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Multidisciplinary approaches to food and foodways in the medieval Eastern Mediterranean

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Sylvie Yona Waksman

Trading goods, trading tastes

Residue analysis of medieval amphorae from the Eastern Mediterranean

Alessandra Pecci, Nicolas Garnier and Sylvie Yona Waksman

Abstract

The POMEDOR project gave the opportunity to investigate the provenance and contents of some of the main types of Middle and Late Byzantine amphorae, for which we had very little information so far. This paper presents the first results obtained by residues analyses on amphorae of types Günsenin III and IV, which were widespread in the Mediterranean and the Black sea in the 12th-13th century AD, and are probably among the latest Mediterranean transport amphorae. We also studied another type of amphora, known only in the Levantine area in the Crusader period.
The samples were analysed with gas chromatography-mass spectrometry. Different extraction methods were carried out in order to identify the residues preserved.
The results of the analyses show wine was likely contained in almost all the amphorae. However, residues of plant oils were also present together with animal origin products and Pinaceae products probably used to coat the amphorae. In general, the results of the analyses seem to indicate that the analysed amphorae were often reused.

Full text

Introduction

1Residue analysis of ceramics has had a great improvement in the last 30 years (Condamin et al. 1976; Evershed 1993; 2008; Garnier et al. 2002; 2009; Pecci 2009; Regert 2011; Nigra et al. 2015). Although there are still problems in the identification of substances and control of contamination, we can obtain reliable data on the contents of ceramic vessels and in particular their coatings (pitch, resin, beeswax and sulfur) (Colombini et al. 2005; Garnier 2007; Garnier & Pecci, forthcoming; Garnier et al. 2009; 2011; Parras et al. 2015; Pecci 2016; Pecci et al. 2010a; 2010b; 2015). During the last years the analysis of amphorae has come back to the attention of international scholars (Garnier & Pecci, forthcoming; Garnier et al. 2009; Pecci & Cau Ontiveros 2014; Pecci & Giorgi, forthcoming; Pecci et al. 2010a, 2010b; 2015; Romanus et al. 2009; Woodworth et al. 2015). Nonetheless, residue analysis of amphorae has not had the same improvement as residue analysis of cooking vessels or other ceramic categories. Moreover, few residue analyses have been carried out until now on amphorae, if we compare them to the number of provenance studies. Until now, few analyses have been carried out in a systematic way, and many of them have been performed in consumption sites where there is a stronger possibility of reuse (Garnier & Pecci, forthcoming). Another problem concerning residue analysis of amphorae is that adequate methods were not always applied, in particular to look for wine, which can only be identified using specific methods (Barnard et al. 2010; Garnier & Valamoti 2016; Guash-Jané et al. 2004; Pecci et al. 2013). Moreover, not enough care is taken to avoid overinterpretations, which are unfortunately common, providing conclusions that look interesting, but lack scientific rigour and valid arguments (Garnier 2015).

  • 1 We are not mentioning here Late Roman/Early Byzantine amphorae, for which many studies are availab (...)
  • 2 These analyses were carried out in the framework of a French-Ukrainian DNIPRO program, directed by (...)

2The archaeometric study of medieval amphorae in the Eastern Mediterranean has been particularly neglected so far,1 with few exceptions focusing on provenance issues mainly (Megaw & Jones 1983; Günsenin & Hatcher 1997; Shapiro 2012; for residues analysis, see Todorova, in this volume). In the framework of the POMEDOR project we had the opportunity to investigate the provenance and contents of some of the main types of Middle and Late Byzantine amphorae (results of provenance studies appear in Waksman et al. 2018; Morozova et al., in this volume). For the study of contents, we focused on amphorae of types Günsenin III and IV (Günsenin 1989), which were widespread in the Mediterranean and the Black Sea in the 12th-13th century AD. These two types were probably among the latest Mediterranean transport amphorae, before they were replaced by other containers, especially barrels (Jacoby 2010; Bevan 2014). A first attempt to analyze residues in a small-size amphora of type Günsenin XX was carried out in 2005 by F. Formenti (unpublished), in order to test the hypothesis that they carried incense (Zelenko 1999); only pine resin was identified back then.2

3We also looked at another type of amphorae, very different from the previous ones, as it is characterized by a restricted geographical distribution, on the Levantine coast, and is found during a limited time, in the Crusader period. The introduction of this new type seems to be related to the arrival of Frankish populations, and residues analyses were to investigate whether they carried specific products.

