Carl Heron

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The Analysis of Organic Residuesand the Study of Pottery UseCARL HE R o N and RI c HARD P. E VE R SH EDPottery Use in ArchaeologyThe durability of ceramics in the archaeological record

provides the archaeologist with abundant material for the study ofvessel use. The determination of pottery use opens up a wide rangeof research possibilities in archaeology (Ericson et al. 1972; Hally1986:267 , including 1 the identification of food preparation andconsumption patterns in human groups, (2) the types of activitiesoccurring at sites or at particular activity loci within sites, (3) anassessment of the period of introduction of specific oodstuffs, and(4) the identification of shifts in subsistence practices and resourceexploitation.

Much of the recent interest in pottery use derives from Brauns pots as tools approach to pottery studies (Braun 1983, in whichvessels are seen as containers designed to satisfy a set of utilitarianroles. Some time ago, Ericson, Read, and Burke 1972 proposed sixmethods for the determination of pottery use, incorporating ethnog-raphy (ethnoarchaeology), the archaeological context, studies of pre-served contents, pollen analysis, chemical analysis of residues, andwear patterns (see also Rice 1987:210-11, which includes additionalapproaches). ln spite of this, Hally 1986 notes that few attemptshave been made to identify how pottery vessels from archaeologicalcontexts were used. Supplementary to the apparent lack of effort inthis research area, Dunnell and Hunt 1990:330 observe that infer-ence of ceramic vessel function is usually indirect and fraught withuncertainty.

Henrickson 1990 distinguishes between the terms fun tion anduse The former is defined as a broad term encompassing the way

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48 CHeron and RP vershed

that a pottery type, ware, or entire assemblage fits into the social,economic, and ritual contexts of a cultural system, and the rolespottery is called upon to play within these contexts. Use refers tothe specific utilitarian task or tasks a pot is put to.

The greatest effort expended in archaeological investigations hasbeen in the determination of intended use by considering the perfor-mance-based physical properties of ceramics. The study by Braun1983 on changes in ceramic technology that may have resulted fromshits in diet and food preparation during the Woodland period inNorth America has been followed by a large number of publicationsfocusing on performance-based relationships e.g., Bronitsky 1986Schiffer and Skibo 1987.These studies have focused on a number ofparameters, including the size and type of temper additions to clays,the morphology of the finished pot, and various fabric tests. Variabil-ity in the properties of the finished product has been interpretedwith respect to puta tive use. The majority of studies have been lirn-ited to one or two vessel types, although Hally 1986 attempted astudy of vessel use within an assemblage of sixteenth-century pot-tery from the Barnett phase in northwestern Georgia, comprising 13morphologically distinct vessel types exhibiting a range of physicalproperties. many cases, the relationship of form and physical prop-erties to actual pottery use may be ambiguous Woods 1986 Fein-man 1989:218, and in some settings, formal variability may havelittle or nothing to do with performance characteristics Miller 1985 .

recent years, ethnoarchaeological observations of pottery useand disposal have provided a substantial data set for potential archae-ological inference e.g., David and Hennig 1972 DeBoer and Lathrap1979 Longacre 1981 Deal 1983. Cross-cultural surveys of ethno-archaeological data that attempt to correla te pottery form with usehave also been undertaken Henrickson and McDonald 1983 . AI-though the uncertainty of this approach for actual archaeologicaltesting has been stressed Bronitsky 1989:5 , discussions of potteryuse will continue to incorporate elements of modern material cul-ture studies in evaluating past behavior.

The principal aim of this paper is to assess the potential of organicchemical analysis in the determination of vessel contents and puta-tive use and to discuss possible areas of future development. Organicresidues are included in a number of processes that contribute to theuse alteration of pottery in the archaeological context [Skibo 1992 .


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Organic Residues and Pottery Function 249Use alteratian includes depasits on vessels, visual defarmatians arwear resulting fram actual use, and absarbed residues.

Chemical Analysis of Organic ResiduesThe patential for analysis of pattery use through the

chemical identificatian af trace quantities of preserved arganic resi-dues was nated some years aga in a review Renfrew 1977:6 af theprincipal areas af ceramic analysis. However, Braun 1983:110 hasdrawn attentian to an imbalance that exists in the scientific study ofceramics, which has focused almost exclusively on the analysis afpotsherds for studies of provenance, trade, and manufacturing tech-nology. By contrast, the development and application af analyticalmethods to the study of organic residues as functional indicators hasbeen relatively slow, although recent developments in analyticalchemistry and biochemistry have opened up possibilities for newareas of investigatian in archaealagy. While some recent reviews ofpottery use have acknowledged the potential for chemical analysisof arganic residues e.g., Rice 199 Henricksan 1990 ,there has beenlittle critical assessment of many important aspects of analysis, in-cluding 1 the selection af samples for study, 2 the variations inthe degree of preservatian of different bialogical materials, and 3 therigorous interpretation of results acquired. Only brief overviews oforganic residue analysis in pottery use studies have appeared e.g.,Rabins 1983 Iones 1986:839 47 Heron et al. 1991c .

Definition and Classification ofOrganic ResiduesThe term organic residue has been used widely by archae-

ologists and archaeological scientists to describe a variety af amor-phous organic remains found at archaeological sites. By definition,organic residues lack the clearly discernible morphological featuresthat characterize other bialogical materials that survive in the ar-chaealogical record, such as wood, bone, leather, seeds, and pollen.

