isotopic discriminants between late bronze age ... - Wiley Online Library

Archaeometry 52, 3 (2010) 380–388

doi: 10.1111/j.1475-4754.2009.00487.x

ISOTOPIC DISCRIMINANTS BETWEEN LATE BRONZE AGE GLASSES FROM EGYPT AND THE NEAR EAST* P. DEGRYSE,1 A. BOYCE,2 N. ERB-SATULLO,3 K. EREMIN,4 S. KIRK,5 R. SCOTT,5 A. J. SHORTLAND,5 J. SCHNEIDER1 and M. WALTON6 1

Centre for Archaeological Sciences, Katholieke Universiteit Leuven, Celestijnenlaan 200E-bus 2408, B-3001 Leuven, Belgium 2 Isotope Geoscience Unit, Scottish Universities Environmental Research Centre (SUERC), Rankine Avenue, East Kilbride, Glasgow G75 0QF, UK 3 Research Laboratory for Archaeology and the History of Art, Dyson Perrins Building, South Parks Road, Oxford OX1 3QY, UK 4 Harvard Art Museum, 32 Quincy Street, Cambridge, MA 02138, USA 5 Centre for Archaeological and Forensic Analysis, Department of Applied Sciences, Security and Resilience, Cranfield University, Shrivenham, Swindon SN6 8LA, UK 6 The Getty Conservation Institute, 1200 Getty Center Drive, Suite 700, Los Angeles, CA 90049-1684, USA

This paper presents oxygen, strontium and neodymium isotopic analysis from a series of Late Bronze Age glasses from Egypt and Mesopotamia. It was found that oxygen and neodymium isotopes alone cannot readily distinguish between glasses from the various sites. However, combined Sr and Nd isotope analysis separate the data into three groups: an Egyptian group with relatively low Sr and Nd ratios; a Late Bronze Age (LBA) Nuzi group with high Sr and low Nd ratios; and an intermediate Sr and high Nd ratio grouping of glasses from Tell Brak. These findings suggest that most of the glass from Nuzi and Tell Brak had different raw materials and hence the glass was probably produced at different manufacturing sites. However, one glass ingot found at Tell Brak (TB1) appears to have Nuzi-type Sr–Nd characteristics. This is the first positive identification of multiple production sites in LBA Mesopotamia and an exceptional example of a glass that may have been exchanged from one LBA site to another. KEYWORDS: LATE BRONZE AGE, GLASS, EGYPT, MESOPOTAMIA, OXYGEN, STRONTIUM AND NEODYMIUM ISOTOPIC ANALYSIS

INTRODUCTION

The study of Late Bronze Age (LBA, 14th century bc) glass, its production and trade, remains a popular topic of archaeological research and has been the subject of a great deal of debate (Nicholson et al. 1997; Shortland 2000a,b; Jackson 2005; Rehren and Pusch 2005; Nikita and Henderson 2006; Walton et al. 2009). The Egyptian sites, especially Amarna (Nicholson 2007) and Qantir (Pusch and Rehren 2007), have led the way in this work, partly because of excellent excavation work carried out here and partly due to the generally good glass preservation. Malkata has been less well studied, but appears to be similar in date and type to Amarna (Keller 1983). In the Near East and Aegean, no glass-making sites have yet been positively identified and, furthermore, in Mesopotamia even the evidence for glass-working is speculative (Oppenheim et al. 1970; Henderson 1998). This is despite the fact that glass is present in quite large quantities from sites such as Nuzi in modern northern Iraq (Starr 1939; Vandiver 1983). *Received 12 January 2009; accepted 27 May 2009 © University of Oxford, 2009

