*Manuscript Click here to view linked References 1 Accepted for publication in Earth and Planetary Science Letters 40 Ar/39Ar age of the Lake Saint Martin impact structure (Canada) – 2 Unchaining the Late Triassic terrestrial impact craters 3 Martin Schmieder1,2*, Fred Jourdan2, Eric Tohver1 and Edward A. Cloutis3 1 School of Earth and Environment, University of Western Australia, 35 Stirling Highway, Crawley, WA 6009, Australia. 4 5 6 7 8 9 2 Western Australian Argon Isotope Facility, Department of Applied Geology and JdL Centre, Curtin University, GPO Box U1987, Perth, WA 6845, Australia. 3 Planetary Spectrophotometer Facility, Department of Geography, University of Winnipeg, Canada. *corresponding author. Tel.: 0061 434 808 655 – Email: martin@suevite.com. 10 11 12 Abstract – New 40Ar/39Ar dating of impact-melted K-feldspars and impact melt rock 13 from the ~40 km Lake Saint Martin impact structure in Manitoba, Canada, yielded 14 three plateau ages and one mini-plateau age in agreement with inverse isochron ages 15 for the K-feldspar melt aliquots and a minimum age for a whole-rock impact melt 16 sample. A combination of two plateau ages and one isochron age, with a weighted 17 mean of 227.8 ± 0.9 Ma [± 1.1 Ma; including all sources of uncertainty] (2σ; MSWD 18 = 0.52; P = 0.59), is considered to represent the best-estimate age for the impact. The 19 concordant 20 rocks in the eastern crater moat domain and the partially melted Proterozoic central 21 uplift granite, suggest that the new dates accurately reflect the Lake Saint Martin 22 impact event in the Carnian stage of the Late Triassic. With a relative error of ± 0.4% 23 on the 40Ar/39Ar age, the Lake Saint Martin impact structure counts among the most 24 precisely dated impact structures on Earth. The new isotopic age for Lake Saint 25 Martin significantly improves upon earlier Rb/Sr and (U–Th)/He results for this 26 impact structure and contradicts the hypothesis that planet Earth experienced the 27 formation of a giant ‗impact crater chain‘ during a major Late Triassic multiple 28 impact event. 40 Ar/39Ar ages for the melted K-feldspars, derived from impact melt 29 Keywords: Lake Saint Martin; 40Ar/39Ar dating; impact melting; K-feldspar; Triassic; Carnian; 30 multiple impact event. 5,896 words, 1 Table, 7 Figs., 1 supplementary Table. 31 1. INTRODUCTION AND GEOLOGIC BACKGROUND 32 1.1. The Lake Saint Martin impact structure, Manitoba 33 The ~40 km-diameter Lake Saint Martin impact structure in the Interlake Region of southern 34 Manitoba (McCabe and Bannatyne, 1970; Bannatyne and McCabe, 1984; Grieve, 2006; Fig. 1) 35 is one of the largest meteorite impact structures in North America. Target rocks comprise 36 Paleoproterozoic (~2.4 Ga) granites of the Superior Province of the Canadian Shield overlain by 37 ~200-400 m of Ordovician to Devonian sedimentary rocks that build up the northeastern margin 38 of the Paleozoic intracratonic Williston Basin (e.g., Grieve, 2006). The shocked and partially 39 melted basement granite is exposed in the central uplift of the impact structure. The annular 40 crater moat is filled with a sequence of impactites including carbonate-dominated and granitic 41 lithic impact breccias, impact melt rocks, and suevitic breccias occasionally summarized under 42 the vernacular term ‗Saint Martin Series‘ (McCabe and Bannatyne, 1970; Simonds and McGee, 43 1979; Grieve, 2006). Shock metamorphic effects in these rocks and minerals led McCabe and 44 Bannatyne (1970) to conclude that Lake Saint Martin is an impact structure, while Currie (1970) 45 still considered it a volcanic cryptoexplosion structure. Largely concealed by post-impact Middle 46 Jurassic intra-crater red beds and evaporites of the Williston Basin, up to ~30 m of Pleistocene 47 glacial drift and the waters of Lake Saint Martin, the impact structure is considered one of the 48 best preserved larger complex terrestrial impact craters formed in a layered, crystalline- 49 sedimentary target. Post-impact evaporitic sediments have preserved large parts of the impact 50 crater and its impact breccia lens from erosion (McCabe and Bannatyne, 1984). However, due to 51 the sedimentary cover surficial outcrop of primary impactites is rather scarce. Numerous 52 drillings since the 1970s revealed the subsurface geology and specific rocks of the Lake Saint 53 Martin impact structure. The composition of the Lake Saint Martin impactor is unknown, but 54 very low concentrations of siderophile elements in the melt rocks (Göbel et al., 1980; Palme, 55 1982; Reimold et al., 1990) suggested a differentiated projectile, possibly an achondrite. 56 57 1.2. 58 Stratigraphically, the Lake Saint Martin impact can be placed between the Devonian and the 59 Middle Jurassic. The youngest shock-deformed sedimentary rocks most likely belong to the 60 Devonian Ashern and Winnipegosis Formations of the northeastern Williston Basin (e.g., 61 Rosenthal, 1988); the evaporitic deposits of the Amaranth Formation that overlie the impact 62 structure are of Middle Jurassic age (McCabe and Bannatyne, 1984). Previous dating of the Lake 63 Saint Martin impact structure employed a wide range of techniques but has not yielded any 64 satisfactory age so far. Early results yielded rather imprecise K/Ar apparent ages of 200 ± 25 and 65 250 ± 25 Ma (McCabe and Bannatyne, 1970) and a Rb/Sr apparent age of 223 ± 32 Ma (Reimold 66 et al., 1990; recalculated from 219 ± 32 Ma according to the revised 67 Nebel et al., 2011). Despite the large error on the age (28%) and the notorious problems 68 associated with this technique in dating impact craters (Jourdan et al., 2009), the Rb/Sr age of 69 Reimold et al. (1990) is currently accepted as the ‗official‘ age for the impact in most impact 70 crater listings in the literature; a slightly modified age value of 220 ± 32 Ma (as also given in 71 Grieve, 2001) is listed in the Earth Impact Database (2013). Apatite and zircon fission track 72 dating gave an age of 208 ± 14 Ma (Kohn et al., 1995). Additional dating attempts using the low- 73 temperature (U–Th)/He technique on apatite and zircon separated from melt rocks resulted in 74 scattered ages with two apparent age peaks around ~214 Ma and ~234 Ma (Wartho et al., 2009; 75 2010). A strontium and sulfur isotopic study of the post-impact evaporites favored an age around Previous age determinations for the Lake Saint Martin impact 87 Rb decay constant of 76 the Devonian/Carboniferous boundary (~360 Ma) for the impact (Leybourne et al., 2007), at 77 odds with the previous isotopic dating results. Clearly, despite several dating attempts using 78 different techniques, the age of the Lake Saint Martin impact still remains poorly constrained. 