31-44

• Mayyas, Abdulraouf. S.
• Douglas, Khaled. A.

This paper discusses the analysis and occurrence of organic residues in Iron Age II pottery sherds excavated at the site of Jneneh. Gas chromatography – mass spectrometry was used for separation and identification of organic constituents. Conventional solvent extraction and alkaline hydrolysis (saponification) were used for the extraction of residues preserved in their fabrics. Three sherds among six unwashed and unhandled sherds showed significant preservation of organic constituents derived from natural materials. The results provide data on the occurrence of beeswax that could have been intentionally added on the internal surface of a collared-rim jar for storing liquid substances or dry goods. Unintentional occurrence of beeswax as a result of storing honey including beeswax fragments of the honeycomb is also possible. In addition, biomarkers of plant oil were detected in a medium jug and a small jar that might have been used for daily needs, such as food preparation. The absence of significant organic constituents in the other three vessels could be attributed to the degradation overtime during burial.

• History and Archaeology
• Chemical sciences

• Archaeology and history
• Iron age

Iron Age Pottery, Jneneh, Ammonite Pottery, Ceramic, Organic Residue, Lipid, Beeswax, Biomarker, Gas Chromatography - Mass Spectrometry, Extraction

Corresponding author: Abdulraouf Mayyas ([email protected])

1. Anderson-Stojanović, V. R., Jones, J. E. (2002) Ancient Beehives from Isthmia. Hesperia, Vol. 71, No 4, 345-376.Aveling, E. M., Heron, C. (1999) Chewing Tar in the Early Holocene: An Archaeological and Ethnographic Evaluation. Antiquity, Vol. 73, 579-584.Baeten, J., Romanus, K., Degryse, P., De Clercq, W., Poelman, H., Verbeke, K., Luypaerts, A., Walton, M., Jacobs, P., De Vos, D., Waelkens, M. (2010) Application of a Multi-Analytical Toolset to a 16th Century Ointment: Identifica-tion as Lead Plaster Mixed with Beeswax. Microchemical Journal, Vol. 95, 227-234.Bonaduce, I., Colombini, M. P. (2004) Characterisation of Beeswax in Works of Art by Gas Chromatography–Mass Spec-trometry and Pyrolysis–Gas Chromatography–Mass Spectrometry Procedures. Journal of Chromatography A, Vol. 1028, 297-306.Boran, G., Karaçam, H. and Boran, M. (2006) Changes in the quality of fish oils due to storage temperature and time. Food Chemistry, Vol. 98, 693-698.Bull, I. D., van Bergen, P. F, Nott, C. J., Poulton, P. R. and Evershed, R. P. (2000) Organic geochemical studies of soils from the Rothamsted classical experiments–V. The fate of lipids in different long-term experiments. Organic Geochemistry, Vol. 31, 389–408.Charters, S., Evershed, R. P., Blinkhorn, P. W., Denham, V. (1995) Evidence for the Mixing of Fats and Waxes in Archaeo-logical Ceramics. Archaeometry, Vol. 37, 113-127.Colombini, M. P. and Modugno, F. (2009) Organic materials in art and archaeology. In Organic Mass Spectrometry in Art and Archaeology, M. P. Colombini and F. Modugno (eds.), John Wiley and Sons, Ltd, Chichester, pp. 3-36.Colombini, M. P., Giachi, G., Modugno, F. and Ribechini, E. (2005) Characterisation of organic residues in pottery vessels of the Roman age from Antinoe (Egypt). Microchemical Journal, Vol. 79, 83-90.Copley, M. S., Rose, P. J., Clapham, A., Edwards, D. N., Horton, M. C. and Evershed, R. P. (2001) Detection of palm fruit lipids in archaeological pottery from