The amorphous nature of organic residues means that their identi-ficatian must rely on chemical analysis. The increasing use of sensi-


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25 Heron and R P Evershed

tive analytical chemical and biochemical techniques has greatly in-creased the scope of organic residue analysis, such that a definitionof organic residues must now include absorbed residues. Absorbedresidues include the trace amounts of organic components dispersedin a bulk inorganic matrix, and remnant biopolymers, that requirethe use of immunological ar amplification techniques to reveal theirpresence in archaeological specimens. Hence, organic residue analy-sis now covers the study of organic deposits on lithics Loy 1991 theanalysis of tars and pitches Evershed et al. 1985 bitumens Connan1988 soils Knights et al. 1983; Pepe et al. 1989; Pepe and Dizabo1990; Bethell et al. 1993 midden deposits Morgan et al. 1984 cop-rolites Lin et al. 1978 and human remains, including DNA [Pboet al. 1989; Hagelberg et al. 1989 and lipids Evershed 1990 19911992; Glaar et al. 1990 .

Both visible and absorbed organic residues are found in associa-tion with pottery vessels and serve as a preliminary means of elas-sification.

Visible Sutjace ResiduesThese are described variously as residues, deposits, or encrustationsand can be observed on both the inner and outer walls of vessels. Sur-face deposits on potsherds may derive from a wide range of sources.Those observed on the outer walls may derive from soot depositedduring the heating of the vessel over a fire. Burnt matter on the in-terior surfaces of sherds may derive from the charring of food or otherbiological material. Resinous substances, applied during manufactur-ing processes to reduce the permeability of porous fabrics, may alsobe observed on potsherds Rice 1987: 163.

Absorbed ResiduesAbsorbed residues result from the contact and subsequent absorp-tion of a vessel s contents into the porous and permeable ceramicwall during vessel use.

is important to draw the distinction between organic residues offood and nonfood originoFood Residues The common association of pottery vessels with foodpreparation ar consumption means that the most widely encountered


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Organic Residues and Pottery Function 25arganic residues will be thase derived fram faadstuffs. The passibili-ties for the absarptian af lipids, such as ails, during starage are clear.During cooking, such as the bailing ar roasting af faad, arganic con-stituents will be liberated ar mabilized fram faadstuffs, thus facili-tating their absarptian in the pat wall. Carbanized visible residuesare presumed to arise fram the burning af faadstuffs due to averheat-ing af vessels during cooking.Nonfood Residues A variety af nanculinary practices can result inthe depasitian af arganic residues an ceramics that cannat be relateddirectly to faad preparatian ar cansumptian. These practices includea wide range af quasi -industrial ar manufacturing processes (Rice1987:210) and the applicatian af sealants to permeable fabrics.

Factors Affecting the Preservation andDecay of Organic Residues in PotteryIn a review af faad preservatian from the past, Luck and

Galdblith (1977)highlight the paradaxical relatianship between edi-ble organic substances (faadstuffs) and preservatian. r a faadstuffto be a digestible campanent af an individuals diet, it must passessproperties that allaw it readily to change physical and chemicalstates in the gastraintestinal tract. Substances fulfilling these criteriaare alsa likely to be susceptible to degradatian by microarganismsactive 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 factarsaffecting the preservatian and decay af arganic matter have been dis-cussed in the geachemical field (Tegelaar 1990; Eglintan and Lagan1991; Lagan et aI. 1991), there has been relatively little investigatianar discussian af such factars in relatian to archaealagical material.Hawever, the same general principles apply to the survival af arganicmatter in bath fields. Evershed and caauthars (Evershed et al. 1992)have discussed some af the processes relating to the decay and preser-vatian af lipids in ancient pattery.Lipids are the mast widely studied campaund class surviving in ar-

chaealagical ceramics. Lipids, by definitian, are the salvent-extract-able campanents af bialagical materials. They have a wide variety af


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252 C Heron and RP vershed

oCH-o---C-R

2 O R and R = alkylCH- O-C-Rf t CH2- 0- 0-CH2CH2N(CH3)3

Fig 6.1. Structures oi commonly occurring lipidsoCH -O-C-R

2 O R, R and R = alkylCH-O-C-RCH - O-C-R2

Triacylglycerol

Cholesterol(animal)c

Nonacosanee

Phospholipid

Sitosterol(plant)

Herxacosanyl palmitate

functions in living tis sues and so occur widely in nature Gunstoneand Norris 1982 . For instance, triglycerides triacylglycerols: e.g.,Fig. 6.la serve as energy stores and are the major components ofplant oils and animal fats, phospholipids e.g., Fig. 6.1b are struc-tural components of cell membranes, sterols e.g., Fig. 6.lc and d arestructural components of cell walls and the precursors of some hor-mones, and long-chain alkyl compounds e.g., Fig. 6.1e and f arecommon constituents of plant and animal waxes.


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Organic Residues and Pottery Function 5

The survival of different components of organic residues over ar-chaeological time depends on their chemical nature and the physico-chemical conditions e.g., pH and redox potential that prevailed inthe immediate burial environment. Eglinton and Logan 1991drawattention to the importance of the entrapment of molecules in en-hancing the possibilities for their survival in geological materials.Entrapment of organic compounds in pottery during use includessuch processes as the microencapsulation of organics in carbonizedsurface residues and the absorption of molecules into pores in theceramic matrix. Entrapment will enhance the survival of organiccompounds by inhibiting the access of microorganisms capable ofdegrading organic matter. The adsorption of molecules on clay sur-faces will further limit their availability as substrates for enzymespresent in microorganisms.