4The samples were analysed with gas chromatography-mass spectrometry. Different extraction methods were carried out in order to identify the residues preserved.

Sampling and methodology

Sampling (fig. 1)

Fig. 1 – Representative examples of the types of amphorae investigated.

Fig. 1 – Representative examples of the types of amphorae investigated.

Amphora of type Günsenin III (above left, BZN322) and intermediate type Günsenin II‑III (above right, sample BZY802) (from excavations of the 23rd Ephorate of Byzantine Antiquities in Dokos site, Chalkida, Greece); amphora of type Günsenin IV (below right, from underwater excavations of Kiev National Taras Shevchenko University in Novy Svet, Crimea); “Levantine” type (below left, sample LEV811, from excavations of the Israel Antiquities Authority in the Hospitallers complex, Acre, Israel) (photos S.Y. Waksman except below right, Kiev National Taras Shevchenko University).

5Three batches of amphorae, one of each type, were sampled for residues analysis. They were selected by archaeologists according to typological considerations. Before samples were submitted to organic residues analysis, chemical analysis of the bodies was carried out by wavelength dispersive X-ray fluorescence in Lyon (CNRS UMR 5138, see e.g. Waksman 2011 for the analytical protocol) in order to select for each batch samples likely to come from a single production site. With this preliminary stage we tried to reduce the number of parameteres which could vary within a batch. However, the contexts of discovery are very diverse.

Amphorae of type Günsenin III

6All the sampled amphorae came from central Greece, mostly from contexts located in or close to Chalcis (modern Chalkida) where these amphorae were manufactured (Waksman et al. 2018). Chalcis was a main maritime gateway for agricultural products of central Greece, and the production of wine is archaeologically well attested in the region in the Byzantine period (Kontogiannis et al., in this volume).

  • 3 We would like to thank warmly S. Skartsis, G. Vaxevanis and N. Kontogiannis for providing these sa (...)

7Four samples were selected together with N. Kontogiannis, S. Skartsis and G. Vaxevanis from the material of rescue excavations carried out by the 23rd Byzantine Ephorate of Chalkida.3 They came from different contexts in the city of Chalcis or its countryside: 1 sample came from a rubbish pit outside the medieval city walls (BZY798, from Mitropoleos street); 1 sample from a domestic area inside the city walls (BZY804, from IKA plot); 2 samples (BZY802, BZY803) came from ancient excavations of what may have been an agricultural installation in the countryside, in the village of Dokos, where several complete amphorae were found. All the amphorae analysed were initially identified as Günsenin III type except for sample BZY802 which is an intermediate type between Günsenin II and III. This may also be the case for BZY798, BZY802, BZY804; all are of Chalcis origin (Waksman et al. 2018).

  • 4 Our many thanks to the directors of the excavation, S. Larson and K. Daly, and to F. Kondyli who i (...)

8The last amphora in this batch (BZN204) was found in Thebes during the ongoing American excavations carried out by Bucknell University in the framework of the Thebes Ismenion Hill Synergasia Project. This almost complete example of Günsenin III type was found in the context of a closed cesspit, and the sampling was carried out during the excavations, in the best possible conditions for the preservation of organic residues.4

Amphorae of type Günsenin IV

  • 5 We would like to thank Y. Morozova and S. Zelenko for their kind collaboration, and A. Shapiro for (...)

9The amphorae of type Günsenin IV came from of a shipwreck located in the bay of Novy Svet in the Crimea (Zelenko 1999; Zelenko & Morozova 2010). Samples (BZN250, BZN252‑254) were taken by Y. Morozova during the 2013 season of the underwater excavations carried out in Novy Svet by the Taras Shevchenko National University of Kiev, under the direction of S. Zelenko.5 The origin of these amphorae has not been identified yet.

Amphorae of the Crusader Levant

  • 6 Many thanks to E.J. Stern and A. Shapiro, and to A. Lester and G. Roccabella for their help in the (...)

10These samples were selected from the material of excavations carried out in northern Israel by the Israel Antiquities Authority, in collaboration with E.J. Stern and A. Shapiro who had previously done their typological and petrographical study (Stern 2012, vol. 1, pp. 38‑40, vol. 2, pp. 34‑35; Shapiro 2012).6 Two amphorae come from the Hospitallers complex in Acre/‘Akko (LEV811, LEV814, Stern 2012, vol. 2, pp. 34‑35, 4.12: 2 and 4.12: 8 respectively). The third one comes from the rural settlement of Horbat ‘Uza (LEV820, Getzov et al. 2009, fig. 3.22: 14). Petrographic analysis carried out by A. Shapiro suggest an origin in northern Lebanon (Shapiro 2012, pp. 106, 109, 119, tabl. 5.4).

