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R. Large, Indranil Mukherjee, D. Gregory, J. Steadman, V. Maslennikov, S. Meffre (2017)
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AUSTRALIAN JOURNAL OF EARTH SCIENCES https://doi.org/10.1080/08120099.2023.2200476 Lithogeochemical and sulfide trace-element systematics across the Permian– Triassic boundary, Perth Basin, Western Australia: constraints on the shallow marine environment during the end-Permian mass extinction a a a b a a E. Lounejeva , J. A. Steadman , R. R. Large , K. Grice , P. Olin and I. Belousov a b CODES, Centre for Ore Deposit and Earth Sciences, University of Tasmania, Hobart, Australia; Western Australian Organic and Isotope Geochemistry Centre, School of Earth and Planetary Science, Curtin University, Perth, Australia ABSTRACT ARTICLE HISTORY Sedimentary pyrite trace-element composition is an established proxy for determining paleo-ocean Received 7 December 2022 Accepted 29 March 2023 geochemistry and atmospheric oxygen concentrations through deep time. However, its applicability over shorter time-scales (i.e. <20 Ma) is not well known. To test this, we targeted fine-grained pyrite in KEYWORDS the Hovea Member of the Kockatea Shale (Perth Basin, Western Australia), which encompasses the laser ablation; LADR; EPMEI; late Permian inertinitic interval and the end-Permian to Early Triassic sapropel, and spans approxi- LPMEI; marginal; shallow mately 10 million years. The end-Permian mass extinction (EPME) was the largest extinction event in marine; Siberian Traps Earth history, and its greatest effect is documented in the marine environment. Samples were col- Large Igneous Province; lected from two oil exploration wells—Redback-2 and Hovea-3—spaced 20 km apart. In the two (Nodosaria) Protonodosaria boreholes, a change in depositional facies (i.e. between the inertinite and sapropel) occurs below the tereta (Crespin 1958); Permian–Triassic boundary and records the transition from a marginal marine to a shelf environment. acidification; anoxia This transition is highlighted by several lithogeochemical indicators (e.g. negative shift d Cvalues and C reduction; increases in Ca, Fe and P), which are themselves tied to fundamental changes in modal org mineralogy between the two zones. Importantly, the sapropel also records a major increase in iron sul- fide burial over that in the inertinite. LA-ICPMS analyses of pyrite demonstrate that trace-element abundance is highest in samples below the facies transition, and in places reaches a few percent, par- ticularly of Ni (4 wt%), Co (1.5 wt%) and As (2.8 wt%). Moreover, these and other trace elements decrease by an order of magnitude in concert with the negative shift in d C values in the sapropel zone. Various whole-rock based paleosalinity indicator ratios (e.g. B/Ga) indicate that the areas of the Perth Basin intersected by Redback-2 and Hovea-3 were not fully connected to the open ocean at the time of the EPME, which leads us to conclude that the very high trace-element values in the sediment- ary sulfides are reflective of regional environmental shifts rather than a global signal. Nonetheless, a geochemical contribution from a distant igneous province, such as the Siberian Traps Large Igneous Province, cannot be ruled out. Our work underscores the strength of sedimentary pyrite as a robust paleoenvironmental proxy in the marine environment and highlights the need for further investiga- tion of pyrite trace-element profiles across the mass extinction interval in other sedimentary sequen- ces around the globe. KEY POINTS 1. LA-ICPMS-based geochemistry of sedimentary pyrite from the Hovea Member of the Kockatea Shale is considered within a lithochemostratigraphic context. 2. The overall interpretation of the results involves a change in depositional setting from the marginal in the late Permian brackish waters to shelfal marine and loss of oxygen in the Early Triassic Perth Basin. Introduction biological processes, such as variation of oxygen levels in During the last 10 years, LA-ICPMS-based geochemical stud- the atmosphere–ocean system (Cannell et al., 2022; ies identified temporal trends between the trace-element Steadman et al., 2020), formation of Large Igneous contents of sedimentary pyrite and some geological and Provinces (LIPs) and mass extinctions (ME) over billions of CONTACT E. Lounejeva elena.lounejeva@utas.edu.au CODES, Centre for Ore Deposit and Earth Sciences, University of Tasmania, Hobart, Tasmania, Australia Supplemental data for this article can be accessed online at https://doi.org/10.1080/08120099.2023.2200476. Editorial handling: Anita Andrew 2023 The Author(s). Published by Informa UK Limited, trading as Taylor & Francis Group. This is an Open Access article distributed under the terms of the Creative Commons Attribution License (http://creativecommons.org/licenses/by/4.0/), which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. The terms on which this article has been published allow the posting of the Accepted Manuscript in a repository by the author(s) or with their consent. 