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Phytolith and FTIR studies applied to combustion structures: The case of the Middle Paleolithic site of El Salt (Alcoy, Alicante)
Quaternary International xxx (2015) 1e11
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Phytolith and FTIR studies applied to combustion structures: The case of the Middle Paleolithic site of El Salt (Alcoy, Alicante) Agata Rodríguez-Cintas, Dan Cabanes*, 1 gica i Arqueom Equip de Recerca Arqueolo etrica Universitat de Barcelona (ERAAUB), Department of Prehistory, Ancient History and Archaeology, University of Barcelona, c/de Montalegre 6-8, 08001, Barcelona, Spain
a r t i c l e i n f o
a b s t r a c t
Article history: Available online xxx
The combination of phytolith and FTIR analyses is a powerful tool to investigate the use of fire by past human populations. Here, we apply these methods to study the hearths of the subunit Xb at the Middle Palaeolithic site of El Salt, in Alcoi. El Salt is characterized by recurrent Neanderthal occupations that produced a succession of combustion structures and other anthropogenic remains. Using FTIR analysis we have been able to detect the presence of ashes, thermally altered clay, and phosphatic minerals in the sediments. Phytolith results point to the use of wood as fuel in subunit Xb. However, most of the phytoliths have been deposited in the site by natural agents, probably in the form of bird guano characterized by the presence of distinctive phytoliths of seed coats from Celtis sp. Differentiating between natural and anthropogenic deposited phytoliths is essential to evaluate the impact produced by human activities in the archaeological sediments. © 2015 Elsevier Ltd and INQUA. All rights reserved.
Keywords: Phytoliths FTIR Hearths Middle Palaeolithic Guano Celtis
1. Introduction The understanding, control and production of fire are a keystone in Human Evolution that produced physical, cognitive and social changes in early human populations (Heizer, 1963; s, 1977). The human control of fire has a seOakley, 1970; Perle ries of adaptive advantages that have been largely discussed in the specialized literature (Heizer, 1963; Cook, 1964; Oakley, 1970; s, 1977). Among other advantages, Gregg and Grybush, 1976; Perle fire allowed humans to expand into regions with colder climates, enlarged human's diet by increasing the range of edible food, and increased the number of working hours and social activities by producing artificial illumination (Oakley, 1970; Leopold and Ardrey, 1972; Stahl et al., 1984; Wrangham et al., 1999). However, when and how humans accomplished a complete control of fire, including its production by archaic populations such as the Neanderthals, is still a debated issue (James, 1989; Weiner et al., 1998; Sandgathe et al., 2011; Berna et al., 2012). Albeit this
* Corresponding author. E-mail addresses: [email protected], [email protected] (D. Cabanes). 1 Current address: Plant Foods in Hominin Dietary Ecology Research Group, Max Planck Institute for Evolutionary Anthropology, Deutscher Platz 6, 04103 Leipzig, Germany.
controversy multiple evidences of deliberate use of fire by Neanderthals has been reported from the Levant and Europe (Albert et al., 1999, 2000, 2003; Madella et al., 2002; Rosen, 2003; Cabanes et al., 2007, 2010; Albert and Cabanes, 2008; Mallol et al., 2010; Aldeias et al., 2012; Fern andez Peris et al., 2012; Goldberg et al., 2012; Vallverdú et al., 2012, and references therein). Defining the preservation state of the combustion structures is a critical aspect to approach the use and control of fire by Neanderthals. Combustion structures might preserve or not depending on numerous aspects such as climatic conditions, sedimentation rates, diagenesis, type of fuel used, and post-depositional disturbation caused by humans or other biogenic agents (Weiner and Goldberg, 1990; Meignen et al., 2001). One of the most successful approaches to define the origin and preservation of combustion structures is the study of the sediment mineralogy by means of Fourier Transformed Infrared Spectroscopy (FTIR) combined with phytoliths analysis from hearths remains (Schiegl et al., 2004; et al., Schiegl and Conard, 2006; Cabanes et al., 2007, 2010; Allue 2012; Mallol et al., 2013; Shahack Gross et al., 2014). Here, we present new evidence from el Salt site hearths from subunit Xb, which follows the previous micromorphology, phytolith and FTIR analyses conducted in the subunit Xa (Mallol et al., 2013). We applied FTIR analysis to identify the presence of calcitic
http://dx.doi.org/10.1016/j.quaint.2015.09.043 1040-6182/© 2015 Elsevier Ltd and INQUA. All rights reserved.
Cabanes, D., Phytolith and FTIR studies applied to combustion structures: The case of the Please cite this article in press as: Rodríguez-Cintas, A., Middle Paleolithic site of El Salt (Alcoy, Alicante), Quaternary International (2015), http://dx.doi.org/10.1016/j.quaint.2015.09.043
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Fig. 1. Map showing the location of El Salt.
ash remains and thermally altered sediments and we used phytolith analysis to study fuel management and human behaviour patterns in relation with fire control. 2. The site El Salt is a Middle Palaeolithic site located in the South East of the Iberian Peninsula (Fig. 1). The site is located in the South East side of the Sierra de Mariola, in Alcoy (Alicante, Spain) at 680 m above sea level, close to the Serpis and Barxell rivers. This area forms part of the mesomediterranean belt. The current annual precipitation is above 500 mm and mean temperature is 14 C (Rivas Martínez, 1987). Vegetation cover is often characterized by Quercus, coniferous forests and Juniperus are sometimes developed. Steppe formations are characterized by Poaceae (such as Stipa and Lygeum), Asteraceae, Chenopodiaceae (such lez-Sampe riz et al., 2010). The as Salsola and Suaeda) (Gonza vicinity of other Middle Palaeolithic sites as Abric del Pastor, Cova Beneito, and Coves d'Estroig, in addition to lithic raw material provisioning zones, makes this area especially active during the Middle Palaeolithic (Iturbe et al., 1993; Faus, 2000;
n et al., 2009; Machado et al., Barciela and Molina, 2005; Galva 2013; etc.). The Middle Paleolithic sedimentary sequence at El Salt has provided dates between 60.7 ± 8.9 and 45.2 ± 3.4 ka BP (Galv an et al., 2014b). These dates place Middle Paleolithic occupations at el Salt during MIS 3, which in the Iberian Peninsula is characterized by variable climate conditions with abrupt climatic changes (Kehl et al., 2014). Vegetation landscapes were highly heterogeneous and responses to differences on climate, geology and altitudinal gradients n and Munuera, 1997; Moreno et al., have been described (Carrio 2012). Pollen and charcoal sequences in the area show dry steppe formations next to coniferous woodland, and an important Mediterranean component including evergreen Quercus, Olea, Pistacia, lez-Sampe riz et al., 2010). and Myrtus during MIS3 (Gonza Thirteen stratigraphic units (S.U.) were described by Fumanal (1994) and grouped in five segments according to the archaeological remains and macroscopic features (Fig. 2a). The first segment, at the base of the sequence, is formed by an archaeologically sterile travertine platform (Unit XIII). The second segment (Units XII-IX) shows the highest concentration of combustion structures and archaeological remains. The third segment (Unit VIII to the lower half of Unit V) shows a decrease of anthropogenic impact and an increase of natural sedimentation with an accumulation of large blocks in Unit VI. Nevertheless, six teeth attributed to a Neanderthal adult were recovered from the base of Unit V (Garralda et al., 2014). The upper half of Unit V, which is archaeologically sterile, forms the fourth segment. The last segment encompasses Units IV-I, which contains Holocene sediments with reworked Upper Palaeolithic, n et al., 2014b). Mesolithic, and Neolithic materials (Galva Archaeological excavations at El Salt have been carried out systematically since 1986. Lately, an integrated multidisciplinary analyses of the archaeological and sedimentary records was carn et al., ried out to examine the archaeological palimpsest (Galva 1991, 2006a, 2006b, 2014a, 2014b; Fumanal, 1994; Dorta et al., mez de la Rua et al., 2010; Machado et al., 2011; 2010; Go Marrero et al., 2011; Sistiaga et al., 2011, 2014; Mallol et al., ndez et al., 2014). 2013; Garralda et al., 2014; Herna Stratigraphic unit X has been dated around 50 ka BP, and to date has provided the greater amount of archaeological remains. For excavation purposes the stratigraphic unit X has
Fig. 2. Stratigraphic units at el Salt and excavation surface in unit X a) stratigraphic scheme showing the main sedimentary features (extracted from Garralda et al., 2014); b) detail of the excavation surface in unit X.