A review of the chemical properties of the major compound classeslikely to be found in organic residues associated with ancient potteryis inappropriate here. However, it is important to stress that thelikelihood of survival of various biological molecules is largely de-pendent upon the chemical reactivity of the functional groups pres-ent in the molecules that make up the organic residues. Significantly,the likelihood for preservation of proteins, carbohydrates, and nu-cleic acids is less than that of lipids Tegelaar 1990; Eglinton andLogan 1991; Logan et al. 1991.However, even lipids contain cherni-cal groups and linkages that will be susceptible to modification ordegradation over archaeological time. For example, Rottlnder andSchlichtherle 1983performed simulation experiments to show thedifferent rates of oxidation of fatty acids possessing different degreesof unsaturation. Oxidation of polyunsaturated fatty acids occursmuch more rapidly than oxidation of monounsaturated fatty acids.Related to this work are investigations of the degradation of wholeplant and animal fats den Dooren De Iong 1961;Morgan et al. 1973;Thornton et al. 1970 . These studies found that fatty materials de-composing anaerobically under waterlogged conditions are suscepti-ble to hydrolysis, hydration, reduction, and carbon-carbon doublebond scission reactions. The formation of lO-hydroxystearic acid andthe scrambling of the double bond position in monounsaturated fattyacids present in adipocere suggest that the mechanism of fat degrada-tion in a waterlogged environment is complex Evershed 1990, 1991,1992 . Fatty materials absorbed in potsherds buried in waterloggedsites would be expected to undergo analogous degradations. The pos-


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54 C eron and RP verslied

sibility for the conversion of oleic acid to palmitic acid in water-logged anaerobic environments den Dooren De Iong 1961 castsdoubt on conclusions drawn from studies using fatty acids as thesole indicators of the nature and origins of fatty remains found inassociation with buried pottery.

The solubility of the various classes of biomolecules will have asignificant influence on their persistence in pottery buried in water-logged environments. The hydrophobic nature of lipids will greatlylimit their solubility in groundwater and hence willlimit their lossfrom potsherds by dissolution and diffusion. Evidence for this hascome from investigations of the possible effects of migration of lipidsfrom the burial soils into potsherds see below . Studies on the com-position of lipids preserved in bog body tissues and the surroundingpeat bog provi de further indications of the lack of mobility of lipidsin groundwater due to their inherent hydrophobicity Evershed andConnolly 1988 .

There is currently much less evidence for the preservation of themore polar biopolymeric constituents of biological materials in an-cient potsherds. Pyrolysis-mass spectrometry PY-MS has providedevidence for the presence of proteins and carbohydrates in charredresidues Oudemans and Boon 1991 . However, where these com-pounds have been released from tissues, for example, by boilingwater during cooking, and absorbed into the ceramic fabric, thentheir subsequent loss by leaching in waterlogged environments islikely to occur. Hydrolysis during aging of polysaccharides and pro-teins will produce the constituent monosaccharide and amino acidsrespectively, which on account of their solubility may be lost frompotsherds by dissolution and diffusion in waterlogged environments.Conversely, and in contrast to lipids, there is a greater likelihood forpolar water-soluble substances to migra te into buried pottery duringthe movement of groundwater. Considerably more work is requiredto establish the extent of preservation and decay of proteins, carbo-hydrates, and other biopolymers in buried pottery.

Certain nonfood natural materials, e.g., hydrophobic resins andwaxes, owing to their high chemical stability or refractory nature,may survive from antiquity in a relatively unchanged state. Thechemistry of many such substances has been surveyed Mills andWhite 1987 .The resistant properties of substances of this type willhave been utilized for a variety of practical purposes, including water-


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Organic Residues and Pottery Functionproofings and adhesives. If pottery vessels were used to colIect, store,ar process such materials, then organic residues indicative of theseactivities should be readily detected. Many plant and animal waxes,e.g., epicuticular leaf waxes and beeswax respectively, are com-posed largely of fulIy saturated long-chain alkyl compounds such ashydrocarbons n-alkanes and wax esters TulIoch 1975; Kolattukudy1976.

Factors Affecting the Contamination ofOrganic Residues in PotteryIn view of the presence of organic matter in soil, it is sur-

prising that apparently so few investigations have addressed the pos-sibility of migration of organic matter into sherds or vice versa Con-damin et al. 1976; Heron et al. 1991b .The organic matter present inthe soil represents the net of all processes, such as the input of plantand animal detritus and microbial synthesis by fungi and bacteria aswell as subsequent degradative processes Braids and Miller 1975and anthropogenic input Knights et al. 1983; Bethell et aI. 1993 . Ina recent study of freshly excavated late Saxon/early medieval sherdsWest Cotton, Northamptonshire, U.K. and adhering burial soil, thedifferences in the lipid compositions, determined by gas chromatog-raphy c c and combined gas chromatography/mass spectrometry C C /M S , led to the conclusion that contamination of preserved lipidsin potsherds by soillipids may not be a serious problem Heron et al.1991b. Clear quantitative and qualitative differences were found be-tween the lipids absarbed in the sherd and those of the soil adheringdirectly to the pot surface. This is attributed to the hydrophobic na-ture of the lipid molecules. However, in some cases, the relationshipis less clear, particularly where the yield of pot residue is very low.In other investigations, the analysis of the internal and external por-tions of sherds have been sampled separately to detect concentrationgradients from the inside to the outside of the vessel wall Condaminet al. 1976 .

While indications are that the lipids preserved in potsherds arelargely unaffected by migration of soil components, the behavior ofmore polar proteinaceous and carbohydrate constituents is much lessclearly understood see above . Rigorous compara tive studies of the


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pratein and carbohydrate content of potsherds and adhering soil arerequired to resolve the questions surraunding their behavior duringburial d. Heran et al. 1991b for lipids). The collection of soil samplesfor analysis along with pottery samples is strangly recommended.

Other samples to be included in a validation study could includekiln wasters or handles not expected to have come into contact withthe contents of the vesseI. Whether handles retain trace amounts oflipid residues or are blanks remains to be addressed. According toGabasio and coauthors Gabasio et al. 1986 , organic matter in pot-sherds can arise not only thraugh use but also fram naturally occur-ring organic matter in the clays, organic temper additions, or kilnfuel. Although carbonized fragments of biological matter, incorpo-rated into the original clay, are commonly found in potsherds, it isunlikely that organic compounds survive the firing pracess, exceptwhere very low temperatures were attained during firing [Iohnson etaI. 1988 . Since many earthenwares were fired at low temperaturesfor only short durations, specific firing experiments could be de-signed to assess the survival of organic matter occurring naturally inclays fram which the vessels are manufactured.