Isotopic discriminants between LBA glasses from Egypt and the Near East

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Despite these problems, recent compositional analysis by LA-ICPMS has shown trace element variations in LBA glass (Shortland 2005; Shortland et al. 2007). Glasses found on Egyptian sites could be distinguished from those found on Mesopotamian sites by virtue of several elements, especially Ti, Zr, Cr and La. This division in the data strongly suggests that there was independent production of glass in these two regions. The exact reason for the trace element variation between Egyptian and Mesopotamian glasses is still unclear. Egyptian glasses tend to be higher in Zr, Ti and La, whereas Near Eastern glasses are higher in Cr. These differences may reflect some impact on the glass composition from the different geologies associated with their unique river systems: the Egyptian Nile and its sediments are dominated by granitic rocks whereas the Tigris/Euphrates is influenced by more mafic terrains (Shortland 2005; Shortland et al. 2007). There are several possibilities of how this signature might be incorporated into the glass. It could be caused by varying plant ash compositions between the two areas, differences in silica source compositions and/or contamination of the melt by clay or grinding debris (Shortland 2005; Rehren and Pusch 2007; Shortland et al. 2007). In order to distinguish between these possibilities, to test whether colours may have been made at different sites and to further illuminate LBA glass-making raw materials and processes, a series of O, Sr and Nd isotopic measurements have been made on glasses from both Mesopotamia and Egypt. The glasses included production debris, ingots and finished objects, as detailed in Table 1. Glasses from the Egyptian sites of Amarna and Malkata have been indistinguishable by these techniques, suggesting they have very similar raw materials and processing technologies. This paper analyses glass from Malkata, but there is every reason to suspect that Amarna glass would be the same. The glass analysed here from all three sites was found distributed across the site, rather than in one room or context. LATE BRONZE AGE GLASS

The best studied LBA glass-making sites are without doubt in Egypt, at Amarna, from the mid 14th century bc (Nicholson 1995a,b, 2007; Shortland 2000a,b) and Qantir (Pusch and Rehren 2007), from the 13th century bc. These two sites present contrasting views of glass-making. Amarna glass-making seems to be dispersed over the site. It is relatively small scale and appears to be producing multiple colours of glass, especially cobalt and copper blues (Shortland 2000a,b; Nicholson 2007). Malkata appears similar in these respects. Furthermore, at Amarna glassmaking and glass-working appear to go on very close to each other, if not in the same furnaces and facilities. Qantir glass-making is on a more industrial scale and is concentrated together rather than being widely dispersed. It seems to specialize in the production of copper-blue glass next to some specialized colours and has very little evidence for working that glass into objects (Pusch and Rehren 2007). A great deal of work has been spent in trying to work out where particular LBA glass objects and/or glass ingots have been produced and how they were traded, especially in working out whether the Amarna model of multiple colours of glass being produced at one site or the Qantir model of specializing in a single colour should be regarded as the dominant model for the LBA (Nicholson et al. 1997; Shortland 2000a; Rehren et al. 2001; Jackson 2005). Work has concentrated on the analysis of glass-working debris and finished objects to try to identify compositional variations that might be indicative of source. Although this work has involved major element studies and more recently, trace element analysis, these questions are yet to be answered. This study, therefore, utilizes an isotopic analysis approach to help resolve some of these issues. © University of Oxford, 2009, Archaeometry 52, 3 (2010) 380–388

Nuzi 1930.82.17 1930.82.50 1930.82.55 1930.66.90b 1930.63.37 1930.60.140a 1930.82.59 Tell Brak TB8 TB1 TB2 TB7 TB10 Egypt—Malkata UPP31 UPP33 UPP39 UPP40 UPP30 UPP5 Vessel Ingot fragment Vessel Cylindrical bead Eye bead Bead Uncertain Ingot fragment Ingot fragment Ingot fragment Ingot fragment Ingot fragment Glass rod Glass rod Glass rod Glass rod Glass rod Glass rod

Translucent blue Opaque turquoise Opaque turquoise Opaque turquoise Opaque turquoise

Translucent blue Translucent blue Translucent blue Opaque blue Opaque blue Colourless

Type

Translucent blue Translucent blue Translucent blue Opaque turquoise Translucent brown Yellow Opaque white