2 E. LOUNEJEVA ET AL. years (Gregory, 2020; Large et al., 2014, 2015, 2020, 2022; ubiquitously present in both deep and shallow marine sedi- Long et al., 2016; Mukherjee & Large, 2016). In more focused mentary rocks of the upper Permian, has been cited as an research, Gregory (2020) and Gregory et al. (2015) demon- indicator of widespread ocean anoxia at the EPME, which strated that the trace-element contents of syn-sedimentary early researchers believed to be the root cause of the event or early diagenetic pyrite from the same sequences could (Cao et al., 2009; Isozaki, 1997; Song et al., 2012). However, vary by more than an order of magnitude over time intervals more recent research has focused on establishing a causa- shorter than 100 million years. In this work, we evaluate the tive link between the emplacement of the Siberian Traps applicability of the sedimentary pyrite proxy on a time-scale Large Igneous Province (STLIP) and the EPME (Ernst & shorter than 20 Ma. For these purposes, we targeted shales Youbi, 2017; Ernst et al., 2021). Regardless of the difference across the Permian–Triassic stratigraphic boundary (PTB). in proposed triggers (i.e. anoxia vs asphyxiation), it is likely The PTB is associated worldwide with the most severe that significant chemical changes in the marine environ- mass extinction in Earth’s history and a significant change ment and atmosphere associated with the EPME can be in the carbon cycle (Baud et al., 1989), both of which are identified using the major, minor and trace-element com- thought to have been triggered by numerous climatic and positions of coeval sediments and syn-sedimentary pyrite. tectono-magmatic drivers (Black et al., 2014; Clarkson et al., 2015; Chen et al., 2015; Ernst, 2014; Ernst & Youbi, 2017; Grice et al., 2007; Metcalfe et al., 2013; Payne & Kump, Regional and local geology of the EPME in the Perth 2007). This mass extinction event has been given different Basin names by different authors, but for simplicity and clarity, The Hovea Member in the northern Perth Basin, Western we will refer to it as the end-Permian mass extinction Australia (Figure 1), was targeted for this study as the only (EPME). The determinative factors causing the EPME are thought to have involved significant disturbance to the bal- marine sequence on the Australian continent that includes the PTB. Two oil-exploration wells—Redback-2 and Hovea- ance of atmospheric gases essential for life on Earth, such as oxygen, methane, carbon dioxide and sulfur dioxide, 3—were selected for sampling, as they contain well-pre- and an increase in toxic metals in the ocean. Pyrite, served intersections of the Hovea Member. Figure 1. Perth Basin’s current location, onshore in Western Australia and offshore in the Indian Ocean (simplified from Geoscience Australia). The inset shows the Gondwana land, paleo-oceans, and the Perth Basin paleo-location based on tectonic reconstructions (Blakey & Ranney, 2018) at the joint point between Antarctica, Australia and Great India. AUSTRALIAN JOURNAL OF EARTH SCIENCES 3 Based on the completion reports for Redback-2 and Methods Hovea-3 and other researchers (Jones, 2011), the Hovea Bulk analyses Member represents the earliest sedimentation product of the Kockatea Shale. It was deposited during post-rift thermal The sediment chemical compositions have been obtained subsidence and marine transgression, and contains two via ICP-AES and ICP-MS instrumental analyses (ALS Minerals distinct facies: a lower package of inertinitic mudstones (INI) Laboratory, four-acid digestion method ME-MS61), achiev- and an upper package of sapropelic (SPI) mudstones. ing an analytical precision of 5% on duplicates. Sulfur The stratigraphic framework of the Hovea Member has been and carbon content was determined using an ELTRA CS- defined by studies of palynofacies (R. Purcell in Origin Ltd, 2000 elemental analyser. 2003, 2010; Thomas et al., 2004; D. Mantle in Lounejeva et al., 2021) and associated invertebrates (Shi et al., 2022), as LA-ICPMS analysis well as a Re–Os age of 253.5 ± 1.4 Ma for the INI top shale in We followed the methodology for LA-ICPMS sedimentary the Hovea-3 borehole, which is equivalent to the late pyrite geochemistry as a proxy to paleo-ocean environment Permian Changhsingian stage (Georgiev et al., 2020). The fully described by Large and co-authors (Gregory, 2020; lower INI contains abundant late Permian palynoflora (D. Gregory et al., 2015, 2020; Large et al., 2014, 2022; Stepanov parvithola Zone) and brachiopods, whereas the SPI contains et al., 2020). This approach involves textural screening of palynofacies belonging to the Earliest Triassic (K. saeptatus suitable sedimentary pyrite material, preparation of polished Zone), as well as C. perthensis bivalves and other inverte- surfaces, in situ pyrite and surrounding matrix analysis via brates from the brachiopod, ammonoid, microconchid and LA-ICPMS, raw data processing and statistics. spinicaudatan groups. The PTB in the Hovea Member is The trace-element contents of pyrite have been ana- located in the lower part of the SPI, between the first lysed across multiple sessions by laser ablation-inductively appearance of the Triassic Griesbachian bivalves and the last coupled-mass spectrometry (LA-ICPMS) at CODES, appearance of the Australian endemic P. microcorpus Zone University of Tasmania. The suite of elements likely incor- palynoflora and associated lingulid species of the latest porated into pyrite structure analysed for this study Permian Changhsingian (Metcalfe et al., 2008, 2015; Shi et al., includes Co, Ni, Pb, Cu, Zn, As, Se, Ag, Sb, Bi, Tl, Au, Mn 2022). The EPME, which occurs below the PTB and straddles and Cd, whereas Al, Si, Ca, Mg and a set of other elements the SPI/INI transition, contains abundant black wood frag- have been analysed for other minerals for signal monitor- ments, degraded organic material and some marcasite ing and the matrix deconvolution. LA-ICPMS mass spec- (Lounejeva et al., 2021; Shi et al., 2022). trometry allows the signal of each element during analysis The most prominent chemostratigraphic changes occur- to be observed to determine whether the element belongs ring at the top of the INI, which is within the EPME, are the to pyrite or to a neighbouring mineral. The primary negative shift or excursion of d C (organic and