79 80 1.3. 81 Together with the ~100 km Manicouagan impact structure in Québec/Canada, the ~9 km Red 82 Wing Creek impact structure in North Dakota/USA, the ~40 km Rochechouart impact structure 83 in France, the ~20 km Obolon impact structure in Ukraine, as well as possibly the ~12 km Wells 84 Creek impact structure in Tennessee/USA and the ~3.2 km Newporte impact structure in North 85 Dakota/USA, the Lake Saint Martin impact structure has been considered the western member of 86 a giant, ~4,500 km-long, ‗impact crater chain‘ along the 22.8° paleolatitude on the Late Triassic 87 Earth (Spray et al., 1998). All of these impact structures, plotted on a paleoglobe at ~214 Ma, lie 88 on reconstructed great circles of identical declination (37.2°). Taking into account the 89 overlapping isotopic and stratigraphic age data available in 1998 and tectonic plate 90 reconstructions for the Late Triassic, Monte Carlo simulations suggested that a random array for 91 the three largest of these impact structures – Manicouagan, Rochechouart, and Lake Saint Martin 92 – was highly unlikely (Spray et al., 1998). The idea was that the proposed multiple impact 93 scenario could have occurred similar to the ‗string-of-pearls‘-style impact of the tidally 94 fragmented comet Shoemaker-Levy 9 on Jupiter in the summer of 1994 (e.g., Crawford et al., 95 1994), within a short period of time. The Late Triassic multiple impact theory was soon vividly 96 discussed in the scientific literature (Kent, 1998; Melosh, 1998; Walkden et al., 2002; Tanner et 97 al., 2004; Carporzen and Gilder, 2006; Grieve, 2006; Zivkovic and Gosnold, 2007; Schmieder Lake Saint Martin as a member of a giant terrestrial impact crater chain? 98 and Buchner, 2008; Schmieder et al., 2010; 2012; Jourdan et al., 2012) and scientific reviews 99 (VanDecar, 1998; Monastersky, 1998; Sankaran, 1999). This study presents a set of new 100 40 Ar/39Ar ages for aliquots of impact-melted K-feldspars and impact melt rocks from different 101 domains within the Lake Saint Martin impact structure. The new isotopic ages will demonstrate 102 that the Lake Saint Martin impact occurred millions of years before the Manicouagan and 103 Rochechouart impacts and that none of the impacts grouped together into an alleged crater chain 104 occurred synchronously. 105 106 2. SAMPLES AND ANALYTICAL METHODS 107 2.1. Impact melt specimens and petrography 108 Whole-rock chips of impact melt rock from the crater moat domain of the Lake Saint Martin 109 impact structure, as well as chips of impact-melted K-feldspars separated from the melt rock and 110 the impact-metamorphosed Precambrian basement granite exposed in the central uplift (Fig. 1) 111 were used for laser step-heating 40Ar/39Ar dating. This approach was chosen to gain isotopic ages 112 from different types of impact melt lithologies representative of different portions of the impact 113 structure. We direct the reader to Simonds and McGee (1979), Reimold et al. (1990) and Grieve 114 (2006) for summaries of the composition, petrography, and geochemistry of the impact melt 115 rocks and breccias at Lake Saint Martin. The brownish to reddish, fine-grained crystalline impact 116 melt rocks (Fig. 2A-B; typically containing ~3.2-3.9 wt% K2O; Grieve, 2006) are moderately to 117 intensely altered and have a matrix of plagioclase, alkali feldspar, pyroxene (augite), quartz, and 118 Fe-Ti oxides. Groundmass crystals are typically ~20-100 µm in crystal length. Larger grains of 119 plagioclase (oligoclase and andesine) commonly exhibit a checkerboard texture, whereas 120 shocked quartz has been partially transformed into aggregates of ballen quartz with marginal 121 melting textures and reaction rims (compare Grieve, 2006; Jourdan et al., 2010). The impact- 122 metamorphosed basement granite (Fig. 2C-D) contains fluidal-vesicular domains of feldspar 123 melt of variable composition with vugs locally lined by adularia. Quartz in the shocked granite 124 mainly occurs in the form of ballen silica, and biotite flakes have been decomposed into 125 microcrystalline opaques. Representative specimens were analyzed using an optical polarization 126 microscope and a VEGA3 TESCAN scanning electron microscope (SEM) equipped with an X- 127 Max 50 silicon drift detector and an energy-dispersive X-ray spectroscopy system at the Centre 128 for Microscopy, Characterisation and Analysis (CMCA) at the University of Western Australia 129 campus. Backscattered electron images were acquired using an acceleration voltage of 15 kV. 130 40 Ar/39Ar dating 131 2.2. 132 40 133 feldspar from the crushed rock (grain size ~500-800 µm in diameter) were carried out at the 134 Western Australian Argon Isotope Facility, Curtin University. We performed analyses on two 135 single-grain aliquots of impact-melted K-feldspar extracted from a fluidal-vesicular impact melt 136 rock recovered from the eastern sector of the impact crater moat (samples LSM-1A and LSM- 137 1B); three particles of melted K-feldspar from the shocked and partially melted basement granite 138 collected in the central uplift domain (samples LSM-2A, LSM-2B and LSM-2C); one whole- 139 rock chip of a moderately altered, brownish impact melt rock (sample LSM-3); and a whole-rock 140 chip (~200 µm in diameter) of an intensely altered, reddish melt rock (sample LSM-4; see 141 Jourdan et al., 2010), which had been irradiated and analyzed in an earlier batch of aliquots. The Ar/39Ar laser step-heating experiments on impact melt rock chips and separates of melted K- 142 melt rock samples were leached in 5N HF for 2 minutes to remove alteration phases on the 143 surface and along fissures (e.g., Baksi, 2007). 