Cabanes, D., Phytolith and FTIR studies applied to combustion structures: The case of the Please cite this article in press as: Rodríguez-Cintas, A., Middle Paleolithic site of El Salt (Alcoy, Alicante), Quaternary International (2015), http://dx.doi.org/10.1016/j.quaint.2015.09.043
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Fig. 3. Location of the combustion structures and control samples analysed in subunit Xb. Scale bar in the pictures is 1 m.
been divided macroscopically in subunits Xa and Xb. During the excavation of this S.U. a total of 60 combustion structures (CS) have been identified. The hearths from S.U. X were concentrated near the travertine wall and were associated with faunal and lithic remains (Fig. 2b). The macrofaunal assemblage was characterized by goat (Capra pyrenaica), deer (Cervus elaphus) and horse (Equus ferus and Equus hydruntinus). Also, small mammals such as lagomorphs (Oryctolagus cuniculus) were present. Occasionally Bos primigenius, turtles (Testudo hermani) and carnivore remains were recovered from this unit. Lithic production was principally based on the exploitation of diverse siliceous raw materials gathered within a 25 km distanceeradius (Galv an et al., 2014a). Knapping systems were mainly ascribed
to the recurrent centripetal and the directional Levallois schemes, although the representation of non-Levallois directional methods was also significant. The introduction of single blanks, retouched or not, as well as the on-site recycling of artefacts were usual technical features of S.U. X assemblages. The predominance of scrapers among the retouched tools was also remarkable. 3. Materials and methods A total of 25 loose sediment samples were collected from the fresh exposed surface of the combustion structures in the subunit Xb during the 2013 field season (Table 1). Control
Cabanes, D., Phytolith and FTIR studies applied to combustion structures: The case of the Please cite this article in press as: Rodríguez-Cintas, A., Middle Paleolithic site of El Salt (Alcoy, Alicante), Quaternary International (2015), http://dx.doi.org/10.1016/j.quaint.2015.09.043
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samples, with no visual indication for thermal alteration, were collected from the same stratigraphic unit (Table 1 and Fig. 3). Morphologically, these combustion structures are ovalshaped and show a recurrent stratigraphy formed by two discrete layers: a) ash layer: white-coloured fine grained sediment at the top of the structure, and b) black layer: blackcoloured organic rich sediment at the base of the structure (Fig. 4). No reddening of the sediment was identified below the black layer in these structures. When possible, at least one sample of each layer was collected for analyses. However, some hearths show signs of weathering and erosion by geological and biological agents that altered the black layer and, in some cases, removed the ash layer. Only in the hearths H44b, H48, H51, H52 and H53 were the ash layers visually identified in the field. Faunal and lithic remains are abundant in both layers, and travertine blocks and limestone cobbles were recovered in a lesser extent (Table 2).
Fig. 4. Detail view of hearth H52 showing the two-layered stratigraphy formed by a top ash layer and a subjacent black layer. Table 1 Main results of the samples analysed in S.U. Xb. Combustion structure
Sample
Hearth field layer identification
FTIR
Calcite origin
Phyt. in 1 g of sediment (millions)
% Anatomically connected phytoliths
Average cell number in anatomical connected phytoliths
% Weathered morphotypes
%Melted morphotypes
H44b
H48
31 32 57 7 8 21
Ash layer Black layer Black layer Black layer Black layer Ash layer
Cl (b) ¼ Ca, Dah, Qz Cl (nb), Ca, Dah, Qz Ca]Cl (b?), Qz, Dah Cl (nb), Ca, Dah, Qz Cl (nb), Ca, Qz, Dah Ca, Cl (b), Dah, Qz
3.7 2.3 3.3 1.9 3.9 2.3
15.2 11.1 5.9 6.7 2.2 0
5.6 3.1 2.4 3.2 2.5 0
5.07 9.52 4.50 11.34 4.89 8.86
0 0 0 0 0 0
H49
22 28
Black layer Black layer
Ca, Cl (b?), Dah, Qz Ca]Cl (nb), Dah, Qz
1.7 3.2
0.7 10.3
2.0 5.2
11.57 2.67
0 0
H51b H52
9 10 15 19 23
Ash layer Ash layer Black layer Black layer Ash layer
Cl (b), Ca, Dah, Qz Cl (nb), Ca, Dah, Qz Cl (nb), Ca, Dah, Qz Cl (nb), Ca, Dah, Qz Ca, Cl (b), Qz
3.6 4.9 3.6 2.5 1.2
41.3 5.5 21.1 6.6 36.7
9.3 2.8 5.7 4.0 4.5
7.86 11.37 8.36 13.93 9.04
0.24 0 0 0 0.30
H53a H53a-b
24 33 35
Cl (nb), Ca, Dah, Qz Ca]Cl (b?), Qz. Dah Ca]Cl (nb), Qz, Dah
2.4 2.6 4.1
35.0 15.6 5.2
9.2 4.8 3.3
4.61 8.64 10.48
0 0 0
36 37
Black layer Ash layer Sediment between hearths Black layer Ash layer
Geogenic Geogenic Geogenic Geogenic Geogenic Anthropogenic (ash) Geogenic Anthropogenic (ash) Geogenic Geogenic Geogenic Geogenic Anthropogenic (ash) Geogenic Geogenic Geogenic
Ca]Cl (b?), Qz, Dah Ca, Cl (b), Qz
3.9 1.1
19.2 7.0
6.9 4.0
9.44 20.26
0 0.44
38 39 29 30 75 (104) 81 (420) 87 (108)
Ash layer Black layer Black layer Ash layer Control Control Control
Cl (b) ¼ Ca, Qz, Dah Cl (nb), Ca, Qz, Dah Cl (nb), Ca, Dah, Qz Cl (b), Ca, Dah, Qz Cl (nb), Ca, Dah, Qz Ca, Cl (nb), Dah, Qz Cl (nb), Ca, Dah, Qz
3.1 4.9 3.0 5.3 3.2 0.5 3.5
4.4 6.1 32.4 41.3 6 0 0
2.8 3.0 5.7 6.7 3 0 0
10.32 9.80 3.72 4.17 8.7 16.7 6.4
0 0 0 0 0 0 0
H45 H46
H51a
H53b
H54 Control samples
Geogenic Anthropogenic (ash) Geogenic Geogenic Geogenic Geogenic Geogenic Geogenic Geogenic
Ca ¼ calcite; Cl ¼ clay; Dah ¼ dahllite; Qz ¼ quartz; (b) ¼ thermally altered clay; (nb) ¼ not thermally altered clay. Minerals are arranged according to their relative peak heights in the FTIR spectrum. Table 2 Presence or absence of faunal and lithic remains, and travertine and limestone fragments in the hearths of subunit Xb. The asterisk indicates the hearths with the uppermost ash layer identified in the field. Faunal remains
H44b* H45 H46 H48* H49 H51* H52* H53* H54*
Flint artifacts
Burnt
Unburnt
Burnt
X e e X e X X X e
e X X
X e e
e e e X e
e X e e e
Travertine Unburnt X X X e e e e e
Limestone
Burnt
Unburnt
Burnt
X X X
e e e
X e X
e X e X e
e e e e e
e e e e e
Cabanes, D., Phytolith and FTIR studies applied to combustion structures: The case of the Please cite this article in press as: Rodríguez-Cintas, A., Middle Paleolithic site of El Salt (Alcoy, Alicante), Quaternary International (2015), http://dx.doi.org/10.1016/j.quaint.2015.09.043
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Mineralogical analysis was carried out using an iS5 FT-IR Nicolet Thermo Scientific Spectrometer. Infrared spectra were obtained using Kbr pellet at 4 cm1 resolution. The origin of calcite, i.e. geogenic or anthropogenic (i.e. ashes), was determined following Regev and Poduska (Regev et al., 2010; Poduska et al., 2011), and clays exposed to high temperatures were identified using specific absorptions in the clay spectrum (Berna et al., 2007). Phytolith extraction followed the method developed by Katz et al. (2010). Between 30 and 40 mg of dry sediment were weighed, transferred to plastic tubes, and 50 ml of 6 N HCl were added to dissolve the carbonates. Then 450 ml of sodium polytungstate at 2.4 g/ml density were added and phytoliths and lighter elements were separated from the rest of the fraction by centrifugation at 5000 rpm for 5 min. The supernatant was then transferred to another tube and 50 ml were placed in a microscope slide to proceed with phytolith identification and quantification. Phytoliths were counted and identified using an Olympus BX-41 optical microscope at 200 and 400. At least 200 individual phytoliths were identified in each slide. Morphological ascription was carried out using the standard literature (Twiss et al., 1969; Brown, 1984; Mulholland and Rapp, 1992; Rosen, 1992; Piperno, 2006). When possible the International Code for Phytolith Nomenclature was followed (Madella et al., 2005). 4. Results 4.1. FTIR results The main minerals forming the sediments analysed are clay and calcite, whereas quartz and dahllite are present in lower concentrations. Anthropogenic calcite (i.e. ashes) is only present in three out of nine ash layers identified in the field (H48, H52 and H53b) and in one of the black layers (H49). The other ash layers samples show calcite of geogenic origin. Clay is thermally altered in all the ash layers sampled and in the black layer from the combustion structures H45, H48 and H53b (Table 1). Control samples are mainly composed by unaltered clay and geogenic calcite (Table 1). 4.2. Phytolith concentration and preservation Phytolith concentrations and morphotypes are homogenous in all the combustion structures despite their mineralogical composition, coloration and stratigraphic position. Phytolith concentrations in the combustion structures range from 1.1 to 5.3 million per gram of sediment, and most of the samples show values between 2 and 4 million of phytolith per gram of sediment (Table 1). Note that the ash layer samples from the combustion structures H52 and H53b contain relatively low concentrations of phytoliths, around 1 million phytoliths per gram of sediment (Table 1). The percentage of weathered phytoliths is relatively low in all the samples (12%), with the notable exception of the ash layer from the combustion structure of H53 where weathered morphotypes reach values above 20%. Melted phytoliths, produced by high temperatures, are identified in the ash layers from H52 and H53b. Control samples show similar values of phytolith concentrations. Samples 75 and 87, collected close to the hearths, show a concentration around 3 million phytoliths per gram of sediment and a low percentage of weathered morphotypes (6.4%). On the other hand, control sample 81, located farther from hearths shows a lower concentration of phytoliths (0.5 millions) and the highest percentage of weathered phytoliths among the control samples (Table 1).