Qasr Ibrim, Egyptian Nubia. Proceedings Biological Sciences / The Royal So-ciety London B, Vol. 268, 593-597.Copley, M. S., Berstan, R., Straker, V., Payne, S., Evershed R. P. (2005a) Dairying in Antiquity. II. Evidence from Ab-sorbed Lipid Residues Dating to the British Bronze Age. Journal of Archaeological Science, Vol. 32, 505-521.Copley, M. S., Berstan, R., Dudd, S. N., Straker, V., Payne, S., Evershed R. P. (2005b) Dairying in antiquity. I. Evidence from Absorbed Lipid Residues Dating to the British Iron Age. Journal of Archaeological Science, Vol. 32, 485-503.Copley, M. S., Berstan, R, Mukherjee, A. J., Dudd, S. N., Straker, V., Payne, S., Evershed R. P. (2005c) Dairying in Antiqui-ty. III. Evidence from Absorbed Lipid Residues Dating to the British Neolithic. Journal of Archaeological Science, Vol. 32, 523-546.Crane, E. 1983. The Archaeology of Beekeeping. Cornell University Press, Ithaca. New York.Dey, P. M. and Harborne, J. M. (eds). (1997) Plant biochemistry, San Diego, London: Academic Press.Dudd, S. N. and Evershed, R. P. (1998) Direct demonstration of milk as an element of archaeological economies. Science, Vol. 282, 1478-1480.Dudd, S. N., Evershed, R. P., Gibson, A. M. (1999) Evidence for Varying Patterns of Exploitation of Animal Products in Different Prehistoric Pottery Traditions Based on Lipids Preserved in Surface and Absorbed Residues. Journal of Archaeological Science, Vol. 26, 1473-1482.Eglinton, G. and Logan, G. A. (1991) Molecular Preservation. Philosophical Transactions of the Royal Society of London. Se-ries B, Vol. 333, 315-328.Evans, K. and Heron, C. (1993) Glue, disinfectant and chewing gum: natural products chemistry in archaeology. Chemis-try and Industry, Vol. 12, 446-449.Evershed, R. P. (1993) Biomolecular Archaeology and Lipids. World Archaeology, Vol. 25, No 1, 74-93.Evershed, R. P. (2008) Organic Residues Analysis in Archaeology: The Archaeological Biomarker Revolution. Archaeome-try, Vol. 50, No 6, 895-924.Evershed, R. P., Charters, S., Quye, A. (1995a) Interpreting Lipid Residues in Archaeological Ceramics: Preliminary Re-sults from Laboratory Simulations of Vessel Use and Burial. Materials Research Society Symposium Proceedings, Vol. 352, 85-95.Evershed, R. P., Stott, A. W., Raven, A., Dudd, S. N., Charters, S., Leyden, A. (1995b) Formation of long-chain ketones in ancient pottery vessels by pyrolysis of acyl lipids. Tetrahedron Letters, Vol. 36, No 48, 8875–8878.Evershed, R. P., Vaughan, S. J., Dudd, S. N., Soles, J. S. 1997. Fuel for Thought? Beeswax in Lamps and Conical Cups from Late Minoan Crete. Antiquity, Vol. 71, No 274, 979-985.Evershed, R. P., Dudd, S. N., Charters, S., Mottram, H., Stott, A. W., Raven, A., Van Bergen, P. F., Bland, H. A. (1999) Lipids as Carriers of Anthropogenic Signals from Prehistory. Philosophical Transactions of the Royal Society Lon-don B, Vol. 354, 19-31.Evershed, R. P., Dudd, S. N., Lockheart, M. J., Jim, S. (2001) Lipids in archaeology. In Handbook of Archaeological Sciences, D. R. Brothwell and A. M. Pollard (eds.), Wiley, Chichester, pp. 331-349.Evershed, R. P., Dudd, S. N., Anderson-Stojanovic, V. R., Gebhard, E. R. (2003) New Evidence for the Use of Combed Ware Pottery Vessels as Beehives in Ancient Greece. Journal of Archaeological Science, Vol. 30, 1-12.Feng, J., Hu, M., Chan, C. K., Lau, P. S., Fang, M., He, L. and Tang, X. (2006) A comparative study of the organic matter in PM2.5 from three Chinese