144 The samples were loaded in multi-pit aluminum discs along with the Fish Canyon sanidine (FCs, 145 age: 28.294 ± 0.037 Ma; Jourdan and Renne, 2007; Renne et al., 2011) used as a neutron fluence 146 monitor, Cd-shielded in order to reduce isotopic interferences, and irradiated for 40 hours in the 147 TRIGA (Denver) nuclear reactor (central position, specific J-values given in Table-Annex 1). 148 After irradiation, the samples were step-heated using a 110 W Spectron Laser Systems 149 instrument, with a continuous Nd-YAG (IR; 1064 nm) laser rastered (1 minute; beam diameter 150 350 µm) over the single-grain aliquots, moved on a x/y/z-mobile sample stage. The gas was 151 purified in a stainless steel extraction line using one GP50 and two AP10 SAES getters. Argon 152 isotopes were measured in static mode using a MAP 215-50 mass spectrometer with a Balzers 153 SEV 217 electron multiplier using nine to ten cycles of peak hopping. The argon results were 154 corrected for mass discrimination, monitored using an automatic air pipette, and provided mean 155 values of 1.004293 ± 0.0025 per dalton (atomic mass unit). The correction factors for interfering 156 isotopes were (39Ar/37Ar)Ca = 7.06 ∙ 10-4 (± 7%), (36Ar/37Ar)Ca = 2.81 ∙ 10-4 (± 3%) determined on 157 CaF2, as well as (40Ar/39Ar)K = 6.76 ∙ 10-4 (± 10%) and (38Ar/39Ar)K = 1.24 ∙ 10-2 (± 32%) 158 measured on K-Fe glass. Blanks were monitored every 3 to 4 steps and typical 40Ar blanks range 159 from 1 ∙ 10-16 to 2 ∙ 10-16 mol. All argon isotopic data are given in the supplementary files (Table- 160 Annex 1). 161 2011) and the LabView-environment Argus program by M.O. McWilliams, the ArArCALC 162 software (Koppers, 2002), and Isoplot 4.1 written by K. R. Ludwig (Berkeley Geochronology 163 Center). All errors in this study are ± 2σ, unless otherwise noted. A plateau is defined by 70- 164 100%, a mini-plateau by 50-70% of the total 40 Ar/39Ar ages were calculated using the K decay constants of Renne et al., (2010; 39 Ar released in at least 5 consecutive steps with 165 ages that overlap within 2σ error limits, and define a probability (P-value) of ≥0.05 using a χ² 166 (chi square) test (e.g., Baksi, 2007). Errors on the age of the monitor and on the decay constants 167 are combined with the internal uncertainties and are provided in brackets (e.g., [1.0] Ma). 168 169 3. 40 170 3.1. Melt rock-hosted K-feldspar 171 40 172 plateau age of 226.7 ± 2.4 Ma (2σ; MSWD = 0.78; P = 0.66; 84% of 173 This aliquot did not develop a statistically representative isochron due to a low spreading (S; 174 Jourdan et al., 2009) value. Except for a single step, all data points in the inverse isochron 175 diagram cluster near the radiogenic axis (compare Schmieder and Jourdan, 2013) and resulted in 176 an age of 227.2 ± 1.5 Ma (2σ; MSWD = 0.79; P = 0.64; 40Ar/36Ar intercept = 288 ± 13; S-value 177 = 31%; Fig. 3B). The second K-feldspar melt aliquot, LSM-1B, yielded a mini-plateau apparent 178 age of 227 ± 5 Ma (2σ; MSWD = 1.70; P = 0.15; 63% of 39Ar released; Fig. 3C) for the first five 179 steps within a tilde-shaped, disturbed age spectrum. The mini-plateau and total fusion apparent 180 ages of this sample are concordant within error with the plateau age obtained for LSM-1A which 181 might suggest that the perturbed spectrum is an effect of 39Ar recoil redistribution induced by the 182 irradiation process (Table 1). The inverse isochron for LSM-1B yielded an age of 228 ± 6 Ma 183 (MSWD = 1.73; P = 0.16; 184 40 185 Mark et al., 2011) within error. 186 Ar/39Ar RESULTS AND INTERPRETATION Ar/39Ar step-heating analysis of the impact-melted K-feldspar LSM-1A yielded a well-defined 40 39 Ar released; Fig. 3A). Ar/36Ar intercept = 289 ± 20; S = 70%; Fig. 3D). The isochron Ar/36Ar intercept values for LSM-1A and LSM-1B are atmospheric (~298.6; Lee et al., 2006; 187 3.2. 188 The aliquots of impact-melted K-feldspars separated from the central uplift granite yielded a 189 plateau age of 227.0 ± 1.2 Ma (2σ; MSWD = 1.00; P = 0.46; 84% of 39Ar) for sample LSM-2A 190 (Fig. 4A). The inverse isochron for this aliquot, including degassing step 1 (with a step apparent 191 age concordant with the plateau age), yielded a slightly sub-atmospheric 192 value of 288 ± 8 and an isochron age of 227.9 ± 1.4 Ma (MSWD = 0.79; P = 0.71; S = 61%; 193 Fig. 4B). The sub-atmospheric ratio might be due to thermally activated isotopic fractionation 194 upon melt emplacement, or fluid circulation after the impact. Whatever the cause for this effect, 195 the isochron-derived age for sample LSM-2A, directly accounting for the initial 196 below ~298.6 (Lee et al., 2006), is here regarded as the more accurate age value for sample 197 LSM-2A (compare, e.g., Jourdan et al., 2008). Sample LSM-2B gave a plateau age of 228.1 ± 198 1.4 Ma (2σ; MSWD = 1.40; P = 0.18; 73% of 39Ar; Fig. 4C). Data points for this aliquot cluster 199 near the radiogenic axis and fail to provide an isochron (Fig. 4D). A third feldspar particle picked 200 from the granite, LSM-02C, yielded a disturbed and tilde-shaped age spectrum from which no 201 plateau or mini-plateau age could be extracted (Fig. 4E). Individual steps in the high-temperature 202 extraction range gave older apparent ages of up to ~260 Ma, suggesting partial inheritance of 203 40 204 Jourdan et al., 2007). No isochron result was obtained for aliquot LSM-02C (Fig. 4F). K-feldspar from central uplift granite 40 Ar/36Ar intercept 40 Ar/36Ar ratio Ar* from an incompletely degassed Precambrian precursor feldspar in this sample (e.g., 205 206 3.3. 