Organic Residues and Pottery UseA large number of processes carried out in pottery vessels,

notably the repeated heating of animal and plant praducts, willleavechemical evidence of this activity. In addition to the preparation,storage, and cooking of food, many other activities will also haverequired the use of pottery vessels. These activities include brewing,tanning, dairying, dyeing, fulling, textile washing, and salt prepara-tion. However, other uses, such as the dry storage of grain or seeds,may yield no detectable residue on analysis, unless the residue wasaccidentally charred to the pot surface.

Evidence exists for the preparation and use of dyestuffs in potteryvessels Biek 1963: 105-12; McGovern and Michel 1984 . Naturaldyestuffs are also known to have been used to decora te ceramicsFoster and Moran 1989 . Earthenware vessels were also used as bee-hives. Gas chramatographic data from analyses of residues fram sus-pected beehives found on coarse ware combed k lt oi fram Vara,Greece, dating fram the fourth to third centuries B.C., are consistent


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Organic Residues and Pottery Function 257with the presence of beeswax Bu lock 1973).There is also evidencefor 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)aswell as the use of large vessels as receptacles for the collection of tarfrom heated wood piles Leglay 1973:529).

Certain vessel uses may be difficult to determine, owing to prob-lems of preservation or retention of diagnostic organic constituents.Determining a previous association with alcoholic beverages posessuch a problem since they comprise a dilute solution of organic com-pounds in water Haevernick 1967). Remains of such beverages willbe more likely in arid environments, following evaporation of thewater and alcohoI. Since the compounds of interest are not presentin abundance, significant quantities of residue may need to be pre-served, as in examples of sealed amphoras from wreck sites Conda-min and Formenti 1976, 1978; Formenti et al. 1979). some cases,pollen or botanical evidence may be invaluable. Dickson 1978) car-ried out pollen analysis of a Bronze Age beaker residue from an in-humation burial at Ashgrove, Fife, U.K. Lime or linden Tilia andmeadowsweet Filipendula pollen were found in abundance, sug-gesting that the contents of the beaker may have been a beverage notunlike mead, flavored with lime honey and meadowsweet. Similarly,Bohncke 1983) undertook pollen analysis of a black greasy materialfrom a Bronze Age food vessel accompanying a burial at Strathallan,Perthshire, U K High percentagesof meadowsweet and ceralian pol-len suggested either a porridge of cereals or a fermented beverageflavored with meadowsweet flowers or extract. Without doubt, thereis much scope for complementary application of pollen analysis andother palaeobotanical information with chemical data.

ostjiiin TreatmentsThe analysis of organic residues found in pottery containers musttake into account a wide range of surface treatments employed toreduce or control the permeability of low-fired ceramics. additionto prefiring surface treatments such as glazing, burnishing, or theapplication of a slip, the use of organic substances to seal the interiorwalls of vessels after firing is also known. Evidence for the use ofpine resin, tar, and pitch sealants on Roman amphoras to facilitatethe transport of liquids is widespread Heron and Pollard 1988).Seal-


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58 CHeron and RP Evershed

ants may also have been applied to other types of vessels used forcooking, storage, serving, and drinking Shepard 1968:93; Rye 1976:119; Arnold 1985: 140; Rice 1987: 163-64; Schiffer 1990; Gianno1990 . Schiffer 1990 has demonstrated that pots coated internallywith resin possess excellent heating effectiveness [the rate at whichthe temperature of water is raised when a vessel is placed over a heatsource . Some potters apply resinous coatings to the exterior surfacesof vessels Foster 1956 .

Ethnographic observations suggest great diversity in modifyingthe permeability of pottery vessels with organic substances. In addi-tion to the use of resins and waxes, foodstuffs have also been used toseal porous vessel walls prior to use. In Papua New Guinea, pots aresealed by boiling paw-paws, yams, or bananas in them May andTuckson 1982:49 . Ethnographic records of Thule Eskimo activitiesindica te that before use, pots were sealed with grease or oil or werelined with stomach pouches or gut Stimmell and Stromberg 1986 .Recognition of postfiring treatments will be more obvious when thesubstances identified are inedible or would not normally constitutea component of diet, as in the case of a resin. However, if the treat-ment involves the use of plant and animal products that are food-stuffs in their own right, for example, milk Cheape 1988: 17 or someother product containing fat, interpretations from chemical analysiswill be complicated. One approach to this problem would be to sam-ple a large array of vessels from a single site. If an organic residuediagnostic of a potential sealant occurs with high frequency, then apostfiring treatment might be suspected.

Multiple Use of Pottery ontainersThere is at present only limited evidence to suggest that organicresidue analysis is able to determine multiple use of a single vessel.Mixtures of foodstuffs are clearly evident from the analytical resultsof some investigations Evershed et ai. 1991 . The problem lies indemonstrating whether this represents a deliberate mixing of food,as in the case of a soup or a stew, or the sequential use of the vesselfor preparing different foods. This problem is not easily resolved butis being considered using data from analytical chemistry, ethnoar-chaeology, and experimental archaeology in the following investiga-tions: 1 by comparison of the composition of surface deposits with


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Organic Residues and Pottery Function 9residues absorbed in the vessel wall, 2 by cooking and charring ex-periments using pots fired under similar conditions to those underinvestigation, and 3 by consideration of ethnoarchaeological dataon the types of vessels used for specific or multiple uses. A consider-ation of use wear may also be appropriate in evaluating multiple use[Skibo 1992 .

Since cooking pots absorb the taste and smell of the food preparedin them, separate pots may be needed for different foods to avoidtainting Arnold 1985: 138-39; Fl and Hofer 1988 . Some ethnoar-chaeological accounts observe that vessels are reused only whenthey have failed in their primary use, such as if the resin coating hasdissipated or if the vessel is cracked [Longacre 1981:63 . Althoughcracked vessels may be repaired to prolong primary use, the pots oreven individual sherds may be put to a wide variety of secondaryuses DeBoer and Lathrap 1979: 125, 127 . Ethnoarchaeological workby Deal 1983 among the Tzeltal Maya in Mexico indicates thatmany residues on pottery result from secondary or tertiary uses ofvessels and repair practices. The relationship between primary andsecondary use merits further consideration, including studies of pot-tery deposition and disposal. It is likely that the multiple use of pot-tery vessels cannot be elucidated by organic residue analysis alone.

