Speleothem samples collected for dating Palaeolithic cave art in Shulgan-Tash cave and for paleoclimate research in Southern Ural in 2013-2017
6/20/2018 Technical report
Yuri Dublyansky* and Yuri Lyakhnitsky** * Institute of Geology, Innsbruck University, Innrain 52, 6020 Innsbruck, Austria
** A.P. Karpinsky Russian Geological Research Institute (VSEGEI), Sredny prospect 74, 199106 St.-Petersburg, Russia
Aknowledgment
Work described in this report was partly funded by a grant of the Head of Government of Republic of Bashkortostan R. Khamitov through the State Organization “Scientific-Production Centre for Protection and Use of Objects of Cultural Heritage”, Ministry of Culture of the Republic of Bashkortostan.
Additional funding was provided through FWF (Austria) grants P257160 and I027070 to YD.
Cite this dataset
Dublyansky, Yuri; Lyakhnitsky, Yuri (2018), “Description of speleothem samples collected for U- series dating of Paleolithic cave art in Shulgan-Tash cave, Southern Ural, Russia”, Mendeley Data, v1 http://dx.doi.org/10.17632/c85nth69rb.1
Fig. 1. Google Earth satellite image showing locations of caves from which samples were collected. Coordinates of the center of this map are: 53.03 N, 57.05 E.
All caves are located in Southern Ural, Russia. 1. INTRODUCTION Location of caves is shown in Fig. 1. In this report we document:
(a) sampling of flowstonein Shulgan- 2. SAMPLING PURPOSES Tash cave for the purpose of dating AND STRATEGIES Palaeolithic parietal art; (b) sampling of stalagmites in Shulgan- 2.1. Sampling flowstone for Tash, Kulyurtamak, Victoria, and dating Palaeolithic Gryoz caves for paleoclimate and cave art paleoenvironmental studies 230 (c) sampling of cryogenic cave calcite The Th-U method has recently emerged as (CCC) in Shulgan-Tash and Victoria a unique tool for accurately and precisely caves for paleoclimate and paleo- dating cave art in the presence of calcite permafrost studies. flowstone (Pike et al. 2012; Aubert et al. 2014; Pons-Branchu et al. 2014; Hoffmann et al. 2016, 2018). If the painting was made on flowstone, the 230Th-U age of the latter
provides the maximum possible age of the painting (terminus post quem). If the painting is covered by a younger flowstone, the age of the latter constrains the minimum age 3 | P a g e
(terminus ante quem) of the art. The shorter the time gap between the deposition of the underlying “canvas” flowstone and the overlying flowstone, the more precise is the dating of the art. Hellstrom (2012) pointed out that any one calcite overgrowth or underlying layer has a relatively low probability of approaching the age of the art. Studies that consider a small number of examples of cave art may therefore return ages that do not lead to a refinement of the age of that art.
Our strategy of sampling the parietal art in Shulgan-Tash cave was to strive to identify all potentially datable paintings in the cave (i.e., those made on old flowstone, those that Fig. 2. Spatio-temporal relationships of flowstone were overgrown by younger flowstone, and and pigment of cave art in Shulgan-Tash cave. a – combinations of both). Typical relationships flowstone and pigment are not in contact; b – flowstone is younger that pigment; c, d – between pigment of paintings and flowstone flowstone is older than pigment; e, f – flowstone are depicted in Fig. 2. is both older and younger than pigment; g – flowstone, both older and younger than pigment, To ascertain that flowstone at a potential is overgrown by a thick layer of tufaceous calcite. sampling location has an unambiguous Red rectangles show possible strategies of stratigraphic relationship with the painting sampling. Note that in a the temporal relationships between paintings and flowstone are each potential location was inspected with a indeterminate, and dating will not yield hand lens. information on the age of cave art.
Cave-wide inspections have shown that paintings at the upper level of the cave (Hall 2.2. Sampling stalagmites of Paintings) were made on barren cave for paleoclimate and walls, and only paintings located at the lower paleoenvironmental level of the cave (Domed Hall, Hall of Signs, and Hall of Chaos) have clear stratigraphic studies relationship with flowstone. In total, we “Common” speleothems, such as stalagmites identified and sampled 20 sites potentially and flowstone are recognized archives for suitable for parietal art dating. paleoclimate studies (e.g., 18O and 13C of calcite, 2H of fluid inclusion water, trace
elements, etc.; Fairchild and Baker, 2012). For specific purpose of this project, speleothems were 230Th-U dated at their tops
and bottoms, thus constraining the time of infiltration of water into the cave (i.e., permafrost-free conditions). Cryogenic cave carbonates (CCC) provide information on the
4 | P a g e
time of occurrence of (degrading) permafrost older and younger flowstone layers, in the study area. sometimes having complex geometry (Fig. 2 e). Sampling of speleothems was preceded by screening of caves in the area, during which 3.2. Small-diameter cores the caves were visited, inspected and sites (cave art dating) potentially suitable for speleothem collection identified. By visual observations we 10 mm-diameter holes were drilled through attempted to identify stalagmites that grew the flowstone using custom-made water- at different times, thus providing the widest cooled diamond drill bits, yielding 8 mm- temporal coverage of speleothem growth. In diameter cores. In most cases cores were order to improve robustness of the record, taken laterally adjacent to the paintings, so we collected 14 stalagmites from four caves that the paint layer was not intersected. This located within 4 km (Fig. 1). technique proved adequate when paintings were made directly on cave walls and were 2.3. Sampling cryogenic overgrown by younger calcite. In cases cave carbonates (CCC) where a pigment layer was “sandwiched” between the older and the younger CCC were not known from the study area flowstone, particularly when the shape and prior to this work. We performed a targeted thickness of growth layers were both search for CCC in all inspected caves. CCC irregular, sub-sampling of pre- and post-paint were found and sampled in two caves, calcite in the laboratory becomes Shulgan-Tash and Victoria. problematic. In a number of cases, therefore, we had to drill cores across the pigment 3. FIELD SAMPLING layer. This technique was approved by the oversight authority, State Organization 3.1. In situ collection of “Centre for the protection and management powders using a hand- of immovable cultural heritage” of the held milling device Ministry of Culture, Republic of (cave art dating) Bashkortostan, Russia. Samples for dating were collected as We concur with Hoffman et al. (2016) that powders using a hand-held milling device by the use of this sampling technique should be carefully removing ca 0.5 mm-thin individual restricted to the most exceptional layers of calcite. This technique allowed circumstances and should, in general, be sampling sites showing a simple flat discouraged. geometry of the flowstone growth layers (cf. Fig. 2 b-d). The approach becomes 3.3. Patching problematic when: (a) paintings were made In order to preserve the visual integrity of on irregular flowstone surfaces (e.g., runnel the paintings and cave formations the small flowstone; Fig. 2 f); (b) paintings are coated holes produced by coring were patched with by thick tufaceous calcite (Fig. 2 g; at some lime putty and the addition of local sand and sites in the Hall of Chaos the thickness of puzzolana. Subsequently, patches were such calcite overgrowth reaches 2 cm); and camouflaged using local natural materials (c) paintings are “sandwiched” between (Fig. 3). 5 | P a g e
3.4. Sampling entire speleothems (paleoclimate studies) Stalagmites were collected in those parts of the caves where their removal caused minimal visual impact. Whenever possible, naturally broken stalagmites were collected. Samples of cryogenic cave calcite (CCC) were taken by collecting between 10 and 100 g of crystals and aggregates from the cave floor (Fig. 4).
