Shine on you crazy diamond : Symbolism and social use of fluorite ornaments in Iberia’s late prehistory

Journal of Lithic Studies (2021) vol. 8, nr. 1, p. 1-17 DOI: https://doi.org/10.2218/jls.3025 Published by the School of History, Classics and Archaeology, University of Edinburgh ISSN: 2055-0472. URL: http://journals.ed.ac.uk/lithicstudies/ Except where otherwise noted, this work is licensed under a CC BY 4.0 licence. Shine on you crazy diamond: Symbolism and social use of fluorite ornaments in Iberia’s late prehistory José Ángel Garrido-Cordero 1, Carlos P. Odriozola 1, Ana C. Sousa 2, Victor S. Gonçalves 2, João Luís Cardoso 3, 4 1. Departamento de Prehistoria y Arqueología. Universidad de Sevilla, Calle Doña María de Padilla, s/n, 41004, Sevilla, Spain. Email: Garrido-Cordero: [email protected]; Odriozola: [email protected] 2. UNIARQ. Centro de Arqueologia da Universidade de Lisboa, Alameda da Universidade 1600-214, Lisboa, Portugal. Email: Sousa: [email protected]; Gonçalves: [email protected] 3. Universidade Aberta, Rua da Escola Politécnica, 1269-001, Lisboa, Portugal. Email: Cardoso: [email protected] 4. Centro de Estudos Arqueológicos do Concelho de Oeiras (Câmara Municipal de Oeiras), Portugal. Abstract: Fluorite ornaments have been recorded in different sites of Europe since Upper Paleolithic. Due to its visual appearance and physical properties, some translucent or transparent mineralogies like fluorite were searched for or casually acquired by late prehistory’s human communities. After intensive research on archaeological contexts from the Iberian Peninsula with personal ornaments from 4th to 2nd millennia BCE, we have recently identified and characterized for the first time an important number of fluorite ornaments, confronting a previous background where little attention was paid. Our work has been carried out in different archaeological collections and museums from the whole Iberian Peninsula by nondestructive techniques (Raman spectroscopy, portable X-ray fluorescence (p-XRF) and X-ray Diffraction (XRD), that revealed the nature of fluorite ornaments and points to its consideration as scarce and highly symbolic items during late prehistory. A total of 36 fluorite beads from 23 sites are here recorded and studied, many of them inedits or wrong catalogued as other mineralogies. These adornments could have important roles in trade and use among the communities of Iberia from the 4th millennium BCE onwards, because of their scarcity and its recurrent association with important funerary complex and exotic materials. Fluorite ornaments could have been significant and special symbols in the development of new and exclusive raw materials in the context of increasing social complexity and inequality. Keywords: Adornments; beads; translucent; fluorite; Iberian Peninsula; late prehistory; Raman spectroscopy; XRD 1. Introduction Personal adornments (beads, pendants, charms…) are determinants to understand symbolic behaviour and identitarian constructions in prehistoric societies (Bar-Yosef Mayer & Porat 2008; Wright & Garrard 2003), giving key information about the metaphoric codes used (Tilley 2 J.A. Garrido-Cordero et al. Journal of Lithic Studies (2021) vol. 8, nr. 1, p. 1-17 DOI: https://doi.org/10.2218/jls.3025 1999) by colour, shape, brightness, and others (Gaydarska & Chapman 2008; Jones & MacGregor 2002). In the Iberian Peninsula, apart from the long-known social value of amber (for a review see Odriozola et al. 2019), transparent or translucent beads are rare, and when recorded they were generally classified as quartz or rock crystal with no further analysis than that of the naked eye. However, besides quartz varieties, there are many more transparent minerals that are not usually considered, for example fluorite, calcite, and many sheet silicates that