Position of Surface ResiduesIn addition to the identification of the organic residue, the natureand position of the residue on the artifact is of importance in estab-lishing its putative use. The nature and distribution of surface resi-dues on the internal wall may indica te how the food was prepared[Andersen and Malmros 1984; Hastorf and DeNiro 1985 , while soot-ing patterns may suggest how the vessel was heated [Hally 1983;Moorhouse 1986; Skibo 1992 .

Residues enveloping the rims ofvessels may indicate sealing agentsused to fix lids or skins across the top of the pot. Documentarysources from the medieval period in Britain indicate the use of differ-ent rim adhesives or specific pr psrstiv fu nc tio ns o orh ou se1986 . Vessels are also known to have been repaired using adhesivessuch 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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26 Heron and R P Evershed

Techniques for the Analysis ofOrganic ResiduesIdentification of the origin of organic residues relies on

matching a unique chemical property of the residue to that of a con-temporary natural materiallikely to have been exploited in antiquity.The analysis of organic residues is not a new field of study. AncientEgyptian Materials and Industries byAlfred Lucas, first published in1926 and updated until the fourth and final edition appeared in 1962with Harris), contains critical discussions on many early results,dating to the late nineteenth century, obtained from studies of mate-rials found at Egyptian and Near Eastern sites. The book providesconsiderable detail on a wide range of organic substances used inantiquity, supplemented extensive wet chemical tests carriedout on substantial finds of organic material preserved in arid loca-tions. The majority of wet chemical tests, such as spot tests, andsolubility and melting point determinations, require relatively largesamples 1mg quantities). Similar work was carried out on potteryand soil samples in Germany during the 1930s von Stokar 1938).The failure to establish a clear identity of many substances resultedfrom processing e.g., heating) in antiquity or aging, with the effectthat the chemical properties of the sample were altered compared tocontemporary reference material.

The application of modern analytical chemical and biochemicaltechniques allows very detailed assessment of the chemical compo-sition of previously intractable organic residues. Such data are ofparticular value in determining the nature and origin of residues, aswell as establishing the presence of decay products and postdeposi-tional contaminants.

Visual InspectionAlthough not an analytical chemical technique, visual inspection ofresidues in potsherds is included here since any macroscopic remainsare of great value in support of chemical data, particularly in the se-lection of reference material for comparison. Interest in the detectionof dietary constituents preserved in surface deposits, or the pot fab-ric, has prompted a range of investigations. Andersen and Malmros1984)conducted microscopic examination of charred deposits foundin three pointed-based vessels from the Ertebolle site at Tybrind Vig,


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Organic Residues and Pottery Function 261Denmark, radiocarbon dated to 4400-3200 B C and recovered un-charred bones, scales, and fin rays from cod Gadus morrhua . In somestudies, fungal hyphae have been observed Bush and Zubrow 1986 ,while in others, workers have reported an absence of morphological re-mains in large numbers of charred deposits Hastorf and DeNiro 1985 .

Elemental AnalysisScanning electron microscopy has been used in the study of visiblesurface residues. The possibility exists for performing quantitativeelemental analysis using instruments that include facilities forenergy-dispersive x-ray analysis, although such data would appear tobe of limited value for discriminating between different foodstuffsd. Bush and Zubrow 1986 . Following experimental work by Duma1972 , who demonstrated that ceramic fabrics take up phosphorusfrom aqueous solutions, the detection of elevated concentrations ofphosphorus in the ceramic matrix has been proposed as a method ofdetermining whether a vessel contained organic matter Cackette etal. 1987 . In the latter study, the authors compared elemental phos-phorus concentrations in an unused ethnographic pot with a cookingvessel and a pot used for boiling water. Using energy-dispersive x-rayfluorescence, they found higher phosphorus concentrations in thepot used for cookng than in the unused vessel or the one used forboiling water. However, Freestone, Meeks, and Middleton Freestoneet al. 1985 reported the ability of pottery to take up phosphorusfrom the burial matrix by a number of possible yet unspecified me-chanisms. Therefore, the possibility exists for high concentrationsof phosphorus arising from postdepositional uptake swamping thataccumulated during vessel use. Dunnell and Hunt 1990 concludefrom their experimental study that, because phosphorus uptake fromthe soil may take place, inferences based on vessel use are unreliableuntil the mechanisms and forms of postdepositional enrichment arebetter understood. Furthermore, phosphorus is present in all plantsand animals, and the demonstration of elevated phosphorus levels invessel walls would provide only a nonspecific indication of use.

Stable lsotope AnalysisInformation concerning the nature of charred plant remains adher-ing to potsherds has been derived from stable carbon 13C and nitro-


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gen 1SN)isotope ratios. These measurements enabled residues of C3and C4 plants and legumes to be differentiated Hastorf and DeNiro1985; Morton and Schwarcz 1988; Morton et al. 1991 . Hastorf andDeNiro 1985 studied 71 burnt visible residues on jars from the UpperMantaro Valley in the Central Peruvian Andes. Stable isotope analy-sis suggested that the jars had been used to cook C3 plants such astubers and quinoa alone or C4 plants maize) and C3plants together,either simultaneously or sequentially. Moreover, their resultsshowed that the vessels had not been used for cooking legumes,either in combination with nonleguminous plants or alone. Theseconclusions are consistent with modern cooking practices carriedout in the same region of the Andes. Problems may occur in thewider application of this technique due to food groups possessingoverlapping 1sN and 13Cvalues Deal 1990:9 .