207 The moderately altered, brownish impact melt rock chip LSM-3 did not yield a plateau in a 208 disturbed, tilde-shaped age spectrum, with younger step ages (~180-200 Ma) in the low- and Impact melt rock 209 high-temperature extraction range and older apparent ages of ~220-230 Ma in the mid- 210 temperature steps (Fig. 5A). This age spectrum is similar to some of the previous age spectra 211 obtained on impact melt rocks from Lake Saint Martin (Schmieder et al., 2012; an unpublished 212 age spectrum for a drill core-derived melt rock sample, acquired with W.H. Schwarz, M. Trieloff 213 and E. Buchner at the Ar laboratory at the University of Heidelberg, Germany) and other spectra 214 for terrestrial impact structures in which hump- and tilde-shapes have been attributed to 215 alteration effects, such as the Dhala impact structure in India (Pati et al., 2010) or the 216 Söderfjärden impact structure in Finland (Schmieder et al., 2014a). When alteration is indeed 217 responsible for hump- and tilde-shaped spectra, the maxima of such age spectra must be strictly 218 considered a minimum age for the formation of the melt rock (e.g., Buchner et al., 2009; 219 Jourdan, 2012). We note that the apparent minimum age for melt rock sample LSM-3 is notably 220 close to the statistically well-defined plateau and isochron ages for the melt rock- and granite- 221 derived K-feldspar melt aliquots. The K/Ca ratio for LSM-3 gave values between ~1 and ~3 222 suggesting no major crystallization of secondary K2O-rich minerals. No isochron could be 223 produced for this altered impact melt rock (Fig. 5B). 224 In contrast to the moderately altered melt rock specimen LSM-3, the intensely altered melt rock 225 sample LSM-4 yielded a distinct staircase-shaped apparent age spectrum. Step ages in the low- 226 temperature extraction range of this spectrum lie around ~140 Ma and gradually increase until 227 they reach a step-age maximum at ~209 Ma before the age values drop again (Fig. 5C). We note 228 that the minimum age derived from the oldest apparent step ages of this age spectrum is ~15- 229 20 Myr younger than the minimum age for the less altered melt rock aliquot LSM-3. The K/Ca 230 ratio varies between ~7 and ~18 suggesting the presence of abundant secondary K2O-rich 231 minerals relative to sample LSM-3. Such an age spectrum likely reflects a mixture between Ar 232 loss and the recrystallization of alteration minerals. As for LSM-3, no isochron was obtained for 233 melt rock sample LSM-4 (Fig. 5D). 234 A summary of the 235 Saint Martin impact structure is presented in Table 1. 40 Ar/39Ar ages and associated statistics for all melt samples from the Lake 236 237 4. DISCUSSION 238 4.1. Age of the Lake Saint Martin impact 239 This study presents the first systematic set of 240 Martin impact structure, obtained from different mineral-melt and whole-rock impact melt 241 specimens. It thereby improves upon earlier dating attempts that resulted in imprecise (and 242 statistically unverifiable) whole-rock K/Ar and Rb/Sr ages (cf. discussion in Jourdan et al., 2009 243 and Jourdan, 2012 about the suitability of the Rb/Sr method for the dating of impact events). The 244 more recent Rb/Sr apparent age of 219 [223] ± 32 Ma obtained for impact melt rocks by 245 Reimold et al. (1990) has been considered the most precise and accurate age for the Lake Saint 246 Martin impact for more than two decades; however, the rather low precision of this result, along 247 with the relevance of this impact structure for a potential giant crater chain, warranted further 248 investigations. Here we present a set of concordant plateau, mini-plateau, and inverse isochron 249 ages obtained for the impact-melted K-feldspars separated from impact melt rock and the 250 partially melted central uplift granite. A combination of two plateau ages (aliquots LSM-1A and 251 LSM-2B) and one inverse isochron age (LSM-2A; taking into account the sub-atmospheric 252 40 253 227.8 ± 0.9 Ma [± 1.1 Ma] (2σ; MSWD = 0.52; P = 0.59; the number in brackets includes the 40 Ar/39Ar ages for the well-preserved Lake Saint Ar/36Ar intercept of 288 ± 8) yields a statistically compelling weighted mean age of 254 full external error). This early Late Triassic mean age is considered as the most precise and 255 accurate age currently available for the Lake Saint Martin impact. As mini-plateau ages are 256 potentially inaccurate (e.g., Jourdan et al., 2009), we did not include the 40Ar/39Ar result for the 257 impact-melted K-feldspar LSM-1B in the final age calculation; however, this mini-plateau age is 258 within error also equivalent with the plateau and isochron ages obtained on the other K-feldspar 259 melt aliquots. The internal consistency of the 260 reproduction of coeval apparent ages from different types of impact melt lithologies gained from 261 two different sample localities across the impact structure provides good confidence that these 262 matching ages accurately reflect the Lake Saint Martin impact. With a relative error on the age of 263 only ± 0.4% (all uncertainties included), Lake Saint Martin now represents one of the most 264 precisely dated impact structures on Earth (compare impact crater ages in the reviews by Jourdan 265 et al., 2009; 2012 and references therein). A summary of all measured 266 plateau and inverse isochron ages, along with the recommended age for the impact, is presented 267 in Fig. 6. Further dating of impact melt samples from natural outcrop and drill cores into the 268 impact structure will be desirable to create an even more extended isotopic data set for the Lake 269 Saint Martin impact in the future (compare, e.g., Buchner et al., 2010). 270 According to the latest International Chronostratigraphic Chart published by the International 271 Commission on Stratigraphy (Cohen et al., 2013), the new 40Ar/39Ar age of 227.8 ± [1.1] Ma for 272 the Late Triassic Lake Saint Martin impact corresponds within error to the ~227 Ma 273 Carnian/Norian boundary. However, Lucas et al. (2012) pointed out that the base of the Norian is 274 probably several million years younger and lies around ~220 Ma based on an extensive set of 275 radioisotopic data. This younger age would place the Lake Saint Martin impact well within the 276 Carnian (lasting from ~237 Ma to ~220 Ma). The strong reverse magnetization in the Lake Saint 40 Ar/39Ar dating results and the independent 40 Ar/39Ar plateau, mini- 277 Martin melt rocks (Coles and Clark, 1982) is in agreement with a number of reversed 278 magnetochrons (within a range of chrons E1r to E13r) during the Carnian time stage (Kent et al., 279 1995; Lucas et al., 2012). 