when thinned to a certain level are capable of transmitting light (Baysal 2017: 6-7). The social value of translucent ornaments made of those minerals would partially stem from its visual and physical properties and its scarcity in the archaeological record (Garrido-Cordero et al. 2020). Fluorite (CaF2) has recently received some attention by researchers in different European late prehistory’s contexts (Cardoso et al. 2012; Garrido-Cordero et al. 2020; Goemaere & Philippo 2010; Goemaere et al. 2013; Honings et al. 2014; Jungels & Goemaere 2007). Fluorite mineral is relatively frequent geologically in the Iberian Peninsula and Western Europe (Anthony et al. 2011; Galán & Mirete 1979), but infrequent in archaeological record. This paper is focused in the role of fluorite adornments as highly scarce and symbolic items, used among the communities of Iberia’s late prehistory, a subject on which little research has been previously carried out. The starting point for this study is a remarkable set of unpublished translucent beads that we have characterized and gathered for the first time. The chemical and contextual analysis of these beads inventoried throws new light on the use and social significance of translucent personal adornments during the increase of social complexity from Late Neolithic to Early Bronze Age. 1.1. Fluorite ornaments in late prehistory. The broader European context In Europe, the small-scale exploitation and consumption of fluorite has been documented in Belgium at Upper Paleolithic sites, mostly during the Magdalenian period (Goemaere et al. 2013; Jungels & Goemaere 2007). In some cases, a large quantity was used, and the mineral was worked in situ (440 g of fluorite at the site of Chaleux) and distributed locally and regionally for the manufacture of adornments (Goemaere et al. 2013). No prehistoric fluorite mines have been identified in Europe. In fact, ethnographic data suggest that outcrops of this type of raw material could have been exploited just occasionally and opportunistically by small groups without any complex logistical organization (Brandl & Trnka 2014: 124). The frequency of its consumption for objects of personal adornment seems to increase during the Neolithic, but is still small compared with other raw materials. In the late 5th and early 4th millennia BCE, some Belgian sites have yielded both manufactured fluorite fragments and others in the process of being made into beads and pendants (Delye et al. 2011; Vermeersch et al. 1990). At Thieusies, several worked fluorite fragments in different colours and four finished beads came to a total weight of 158.4 g (Vermeersch et al. 1990: 51-52). From the Late Neolithic to the Copper Age (5th-3rd millennia BCE) the number of sites where this raw material was used to make adornments increases considerably. Fluorite beads have been found at Neolithic sites in the north of France (Hauzeur & Cauwe 2012: 39), in the Paris Basin (Polloni 2008) and in the south-west, especially between Perpignan and Narbonne (Roscian et al. 1992: 233-234). Their distribution coincides with the main outcrops of fluorite in the Central Massif and the Pyrenees, and supports the idea of local exploitations near the outcrops and distribution on a regional scale. In Predinastic Egypt (4th millennium BCE), fluorite ornaments are also reported (Nai 2014: 77). Fluorite continued to be used occasionally for personal adornments in the 2nd millennium BCE. Fluorite beads are referred at Bronze Age levels in Mol, Belgium (Warmenbol 2001) or Midea, Greece (Demakopoulou et al. 1996). J.A. Garrido-Cordero et al. 3 Journal of Lithic Studies (2021) vol. 8, nr. 1, p. 1-17 DOI: https://doi.org/10.2218/jls.3025 Unlike other parts of Europe, no personal adornment made from fluorite is known in the Iberian Peninsula before the 4th millennium