kerogen) calibration standards include the in-house reference values, recognised worldwide and linked to the end- materials STDGL2b2 (Danyushevsky et al., 2011) and Permian mass extinction interval (EPMEI) and the STLIP STDGL3 (Belousov et al., 2014, 2023) for quantification of (Korte & Kozur, 2010; Metcalfe et al., 2013), and a positive 34 siderophile and chalcophile elements, and the USGS refer- spike in d S values of marcasite–pyrite (Lounejeva et al., ence material GSD-1G (Jochum, 2014), for quantification of 2021) that has allowed geochemical correlation of the lithophile elements. A natural pyrite standard PPP-1 (Gilbert Hovea Member P. microcorpus Zone (Grice et al., 2007; et al., 2014) was used to quantify sulfur. Instrumental speci- Lounejeva et al., 2021; Metcalfe et al., 2015; Nabbefeld fications are provided in the Supplemental data. et al., 2010; Sial et al., 2020; Thomas & Barber, 2004). The raw results have been reduced using the inhouse- Multiple bulk-rock geochemical studies of the Hovea developed method (Stepanov et al., 2020), which is based Member have revealed contrasting geochemical changes on the Excel spreadsheets and the Basic script templates across the EPMEI, suggesting a discontinuous sedimentary for mass balance and Fe–S linear regression. In addition, record or geochemical mixing around the SPI/INI interface. matrix-pyrite deconvolution is possible using the Laser Some studies infer anoxia well before the EPMEI, indicating a Ablation Data Reduction (LADR) software from Norris change to euxinia in the photic zone in the early Triassic Scientific (https://norsci.com/?p=ladr). The ioGAS software (Georgiev et al., 2020; Grice, Cao, et al., 2005; Grice, Summons, from IMDEX (https://iogas.imdexlimited.com) has been used et al., 2005; Grice, Twitchett, et al., 2005), whereas some others for basic statistics and presentation of the data. strengthen the temporal link to different stages of the STLIP activity (Sial et al., 2020). Pyrite is commonly the main host for several redox-sensitive elements (e.g. Se, Co, As, Ni, Cu, Bi, Ag); Results thus, we investigated whether pyrite in the Hovea Member Sampling, lithology and mineralogy retained a record of the inferred changes. A full data set of the trace elements in sedimentary pyrite (TESPy) from Redback-2 For this study, we targeted pyrite-bearing mudstones in and Hovea-3 boreholes as determined by LA-ICPMS along Redback-2 (3788–3935 m depth) and Hovea-3 with the sediment bulk geochemistry. (1968.6–1995.4 m) boreholes, stored at the Geological 4 E. LOUNEJEVA ET AL. Figure 2. Core photographs from Hovea-3 well (WAPIMS, Origin Ltd). Yellow circles: samples selected for bulk rock and red squares for LA-ICPMS analysis of sedimentary pyrite. Diamond shapes: samples where marcasite was identified (Lounejeva et al., 2021). The white line at 1980.95 m depth marks the boundary between the inertinitic and the sapropel (Thomas et al., 2004) and the shift in d C values (Sial et al., 2020). Survey of Western Australia’s Core Repository in Carlisle, fossiliferous and calcareous mudstones where siderite is WA. A total of 48 samples were collected with their distri- present as thin layers, calcite mostly as nodules and perva- bution shown in Figures 2 and 3, with a complete list of sive cement or streak veins; dolomite presence has been samples, methods and results in the Supplemental data. inferred from the rhombic shape. The SPI/INI interface pos- The rock chips were sectioned, placed in 25 mm round ition is in agreement with the uppermost record of inertin- mounts of epoxy resin, polished with and examined by ite in the completion reports, i.e. at RB2-3804.14/3804.15 reflected light optical microscopy to reveal pyrite morph- and at HO3-1980.95 m depth (Figure 2). ology in its textural context and guide LA-ICPMS analysis. The mineral content follows lithological changes. In RB2, Rock powder for whole-rock analyses was micro-drilled pyrite is less abundant (<2 wt%) in the Permian INI than in and milled from offcuts. A general description of lithofacies the Triassic SPI (up to 9%), where the eye-catching pyrite and mineralogy has been adopted from the Redback-2 and nodules are better developed through diagenesis. Quartz dominates the INI (30–45%) but is less abundant in the SPI Hovea-3 well-completion reports (Origin Ltd, 2003, 2010), as well as the study by Jafary Dargahi and Rezaee (2013). (15–20%). Clays (illite–mica, illite–smectite and chlorite) X-ray diffraction was used to determine the composition of constitute 40–60% of the INI but give way to kaolinite (up siderite nodule and scanning electron microscopy (SEM) to 10%) and calcite (up to 25%) in the SPI. Other identified with energy dispersive x-ray spectrometry (EDS) for some traces (2%) include feldspar, barite, pyroxene, titanite, mineral identification and backscattered electron imaging. Mn-rich carbonates, detrital zircons with some primary In both cores, the Permian dark grey and black fine apatite inclusions, anatase (RB2-3806.51), monazite mudstones, which are interbedded with silty sandstones, (RB2-3807.35), galena and barite globules <10 mm (RB2- and in places bioturbated, are composed mostly by clays, 3808.13). Some Hg-containing smectite has been identified with variable content of quarts and pyrite. The Triassic sedi- during the SEM study at RB2-3821.3, that is 15 m below ments are dark brown, brittle, microlaminated siliceous, the shift in d C values. Sporadic siderite nodules, 5–10 cm AUSTRALIAN JOURNAL OF EARTH SCIENCES 5 Figure 3. Studied samples’ depth distribution in the RB2 and H3 cores. Lithological description and palynological zones are from Jafary Dargahi (2014), Lounejeva et al. (2021), Origin Ltd (2003, 2010) and Thomas