5
4.3. Phytolith morphotypes Fig. 5 shows the results for the phytolith morphotypes identification in the ash layers, black layers, and control samples. In the ash and black layers most of the phytolith identified have been formed in monocotyledonous plants, which include grasses, sedges, and generic monocotyledonous morphotypes that can be found in both grasses and sedges (Twiss et al., 1969; Rosen, 1992; Bamford et al., 2006). Leaf and stem phytoliths from grasses are overrepresented in most of the samples, with the exceptions of the black layer sample of H54 and one of the ash layer sample of H51. Phytoliths in anatomical connection from monocotyledonous plants are usually formed by long cells in combination with short cells or papillae (Fig. 6aeb and Fig. 7). Most of the grass short cells belong to C3 pooid (festucoid) type (rondel and rondel tower), whereas C4 chloridoid (saddle) and C4 panicoid (lobate forms) are present in lower concentrations (Fig. 8). Because most of the phytoliths recovered belong to grasses it can be assumed that generic monocotyledonous morphotypes derived also from these plants. Control samples produce similar results showing phytolith assemblages mainly composed by grasses with a high presence of C3 grass short cells (Fig. 5c). Phytolith morphotypes from wood and bark show values that range between 2 and 14%, whereas phytoliths from dicotyledonous leaves show in general lower percentages (0.5e8%). Multicellular polyhedral and jigsaw puzzle structures have been recovered despite their low preservation in archaeological sediments and natural soils (Piperno, 2006) (Figs. 6c and 7). Irregular verrucate phytoliths from dicotyledonous seeds and fruits are present in all the samples in different amounts (Figs. 5 and 6d). These are especially abundant in the form of multicellular structures in the black layer samples (Fig. 7b). Some of these morphotypes are originated in Celtis sp. seed coats (Fig. 6d) and have been previously identified in S.U. Xa (Mallol et al., 2013). Phytolith assemblages in control samples are mostly formed by grass and generic monocotyledonous morphotypes. Wood and bark and dicotyledonous leaf morphotypes show low percentages, and seed/fruit phytoliths are present in all the control samples in considerable amounts (Fig. 5c). Fig. 9 shows the distribution of the main phytolith morphotypes categories according to the calcite FTIR's identification for the hearth samples and control samples. No significant differences can be observed on the distribution of the main phytolith categories, with the exception of dicotyledonous fruit/seed phytoliths, which are underrepresented in the anthropogenic calcite (i.e. ash) samples. 5. Discussion The presence of anthropogenic calcite in the ash layers of H48, H52 and H53b, in concurrence with the presence of thermally altered clay and small amounts of melted phytoliths in H52 and H53b points to an in situ preservation of the ash remains in these combustion structures. However, the remaining combustion structures do not show mineralogical evidence for ashes in the layers identified in the field as ash layer, although the clay mineral was thermally altered. This is probably due to the dissolution of ashes or their mixing with the geogenic matrix by syndepositional or postdepositional processes. Dahllite is present in low amounts in all the samples, indicating that calcite diagenesis is still in the initial stages (Karkanas et al., 2000). The presence of dahllite can be related to the deposition of bird guano containing high amounts of phosphates (Shahack-Gross et al., 2004).
Cabanes, D., Phytolith and FTIR studies applied to combustion structures: The case of the Please cite this article in press as: Rodríguez-Cintas, A., Middle Paleolithic site of El Salt (Alcoy, Alicante), Quaternary International (2015), http://dx.doi.org/10.1016/j.quaint.2015.09.043
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Rodríguez-Cintas, D. Cabanes / Quaternary International xxx (2015) 1e11 A.
Fig. 5. Phytolith morphotype identification and anatomical origin in a) ash layer, b) black layer, and c) control samples.
Phytolith assemblages in unit Xb seem to be fairly well preserved; the percentage of weathered phytolith is relatively low in most of the samples, phytolith with delicate decorations have been identified, and phytoliths with an assumed large surface area to volume ratio, such as polyhedrals or jigsaw puzzles, have been recovered (Cabanes et al., 2011; Cabanes and ShahackGross, 2015). The presence of wood and bark phytoliths indicates the use of the use of wood as fuel in the hearths studied. Moreover, no significant amount of highly fragmented burnt bones was identified during the excavation, ruling out bone as a main source of fuel (Yravedra and Uzquiano, 2013) and as the origin of dahllite. Nevertheless, the presence of wood and bark phytoliths is low in all the samples when compared to the monocotyledonous percentages. Grasses are higher
accumulators of silica than woody dicotyledonous, producing higher amounts of phytoliths per gram of original plant material (Albert and Weiner, 2001). In addition, grass phytoliths can be present in the form of contamination (up to 30% of the assemblage) in woody dicotyledonous plants (Albert and Weiner, 2001; Tsarsidou et al., 2007). However, here the presence of monocotyledonous morphotypes, including grass and generic monocotyledonous, ranges from 41 to 75% of the phytoliths identified. Therefore, grasses might have been deposited in the sediment by ways other than wood and bark contamination. In previous works, the presence of high percentage of monocotyledonous morphotypes have been linked to the existence of a grass bedding in Mousterian occupations at el Esquilleu site (Cabanes et al., 2010; Mallol et al., 2010) and MSA layers at
Cabanes, D., Phytolith and FTIR studies applied to combustion structures: The case of the Please cite this article in press as: Rodríguez-Cintas, A., Middle Paleolithic site of El Salt (Alcoy, Alicante), Quaternary International (2015), http://dx.doi.org/10.1016/j.quaint.2015.09.043
Fig. 6. Light microscope images of phytolith morphotypes recovered in the hearth samples. a) Elongate cell altered from hearth H46 (sample 8); b) Melted phytolith from hearth H52 (sample 23); c) Rugulate long cells in anatomical connection from monocotyledonous leaf in hearth H54 (sample 30); d) Wavy long cells and rondel short cells in anatomical connection from grasses in hearth H54 (sample 30); e) Jig-saw puzzle multicellular structure formed in dicotyledonous leaf in hearth H51a (sample 9); f) Spheroid psilate from wood/bark in hearth H48 (sample 22); g) Multicellular structure formed by irregular verrucate morphotypes, probably from Celtis sp. seed coats, in hearth H44b (sample 32); h) Irregular verrucate morphotype in hearth H54 (sample 30).