4. FIELD SAMPLING SCHEDULE Sampling of calcite associated with Palaeolithic cave art in Shulgan-Tash cave was carried out in three stages.
Stage 1. Pilot sampling was carried in June 2013. The aim of this campaign was to Fig. 3. Patching and camouflaging the holes: determine whether calcite underlying and (a) 10 mm-diameter hole patched with lime putty; overgrowing cave art is datable using the (b) the hole was subsequently camouflaged with 230Th-U method. At this stage, several local clay. powder samples were collected using a growth layers and the lack of a marker hand-held milling device. horizon between the two stages of calcite deposition. Upon obtaining permission from Stage 2. The main sampling was carried out the overseeing authorities, we drilled several in June 2015. In most cases sampling was cores across the paint layers. In addition, done by small-diameter coring through several new sites were sampled in the Hall of flowstone adjacent to paintings. In two cases, samples represented fragments of runnel flowstone which were chipped off the wall with a scalpel (outside the painted area).
Stage 3. Additional sampling was carried out in November 2015. Several sites, where initial sampling by coring adjacent to the painted area had yielded unsatisfactory dating results, were re-sampled. In these cases we were not able to clearly separate sub- samples of pre- and post-paint calcite Fig. 4. Collection of cryogenic cave calcite in the Hall of Rainbow, Shulgan-Tash cave. Photo R. Shone. due to the complex geometry of 6 | P a g e
Signs.
Sampling of stalagmites and CCC was carried out on several field expeditions between 2013 and 2017.
5. LABORATORY SUB- SAMPLING Samples, collected in situ as powders, were subjected to dating as is. Samples, collected as mini-cores were cut longitudinally using a high-precision diamond saw (Buehler Isomet). The resulting flat surfaces were manually ground and polished using SiC powders and water-based diamond suspensions. For documentation purposes, polished core surfaces were scanned at 1200 dpi. In cases of complex morphologies of growth layers Fig. 5. Polished central slab of two stalagmites (sample the outer surface of cores was polished as VIC-2, Victoria cave). The older (broken) stalagmite grew during the Last Interglacial; the younger grew well. This helped tracing the curvilinear during the Holocene. Results of 230Th-U dating are nature of flowstone layers and allowed shown. accurate sampling for dating. Sub-samples for dating were taken using a hand-held milling device (Proxxon) in an Air Clean 600 laminar flow hood. Several powdered sub- samples between 6 to 200 mg were obtained from each sample in order to test for stratigraphic consistency of ages.
Stalagmites were sub-sampled along polished slabs cut along their growth axes. Each stalagmite was initially characterized using top and bottom ages (Fig. 5). Additional ages were obtained from stalagmites showing a complex history of growth in order to constrain discrete growth episodes and refine a depth-age model.
Small grains of CCC were ground entirely and dated; from larger grains sub-samples for dating were milled.
7 | P a g e
6. SHULGAN-TASH CAVE junction. It can be accessed through an inclined passage followed by a 14 m-high Shulgan-Tash cave is located in the Republic ascending shaft. From the top of the shaft of Bashkortostan, Russia, within the Shulgan- the cave continues for ca 700 m in north- Tash Natural Reserve (53.044°N, 57.064°E). eastward and then northward direction, The cave is located within the Saryk-Oskan forming a series of halls. The first of them, massif, built of folded Devonian and Hall of Paintings, also hosts parietal art. In Carboniferous limestone. The massif raises the northernmost Hall of Abyss, the cave ca 120 m above the Belaya River (Fig. 6). The steeply descends to the lower level. In this large arched cave entrance, ca 20 m high and hall the Underground Shulgan brook flows 40 m wide, is hidden in a side canyon cutting for ca 200 m, terminating downstream in a the eastern slope of the massif and cannot sump (70 m-long, 12 m-deep). Upstream, the be seen from the river. The surveyed length of the cave is 3,341 m, and the vertical distance between the entrance and the highest part is ca 80 m. The cave has two dry “levels” in addition to an underwater part. A large lake- spring called Blue Lake discharges underneath the entrance portal, flowing out of the cave as a small brook. The lake provides access to the underwater part of the cave, which was explored by SCUBA divers to a depth of ca 80 m.