et al. (2004). The straight line corresponds to the negative shift in d C values of –7& VPDB in both drill holes (Lounejeva et al., 2021). (a) Example of laminated texture in Triassic carbonaceous mudstones (RB2-3803–3805 m depth). (b) Fragment of brown siderite nodule and iron sulfide localised and circled (selected for this study from the RB2-3806–3807 m depth). (c) Example of bioturbation textures in Permian silty mudstones. across, are visible in RB2 cores. The nodules analysed at framboids spread in a siliceous clastic matrix or inside the RB2-3806.55, 3807.15 and 3820.4 m depth are 60 wt% sid- bryozoan cavities. In contrast, no marine fauna has been erite, 10–12.5 wt% fluorapatite, 10 wt% quartz, 7% calcite, observed in the studied samples from Redback-2 Permian 10 wt% illite and trace chlorite. A similar mineralogical con- INI sandstone, except a few nodules of pyritised fossils tent but lacking siderite nodules has been described for (RB2-3814.5 m; also see anomalous samples). the Hovea Member from the HO3 borehole (Georgiev et al., In RB2, the previously defined Indeterminate interval 2020). about 5 m between 3804 and 3808.9 m at the top of the 35 m-thick INI, contains rare Protohaploxypinus microcorpus Zone palynomorphs with abundant black wood, inertinite, Microfossils and the EPMEI degraded amorphous organic matter, large siderite nodules and small-sized pyrite framboids (Lounejeva et al., 2021). Abundant remnants of sea bottom creatures have been observed under reflected light in the Hovea-3 Permian This has recently been considered as the latest Permian sediments from 1983.2 to 1991 m depth. The fossils are mass extinction interval (Shi et al., 2022), and so we refer to this interval as the EPMEI. Despite only 50 km separat- best preserved in the middle of the interval but frequently broken next to enclosing sandstones. The only foraminifer ing the boreholes, the Hovea Member and, consequently, identified by Patrick Quilty (personal communication) with the extinction interval in the Hovea-3 borehole are thinner, little doubt is Nodosaria tereta Crespin 1958 (current <3 m, and should be constrained between the last bryozo- accepted name Protonodosaria tereta Crespin 1958) ans at 1983.50 m and the first Triassic bivalves at 1980.85. (Figure 5k) in HO3-1987.84. Some other species have been This is within the P. microcorpus Zone (1981–1984.2 m) and only tentatively identified, including bryozoans, sponge spi- only 10 m above the Dongara sediments, appearing at cules (diactinal monaxons [simple and pointed at both 1992.5 m depth (Thomas et al., 2004). ends]), foraminifera (Nodosaria ragatti, Tolypammina or Further, we correlate the data by a relative depth Calcitirnella) and algae (Solenopora). Scarce pyrite in a sub- assigning ‘level zero’ at RB2-3806.5 and HO3-1980.95 m interval 1983.20–1987.84 m is present as very fine corresponding to the prominent negative shift in d C 6 E. LOUNEJEVA ET AL. Figure 4. Selected bulk geochemical parameters in Hovea Member sediments discussed in the text. values and the lowest organic carbon content in both of magnitude, from an average of 0.5 wt% in the upper boreholes (Lounejeva et al., 2021; Thomas & Barber, 2004). Permian black shales to 9.5 wt% within and above the EPMEI, in the Triassic calcareous and fossiliferous mud- stones. Accordingly, Ca is followed by Sr and, to less Bulk sediment geochemical composition extent, by Mn. Sodium content is significantly lower in Hovea-3 (0.2 wt%) than in RB2 (0.5 wt%). Pyrite-like ele- The full data set of bulk geochemistry (Supplemental data) ments correlate well with each other, REEs in HO3 correlate includes the results of 43 bulk analyses of major and trace with Ca, P, Y and U (R > 0.9), and alkalis (Li, Cs) correlate elements for Redback-2 sediments, and 42 results for with the post-transition metals (Al, Ga, In). Hovea-3 sediments for rare earth elements (REEs), boron A major increase in several ratios argued by other and an additional analysis for the bulk sulfur isotope values authors as indicative of the paleoenvironment (Dymond (d S), total carbon and sulfur. The results of basic statistics, et al., 1992; McKay & Algeo, 2013; Remırez & Algeo, 2020; enrichment factors and reference values for the Average Tribovillard et al., 2006) also occurs above the EPMEI. In Black Shale and Post-Archean Australian Shale are provided particular, the increase in ratios indicative of redox (S/Fe, in the Supplemental data, and geochemical parameters Fe/Al, Mo/Al, Cu/Zn, La/Ce, Mo/U), productivity (TOC, 2.2– most relevant for this study are shown in Figure 4. 4.5 wt%; P/Ti, 548–1742 mg/g; Ag, 0.18–0.43 mg/g; Ag/Ba), In both boreholes, the major-element composition of water depth (Mn/Fe, Mn/Ti), salinity (B/Ga, Sr/Ba) and hot- the Permian inertinitic interval is distinct from the Triassic sapropel, whereas the EPME contains the various swings and-arid climate (Sr/Cu) correlate with each other in and spikes in both isotopic and elemental ratios. A double Triassic samples. The average Ba content (534 mg/g) in or triple increase above the EPMEI in content of elements Permian samples decreases (312 mg/g) in the Triassic sam- with affinity to pyrite (Fe, S, Ag, Bi, Cd, Cu, Mo, Te, Zn, Sb, ples and has a negative correlation with organic carbon, Tl and TOC), carbonates and phyllosilicates (Ca, Sr, Mn, La, sulfur and silver contents (Figure 4). Other insights from U, B) contrasts with the decrease in immobile elements (Hf, the bulk geochemistry come from REEs in HO3, and siderite Zr, Th, Ti, Ta, Nb), Mg and K. Calcium increases by an order nodules and some enrichment factors in RB2. AUSTRALIAN JOURNAL OF EARTH SCIENCES 7 The HO3 sediment PAAS-normalised REY patterns The