Colour

© University of Oxford, 2009, Archaeometry 52, 3 (2010) 380–388

0.00002 0.00001 0.00001 0.00002 0.00002 0.00001

0.0001

0.70821 0.70785 0.70780 0.70793 0.70793 0.70787 0.70805

0.0002 0.0001

0.70839 0.70810

0.00001

0.70843

2s

0.00001 0.00001

Sr/86Sr

0.70838 0.70837

87

Nd/143Nd

low signal low signal low signal 0.512169 0.512194 0.512183

0.512472

0.512170 0.512372

0.512179

0.512150 0.512189

144

Table 1 Results of the oxygen, strontium and neodymium isotopic analyses

0.000012 0.000006 0.000006

0.000012

0.000032 0.000009

0.000008

0.000010 0.000018

2s

-9.1 -8.7 -8.9

-3.2

-9.1 -5.2

-9.0

-9.5 -8.8

e Nd

16.5

17.7 16.4

16.0 16.2 15.2 18.1 18.6

18.2

d18O

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Glass of this period was probably made by the combination of quartz(ite) pebbles, plant ash and colorant(s) with or without the deliberate addition of further lime (Turner 1956). Analysis of different isotope systems can give information on several aspects of these mineral raw materials used (Degryse et al. 2009). Oxygen isotope analysis was one of the first isotopic techniques to be applied to vitreous materials (Brill 1970). A natural range in d18O values of quartz sands and quartz veins or pebbles exists, depending on their specific geological origin, e.g., erosion from magmatic rocks or formation in varying hydrothermal or metamorphic conditions. Brill and co-workers (Brill 1970; Brill et al. 1999) state that the oxygen isotopic composition of ancient glass will be mainly dependent on the silica source used, as it is the predominant component supplying oxygen, with only minor influences of flux and stabilizer. The application of strontium isotopes to ancient glass depends primarily on the assumption that the strontium in the glass is incorporated with the lime-bearing constituents (Wedepohl and Baumann 2000). Strontium in LBA glass is hence principally derived from the plant ash used, the 87 Sr/86Sr isotope ratio thus reflecting the bio-available strontium of the soil on which these plants grew. This in turn reflects the geological origin of the soil (Freestone et al. 2003). Rehren (2008) has argued for an additional (potentially) significant Ca, and hence Sr, contribution to LBA glass from the parting layer of the crucibles used, being absorbed during glass melting. The Nd in glass is likely to have originated from the non-quartz mineral content of the silica raw material, and is typical for the geological environment from which this raw material originates (Degryse and Schneider 2008). Nd isotopes are used as an indicator of the provenance of siliciclastic sediments in a range of geological environments (Banner 2004).

METHODOLOGY

The 21 samples selected for isotopic analysis are shown in Table 1. Glass from three sites was selected for analysis, Malkata in Egypt and Nuzi and Tell Brak in Mesopotamia. Due to the small sample size of some of the samples, not all samples could be analysed by all techniques. However, all have been subjected to SEM-WDS following methodologies laid out in Shortland and Eremin (2006). A small range of colours was chosen for both Egypt and Mesopotamia to try to determine if there might be variation in production site by colour.

Strontium–neodymium isotopes For Sr–Nd isotope analysis, samples were weighed into Teflon screw-top beakers and dissolved in a 3:1 mixture of 22 M HF and 14 M HNO3 on a hot plate. Solutions were dried and dissolved in aqua regia. For separation of Sr and Nd from the same sample solutions, sequential extraction methods developed by Pin et al. (1994) were utilized and slightly modified. Sr and REE were separated using 2 M HNO3 on coupled miniaturized Teflon columns containing 50 ml of EICHROM Sr and TRU resin, respectively, and eluted with deionized water. For separation of Nd, the REE cut was further passed trough a column containing 2 ml EICHROM Ln resin. For this, the column was washed with 5.5 ml 0.25 M HCl after adding the sample. Nd was then stripped off using 4 ml 0.25 M HCl. All measurements were performed on a six-collector FINNIGAN MAT 262 thermal ionization mass spectrometer (TIMS) running in static multicollection mode. Sr isotopic ratios were normalized to 86Sr/88Sr = 0.1194, Nd isotopic ratios were normalized to 146Nd/144Nd = 0.7219. Repeated static measurements of the NBS 987 standard over the duration of the study yielded an average 87Sr/86Sr ratio of 0.71025 1 2 (2s). Repeated © University of Oxford, 2009, Archaeometry 52, 3 (2010) 380–388