From the entrance, the large horizontal Main Gallery (ca 200 m-long, 19 m-wide, 8 m-high; Fig. 7) leads to a Y-shaped junction. There, one branch continues through a restriction in a north- easterly and easterly direction, forming a series of spacious halls: Domed Hall, Hall of Signs, and Hall of Chaos (Fig. 6). The far end of this 350 m-long lower level (in
Hall of Chaos) is only 25-30 m higher than the entrance. The Fig. 6. Outline of the main part of Shulgan-Tash cave (in walls of all three halls host dark blue) projected on the topography of the Saryk- Palaeolithic cave art. Oskan massif. Red spots on cave walls indicate locations of cave art. Isohypses show 5 m increments. Surface The upper level of the cave is topography (photogrammetric survey) by O.A. Minnikov located to the north of the Y- (Russian Geographic Society); cave outline by Lyakhnitsky et al. (2015). 8 | P a g e
brook can be followed northward through a partly flooded gallery to another sump (10 m-long, 4 m-deep). The cave continues behind this sump in northeasterly direction as a series of galleries and sumps until it reaches the terminal sump (175 m-long, 13 m-deep; not shown in Fig. 6).
All halls hosting cave art have a year-round relative humidity near 100% and an air Fig. 7. Shulgan-Tash cave, Main gallery, looking back to the temperature of 2.4 to 7.6 C, entrance. Photo R. Shone. which is markedly warmer that the mean annual temperature in the area (+1.2 C; Chervyatsova et al. 2015), likely reflecting the ascending geometry of the cave lacking an upper entrance.
7. SAMPLING FLOWSTONE In subsequent text, where ASSOCIATED WITH applicable, individual paintings are referred to using nomenclature PARIETAL ART IN from Lyakhnitsky et al. (2015); their SHULGAN-TASH CAVE numeric IDs are preceded by a Samples for 230Th-U dating were taken in number sign (#). Domed Hall, Hall of Signs and Hall of Chaos, all located on the lower level of the cave (Fig. 6). No flowstone coatings suitable for dating were found in the only decorated hall of the upper level (Hall of Paintings). A summary of samples associated with cave art is given in Table 1.
In several sampling locations in the Hall of Chaos the youngest flowstone has a tufaceous character. This calcite has not been dated because it was impure (high contents of Fe and Si by micro-XRF analysis).
9 | P a g e
Table 1 : List of samples collected for 230Th-U dating of cave art in Shulgan-Tash cave
# Sample ID Painting # Painting name Location in the hall (this study) according to according to Lyakhnitsky et al. Lyakhnitsky et al. (2015) (2015) Hall Domed 1 ShT01 No # No name W wall, Niche 2 ShT13 6-1 Grid E wall Hall of Signs 3 ShT03 12-1 Double triangle W part of N wall 4 ShT17 15-1 Dash line Middle part of N wall 5 ShT18a No # No name Middle part of N wall 6 ShT19 No # No name Middle part of N wall 7 ShT20 No # No name Middle part of N wall 8 ShT21 No # No name Middle part of N wall Hall of Chaos 9 YD01, 02 20-4 Upper horse Middle part of S wall 10 YD03 to 07 20-2 Trapezium Middle part of S wall 11 YD08 20-1 Lower horse Middle part of S wall 12 ShT05 20-1 Lower horse Middle part of S wall 13 ShT06 20-6 New Middle part of S wall anthropomorph 14 ShT07 22-17 Slant lines Slot 15 ShT08 22-20 Large triangle Slot 16 ShT09, ShT09bis 22-7 Upper slingshot Slot 17 ShT10, ShT10bis 22-12 Lower slingshot Slot 18 ShT11bis 22-19 Extreme left Slot 19 ShT14 22-13 Tower Slot 20 ShT15 22-13 Tower, Black wedge Slot 21 ShT16 22-14 Red couple Slot 22 ShT12 23-1 Remote mammoth NE part of the hall
7.1. Domed Hall Domed Hall is the first of the three halls hosting Palaeolithic parietal art at the lower level of the cave. It is separated from the ca 200 m-long Main Gallery by a wide but low restriction called Throat. Two sites were sampled in Domed Hall: one on the upper lip of the Niche in the western wall (sample ShT01) and another near the painting #6-1 on the eastern wall of the hall (sample ShT13; Fig. 8).
Sample ShT01 Sample was taken above the Niche in the western wall of the hall. A 55 cm Fig. 8. Sampling sites in Hall Domed. Survey by rectangular area cleaned off from Y. Lyakhnitsky. tufaceous flowstone by archaeologists exposed poorly preserved (washed out) pigment. A core was obtained across the The pigment rests on a thin (ca 0.3 mm) layer flowstone into the bedrock near the cleaned of calcite of uncertain origin and is area (Fig. 9). overgrown with a 8 mm-thin layer of tufaceous calcite. Three subsamples were taken for dating from the calcite overgrowth (Fig. 10).
Fig. 10. Core ShT01, longitudinal cut. Fig. 9. Location of core ShT01 (red arrow; patched with white The oxidized pigment layer can be seen lime putty) to the left of the rectangular area where the at the base of porous tufaceous calcite. flowstone was removed by archaeologists above the Niche in Three subsamples taken for dating are the western wall of the Domed Hall. Pigment exposed in the outlined. cleaned rectangle is poorly preserved (faint colour).
Sample ShT13 A series of narrow, <5 mm- wide, flowstone “runnels”, forming a root-like bunches are present on the otherwise barren eastern wall of Domed Hall. Painting #6-1 uses both the wall and the flowstone as the “canvas” (Figs. 11 a, b). On visual basis, the latter represents a single depositional episode. It was sampled for dating (chipped off) above the painted area.
Fig. 11. Painting #6-1 on the eastern wall of the Domed Hall. (a) general view; (b) close-up on the area delineated by a red rectangle in a. Pigment covers both barren limestone wall and flowstone. Sample ShT13 was taken from one of the thin “runnels” some 10 cm above the painted area.
12 | P a g e
7.2. Hall of Signs Hall of Signs is the second in the series of three halls hosting Palaeolithic parietal art at the lower level of the cave (Fig. 12).
Fig. 12. Sampling sites in Hall of Signs. Survey by Y. Lyakhnitsky.