lnfrared SpectroscopyInfrared IR spectroscopy has been used to investigate visible resi-dues without prior extraction of organic constituents. However, un-less substantial quantities of organic constituents are preserved inthe deposits, inorganic absorptions due largely to phosphates andcarbonates may domina te the spectra Heron 1989: 123-24 . Infraredspectroscopy has also been used to study solvent extracts of bothvisible residues and sherds Needham and Evans 1987; Hill andEvans 1989. Infrared spectra may provide a useful fingerprint,even though residues may comprise a complex mixture of con-stituents. However, IR absorption bands tend to merge into a seriesof broad envelopes due to the large number of bond types that resultfrom degradation during vessel use and burial. Infrared spectros-copy has been applied successfully to the identification of aged soft-wood 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 Pollard1988 . Although it is possible to fingerprint nonfood or naturalproduct residues using IR spectroscopy, the usefulness of the tech-nique is limited for the study of most organic residues because IRspectroscopy lacks the selectivity and sensitivity necessary for thecharacterization and detection of complex mixtures of organicconstituents.


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Nuclear Magnetic Resonance SpectroscopyNuclear magnetic resanance NMR is widely used in natural productchemistry for elucidating the structure af arganic substances. How-ever, NMR has relatively limited application in the study af organicresidues because of the small amounts of organic matter availablefar study. The investigatian of a dark brown liquid remaved fram aglass flask, dated the sixth faurth century B.C. Syria , is ofrelevance here Beck et aI. 1974 . Nuclear magnetic resanance pro-vided evidence for the substance being a degraded oil. Oudemansand Boon [personal cammunicatian have faund solid-state NMR be af value in the analysis of the carbohydrate content af carbonizedvisible residues. The data are camplementary that obtained bypyrolysis-mass spectrometry Oudemans and Boon 1991 .

Thin Layer ChromatographySolvent extraction of patsherds and residues yields lipid extracts thatcan be investigated by a range of chromatagraphic techniques. Thinlayer chromatagraphy TLc rnethods have been used in investiga-tions of organic residues y amang athers, Gurfinkel and Franklin1988 and Rottlander and Schlichtherle 1979 . Hawever, as with IR,interpretatians based an TLC are greatly cornplicated by the effects afdecay that frequently yield a range of cornpounds af slightly differingstructure. Improved selectivity and sensitivity is attainable y use afGC ar high-perfarmance liquid chromatagraphy HPLC , which arecapable of resalving individual molecular species.HighPerformance Liquid ChromatographyHigh-perfarmance liquid chramatagraphy has Iound relatively littleuse in the study ofarganic residues in ceramics. Notable examples in-clude the analysis af lipid residues in a 1,500-year-ald Mediterraneanamphora and an oil larnp Passi et al. 1981.In this study, fatty acidsfreed fram acyllipids by hydrolysis were analyzed by HPLC as theirphenacyl esters. The study shawed that although some acyllipidsare preserved in ceramics, great care must be taken assess theeffects af decay and microbial contamination befare praceeding withinterpretation of their arigin. Althaugh HPLC was effective in this


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264 C. Heron and R PEvershed

Figure 6 Cacao alkaloids from Maya ceramic vessels identified throughHPLcMS

Caffeine Theobromine

instance, GC is generally preferred to HPLC for the analysis of lipidsdEvershed et al. 1990 Evershed et al. 1992for further discussions).

A more recent application of HPLC Hurst et al. 1989 Hall et al.1990) succeeded in demonstrating the presence of cacao alkaloids,caffeine Fig.6.2a) and theobromine Fig.6.2b), in three Maya vesselsof the Early Classic period. Their findings were consistent with thepresence of hieroglyphs on one of the vessels that suggested a useassociated with cacao. This investigation demonstrates the useful-ness of combining chromatographic techniques on-line with massspectrometry see below for further discussions).

Gas h tom togiphv and Gas ChromatagraphyMass SpectrametryGas chromatography and gas chromatagraphy/mass spectrometryare the preferred techniques for the analysis af lipid extracts of visi-ble and absorbed residues obtained by solvent extraction [Patrick etal. 1985 Evershed et al. 1990).The possibility of performing nondes-tructive extractions of organic residues from ceramics has been con-sidered but has yet to be rigorously evaluated LeCarpentier et al.1987 Gerhardt et al. 1990).Such an approach is potentially attractivefor the study of rare ar valuable artifacts.


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Organic Residues and Pottery Function 65The value of GClies in its ability to resolve the individual cornpo-

nents of the often complex mixture of lipids found in potsherds.Capillary GC is much more readily interfaced with mass spec-trometry, thus allowing on-line separation and characterizationof the individual compounds as they elute from the Liquid chro-matography/mass spectrometry LC/MS)offers similar advantages tothe analysis of more polar substances, as discussed above in relationto the study of cacao residues [Hurst et al. 1989).

Some notable successes of GCand GC/MSinclude the identificationof softwood resin, tar, and pitch of Pinus sp. in Roman transportamphoras. These were characterized through their component diter-penoids Fig. 6.3a and b, see Robinson et aI. 1987; Heron and Pollard1988; Beck et al. 1989).The detection of triterpenoids from Pistaciasp. has also confirmed the identity of the resins contained in theCanaanite amphoras from the Late Bronze Age shipwreck at UluBurun in southern Turkey [Mills and White 1989).The characteriza-tion of triterpenoid compounds, notably betulin 6.3c), found in largequantities in the bark of the birch tree Betula sp.], has confirmedthe widespread use of birch wood and birch-bark tar prehistoriccommunities [Binder et al. 1990; Hayek et aI. 1990; Heron et aI.1991a).Most of the evidence for these materials comes from potteryvessels used to produce and store the derived tar. Tars were also usedto modify the properties of pottery vessels, for example, through theapplication of a sealant or as an adhesive for repairing [Charters et al.1993) or applying decorations such as cut-out patterns of birch barkto pots Vogt 1949).Gas chromatography/mass spectrometry has alsobeen used by Connan 1988) to characterize and source natural bitu-men samples associated with a range of artifacts from Mesopotamia,including potsherds.

