Carl Heron

6
The Analysis of Organic Residues and the Study of Pottery Use

CARL HE R
o N and
RI
c HARD
P. E VE R SH ED
Pottery Use in Archaeology

The durability of ceramics in the archaeological record provides the archaeologist with abundant material for the study of vessel use. The determination of pottery use opens up a wide range of research possibilities in archaeology (Ericson et al. 1972; Hally 1986:267), including (1) the identification of food preparation and consumption patterns in human groups, (2) the types of activities occurring at sites or at particular activity loci within sites, (3) an assessment of the period of introduction of specific oodstuffs, and (4) the identification of shifts in subsistence practices and resource exploitation. Much of the recent interest in pottery use derives from Braun's "pots as tools" approach to pottery studies (Braun 1983), in which vessels are seen as containers designed to satisfy a set of utilitarian roles. Some time ago, Ericson, Read, and Burke (1972) proposed six methods for the determination of pottery use, incorporating ethnography (ethnoarchaeology), the archaeological context, studies of preserved contents, pollen analysis, chemical analysis of residues, and wear patterns (see also Rice 1987:210-11, which includes additional approaches). ln spite of this, Hally (1986) notes that few attempts have been made to identify how pottery vessels from archaeological contexts were used. Supplementary to the apparent lack of effort in this research area, Dunnell and Hunt (1990:330) observe that "inference of ceramic vessel function is usually indirect and fraught with uncertainty." Henrickson (1990) distinguishes between the terms function and use. The former is defined as a broad term encompassing the way
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C. Heron and R. P Evershed
that a pottery type, ware, or entire assemblage fits into the social, economic, and ritual contexts of a cultural system, and the roles pottery is called upon to play within these contexts. Use refers to the specific utilitarian task or tasks a pot is put to. The greatest effort expended in archaeological investigations has been in the determination of intended use by considering the performance-based physical properties of ceramics. The study by Braun (1983) on changes in ceramic technology that may have resulted from shits in diet and food preparation during the Woodland period in North America has been followed by a large number of publications focusing on performance-based relationships (e.g., Bronitsky 1986j Schiffer and Skibo 1987). These studies have focused on a number of parameters, including the size and type of temper additions to clays, the morphology of the finished pot, and various fabric tests. Variability in the properties of the finished product has been interpreted with respect to puta tive use. The majority of studies have been lirnited to one or two vessel types, although Hally (1986) attempted a study of vessel use within an assemblage of sixteenth-century pottery from the Barnett phase in northwestern Georgia, comprising 13 morphologically distinct vessel types exhibiting a range of physical properties. In many cases, the relationship of form and physical properties to actual pottery use may be ambiguous (Woods 1986j Feinman 1989:218), and in some settings, formal variability may have little or nothing to do with performance characteristics (Miller 1985). In recent years, ethnoarchaeological observations of pottery use and disposal have provided a substantial data set for potential archaeological inference (e.g., David and Hennig 1972j DeBoer and Lathrap 1979j Longacre 1981j Deal 1983). Cross-cultural surveys of ethnoarchaeological data that attempt to correla te pottery form with use have also been undertaken (Henrickson and McDonald 1983). AIthough the uncertainty of this approach for actual archaeological testing has been stressed (Bronitsky 1989:5), discussions of pottery use will continue to incorporate elements of modern material culture studies in evaluating past behavior. The principal aim of this paper is to assess the potential of organic chemical analysis in the determination of vessel contents and putative use and to discuss possible areas of future development. Organic residues are included in a number of processes that contribute to the use alteration of pottery in the archaeological context [Skibo 1992).
Organic Residues and Pottery Function
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Use alteratian includes depasits on vessels, visual defarmatians ar wear resulting fram actual use, and absarbed residues.
Chemical Analysis of Organic Residues

The patential for analysis of pattery use through the chemical identificatian af trace quantities of preserved arganic residues was nated some years aga in a review by Renfrew (1977:6)af the principal areas af ceramic analysis. However, Braun (1983:110) has drawn attentian to an imbalance that exists in the scientific study of ceramics, which has focused almost exclusively on the analysis af potsherds for studies of provenance, trade, and manufacturing technology. By contrast, the development and application af analytical methods to the study of organic residues as functional indicators has been relatively slow, although recent developments in analytical chemistry and biochemistry have opened up possibilities for new areas of investigatian in archaealagy. While some recent reviews of pottery use have acknowledged the potential for chemical analysis of arganic residues (e.g., Rice 1990j Henricksan 1990), there has been little critical assessment of many important aspects of analysis, including (1) the selection af samples for study, (2) the variations in the degree of preservatian of different bialogical materials, and (3)the rigorous interpretation of results acquired. Only brief overviews of organic residue analysis in pottery use studies have appeared (e.g., Rabins 1983j Iones 1986:839-47j Heron et al. 1991c).
Definition and Classification of Organic Residues