Sample ShT03 The painting #12-1 is located in the western part of the northern wall of the Hall of Signs. The painting is made on the barren limestone wall. To the left of the painting the rock is coated with ca 1 mm- thin layer of flowstone. The temporal relationship between the painting and flowstone is unclear. The latter has either fallen off the rock due to natural causes or was chipped off by ancient Fig. 13. Location of core ShT3 (patched with lime putty) near painting people prior to painting. #12-1. The core intersected a thin layer of flowstone, which is absent Sample ShT3 was taken as a (chipped off before painting?) beneath the painting. core across the flowstone (Fig. 13). The flowstone consists of a single layer of white translucent calcite showing a columnar fabric.
13 | P a g e
Fig. 14. Sampling site ShT17 in the middle part of north wall of the Hall of Signs. (a) before coring; (b) after coring. Reddish poorly preserved paint can be seen between colonnettes of porcellaneous flowstone.
Sample ShT17 Sample ShT17 was taken near painting #15-1, located in central part of the northern wall of the Hall of Signs. Although reddish pigment is undoubtedly present on the wall, no distinct figures are recognizable. The pigment is covered by discontinuous thin layer of flowstone, which in places forms miniature colonnettes -1 2 cm-wide (Fig. 14). Flowstone calcite has a porcellaneous fabric and contains, on average, one order of magnitude less U (ca 0.15 ppm) than other flowstone types in the cave.
The section of the colonnette intersected by core ShT17 is shown in Fig. 15. Three Fig. 15. Longitudinal section of core subsamples of porcellaneous calcite were ShT17. The pigment layer is present at collected for dating. the base of calcite. Subsamples taken for dating are outlined.
14 | P a g e
Fig. 17. Core ShT20. The strongly weathered (limonitized) pigment layer can be seen at the base of calcite crust. The flowstone has a porcellaneous fabric and exhibits a weak layering. Subsamples taken for dating are outlined.
The sample was taken across a flowstone colonnette built of porcellaneous calcite, Fig. 16. Site of sample ShT20 in the middle part of the located in the central part of the northern northern wall of the Hall of Signs. (a) general view; wall of the Hall of Signs. The flowstone (b) close-up on area marked by red rectangle in a. A core was drilled through a broken (vandalized) covers the very poorly preserved (barely colonnette flowstone composed of porcellaneous recognizable) patch of reddish pigment calcite covering a poorly preserved patch of pigment. (Fig. 16). A series of three subsamples (Fig. 17) were taken from the core for dating. Sample ShT20 Sample ShT21 The sample was taken in the central part of the northern wall of the Hall of Signs between paintings #14-4 and #14-2. In this part of the wall thin “runnel” flowstone of porcellaneous calcite was deposited over poorly preserved paintings (disfigured patches of reddish pigment). The sample was taken from the “runnel” outside the painted area using handheld milling tool (Fig. 18).
Fig. 18. Removing the upper, dirty layer of calcite prior to collection of sample ShT21 using a handheld milling tool. 15 | P a g e
7.3. Hall of Chaos Hall of Chaos (Fig. 19) is the third in a series of chambers hosting Palaeolithic parietal art on the lower level of Shulgan-Tash cave.
Fig. 19. Sampling sites in Hall of Chaos. Survey by Y. Lyakhnitsky.
16 | P a g e
Fig. 20. Sampling sites at composition #20 in Hall of Chaos: (a) photograph; (b) scheme. Blue squares indicate position of samples obtained by in-situ milling; red circles indicate positions of cores. Red dashed rectangle in b outlines painting formerly tentatively interpreted as an anthropomorphic figure (Lyakhnitsky et al. 2015).
Fig. 21. Sampling at painting #20-6 in the Hall of Chaos. (a) painting (New anthropomorph) as seen during sampling in 2015 (photo Y. Dublyansky); (b) the same painting (Bactrian camel) after removal of overlying flowstone in November 2017 (photo A. Pakhunov).
Composition #20 1976 members of archaeological expedition led by Otto Bader discovered a small spot This composition is located on a rocky slab in from which seeping water had washed out the middle part of southern wall of the hall red paint. Restorers removed the several cm- (Fig. 19). Prior to 1976 this part of the wall thick tufaceous flowstone from part of the was entirely coated with a thick layer of wall, revealing figures of two horses brownish tufaceous calcite flowstone. In 17 | P a g e
(paintings #20-1 and 20-3) and two trapeziums (#20-2 and 20- 5) (Fig. 20). A several mm-thick layer of semi-translucent flowstoneshowing a columnar texture was present beneath tufaceous calcite. Part of this layer was left in place by the restorers to protect the paintings from effects of water, which is abundant on this part of the wall. In 2008 part of another painting was cleared from calcite (#20-6). This painting was tentatively Fig. 22. Site of collection of samples YD01 and YD02 near painting interpreted as an #20-3. The samples were milled from “canvas” flowstone (ca 2 mm- anthropomorphic figure. An thick, on which pigment is seen in the right part of the photo). The alternative interpretation was flowstone is broken off in the upper middle part of the frame, exposing dark limestone bedrock. Grayish flowstone deposited that this is part of a zoomorphic since 1976 is seen to the left and up of the instrument. figure Lyakhnitsky( et al. 2015). The latter interpretation proved correct in remains an unsolved task. November 2017 when further cleaning of the Samples YD01 and YD02 wall revealed a Bactrian camel (Devlet et al 2018; Fig. 21). Samples were taken near the upper painting of the horse (#20-3). At this location, the The state of preservation of the paintings of overlying flowstone had been removed by this composition is variable. In some restorers and the ocher of the painting was paintings the pigment is partly hydrated (limonitized). Apparently, hydration was ongoing for a long time and occurred due to water seeping beneath the layer of tufaceous flowstone. Depending on the season, modern seepage water is either in equilibrium with or supersaturated with respect to calcite; in places the water deposited thin layers of white calcite on the previously cleaned surfaces. Preservation Fig. 23. Site of collection of samples YD03 to YD07 in the central part of paintings in such dynamic of painting #20-2. The picture was taken after collection of the hydrological conditions penultimate sample, YD06.