downhole trends of TESPy are similar in Redback-2 and (Figure 4) are almost flat, but with a moderate change Hovea-3. In both boreholes, there is an interval in the late noticeable around the SPI/INI boundary. Below 1980.95 m, Permian inertinitic interval below the d C anomaly where a Ce positive anomaly (calculated following Tostevin, 2021) pyrite is enriched in elements with pyrite affinity, namely As, is barely perceptible, but in the overlying 5 cm, a pro- Ni, Co, Mo, Tl, Ag and Sb. In RB2, this interval comprises at nounced Ce anomaly and a positive Y anomaly appear least 15 m of pyritic mudstones and black shales (from 3806.5 within a fractionated HREE-enriched pattern that is strongly down to 3821 m depth) that correlates with about 5 m correlated with P and Ca; these subsamples also contain (1983.5–1988.5 m) of fossils and trace-element-rich pyrite in four to four times more Ni, Co, Sb, Mo and Mn than the HO3 mudstones. In both boreholes, the concentration of underlying samples. The overlying 5 cm still preserve a sub- these elements decreases by several orders of magnitude in tle Y anomaly but a Ce anomaly is reduced, and REEs cor- the Triassic sapropelic pyrite, whereas, Mn, Cu, Zn and Cd relate with the highest Ca (24%), Sr, total carbon and increase significantly in the Triassic interval. Y/Ho (42). The RB2-3701.1 siderite nodule contains more than 70% Discussion siderite–apatite, but also calcite and quartz. The conse- quent spike in Fe (22.2 wt%), Ca (7.5 wt%), P (>1 wt%), Mn Pyrite trace-element geochemistry across the decline (0.5 wt%) and REEs (La, CE) relative to the Hovea Member in d C values background coincides with the organic carbon isotopic The most noticeable feature of TESPy patterns in both bore- decline. holes (Figure 7), during the EPMEI in the lowermost Triassic Aluminium contents vary in RB2 from 6 to 10 wt%. The is a drop by an order of magnitude from the high concentra- Al-normalised patterns of the Hovea Member sediments are tion of Ni–Co–As in the range of thousands of micrograms compared with the Average Black Shale (ABS, Ketris & per gram in the latest Permian. The TESPy concentrations in Yudovich, 2009) by calculating enrichment factors the Triassic sediments are twice as high in HO3 as in RB2 but (EF ¼ R /R .). The comparison reveals that element SAMPLE ABS still within the Paleozoic–Mesozoic range (Gregory et al., alkalis (Li, Rb, Cs), REE and Pb are moderately above (EF ¼ 2015). This main change coincides with (1) the global organic 2–4), and P, Cd, Te, Sb and immobile elements are well carbon cycle perturbation, (2) a change in regional depositio- below the ABS (EF < 0.4). The bulk Ni content throughout nal environment and (3) the rock source and the nature and the RB2 sequence is within the reference range for shales availability of organic matter. (40–80 mg/g, EF1); however, a few Permian horizons are exceptionally enriched in arsenic (EF >5) and, to less ABS extent, Ni and Co, whether compared with the ABS, the Constraints on the depositional setting and Post-Archean Australian Shale (PAAS; Nance & Taylor, 1976) paleoenvironment of the Hovea Member or the Cariaco Basin shelf shale (Martinez et al., 2010). A general deepening of the Perth Basin in the Early Triassic, coincident with rifting off the western margin of Framboidal and disseminated sedimentary pyrite the Yilgarn Craton, has been identified previously using geochemistry several lines of structural and geophysical evidence (Jones, 2011). The macro- and micro-textural features of the sapro- Pyrite types pel (e.g. visible bivalves and brachiopods, abundant spiny Representative types of pyrite analysed during this study acritarchs, elevated organic carbon, etc.) provide strong evi- are shown in Figure 5 (photos of each sample, including dence for a marine environment from the onset of the some microfossils, are shown in the Supplemental data). We Triassic. In addition, the prevalence of the microlaminated analysed single framboids, framboidal aggregates (or clus- carbonate texture in the sapropel (likely microbial in ori- ters) and euhedral disseminated crystals <30 mm(Figure gin), the presence of frequent diagenetic pyrite nodules 5a–d). The euhedral marcasite–pyrite intergrowths in the 13 and paleoenvironment indicators are consistent with a d C-EPMEI interval and a few pyrite nodules (Figure 5g, i, j) deeper, saline, anoxic and productive environment (this have been characterised. work; Georgiev et al., 2020; Lounejeva et al., 2021; Thomas et al., 2004). LA-ICPMS results However, ascertaining the depositional environment of The calculated contents of Mn, Co, Ni, As, Mo, Cu, Zn, Cd, the Permian sections of the Hovea Member (i.e. the inerti- Mo, Te, Pb, Se, Bi, Tl and Ag in the analysed pyrites from nitic interval) has proven to be less straightforward. The both boreholes are shown in Figures 6 and 7. Using major overall sedimentological and structural development of the and minor element changes, the EPMEI was split into Perth Basin was multi-faceted, with differential deepening upper and lower, and the low-profile interval 3823.8– across the graben at various times (e.g. Haig et al., 2017; 3835 m in the RB2 INI interval separated to assess general Song & Cawood, 2000). This was especially so in the initial trends (Table 1). stages of basin opening during the late Permian (Dillinger 8 E. LOUNEJEVA ET AL. Figure 5. Examples of the Hovea Member pyrite viewed in reflected light: (a) single framboid; (b) framboidal aggregate or cluster; (c) a porous pyrite nodule preserving the boundaries of the original framboids; (d) disseminated euhedral crystals 20 mm large, RB2-3806.51; (e) a diagenetic pyrite nodule, RB2-3796.8; (f) a framboidal aggregate and single