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measurements of the La Jolla Nd standard yielded 143Nd/144Nd = 0.511848 1 0.000009 (2s). Total procedural blanks did not exceed 30 pg Sr and 50 pg Nd and were found to be negligible. Oxygen isotopes All separates were analysed using a laser fluorination procedure, involving total sample reaction with excess ClF3 using a CO2 laser as a heat source (in excess of 1500°C; Sharp 1990). All combustions resulted in 100% release of O2 from the silica lattice. This O2 was then converted to CO2 by reaction with hot graphite, then analysed online by a VG SIRA 10 spectrometer. Reproducibility is better than 10.3‰ (1s). Results are reported in standard notation (d18O) as per mil (‰) deviations from the Standard Mean Ocean Water (V-SMOW) standard. RESULTS AND DISCUSSION

The WDS analyses showed that all the glasses were of a soda–lime–silicate composition with significant magnesia and potash that is typical of plant ash fluxed glass of the Late Bronze Age (Table 2). Several different colorants and colouring strategies were identified. The majority are copper blue, but the exceptions are cobalt blue (UPP30 and UPP40), cobalt and copper blue (UPP33), lead antimonate yellow (1930.60.140a), calcium antimonate white (1930.82.59) and deliberate colorant free (UPP5 and 1930.63.37). The results of the isotopic analyses are shown in Table 1. During the measurement of oxygen isotopes, one sample from Nuzi and two from Tell Brak had low oxygen yields, making the measurements somewhat questionable. Reported values in Table 1 represent the average of multiple measurements, except in cases where only a single measurement was made (objects 1930.82.59, 1930.60.140a and TB2). The d18O values of the six Nuzi and three Tell Brak samples all lie in the range 16.0–18.6, six lying between 16.0 and 16.6. There is no obvious separation between the two sites. No oxygen isotope values were run for the Egyptian samples because these have been well characterized by Brill et al. (1999; 311–16). They conducted six analyses of Amarna glasses of various colours (O-1, O-35, O-36, O-37, O-39 and 1515) and one of an unprovenanced Egyptian glass (O-30). The values of these Egyptian glasses lie between 15.12 and 17.46. LBA glasses from Mesopotamia and Egypt do not separate based on their oxygen isotope signatures alone. All Tell Brak samples lie within two standard deviations of the Nuzi average. The same is true for earlier measurements on Egyptian glass. As may be seen in Figure 1, Egyptian (Malkata) glasses contain the lowest Sr ratios, ranging between 0.70780 and 0.70793. The Nuzi samples range between 0.70837 and 0.70849. Two Tell Brak samples have an intermediate value of 0.70810–0.70821, between the Egyptian and Nuzi groups. Their isotopic signature is more than two standard deviations from the mean of both the Nuzi and Egyptian groups. One Tell Brak sample (the ingot fragment TB1) is identical in Sr isotopic composition to the Nuzi glass with a 87Sr/86Sr value of 0.70839. The Nd isotope signatures from glasses of different origins also display marked differences. Unfortunately, Nd measurements for four of the Egyptian glasses failed because the sample size was too small, leading to a low Nd yield, but the remainder fall into the range between 0.512169 and 0.512194. The Nuzi samples are very similar at between 0.512150 and 0.512189. One Tell Brak glass, TB1—the same sample that has an identical Sr isotopic composition to the Nuzi material—has a Nd signature of 0.512170, identical to the Nuzi glasses. Two Tell Brak samples with Nd signatures of 0.512472 and 0.512372 are several standard deviations away from the mean signature of the Nuzi and Egyptian glasses. © University of Oxford, 2009, Archaeometry 52, 3 (2010) 380–388

SiO2 Al2O3 CaO MgO Na2O K2O FeO TiO2 CoO CuO MnO NiO ZnO As2O5 SnO2 Sb2O5 BaO PbO2 Cr2O3 P2O5 SO3 Cl SrO Total

1930. 82.50

65.76 0.37 8.58 4.02 14.36 3.12 0.19 0.00 0.00 2.10 0.00 0.00 0.00 na 0.00 0.06 0.00 0.00 0.00 0.11 0.24 1.08 0.00 99.61