megacities in three different climatic zones. Atmospheric Environment, Vol. 40, 3983-3994.Feng, J., Chan, C. K., Fang, M., Hu, M., He, L. and Tang, X. (2005) Impact of meteorology and energy structure on solvent extractable organic compounds of PM2.5 in Beijing, China. Chemosphere, Vol. 61, 623-632.Garnier, N., Cren-Olivé C., Rolando, C., Regert, M. (2002) Characterization of Archaeological Beeswax by Electron Ioni-zation and Elctrospray Ionization Mass Spectrometry. Analytical Chemistry, Vol. 74, 4868-4877.Giorgi, G., Salvini, L., Pecci, A. (2010) The meals in a Tuscan building yard during the Middle Age. Characterization of organic residues in ceramic potsherds. Journal of Archaeological Science, Vol. 37, 1453-1457.Gregg, M. W. Banning, E. B., Gibbs, K. and Slater, G. F. (2009) Subsistence practices and pottery use in Neolithic Jordan: molecular and isotopic evidence. Journal of Archaeological Science, Vol. 36, 937-946.Gunstone, F. D., Harwood, J. L. and Dijkstra A. J. (eds). (2007) The Lipid Handbook. 3rd edition. CRC Press, Boca Raton.Hawkins, R. K. (2013) How Israel Became a People. Abingdon Press, Nashville.Heron, C., Evershed, R. P., Goad, L. J. (1991) Effects of Migration of Soil Lipids on Organic Residues Associated with Buried Potsherds. Journal of Archaeological Science, Vol. 18, 641-59.Heron, C., Nemcek, N., Bonfield K. M., Dixon D., Ottaway, B. S. (1994) The Chemistry of Neolithic Beeswax. Naturwis-senschaften, Vol. 81, 266-269.Herr, L. G. (2001) The history of the collard rim pithos at Tell el-Umeiry, Jordan. In Studies in the Archaeology of Israel and Neighboring Lands in Memory of Douglas L. Esse, S. R. Wolff (ed.), The Oriental Institute of the University of Chicago, Studies in Ancient Oriental Civilization, No. 59, Chicago, Illinois, pp. 237-350.Humphrey, J. W., Oleson, J. P., and Sherwood, A. N. (1998) Greek and Roman Technology: A Sourcebook 137. Routledge, London.Hübner, U. (1992) Die Ammoniter, Untersuchungen zur Geschichte, Kulture, und Relegion eines transjordanischen Volkes im 1. Jarhtausend v. Chr. Harrasowitz Verlag, Wiesbaden, Germany.Ibrahim, M. M. 1978. The collared-rim jar of the Early Iron Age. In Archaeology in the Levant, R. Moorey and P. Parr (eds). Warminster: Aris and Phillips. pp. 117-124.Isaksson, S. and Hallgren, F. (2012) Lipid residue analyses of Early Neolithic funnel-beaker pottery from Skogsmossen, eastern Central Sweden, and the earliest evidence of dairying in Sweden. Journal of Archaeological Science, Vol. 39, 3600-3609.Killebrew, A. E. (2001) The collared pithos in context: A typological, technological, and functional reassessment. In Stud-ies in the archaeology of Israel and neighboring lands in memory of Douglas L. Esse, S. R. Wolff (ed.), The Oriental In-stitute of the University of Chicago, Studies in Ancient Oriental Civilization, No. 59, Chicago, Illinois, pp. 377-398.Killops, S. D. and Killops, V. J. (1993) An introduction to organic geochemistry, Longman Scientific and Technical, New York.Kimpe, K., Jacobs, P. A., Waelkens, M. (2002) Mass Spectrometric Methods Prove the Use of Beeswax and Ruminant Fat in Late Roman Cooking Pots. Journal of Chromatography A, Vol. 968, 151-160.Kimpe, K., Drybooms, C., Schrevens, E., Jacobs, P. A., Degeest, R. and Waelkens, M. (2004) Assessing the relationship between form and use of different kinds of pottery from the archaeological site Sagalassos (southwest Turkey) with lipid analysis. Journal