18 | P a g e
flowstone between the vertical lines of the painting (Fig. 23). Five samples, YD03 to YD07, were taken by consecutive milling of thin layers of this calcite.
Sample YD08 At painting #20-1 only a ca 0.5 mm-thin layer of flowstone was left by the restorers (Fig. 24). Sample YD08 was taken from flowstone overgrowing the painting. The age of this sample is slightly too old because of the inadvertent contamination Fig. 24. Sampling site (YD08, post-paint flowstone) near by the calcite from underlying pre-paint the lower painting of the horse (#20-1). Note traces of chisel on the surface of the flowstone left by restorers. layer. exposed (Fig. 22). Two samples were taken Sample ShT05 using handheld milling device, each The core was taken several cm below the representing a ca 0.5 mm-thin layer of painting #20-1 (Fig. 25). A layer of pigment is calcite. present in the core, marking the boundary between the pre-paint and post-paint flowstone (Fig. 26).
Samples YD03 to YD07 Sampling was performed near one of the trapeziums (#20-2). The restorers left a relatively thick layer of young (post-paint)
Fig. 25. Site of collection of sample ShT05 below the Fig. 26. Core ShT05. From top to bottom: painting #20-1 (drill hole is patched with lime putty). tufaceous calcite, layered flowstone Hind legs of the lower horse are seen in the upper part showing a columnar fabric and limestone of the frame. The pigment is protected with a thin (<0.5 of the cave wall. The pigment layer marks mm) layer of translucent flowstone, followed by a layer the boundary between the pre- and post- of grayish flowstone and a thick layer of grey tufaceous paint flowstone layers. Positions of sub- flowstone. samples taken for dating are outlined.
19 | P a g e
Sample ShT06 This sampling point is located to the left of the putative “anthropomorphic” painting #20-6 (Fig. 27). After removal of overgrowing calcite in November 2017, the painting turned out to be one of a Bactrian camel (Devlet et al. 2018; Fig. 21b).
A core was drilled through a thick layer of tufaceous calcite and thin laminated calcite into the bedrock. Similarly to core ShT05, this core also features two layers of laminated flowstoneshowing a columnar fabric, separated by the paint layer (Fig. 28).
Samples for dating were collected from pre- paint and post-paint flowstone layers.
Fig. 28. Core ShT06. From top to bottom: tufaceous calcite, layered flowstone with columnar fabric, and limestone of the cave wall. The pigment layer marks the boundary between the pre- and post- paint flowstone. Sub-samples taken for Fig. 27. Location of sample ShT06 near painting #20-6. dating are outlined.
20 | P a g e
Group of paintings #22 This group of paintings is located in the recess called “Slot” in the Hall of Chaos. Slot represents a small chamber with a flat floor and a flat ceiling both inclined southward at an angle of ca 30°, separated by a distance of ca 1.5 m. Paintings are present on the ceiling (Fig. 29) and in places are overgrown by flowstone runnels.
Sample ShT7 A core was drilled through a runnel flowstone (incipient drapery) near the upper part of painting #22-17 (Fig.
30). The flowstone consists of clear translucent calcite with the columnar Fig. 29. Sampling in the Slot of the Hall of Chaos (group of fabric. paintings #20). All paintings are made on the ceiling of the Slot. Survey by Y. Lyakhnitsky. Four subsamples were taken in micro- stratigraphic order for dating (Fig. 31). One of the samples was inadvertently contaminated by material from the youngest outer flowstone (yellow circle in Fig. 31).
The very faint layer of pigment seen in the core does not belong to the painting per se; rather, it is likely a result of lateral diffusion of pigment along the rock surface.
Fig. 31. Calcite flowstone in core ShT07. The pigment layer is barely seen at the contact between flowstone and altered (bleached) fractured limestone bedrock. Sub-samples taken for dating are Fig. 30. Location of sample ShT07. A core was drilled outlined. Yellow circle marks the place of through runnel flowstone partly covering the painting #22- possible contamination of subsample 17. The core hole (white spot) was patched with lime putty. ShT07-3 by younger calcite.
21 | P a g e
Fig. 32. Location of sample ShT08. Core is taken across runnel flowstone partly covering painting #22-20.
Fig. 33. Core ShT08. The pigment layer is Sample ShT08 clearly visible at the contact with the The core was drilled through runnel altered (bleached) bedrock limestone. flowstone near painting #22-20 (Fig. 32). Sub-samples taken for dating are outlined. Three subsamples were taken for dating in microstratigraphic order (Fig. 33). presence of paint layer allowed precise sub- sampling for dating (Fig. 35). Samples ShT09 and ShT09bis Samples were taken as cores near the painting #22-7. The initial core ShT09 was drilled outside of the painting (Fig. 34) and yielded inconsistent ages because the individual layers could not be precisely separated.
The coring was repeated, this time through the pigment layer (ShT09bis), and the
Fig. 35. Core ShT09bis. Sub-samples Fig. 34. Sampling site ShT09 near painting #22-7. taken for dating are outlined.
22 | P a g e
Fig 36. Sampling site ShT10 near painting #22-12.
Samples ShT10 and ShT10bis Fig. 37. Core ShT10bis. Sub-samples A core was drilled through runnel flowstone taken for dating are outlined. The wall- rock in this core is white crystalline vein overgrowing the painting #22-12 (Fig. 36). calcite. The initial core ShT10 was drilled outside the overgrowing the painting #22-19 (Fig. 38). painting. Its internal layering was indistinct Core ShT11 was not analyzed by technical and yielded inconsistent dating results. reasons. Three sub-samples from core Therefore, a second core, ShT10bis, ShT11bis were taken for dating (Fig. 39). intersecting the paint layer, was drilled. Three subsamples were taken from this core for dating (Fig. 37).