280 281 4.2. 282 The systematic study of a set of different impact melt samples from Lake Saint Martin helps with 283 the interpretation and understanding of ‗alteration age‘ spectra and minimum ages derived from 284 40 285 plateau and isochron ages for the Lake Saint Martin impact are within the range of the ‗minimum 286 age‘ of ~220-230 Ma for the impact melt rock sample LSM-3 and results from Schmieder et al. 287 (2012) who reported a similar minimum age of ~225 Ma for an additional impact melt rock 288 specimen. In this case, the minimum age for the moderately altered impact melt rock sample 289 LSM-3 closely approaches the statistically more robust plateau and isochron ages. In contrast, 290 the intensely altered impact melt rock LSM-4 yielded apparent step ages no older than ~209 Ma, 291 which are still notably younger than the age of ~228 Ma determined for the impact in this study. 292 Such alteration age spectra are generally difficult to interpret unless more robust isotopic ages 293 (e.g., a set of concordant 40Ar/39Ar plateau ages from fresh or less altered impact melt specimens; 294 or statistically compelling U/Pb ages from melt-grown zircons) and stratigraphic age constraints 295 are available. Minimum impact ages inferred from step-age maxima in 40Ar/39Ar age spectra can 296 be considerably – in cases up to several hundred Myr – younger than the real formation age of an 297 impact melt rock. This effect is exemplified by the ≥1.7 Ga Dhala impact structure in India that Implications for rock alteration effects and low-temperature geochronometers Ar/39Ar step-heating analysis, in particular bell-shaped and/or tilde-shaped age spectra. The 40 Ar/39Ar ages of ~1.0 Ga, whereas field geologic relationships 298 produced minimum apparent 299 indicate a much older, Paleoproterozoic, minimum age for the impact (Pati et al., 2010). 300 The concordant plateau, mini-plateau and inverse isochron 40Ar/39Ar ages obtained in this study, 301 moreover, critically question the indiscriminate use of age data obtained from low-temperature 302 geochronometers, such as the (U–Th)/He dating method (e.g., Farley, 2002; Reiners, 2005) that 303 records thermal events at closure temperatures of ~200°C for zircon and as low as ~60°C for 304 apatite. None of the previous (U–Th)/He age peaks at ~180 Ma, ~214 Ma and ~234 Ma for 305 zircon and apatite grains recovered from impact melt rocks from Lake Saint Martin (Wartho et 306 al., 2009; 2010) have reliably identified the age of the impact within error. According to Kohn et 307 al. (1995), rocks in the Williston Basin have been overprinted by an Eocene thermal event that 308 caused the partial resetting of low-temperature geochronometers, such as apatite fission track and 309 (U–Th)/He. The cooling of larger impact craters and long-lived hydrothermal activity may have 310 an additional effect on isotopic systems with low closure temperatures. Recent 40Ar/39Ar results 311 for the ~23 km Lappajärvi impact structure in predominantly crystalline rocks of Finland 312 suggested comparatively slow crater cooling over ~0.6-1.6 Myr (Schmieder and Jourdan, 2013). 313 However, because of the higher amounts of subsurface water, porosity, and permeability in 314 sedimentary targets and water-promoted convective cooling (e.g., Kirsimäe et al., 2002), the 315 Lake Saint Martin crater may have cooled considerably faster. This ‗crater cooling lag‘ would 316 not explain, for example, the apparent zircon and apatite (U–Th)/He age clusters around ~214 317 Ma and ~180 Ma, respectively. So far, the (U–Th)/He technique has been applied to twelve 318 impact structures (e.g., Wartho et al., 2012a), from which only one, the ~7 km Wetumpka impact 319 structure in Alabama/USA (Wartho et al., 2012b), yielded a subset of apparent ages that are 320 consistent within uncertainty with biostratigraphic ages. Our understanding of the applicability of 321 the (U–Th)/He to impact crater dating is currently at an early stage. Inaccurate results prompt us 322 to advise caution in using this technique to date impact events without any robust age constraints. 323 Extensive testing and calibration of the method against well-dated (impact melt-hosted) mineral 324 specimens is required until we fully understand what constitutes a ‗valid‘ (U–Th)/He impact 325 crater age, especially with respect to the potential effects of shock metamorphism on the 326 retention and diffusion of He in zircon (e.g., van Soest et al., 2010). Some of the previous results 327 were compromised and of doubtful geological significance, either reflecting impact-induced 328 crustal uplift and slow crater cooling (Biren et al., 2012), post-impact thermal heating and 329 resetting not related to the impact (Wartho et al., 2010; van Soest et al., 2011), or the proposed 330 impact age was based on statistically invalid dating results (e.g., Young et al., 2013). 331 332 4.3. 333 To reliably assess the Late Triassic multiple impact theory proposed by Spray et al. (1998), 334 according to which several impact events occurred virtually synchronously, narrow error ranges 335 associated with the individual impact ages are crucial (see impact timing scheme in Fig. 7). At 336 least two of the impacts involved in the postulated scenario, Rochechouart in France and Obolon 337 in Ukraine, were previously dismissed based on their non-synchronous ages (Schmieder and 338 Buchner, 2008; Schmieder et al., 2010). The age of the ~100 km Manicouagan impact structure 339 in Québec has been precisely determined at 215.56 ± 0.05 Ma (Ramezani et al., 2005) and 214 ± 340 1 Ma (Hodych and Dunning, 1992) using U/Pb dating of impact melt-grown zircons. 