Methods

11Each sample was pulverized and subjected to different extraction methods:

  • a) The lipid extract (LE) was obtained for all the samples following Evershed’s method, to identify the presence of the organic coatings and the animal and vegetal products (Mottram et al. 1999). The ground sample was extracted once with dicholoromethane/methanol (1:1 v/v, 3 mL) in a sonication bath for 40 min at 70°C. The liquid fraction was recovered after centrifugation and dried using a gentle stream of nitrogen.
  • b) All pulverized LE samples were then submitted to the extraction method published by Garnier and Valamoti (2016), to identify grape and fermentation biomarkers, and to distinguish white from dark grape.
  • c) Samples BZN204 and BZY804 from Greece, LEV811, LEV814 from Israel and BZN250, BZN252 and BZN253 from Crimea were also extracted following the method published by Pecci et al. (2013) to identify wine biomarkers (both grape and fermentation biomarkers). When this extraction is carried out directly on the pulverized sample, like in this case, it does not allow to differentiate if syringic acid derives from malvidine, and therefore from dark grape, or from other substances.

12Extracts a and b were derivatized and analysed with gas chromatography-mass spectrometry using GC-MS (Thermo GC Trace Ultra fitted with a column Phenomenex Zb-5MSi 20 m long, 0.18 mm internal diameter, 0.1 µm film thick, coupled to a DSQ II mass spectrometer used in electronic impact mode at 70 eV, for extracts a and b. Extracts of method c were derivatized and analysed using a Thermo Scientific Trace GC Ultra chromatograph equipped with a column TRB-5MS Teknokroma 5% phenyl 95% methyl polysiloxane, 30 m long, 0.25 mm internal diameter, 0.25 µm film thick and coupled with a Thermo Scientific ITQ900 mass spectrometer operated in the electron ionization mode (70 eV).

Results of the analyses

Results of the analysis of the Günsenin III amphorae from Greece

13All the samples of types Günsenin III and II‑III (BZN204, BZY798, BZY802, BZY803 and BZY804) show the markers of an organic coating of Pinaceae products used for waterproofing the ceramic.

14In the chromatograms of extraction b, the presence of tartaric acid in BZY804 and BZY798, and malic and tartaric acids in the other samples, indicates that very likely grape juice was present in all the amphorae. In fact, although tartaric acid is also present in other fruits (i.e. tamarind, Barnard et al. 2010), it is likely that in this area of the world and this period, tartaric acid is related to grape and a derivative of grape juice was contained in amphorae (Pecci et al. 2013; Garnier & Valamoti 2016) (fig. 2). In BZY802 and BZY803 the presence of syringic acid suggests that the juice was “red”. According to the implemented double-step extraction methodology, this acid is absent in the first lipid extract i.e. absent in the free form in the sampled amphorae, but it is present in the extract b resulting of an acid-catalysed extraction; this allows confirming the origin of the syringic acid from malvidine and its derivatives, i.e. from dark or teinturier grape (Barnard et al. 2010; Garnier & Valamoti 2016). Extraction c indicates the presence of succinic, malonic and fumaric acids, besides tartaric acid in sample BZN204 and succinic, malic and tartaric acid in sample BZY804 (fig. 3). These acids are markers of fermentation, and suggest the grape derivative placed in the amphora was wine.

Fig. 2 – Chromatogram of the extract b of sample BZY798.

Fig. 2 – Chromatogram of the extract b of sample BZY798.

Fig. 3 – Chromatogram of the extract c of sample BZN204.

Fig. 3 – Chromatogram of the extract c of sample BZN204.

15In all the amphorae cholesterol is also detected that indicates animal products or contamination. If it derives from animal products, these products could derive from a re-use of the amphorae, or from the use of animal origin products mixed with the coniferous products used for the coating. The presence of 3‑methoxyserrat-14-en-21-one in BZN204 refines the identification of the pitch to Pinaceae wood (fig. 4).

16Moreover β-sitosterol in samples BZY798 and BZN204 suggests that a plant oil was present in the samples.

Fig. 4 – Chromatogram of the extract a of sample BZY798.

Fig. 4 – Chromatogram of the extract a of sample BZY798.