Pyrolysis MethodsCharacterization of visible residues has been investigated usinganalytical pyrolysis techniques such as Curie-point pyrolysis massspectrometry CUPY-MS)and Curie-point pyrolysis gas chromatog-raphy/mass spectrometry CuPY-GC/MS;see Oudemans and Boon1991). No sample preparation is required, and analysis can be per-formed on very small samples 20-30 f.Lg).The analysis of 33 surfacedeposits observed on distinctive pottery types from a native Roman


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266 C. Heron and RP Evershed

Figure 6 iterpenoids and triterpenoids idemified through andGCMS

\O 2 3

Methy dehydroabietate Retene b

Jl

O

Betulinc

settlement at Uitgeest-Groot Dorregeest (Netherlands) allowed py-rolysis fingerprints to be obtained. A notable advantage of thesepyrolysis techniques lies in their ability to assess the protein, carbo-hydrate, and lipid content of residues simultaneously in samples,although more specific assignments are difficult. Discriminant analy-sis of the data suggested several groups of residues of different chemi-cal composition associated with the specific vessel forms.


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Organic Residues and Pottery unction 267

Use af Malecular MarkersThe preferred approach to the characterization of organic

residues is based on chemotaxonomic and phylogenetic principles.This relies on matching a specific chemical property, generally thepresence of a particular compound structure or distribution of com-pounds, to that of a contemporary plant or animal natural productreference material . This in itself is not without problems, since in-dividual compounds may be found across a broad range of materialsof different origino A knowledge of the plant and animal specieslikely to have been exploited in antiquity is of value in selectingcontemporary materials for compara tive purposes Deal et al. 1991 .Since the published literature details only domesticated species orcommercially important wild species, the results of experimentalstudies and Iaboratory cooking simulations can be incorporated intothe database. The development of such databases is an integral com-ponent of the organic residue research.

nalytical MethodAn analytical protocol for the study of lipid residues from potsherdshas been outlined elsewhere Evershed et al. 1990 and is not detailedhere. Briefly, prior to analysis, organic residues are isolated from theinorganic matrix a finely ground potsherd or a partially carbonizeddeposit], by solvent extraction, to provide a totallipid extract. Thetotallipid extracts are submitted directly to GC with a minimum ofsample work-up. Only trimethylsilylation is required to enhance GCproperties. Gas chromatography has the potential to separate indi-vidual molecular species from what are often complex mixtures, andidentification proceeds by comparison with reference compounds.Combined GC/MS provides the essential structural information re-quired for unambiguous identification of each compound.

Lipid extracts are commonly analyzed by GC after saponification[alkaline hydrolysis of the preserved acyllipid components of theresidue. However, high-temperature GC and GC/MS allow intact acyllipids, such as triacylglycerols, diacylglycerols, monoacylglycerols,and wax esters to be analyzed without saponification, thus providingcompositional information that would otherwise be lost Evershedet al. 1990; Evershed 1992 .A similar approach has been reported for


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68 CHeron and RP Evershed

the use of high-temperature GC for the fingerprinting of nonfoodnatural products Glastrup 1989 The use of high-temperature GCanalysis has demonstrated the survival of acyl lipids, alkyl com-pounds, and sterols in a large number of potsherds of Bronze Age,Roman, and late Saxon/early medieval periods sampled from theRaunds Area Project Evershed et aI. 1990; Evershed 1992

Fatty cids as iotn tketsAlthough fatty acid profiles can provide useful information on theorigin of residues, their diagnostic potential is limited when consid-ered in isolation. Most fats and oils differ in composition accordingto the relative proportions of a somewhat narrow range of major fattyacids Paul and Southgate 1978 Furthermore, specific fats and oilscan exhibit marked variability in composition of individual fattyacids. Factors such as soil type, clima te, and method ofprocessing canaffect the composition of plant and seed oils, while animal fats mayvary in composition as a result of diet and the particular part of theanimal from which the fat is derived Mills and White 1987:26-28

A review of the archaeological literature revealed references tomore than 20 different aged fat or oil residues determined by chemi-cal analysis Heron 1989:88 Unfortunately, it is difficult to knowhow differentiation between the wide range of possible fats or oilswas achieved. It is impossible to assess or compare results with suchunsubstantiated statements, many of which do not include data ortechnical descriptions. Such statements serve no purpose, either forthe archaeologist or the residue analyst, and we urge that these berejected on scientific grounds. Some interpretations are supportedby supplementary data such as documentary evidence Morgan andTitus 1985 The problem of similarities in the composition of par-ticular fats or oils is accentuated in archaeological contexts by oxida-tive and microbial degradation den Dooren de Iong 1961; Morgan etaI. 1984; Evershed 1990; Evershed 1992 Without exception the morelabile unsaturated fatty acids are depleted in aged samples, resultingin a concomitant increase in the relative proportions of saturatedfatty acids Morgan et aI. 1973 The survival of polyunsaturated fattyacids in sherds, commonly the major constituents of fish and vege-table oils, is rare. However, reports of traces of linoleic acid C18:2) inancient human soft tissue remains Evershed Connolly 1988;Glaar et aI. 1990 and dry maize seeds from Anasazi sites up to


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Organic Residues and Pottery Function 91,700 years old Priestley et al. 1981 suggests that a degree of survivalmay be possible under certain preservation conditions.