341 The ~40 km Rochechouart impact structure in France was previously dated at an 40Ar/39Ar age of 342 214 ± 8 Ma (Kelley and Spray, 1997), obtained from UV laser ablation spots in the matrix of A geochronologic appraisal of the Late Triassic multiple impact hypothesis 343 melt-bearing pseudotachylitic breccia veins. However, these melt veins are known to contain 344 considerable amounts of undigested Precambrian to Paleozoic feldspar clasts and hydrothermal 345 fillings (Reimold et al., 1987); moreover, spot fusion apparent ages within a range between 346 ~230 Ma and ~1.7 Ga and an isochron 347 1997) indicated contamination by extraneous argon. The age for the Rochechouart impact was 348 recently revised to 202.8 ± 2.2 Ma (Schmieder et al., 2010) obtained from two 40Ar/39Ar plateau 349 ages for K-feldspar from an impact-metamorphosed gneiss. The other candidate craters for the 350 Triassic ‗crater chain‘ have only been imprecisely dated. The ~20 km marine Obolon impact 351 structure in Ukraine (Gurov et al., 2009) had earlier been estimated at a stratigraphic age of 215 352 ± 25 Ma (Masaitis et al., 1980; Spray et al., 1998), but K/Ar dating of the Obolon impact glass 353 and melt rock gave a Jurassic apparent age of 169 ± 7 Ma (Masaitis, 1999; Valter et al., 1999; 354 Gurov et al., 2009). A simple paleogeographic test further supports a Jurassic maximum age for 355 the Obolon impact structure; only from the Early Jurassic onward did the paleoenvironmental 356 conditions in the Donets Graben of the Ukrainian Shield change from continental sedimentation 357 into a marine environment and provided the setting for the submarine Obolon impact (Schmieder 358 and Buchner, 2008). The age of the ~9 km Red Wing Creek impact structure in the Williston 359 Basin of North Dakota is stratigraphically constrained to roughly ~200-220 Ma (Koeberl et al., 360 1996). Other loose stratigraphic age estimates for Red Wing Creek are 200 ± 25 Ma (Gerhard et 361 al., 1982) and 200 ± 5 Ma (Grieve, 1991), however, no fresh impact melt lithologies are known 362 from this impact site that could be used for more precise and accurate isotopic dating. Within the 363 extended list of potential craters within the suspected multiple impact system (Spray et al., 364 1998), the ~3 km Newporte impact structure in North Dakota has a Cambrian stratigraphic age of 365 ~500 Ma (Koeberl and Reimold, 1995), which is in conflict with the Late Triassic multiple 40 Ar/36Ar intercept value of >500 (Kelley and Spray, 366 impact scenario. The age of the ~12 km Wells Creek impact structure in Tennessee is poorly 367 known and given as 200 ± 100 Ma (Grieve, 2001). 368 From a geochronologic perspective, the refined 40Ar/39Ar age of ~228 Ma for Lake Saint Martin 369 demonstrates that the Obolon, Rochechouart, Manicouagan and Lake Saint Martin impact events 370 were far from synchronous. At least ~10 Myr, and up to >40 Myr, lie between each of the impact 371 events (Fig. 7). This also rules out any potential connection between the postulated large-scale 372 multi-impact scenario and extinction events during the Triassic (e.g., Benton, 1988; Hallam and 373 Wignall, 1997; Sephton et al., 2002; Tanner et al., 2004). 374 375 4.4. 376 In addition to the time constraints gained from isotopic dating, the compositions of the respective 377 impactors can be used as an additional argument for or against a cosmic combination strike. We 378 refer to Goderis et al. (2012), Koeberl et al. (2012) and Koeberl (2014) for recent reviews on the 379 identification of impactor signatures in impactites. The proposed Late Triassic multiple impacts 380 should, thus, also be appraised with regards to their potential impactor signatures. No conclusive 381 impactor traces, with siderophile elements below detection limit, could be gained from the 382 impact melt rocks at Manicouagan (Palme et al., 1978) and Lake Saint Martin (Göbel et al., 383 1980; Palme, 1982; Reimold et al., 1990), which might suggest a differentiated asteroid as the 384 parent body for achondritic projectiles. In contrast, the Rochechouart impact structure in France 385 (Koeberl et al., 2007; Tagle et al., 2009) and the Obolon impact structure in Ukraine (Valter and 386 Ryabenko, 1977; Masaitis, 1999) carry siderophile element patterns that favour the impact of 387 iron meteorites. The meteorite type for the Red Wing Creek impact structure is uncertain, but Geochemical constraints on impacting bodies 388 Koeberl et al. (1996) found a possible chondritic contamination pattern in impact breccias 389 recovered from drill cores. 390 Despite this apparent difference in impacting bodies for the Manicouagan, Lake Saint Martin, 391 Rochechouart, Obolon, and Red Wing Creek impact structures, one could argue that double and 392 multiple meteorite impacts could in fact involve a mixture of materials (Schmieder et al., 2013). 393 One such example, yet on a much smaller scale, is the fall of the Almahata Sitta meteorite in 394 northern Sudan on October 7, 2008, which comprised a variety of chondritic and achondritic 395 (ureilitic) lithologies (Bischoff et al., 2010). We acknowledge that asteroids commonly represent 396 ‗rubble piles‘ (Richardson et al., 1998; 2002), such as asteroid 25143 Itokawa (e.g. Fujiwara et 397 al., 2006), and can hence be composed of different types of materials. Moreover, a larger asteroid 398 can capture a smaller asteroid in space and thereby generate a binary asteroid system (such as, 399 e.g., asteroid 243 Ida and its satellite Dactyl; Chapman et al., 1995) of two bodies of different 400 composition, fragments of which may eventually impact Earth. It seems somewhat unlikely that 401 the incoming fragments of a tidally disrupted larger rubble pile asteroid or comet, such as 402 Shoemaker Levy-9 (e.g., Shoemaker et al., 1993; Crawford et al., 1994), would be heterogeneous 403 to the extent that they generate a chain of impact craters in which each one leaves a different 404 geochemical fingerprint; however, unless this type of scenario (i.e., impact of variable-type 405 cosmic rubble) is proven impossible in terms of celestial mechanics, one should consider the 406 theoretical possibility that a geochemically heterogeneous impact system can occur over 407 geologic time. On the other hand, impact melt lithologies at terrestrial impact structures can lack 408 a clear and representative meteoritic signature (e.g., Goderis et al., 2010), for example due to the 409 incomplete homogenization of the impactor-derived elements and the local impact melt, 410 fractionation of the meteoritic signature elements (e.g., Palme et al., 1979; Palme 1982), 411 differentiation of larger impact melt bodies (e.g., O‘Connell-Cooper and Spray, 2011), as well as 412 post-impact alteration. For the given uncertainties on the exact composition of the meteorites that 413 generated the Lake Saint Martin, Manicouagan, Rochechouart, Obolon and Red Wing Creek 414 impact structures we stress that the geochemical constraints cannot serve as reliable evidence for 415 or against a multiple impact scenario. 