Cabanes, D., Phytolith and FTIR studies applied to combustion structures: The case of the Please cite this article in press as: Rodríguez-Cintas, A., Middle Paleolithic site of El Salt (Alcoy, Alicante), Quaternary International (2015), http://dx.doi.org/10.1016/j.quaint.2015.09.043
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Fig. 7. Percentage of monocotyledonous, dicotyledonous leaf, and dicotyledonous seed/fruit morphotypes in anatomical connection: a) ash layer, b) black layer, and c) control samples.
Sibudu rockshelter (Wadley et al., 2011). In both cases the presence of a high number of phytoliths in anatomical connection, identified both in thin section and phytolith analysis, pointed to the existence of monocotyledonous leaf beddings. The percentage of anatomically connected phytoliths from grasses in S.U. Xb is low in most of the samples analysed, and only increase when multicellular structures formed in dicotyledonous fruit/seeds coats are also present in high amounts (Fig. 7). The most noticeable exception is the ash layer sample from H52 where monocotyledonous phytoliths in anatomical connection represent more than 30% of the phytolith assemblage. In the rest of the samples when anatomically connected phytoliths are present in high amounts these are formed almost exclusively by dicotyledonous seed/fruit morphotypes. Micromorphological analyses carried out in subunit Xb (Mallol et al., 2013) have not revealed the presence of any bedding structure so far. Postdepositional processes implying the sediment reworking or phytolith dissolution might lead to the disarticulation of anatomically connected phytoliths (Cabanes et al., 2009, 2010, 2012; Jenkins, 2009). However, in S.U Xb the different degree of anatomical connection between fruits/seeds
and grasses rules out postdepositional processes as responsible for the disarticulation of anatomically connected phytoliths. Biostratinomic processes in this case might have regulated the degree of phytolith anatomical connection. The fruit/seed phytoliths recovered from in S.U. Xb are very similar to those of hackberry (Piperno, 2006), and Celtis sp. seed coats seeds have been previously identified in the site (Mallol et al., 2013). Mediterranean hackberry seeds have been identified in other European Palaeolithic sites (Laville and nault-Miskovsky, 1977; Allue et al., 2015). However, the curRe rent distribution of Mediterranean hackberry trees in solitary individuals or small groups is related to dispersal of fruits by frugivores, primary birds and occasionally by other vertebrates (Traba et al., 2006). The data presented here shows a higher accumulation of fruit/seed phytoliths in the sediments with lower anthropogenic component (Fig. 9). In addition, multicellular structures from dicotyledonous seed/fruit are more abundant in the black layer, which results from the accidental combustion of previously deposited materials in the site (Mallol et al., 2013). Thus, phytolith assemblage composition in S.U. Xb points out to an accumulator agent other than humans for most of these microbotanical remains. The most parsimonious explanation for the presence of Mediterranean hackberry phytoliths in the site is their introduction in the form of bird guano, which is in accordance with the presence of phosphatic minerals showed by FTIR analysis. Phytolith concentration and composition of the control samples also points out to a natural origin of the phytolith recovered, however the presence of small amounts of ashes dispersed by trampling could explain the low percentages of wood and bark phytoliths detected in the control samples (Cabanes et al., 2007). Additionally, preceding analyses in the subjacent S.U. Xa show as well a natural origin for most of the phytoliths assemblages recovered in the combustion structures investigated (Mallol et al., 2013). The fuel used (i.e. wood) and the archaeological remains related to the combustion structures indicate that the hearths analysed here are rather simple and without any specialized function. The low anthropogenic impact in the sediments and the presence of phytoliths deposited by natural agents indicate a low sedimentation rate for S.U. Xb and an ephemeral nature of the combustion structures. In this sense, the presence of 60 discrete combustion structures in this stratigraphic unit is probably the result of a palimpsest overlapping different occupations events, rather than the consequences of an exceptional occupation intensity. However, the area studied here is relatively small and further excavation and sampling will be necessary to confirm that the remaining combustion structures in S.U. Xb follow the same pattern. Despite the simplicity of the combustion structures studied so far, the data obtained from el Salt shows that Neanderthal populations have full capacity to start and control a fire each time they visited the site, regardless of the duration or the intensity of the occupation. 6. Conclusions Phytolith and FTIR analysis of the combustion structures points out to natural deposition of the sediments in S.U. Xb. Albeit sediment preservation conditions are fairly good the anthropogenic sedimentary signal is limited to few evidences of ash, thermally altered clay and low amounts of wood and bark phytoliths derived from the fuelwood used in the combustion structures. The hearths analysed can be considered the result of ephemeral activity, which did not last long enough to leave a clearer anthropogenic signal in the sediments. Further research is
Cabanes, D., Phytolith and FTIR studies applied to combustion structures: The case of the Please cite this article in press as: Rodríguez-Cintas, A., Middle Paleolithic site of El Salt (Alcoy, Alicante), Quaternary International (2015), http://dx.doi.org/10.1016/j.quaint.2015.09.043
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Fig. 8. Light microscope images of grass short cells identified in the hearth samples. a) Pooid (festucoid) short cells in hearth H48 sample 21, note the partial dissolution observed on the top of both short cells: 1. Rondel short cell. 2. Rondel tower short cell; b) Rondel tower short cell from hearth H51b sample 19; c) rondel short cell from hearth H51b sample 19; d) polylobate short cell from hearth H45 sample 57.
neo de los grupos neandertales en la region central del Mediterra rico. Una propuesta metodolo gica de aproximacio n al proceso Ibe rico y al marco paleoambiental’ (HAR2012-32703, MICINNhisto FEDER) and the Cultural Heritage Department of the Valencia Government, under the direction of Professor Bertila Galv an of Universidad de La Laguna. D. Cabanes has been supported by a Juan de la Cierva post-doctoral contract (JCI-2011-10972). This research is part of the activities of the ERAAUB (2014 SGR 845), thanks to the del DIEU, support of Comissionat d'Universitats, Recerca i Innovacio Generalitat de Catalunya.
90 80 70 60
%
50 40 30 20
References
10 0 Monocotyledonous
Wood/Bark
Dicotyledonous leaf
Antropogenic calcite (ash)
Dicotyledonous fruit/seed
Geogenic calcite
Weathered
Control samples
Fig. 9. Main phytolith morphotypes categories averaged according to the origin of calcite in FTIR analysis. Error bars indicate 1s standard deviation.
necessary to determine if the main activity area was located elsewhere, and therefore missed in the current study, or by the contrary, if the low anthropogenic signal was the result of short sporadic visits to the site by small groups of Neanderthals. The data obtained indicate that Neanderthal populations at El Salt were capable of starting and controlling fire using nonspecialized combustion structures. Acknowledgements We thank to the members of the research team “Sociedades cazadoras-recolectoras paleolíticas” based at Universidad de La Laguna for their support and help with field tasks. Archaeological n research at El Salt is funded by Spanish IþD Project ‘La Desaparicio
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Phytolith and FTIR studies applied to combustion structures: The case of the Middle Paleolithic site of El Salt (Alcoy, Alicante) Agata Rodríguez-Cintas, Dan Cabanes*, 1 gica i Arqueom Equip de Recerca Arqueolo etrica Universitat de Barcelona (ERAAUB), Department of Prehistory, Ancient History and Archaeology, University of Barcelona, c/de Montalegre 6-8, 08001, Barcelona, Spain
a r t i c l e i n f o
a b s t r a c t
Article history: Available online xxx
The combination of phytolith and FTIR analyses is a powerful tool to investigate the use of fire by past human populations. Here, we apply these methods to study the hearths of the subunit Xb at the Middle Palaeolithic site of El Salt, in Alcoi. El Salt is characterized by recurrent Neanderthal occupations that produced a succession of combustion structures and other anthropogenic remains. Using FTIR analysis we have been able to detect the presence of ashes, thermally altered clay, and phosphatic minerals in the sediments. Phytolith results point to the use of wood as fuel in subunit Xb. However, most of the phytoliths have been deposited in the site by natural agents, probably in the form of bird guano characterized by the presence of distinctive phytoliths of seed coats from Celtis sp. Differentiating between natural and anthropogenic deposited phytoliths is essential to evaluate the impact produced by human activities in the archaeological sediments. © 2015 Elsevier Ltd and INQUA. All rights reserved.