framboids with diagenetic overprint (‘spongy’ pyrite) between the Triassic carbonate micro lamina, HO3-1973.05; (g) deteriorated framboidal aggregate Pb and Se rich, RB2-3808.13; (h) well-developed framboidal aggregate Ni, Co and As-rich, RB2-3813.6; (i) marcasite euhedral crystals, Mn-rich, RB2-3806.55; (j) single framboids and clusters inside the Permian bryozoan cavities, H3-1987.84; (k) fossil foraminifer Nodosaria tereta Crespin 1958 from the Permian sediments, HO3-1987.03; and (l) pyritised fossils from the Permian shales, RB2-3814.5. The white scale bars are 100 mm wide. et al., 2022). Consequently, the depositional environment of In Hovea-3, the SPI/INI interface has been recognised at the inertinitic interval of the Hovea Member, is argued, 1980.95 m depth, and the inertinitic interval below contains with some authors favouring a fully marine section and abundant microplankton (mostly freshwater algae), which others postulating a brackish to freshwater regime (e.g. Thomas et al. (2004) used to interpret a nearshore environ- Jafary Dargahi & Rezaee, 2013; Georgiev et al., 2020; ment. More recently, Georgiev et al. (2020) postulated shal- Metcalfe et al., 2008, 2013; Shi et al., 2022; Thomas et al., lowing toward the INI top based on the recognition of 2004). We consider the various lines of evidence presented specific terrestrial organic matter in the Hovea-3 core. Our in this and previous studies and discuss them by individual interpretation is a predominantly brackish environment for wells below. the inertinitic interval based on intermediate values of AUSTRALIAN JOURNAL OF EARTH SCIENCES 9 Figure 6. Comparison of downhole profiles for Ni, As, Pb, Mn and Cu in the bulk and in sedimentary pyrite. Sr/Ba (0.2–0.5) in both boreholes and B/Ga (4–6) in Hovea- sharp shallowing upward 3808 m, based on gamma-ray 3, between the thresholds for paleosalinity defined by Wei response from pyritic mudstone and black shale dominat- and Algeo (2020). We place greater emphasis on the B/Ga ing the entire inertinitic interval. Jafary Dargahi and Rezaee ratio owing to the potential spurious influence of carbon- (2013) defined pyritic mudstones as clays with abundant ate on Sr/Ba ratios in a given section (Figure 4). pyrite nodules and veins of likely diagenetic origin, indicat- As for Redback-2, rare marine invertebrates and palyno- ing a reducing environment, and the black shale as facies indicative of nearshore marine have been reported organic-rich clays slightly silty with some pyrite indicating for the Redback-2 3804–3806 m depth interval (Shi et al., calm anaerobic environment. This conflicts with palynology, 2022; Origin Ltd, 2010), i.e. only in the higher horizons of but given the presence of pyritised nodules of sponge spi- the inertinitic interval and above the decline in d C values cules localised in this study in RB2-3814.5, we also consider (Lounejeva et al., 2021). Nevertheless, down to 3827 m deepening. However, our lithogeochemical and mineral- depth, the organic matter is destroyed, and palynofacies ogical data are inconsistent with a ‘normal marine’ environ- are very rare and poorly preserved, rendering palynological ment, i.e. a low carbon and sulfur profile (TOS0.5 wt%, interpretation difficult and varying between questionable TOC2 wt%), highly variable but generally high TOC/TOS estuarine and terrestrial, although marine influence has ratios (3.4), eventual enrichment of the bulk in d S val- WR been suggested based on the presence of rare spinose ues 45 to 29‰ VCDT at 3813 to 3811 m depth) sug- acritarchs (Lounejeva et al., 2021; Origin Ltd, 2010). gesting some restriction, brackish water indications and Therefore, we draw on the interpretation of Jafary Dargahi presence of unusual framboidal aggregates extremely and Rezaee (2013) who suggested a slight sea-level rise enriched in As, Ni and Co, and deteriorated aggregates culminated at 3812–3814 m depth and followed by a enriched in Se and Pb. 10 E. LOUNEJEVA ET AL. Figure 7. Main trend of framboidal and disseminated pyrite geochemistry across the EPMEI and the declining d C values (relative depth 0) preceding the Permian–Triassic boundary in Hovea Member sediments, Kockatea Shale, WA. In both boreholes, Hovea 3 and Redback 2, the late Permian pyrite preferentially concentrates Ni, Co, As and other elements in a shallow depositional environment with fluctuating oxygen minimum from oxic to anoxic, whereas the early Triassic is dominated by redox-sensitive elements like Cu and Mn proper for a deeper anoxic marine. Table 1. Framboidal and disseminated pyrite compositions from the Hovea Member. Geometric mean per depth interval of trace-element concentration (mg/g) Interval Depth (m) As Co Ni Ag Se Sb Te Tl Pb Bi Mo Mn Cu Zn Cd HO3 Triassic 1968.3–1980.4 346 88 184 3.1 13 9.5 1.2 3.7 149 1.5 25 1082 468 156 1.1 RB2 Triassic 3791–3803.76 275 94 157 2.1 13 7.7 1.4 2.2 122 1.3 30 957 247 112 2.4 RB2 EPMEI upper 3805.4–3806.55 245 140 300 2.4 17 9.1 2.9 1.1 129 1.4 21 630 165 43 1.2 RB2 EPMEI lower 3807–3808.13 650 648 784 2.5 16 15.6 2.5 2.1 373 9.7 12 94 180 23 0.2 RB2 Permian 3808.9–3821.3 2186 730 1513 9.2 22 27.6 1.7 7.7 320 1.3 21 35 136 14 0.3 RB2 Permian 3823.8–3835 702 196 600 2 22 7 3 1 429 2 15 33 146 21 0.4 HO3 Permian 1981.45–1992 1024 400 656 7.6 22 5.7 2.8 12.0 289 3.9 28 347 258 71 1.1 Trace-element anomalism in pyrite aggregates from contain up to 4.7 wt% Ni, 1.6 wt% Co, and 2.8 wt% As. Well- Redback-2 preserved metal-rich framboids are shown in Figure 5h. The large diameter (35 ± 10 mm) of framboids is compatible Ni–Co–As-rich pyrite (pyrite pearls and pyritised fossils). with either dysoxic or anoxic sedimentary environments, Transitional metal contents in this late Permian