The term organic residue has been used widely by archaeologists and archaeological scientists to describe a variety af amorphous organic remains found at archaeological sites. By definition, organic residues lack the clearly discernible morphological features that characterize other bialogical materials that survive in the archaealogical record, such as wood, bone, leather, seeds, and pollen. The amorphous nature of organic residues means that their identificatian must rely on chemical analysis. The increasing use of sensi-
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tive analytical chemical and biochemical techniques has greatly increased the scope of organic residue analysis, such that a definition of organic residues must now include absorbed residues. Absorbed residues include the trace amounts of organic components dispersed in a bulk inorganic matrix, and remnant biopolymers, that require the use of immunological ar amplification techniques to reveal their presence in archaeological specimens. Hence, organic residue analysis now covers the study of organic deposits on lithics (Loy 1991), the analysis of tars and pitches (Evershed et al. 1985), bitumens (Connan 1988), soils (Knights et al. 1983; Pepe et al. 1989; Pepe and Dizabo 1990; Bethell et al. 1993), midden deposits (Morgan et al. 1984), coprolites (Lin et al. 1978), and human remains, including DNA [Pbo et al. 1989; Hagelberg et al. 1989) and lipids (Evershed 1990, 1991, 1992; Glaar et al. 1990). Both visible and absorbed organic residues are found in association with pottery vessels and serve as a preliminary means of elassification. Visible Sutjace Residues These are described variously as residues, deposits, or encrustations and can be observed on both the inner and outer walls of vessels. Surface deposits on potsherds may derive from a wide range of sources. Those observed on the outer walls may derive from soot deposited during the heating of the vessel over a fire. Burnt matter on the interior surfaces of sherds may derive from the charring of food or other biological material. Resinous substances, applied during manufacturing processes to reduce the permeability of porous fabrics, may also be observed on potsherds (Rice 1987: 163). Absorbed Residues Absorbed residues result from the contact and subsequent absorption of a vessel's contents into the porous and permeable ceramic wall during vessel use. It is important to draw the distinction between organic residues of food and nonfood origino Food Residues. The common association of pottery vessels with food preparation ar consumption means that the most widely encountered
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arganic residues will be thase derived fram faadstuffs. The passibilities for the absarptian af lipids, such as ails, during starage are clear. During cooking, such as the bailing ar roasting af faad, arganic constituents will be liberated ar mabilized fram faadstuffs, thus facilitating their absarptian in the pat wall. Carbanized visible residues are presumed to arise fram the burning af faadstuffs due to averheating af vessels during cooking. Nonfood Residues. A variety af nanculinary practices can result in the depasitian af arganic residues an ceramics that cannat be related directly to faad preparatian ar cansumptian. These practices include a wide range af "quasi -industrial ar manufacturing" processes (Rice 1987:210) and the applicatian af sealants to permeable fabrics.
Factors Affecting the Preservation and Decay of Organic Residues in Pottery

In a review af faad preservatian from the past, Luck and Galdblith (1977) highlight the paradaxical relatianship between edible organic substances (faadstuffs) and preservatian. For a faadstuff to be a digestible campanent af an individual's diet, it must passess properties that allaw it readily to change physical and chemical states in the gastraintestinal tract. Substances fulfilling these criteria are alsa likely to be susceptible to degradatian by microarganisms active in the burial environment. Organic materials, such as faadstuffs, that will have come inta cantact with pattery vessels during their use are campased af lipids, proteins, carbahydrates, and ather biapalymers. Althaugh the factars affecting the preservatian and decay af arganic matter have been discussed in the geachemical field (Tegelaar 1990; Eglintan and Lagan 1991; Lagan et aI. 1991), there has been relatively little investigatian ar discussian af such factars in relatian to archaealagical material. Hawever, the same general principles apply to the survival af arganic matter in bath fields. Evershed and caauthars (Evershed et al. 1992) have discussed some af the processes relating to the decay and preservatian af lipids in ancient pattery. Lipids are the mast widely studied campaund class surviving in archaealagical ceramics. Lipids, by definitian, are the salvent-extractable campanents af bialagical materials. They have a wide variety af
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C. Heron and R. P Evershed occurring lipids.
Fig. 6.1. Structures oi commonly
o
CH -O-C-R
o
II
CH -o---C-R
II R, R' and R" = alkyl
CH -O-C-R'
II
CH-
I I
R and R'
alkyl
II
O-C-R'
CH 2
O-C-R"
CH - 02
ft 1
+
0-CH CH N(CH )3 2 2 3
0-
Triacylglycerol
Phospholipid
HO
Cholesterol (animal)
HO
Sitosterol (plant) d
Nonacosane
Herxacosanyl
palmitate
functions in living tis sues and so occur widely in nature (Gunstone and Norris 1982). For instance, triglycerides (triacylglycerols: e.g., Fig. 6.la) serve as energy stores and are the major components of plant oils and animal fats, phospholipids (e.g., Fig. 6.1b) are structural components of cell membranes, sterols (e.g., Fig. 6.lc and d) are structural components of cell walls and the precursors of some hormones, and long-chain alkyl compounds (e.g., Fig. 6.1e and f) are common constituents of plant and animal waxes.
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The survival of different components of organic residues over archaeological time depends on their chemical nature and the physicochemical conditions (e.g., pH and redox potential) that prevailed in the immediate (burial) environment. Eglinton and Logan (1991)draw attention to the importance of the entrapment of molecules in enhancing the possibilities for their survival in geological materials. Entrapment of organic compounds in pottery during use includes such processes as the microencapsulation of organics in carbonized surface residues and the absorption of molecules into pores in the ceramic matrix. Entrapment will enhance the survival of organic compounds by inhibiting the access of microorganisms capable of degrading organic matter. The adsorption of molecules on clay surfaces will further limit their availability as substrates for enzymes present in microorganisms. A review of the chemical properties of the major compound classes likely to be found in organic residues associated with ancient pottery is inappropriate here. However, it is important to stress that the likelihood of survival of various biological molecules is largely dependent upon the chemical reactivity of the functional groups present in the molecules that make up the organic residues. Significantly, the likelihood for preservation of proteins, carbohydrates, and nucleic acids is less than that of lipids (Tegelaar 1990; Eglinton and Logan 1991; Logan et al. 1991). However, even lipids contain chernical groups and linkages that will be susceptible to modification or degradation over archaeological time. For example, Rottlnder and Schlichtherle (1983) performed simulation experiments to show the different rates of oxidation of fatty acids possessing different degrees of unsaturation. Oxidation of polyunsaturated fatty acids occurs much more rapidly than oxidation of monounsaturated fatty acids. Related to this work are investigations of the degradation of whole plant and animal fats (den Dooren De Iong 1961; Morgan et al. 1973; Thornton et al. 1970). These studies found that fatty materials decomposing anaerobically under waterlogged conditions are susceptible to hydrolysis, hydration, reduction, and carbon-carbon double bond scission reactions. The formation of lO-hydroxystearic acid and the scrambling of the double bond position in monounsaturated fatty acids present in adipocere suggest that the mechanism of fat degradation in a waterlogged environment is complex (Evershed 1990, 1991, 1992). Fatty materials absorbed in potsherds buried in waterlogged sites would be expected to undergo analogous degradations. The pos-
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C. Heron and R. P Everslied
sibility for the conversion of oleic acid to palmitic acid in waterlogged anaerobic environments (den Dooren De Iong 1961) casts doubt on conclusions drawn from studies using fatty acids as the sole indicators of the nature and origins of fatty remains found in association with buried pottery. The solubility of the various classes of biomolecules will have a significant influence on their persistence in pottery buried in waterlogged environments. The hydrophobic nature of lipids will greatly limit their solubility in groundwater and hence willlimit their loss from potsherds by dissolution and diffusion. Evidence for this has come from investigations of the possible effects of migration of lipids from the burial soils into potsherds (see below). Studies on the composition of lipids preserved in bog body tissues and the surrounding peat bog provi de further indications of the lack of mobility of lipids in groundwater due to their inherent hydrophobicity (Evershed and Connolly 1988). There is currently much less evidence for the preservation of the more polar biopolymeric constituents of biological materials in ancient potsherds. Pyrolysis-mass spectrometry (PY-MS) has provided evidence for the presence of proteins and carbohydrates in charred residues (Oudemans and Boon 1991). However, where these compounds have been released from tissues, for example, by boiling water during cooking, and absorbed into the ceramic fabric, then their subsequent loss by leaching in waterlogged environments is likely to occur. Hydrolysis during aging of polysaccharides and proteins will produce the constituent monosaccharide and amino acids respectively, which on account of their solubility may be lost from potsherds by dissolution and diffusion in waterlogged environments. Conversely, and in contrast to lipids, there is a greater likelihood for polar (water-soluble) substances to migra te into buried pottery during the movement of groundwater. Considerably more work is required to establish the extent of preservation and decay of proteins, carbohydrates, and other biopolymers in buried pottery. Certain nonfood natural materials, e.g., hydrophobic resins and waxes, owing to their high chemical stability or refractory nature, may survive from antiquity in a relatively unchanged state. The chemistry of many such substances has been surveyed (Mills and White 1987). The resistant properties of substances of this type will have been utilized for a variety of practical purposes, including water-
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proofings and adhesives. If pottery vessels were used to colIect, store, ar process such materials, then organic residues indicative of these activities should be readily detected. Many plant and animal waxes, e.g., epicuticular leaf waxes and beeswax respectively, are composed largely of fulIy saturated long-chain alkyl compounds such as hydrocarbons (n-alkanes) and wax esters (TulIoch 1975; Kolattukudy 1976).
Factors Affecting the Contamination of Organic Residues in Pottery