Keywords: Phytoliths FTIR Hearths Middle Palaeolithic Guano Celtis
1. Introduction The understanding, control and production of fire are a keystone in Human Evolution that produced physical, cognitive and social changes in early human populations (Heizer, 1963; s, 1977). The human control of fire has a seOakley, 1970; Perle ries of adaptive advantages that have been largely discussed in the specialized literature (Heizer, 1963; Cook, 1964; Oakley, 1970; s, 1977). Among other advantages, Gregg and Grybush, 1976; Perle fire allowed humans to expand into regions with colder climates, enlarged human's diet by increasing the range of edible food, and increased the number of working hours and social activities by producing artificial illumination (Oakley, 1970; Leopold and Ardrey, 1972; Stahl et al., 1984; Wrangham et al., 1999). However, when and how humans accomplished a complete control of fire, including its production by archaic populations such as the Neanderthals, is still a debated issue (James, 1989; Weiner et al., 1998; Sandgathe et al., 2011; Berna et al., 2012). Albeit this
* Corresponding author. E-mail addresses: [email protected], [email protected] (D. Cabanes). 1 Current address: Plant Foods in Hominin Dietary Ecology Research Group, Max Planck Institute for Evolutionary Anthropology, Deutscher Platz 6, 04103 Leipzig, Germany.
controversy multiple evidences of deliberate use of fire by Neanderthals has been reported from the Levant and Europe (Albert et al., 1999, 2000, 2003; Madella et al., 2002; Rosen, 2003; Cabanes et al., 2007, 2010; Albert and Cabanes, 2008; Mallol et al., 2010; Aldeias et al., 2012; Fern andez Peris et al., 2012; Goldberg et al., 2012; Vallverdú et al., 2012, and references therein). Defining the preservation state of the combustion structures is a critical aspect to approach the use and control of fire by Neanderthals. Combustion structures might preserve or not depending on numerous aspects such as climatic conditions, sedimentation rates, diagenesis, type of fuel used, and post-depositional disturbation caused by humans or other biogenic agents (Weiner and Goldberg, 1990; Meignen et al., 2001). One of the most successful approaches to define the origin and preservation of combustion structures is the study of the sediment mineralogy by means of Fourier Transformed Infrared Spectroscopy (FTIR) combined with phytoliths analysis from hearths remains (Schiegl et al., 2004; et al., Schiegl and Conard, 2006; Cabanes et al., 2007, 2010; Allue 2012; Mallol et al., 2013; Shahack Gross et al., 2014). Here, we present new evidence from el Salt site hearths from subunit Xb, which follows the previous micromorphology, phytolith and FTIR analyses conducted in the subunit Xa (Mallol et al., 2013). We applied FTIR analysis to identify the presence of calcitic
http://dx.doi.org/10.1016/j.quaint.2015.09.043 1040-6182/© 2015 Elsevier Ltd and INQUA. All rights reserved.
Cabanes, D., Phytolith and FTIR studies applied to combustion structures: The case of the Please cite this article in press as: Rodríguez-Cintas, A., Middle Paleolithic site of El Salt (Alcoy, Alicante), Quaternary International (2015), http://dx.doi.org/10.1016/j.quaint.2015.09.043
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Fig. 1. Map showing the location of El Salt.
ash remains and thermally altered sediments and we used phytolith analysis to study fuel management and human behaviour patterns in relation with fire control. 2. The site El Salt is a Middle Palaeolithic site located in the South East of the Iberian Peninsula (Fig. 1). The site is located in the South East side of the Sierra de Mariola, in Alcoy (Alicante, Spain) at 680 m above sea level, close to the Serpis and Barxell rivers. This area forms part of the mesomediterranean belt. The current annual precipitation is above 500 mm and mean temperature is 14 C (Rivas Martínez, 1987). Vegetation cover is often characterized by Quercus, coniferous forests and Juniperus are sometimes developed. Steppe formations are characterized by Poaceae (such as Stipa and Lygeum), Asteraceae, Chenopodiaceae (such lez-Sampe riz et al., 2010). The as Salsola and Suaeda) (Gonza vicinity of other Middle Palaeolithic sites as Abric del Pastor, Cova Beneito, and Coves d'Estroig, in addition to lithic raw material provisioning zones, makes this area especially active during the Middle Palaeolithic (Iturbe et al., 1993; Faus, 2000;
n et al., 2009; Machado et al., Barciela and Molina, 2005; Galva 2013; etc.). The Middle Paleolithic sedimentary sequence at El Salt has provided dates between 60.7 ± 8.9 and 45.2 ± 3.4 ka BP (Galv an et al., 2014b). These dates place Middle Paleolithic occupations at el Salt during MIS 3, which in the Iberian Peninsula is characterized by variable climate conditions with abrupt climatic changes (Kehl et al., 2014). Vegetation landscapes were highly heterogeneous and responses to differences on climate, geology and altitudinal gradients n and Munuera, 1997; Moreno et al., have been described (Carrio 2012). Pollen and charcoal sequences in the area show dry steppe formations next to coniferous woodland, and an important Mediterranean component including evergreen Quercus, Olea, Pistacia, lez-Sampe riz et al., 2010). and Myrtus during MIS3 (Gonza Thirteen stratigraphic units (S.U.) were described by Fumanal (1994) and grouped in five segments according to the archaeological remains and macroscopic features (Fig. 2a). The first segment, at the base of the sequence, is formed by an archaeologically sterile travertine platform (Unit XIII). The second segment (Units XII-IX) shows the highest concentration of combustion structures and archaeological remains. The third segment (Unit VIII to the lower half of Unit V) shows a decrease of anthropogenic impact and an increase of natural sedimentation with an accumulation of large blocks in Unit VI. Nevertheless, six teeth attributed to a Neanderthal adult were recovered from the base of Unit V (Garralda et al., 2014). The upper half of Unit V, which is archaeologically sterile, forms the fourth segment. The last segment encompasses Units IV-I, which contains Holocene sediments with reworked Upper Palaeolithic, n et al., 2014b). Mesolithic, and Neolithic materials (Galva Archaeological excavations at El Salt have been carried out systematically since 1986. Lately, an integrated multidisciplinary analyses of the archaeological and sedimentary records was carn et al., ried out to examine the archaeological palimpsest (Galva 1991, 2006a, 2006b, 2014a, 2014b; Fumanal, 1994; Dorta et al., mez de la Rua et al., 2010; Machado et al., 2011; 2010; Go Marrero et al., 2011; Sistiaga et al., 2011, 2014; Mallol et al., ndez et al., 2014). 2013; Garralda et al., 2014; Herna Stratigraphic unit X has been dated around 50 ka BP, and to date has provided the greater amount of archaeological remains. For excavation purposes the stratigraphic unit X has
Fig. 2. Stratigraphic units at el Salt and excavation surface in unit X a) stratigraphic scheme showing the main sedimentary features (extracted from Garralda et al., 2014); b) detail of the excavation surface in unit X.