Samples ShT11 and ShT11bis Cores were drilled through runnel flowstone
Fig. 38. Sampling site ShT11. The cores were drilled through Fig. 39. Core ShT11bis. Pigment is runnel flowstone near the painting #22-19. Sample ShT11 visible at the interface with the was not analyzed. bleached limestone. Sub-samples taken for dating are outlined. 23 | P a g e
Fig. 40. Sampling site ShT14: runnel flowstone Fig. 41. Core ShT14b. Sub-samples taken for overgrowing painting #22-13. dating are outlined. Pigment layer is visible between subsamples ShT14b-5 and ShT14b-6.
Sample ShT14 b The core was drilled through runnel flowstone overgrowing the painting #22-13 (Fig. 40). Four sub-samples of calcite overgrowing the pigment and tree sub- samples of the „canvas” flowstone were taken for dating (Fig. 41).
24 | P a g e
Fig. 43. Core ShT15. Sub-samples for dating are outlined.
painting area. The core was drilled in this thicker part of flowstone and did not intersect the pigment.
The upper ca 0.5 mm-thin layer of flowstone was removed to avoid contamination. Three petrographically distinct layers below were sub-sampled for dating (Fig. 43).
Fig. 42. Sampling site ShT15, near lower left part of painting #22-13. (a) overview; (b) close-up of area outlined by red rectangle in b; (c) close-up of the hole, showing thin layer of calcite flowstone above dark grey bedrock.
Sample ShT15 At sampling site ShT15 near painting #22-13, the spatial relationships between painting and flowstone are not entirely clear (Fig. 42). Apparently, the dark painting was made on a thin old flowstone and later became coated by a very thin layer of flowstone. The flowstone is slightly thicker outside the
25 | P a g e
Fig. 45. Core ShT16. The pigment layer is present at the interface between the bedrock and the flowstone. Sub-samples Fig. 44. Sampling site ShT16 near painting #22-14. for dating are outlined.
Sample ShT16 Sample ShT12 The core was drilled through runnel The sampling site is in the northwestern part flowstone covering painting #22-14 (Fig. 44). of the Hall of Chaos, on the eastern wall, Three sub-samples were obtained from this below painting #23-1. The runnel flowstone core (Fig. 45). covers the painting, (Fig. 46) which is located some 4 m above the cave floor. The sample was chipped off the flowstone near the painting.
Fig. 46. Sampling site ShT12. Runnel flowstone (red arrows) and painting #23-1 (white arrow).This painting is located in ca 4 m above the cave floor.
26 | P a g e
8. SAMPLES OF STALAGMITES AND CRYOGENIC CAVE CARBONATES (CCC) Nine stalagmites were collected in four caves of the Shulgan-Tash Natural Reserve: Shulgan- Tash, Kulyurtamak, Grioz and Victoria caves, located within 6 km (see Fig. 1). CCCs were found and sampled in two caves, Shulgan-Tash and Victoria. The list of samples is presented in Table 2.
Table 2 : List of stalagmites and CCCs collected for 230Th-U dating in four caves
# Sample ID Speleothem Location in cave Shulgan-Tash cave 1 YD-K1 Stalagmite Rainbow Hall (upper level of the cave) 2 YD-K2 Stalagmite Rainbow Hall (upper level) 3 YD-K3 Stalagmite Rainbow Hall (upper level) 4 YD-K6 Stalagmite Rainbow Hall (upper level). Stalagmite on the clay/lake deposit in central part of the hall. 5 SHT2 CCC Rainbow Hall (upper level). On the surface of clay/lake deposit. 6 SHU01 CCC Rainbow Hall (upper level). On the surface of clay/lake deposit. 7 SU6 CCC Rainbow Hall (upper level). On the surface of clay/lake deposit. 8 SHT2-2017 CCC Rainbow Hall (upper level). Pocket ca 1 m below the surface of clay/lake deposit. Kulyurtamak cave 9 YD-K3 Stalagmite Victoria cave 10 VIC-1 Stalagmite Lower gallery 11 VIC-2 Stalagmite Upper gallery 12 VIC-3 Stalagmite Upper gallery 13 VIC1_CCC CCC Upper gallery 14 VIC2_CCC CCC Upper gallery 15 VIC03a_CCC CCC Upper gallery 16 VIC03b_CCC CCC Upper gallery 17 VIC05a_CCC CCC Upper gallery 18 VIC05b_CCC CCC Upper gallery 19 VIC06a_CCC CCC Upper gallery 20 VIC06b_CCC CCC Upper gallery Gryoz cave 21 GRZ-1 Stalagmite
Fig. 47. Map of Shulgan-Tash cave showing locations of sites where stalagmites and CCC were collected. Simplified from Lyaknnitsky et al. (2015).
8.1. Stalagmites and CCCs from Shulgan-Tash Several additional stalagmites collected at the lower level, in the Hall of Chaos, were cave too impure to yield reliable 230Th-U ages Stalagmites for this study were collected at (samples are not reported here). the upper level of the cave, in the vicinity of the Hall of Rainbow (Fig. 47).
Fig. 48. Stalagmite YD-K1, in the Calcite Gallery of the Hall of Rainbow. Stalagmite YD-K1. Collected in the first quarter of the Calcite Gallery of the Hall of Rainbow, stalagmite was located in ca 2.5 m above the floor on a sloping wall (Fig. 48). Fig. 49. Stalagmite YD-K1, polished slab. Samples for dating are marked. Dripping was slow, less than 1 drop per minute. In this part of the cave a RH = 94% and T = 8.1C.
A polished slab cut from the central part of the stalagmite is shown in Fig. 49.
Stalagmite YD-K2. Collected ca 10 m further into the Calcite Gallery (past the “window” on its eastern side). No active dripping occurred on the stalagmite (Fig. 50).
The polished slab cut from the central part of the stalagmite is shown in Fig. 51.
Fig. 50. Stalagmite YD-K2 in the Calcite Gallery of Fig. 51. Stalagmite YD-K2, polished slab. the Hall of Rainbow. Samples for dating are marked. 2 | P a g e
Fig. 52. Stalagmite YD-K3 in the northern part of the Hall of Rainbow.