The effects of decay complicate direct comparison of aged lipidresidues with tables of contemporary food composition Paul andSouthgate 1978; Rottlnder 1990 . Problems of interpretation areexemplified by conversion in anaerobic environments of the unsatu-rated acyllipids to adipocere, a mixture of predominantly free satu-rated fatty acids den Dooren De [ong 1961; Thornton et al. 1970 .Although degradation can be retarded due to incompletely under-stood mechanisms of preservation, assigning residues to specificfood sources based solely on fatty acid composition may be unreli-able. This includes the so-called palmitic-to-stearic acid ratio andthe percentage of saturated fats, since these are often degradationproducts derived from other acids. A much more realistic approachis the differentiation between general categories of foods such asdairy products Evershed et al. 1992 ,fish and marine mammallipidsPatrick et l 1985; Dea11990 , animal fats, and vegetable oils Heronet al. 1991c based on more readily distinguishable compositions.

Sterols as iom tketsWhile GC is appropriate for sensitive separations of the lipid extracts,GC/MS is generally required to detect the trace amounts of sterolpresent. Although sterols are mino r constituents usually less than1 of plant and animal products, their structures are diagnostic ofthe nature of the source foodstuff. The biosynthesis of cholesterolsee Fig. 6.lc by animals and alkylated sterols e.g., sitosterol, seeFig. 6.1d by higher plants enables animal- and plant-derived resi-dues, or a mixture of the two, to be identified Evershed et al. 1990;Heron et al. 1991c .The susceptibility of sterols to structural alter-ation as a result of cooking and postburial diagenetic processeshas been discussed elsewhere Evershed et al. 1992 . Due to theubiquitous occurrence of cholesterol in our fingerprints, it is impor-tant to stress the potential threat of contaminating sherds throughhandling.Other iom tketsLong-chain alkyl compounds congruent with epicuticular leaf waxcomponents of Biassica vegetables have also been identified in a


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Organic Residues and Pottery Functian 7been 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 ofabsorbed lipids in large numbers of potsherds,

2 the use of GC and G 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, and5 the integration of analytical chemical data with typological,

petrological, manufacturing, and contextual informationwith the aim of defining specific or general patterns ofvessel use.

Ongoing excavation at the site has allowed the implementation,in the field, of specific, project-designed sampling strategies, includ-ing handling and storage. Care has been taken not to remove possiblesurface residues, as well as soil adhering to the sherd, to enable com-parative analysis. Storage in paper bags rather than plastic bags re-moves the problem of plasticizer contamination of samples. All pot-tery submitted for residue analysis is examined by pottery specialistsand given full contextual description. The large number of samplesand the selectivity ofmaterial enables the project workers to examinea range of potential variables that may affect the quality of resultsgleaned from single samples, such as the correlation of soil type orother conditions with preservation, multiple use, and variation inresidue composition within the same pot.

It is important to stress the need for an integrated approach to thesampling, analysis, and interpretation of organic residues. At thesampling level, collaboration between the laboratory and the field-worker is essential to ensure a consistent strategy. When interpretingthe data, consideration must be given to complementary areas ofresearch, notably environmental and dietary evidence derived fromfloral and faunal assemblages.

There are few examples of the incorporation of more than a singleanalytical technique for the analysis of organic residues. Oeal and co-workers 1991compare stable isotopic data with GC and G MS data,while Skibo 1992has undertaken a comprehensive investigation ofuse alteration that combines G MS of fatty acids in residues, distri-


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272 C. Heron and RP vershed

bution and composition of soot deposits, and use wear evaluation ofan ethnoarchaeological pottery assemblage from the Philippines.

There is also potential for extending the range of compound classesstudied, to cover the survival of carbohydrates and proteins. Theseare major components of foodstuffs, and their analysis would com-plement the identification of lipid species for the purposes of classifi-cation. While the nature of ceramic residue analysis is specific to thecontents and uses of individual vessels, wider implications are com-mon to other areas of research. Potential also exists for defining ac-tivity areas related to pot discard within settlements. The organicresidue data from the potsherds analyzed at Liverpool are beingstored as a database that will eventually contain further experimen-tal data and reference samples from modern equivalents. Once fullycompiled, the database will provide a reference for future research inthis field. It is planned that the arganic residue data will eventuallybe stored and used in future research at other archaeological sitesthroughout the British Isles.

ConclusionsThe analysis and interpretation of organic residues re-

tained in pottery vessels is a developing field of study. Using chemi-calor biochemical information in archaeological interpretation is nota simple ar routine procedure, although it is clear from the foregoingdiscussions that considerable promise exists in the use of modernanalytical chemical techniques to deduce the composition of organicresidues. Characterization of organic residues is based on the iden-tification of specific molecules that may indica te a plant or animalarigin for the residue. While organic residue analysis may provi deinformation regarding the food on the plate Bush and Zubrow1986:38), it does not allow us to compile a prehistoric menu. AI-though some exciting insights into food preparation and consump-tion have been made, the chemical analysis of food residues is nomore a reconstruction of past diet than is the study of archaeobo-tanical remains Miksicek 1987:239). The limiting factors ofdifferen-tial preservation, recovery, and degradation are also evident in or-ganic residue analysis.

When considered together with other ceramic, environmental,and ethnographic data, organic residue analysis of preserved biologi-


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cal matter can help to define actual vessel use. Archaeologists willbenefit from an awareness of the potential and limitations of applica-tions of the hard sciences. In this light, failures as well as successesin organic residue analysis can be addressed in terms of explanationsthat contribute to the developing application of this research area.Pinally, we concur with Feinmans ( 1989:219) conviction that in ex-perimenting with and refining new techniques of pottery analysis,the research questions should be framed with key issues of humanbehavior in mind.

knowl edgmentsThe authors would like to thank the Science and Engineer-

ing Research Council Science-Based Archaeology Committee (SERC-SBAC) and English Heritage (Historic Buildings and MonumentsCommission - England) for financial support to the Raunds AreaProject ceramic residues research programo Coworkers at the North-amptonshire Archaeology Unit are also thanked for their invaluablecollaboration. We are grateful for the contributions of Iohn Goadand Varian Denham for their comments on an earlier draft of themanuscript.

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