Cabanes, D., Phytolith and FTIR studies applied to combustion structures: The case of the Please cite this article in press as: Rodríguez-Cintas, A., Middle Paleolithic site of El Salt (Alcoy, Alicante), Quaternary International (2015), http://dx.doi.org/10.1016/j.quaint.2015.09.043
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Fig. 3. Location of the combustion structures and control samples analysed in subunit Xb. Scale bar in the pictures is 1 m.
been divided macroscopically in subunits Xa and Xb. During the excavation of this S.U. a total of 60 combustion structures (CS) have been identified. The hearths from S.U. X were concentrated near the travertine wall and were associated with faunal and lithic remains (Fig. 2b). The macrofaunal assemblage was characterized by goat (Capra pyrenaica), deer (Cervus elaphus) and horse (Equus ferus and Equus hydruntinus). Also, small mammals such as lagomorphs (Oryctolagus cuniculus) were present. Occasionally Bos primigenius, turtles (Testudo hermani) and carnivore remains were recovered from this unit. Lithic production was principally based on the exploitation of diverse siliceous raw materials gathered within a 25 km distanceeradius (Galv an et al., 2014a). Knapping systems were mainly ascribed
to the recurrent centripetal and the directional Levallois schemes, although the representation of non-Levallois directional methods was also significant. The introduction of single blanks, retouched or not, as well as the on-site recycling of artefacts were usual technical features of S.U. X assemblages. The predominance of scrapers among the retouched tools was also remarkable. 3. Materials and methods A total of 25 loose sediment samples were collected from the fresh exposed surface of the combustion structures in the subunit Xb during the 2013 field season (Table 1). Control
Cabanes, D., Phytolith and FTIR studies applied to combustion structures: The case of the Please cite this article in press as: Rodríguez-Cintas, A., Middle Paleolithic site of El Salt (Alcoy, Alicante), Quaternary International (2015), http://dx.doi.org/10.1016/j.quaint.2015.09.043
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samples, with no visual indication for thermal alteration, were collected from the same stratigraphic unit (Table 1 and Fig. 3). Morphologically, these combustion structures are ovalshaped and show a recurrent stratigraphy formed by two discrete layers: a) ash layer: white-coloured fine grained sediment at the top of the structure, and b) black layer: blackcoloured organic rich sediment at the base of the structure (Fig. 4). No reddening of the sediment was identified below the black layer in these structures. When possible, at least one sample of each layer was collected for analyses. However, some hearths show signs of weathering and erosion by geological and biological agents that altered the black layer and, in some cases, removed the ash layer. Only in the hearths H44b, H48, H51, H52 and H53 were the ash layers visually identified in the field. Faunal and lithic remains are abundant in both layers, and travertine blocks and limestone cobbles were recovered in a lesser extent (Table 2).
Fig. 4. Detail view of hearth H52 showing the two-layered stratigraphy formed by a top ash layer and a subjacent black layer. Table 1 Main results of the samples analysed in S.U. Xb. Combustion structure
Sample
Hearth field layer identification
FTIR
Calcite origin
Phyt. in 1 g of sediment (millions)
% Anatomically connected phytoliths
Average cell number in anatomical connected phytoliths
% Weathered morphotypes
%Melted morphotypes
H44b
H48
31 32 57 7 8 21
Ash layer Black layer Black layer Black layer Black layer Ash layer
Cl (b) ¼ Ca, Dah, Qz Cl (nb), Ca, Dah, Qz Ca]Cl (b?), Qz, Dah Cl (nb), Ca, Dah, Qz Cl (nb), Ca, Qz, Dah Ca, Cl (b), Dah, Qz
3.7 2.3 3.3 1.9 3.9 2.3
15.2 11.1 5.9 6.7 2.2 0
5.6 3.1 2.4 3.2 2.5 0
5.07 9.52 4.50 11.34 4.89 8.86
0 0 0 0 0 0
H49
22 28
Black layer Black layer
Ca, Cl (b?), Dah, Qz Ca]Cl (nb), Dah, Qz
1.7 3.2
0.7 10.3
2.0 5.2
11.57 2.67
0 0
H51b H52
9 10 15 19 23
Ash layer Ash layer Black layer Black layer Ash layer
Cl (b), Ca, Dah, Qz Cl (nb), Ca, Dah, Qz Cl (nb), Ca, Dah, Qz Cl (nb), Ca, Dah, Qz Ca, Cl (b), Qz
3.6 4.9 3.6 2.5 1.2
41.3 5.5 21.1 6.6 36.7
9.3 2.8 5.7 4.0 4.5
7.86 11.37 8.36 13.93 9.04
0.24 0 0 0 0.30
H53a H53a-b
24 33 35
Cl (nb), Ca, Dah, Qz Ca]Cl (b?), Qz. Dah Ca]Cl (nb), Qz, Dah
2.4 2.6 4.1
35.0 15.6 5.2
9.2 4.8 3.3
4.61 8.64 10.48
0 0 0
36 37
Black layer Ash layer Sediment between hearths Black layer Ash layer
Geogenic Geogenic Geogenic Geogenic Geogenic Anthropogenic (ash) Geogenic Anthropogenic (ash) Geogenic Geogenic Geogenic Geogenic Anthropogenic (ash) Geogenic Geogenic Geogenic
Ca]Cl (b?), Qz, Dah Ca, Cl (b), Qz
3.9 1.1
19.2 7.0
6.9 4.0
9.44 20.26
0 0.44
38 39 29 30 75 (104) 81 (420) 87 (108)
Ash layer Black layer Black layer Ash layer Control Control Control
Cl (b) ¼ Ca, Qz, Dah Cl (nb), Ca, Qz, Dah Cl (nb), Ca, Dah, Qz Cl (b), Ca, Dah, Qz Cl (nb), Ca, Dah, Qz Ca, Cl (nb), Dah, Qz Cl (nb), Ca, Dah, Qz
3.1 4.9 3.0 5.3 3.2 0.5 3.5
4.4 6.1 32.4 41.3 6 0 0
2.8 3.0 5.7 6.7 3 0 0
10.32 9.80 3.72 4.17 8.7 16.7 6.4
0 0 0 0 0 0 0
H45 H46
H51a
H53b
H54 Control samples
Geogenic Anthropogenic (ash) Geogenic Geogenic Geogenic Geogenic Geogenic Geogenic Geogenic
Ca ¼ calcite; Cl ¼ clay; Dah ¼ dahllite; Qz ¼ quartz; (b) ¼ thermally altered clay; (nb) ¼ not thermally altered clay. Minerals are arranged according to their relative peak heights in the FTIR spectrum. Table 2 Presence or absence of faunal and lithic remains, and travertine and limestone fragments in the hearths of subunit Xb. The asterisk indicates the hearths with the uppermost ash layer identified in the field. Faunal remains
H44b* H45 H46 H48* H49 H51* H52* H53* H54*
Flint artifacts
Burnt
Unburnt
Burnt
X e e X e X X X e
e X X
X e e
e e e X e
e X e e e
Travertine Unburnt X X X e e e e e
Limestone
Burnt
Unburnt
Burnt
X X X
e e e
X e X
e X e X e
e e e e e
e e e e e
Cabanes, D., Phytolith and FTIR studies applied to combustion structures: The case of the Please cite this article in press as: Rodríguez-Cintas, A., Middle Paleolithic site of El Salt (Alcoy, Alicante), Quaternary International (2015), http://dx.doi.org/10.1016/j.quaint.2015.09.043
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Mineralogical analysis was carried out using an iS5 FT-IR Nicolet Thermo Scientific Spectrometer. Infrared spectra were obtained using Kbr pellet at 4 cm1 resolution. The origin of calcite, i.e. geogenic or anthropogenic (i.e. ashes), was determined following Regev and Poduska (Regev et al., 2010; Poduska et al., 2011), and clays exposed to high temperatures were identified using specific absorptions in the clay spectrum (Berna et al., 2007). Phytolith extraction followed the method developed by Katz et al. (2010). Between 30 and 40 mg of dry sediment were weighed, transferred to plastic tubes, and 50 ml of 6 N HCl were added to dissolve the carbonates. Then 450 ml of sodium polytungstate at 2.4 g/ml density were added and phytoliths and lighter elements were separated from the rest of the fraction by centrifugation at 5000 rpm for 5 min. The supernatant was then transferred to another tube and 50 ml were placed in a microscope slide to proceed with phytolith identification and quantification. Phytoliths were counted and identified using an Olympus BX-41 optical microscope at 200 and 400. At least 200 individual phytoliths were identified in each slide. Morphological ascription was carried out using the standard literature (Twiss et al., 1969; Brown, 1984; Mulholland and Rapp, 1992; Rosen, 1992; Piperno, 2006). When possible the International Code for Phytolith Nomenclature was followed (Madella et al., 2005). 4. Results 4.1. FTIR results The main minerals forming the sediments analysed are clay and calcite, whereas quartz and dahllite are present in lower concentrations. Anthropogenic calcite (i.e. ashes) is only present in three out of nine ash layers identified in the field (H48, H52 and H53b) and in one of the black layers (H49). The other ash layers samples show calcite of geogenic origin. Clay is thermally altered in all the ash layers sampled and in the black layer from the combustion structures H45, H48 and H53b (Table 1). Control samples are mainly composed by unaltered clay and geogenic calcite (Table 1). 4.2. Phytolith concentration and preservation Phytolith concentrations and morphotypes are homogenous in all the combustion structures despite their mineralogical composition, coloration and stratigraphic position. Phytolith concentrations in the combustion structures range from 1.1 to 5.3 million per gram of sediment, and most of the samples show values between 2 and 4 million of phytolith per gram of sediment (Table 1). Note that the ash layer samples from the combustion structures H52 and H53b contain relatively low concentrations of phytoliths, around 1 million phytoliths per gram of sediment (Table 1). The percentage of weathered phytoliths is relatively low in all the samples (12%), with the notable exception of the ash layer from the combustion structure of H53 where weathered morphotypes reach values above 20%. Melted phytoliths, produced by high temperatures, are identified in the ash layers from H52 and H53b. Control samples show similar values of phytolith concentrations. Samples 75 and 87, collected close to the hearths, show a concentration around 3 million phytoliths per gram of sediment and a low percentage of weathered morphotypes (6.4%). On the other hand, control sample 81, located farther from hearths shows a lower concentration of phytoliths (0.5 millions) and the highest percentage of weathered phytoliths among the control samples (Table 1).