of Archaeological Science, Vol. 31, No 11, 1503-1510.Knappett, C., Kilikoglou, V., Steele, V., Stern, B. (2005) The circulation and consumption of Red Lustrous Wheel-made ware: petrographic, chemical and residue analysis. Anatolian Studies, Vol. 55, 25-59.Kolattukudy, P. E. (1976) Chemistry and biochemistry of natural waxes, Elsevier, Amsterdam/ Kurzweil, A. and Todten-haupt, D., 1990, Teer aus Holz, Berlin, Museumsdorf Düppel.Lattuati-Derieux. A., Egasse, C., Regert, M., Chung, Y., Lavédrine, B. (2009) Case Study: Characterization and Degrada-tion Pathways of Ancient Korean Waxed Papers. Journal of Cultural Heritage, Vol. 10, 422-427.Logan, G. A., Fredericks, D. J., Smith. C. and Heggie, D. T. (2001) Sources of organic matter in Wallis Lake. AGSO Re-search Newsletter, Vol. 34, 15-20.Mayyas, A. S., Stern, B., Coningham, R., Fazeli, H. and Gillmore, G. (2012) Beeswax preserved in a Late Chalcolithic bev-elled rim bowl from the Tehran Plain, Iran. The journal of the British Institute of Persian Studies, Vol. 50, 13-25.Mayyas, A., Douglas, K., Hoffmann, T., Thorenz, U., Bany Yaseen, I., and El-Khalili, M. (2013) Organic residues pre-served in archaeological ceramics from the Early Bronze Age site of Khirbet Al-batrawy in north-central Jor-dan. Mediterranean Archaeology and Archaeometry, Vol. 13, No 2, 189-206.Mazar, A., Panitz-Cohen, N. (2007) It is the Land of Honey: Beekeeping at Tel Rehov. Near Eastern Archaeology, Vol. 70, No 4, 202-219.Mazar, A., Namdar, D., Panitz-Cohen, N., Neumann, R., Weiner, S. (2008) The Iron Age Beehives at Tel Rehov in the Jordan Valley: Archaeological and Analytical Aspects. Antiquity, Vol. 82, 629-639.McGovern, P. E., Zhang, J., Tang, J., Zhang, Z., Hall, G. R., Moreau, R. A., Alberto Nuňez, A., Eric D. Butrym,E. D., Rich-ards, M. P., Wang, C., Cheng, G., Zhao, Z. and Wang, C. (2004) Fermented beverages of pre- and proto-historic China. The National Academy of Sciences of the USA (PNAS), Vol. 101, No 51, 17593-17598.Mills, J. S., White, R. (eds.). (1994) Organic Chemistry of Museum Objects, 2nd edition. London, Butterworths.Mottram, H. R., Dudd, S. N., Lawrence, G. J., Stott, A. W., Evershed, R. P. (1999) New chromatographic, mass spectro-metric and stable isotope approaches to the classification of degraded animal fats preserved in archaeological pottery. Journal of Chromatography A, Vol. 833, 209-221.Namdar, D., Neumann, R., Goren, Y., Weiner, S. (2009) The Contents of Unusual Cone-Shaped Vessels (Cornets) from the Chalcolithic of the Southern Levant. Journal of Archaeological Science, Vol. 36, 629-636.Needham, S., Evans, J. (1987) Honey and Dripping: Neolithic Food Residues from Runnymede Bridge. Oxford Journal of Archaeology, Vol. 6, No 1, 21-28.Panagiotakopulu, E., Buckland, P. C., Day, P. M. (1995) Natural Insecticides and Insect Repellents in Antiquity: A Re-view of the Evidence. Journal of Archaeological Science, Vol. 22, 705-710.Parras, D. J., Sánchez, A., Ramos, N., Ariza, M. O. R., Tuñón, J. A. (2011) Identification of fats and beeswax in ceramic vessels of tomb 121 of Castellón Alto (Galera, Granada). Coalition, Vol. 22, 7-13.Raban, A. (2001) Standardized collared-rim pithoi and short–lived settlements. In Studies in the Archaeology of Israel and Neighboring Lands in Memory of Douglas L. Esse, S. R. Wolff (ed.), The Oriental Institute of the University of Chicago, Studies in Ancient Oriental Civilization, No. 59, Chicago, Illinois, pp. 