First results on thermally induced porosity in chlorite cooking vessels from Merv (Turkmenistan) and implications for the formation and preservation of archaeological lipid residues

Excavations at the ancient city of Merv in Turkmenistan have yielded a significant assemblage of ceramic and stone vessel fragments from contexts dating to the Sasanian and medieval periods (5th–13th centuries AD). Many of the vessel fragments are encrusted with apparent food residue deposits offering scope for organic residue analysis and the potential to compare the use of these two very different vessel types. To enable meaningful comparison we sought to establish whether the vessel stone (a talc-chlorite schist) can absorb and preserve organic residues indicative of past use. This paper reports the first investigation to address this question using standard methods for archaeological residue analysis coupled with study of the properties of the schist fabric and basic absorption experiments. The results demonstrate that heating during cooking, even at relatively low temperatures, modifies the stone microstructure by increasing its porosity. These pores enhance the absorption capacity of the schist fabric such that chlorite cooking pots can absorb and preserve sufficient organic residue to reflect the original processing of foodstuffs, as has been previously demonstrated for ceramic fabrics. Comparison of pore capacity, archaeological residue yield and experimental absorption indicates the significance of pore-size distribution for the relative retention and preservation of organic residues in these fabrics. The results of this study indicate that a wider range of archaeological material may be suitable for absorbed residue analysis than has previously been recognised. The findings also challenge previous assumptions concerning the relationship between the properties of chlorite vessels and their mode of use in Central Asia and Near East in antiquity.     

Metallurgical ceramics from Mayapán,Yucatán,Mexico

Recent excavations at the Postclassic (AD 1050–1440) Maya site of Mayapán, Mexico, have uncovered a variety of metal objects, metal production debris, and ceramic objects that appear to be linked to metallurgical activities at the site. Our present study investigates a corpus of small ceramic objects to determine if these objects was used in metallurgical processes such as lost-wax casting. A variety of analytical techniques was utilized, including x-ray fluorescence, electron probe, petrography, and reflected light microscopy. Metal residues were detected on the surfaces of several objects, and copper prills were identified within the ceramic fabric, suggesting that the ceramics were exposed to liquid metal during remelting and/or casting events. A comparison of the microstructures of these metallurgical ceramics to typical ceramics from Mayapán demonstrates that the fabrics are very different, and suggests that the metallurgical ceramics were specifically engineered to function in the high temperature environment required for metallurgy. The distribution of metal and metallurgical ceramics across the site of Mayapán suggests that metal production activities may have been more widely distributed and practiced than earlier thought.     

Teotihuacan pottery as evidence for subsistence practices involving maguey sap

As in most other pre-industrial cities, urban life at Teotihuacan was closely intertwined with ceramic technology, perhaps nowhere more so than in the realm of foodways. Here, we use two kinds of information derived from ancient pottery—ceramic residues and intra-site sherd distribution patterns—to shed new light on the city’s subsistence economy. We concentrate in particular on the amphora, a type of vessel that may have been used to contain aguamiel and pulque, liquid foodstuffs made of maguey sap. Distributional data distilled from surface collections of the Teotihuacan Mapping Project are informative about patterned variation in the use of these pots at the scale of the entire city. More focused analyses are aimed at chemical characterization of organic residues preserved in ceramic sherds recovered from recent excavations. Part of a broader project aimed at identifying both animal and plant remains, the results of the residue analysis provide the first direct identification of pulque remains in Teotihuacan pottery.     