In view of the presence of organic matter in soil, it is surprising that apparently so few investigations have addressed the possibility of migration of organic matter into sherds or vice versa (Condamin et al. 1976; Heron et al. 1991b).The organic matter present in the soil represents the net of all processes, such as the input of plant and animal detritus and microbial synthesis by fungi and bacteria as well as subsequent degradative processes (Braids and Miller 1975) and anthropogenic input (Knights et al. 1983; Bethell et aI. 1993). In a recent study of freshly excavated late Saxon/early medieval sherds (West Cotton, Northamptonshire, U.K.) and adhering burial soil, the differences in the lipid compositions, determined by gas chromatography (cc) and combined gas chromatography/mass spectrometry (CC/MS), led to the conclusion that contamination of preserved lipids in potsherds by soillipids may not be a serious problem (Heron et al. 1991b). Clear quantitative and qualitative differences were found between the lipids absarbed in the sherd and those of the soil adhering directly to the pot surface. This is attributed to the hydrophobic nature of the lipid molecules. However, in some cases, the relationship is less clear, particularly where the yield of pot residue is very low. In other investigations, the analysis of the internal and external portions of sherds have been sampled separately to detect concentration gradients from the inside to the outside of the vessel wall (Condamin et al. 1976). While indications are that the lipids preserved in potsherds are largely unaffected by migration of soil components, the behavior of more polar proteinaceous and carbohydrate constituents is much less clearly understood (see above). Rigorous compara tive studies of the
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pratein and carbohydrate content of potsherds and adhering soil are required to resolve the questions surraunding their behavior during burial (d. Heran et al. 1991b for lipids). The collection of soil samples for analysis along with pottery samples is strangly recommended. Other samples to be included in a validation study could include kiln wasters or handles not expected to have come into contact with the contents of the vesseI. Whether handles retain trace amounts of lipid residues or are "blanks" remains to be addressed. According to Gabasio and coauthors (Gabasio et al. 1986), organic matter in potsherds can arise not only thraugh use but also fram naturally occurring organic matter in the clays, organic temper additions, or kiln fuel. Although carbonized fragments of biological matter, incorporated into the original clay, are commonly found in potsherds, it is unlikely that organic compounds survive the firing pracess, except where very low temperatures were attained during firing [Iohnson et aI. 1988). Since many earthenwares were fired at low temperatures for only short durations, specific firing experiments could be designed to assess the survival of organic matter occurring naturally in clays fram which the vessels are manufactured.
Organic Residues and Pottery Use