Stalagmite YD-K3. Collected in the northern Fig. 53. Stalagmite YD-K3, polished slab. part of the Hall of Rainbow, in a flat slot-like Locations of samples collected for dating passage, on a vertical rock slab located on are marked. the eastern side of the slot. No dripping water was observed (Fig. 52).
The polished slab cut from the central part of the stalagmite is shown in Fig. 53.
Sample YD_K6. This stalagmite was displaced by cave visitors; it was found overturned and embedded in clay in the central part of the Hall of Rainbow.
A slab cut from the central part of the stalagmite is shown in Fig. 54.
Fig. 54. Stalagmite YD-K6; slab. Locations of samples collected for dating are marked. 3 | P a g e
8.2. Cryogenic calcite Another occurrence of CCC was found as a small pocket in the clayey pool deposits, Cryogenic calcite was initially found on the approximately 1 m below its surface, surface of ca 2 m-thick clayey lake deposits exposed in the wall of a small ravine (Fig. 55). (Fig. 54). Calcite occurs in an area of ca 188 The deposit consists of the calcite with m, commonly associated with cracks in the smaller grain sizes (0.2-2.0 mm) as compared clay. Along with calcite, cm-scale spherulitic to the CCC found on the clay surface. aggregates of cryogenic gypsum are present (Fig. 55), whose cryogenic origin was confirmed by isotopic analysis of the gypsum hydration water.
Fig. 55. CCC (brown) and cryogenic gypsum (light coloured) from the Hall of Rainbow, upper level of Shulgan-Tash cave.
Fig. 54. Cryogenic cave calcite in clay in the Hall Fig. 56. Occurrence of CCC ca 1 m below the of Rainbow, upper level of Shulgan-Tash cave. surface of clay deposits in the Hall of Rainbow, (a) CCC on the clay surface; (b) close-up; (c) CCC upper level of Shulgan-Tash cave. (a) lens of CCC in open cracks of the clayey deposits. in clay; (b) close-up.
4 | P a g e
Fig. 57. Map and vertical projection of Kulyrtamak cave. Location of stalagmite YD-K4 is marked by yellow circle. Survey by Y. Sokolov and O. Schastnaya (2009).
8.3. Stalagmite from Total length of the cave is 420 m, and amplitude - 43 m. The cave consists of Kulyurtamak cave several chambers and passages forming a Kulyurtamak cave is located near the mouth three-dimensional array (Fig. 57). The cave of the ravine Kulyurt, some 40 m above its morphology suggests a phreatic origin. One bottom. The cave opens in the middle part of stalagmite was collected in central part of the steep rocky slope. Cave coordinates: the cave. 53.023N, 57.013E; altitude ca 350 m a.s.l.
The entrance is an asymmetrical arch 8 m wide and 5 m high which leads to a small chamber (still in the daylight zone). In this chamber archaeologists found Palaeolithic artefacts.
5 | P a g e
Fig. 58. Stalagmite YD-K4 in Kulyurtamak cave.
Stalagmite YD-K4. Collected in central part of Kulyurtamak cave, on a ledge (Fig. 58).
The polished slab cut from the central part of Fig. 59. Stalagmite YD-K4, polished slab. the stalagmite is shown in Fig. 59. Locations of samples collected for dating are marked.
6 | P a g e
Fig. A60. Map and vertical cross-section of Victoria cave (including surface topography). Sampling locations are indicated by yellow (stalagmites) and blue (CCC) circles. Survey by S. Tkachev, A. Afanasiev, I. Gaynutdinov, S. Muslukhov, and Y. Sokolov (2012-2016).
8.4. Stalagmites and CCC horizontal gallery of the lower level of the cave. A small stream starts at a sump located from Victoria cave ca 30 m upstream. The stream continues The cave is located near the unpaved road along the gallery for ca 670 m and disappears connecting the villages Shulganovo and in another sump. The gallery has a mean Kutanovo. Cave coordinates: 53.049N, width of 3-6 m and a height ranging from 3 57.045E, altitude 380 m a.s.l. to 10 m. In places the gallery hosts zones of large collapsed blocks as well as small inflows The cave is accessed via a vertical shaft (Fig. of water from side channels or fractures (not 60), starting as a steep karstified fracture, exceeding 0.2 L/s). continuing as a steep undulate solution tube with a vertically elongated cross-section (ca Up to 4 m thick deposits of clay with sand 0.5 1.5 m), then again a steep karstified lenses are exposed on the walls of the fracture, entering, at a depth of 82 m, the gallery; these deposits were cut by the
7 | P a g e
stream (Fig. 61). Stalagmites of Holocene age grow on top of these clay deposits. The stream bed is either bedrock, or, in places, cuts into a flowstone deposit.A flowstone dam is preserved across the channel, creating a small pool. U-Th analysis of the dam flowstone yielded Holocene age (ca 5 ka).
Some 300 m downstream of the entrance shaft, the gallery widens, creating an inclined hall in the western wall. The hall ascends at ca 45° in southwesterly direction; its upper part narrows, leading to the upper level of the cave, located ca 40 m above the lower one. This level consists of a gallery, which morphologically is strikingly similar to the lower gallery except for the absence of a stream. The upper gallery has a canyon-like cross-section and formerly hosted a fast-flowing stream (indicated by small scallops on the walls; Fig. 62a). Similar to the lower gallery, the stream water had Fig. 61. Massive clay and sand deposits cut by the cave become supersaturated with respect stream and exposed along the wall of the lower gallery of to calcite, leading to the deposition of Victoria cave. (a) general view; (b) close-up of red rectangle shown in (a). Note stalagmite of Holocene age on top of the massive flowstone and calcite dams, clay (red arrow). which later were destroyed (dissolved) so that only small traces of the flowstone are left on the passage walls (Fig. 62b).