interval are whereas the lenticular shape of the aggregate and lack of generally high (100–4000 mg/g), but some framboids and deformation of the adjacent strata suggest free growth in nodules in the inertinitic interval 3812–3814 m depth may AUSTRALIAN JOURNAL OF EARTH SCIENCES 11 Figure 8. Backscattered electron image of a framboidal nodule fragment anomalously enriched in Ni, Co and As from Redback-2 3813.8 m depth and energy dispersive x-ray elemental maps from one framboid. The optical image under reflected light is shown in Figure 5h. unconsolidated mud. A closer look at the Ni–As–Co distri- Table 2. Pyrite–marcasite composition from the Hovea Member. bution in secondary electrons (Figure 8) confirmed the Element Median (mg/g) Standard deviation (n¼ 36) absence of gersdorffite (NiAsS) and revealed that metals Mn 3715 6260 are relatively enriched on framboidal edges and joints com- Co 25 146 Ni 147 350 posed of likely secondary diagenetic pyrite. The level of Cu 226 480 trace-metal concentration is above the Proterozoic and Zn 24 301 As 188 239 Phanerozoic average pyrite but comparable with the Se 31 30 Archean diagenetic pyrites (Large et al., 2014). Mo 19 16 Ag 2 9 Cd 1 1 Se–Pb-rich pyrite aggregates (mottled pyrite, RB2- Sb 12 20 3808.13). Abnormally high contents of Pb (0.4–2.4 wt%) Te 10 18 and Se (0.05–0.2 wt%), correlate positively with each other, Tl 2 3 Pb 114 588 and contain elevated Cu (0.14 wt%), Ni (0.6 wt%) and As Bi 3 6 (0.4 wt%), and depleted Bi and Te contents. The Se–Pb aggregates have been found at RB2-3808.13, 2 m below the shift in d C values and within the interval of shallow- indicator of potential acidification (Lounejeva et al., 2021) water environment interpretated from the gamma-reson- whereas atmospheric dust has been found to be an essential ance study. Pyrite in these aggregates acquired angular source of P, REE, Mn–Fe oxyhydroxide particles in both coastal shapes, and space between the pyrite crystals is rather and open ocean waters (Bayon et al., 2004;Greaves et al., filled with iron hydroxide than with sulfide and degraded 1999;Richon et al., 2018). Nenes et al. (2011)argued that organic matter (Figure 5g; Supplemental data). atmospheric acidification of aerosols is the prime mechanism producing soluble phosphorus from soil-derived minerals and Manganese-rich pyrite–marcasite from the EPMEI. The that these processes could promote formation of siderite–apa- LA-ICPMS analysis revealed a highly variable compositions of tite nodules. Whether acidification is related to the STLIP activ- pyrite–marcasite euhedral crystals from the EPMEI in both ity and the hypothesised associated acid rains (Black et al., boreholes (Figure 5i; Table 2;36 analyses). Marcasite trace- 2014), ocean acidification (Clarkson et al., 2015) or a marginal element contents are dominated by Mn (0.02–2.2 wt%; low dynamic environment is not yet clear. To understand median ¼ 3500 mg/g), with much lower amounts of other ele- whether the presence of iron bisulfides depleted in trace ele- ments, including Co and Ni. A characteristic of the Hovea ments within the mass extinction interval is incidental, an Member, Mn-rich marcasite in mudstone matrix and apatite ongoing study will include analysis of pyrite and marcasite within siderite nodules, could be an indirect indication of reported from the deeper marine Permian–Triassic sediments, acidified atmospheric aerosol. Formation of marcasite along e.g. the abyssal black shales at the Ubara section in Japan with pyrite favoured by pH drop has been considered an (Algeo et al., 2011;Lounejeva et al., 2021). 12 E. LOUNEJEVA ET AL. the last record of sponges and bryozoans at HO3-1983.67 Regional tectonic arrangements at the end of Permian and a 5‰ VPDB decline of d C values within the next 2.5 m To reconcile the inconsistencies between interpretation of at the top of the inertinitic interval. the depositional setting and geochemical parameters for The long-term anoxia in Neo Tethys preceding the the inertinitic interval, we consider the regional tectonics EPME, which has been inferred based on measurements of and invoke intensification of weathering and fast burial. framboidal pyrite diameters (5 ± 2 mm) in Hovea-3, may be Large et al. (2017) concluded that shales with high Ni, As, interpreted as ‘deep marine’ environments (Bond & Mo or Co, which are several orders of magnitude higher Wignall, 2010). The smaller framboids in Hovea 3 sediments than in this study, require a tectonic configuration that below the boundary, observed and analysed in this study, maximises weathering rates. The Permian Hovea Member are however localised within the 7 m interval along with metal-rich pyrite strata are coeval with sandstones contain- bryozoans and other fauna fossils or within a silty sand- ing Precambrian zircons likely sourced from the Yilgarn stone with some iron oxides contradicting the interpret- Craton (Cawood & Nemchin, 2000). Thus, the Perth Basin of ation of long-term anoxia. Our observations rather support the late Permian time could involve weathering of Ni–Co- shoaling or short-term upwelling of deeper anoxic/sulfidic rich Archean komatiites of the Yilgarn Craton and fluvial waters seeding some pyrite into sediments deposited near input carrying oxy-anionic metals such as As, whereas shore, a mechanism proposed by several authors to explain eventual shoaling of anoxic waters could promote forma- similar contradictions found around the PTB elsewhere tion of pyrite enriched in both transitional and oxi-anionic (Kershaw & Liu, 2015; Shen et al., 2011). In contrast, the metals. In contrast, the Triassic sequences, deposited RB2 sediments contain framboidal pyrite of highly variable mostly in a deeper marine