 15 16 plagioclase (pl) that is characterized by the positive Eu and Sr MgO of cpx (wt.%) anomalies (Drake and Weill, 1975; Ching-oh et al., 1974). Thus, Figure 6. TiO2 versus MgO of the clinopyroxenes in the Shuangliao basalts. the lower gabbroic oceanic crust should have positive Eu and Sr The dashed area represent the composition region of the clinopyroxenes anomalies (e.g., Bach et al., 2001). Meanwhile, the upper oceanic from the lower continental crust in eastern China (from Zhang and Zhang crust is composed by MORB, which has no Eu and Sr anomalies (2007) and references therein). (e.g., Kelley et al., 2003). In Figs. 8a and 8b, negative correlations can be observed between the δ18O values of the cpx phenocrysts Error bar ±0.5‰ and Eu anomalies (Eu/Eu*), Sr anomalies (Sr/Sr*) of whole rocks Cpx N-MORB for the Shuangliao basalts, suggesting two components in the EM1 mantle source: Component I with low δ18O value and positive Eu 18 EM2 and Sr anomalies; Component II with high δ O value and weak HIMU Eu and Sr anomalies. Because the Eu and Sr anomalies are typi- cally associated with pl (Drake and Weill, 1975; Ching-oh et al., 50.1 Ma BBT2 1974) and the pl is rare in the Shuangliao basalts (Chen et al., 18 49.7 Ma BLS7 2015b; Xu et al., 2012), the pl contribution with the low δ O 51.0 Ma DHLB10 values should have been present in the mantle source of the ba- salts. This is consistent with the low δ18O characteristics of the 43.0 Ma XTEJ4 high temperature hydrothermally altered lower gabbroic oceanic crust (Gao et al., 2006; Bach et al., 2001; Hoffman et al., 1986; Gregory and Taylor, 1981). In addition, the basalts with high δ18O 3456789101112 values have no Eu anomaly and relatively weak Sr anomaly which δ18O (‰) are similar to the features of the upper oceanic crust undergone the Figure 7. Oxygen isotope compositions of the clinopyroxenes phenocrysts low temperature hydrothermal alteration (Gao et al., 2006; Kelley in the Shuangliao basalts. The range of δ18O values of the clinopyroxenes et al., 2003; Hoffman et al., 1986; Gregory and Taylor, 1981). phenocrysts in N-MORB, EM1, EM2 and HIMU are calculated from the Therefore, the negative correlations between the δ18O values of δ18O values of the olivine phenocrysts (Eiler et al., 1997), assuming an the cpx phenocrysts and the Eu and Sr anomalies are exactly cor- equilibrium fractionation of 0.4‰ (Mattey et al., 1994). The erupted ages of respond to the whole section of the oceanic crust, providing a the Shuangliao basalts are from Xu et al. (2012). clear evidence that a whole recycled oceanic crust was involved in the mantle source of these continental intraplate basalts and the affect the oxygen isotope composition of the magma (decreas- proportions of these components varied with time (in the mantle ing the δ18O values of the sample), the water content of XTEJ4 source of earlier basalts (~51 Ma), the recycled upper oceanic basalt (with the lowest δ18O value) is lower than those of other crust component dominated, whereas the lower oceanic crust basalts in the Shuangliao volcanic field (Chen et al., 2015b) and component was involved in during the younger eruptive cycle argues against such an interaction as the cause for the low δ18O (~43 Ma)). values. Additionally, the selected cpx phenocrysts are all fresh It is worth noting that the H2O/Ce ratios of the Shuangliao without crack and inclusion (Chen et al., 2015b), which can basalts (158–737) display a positive correlation with (Ba/Th)n eliminate the effect of the alteration on the surface. (n means primitive mantle normalization) and a negative corre- Overall, the typical oxygen isotope profile of altered oceanic lation with Ce/Pb (Chen et al., 2015b), and the XTEJ4 basalt crust recorded by the cpx phenocrysts in the Shuangliao basalts with the lowest δ18O compositions (4.10‰–5.32‰) is charac- represents the heterogeneity of the mantle source, which means terized by a significant K positive anomaly, high H2O/Ce (566) both components with high and low δ18O values were involved in and Ba/Th (105) ratios. All these suggest the presence of an- the mantle source. On the other hand, the variation in oxygen other component with high (Ba/Th)n and low Ce/Pb in the isotope compositions within each sample is most likely caused by mantle source. The marine sediments characterized by high magma mixing in a complex magma plumbing system shortly (Ba/Th)n and low Ce/Pb can serve as such component (Dixon before the eruption. In fact, the δ18O features of the cpx et al., 2002; Plank and Langmuir, 1998), but they also have phenocrysts within the single sample of the Shuangliao basalts are high δ18O values (Eiler, 2001; Gregory and Taylor, 1981). Here,