416 417 4.5. 418 Finally, the statistical probability for a multiple impact event on Earth in the Late Triassic should 419 be briefly evaluated based on the timing and paleopositions of the impact events in plate 420 reconstructions for North America (Laurentia) and Eurasia (see Spray et al., 1998; Walkden et 421 al., 2002). Using the estimated paleolatitudes and -longitudes of the impact craters as input 422 parameters in Monte Carlo simulations, Spray et al. (1998) calculated a low probability of P 423 <0.08 (<0.008 if the longitudinal range is included) for the event that the linear arrangement of 424 the three ‗main‘ E-W-aligned craters, Rochechouart, Manicouagan, and Lake Saint Martin, is a 425 random array. The probability for an aligned random strike decreases even further for five 426 impact structures (i.e., including Obolon and Red Wing on great circles; however, no statistical 427 probability was given for such an event). As the crater alignment was very unlikely a result of 428 random chance and because the imprecise age constraints for the craters agreed well within this 429 calculation, Spray et al. (1998) concluded that the five craters may represent a chain of impact 430 structures probably formed ‗within hours‘. 431 The general expectation that linear arrays of apparently coeval impacts constitute a combination 432 strike, as supported by statistical modeling, may be in analogy to some of the binary impact Statistical considerations 433 systems on Earth, including the proposed doublet craters of the West and East Clearwater Lake 434 impact structures in Canada and the Suvasvesi North and South impact structures in Finland. 435 Despite very low calculated likelihoods for their random origin in close proximity to the 436 respective fellow crater (Miljković et al., 2013), differing 40Ar/39Ar dating results for impact melt 437 rocks from each of these impact structures rather suggest that the impacts occurred millions of 438 years apart (see Schmieder et al., 2014b for a discussion and references therein for earlier dating 439 results). 440 Based on the size-frequency distribution of Earth-crossing asteroids and their encounter 441 frequency with the Earth-Moon system, Bottke et al. (1997) estimated that the production rate for 442 impact crater chains on Earth after S-type (Shoemaker-Levy 9) tidal disruption is less than 0.1 443 crater chains in 3.8 Gyr. While we acknowledge that these statistics are derived from numerical 444 modeling, the results by Bottke et al. (1997) suggest a very low chance of producing a terrestrial 445 impact crater chain in younger geologic history. We recommend that proposed terrestrial impact 446 crater chains and doublets should be systematically accompanied by isotope dating. Even more 447 delicate is the case of extraterrestrial impact crater chains and doublets, for which no absolute 448 ages can be obtained without sample return missions. Although crater counting (e.g., Neukum et 449 al., 2001) helps to some extent, this study shows that fortuitously aligned, yet unrelated impact 450 craters may also occur on asteroids and other planets in the Solar System. 451 452 5. 453 The ~40 km Lake Saint Martin impact structure in Manitoba, Canada, has been 454 at a Carnian age of 227.8 ± 0.9 Ma [± 1.1 Ma] (2σ; MSWD = 0.52; P = 0.59) by combining two CONCLUSIONS 40 Ar/39Ar-dated 455 plateau ages and one isochron age obtained on different aliquots of impact-melted K-feldspar. 456 With a relative error of ± 0.4% on the isotopic age, the Lake Saint Martin impact structure has 457 advanced to one of the most precisely dated larger impact structures on Earth. The new dating 458 results demonstrate that none of the impacts that constituted the postulated Late Triassic multiple 459 impact event were synchronous. Moreover, our data suggest that high-temperature isotopic 460 chronometers are currently the preferred means of dating impact events. Where possible, 461 statistical model results arguing that linear arrays of multiple impact craters, as well as closely 462 spaced apparent crater pairs, are most likely synchronous should be assessed in the light of 463 precise and accurate isotopic dating results. 464 465 Acknowledgements: We thank Celia Mayers and Adam Frew, Curtin University, for their helpful 466 support during sample preparation, Ruth Bezys for the earlier supply of some of the sample 467 materials used, and Rebecca Wilks for review of an earlier draft of this manuscript. The authors 468 acknowledge the facilities, and the scientific and technical assistance of the Australian 469 Microscopy & Microanalysis Research Facility at the Centre for Microscopy, Characterisation & 470 Analysis, The University of Western Australia, a facility funded by the University, State and 471 Commonwealth Governments. We thank the reviewers Vera A. Fernandes and Wolf Uwe 472 Reimold for their constructive comments that helped improve our manuscript, as well as the 473 Associate Editor Christophe Sotin for careful handling. Sample collection was supported by a 474 CARN grant from the Canadian Space Agency to EC. This project is supported by an ARC 475 Discovery grant to FJ and ET. 476 477 REFERENCES 478 Baksi, A.K., 2007. A quantitative tool for detecting alteration in undisturbed rocks and minerals 479 – II: Application to argon ages related to hotspots. In: Foulger, G. R., Jurdy, D. M. (Eds.), 480 Plates, Plumes and Planetary Processes. GSA Spec. 