BCE, although many sites with fluorite have not been dated by radiocarbon or the finds are not directly associated with a dated level. Before this paper, only Cardoso et al. (2012) confronted regional identification of five fluorite beads in Portugal. Also, fluorite beads were reported in the Iberian peninsula in the megaliths of Gabrieles 6 (Blanco & Rothenberg 1981: 284), La Velilla (Villalobos 2015: 304), mámoa 5 do Leandro (Ribeiro & Loureiro 2015) and dolmen of Areita (Gomes et al. 1998), while one bead of fluorite was identified for the Bronze Age tomb 111 of Fuente Álamo (Pozo et al. 2002). 2. Materials and methods A total of 23 sites in the Iberian Peninsula with a total number of 36 items made of fluorite are reported in this work (Figure 1, Table 1). Archaeological background on the sites studied here can be found at Supplementary Material 1. From this total, 28 fluorite beads from 20 sites were directly analyzed for this paper (Figure 2) by Raman spectroscopy and portable XRF. Also, X-ray diffraction (XRD) has been possible to perform when the museums granted the transport of materials to the laboratory. Table 1. Inventory of fluorite items in Iberian late prehistory. Period legend: LN, Late Neolithic; C, Copper Age; B, Bronze Age. Mineralogy legend: F: fluorite; C: calcite; Q: quartz; Ame: amethyst. Site ID Type Period Expected mineralogy Actual mineralogy Colour Weight (g) Techniques / results p-XRF Raman XRD Casa da Moura CMR-436 Natural cave LN/ C F F Transparent smoky 22.6 Ca F (T 2g + PL) - Poço Velho CCG-159 Natural cave LN/ C F - Green - Si - - Leceia LC93-TA-C3 Site - fortified C F F Yellow/Green - Ca F (PL) F Vila Nova de São Pedro ARQ-VNSP964-46 Site - fortified C - F Transparent smoky 0.7 Ca - - Lapa do Bugio LB-0011-3 Natural Cave LN/ C F F Green 10.6 Ca F (PL) - Lapa do Bugio LB-0011-4 Natural Cave LN/ C F F Green 7.2 Ca F (PL) - São Paulo 2 MMA-5743 Artificial Cave LN/ C - F Pale green 26.3 Ca F (PL) - Olival da Pega 1 21815A Megalith LN/ C - F Green 6.5 Ca F (PL) - Olival da Pega 1 21815B Megalith LN/ C - F Green 2.0 Ca F (PL) - Anta Grande da Comenda da Igreja 2011.54.278 Megalith LN/ C - F White 19.8 Ca F (T2g + PL) - Anta Grande da Comenda da Igreja 985.51.617 Megalith LN/ C - F White 16.0 Ca F (T2g + PL) - Anta Grande da Comenda da Igreja 985.51.670 Megalith LN/ C - F Pale green 3.7 Ca F (PL) - 4 J.A. Garrido-Cordero et al. Journal of Lithic Studies (2021) vol. 8, nr. 1, p. 1-17 DOI: https://doi.org/10.2218/jls.3025 Site ID Type Period Expected mineralogy Actual mineralogy Colour Weight (g) Techniques / results p-XRF Raman XRD Tituaria 998.16.42 Tholos C C F Yellow/Green 3.6 Ca F (PL) - Anta dos Penedos de São Miguel PSM-112 Megalith LN/ C - F Green 2.6 Ca F (PL) - Gruta da Marmota MRO/S-25 Natural cave LN - F Green 8.0 Ca F (PL) - Gruta da Marmota MMT-26 Natural cave LN - F Green 5.1 Ca - F Cabeço da Ministra 25992-1 Natural cave LN/ C - F Green 5.6 Ca - - Cabeço da Ministra 25992-2 Natural cave LN/ C - F Green 5.0 Ca - - Mámoa 5 do Leandro - Megalith LN/ C F - - - - - - Dolmen de Areita ART-96-60 Megalith LN/ C F - Pale blue - - - - El Pozuelo 1 IG-313/51 Megalith LN/ C Q F Transparent/ Yellow 1.7 Ca F (PL) - El Pozuelo 5 N/A Megalith LN/ C Q F Green 2.0 Ca F (PL) F El Pozuelo 7 1848 Megalith LN/ C Q F Yellow/Green 3.2 Ca F (T 2g + PL) - Los Gabrieles 6 IG-3486/22 Megalith LN/ C F F Green 21.2 Ca F (PL) - Cueva del Vaquero - Tholos C Q F Green 90.1 Ca - - “La Emisora” - Artificial cave? C - F Green 1.2 Ca - - Los Millares 12 - Tholos C Ame. F Violet - Ca F (T2g) - Los Millares 12 - Tholos C Ame. F Violet - Ca F (T2g) - Los Millares 12 - Tholos C Ame. F Violet - Ca F(T 2g ) - Los Millares 12 - Tholos C Ame. F Violet - Ca F (T 2g ) - Los Millares 12 - Tholos C Ame. F Violet - - - - La Velilla - Megalith LN/ C C F Green - Ca - - Cau de