A large number of processes carried out in pottery vessels, notably the repeated heating of animal and plant praducts, willleave chemical evidence of this activity. In addition to the preparation, storage, and cooking of food, many other activities will also have required the use of pottery vessels. These activities include brewing, tanning, dairying, dyeing, fulling, textile washing, and salt preparation. However, other uses, such as the dry storage of grain or seeds, may yield no detectable residue on analysis, unless the residue was accidentally charred to the pot surface. Evidence exists for the preparation and use of dyestuffs in pottery vessels (Biek 1963: 105-12; McGovern and Michel 1984). Natural dyestuffs are also known to have been used to decora te ceramics (Foster and Moran 1989). Earthenware vessels were also used as beehives. Gas chramatographic data from analyses of residues fram suspected beehives found on coarse ware combed kalatboi fram Vara, Greece, dating fram the fourth to third centuries B.C., are consistent
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with the presence of beeswax (Bu'lock 1973).There is also evidence for the distillation of pine tar and birch-bark tar in closed vessels, with one pot being inverted on top of another (Heron et al. 1991a) as well as the use of large vessels as receptacles for the collection of tar from heated wood piles (Leglay 1973:529). Certain vessel uses may be difficult to determine, owing to problems of preservation or retention of diagnostic organic constituents. Determining a previous association with alcoholic beverages poses such a problem since they comprise a dilute solution of organic compounds in water (Haevernick 1967). Remains of such beverages will be more likely in arid environments, following evaporation of the water and alcohoI. Since the compounds of interest are not present in abundance, significant quantities of residue may need to be preserved, as in examples of sealed amphoras from wreck sites (Condamin and Formenti 1976, 1978; Formenti et al. 1979). In some cases, pollen or botanical evidence may be invaluable. Dickson (1978) carried out pollen analysis of a Bronze Age beaker residue from an inhumation burial at Ashgrove, Fife, U.K. Lime or linden (Tilia) and meadowsweet (Filipendula) pollen were found in abundance, suggesting that the contents of the beaker may have been a beverage not unlike mead, flavored with lime honey and meadowsweet. Similarly, Bohncke (1983) undertook pollen analysis of a black greasy material from a Bronze Age food vessel accompanying a burial at Strathallan, Perthshire, U'K. High percentagesof meadowsweet and ceralian pollen suggested either a porridge of cereals or a fermented beverage flavored with meadowsweet flowers or extract. Without doubt, there is much scope for complementary application of pollen analysis and other palaeobotanical information with chemical data.
Postjiiing Treatments
The analysis of organic residues found in pottery containers must take into account a wide range of surface treatments employed to reduce or control the permeability of low-fired ceramics. In addition to prefiring surface treatments such as glazing, burnishing, or the application of a slip, the use of organic substances to seal the interior walls of vessels after firing is also known. Evidence for the use of pine resin, tar, and pitch sealants on Roman amphoras to facilitate the transport of liquids is widespread (Heron and Pollard 1988). Seal-
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C. Heron and R. P. Evershed
ants may also have been applied to other types of vessels used for cooking, storage, serving, and drinking (Shepard 1968:93; Rye 1976: 119; Arnold 1985: 140; Rice 1987: 163-64; Schiffer 1990; Gianno 1990). Schiffer (1990) has demonstrated that pots coated internally with resin possess excellent heating effectiveness [the rate at which the temperature of water is raised when a vessel is placed over a heat source). Some potters apply resinous coatings to the exterior surfaces of vessels (Foster 1956). Ethnographic observations suggest great diversity in modifying the permeability of pottery vessels with organic substances. In addition to the use of resins and waxes, foodstuffs have also been used to seal porous vessel walls prior to use. In Papua New Guinea, pots are sealed by boiling paw-paws, yams, or bananas in them (May and Tuckson 1982:49). Ethnographic records of Thule Eskimo activities indica te that before use, pots were sealed with grease or oil or were lined with stomach pouches or gut (Stimmell and Stromberg 1986). Recognition of postfiring treatments will be more obvious when the substances identified are inedible or would not normally constitute a component of diet, as in the case of a resin. However, if the treatment involves the use of plant and animal products that are foodstuffs in their own right, for example, milk (Cheape 1988: 17) or some other product containing fat, interpretations from chemical analysis will be complicated. One approach to this problem would be to sample a large array of vessels from a single site. If an organic residue diagnostic of a potential sealant occurs with high frequency, then a postfiring treatment might be suspected. Multiple Use of Pottery Containers
There is at present only limited evidence to suggest that organic residue analysis is able to determine multiple use of a single vessel. Mixtures of foodstuffs are clearly evident from the analytical results of some investigations (Evershed et ai. 1991). The problem lies in demonstrating whether this represents a deliberate mixing of food, as in the case of a soup or a stew, or the sequential use of the vessel for preparing different foods. This problem is not easily resolved but is being considered using data from analytical chemistry, ethnoarchaeology, and experimental archaeology in the following investigations: (1) by comparison of the composition of surface deposits with
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residues absorbed in the vessel wall, (2) by cooking and charring experiments using pots fired under similar conditions to those under investigation, and (3) by consideration of ethnoarchaeological data on the types of vessels used for specific or multiple uses. A consideration of use wear may also be appropriate in evaluating multiple use [Skibo 1992). Since cooking pots absorb the taste and smell of the food prepared in them, separate pots may be needed for different foods to avoid tainting (Arnold 1985: 138-39; Fl and Hofer 1988). Some ethnoarchaeological accounts observe that vessels are reused only when they have failed in their primary use, such as if the resin coating has dissipated or if the vessel is cracked [Longacre 1981:63). Although cracked vessels may be repaired to prolong primary use, the pots or even individual sherds may be put to a wide variety of secondary uses (DeBoer and Lathrap 1979: 125, 127). Ethnoarchaeological work by Deal (1983) among the Tzeltal Maya in Mexico indicates that many residues on pottery result from secondary or tertiary uses of vessels and repair practices. The relationship between primary and secondary use merits further consideration, including studies of pottery deposition and disposal. It is likely that the multiple use of pottery vessels cannot be elucidated by organic residue analysis alone. Position of Surface Residues In addition to the identification of the organic residue, the nature and position of the residue on the artifact is of importance in establishing its putative use. The nature and distribution of surface residues on the internal wall may indica te how the food was prepared [Andersen and Malmros 1984; Hastorf and DeNiro 1985), while sooting patterns may suggest how the vessel was heated [Hally 1983; Moorhouse 1986; Skibo 1992). Residues enveloping the rims of vessels may indicate sealing agents used to fix lids or skins across the top of the pot. Documentary sources from the medieval period in Britain indicate the use of different rim adhesives for specific prepsrstive functions (Moorhouse 1986). Vessels are also known to have been repaired using adhesives such as birch-bark tar [Sauter 1967; Binder et al. 1990; Charters et al. 1993) and other resinous substances (DeBoer and Lathrap 1979:127; Gianno 1990).
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Techniques for the Analysis of Organic Residues