Results of the analysis of the Günsenin IV amphorae from Crimea

17The samples of type Günsenin IV (BZN250, BZN252 to 254) belong to amphorae recovered in a shipwreck. The results of the analyses are typical of amphorae found in underwater contexts, in which pitch is present: dehydroabietic acid present in free and methylated form, and other acids typical of Pinaceae products are present in high amounts. Moreover, retene indicates these products were heated at a high temperature and correspond to pitch. These acids are very well preserved and very abundant. In some cases, an organic coating is still visible even to the naked eye. In sample BZN254 the abundance of abietic acid suggests the coating comes from an Abies sp. tree (fig. 5).

Fig. 5 – Chromatogram of the extract a of sample BZN254.

Fig. 5 – Chromatogram of the extract a of sample BZN254.

18The presence of tartaric acid, malic and syringic acids in extraction b indicates that a dark grape derivative was present in the amphorae: as said above, tartaric acid can be related also to other fruits, although it is likely that the content of the amphorae was wine. Succinic acid together with tartaric acid in extraction c of samples BZN250, 252 and 253 confirms the fermented beverage. Wine was a dark (red) wine as revealed by the syringic acid in extraction b (Barnard et al. 2010). β-sitosterol is present in three of the four samples. This is related with the presence of fatty vegetal products, possibly oils.

Results of the analysis of Levantine amphorae

19The samples from Israel (LEV811, LEV814 and LEV820) are very polluted by modern synthetic materials such as plastics and plasticizers. In fact, phtalates are detected in high amount in all chromatograms. However, it is possible to identify markers of the original content of the amphorae. The presence of tartaric acid and malic acids in extraction b of all the samples indicates that grape juice/wine was present in the amphorae. The succinic, isocitric and malic acids identified together with the tartaric acid in extraction c of sample LEV811 and succinic and tartaric acids in LEV814, confirm that wine was contained in the amphorae. The presence of syringic acids in extraction b of sample LEV811 suggests it was red wine. In the other two samples there is no syringic acid. Although the literature suggests that in these cases the juice/wine was “white” (Guash-Jané et al. 2006), we are more cautious and we consider that if syringic acid is present we can confirm the juice was red, while if the acid is not identified we cannot be sure of the colour of the wine.

20In the three samples the presence of cholesterol indicates the presence of contamination from the burial context or of animal products, possibly related to the coating of the amphorae. Moreover, the presence of β-sitosterol together with linoleic acid indicates that there was also a plant oil different from olive oil.

21The latter point, together with the absence of red wine markers in 2 out of the 3 samples, seem to differentiate this type of amphorae from the Byzantine types Günsenin III and IV. Further systematic analyses would be requested to confirm this trend, and to understand if it may have any relationship with the Frankish presence in the Levant.

Conclusion

22Although carried out on a limited number of samples, this study is among the very first investigations of the contents of medieval amphorae in the Eastern Mediterranean.

23An interesting result is that Pinaceae products were used to coat all the amphorae, irrespective of the type and of the context of recovery. This confirms the results obtained performing residue analysis of amphorae until now (Garnier 2003; 2007; Garnier & Pecci, forthcoming; Garnier et al. 2009; Pecci 2009; Pecci et al. 2010a; 2010b; Woodworth et al. 2015). Pinaceae products are particularly abundant in samples from Crimea. This is probably related to the fact that the recovery context is a shipwreck, which allows a good preservation of organic materials. In this case we were able to suggest that in one amphora the coating was from Abies sp. wood.

24If they do not derive from contamination, animal origin products in some of the amphorae found in Greece or in Israel may be related either to the use of these products to soften the coating of the amphorae, or to the content of the amphorae.

25The results of the analyses show that grape juice/wine was contained in all the analysed amphorae, indicating the importance of the trading and consumption of this product in the medieval Eastern Mediterranean. In the cases of type Günsenin IV and of some samples of types Günsenin III, II‑III and Levantine amphorae, it was possible to assess that the grape derivative was a red wine, due to the presence of syringic acid. However, when this acid is absent we do not dare suggesting that the wine was white as the amphorae have been taken from different excavations and no comparison among samples from the same context is possible. In some of the amphorae, residues of plant oils were also present.

26One of the major problems of residue analysis of ceramic vessels is that the ceramic matrix absorbs the different substances with which it comes into contact. Therefore, it is not possible to know which substance was absorbed first, and which later, nor if more than one substance were present at the same time (i.e. if animal products were mixed to Pinaceae products for the coating, or if they were separate). This has an important consequence in the interpretation of the results obtained: when residues of different substances are absorbed, we are not able to determine if they were present together in the primary use of the amphora, or in the case of re-use which one was the initial content.