Typical Oxygen Isotope Profile of Altered Oceanic Crust Recorded in Continental Intraplate Basalts 585

10 10 (a) (b) 8 8

6 N-MORB 6 N-MORB

O (‰) O (‰) 4

18 18 4

δ δ 51 Ma BBT 2 51 Ma 43 Ma BLS7 2 DHLB10 2 43 Ma XTEJ4 0 0 0.8 0.9 1.0 1.1 1.2 1.3 1.0 1.2 1.4 1.6 1.8 2.0 2.2 2.4 2.6 Eu/Eu* Sr/Sr* 16 16 GLOSS GLOSS 14 (c) 14 (d)

12 Dehydrated UOC 12 10 10 Dehydrated UOC

8 35% 8 35%

O (‰) O (‰) DMM 25% 25% 15% 15% 15%

18 18 15% 5% 10%

δ δ 10% 6 5% 5% 6 5% 5% 0.5% 1% 5% 25% 0.5% 1% 35% 15% DMM 15% 35% 4 25% 4 2 2 Dehydrated LOC Dehydrated LOC 0 0 0 200 400 600 800 1 000 1 200 1 400 60 80 100 120 140 160 Ba/Th HO/Ce2

18 Figure 8. Comparison of the range of δ O values in the clinopyroxenes phenocrysts and the trace element ratios (Eu/Eu*, Sr/Sr* and H2O/Ce) of the Shuan- gliao basalts. The Eu/Eu*, Sr/Sr* and H2O/Ceare calculated from Chen et al. (2015b). The black lines are mix lines calculated between depleted mantle (DMM) and upper oceanic crust (UOC), lower oceanic crust (LOC), marine sediments (GLOSS). The δ18O values of DMM, GLOSS, UOC and LOC are from Eiler