Identification of the origin of organic residues relies on matching a unique chemical property of the residue to that of a contemporary natural materiallikely to have been exploited in antiquity. The analysis of organic residues is not a new field of study. Ancient Egyptian Materials and Industries by Alfred Lucas, first published in 1926 and updated until the fourth and final edition appeared in 1962 (with Harris), contains critical discussions on many early results, dating to the late nineteenth century, obtained from studies of materials found at Egyptian and Near Eastern sites. The book provides considerable detail on a wide range of organic substances used in antiquity, supplemented by extensive "wet" chemical tests carried out on substantial finds of organic material preserved in arid locations. The majority of wet chemical tests, such as "spot" tests, and solubility and melting point determinations, require relatively large samples (> 1 mg quantities). Similar work was carried out on pottery and soil samples in Germany during the 1930s (von Stokar 1938). The failure to establish a clear identity of many substances resulted from processing (e.g., heating) in antiquity or aging, with the effect that the chemical properties of the sample were altered compared to contemporary reference material. The application of modern analytical chemical and biochemical techniques allows very detailed assessment of the chemical composition of previously intractable organic residues. Such data are of particular value in determining the nature and origin of residues, as well as establishing the presence of decay products and postdepositional contaminants. Visual Inspection Although not an analytical chemical technique, visual inspection of residues in potsherds is included here since any macroscopic remains are of great value in support of chemical data, particularly in the selection of reference material for comparison. Interest in the detection of dietary constituents preserved in surface deposits, or the pot fabric, has prompted a range of investigations. Andersen and Malmros (1984) conducted microscopic examination of charred deposits found in three pointed-based vessels from the Ertebolle site at Tybrind Vig,
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Denmark, radiocarbon dated to 4400-3200 B.C., and recovered uncharred bones, scales, and fin rays from cod (Gadus morrhua). In some studies, fungal hyphae have been observed (Bush and Zubrow 1986), while in others, workers have reported an absence of morphological remains in large numbers of charred deposits (Hastorf and DeNiro 1985). Elemental Analysis Scanning electron microscopy has been used in the study of visible surface residues. The possibility exists for performing quantitative elemental analysis using instruments that include facilities for energy-dispersive x-ray analysis, although such data would appear to be of limited value for discriminating between different foodstuffs (d. Bush and Zubrow 1986). Following experimental work by Duma (1972), who demonstrated that ceramic fabrics take up phosphorus from aqueous solutions, the detection of elevated concentrations of phosphorus in the ceramic matrix has been proposed as a method of determining whether a vessel contained organic matter (Cackette et al. 1987). In the latter study, the authors compared elemental phosphorus concentrations in an unused ethnographic pot with a cooking vessel and a pot used for boiling water. Using energy-dispersive x-ray fluorescence, they found higher phosphorus concentrations in the pot used for cookng than in the unused vessel or the one used for boiling water. However, Freestone, Meeks, and Middleton (Freestone et al. 1985) reported the ability of pottery to take up phosphorus from the burial matrix by a number of possible yet unspecified mechanisms. Therefore, the possibility exists for high concentrations of phosphorus arising from postdepositional uptake swamping that accumulated during vessel use. Dunnell and Hunt (1990) conclude from their experimental study that, because phosphorus uptake from the soil may take place, inferences based on vessel use are unreliable until the mechanisms and forms of postdepositional enrichment are better understood. Furthermore, phosphorus is present in all plants and animals, and the demonstration of elevated phosphorus levels in vessel walls would provide only a nonspecific indication of use. Stable lsotope Analysis Information concerning the nature of charred plant remains adhering to potsherds has been derived from stable carbon (13C) and nitro-
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gen (1SN) isotope ratios. These measurements enabled residues of C3 and C4 plants and legumes to be differentiated (Hastorf and DeNiro 1985; Morton and Schwarcz 1988; Morton et al. 1991). Hastorf and DeNiro (1985) studied 71 burnt visible residues on jars from the Upper Mantaro Valley in the Central Peruvian Andes. Stable isotope analysis suggested that the jars had been used to cook C3 plants such as tubers and quinoa alone or C4 plants (maize) and C3 plants together, either simultaneously or sequentially. Moreover, their results showed that the vessels had not been used for cooking legumes, either in combination with nonleguminous plants or alone. These conclusions are consistent with modern cooking practices carried out in the same region of the Andes. Problems may occur in the wider application of this technique due to food groups possessing overlapping 1sN and 13Cvalues (Deal 1990:9). lnfrared Spectroscopy Infrared (IR) spectroscopy has been used to investigate visible residues without prior extraction of organic constituents. However, unless substantial quantities of organic constituents are preserved in the deposits, inorganic absorptions due largely to phosphates and carbonates may domina te the spectra (Heron 1989: 123-24). Infrared spectroscopy has also been used to study solvent extracts of both visible residues and sherds (Needham and Evans 1987; Hill and Evans 1989). Infrared spectra may provide a useful "fingerprint," even though residues may comprise a complex mixture of constituents. However, IR absorption bands tend to merge into a series of broad envelopes due to the large number of bond types that result from degradation during vessel use and burial. Infrared spectroscopy has been applied successfully to the identification of aged softwood (probably pine) resins and heated derivatives (Beck et al. 1989), although it is desirable to confirm assignments using GC and GC/ MS (Evershed et al. 1985; Robinson et al. 1987; Heron and Pollard 1988). Although it is possible to "fingerprint" nonfood or natural product residues using IR spectroscopy, the usefulness of the technique is limited for the study of most organic residues because IR spectroscopy lacks the selectivity and sensitivity necessary for the characterization and detection of complex mixtures of organic constituents.
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Nuclear Magnetic Resonance Spectroscopy Nuclear magnetic resanance (NMR) is widely used in natural product chemistry for elucidating the structure af arganic substances. However, NMR has relatively limited application in the study af organic residues because of the small amounts of organic matter available far study. The investigatian of a dark brown liquid remaved fram a glass flask, dated ta the sixth ta faurth century B.C. (Syria), is of relevance here (Beck et aI. 1974). Nuclear magnetic resanance provided evidence for the substance being a degraded oil. Oudemans and Boon [personal cammunicatian) have faund solid-state NMR ta be af value in the analysis of the carbohydrate content af carbonized visible residues. The data are camplementary ta that obtained by pyrolysis-mass spectrometry (Oudemans and Boon 1991). Thin Layer Chromatography Solvent extraction of patsherds and residues yields lipid extracts that can be investigated by a range of chromatagraphic techniques. Thin layer chromatagraphy (TLc) rnethods have been used in investigations of organic residues by, amang athers, Gurfinkel and Franklin (1988) and Rottlander and Schlichtherle (1979). Hawever, as with IR, interpretatians based an TLC are greatly cornplicated by the effects af decay that frequently yield a range of cornpounds af slightly differing structure. Improved selectivity and sensitivity is attainable by use af GC ar high-perfarmance liquid chromatagraphy (HPLC), which are capable of resalving individual molecular species. High-Performance Liquid Chromatography
High-perfarmance liquid chramatagraphy has Iound relatively little use in the study of arganic residues in ceramics. Notable examples include the analysis af lipid residues in a 1,500-year-ald Mediterranean amphora and an oil larnp (Passi et al. 1981). In this study, fatty acids freed fram acyllipids by hydrolysis were analyzed by HPLC as their phenacyl esters. The study shawed that although some acyllipids are preserved in ceramics, great care must be taken ta assess the effects af decay and microbial contamination befare praceeding with interpretation of their arigin. Althaugh HPLC was effective in this
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C. Heron and R. P. Evershed