A MULTI‐ANALYTICAL APPROACH FOR THE CHARACTERIZATION OF COMMODITIES IN A CERAMIC JAR FROM ANTINOE (EGYPT)*

This paper describes a multi‐analytical chemical study performed on the original, almost totally conserved, content of a small ceramic jar from the Antinoe archaeological site (fifth to seventh centuries ad, Roman Egypt) and now belonging to the archaeological collection of the Istituto Papirologico ‘Girolamo Vitelli’ (Florence, Italy). Scanning electron microscopy with an energy‐dispersive X‐ray spectrometer (SEM–EDX), Fourier transformed infrared spectroscopy (FTIR) and X‐ray diffraction (XRD) were all used to characterize the inorganic components of the archaeological material. The organic substances were analysed using FTIR, direct exposure mass spectrometry (DE–MS) and gas chromatography – mass spectrometry (GC–MS). The inorganic component essentially consisted of halite (NaCl). Among the NaCl crystals, lamellar elements were identified. They were chemically characterized by carbonato‐apatite and showed a concentric morphology typical of the scales of small fish. The most prevalent organic constituents of the sample were monocarboxylic acids, α,ω‐dicarboxylic acids, and cholesterol and its oxidation products. The organic material composition was consistent with the occurrence of lipids of animal origin. In addition, diterpenes related to pine pitch were also identified. The overall results suggest that the material recovered in the small ceramic jar found in Antinoe is a residue of fish‐based pickles such as garum, muria, allex and liquamen, which were commonly used in Roman times.     

Adhesive Production and Pottery Function During the Iron Age at the Site of Grand Aunay (Sarthe,France)*

A combination of elemental, functional and molecular analyses performed on amorphous organic residues dating from the Iron Age was developed in order to identify these remains and to understand their relationship with ceramic vessels in which some of them were found. These analyses made it possible to distinguish between ceramic vessels used for the production or storage of adhesive materials, mainly birch bark tar, and those dedicated to the preparation of culinary commodities, which contained animal fats. The organization of the production of adhesives is described and the addition of beeswax to birch bark tar is reported for the first time. The use of birch bark tar for coating ceramic vessels is also discussed.     

Analysis of adhering organic residues of two “coupes-à-socles” from the Neolithic funerary site “La Hougue Bie” in Jersey: evidences of birch bark tar utilisation

The “coupes-à-socle” (footed cups) are ceramics which can be found in domestic Neolithic contexts in Brittany (Castellic, Auzay-Sandun), but more generally in non-domestic areas. Their ceremonial function has often been evoked, in particular as a perfume burner. The analysis by GC and GC/MS of two samples from the “Hougue Bie” (Jersey) passage graves showed the presence of vegetable fatty acids, degraded n-alkanes and terpenoïds, biomarkers of birch bark tar. The presence of such substances could be explained either by the use of the “coupes-à-socle” for burning birch bark tar as an odoriferous product or their use as an everyday vessel for heating and increasing tar plasticity. However, the limited occurrence of this type of ceramic in habitat sites supports the former utilisation. This first report of the presence of birch bark tar in “coupes-à-socle” thus suggests use of this tar as an odoriferous product, in addition to its numerous, previously recognised, more technical uses.     

Fuel For Lamps: Organic Residues Preserved in Iron Age Lamps Excavated at the Site of Sahab in Jordan

Five Iron Age ceramic lamps from a tomb at the site of Sahab in the south‐eastern part of central Jordan were analysed using gas chromatography – mass spectrometry (GC–MS). The results of this study provide data on the type of fuel used in three of these lamps. The study proposes that animal fat, possibly of ruminant origin, was used in three Early Iron Age II lamps. The material used in the other two Iron Age I lamps could not be determined due to the absence of diagnostic biomarkers. The data obtained from the lamps can be put in conjunction with the archaeological evidence on the availability of domestic animals and, most probably, use of their products at the site of Sahab during the Iron Age.     