5
4.3. Phytolith morphotypes Fig. 5 shows the results for the phytolith morphotypes identification in the ash layers, black layers, and control samples. In the ash and black layers most of the phytolith identified have been formed in monocotyledonous plants, which include grasses, sedges, and generic monocotyledonous morphotypes that can be found in both grasses and sedges (Twiss et al., 1969; Rosen, 1992; Bamford et al., 2006). Leaf and stem phytoliths from grasses are overrepresented in most of the samples, with the exceptions of the black layer sample of H54 and one of the ash layer sample of H51. Phytoliths in anatomical connection from monocotyledonous plants are usually formed by long cells in combination with short cells or papillae (Fig. 6aeb and Fig. 7). Most of the grass short cells belong to C3 pooid (festucoid) type (rondel and rondel tower), whereas C4 chloridoid (saddle) and C4 panicoid (lobate forms) are present in lower concentrations (Fig. 8). Because most of the phytoliths recovered belong to grasses it can be assumed that generic monocotyledonous morphotypes derived also from these plants. Control samples produce similar results showing phytolith assemblages mainly composed by grasses with a high presence of C3 grass short cells (Fig. 5c). Phytolith morphotypes from wood and bark show values that range between 2 and 14%, whereas phytoliths from dicotyledonous leaves show in general lower percentages (0.5e8%). Multicellular polyhedral and jigsaw puzzle structures have been recovered despite their low preservation in archaeological sediments and natural soils (Piperno, 2006) (Figs. 6c and 7). Irregular verrucate phytoliths from dicotyledonous seeds and fruits are present in all the samples in different amounts (Figs. 5 and 6d). These are especially abundant in the form of multicellular structures in the black layer samples (Fig. 7b). Some of these morphotypes are originated in Celtis sp. seed coats (Fig. 6d) and have been previously identified in S.U. Xa (Mallol et al., 2013). Phytolith assemblages in control samples are mostly formed by grass and generic monocotyledonous morphotypes. Wood and bark and dicotyledonous leaf morphotypes show low percentages, and seed/fruit phytoliths are present in all the control samples in considerable amounts (Fig. 5c). Fig. 9 shows the distribution of the main phytolith morphotypes categories according to the calcite FTIR's identification for the hearth samples and control samples. No significant differences can be observed on the distribution of the main phytolith categories, with the exception of dicotyledonous fruit/seed phytoliths, which are underrepresented in the anthropogenic calcite (i.e. ash) samples. 5. Discussion The presence of anthropogenic calcite in the ash layers of H48, H52 and H53b, in concurrence with the presence of thermally altered clay and small amounts of melted phytoliths in H52 and H53b points to an in situ preservation of the ash remains in these combustion structures. However, the remaining combustion structures do not show mineralogical evidence for ashes in the layers identified in the field as ash layer, although the clay mineral was thermally altered. This is probably due to the dissolution of ashes or their mixing with the geogenic matrix by syndepositional or postdepositional processes. Dahllite is present in low amounts in all the samples, indicating that calcite diagenesis is still in the initial stages (Karkanas et al., 2000). The presence of dahllite can be related to the deposition of bird guano containing high amounts of phosphates (Shahack-Gross et al., 2004).
Cabanes, D., Phytolith and FTIR studies applied to combustion structures: The case of the Please cite this article in press as: Rodríguez-Cintas, A., Middle Paleolithic site of El Salt (Alcoy, Alicante), Quaternary International (2015), http://dx.doi.org/10.1016/j.quaint.2015.09.043
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Fig. 5. Phytolith morphotype identification and anatomical origin in a) ash layer, b) black layer, and c) control samples.
Phytolith assemblages in unit Xb seem to be fairly well preserved; the percentage of weathered phytolith is relatively low in most of the samples, phytolith with delicate decorations have been identified, and phytoliths with an assumed large surface area to volume ratio, such as polyhedrals or jigsaw puzzles, have been recovered (Cabanes et al., 2011; Cabanes and ShahackGross, 2015). The presence of wood and bark phytoliths indicates the use of the use of wood as fuel in the hearths studied. Moreover, no significant amount of highly fragmented burnt bones was identified during the excavation, ruling out bone as a main source of fuel (Yravedra and Uzquiano, 2013) and as the origin of dahllite. Nevertheless, the presence of wood and bark phytoliths is low in all the samples when compared to the monocotyledonous percentages. Grasses are higher
accumulators of silica than woody dicotyledonous, producing higher amounts of phytoliths per gram of original plant material (Albert and Weiner, 2001). In addition, grass phytoliths can be present in the form of contamination (up to 30% of the assemblage) in woody dicotyledonous plants (Albert and Weiner, 2001; Tsarsidou et al., 2007). However, here the presence of monocotyledonous morphotypes, including grass and generic monocotyledonous, ranges from 41 to 75% of the phytoliths identified. Therefore, grasses might have been deposited in the sediment by ways other than wood and bark contamination. In previous works, the presence of high percentage of monocotyledonous morphotypes have been linked to the existence of a grass bedding in Mousterian occupations at el Esquilleu site (Cabanes et al., 2010; Mallol et al., 2010) and MSA layers at
Cabanes, D., Phytolith and FTIR studies applied to combustion structures: The case of the Please cite this article in press as: Rodríguez-Cintas, A., Middle Paleolithic site of El Salt (Alcoy, Alicante), Quaternary International (2015), http://dx.doi.org/10.1016/j.quaint.2015.09.043
Fig. 6. Light microscope images of phytolith morphotypes recovered in the hearth samples. a) Elongate cell altered from hearth H46 (sample 8); b) Melted phytolith from hearth H52 (sample 23); c) Rugulate long cells in anatomical connection from monocotyledonous leaf in hearth H54 (sample 30); d) Wavy long cells and rondel short cells in anatomical connection from grasses in hearth H54 (sample 30); e) Jig-saw puzzle multicellular structure formed in dicotyledonous leaf in hearth H51a (sample 9); f) Spheroid psilate from wood/bark in hearth H48 (sample 22); g) Multicellular structure formed by irregular verrucate morphotypes, probably from Celtis sp. seed coats, in hearth H44b (sample 32); h) Irregular verrucate morphotype in hearth H54 (sample 30).
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Fig. 7. Percentage of monocotyledonous, dicotyledonous leaf, and dicotyledonous seed/fruit morphotypes in anatomical connection: a) ash layer, b) black layer, and c) control samples.