through
Figure 6.2. Cacao alkaloids from Maya ceramic vessels. identified

HPLc!MS.
Caffeine
Theobromine b
instance, GC is generally preferred to HPLC for the analysis of lipids (d. Evershed et al. 1990j Evershed et al. 1992 for further discussions). A more recent application of HPLC (Hurst et al. 1989j Hall et al. 1990) succeeded in demonstrating the presence of cacao alkaloids, caffeine (Fig. 6.2a) and theobromine (Fig. 6.2b), in three Maya vessels of the Early Classic period. Their findings were consistent with the presence of hieroglyphs on one of the vessels that suggested a use associated with cacao. This investigation demonstrates the usefulness of combining chromatographic techniques "on-line" with mass spectrometry (see below for further discussions). Gas Chtomatogiaphv and Gas Chromatagraphy/ Mass Spectrametry Gas chromatography and gas chromatagraphy/mass spectrometry are the preferred techniques for the analysis af lipid extracts of visible and absorbed residues obtained by solvent extraction [Patrick et al. 1985j Evershed et al. 1990).The possibility of performing nondestructive extractions of organic residues from ceramics has been considered but has yet to be rigorously evaluated (LeCarpentier et al. 1987j Gerhardt et al. 1990).Such an approach is potentially attractive for the study of rare ar valuable artifacts.
265
The value of GClies in its ability to resolve the individual cornponents of the often complex mixture of lipids found in potsherds. Capillary GC is much more readily interfaced with mass spectrometry, thus allowing "on-line" separation and characterization of the individual compounds as they elute from the cc. Liquid chromatography/mass spectrometry (LC/MS) offers similar advantages to the analysis of more polar substances, as discussed above in relation to the study of cacao residues [Hurst et al. 1989). Some notable successes of GCand GC/MSinclude the identification of softwood resin, tar, and pitch of Pinus sp. in Roman transport amphoras. These were characterized through their component diterpenoids (Fig. 6.3a and b, see Robinson et aI. 1987; Heron and Pollard 1988; Beck et al. 1989). The detection of triterpenoids from Pistacia sp. has also confirmed the identity of the resins contained in the Canaanite amphoras from the Late Bronze Age shipwreck at Ulu Burun in southern Turkey [Mills and White 1989). The characterization of triterpenoid compounds, notably betulin (6.3c), found in large quantities in the bark of the birch tree (Betula sp.], has confirmed the widespread use of birch wood and birch-bark tar by prehistoric communities [Binder et al. 1990; Hayek et aI. 1990; Heron et aI. 1991a). Most of the evidence for these materials comes from pottery vessels used to produce and store the derived tar. Tars were als o used to modify the properties of pottery vessels, for example, through the application of a sealant or as an adhesive for repairing [Charters et al. 1993) or applying decorations such as cut-out patterns of birch bark to pots (Vogt 1949). Gas chromatography/mass spectrometry has also been used by Connan (1988) to characterize and source natural bitumen samples associated with a range of artifacts from Mesopotamia, including potsherds. Pyrolysis Methods Characterization of visible residues has been investigated using analytical pyrolysis techniques such as Curie-point pyrolysis mass spectrometry (CUPY-MS) and Curie-point pyrolysis gas chromatography/mass spectrometry (CuPY-GC/MS;see Oudemans and Boon 1991). No sample preparation is required, and analysis can be performed on very small samples (20-30 f.Lg). The analysis of 33 surface deposits observed on distinctive pottery types from a native Roman
266

and triterpenoids idemified through
GC
Figure 6.3. Diterpenoids

GC/MS.
and
CO CH 2 3 Methy! dehydroabietate Retene
Jl
HO
Betulin
settlement at Uitgeest-Groot Dorregeest (Netherlands) allowed pyrolysis "fingerprints" to be obtained. A notable advantage of these pyrolysis techniques lies in their ability to assess the protein, carbohydrate, and lipid content of residues simultaneously in samples, although more specific assignments are difficult. Discriminant analysis of the data suggested several groups of residues of different chemical composition associated with the specific vessel forms.
267
Use af Malecular Markers