A COMPARISON OF METHODS FOR ESTABLISHING FATTY ACID CONCENTRATION GRADIENTS ACROSS POTSHERDS: A CASE STUDY USING LATE BRONZE AGE CANAANITE AMPHORAE*

Canaanite amphorae fragments in fabrics believed to be associated with the bulk transport of vegetable oils from the fourteenth‐century BC site of Amarna, Egypt, have been examined. A comparison is made between solvent extraction, saponification and the use of TMTFTH (m‐trifluoromethylphenyl)trimethylammomum hydroxide, used here for the combined extraction and derivatization of ceramic‐absorbed organic residues. Extracts were studied using gas chromatography and gas chromatography‐mass spectrometry. The extraction of fatty acids from small ceramic samples has established concentration gradients of absorbed organic matter from the inner to the outer surfaces of the sherds.     

Combining residue analysis of floors and ceramics for the study of activity areas at the Garum Shop at Pompeii

In this paper, we propose the application—for the first time in the Mediterranean area—of the combination of the study of chemical residues in floors and ceramics, with the aim of providing information about the activities carried out in archeological buildings. We chose the Garum Shop at Pompeii to test the method. In fact, due to the peculiarity of this archeological context, it provided an ideal case in which the activities performed are in part known, and the ceramic vessels recovered are still in situ. Floor samples were studied by means of spot tests developed in Mexico aimed at identifying the presence of phosphates, fatty acids, and protein residues, while the organic residues preserved in the ceramic matrix of amphorae, dolia, and other ceramic vessels were studied by gas chromatography coupled with mass spectrometry. Moreover, we integrated the data obtained with specific studies directed at better identifying the solid residues found inside two of the amphorae studied: botanical studies of fruit stones recovered in a Dressel 20 amphora and the characterization of the lime preserved in an African amphora. The research allowed for the identification of the traces of some of the activities performed, such as cooking and producing garum in the floors of the building, and the use and re-use of amphorae and dolia before the Vesuvian eruption.     

Identifying wine markers in ceramics and plasters using gas chromatography–mass spectrometry. Experimental and archaeological materials

The identification of the organic residues preserved in archaeological materials yields good insights into understanding food production, trade and consumption. Wine is one of the most important beverages produced, traded and consumed in the Mediterranean area. Consequently, it is important to identify its presence in ancient materials. Nevertheless, the identification of wine markers is still an object of discussion. We present here the results obtained from analysing different materials using gas chromatography/mass spectrometry (GC/MS), which allowed for the identification of tartaric acid and other markers of wine. The method was first tested on experimental and traditional materials that have been used until recently to store and/or produce wine and was then used for investigating archaeological materials. The experiments also involved the degradation of wine through cooking, drastic heating and burial for seven years. The results from the analysis of ceramic and plaster materials are discussed.     

EVIDENCE FOR THE MIXING OF FATS AND WAXES IN ARCHAEOLOGICAL CERAMICS

Lipid residues from two Late Saxon/early medieval ceramic vessels recovered from excavations at West Cotton, Raunds, Northamptonshire, U.K., have been investigated by high-temperature gas chromatography (GC) and GC/mass spectrometry (GC/MS). The solvent extracts of sherds sampled from different points on each vessel (i.e., base, body and rim) were analysed quantitatively and qualitatively and compounds were identified which were characteristic of beeswax and animal fat. Furthermore, by determining the sites of accumulation of the specific lipid types and their concentrations in different parts of the vessels it can be inferred that the beeswax was added to the vessels prior to the addition of the fat. It was concluded that the two vessels performed different functions in antiquity.     

Determining Olmec maize use through bulk stable carbon isotope analysis

Bulk stable carbon isotope analysis on absorbed organic residues in ceramics can be an effective method for discerning patterns of maize use when the ceramics come from relatively uniform archaeological contexts. The bulk stable carbon isotope method is faster and less costly than the more commonly used compound-specific stable carbon isotope analysis. Moreover, the bulk stable carbon isotope method can determine the presence of C4 plant carbon in samples in which organic compounds have degraded. Bulk stable carbon isotope analysis was used to discern patterns of maize (Zea mays mays) use among a sample of 24 ceramic sherds from an Early Franco Period feasting deposit (ca. cal 650 B.C.) at the Olmec site of San Andrés, La Venta, Tabasco, Mexico. A comparison of the δ 13C results of different categories of ceramics showed that proportionally more maize was used in luxury beverage service wares than in utilitarian vessels, suggesting that maize-based beverages were prominent in this probable elite feasting episode.     