8 | P a g e
Fig. A62. Upper gallery of Victoria cave. (a) scallops on the right wall indicating fast-flowing water (gallery width ca 1.5 m); (b) remnants of stream bed flowstone and dam on the wall (width of frame ca 3 m).
The cave microclimate is quite stable in the upper gallery, where the temperature is 5.6C throughout the year. In the lower gallery, the air temperature is less stable because of the presence of the stream. The temperature there is stable (5.8C) from July to November. It gradually decreases to 5.5C in December-April and drops abruptly to 4.7C in March-April due to active snowmelt. After mid-April the temperature raises quite fast, reaches 6.1C in June and then gradually decreases to 5.8C by July.
9 | P a g e
The upper gallery hosts abundant speleothems, comprising several generations of stalagmites. Many old stalagmites are broken and overgrown by younger, Holocene flowstone and stalagmites (Fig. 63).
Fig. 63. Broken stalagmites (primarily MIS5e in age) overgrown by younger (Holocene) flowstone and stalagmites in the upper gallery of Victoria cave. Cryogenic calcite was found in the terminal part of the upper gallery (see Fig. 60). It occurs as two distinct layers, white and brownish (Fig. 64), of which the white layer is younger and covers less space.
Fig. 64. Deposits of CCC in the upper gallery of Victoria cave. The white layer of CCC is underlain by a brownish one. Around this block, brown CCC is present on the cave floor (arrows) and is not mantled by white CCC. Width of photo ca 60 cm.
10 | P a g e
Fig. 65. Stalagmites collected in Victoria cave – polished central slabs. (a) VIC1; (b) VIC2; (c) VIC3. Locations of subsamples for dating are marked and labeled.
Slabs cut from central parts of four stalagmites collected from the cave are shown in Fig. 65.
The morphology of cryogenic calcite is shown in Fig. 66. Note that some CCC in this cave show morphologies diagnostic of glendonite – a pseudomorphs of calcite after ikaite.
Fig. 66. CCC from Victoria cave, represented by calcite and glendonite (pseudomorph after ikaite). Images by O. Kadebskaya.
11 | P a g e
Fig. 67. Map and vertical projection of Gryoz cave. Location of stalagmite sample GRZ1 is marked by yellow circle. Survey by Y. Sokolov (1990).
8.5. Stalagmites from Gryoz cave Cave coordinates: 53.027N, 57.011E, altitude 390 m a.s.l. The cave consists of a series of halls and small galleries, connected by short shafts (Fig. 67). The stalagmite was collected in a hall, ca 150 m from the entrance. A slab cut from its central part is shown in Fig. 68.
Fig. 68. Stalagmite collected in Gryoz cave (GRZ1) – polished central slab. Locations of subsamples taken for dating are marked.
12 | P a g e
REFERENCES carbonate crusts reveals Neandertal origin of Iberian cave art. Science 359: 1. Aubert, M., Brumm, A., Ramli, M., 912-915. DOI: 10.1126/science.aap7778 Sutikna, T., Saptomo, E.W., Hakim, B., Morwood, M.J., van den Bergh, G.D., 8. Lyakhnitsky, Y., Minnikov, O., Yushko, A. Kinsley, L., Dosseto, A. (2014): (2015): Paintings and signs of Pleistocene cave art from Sulawesi, Shulgantash (Kapova) cave. Catalogue of Indonesia. Nature 514: 223-228. DOI: images. Ufa: Kitap, 288 p. 10.1038/nature13422 9. Pike A.W.G., Hoffmann D.L., García-Diez 2. Chervyatsova O.Y., Leonova L.V., M., Pettitt P.B., Alcolea J., De Balbín R., Potapov S.S., Lyahnitsky Y.S., Kuzmina González-Sainz C., de las Heras C., L.Y., Zhitenev V.S. (2015): The problem Lasheras J.A., Montes R., Zilhao J. of mineral formation and corrosion on (2012): U-Series Dating ofPalaeolithic the substrates of Palaeolithic art of the Art in 11 Caves in Spain, Science 336: Shulgan-Tash cave. In: Khismatdinova 1409-1413. DOI: F.G., Kotov V.G. Nafikov S.V. (Eds.) 10.1126/science.1219957 Ancient sanctuaries: Archaeology, ritual, 10. Pons-Branchu, E., Bourrillon, R., Conkey, mythology. Materials of International M.W., Fontugne, M., Fritz, C., Gárate, D., Scientific Symposium, Ufa: Institute for Quiles, A., Rivero, O., Sauvet, G., Tosello, History Publishing House. p. 143-156. G., Valladas, H., White, R. (2014): 3. Devlet, E.G, Guillamet, E., Pakhunov, Uranium-series dating of carbonate A.S., Grigoriev, N.N., Gainullin, D.A. formations overlying Palaeolithic art: (2018): Preliminary results of studies of interest and limitations. Bulletin de la the camel figure at the Chamber of Société préhistorique française 111: 211- Chaos at Shulgan-Tash (Kapova) cave. 224. Ural Histor. Journ. 1(58): 126-133. 4. Fairchild I.J., Baker A. (2012): Speleothem science. From Process to Past Environments. Willey-Blackwell. ISBN: 978-1-405-19620-8 5. Hellstrom, J. (2012): Absolute Dating of Cave Art, Science 336: 1387-1388. DOI: 10.1126/science.1224185 6. Hoffmann, D.L., Pike, A.W.G., García- Diez, M., Pettitt, P.B., Zilhão, J. (2016): Methods for U-series dating of CaCO3 crusts associated with Palaeolithic cave art and application to Iberian sites, Quaternary Geochronology 36: 104-119. DOI: 10.1016/j.quageo.2016.07.004 7. Hoffmann D.L., Standish C.D., García- Diez M., Pettitt P.B., Milton J.A., Zilhão J., Alcolea-González J.J., Cantalejo-Duarte P., Collado H., de Balbín R., Lorblanchet M., Ramos-Muñoz J., Weniger G.-Ch., Pike A.W.G. (2018): U-Th dating of 13 | P a g e