The preferred approach to the characterization of organic residues is based on chemotaxonomic and phylogenetic principles. This relies on matching a specific chemical property, generally the presence of a particular compound structure or distribution of compounds, to that of a contemporary plant or animal natural product (reference material). This in itself is not without problems, since individual compounds may be found across a broad range of materials of different origino A knowledge of the plant and animal species likely to have been exploited in antiquity is of value in selecting contemporary materials for compara tive purposes (Deal et al. 1991). Since the published literature details only domesticated species or commercially important wild species, the results of experimental studies and Iaboratory cooking simulations can be incorporated into the database. The development of such databases is an integral component of the organic residue research. Analytical Method An analytical protocol for the study of lipid residues from potsherds has been outlined elsewhere (Evershed et al. 1990)and is not detailed here. Briefly, prior to analysis, organic residues are isolated from the inorganic matrix (a finely ground potsherd or a partially carbonized deposit], by solvent extraction, to provide a totallipid extract. The totallipid extracts are submitted directly to GC with a minimum of sample work-up. Only trimethylsilylation is required to enhance GC properties. Gas chromatography has the potential to separate individual molecular species from what are often complex mixtures, and identification proceeds by comparison with reference compounds. Combined GC/MS provides the essential structural information required for unambiguous identification of each compound. Lipid extracts are commonly analyzed by GC after saponification [alkaline hydrolysis) of the preserved acyllipid components of the residue. However, high-temperature GC and GC/MS allow intact acyl lipids, such as triacylglycerols, diacylglycerols, monoacylglycerols, and wax esters to be analyzed without saponification, thus providing compositional information that would otherwise be lost (Evershed et al. 1990; Evershed 1992).A similar approach has been reported for
268
the use of high-temperature GC for the "fingerprinting" of nonfood natural products (Glastrup 1989). The use of high-temperature GC analysis has demonstrated the survival of acyl lipids, alkyl compounds, and sterols in a large number of potsherds of Bronze Age, Roman, and late Saxon/early medieval periods sampled from the Raunds Area Project (Evershed et aI. 1990; Evershed 1992). Fatty Acids as Biotnatkets Although fatty acid profiles can provide useful information on the origin of residues, their diagnostic potential is limited when considered in isolation. Most fats and oils differ in composition according to the relative proportions of a somewhat narrow range of major fatty acids (Paul and Southgate 1978). Furthermore, specific fats and oils can exhibit marked variability in composition of individual fatty acids. Factors such as soil type, clima te, and method of processing can affect the composition of plant and seed oils, while animal fats may vary in composition as a result of diet and the particular part of the animal from which the fat is derived (Mills and White 1987:26-28). A review of the archaeological literature revealed references to more than 20 different aged fat or oil residues determined by chemical analysis (Heron 1989:88). Unfortunately, it is difficult to know how differentiation between the wide range of possible fats or oils was achieved. It is impossible to assess or compare results with such unsubstantiated statements, many of which do not include data or technical descriptions. Such statements serve no purpose, either for the archaeologist or the residue analyst, and we urge that these be rejected on scientific grounds. Some interpretations are supported by supplementary data such as documentary evidence (Morgan and Titus 1985). The problem of similarities in the composition of particular fats or oils is accentuated in archaeological contexts by oxidative and microbial degradation (den Dooren de Iong 1961; Morgan et aI. 1984; Evershed 1990; Evershed 1992). Without exception the more labile unsaturated fatty acids are depleted in aged samples, resulting in a concomitant increase in the relative proportions of saturated fatty acids (Morgan et aI. 1973). The survival of polyunsaturated fatty acids in sherds, commonly the major constituents of fish and vegetable oils, is rare. However, reports of traces of linoleic acid (C18:2) in ancient human soft tissue remains (Evershed & Connolly 1988; Glaar et aI. 1990) and dry maize seeds from Anasazi sites up to
269
1,700 years old (Priestley et al. 1981)suggests that a degree of survival may be possible under certain preservation conditions. The effects of decay complicate direct comparison of aged lipid residues with tables of contemporary food composition (Paul and Southgate 1978; Rottlnder 1990). Problems of interpretation are exemplified by conversion in anaerobic environments of the unsaturated acyllipids to adipocere, a mixture of predominantly free saturated fatty acids (den Dooren De [ong 1961; Thornton et al. 1970). Although degradation can be retarded due to incompletely understood mechanisms of preservation, assigning residues to specific food sources based solely on fatty acid composition may be unreliable. This includes the so-called palmitic-to-stearic acid ratio and the percentage of saturated fats, since these are often degradation products derived from other acids. A much more realistic approach is the differentiation between general categories of foods such as dairy products (Evershed et al. 1992), fish and marine mammallipids (Patrick et al, 1985; Dea11990), animal fats, and vegetable oils (Heron et al. 1991c) based on more readily distinguishable compositions. Sterols as Biomatkets While is appropriate for sensitive separations of the lipid extracts, GC/MS is generally required to detect the trace amounts of sterol present. Although sterols are mino r constituents (usually less than 1%) of plant and animal products, their structures are diagnostic of the nature of the source foodstuff. The biosynthesis of cholesterol (see Fig. 6.lc) by animals and alkylated sterols (e.g., sitosterol, see Fig. 6.1d) by higher plants enables animal- and plant-derived residues, or a mixture of the two, to be identified (Evershed et al. 1990; Heron et al. 1991c). The susceptibility of sterols to structural alteration as a result of cooking and postburial diagenetic processes has been discussed elsewhere (Evershed et al. 1992). Due to the ubiquitous occurrence of cholesterol in our fingerprints, it is important to stress the potential threat of contaminating sherds through handling.
GC
Other Biomatkets Long-chain alkyl compounds congruent with epicuticular leaf wax components of Biassica vegetables have also been identified in a
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number of potsherds from a medieval hamlet at West Cotton, Northamptonshire, U.K. (Evershed et al. 1991; Evershed et al. 1992). The inference of these findings is that the vessels from which the sherds derived had been used in the boiling of Brassica vegetables, presumably cabbage or possibly turnip leaves. During cooking, the wax would have been mobilized from the leaf surface and become free to migrate into the fabric of the pot wall. Such a method of determining vegetable components in the diet through leaf wax recognition has potentially wide application. This is a finding that perhaps satisfies Dimbleby's (1978:91) claim that "[i]t is not beyond the bounds of possibility that one day the biochemist will enable us to deduce the previous presence of plant material even though all visible trace has gone." This has made it possible for us to propose a new method of recognizing the preparation and likely consumption of vegetables in the past (Evershed et al. 1991).
Current Research and Future Prospects