493-518.Reber, E. A. and Evershed, R. P. (2004a) How did Mississippians prepare maize? The application of compound-specific carbon isotope analysis to absorbed pottery residues from several Mississippi valley sites. Archaeometry, Vol. 46, No 1, 19-33.Reber, E. A. and Evershed, R. P. (2004b) Identification of maize in absorbed organic residues: A cautionary tale. Journal of Archaeological Science, Vol. 31, 399-410.Regert, M. (2004) Investigating the History of Prehistoric Glues by Gas Chromatography-Mass Spectrometry. Journal of Separation Science, Vol. 27, 244-254.Regert, M., Bland, H. A., Dudd, S. N., van Bergen, P. F. and Evershed, R. P. (1998) Free and bound fatty acid oxidation products in archaeological ceramic vessels. Proceedings of the Royal Society of London B, Vol. 265, 2027-2032.Regert, M., Colinart, S., Degrand L., Decavallas, O. (2001) Chemical Alteration and Use of Beeswax through Time: Accel-erated Ageing Tests and Analysis of Archaeological Samples from Various Environmental Contexts. Archae-ometry, Vol. 43, No 4, 549-569.Regert, M., Vacher, S., Moulherat, C., Decavallas, O. (2003a) Adhesive Production and Pottery Function During the Iron Age at the Site of Grand Aunay (Sarthe, France). Archaeometry, Vol. 45, No 1, 101-120.Regert, M., Garnier, N., Decavallas, O., Cren-Olivé, C., Rolando, C. (2003b) Structural Characterization of Lipid Constit-uents from Natural Substances Preserved in Archaeological Environments. Measurement Science and Technolo-gy, Vol. 14, 1620-1630.Regert, M., Langlois, J., Colinart, S. (2005) Characterisation of Wax Works of Art by Gas Chromatographic Procedures. Journal of Chromatography A, Vol. 1091, 124-136.Ribechini, E., Orsini, S., Silvano, F. and Colombini, M. P. (2009) Py-GC/MS, GC/MS and FTIR investigations on LATE Roman-Egyptian adhesives from opus sectile: New insights into ancient recipes and technologies. Analytica Chimica Acta, Vol. 638, 79-87.Rogge, W. F., Medeiros, P. M. and Simoneit, B. R. T. (2006) Organic marker compounds for surface soil and fugitive dust from open lot dairies and cattle feedlots. Atmospheric Environment, Vol. 40, 27–49.Shimoyama, A., Kisu, N., Harada, K., Wakita, S., Tsuneki, A. and Iwasaki, T. (1995) Fatty acid analysis of archaeological pottery vessels excavated in Tell Matsuma, Syria. Bulletin of the Chemical Society of Japan, Vol. 68, 1565-1568.Spangenberg, J. E., Jacomet, S. and Schibler, J. (2006) Chemical analyses of organic residues in archaeological pottery from Arbon Bleiche 3, Switzerland evidence for dairying in the late Neolithic. Journal of Archaeological Science, Vol. 33, 1-13.Stern, B., Heron, C., Corr, L. Serpico, M. and Bourriau, J. (2003) Compositional variations in aged and heated pistacia resin found in late Bronze Age Canaanite amphorae and bowls from Amarna, Egypt. Archaeometry, Vol. 45, No 3, 457-469.Van Bergen, P. F., Peakman, T. M., Leigh-Firbank, E. C., Evershed, R. P. (1997) Chemical Evidence for Archaeological Frankincense: Boswellic Acids and Their Derivatives in Solvent Soluble and Insoluble Fractions of Resin-Like Materials. Tetrahedron Letters, Vol. 38, No 48, 8409-8412.Van Bergen, P. F., Bergen, A., Nott, C. J., Bull, I. D., Poulton, R. P. and Evershed, R. P. (1998) Organic geochemical studies of soils from the Rothamsted classical experiments-IV. Preliminary results from a study of the effect of soil pH on organic matter decay. Organic Geochemistry, Vol. 29, No 5-7, 1779-1795.