(2001). The H2O/Ce ratios of DMM, GLOSS, UOC and LOC are from Dixon et al. (2002) and Plank and Langmuir (1998). The ratio of Ba/Th for DMM, GLOSS, UOC and LOC is calculated from Bach et al. (2001), Kelley et al. (2003), Plank and Langmuir (1998) and Workman and Hart (2005). we conducted a mass balance calculation to determine whether to the later ones (~43 Ma). Considering the water-rich sediment the involvement of a sediment component can match the low is generally most fusible, its addition to the mantle might be a δ18O in the Shuangliao mantle source. Basing on the equation trigger of the melting. The δ18O as well as the trace element ratios (e.g., Ba/Th) ci melt  (aC i  bC i  cC i )/ of the Shuangliao basalts significantly varied with the eruption c j DMM LOC GLOSS melt (7) ages (Figs. 7 and 8), indicating that the contributions of differ- j j j (aCDMM  bCLOC  cCGLOSS ) ent recycled oceanic components in the mantle source changed within the time interval of the Shuangliao volcanoes’ formation. where i and j represent the element; C i , C i , C i and melt DMM LOC The Pacific slab is constantly subducting under eastern China C i are the concentration of element i in melt, DMM (de- GLOSS for at least the last 80 Ma (Maruyama et al., 1997) and con- pleted mantle), LOC (lower oceanic crust) and GLOSS (marine tinuously transports recycled materials to the deep mantle. sediments), a, b and c are the proportions of the components Therefore, the temporal heterogeneity of the source compo- (a+b+c=1). The δ18O value, H O/Ce and Ba/Th ratios were used 2 nents shown by the Shuangliao basalts is likely to be caused by for the mass-balance calculation. The results show that the the ongoing Pacific slab subduction. In other words, the Pacific XTEJ4 basalts with the lowest δ18O value and highest H O/Ce 2 slab is likely the source of the enriched components in the con- ratio can be mixed by 72.5% DMM, 26% LOC and 1.5% tinental basalts from eastern China (Chen et al., 2017). GLOSS (the δ18O value, H O/Ce and Ba/Th ratios of DMM, 2 LOC and GLOSS are from Eiler (2001), Workman and Hart 5 CONCLUSIONS (2005), Dixon et al. (2002), Bach et al. (2001) and Plank and (1) The δ18O values of the cpx phenocrysts in the Shuan- Langmuir (1998)), which means that the mantle source of the gliao Cenozoic basalts vary widely (from 4.10‰ to 6.73‰), basalts with the low δ18O compositions can contain a water-rich exceeding the value of cpx in typical MORB and mantle peri- sediment component. Furthermore, we calculated the mixing dotites and falling in the range of oxygen isotope compositions lines between DMM and UOC (upper oceanic crust), LOC, of an altered oceanic crust, which provides a clear evidence that GLOSS. All points are within the areas of the mix lines and the a recycled oceanic slab was involved in the mantle source of relative contributions of these recycled oceanic components in these continental basalts. the mantle source varied significantly within a limited time (Figs. (2) The relative contribution of the enriched source com- 8c and 8d). In combination with the ages of the Shuangliao ba- ponents in the mantle source has changed with time. More salts, the contribution of the recycled sediments in the mantle water-rich sediment component is observed in the mantle source seems to increase from earlier volcanic events (~51 Ma) source of the youngest Shuangliao basalts, which might be the

586 Huan Chen, Qun-Ke Xia, Etienne Deloule and Jannick Ingrin trigger for mantle melting. Eiler, J. M., Schiano, P., Kitchen, N., et al., 2000. Oxygen-Isotope Evidence (3) Given the Pacific slab is constantly subducting under for Recycled Crust in the Sources of Mid-Ocean-Ridge Basalts. Nature, eastern Asia and is expected to continuously transport recycled 403(6769): 530–534. doi:10.1038/35000553 materials into the deep mantle, such ongoing subduction is a Farmer, G. L., 2014. Continental Basaltic Rocks. In: Holland, H., Turekian, K., reasonable explanation for the variations of recycled compo- eds., Treatise on Geochemistry, Second Edition. Elsevier, Amsterdam. nents in the mantle source over time. 75–110 Fichtner, A., Villaseñor, A., 2015. Crust and Upper Mantle of the Western ACKNOWLEDGMENTS Mediterranean—Constraints from Full-Waveform Inversion. Earth and This research was supported by the National Natural Sci- Planetary Science Letters, 428: 52–62. doi:10.1016/j.epsl.2015.07.038 ence Foundation of China (Nos. 41225005 and 41173047). We Fitzsimons, I. C. W., Harte, B., Clark, R. M., 2000. SIMS Stable Isotope thank Andrey Gurenko and Nordine Bouden for their help in Measurement: Counting Statistics and Analytical Precision. SIMS analysis. The constructive comments and suggestions Mineralogical Magazine, 64(1): 59–83. doi:10.1180/002646100549139 from two anonymous reviewers are greatly appreciated. The Gao, Y. J., Hoefs, J., Przybilla, R., et al., 2006. A Complete Oxygen Isotope final publication is available at Springer via Profile through the Lower Oceanic Crust, ODP Hole 735B. Chemical http://dx.doi.org/10.1007/s12583-017-0798-5. Geology, 233(3/4): 217–234. doi:10.1016/j.chemgeo.2006.03.005 Gregory, R. T., Taylor, H. P. Jr., 1981. 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