A justifiable criticism of organic residue investigations stems from the tendency toward the sampling of small numbers of vessels. That is not to say that chemical analysis of an organic residue from a single vessel or a limited number of vessels is to be discouraged where a specific archaeological question might be answered. However, analysis of a single vessel can provi de no means of deducing whether that vessel is typical ar atypical of its type, unless judged against a background knowledge of the general pattern of use. In an effort to address this problem, the potential for a systematic study of a large assemblage of potsherds is being investigated in the laboratory of one of the authors (Evershed). The ceramic samples originate from pottery assemblages from sites excavated as part of the Raunds Area Project (Foard and Pearson 1985; Dix 1986-1987), an extensive multiperiod investigation of settlement, landscape, and environment in an area of 40 square kilometers in the Nene Valley, Northamptonshire, U'K. The ceramic research centers on samples recovered from prehistoric, Roman, and late Saxon/medieval sites. At the time of writing (spring 1992), the research program has been underway for three years. A range of practical aspects of the analysis, sampling, and interpretation of lipid residues found in pottery has
Organic Residues and Pottery Functian
271
been addressed and summarized above in the appropriate sections. Specific paints that have been considered include (1) the development of an analytical protocol for the analysis of absorbed lipids in large numbers of potsherds, (2) the use of GC and GC/MS for the analysis of lipids, (3) the use of biological marker compounds to identify the origins of absorbed Iipids, (4) the detection of sites of accumulation of absorbed lipids in ancient vessels and the application of this to infer use, and (5) the integration of analytical chemical data with typological, petrological, manufacturing, and contextual information with the aim of defining specific or general patterns of vessel use. Ongoing excavation at the site has allowed the implementation, in the field, of specific, project-designed sampling strategies, including handling and storage. Care has been taken not to remove possible surface residues, as well as soil adhering to the sherd, to enable comparative analysis. Storage in paper bags rather than plastic bags removes the problem of plasticizer contamination of samples. All pottery submitted for residue analysis is examined by pottery specialists and given full contextual description. The large number of samples and the selectivity of material enables the project workers to examine a range of potential variables that may affect the quality of results gleaned from single samples, such as the correlation of soil type or other conditions with preservation, multiple use, and variation in residue composition within the same pot. It is important to stress the need for an integrated approach to the sampling, analysis, and interpretation of organic residues. At the sampling level, collaboration between the laboratory and the fieldworker is essential to ensure a consistent strategy. When interpreting the data, consideration must be given to complementary areas of research, notably environmental and dietary evidence derived from floral and faunal assemblages. There are few examples of the incorporation of more than a single analytical technique for the analysis of organic residues. Oeal and coworkers (1991)compare stable isotopic data with GC and GC/MS data, while Skibo (1992) has undertaken a comprehensive investigation of use alteration that combines GC/MS of fatty acids in residues, distri-
272
bution and composition of soot deposits, and use wear evaluation of an ethnoarchaeological pottery assemblage from the Philippines. There is also potential for extending the range of compound classes studied, to cover the survival of carbohydrates and proteins. These are major components of foodstuffs, and their analysis would complement the identification of lipid species for the purposes of classification. While the nature of ceramic residue analysis is specific to the contents and uses of individual vessels, wider implications are common to other areas of research. Potential also exists for defining activity areas related to pot discard within settlements. The organic residue data from the potsherds analyzed at Liverpool are being stored as a database that will eventually contain further experimental data and reference samples from modern equivalents. Once fully compiled, the database will provide a reference for future research in this field. It is planned that the arganic residue data will eventually be stored and used in future research at other archaeological sites throughout the British Isles.
Conclusions
The analysis and interpretation of organic residues retained in pottery vessels is a developing field of study. Using chemicalor biochemical information in archaeological interpretation is not a simple ar routine procedure, although it is clear from the foregoing discussions that considerable promise exists in the use of modern analytical chemical techniques to deduce the composition of organic residues. Characterization of organic residues is based on the identification of specific molecules that may indica te a plant or animal arigin for the residue. While organic residue analysis may provi de information regarding the "food on the plate" (Bush and Zubrow 1986:38), it does not allow us to compile a "prehistoric menu." AIthough some exciting insights into food preparation and consumption have been made, the chemical analysis of food residues is no more a "reconstruction" of past diet than is the study of archaeobotanical remains (Miksicek 1987:239). The limiting factors of differential preservation, recovery, and degradation are als o evident in organic residue analysis. When considered together with other ceramic, environmental, and ethnographic data, organic residue analysis of preserved biologi-
273
cal matter can help to define actual vessel use. Archaeologists will benefit from an awareness of the potential and limitations of applications of the hard sciences. In this light, failures as well as successes in organic residue analysis can be addressed in terms of explanations that contribute to the developing application of this research area. Pinally, we concur with Feinman's (1989:219) conviction that in experimenting with and refining new techniques of pottery analysis, the research questions should be framed with key issues of human behavior in mind.
Acknowledgments
The authors would like to thank the Science and Engineering Research Council Science-Based Archaeology Committee (SERCSBAC) and English Heritage (Historic Buildings and Monuments Commission - England) for financial support to the Raunds Area Project ceramic residues research programo Coworkers at the Northamptonshire Archaeology Unit are also thanked for their invaluable collaboration. We are grateful for the contributions of Iohn Goad and Varian Denham for their comments on an earlier draft of the manuscript.
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6

The Analysis of Organic Residues and the Study of Pottery Use

Pottery Use in Archaeology

C. Heron and R. P Evershed

Organic Residues and Pottery Function

Chemical Analysis of Organic Residues

Definition and Classification of Organic Residues

C. Heron and R. P Evershed

Organic Residues and Pottery Function

Factors Affecting the Preservation and Decay of Organic Residues in Pottery

C. Heron and R. P Evershed occurring lipids.

Fig. 6.1. Structures oi commonly

II R, R' and R" = alkyl

Organic Residues and Pottery Function

C. Heron and R. P Everslied

Organic Residues and Pottery Function

Factors Affecting the Contamination of Organic Residues in Pottery

C. Heron and R. P Evershed

Organic Residues and Pottery Use

Organic Residues and Pottery Function

C. Heron and R. P. Evershed

Organic Residues and Pottery Function

C. Heron and R. P Evershed

Techniques for the Analysis of Organic Residues

Organic Residues and Pottery Function

C. Heron and R. P Evershed

Organic Residues and Pottery Function

C. Heron and R. P. Evershed

Figure 6.2. Cacao alkaloids from Maya ceramic vessels. identified

Organic Residues and Pottery Function

C. Heron and R. P Evershed

Figure 6.3. Diterpenoids

CO CH 2 3 Methy! dehydroabietate Retene

Organic Residues and Pottery Function

Use af Malecular Markers

C. Heron and R. P Evershed

Organic Residues and Pottery Function

C. Heron and R. P Evershed

Current Research and Future Prospects

Organic Residues and Pottery Functian

C. Heron and R. P Evershed

Organic Residues and Pottery Function

C. Heron and R. P Evershed

Organic Residues and Pottery Function

C. Heron and R. P Evershed

Organic Residues and Pottery Function

C. Heron and R. P Evershed

Organic Residues and Pottery Function

C. Heron and R. P Evershed

Organic Residues and Pottery Function

C. Heron and R. P Evershed

Organic Residues and Pottery Function

C. Heron and R. P Evershed

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