oxygen-depleted (euxinic– size formed likely in an oxic–dysoxic marine-influenced anoxic) environment, lacking metal-enriched pyrite or sediments and probably eventually separated from the rest Precambrian detritus could be sourced from the Ni-poor of the basin. Pinjarra Orogen (Veevers, 2006; Veevers & Tewari, 1995). Conclusions and implications Does the Perth Basin contain a global geochemical Whole-rock and pyrite trace element data record dis- record of the EPME linked to STLIP activity? tinct changes in samples bridging the transition from The Hovea Member sediments display the prominent nega- the Permian to the Triassic in the Perth Basin. The pyrite tive carbon isotopic excursion of 7‰ VPDB across the PTB successfully records ocean chemistry changes over an (Lounejeva et al., 2021) coinciding with the regional interval of less than 20 Ma years. Sedimentary pyrite and whole-rock chemistry from this rearrangement. The d C (organic and carbonate) excur- interval may be used as a proxy for a shallow marine sions are characteristic of the Paleozoic–Mesozoic carbon environment during the EPME. cycle perturbation worldwide (Korte & Kozur, 2010) and Special care must be taken regarding petrography and have been linked to massive release of methane and car- geochemistry in all pyrite proxy studies (i.e. lessons bon dioxide owing to Siberian Traps volcanic intrusion into learned from Large et al., 2014, 2022, Gregory, 2020; coal measures (Shen et al., 2011) and carbonates (Burgess Gregory et al., 2015); virtually no sedimentary pyrite will et al., 2017). ever have more than 1 wt% Co, Ni or As. Any pyrite Spikes of high metal contents preceding the EPMEI are with such concentrations is not sedimentary but may evident in the Hovea Member bulk sediments and pyrite. be diagenetic, if not hydrothermal. High toxic metal contents, i.e. Hg, Co and As, were also The whole-rock and pyrite geochemistry of the linked to STLIP ash loading and were postulated in northern Permian/Triassic boundary section in borehole Redback- Pangaea as the cause for the extinction of siliceous sponges 2, Perth Basin, supports a change from a shallow and in the ocean (Grasby et al., 2015). An exceptionally high Ni, relatively oxygenated latest Permian to a deeper early Co and As content in the Hovea Member upper Permian Triassic anoxic (euxinic) marine depositional environ- sedimentary pyrite can also be explained by regional weath- ment. The shallow deposition setting in the Perth Basin ering input and diagenetic overprint rather than a global was metal-enriched well before the late Permian extinc- mechanism of metal delivery. However, a temporal link with tion onset. a distant Ni source cannot be excluded, as global dispersion Manganese, copper, zinc and cadmium deconvolution and loading of Ni-rich aerosol particles into the Panthalassic from the matrix should be considered with caution. Ocean (Li et al., 2021) have been proposed and related to proliferation of methanogen Methanosarcina, which resulted in an abrupt anoxia expansion and the EPME (Rothman et al., Acknowledgements 2014). Moreover, the highest content of Hg 437 ng/g and We thank the GSWA core library for assistance with sample collection. the first decline d C per 3‰ VPDB have been identified org We thank A. Cuison and M. Chapple-Smith for sample preparation, in Hovea-3 sediments at 1983.48 m depth (Sial et al., 2020), S. Gilbert for technical assistance with the LA-ICP-MS analysis and at the inception of the EPMEI. These changes occur above K. Goemann for help with SEM work. We also appreciate the AUSTRALIAN JOURNAL OF EARTH SCIENCES 13 constructive and critical comments from Ian Metcalfe and an anonym- Bond, D. P. G., & Wignall, P. B. (2010). Pyrite framboid study of marine Permian–Triassic boundary sections: A complex anoxic event and its ous reviewer. relationship to contemporaneous mass extinction. Geological Society of America Bulletin, 122(7–8), 1265–1279. https://doi.org/10.1130/ B30042.1 Disclosure statement Burgess, S. D., Muirhead, J. D., & Bowring, S. A. (2017). Initial pulse of No potential conflict of interest was reported by the author(s). Siberian Traps sills as the trigger of the end-Permian mass extinc- tion. Nature Communications, 8(1), 164. art. https://doi.org/10.1038/ s41467-017-00083-9 Funding Cannell, A., Blamey, N., Brand, U., Escapa, I., & Large, R. (2022). A revised sedimentary pyrite proxy for atmospheric oxygen in the This work was supported by an Australian Research Council Discovery Paleozoic: Evaluation for the Silurian–Devonian–Carboniferous (ARC) grant to R. Large [DP150102578]. K. Grice acknowledges the ARC period and the relationship of the results to the observed bio- for DORA and DP grants for this work. sphere record. Earth-Science Reviews, 231, 104062. https://doi.org/10. 1016/j.earscirev.2022.104062 Cao, C., Love, G. D., Hays, L. E., Wang, W., Shen, S., & Summons, R. E. ORCID (2009). Biogeochemical evidence for euxinic oceans and ecological disturbance presaging the end-Permian mass extinction event. E. Lounejeva http://orcid.org/0000-0002-2462-8623 Earth and Planetary Science Letters, 281(3–4), 188–201. https://doi. J. A. Steadman http://orcid.org/0000-0003-4679-3643 org/10.1016/j.epsl.2009.02.012 R. R. Large http://orcid.org/0000-0003-0012-0101 Cawood, P. A., & Nemchin, A. A. (2000). Provenance record of a rift K. 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Australian Journal of Earth Sciences – Taylor & Francis
Published: Jul 4, 2023
Keywords: laser ablation; LADR; EPMEI; LPMEI; marginal; shallow marine; Siberian Traps Large Igneous Province; ( Nodosaria) Protonodosaria tereta (Crespin 1958); acidification; anoxia
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