1930. 82.17

66.0 0.93 4.80 4.94 17.36 3.00 0.42 0.04 0.00 1.20 0.06 0.00 0.00 na 0.00 0.09 0.00 0.00 0.00 0.18 0.38 0.59 0.00 98.96

62.29 0.69 6.12 6.31 16.96 4.79 0.30 0.03 0.00 1.13 0.00 0.00 0.00 na 0.00 0.15 0.00 0.00 0.00 0.21 0.39 0.63 0.00 97.70

1930. 82.55

65.73 0.28 8.93 3.57 12.63 2.58 0.11 0.00 0.00 1.69 0.00 0.00 0.00 na 0.00 3.11 0.00 0.00 0.00 0.23 0.34 0.79 0.00 99.13

1930. 66.90b 66.72 0.63 6.39 4.94 16.91 2.43 0.31 0.06 0.00 0.00 0.00 0.00 0.00 na 0.00 0.06 0.04 0.00 0.00 0.16 0.16 1.18 0.00 95.36

1930. 63.37 66.53 1.20 3.10 3.85 13.70 1.49 0.45 0.05 0.00 0.02 0.04 0.00 0.00 na 0.00 0.50 0.00 8.10 0.00 0.10 0.28 0.63 0.01 101.25

1930. 60.140a 64.97 0.39 7.81 4.77 15.24 2.85 0.19 0.03 0.00 0.02 0.00 0.00 0.00 na 0.00 2.28 0.00 0.00 0.00 0.15 0.30 0.83 0.17 99.39

1930. 82.59 62.2 0.4 6.5 6.7 19.3 2.6 0.3 0.02 0.03 0.72 0.04 0.05 0.02 0.04 0.00 0.00 0.01 0.01 0.04 0.12 0.22 0.91 na 98.56

TB8

64.6 0.2 8.5 3.0 17.4 1.8 0.1 0.03 0.00 1.22 0.02 0.02 0.02 0.04 0.02 2.10 0.00 0.03 0.04 0.13 0.29 0.62 na 99.86

TB1

70.5 0.2 6.1 2.6 14.6 1.5 0.1 0.03 0.00 1.63 0.02 0.00 0.09 0.03 0.02 1.74 0.00 0.01 0.01 0.14 0.25 0.69 na 99.67

TB2

68.6 0.5 8.9 3.0 13.3 2.1 0.2 0.03 0.03 0.76 0.02 0.04 0.02 0.06 0.01 1.36 0.01 0.02 0.00 0.20 0.25 0.89 na 97.83

TB7

66.2 0.1 4.7 6.3 18.6 2.5 0.1 0.02 0.04 0.04 0.02 0.00 0.05 0.08 0.00 0.00 0.00 0.02 0.02 0.21 0.62 0.45 na 98.04

TB10

60.3 0.7 6.3 4.5 20.8 2.7 0.4 0.05 0.02 0.67 0.03 0.02 0.01 0.03 0.34 1.28 0.02 0.00 0.01 0.31 0.44 1.03 na 100.8

UPP 31 63.4 1.8 7.5 4.0 19.7 0.7 0.5 0.07 0.12 0.46 0.10 0.04 0.03 0.01 0.02 0.00 0.02 0.00 0.01 0.09 0.27 1.23 na 101.9

UPP 33 62.0 0.6 8.8 4.1 17.5 1.9 0.5 0.06 0.01 1.80 1.17 0.01 0.01 0.01 0.16 0.06 0.04 0.02 0.02 0.13 0.32 0.77 na 100.7

UPP 39 57.2 4.2 4.9 4.8 23.3 1.0 0.7 0.08 0.21 0.03 0.35 0.15 0.25 0.04 0.00 0.89 0.04 0.01 0.04 0.27 0.54 0.98 na 99.2

UPP 40

59.8 2.0 9.2 5.8 20.0 0.7 0.3 0.07 0.05 0.15 0.06 0.04 0.07 0.04 0.04 0.29 0.02 0.02 0.01 0.08 0.32 0.99 na 101.0

UPP 30

67.1 1.1 8.6 3.9 14.2 3.0 0.6 0.08 0.01 0.00 0.03 0.02 0.01 0.01 0.02 0.00 0.04 0.01 0.01 0.15 0.21 0.85 na 99.9

UPP 5

Table 2 WDS analyses for the glasses in the study. All analyses normalized to 100%, na = not analysed. Some have previously been published in Shortland and Eremin (2006)

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P. Degryse et al.