I'Olivar d'en Margall 16477-7 Natural cave C C F Translucent green 3.1 Ca F (PL) - Cau de I'Olivar d'en Margall 16477-17 Natural cave C C F Translucent white 1.6 Ca F (PL) - Anta Grande do Zambujeiro ME-3760 Megalith C - F Pink 26.5 Ca F (T2g) F Fuente Álamo, tomb 111 VI-1 Pithos B F F Translucent - Ca F (T 2g + PL) - Fuente Álamo tomb 111 DJ83773 Pithos B F F Transparent 0.5 Ca F (T 2g + PL) - J.A. Garrido-Cordero et al. 5 Journal of Lithic Studies (2021) vol. 8, nr. 1, p. 1-17 DOI: https://doi.org/10.2218/jls.3025 Figure 1. Iberian late prehistory sites and materials cited and studied in the text, compared with fluorite geological occurrence in the Iberian Peninsula. 1. Anta Grande da Comenda da Igreja. 2. Anta Grande do Zambujeiro. 3. Anta dos Penedos de São Miguel. 4. Cabeço da Ministra. 5. Casa da Moura. 6. Cau de l´Olivar d´en Margall. 7. Cueva del Vaquero. 8. Dolmen de Areita. 9. El Pozuelo 1. 10. El Pozuelo 5. 11. El Pozuelo 7. 12. Fuente Álamo. 13. Gruta da Marmota. 14. La Emisora (Valencina). 15. La Velilla. 16. Lapa do Bugio. 17. Leceia. 18. Los Gabrieles 6. 19. Mámoa 5 do Leandro. 20. Necrópolis de Los Millares. 21. Olival da Pega 1. 22. Poço Velho. 23. São Paulo 2. 24. Tituaria. 25. Vila Nova de São Pedro. Raman spectroscopy was performed using a portable BWTEK iRaman Plus device. The laser diode operated with a wavelength of 785 nm produces a power of up to 420 mW in the laser port. Filters were not used to reduce the power of the laser. The selected range of the measurement spectrum was between 150 and 3300 cm-1 with a high efficiency quantum CCD detector. The selected measurement accuracy was 4 cm-1. The measurement conditions, as regards the laser power and integration time have varied from one object to another in order to obtain the best possible Raman signal. Chemical composition was measured by an Oxford Instrument XMET-7500 p-XRF equipped with a Rh tube, a silicon drift detector (SDD), and an automatic 5-position filter changer. Quantification was obtained using the SOILS-LE program based on fundamental parameter (FP) method. This method is the most appropriate when no standardized method is available or when a large number of elements have to be analyzed (Beckhoff et al., 2006: 403). XRD analysis was performed using a Panalytical X’Pert Pro θ/θ diffractometer equipped with Cu Kα source (1.5406 Å) operating at 45 kV and 40 mA. A PixCel detector was used and the data were collected on transmission mode with a 2D detector. Patterns were obtained using 6 J.A. Garrido-Cordero et al. Journal of Lithic Studies (2021) vol. 8, nr. 1, p. 1-17 DOI: https://doi.org/10.2218/jls.3025 a step width of 0.053º 2θ between 5º and 70º 2θ and a counting time of 155 s per step at ambient temperatures. An incident beam PreFIX module with X-ray mirror for Cu radiation was used to allow non-destructive analysis. Figure 2. A sample of beads analyzed in this paper. 3. Results and discussion Of the 25 Raman analyzed beads only a set formed by Los Millares translucent pale violet beads, El Pozuelo 7 colourless bead and the translucent pale pink beads from Casa da Moura, Anta Grande da Comenda da Igreja, Anta Grande do Zambujeiro and Fuente Álamo tomb 111 (CMR-436, AGCI-2011.154.278, AGCI-985.51.617, ME-3760, FA-T111-DJ83773 and FAT111-VI-1) records the fluorite diagnostic T2g Raman band at c. 320 cm-1. Therefore, this set of 11 beads are most likely fluorite (Figure 3). However, the translucent pale pink beads (CMR-436, AGCI-2011.154.278, AGCI985.51.617, FA-T111-DJ83773 and FA-T111-VI-1) accounts for additional bands to the T2g Raman active band at lower and higher frequencies that remain to be explained (Figure 3, right). These additional bands to the fluorite diagnostic T2g Raman band may be caused by 1) the accommodation of Y, Sr, Ba ... and REEs in substitution of Ca (Chen & Stimets 2014; Cherniak et al. 2001; Lenz et al. 2015; Sverdrup 1968; Tu & Sievers 2002); 2) by radiation-induced J.A. Garrido-Cordero et al. 7 Journal of Lithic Studies (2021) vol. 8, nr. 1, p. 1-17 DOI: https://doi.org/10.2218/jls.3025 defects (Alencar et al. 2016), which could also cause colourless fluorites to become coloured (Alencar et al. 2016; Schmalzl et al. 2003); or 3) as argued recently by Vandenabeele and Edwards (2018: 327-328) could be caused by the interference pattern (ripple) generated by the edge filters in luminescent samples. Figure 3. Raman spectra in the diagnostic region, left) set of samples that shows solely the fluorite diagnostic T2g Raman band at c. 320 cm-1, right) set of samples that shows the fluorite diagnostic T2g Raman band at c. 320 cm1 and additional bands at lower and higher frequencies. Beside these features in the diagnostic region, a set of bands appear in the frequency-shift region between 1000 and 2500 cm-1 that are the result of the 785 nm laser induced fluorescence and photoluminescence (PL) (Figure 4). Fluorite PL pattern is most likely due to the presence of REE3+ ions, mainly Nd, at C4v sites (Freeth & Jones 1982; Payne et al. 1991). PL bands have been formerly proposed as mineral characteristic (Chen & Stimets 2014), therefore the match between fluorite reference PL spectra and the here recorded would support the identification of all the analyzed specimens as fluorite. However, no exhaustive database exists for mineral identification by means of the PL spectra and their usability is therefore limited and still under research. Recent studies (Zhuk 2017) have shown that in some cases calcite shows PL spectra very similar to that of fluorite leading to a misclassification of the specimen, and therefore preventing the immediate classification of these beads as fluorite. This is true because Ca substitutions by REE elements in calcite crystal lattice result in a similar laser induced photoluminescence to that of fluorite crystals (Gaft et al. 2001). Except for Los Millares specimens that lack the 1137 cm-1 band and show differences in position and intensity of the bands in this region, that might be associated with the accommodation of REE3+ in substitution for Ca (Chen & Stimets 2014; Cherniak et al. 2001; Lenz et al. 2015; Sverdrup 1968; Tu and Sievers 2002), the spectra of this set of beads (Figure 4) accounts for the typical fluorite PL spectrum (Andò & Garzanti 2014). 8 J.A. Garrido-Cordero et al. Journal of Lithic Studies (2021) vol. 8, nr. 1, p. 1-17 DOI: https://doi.org/10.2218/jls.3025 Figure 4. Raman spectra in the frequency-shift region between 1000 and 2500 cm-1 showing the typical fluorite PL spectra. Therefore, based on 1) the presence of the T2g Raman band, 2) the coincidence of the PL of the specimens with that of fluorite, and 3) the chemical composition of the beads; fluorite is proposed as the main mineral phase for these 11 beads. Even though 15 of the analyzed beads (LB-0011, LB-0012, OP-21815B, OP-21815A, AGCI-985.51.670, TIT-988.16.42, MRO/S-25, SP2-5743, PSM-112, LC93-FA-C3, El Pozuelo 1, El Pozuelo 5, Los Gabrieles 6 and Cau de l´Olivar d´en Margall 16477-7 and 16477-17) lack the T2g band, their chemical composition J.A. Garrido-Cordero et al. 9 Journal of Lithic Studies (2021) vol. 8, nr. 1, p. 1-17 DOI: https://doi.org/10.2218/jls.3025 and PL spectra (Figure 5) make it impossible for us to exclude fluorite as the main mineral phase of these 15 beads. Calcite is off the table for these 15 specimens because they all lack the calcite Raman spectral features at 284, 710 and 1085 cm-1 (Chen & Stimets 2014; Sood et al. 1981). In addition to p-XRF and Raman spectroscopy, XRD analysis has been performed on a selection of this set of 15 beads and on ME-3760. 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