Tetrahedron baked-clay objects from an early woodland context at the Jaketown site,Mississippi

Excavations undertaken in 1951 at the Jaketown site revealed a dense deposit of fragmented and intact pyramid-shaped baked-clay objects (BCOs) at the base of Mound A. This deposit was associated with the site’s Early Woodland component. Recent fieldwork at Jaketown also encountered the same tetrahedron deposit and identified an additional and distinct pit feature filled with the objects. In this article, we present the results of analyses that examine the production, composition, chronology, and function of these enigmatic baked-clay artifacts. Following a hiatus associated with massive flooding in the Mississippi Valley ca. 3200–2850 cal B.P., Jaketown was re-occupied by people who shared ceramic affinities with groups to the south and to the east and, who like many contemporaries, used BCOs as a part of their cooking technology. The tetrahedron deposit represents one of the earliest dated Tchula contexts at ca. 2600 cal B.P., and was used over a short time for a social purpose that brought populations together for food consumption as a means of encouraging cooperation.     

Ceramic form and function in the Neolithic Gulf. A view from Bahra 1

This paper discusses the possible functions of ceramic vessels in the Neolithic Gulf, based on new data from the Ubaid-related settlement of Bahra 1 (Kuwait). Two pottery groups identified at the site—Ubaid Ware and Coarse Red Ware—are found in great numbers and variety of forms which provides grounds for a reconsideration of the role of pottery vessels in the societies of the Gulf. Analysis of this material reveals a more varied function of pottery vessels compared to that suggested in earlier studies. It was also possible to define the function of certain pottery vessels in more detail, both in their economic and social context.     

Lake levels,mobility and lithic raw material selection and reduction strategies: A Great Lakes case study

Abstract

It has recently been proposed that lowered lake levels after 4250 BP broadened opportunities for mobility and interaction patterns among hunter-gatherer populations in the Saginaw drainage and in Michigan more broadly (; ). Here, data are presented on chipped stone reduction strategies as reflected in two site assemblages in Bay City, Michigan (20BY28, 20BY387) that bridge this key point in time. The earliest Late Archaic components of these sites, occupied during the higher than modern post Nipissing recession ca. 3200 BP, are typified by on-site reduction of local cherts, often utilising a bipolar reduction strategy. Subsequent uses of the area largely shifted to lower elevations. The more recent site components contain both more diverse projectile styles, many of which can be linked with Ontario types, and higher occurrences of non-local raw materials, specifically Onondaga chert apparently arriving at the site as preforms. The last use of these sites occurred during the Late Woodland, also during lower water levels approaching modern, and reflecting the highest use of Onondaga chert. We suggest that these changes resulted from shifting mobility and exchange patterns, facilitated in part by lowered post Nipissing water levels.     

The contents of unusual cone-shaped vessels (cornets) from the Chalcolithic of the southern Levant

Cornets are cone-shaped ceramic vessels, characteristic of the Chalcolithic period (ca. 4700–3700 BC) in Israel and Jordan. Their contents and use are unknown. Gas chromatography with flame ionization and mass-selective detection, showed that extracts of cornets from five different sites with different related activities (domestic, habitation cave and a cultic complex) all contain the same assemblage of mainly n-alkanes adsorbed within their walls. This assemblage differs from those found in other types of ceramic vessels from the same sites, as well as from the residues found within the associated sediments. The assemblage of odd and even-numbered n-alkanes found in the cornets is almost identical to that found in the residues of beeswax heated on modern ceramic fragments, as well as in a beehive from the Iron Age IIA strata at Tel Rehov, Israel. Thus the cornets are most likely to have contained beeswax. The presence of beeswax in the cornets contributes to our understanding of the Chalcolithic period; a time when secondary products such as milk, olive oil and wine are thought to have come into use.     