27Therefore, in general, it is difficult to say if the analysed amphorae had a preferred content, although the fact that wine is present in all the samples could give us a hint. However, the results indicate that the amphorae seem to have been reused, possibly several times.

28To achieve better understanding of the content of the types analysed we should go on doing more and more systematic analyses, preferentially on amphorae coming from shipwrecks that present less chances of having been reused, although there is evidence of reuse for amphorae found in shipwrecks too (van Doorninck 1989). Nonetheless the results obtained are very promising, and we are confident that this first step can stimulate further research.

Acknowledgements

29This study was funded by the French National Research Agency (ANR) through the POMEDOR project (People, pottery and food in the medieval Eastern Mediterranean, www.pomedor.mom.fr), directed by Yona Waksman, and we acknowledge the support of the ANR under reference ANR-12‑CULT-0008.

30It is also part of the activities of the ERAAUB, Consolidated Group (2014 SGR 845) funded by the Comissionat per a Universitats i Recerca del DIUE of the Generalitat de Catalunya, of the Ramon y Cajal contract of Alessandra Pecci (RYC 2013‑13369) funded by the Spanish Ministry and the RACAMed Project (HAR2017-84242-P). We are grateful to our colleagues who provided samples for this study (n. 2 to 5), as well as to the authorities who gave us permission to proceed to sampling and to export samples for analysis.

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Notes

1 We are not mentioning here Late Roman/Early Byzantine amphorae, for which many studies are available (e.g. Pecci 2018; Yangaki 2014).

2 These analyses were carried out in the framework of a French-Ukrainian DNIPRO program, directed by S. Zelenko (Taras Shevchenko National University of Kiev), and by S.Y. Waksman.

3 We would like to thank warmly S. Skartsis, G. Vaxevanis and N. Kontogiannis for providing these samples and for information about the contexts.

4 Our many thanks to the directors of the excavation, S. Larson and K. Daly, and to F. Kondyli who is in charge of the study of this material, for giving us access to it and for organizing the sampling, and to N. Kontogiannis, S. Skartsis, G. Vaxevanis and H. Wurmser for their help.

5 We would like to thank Y. Morozova and S. Zelenko for their kind collaboration, and A. Shapiro for translating the paper by Zelenko (1999) into English.

6 Many thanks to E.J. Stern and A. Shapiro, and to A. Lester and G. Roccabella for their help in the storerooms.

List of illustrations

Title Fig. 1 – Representative examples of the types of amphorae investigated.
Caption Amphora of type Günsenin III (above left, BZN322) and intermediate type Günsenin II‑III (above right, sample BZY802) (from excavations of the 23rd Ephorate of Byzantine Antiquities in Dokos site, Chalkida, Greece); amphora of type Günsenin IV (below right, from underwater excavations of Kiev National Taras Shevchenko University in Novy Svet, Crimea); “Levantine” type (below left, sample LEV811, from excavations of the Israel Antiquities Authority in the Hospitallers complex, Acre, Israel) (photos S.Y. Waksman except below right, Kiev National Taras Shevchenko University).
URL http://books.openedition.org/momeditions/docannexe/image/10274/img-1.jpg
File image/jpeg, 812k
Title Fig. 2 – Chromatogram of the extract b of sample BZY798.
URL http://books.openedition.org/momeditions/docannexe/image/10274/img-2.jpg
File image/jpeg, 347k
Title Fig. 3 – Chromatogram of the extract c of sample BZN204.
URL http://books.openedition.org/momeditions/docannexe/image/10274/img-3.jpg
File image/jpeg, 243k
Title Fig. 4 – Chromatogram of the extract a of sample BZY798.
URL http://books.openedition.org/momeditions/docannexe/image/10274/img-4.jpg
File image/jpeg, 301k
Title Fig. 5 – Chromatogram of the extract a of sample BZN254.
URL http://books.openedition.org/momeditions/docannexe/image/10274/img-5.jpg
File image/jpeg, 414k

Author(s)

Universitat de Barcelona, Equip de Recerca Arqueològica i Arqueomètrica (ERAAUB), Departament de Prehistòria, Història Antiga i Arqueologia, Facultat de Geografia i Història, c/ Montalegre 6‑8, 08001 Barcelona, Spain, alepecci@gmail.com

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