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Sci. 47, 718 1243–1255. 719 720 721 722 723 724 725 726 727 728 729 730 731 732 733 734 Zivkovic, V.B., Gosnold, W., 2007. The Lake Saint Martin impact structure and its relation to a multiple impact event. AGU Fall Meeting 2007, abstr. no. U23A-0857. 735 FIGURE CAPTIONS 736 Fig. 1: Landsat-5 satellite image of Lake Saint Martin in Manitoba, Canada (scene path 032, row 737 024, acquired on 04 April 2010) and outline of the estimated outer limits of the largely sediment- 738 and water-covered ~40 km-diameter impact structure according to Bannatyne and McCabe 739 (1984). Impact melt rock from the eastern crater moat and a partially melted Proterozoic granite 740 from the central uplift (inset images; both rock specimens ~10 cm in maximum length) were 741 sampled for 40Ar/39Ar dating. Satellite image source: USGS. 742 Fig. 2: Optical microscopic and backscattered electron images (BEI) of the fine-grained, 743 crystalline melt rock from the Lake Saint Martin impact structure and the impact metamorphosed 744 granite exposed in the central uplift. A: General appearance of the melt rock with a larger grain 745 of ballen quartz (plane polarized light). B: The melt rock is predominantly composed of 746 plagioclase (Plg; a larger phenocryst of andesine is shown), K-feldspar (Kfs), Quartz (Qtz), 747 pyroxene (Px), and Fe-Ti oxides. C: Optical image of ballen silica surrounded by fluidal-textured 748 feldspar (cross polarized light). D: BEI close-up of the granite, locally with idiomorphic K- 749 feldspar (adularia; Adu). The images are representative of the rock samples from which the 750 dating aliquots were separated. 751 Fig. 3: 752 impact-melted K-feldspars separated from the Lake Saint Martin impact melt rock. A: Age 753 spectrum (plateau) for aliquot LSM-1A. B: Inverse isochron for LSM-1A. C: Age spectrum 754 (mini-plateau) for aliquot LSM-1B. D: Inverse isochron for LSM-1B. Errors are given at the 2σ 755 level. 756 Fig. 4: 757 K-feldspar specimens separated from the partially melted basement granite exposed in the central 758 uplift of the Lake Saint Martin impact structure. A: Age spectrum (plateau) for aliquot LSM-2A. 759 B: Inverse isochron for LSM-2A with inset for magnification of data point array. C: Age 760 spectrum (plateau) for aliquot LSM-2B. D: Inverse isochron plot for LSM-2B with inset for 761 zoom on data point cluster. E: Age spectrum (disturbed) for aliquot LSM-2C. F: Inverse 762 isochron plot for LSM-2C. Errors are given at the 2σ level. 40 40 Ar/39Ar age spectra and corresponding inverse isochron plots for two aliquots of Ar/39Ar age spectra and corresponding inverse isochron plots for three impact-melted 763 Fig. 5: 40Ar/39Ar age spectra and corresponding K/Ca and inverse isochron plots for two whole- 764 rock chips of the Lake Saint Martin impact melt rock. A: Age spectrum (disturbed) and K/Ca 765 ratio for moderately altered aliquot LSM-3. B: Inverse isochron plot for LSM-3. C: Age 766 spectrum (disturbed) and K/Ca ratio for intensely altered aliquot LSM-4. B: Inverse isochron plot 767 for LSM-4. Errors are given at the 2σ level. 768 Fig. 6: Summary of measured 769 (alteration) apparent ages for the Lake Saint Martin impact melt aliquots along with statistical 770 age combinations for plateau and isochron ages. All ages are in million years. The weighted 771 mean of two plateau ages and one inverse isochron age is here considered the best-estimate age 772 for the Lake Saint Martin impact. Error boxes are 2σ. 773 Fig. 7: Compilation of selected terrestrial meteorite impacts during the Triassic and the 774 postulated Late Triassic multiple impact theory, modified after Spray et al. (1998). *Lucas et al. 775 (2012) suggested an age of ~220 Ma for the Carnian/Norian boundary, which has an age of 776 ~227 Ma in the current International Stratigraphic Chart (Cohen et al., 2013). Impact age data 777 from Koeberl et al. (1996), Ramezani et al. (2005), Buchner and Schmieder (2008), Schmieder et 778 al., (2010) and this study. 40 Ar/39Ar plateau, mini-plateau, inverse isochron and minimum Fig. 1 Click here to download high resolution image Fig. 2 Click here to download high resolution image Fig. 3 Click here to download high resolution image Fig. 4 Click here to download high resolution image Fig. 5 Click here to download high resolution image Fig. 6 Click here to download high resolution image Fig. 7 Click here to download high resolution image Table 1 Click here to download Table: Table1.pdf Table 1: Summary of plateau, mini-plateau and isochron ages, along with internal statistics for recrystallized feldspar melt particles and impact melt rock, Lake Saint Martin impact structure. Ages noted in bold were used for the calculation of the recommended weighted-mean age for the impact. Age spectrum characteristics Isochron characteristics 40 n Ar/36Ar intercept (±2σ) MSWD P Spreading factor (%) 227.2 ± 1.5 12 288 ± 13 0.79 0.64 31 0.15 228 ± 6 5 289 ± 20 1.73 0.16 70 1.00 0.46 227.9 ± 1.4 19* 288 ± 8 0.79 0.71 61 1.38 0.18 39 Sample ID Apparent age (Ma, ±2σ) Total Ar released (%) n Attribute MSWD 226.7 ± 2.4 84 12 Plateau 227 ± 5 63 5 227.0 ± 1.2 84 228.1 ± 1.4 73 P Isochron age (Ma, ±2σ) 0.78 0.66 Mini-plateau 1.70 18 Plateau 11 Plateau K-feldspar melt aliquots LSM-1A LSM-1B Impact melt rock, crater moat domain (single grain) LSM-2A LSM-2B Partially melted Precambrian granite, central uplift (single grain) LSM-2C ― no isochron ― ― no plateau ― ― no isochron ― Impact melt rock aliquots LSM-3 moderately altered (whole rock) ≥220-230 hump-shaped spectrum (minimum age) ― no isochron ― LSM-4 intensely altered (whole rock) ≥209 staircase-shaped spectrum (minimum age) ― no isochron ― Weighted mean of 2 plateau ages and 1 isochron age: * 227.8 ± (0.9) [1.1] Ma (2σ; MSWD = 0.52; P = 0.59) isochron includes degassing step 1 not part of (but with a step apparent age concordant with) the age plateau section. Supplementary Table-Annex 1 Click here to download Supplementary material for on-line publication only: Table-Annex1.xlsx