IDENTIFICATION,PROCESSING AND USE OF RED PIGMENTS (HEMATITE AND CINNABAR) IN THE VALENCIAN EARLY NEOLITHIC (SPAIN)

The results of the first elemental and structural physicochemical analyses (SEM–EDX, TXRF, XRD, FTIR, GC and EDXRF) of Early Neolithic red pigment samples from the region of Valencia confirm one of the earliest uses of cinnabar (HgS) in Spain (5300 to 5000 cal bc ). They also inform on the storage of massive quantities of hematite and the development of specific technologies of hematite‐based paint production and use. The samples were recovered at the three most significant Early Neolithic sites of the Mediterranean coast of Spain: Cova de l'Or (Beniarrés, Alacant), Cova de la Sarsa (Bocairent, Valencia) and Cova Fosca (Vall d'Ebo, Valencia), which together have provided the most important European collection of Cardial ceramic ware (chronoculturally diagnostic of the Early Neolithic).     

Subsistence practices and pottery use in Neolithic Jordan: molecular and isotopic evidence

This paper presents direct evidence of subsistence practices and pottery use at a Late Neolithic site at al-Basatîn, northern Jordan. Measurable concentrations of C_16:0 and C_18:0 were recovered from 8 of 10 archaeological pottery fragments through use of a microwave-assisted silica gel and aminopropyl solvent protocol developed for the isolation and concentration of free fatty acids in marine sediments. Subsequent isotopic analysis of the surviving C_16:0 and C_18:0 saturated fatty acids revealed ∂¹³C ratios consistent with those of adipose fats of ruminant and non-ruminant animals pastured on lands adjacent to the Jordan Valley. The high recovery of diagnostic compounds from the al-Basatîn material is discussed in context of a wider examination of the initial development and use of pottery in the Fertile Crescent, and the emerging debate concerning the efficacy of stable carbon isotope values in characterizing organic residues embedded in pottery fragments recovered from the earliest ceramic horizons in the Middle East and Europe.     

Evidence of early tobacco in Northeastern North America?

While tobacco use was a widespread and important social practice among Native Americans during the Historic Period, the prehistoric origins of the practice are poorly understood. Smoking pipes significantly predate botanical evidence of tobacco in Eastern North America. A promising technique for addressing this problem is gas chromatography/mass spectroscopy (GC/MS) analysis to identify nicotine or related compounds in smoking pipe residues. GC/MS analysis of a smoking pipe dating to approximately 300 B.C. from the Boucher Site, a Middlesex-complex site from Vermont, has produced evidence of nicotine decay products. This is interpreted as evidence for an Early Woodland Period origin for tobacco use in Eastern North America. The cultural and chronological implications of this finding are discussed.     

FTIR AND SOLID‐STATE 13C CP/MAS NMR SPECTROSCOPY OF CHARRED AND NON‐CHARRED SOLID ORGANIC RESIDUES PRESERVED IN ROMAN IRON AGE VESSELS FROM THE NETHERLANDS*

In this study, solid‐state ¹³C magnetic resonance spectroscopy using cross‐polarization combined with high‐powered proton decoupling and magic‐angle sample spinning and Fourier transform infrared spectroscopy using a diamond anvil cell, are employed to give information about the organic functional groups present in charred and non‐charred solid organic residues and to give an insight into the degree of condensation of the chars. Residues were preserved in ceramic vessels recovered from the indigenous settlement of Uitgeest–Groot Dorregeest, dating back to the Roman period. In addition, the application of these solid‐state techniques is used for verification of earlier results obtained in analytical pyrolysis studies and to clarify the relationship between the already thermally degraded charred residues and the controlled heating fragmentation taking place during analytical pyrolysis and direct temperature‐resolved mass spectrometry.