Sibudu rockshelter (Wadley et al., 2011). In both cases the presence of a high number of phytoliths in anatomical connection, identified both in thin section and phytolith analysis, pointed to the existence of monocotyledonous leaf beddings. The percentage of anatomically connected phytoliths from grasses in S.U. Xb is low in most of the samples analysed, and only increase when multicellular structures formed in dicotyledonous fruit/seeds coats are also present in high amounts (Fig. 7). The most noticeable exception is the ash layer sample from H52 where monocotyledonous phytoliths in anatomical connection represent more than 30% of the phytolith assemblage. In the rest of the samples when anatomically connected phytoliths are present in high amounts these are formed almost exclusively by dicotyledonous seed/fruit morphotypes. Micromorphological analyses carried out in subunit Xb (Mallol et al., 2013) have not revealed the presence of any bedding structure so far. Postdepositional processes implying the sediment reworking or phytolith dissolution might lead to the disarticulation of anatomically connected phytoliths (Cabanes et al., 2009, 2010, 2012; Jenkins, 2009). However, in S.U Xb the different degree of anatomical connection between fruits/seeds
and grasses rules out postdepositional processes as responsible for the disarticulation of anatomically connected phytoliths. Biostratinomic processes in this case might have regulated the degree of phytolith anatomical connection. The fruit/seed phytoliths recovered from in S.U. Xb are very similar to those of hackberry (Piperno, 2006), and Celtis sp. seed coats seeds have been previously identified in the site (Mallol et al., 2013). Mediterranean hackberry seeds have been identified in other European Palaeolithic sites (Laville and nault-Miskovsky, 1977; Allue et al., 2015). However, the curRe rent distribution of Mediterranean hackberry trees in solitary individuals or small groups is related to dispersal of fruits by frugivores, primary birds and occasionally by other vertebrates (Traba et al., 2006). The data presented here shows a higher accumulation of fruit/seed phytoliths in the sediments with lower anthropogenic component (Fig. 9). In addition, multicellular structures from dicotyledonous seed/fruit are more abundant in the black layer, which results from the accidental combustion of previously deposited materials in the site (Mallol et al., 2013). Thus, phytolith assemblage composition in S.U. Xb points out to an accumulator agent other than humans for most of these microbotanical remains. The most parsimonious explanation for the presence of Mediterranean hackberry phytoliths in the site is their introduction in the form of bird guano, which is in accordance with the presence of phosphatic minerals showed by FTIR analysis. Phytolith concentration and composition of the control samples also points out to a natural origin of the phytolith recovered, however the presence of small amounts of ashes dispersed by trampling could explain the low percentages of wood and bark phytoliths detected in the control samples (Cabanes et al., 2007). Additionally, preceding analyses in the subjacent S.U. Xa show as well a natural origin for most of the phytoliths assemblages recovered in the combustion structures investigated (Mallol et al., 2013). The fuel used (i.e. wood) and the archaeological remains related to the combustion structures indicate that the hearths analysed here are rather simple and without any specialized function. The low anthropogenic impact in the sediments and the presence of phytoliths deposited by natural agents indicate a low sedimentation rate for S.U. Xb and an ephemeral nature of the combustion structures. In this sense, the presence of 60 discrete combustion structures in this stratigraphic unit is probably the result of a palimpsest overlapping different occupations events, rather than the consequences of an exceptional occupation intensity. However, the area studied here is relatively small and further excavation and sampling will be necessary to confirm that the remaining combustion structures in S.U. Xb follow the same pattern. Despite the simplicity of the combustion structures studied so far, the data obtained from el Salt shows that Neanderthal populations have full capacity to start and control a fire each time they visited the site, regardless of the duration or the intensity of the occupation. 6. Conclusions Phytolith and FTIR analysis of the combustion structures points out to natural deposition of the sediments in S.U. Xb. Albeit sediment preservation conditions are fairly good the anthropogenic sedimentary signal is limited to few evidences of ash, thermally altered clay and low amounts of wood and bark phytoliths derived from the fuelwood used in the combustion structures. The hearths analysed can be considered the result of ephemeral activity, which did not last long enough to leave a clearer anthropogenic signal in the sediments. Further research is
Cabanes, D., Phytolith and FTIR studies applied to combustion structures: The case of the Please cite this article in press as: Rodríguez-Cintas, A., Middle Paleolithic site of El Salt (Alcoy, Alicante), Quaternary International (2015), http://dx.doi.org/10.1016/j.quaint.2015.09.043
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Fig. 8. Light microscope images of grass short cells identified in the hearth samples. a) Pooid (festucoid) short cells in hearth H48 sample 21, note the partial dissolution observed on the top of both short cells: 1. Rondel short cell. 2. Rondel tower short cell; b) Rondel tower short cell from hearth H51b sample 19; c) rondel short cell from hearth H51b sample 19; d) polylobate short cell from hearth H45 sample 57.
neo de los grupos neandertales en la region central del Mediterra rico. Una propuesta metodolo gica de aproximacio n al proceso Ibe rico y al marco paleoambiental’ (HAR2012-32703, MICINNhisto FEDER) and the Cultural Heritage Department of the Valencia Government, under the direction of Professor Bertila Galv an of Universidad de La Laguna. D. Cabanes has been supported by a Juan de la Cierva post-doctoral contract (JCI-2011-10972). This research is part of the activities of the ERAAUB (2014 SGR 845), thanks to the del DIEU, support of Comissionat d'Universitats, Recerca i Innovacio Generalitat de Catalunya.
90 80 70 60
%
50 40 30 20
References
10 0 Monocotyledonous
Wood/Bark
Dicotyledonous leaf
Antropogenic calcite (ash)
Dicotyledonous fruit/seed
Geogenic calcite
Weathered
Control samples
Fig. 9. Main phytolith morphotypes categories averaged according to the origin of calcite in FTIR analysis. Error bars indicate 1s standard deviation.
necessary to determine if the main activity area was located elsewhere, and therefore missed in the current study, or by the contrary, if the low anthropogenic signal was the result of short sporadic visits to the site by small groups of Neanderthals. The data obtained indicate that Neanderthal populations at El Salt were capable of starting and controlling fire using nonspecialized combustion structures. Acknowledgements We thank to the members of the research team “Sociedades cazadoras-recolectoras paleolíticas” based at Universidad de La Laguna for their support and help with field tasks. Archaeological n research at El Salt is funded by Spanish IþD Project ‘La Desaparicio
Albert, R.M., Cabanes, D., 2008. Fire in prehistory: an experimental approach to combustion processes and phytolith remains. Israel Journal of Earth Sciences 56, 175e189. Albert, R.M., Weiner, S., 2001. Study of phytoliths in prehistoric ash layers using a quantitative approach. In: Meunier, J.D., Colin, F. (Eds.), Phytoliths: Applications in Earth Sciences and Human History. A.A Balkema Publishers, Lisse, pp. 251e266. Albert, R.M., Lavi, O., Estroff, L., Weiner, S., 1999. Mode of occupation of Tabun Cave, Mt Carmel, Israel during the Mousterian period: a study of the sediments and phytoliths. Journal of Archaeological Science 26, 1249e1260. Albert, R.M., Weiner, S., Bar-Yosef, O., Meignen, L., 2000. Phytoliths in the Middle Palaeolithic deposits of Kebara Cave, Mt Carmel, Israel: study of the plant materials used for fuel and other purposes. Journal of Archaeological Science 27, 931e947. Albert, R.M., Bar-Yosef, O., Meignen, L., Weiner, S., 2003. Quantitative phytolith study of hearths from the Natufian and Middle Palaeolithic levels of Hayonim Cave (Galilee, Israel). Journal of Archaeological Science 30, 461e480. Aldeias, V., Goldberg, P., Sandgathe, D., Berna, F., Dibble, H.L., McPherron, S.P., Turq, A., Rezek, Z., 2012. Evidence for Neandertal use of fire at Roc de Marsal (France). Journal of Archaeological Science 39 (7), 2414e2423. , E., Cabanes, D., Sole , A., Sala, R., 2012. Hearth functioning and forest resource Allue exploitation based on the archeobotanical assemblage from Level J. In: Carbonell, E. (Ed.), High Resolution Archaeology and Neanderthal Behavior. Springer, Dordrecht, Heliderberg, New York, London, pp. 373e385. , E., C sito, I., Canals, A., Rodríguez, A., Rosell, J., Bermúdez de Allue aceres, I., Expo Castro, J.M., Carbonell, E., 2015. Celtis remains from the Lower Pleistocene of Gran Dolina, Atapuerca (Burgos, Spain). Journal of Archaeological Science 53, 570e577.
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Cabanes, D., Phytolith and FTIR studies applied to combustion structures: The case of the Please cite this article in press as: Rodríguez-Cintas, A., Middle Paleolithic site of El Salt (Alcoy, Alicante), Quaternary International (2015), http://dx.doi.org/10.1016/j.quaint.2015.09.043