144

Nd/143Nd

386

87

Sr/86Sr

Figure 1 Sr against Nd isotopic ratios for the glasses of the study.

The fact that the Egyptian and Nuzi glass samples have similar Nd isotopic compositions is remarkable, but not exceptional. The range in Nd isotopic composition of known eastern Mediterranean coastal or inland silica sources for glass production reported by Degryse and Schneider (2008) and Henderson et al. (2009) concurs well with the values found for the aforementioned glasses. This limits the possibilities of one isotope system alone to be able to distinguish several sources of LBA glass raw materials, and stresses the necessity of using combined systems. Taking the Sr and Nd data together, an Egyptian (Malkata) and Nuzi group can be recognized, next to more disperse analyses for Tell Brak, but each grouping with statistically distinct isotopic characteristics. The Egyptian glasses have low Sr and Nd ratios, whereas the Nuzi (and one Tell Brak) glasses have low Nd ratios but high Sr ratios. In contrast, the remaining two Tell Brak samples have high Nd ratios and intermediate Sr ratios. The Sr isotopic composition clearly distinguishes Egyptian and Nuzi productions of glass, while its Nd isotopic composition is similar. Both groups hence have a lime source with contrasting Sr characteristics, but have silica raw materials of similar Nd isotopic compositions. One of the glasses found in Tell Brak, a fragment of an ingot, is identical to the Nuzi glasses, suggesting that it may have shared a source with the Nuzi glass. However, the two other Tell Brak glasses are distinct from the Nuzi glasses with a separate silica source (different Nd isotopic composition) and a separate plant ash (intermediate Sr isotopic composition). As the analyses values of both samples lie far apart, it is unclear if this should be regarded a separate Tell Brak group, or whether all Tell Brak glass analysed had different origins. However, SEM-WDS (Shortland and Eremin 2006) and LA-ICPMS analyses (Shortland et al. 2007) for glasses from Nuzi and Tell Brak showed no distinguishing features, as they formed a continuous group for both major and trace elements. CONCLUSIONS

When analysing only the oxygen or neodymium isotope system in LBA glasses from Egypt and Mesopotamia, different provenances cannot be readily distinguished, as there is too much overlap between groups. Sr isotope analysis offers a more distinguishing technique. However, as this paper has shown, the combined analysis of these isotope systems, especially for Sr–Nd, is most © University of Oxford, 2009, Archaeometry 52, 3 (2010) 380–388


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successful. First, it has shown clear differences between Egyptian and Mesopotamian glasses that reinforce those seen in trace elements (Shortland 2005; Shortland et al. 2007). More importantly, for the first time it has shown distinct groups within the Mesopotamian sites, most Nuzi and Tell Brak glasses being distinct both in Sr and Nd ratios. Not only that, but despite the low number of glasses analysed, one glass found in Tell Brak seems to have a Sr–Nd isotopic composition that is typical of the glasses from Nuzi, suggesting exchange either between these two sites, or between Tell Brak and a third site which was supplying Nuzi with glass. LBA glasses that can be identified as having been traded are exceptional, despite literary and archaeological evidence that the trade took place (e.g., the Uluburun shipwreck), and are analytically proven only in rare cases (Walton et al., 2009). This paper shows the value of isotopic studies on the provenancing of LBA glass from Egypt and the Near East. Further Sr and Nd analyses combined with a growing database of major and trace element data, and exploration of the potential of oxygen isotope analysis for the same glasses, promise to delineate new compositional groupings, point to new production areas and sites and further illuminate the trade in this interesting and valuable material. ACKNOWLEDGEMENTS

The authors would like to thank all those institutions that contributed material to this study of early glasses, including James Armstrong (Harvard Semitic Museum), Joan Oates (McDonald Institute), the Victoria Museum of Egyptian Antiquities (Uppsala) and Nationalmuseet (Copenhagen) and two anonymous referees for their most useful comments.

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