Documenta Praehistorica XLI (2014) Neolithic and Eneolithic activities inferred from organic residue analysis of pottery from Mala Triglavca, Moverna vas and Ajdovska jama, Slovenia Lucija {oberl1*, Milena Horvat2, Andreja ?ibrat Ga[pari;2, Marko Sraka2, Richard Evershed1 and Mihael Budja2 1 Organic Geochemistry Unit, School of Chemistry, University of Bristol, UK lucija.soberl@gmail.com 2 Department of Archaeology, Faculty of Arts, University of Ljubljana, SI ABSTRACT - The research discussed in this pap^^ focused on the analysis and identification of organic residues either preserved as visible or absorbed organic remains on Neolithic and Eneolithic pottery from various archaeological and geographical contexts. These are connected with various food preparation strategies and past human activities, i.e. cave burials in Ajdovska jama (food as a grave good/offering), the rock shelter at Mala Triglavca (meat and dairy animal husbandry practices) and Moverna vas, which had a long occupation sequence (complex farming and animal management). The preservation of biomarkers mirrored past human activities and different pottery uses at various types of sites. The carbon stable isotope ratios of primary fatty acids in lipid pottery extracts confirmed the presence of adipose and dairy fats as well as biomarkers ofplant fats, beeswax and birch bark tar. IZVLEČEK - Predstavljeno raziskovalno delo se je osredotočalo na analizo in identifikacijo organskih ostankov na površini neolitske in eneolitske keramike ter ostankov lipidov absorbiranih v keramično matrico vzorcev iz različnih arheoloških in geografskih kontekstov. Ti so povezani z različnimi strategijami priprave hrane in preteklimi človeškimi aktivnostmi - pokopi v Ajdovski jami (hrana kot grobni pridatek), skalni previs Mala Triglavca (mesna in mlekarska živinoreja) ter naselbina Moverna vas z dolgo stratigrafsko sekvenco (kompleksno poljedelstvo in živinoreja). Različne tipe najdišč je bilo mogoče povezati z raznolikimi dejavnostmi in raznoliko uporabo keramičnih posod prek ohranjenih biomarkerjev. Analiza razmerja stabilnih izotopov glavnih maščobnih kislin v keramičnih ekstraktih je potrdila prisotnost mesnih in mlečnih maščob glavnih domestikatov kakor tudi navzočnost lipidnih biomarkerjev rastlinskega izvora, ostanke čebeljega voska in smole. KEY WORDS - Neolithic; Eneolithic; lipid residue analysis; pottery; stable isotopes; birch bark tar; beeswax Introduction Archaeological research has benefited greatly in the past twenty years from an exponential increase in interdisciplinary studies incorporating analytical sciences. Two major fields of archaeological investigation, predominantly in prehistoric periods, have been trying to understand past diets and the mobility of populations by analysing osteological material and ceramics. The porous surface of these two commonly found archaeological artefacts enables * author for correspondence organic molecules such as lipids, proteins and nucleic acids to become entrapped and preserved through millennia. Unglazed pottery has proved to be an ideal analytical medium: on the one hand, it readily absorbs organic compounds during cooking, food storage and consumption, while it also serves as an indicator of past lifestyles, kinship, animal husbandry practices, DOI>10.4312\dp.41.9 149 Lucija Sober!, Milena Horvat, Andreja Žibrat Gašparič, Marko Sraka, Richard Evershed and Mihael Budja agriculture, trade or ritual practices (Boast2002; Gibson 2002). Although organic molecules are prone to degradation processes during pottery use or during the post-depositional period, it has been found that adequate concentrations of lipids can be preserved either as absorbed residues or visible food crusts and retrieved through organic solvent extraction (Heron, Evershed 1993; Ever-shed 2008; Craig 2004; Saul et al. 2013). Sites selection Among the various Slovenian Neolithic and Eneolithic sites available, three were chosen for lipids analyses (Fig. 1). The two with the longest settlement sequence, i.e. Mala Triglavca and Moverna vas, are embedded in different environmental and cultural contexts. The third, Ajdovska jama, is a burial site with strong evidence of burial ceremonies and rituals. The Mala Triglavca rock shelter is located on the Dinaric Karst in south-western Slovenia, 15km from the Northern Adriatic coast. The AMS 14C dates show a long sequence of human activities from the 8th to the 3rd millennium calBC, combined with natural and geomorphological post-depositional disturbances. The Moverna vas open-air site is situated in the karstified Bela Krajina region in the south-eastern part of Slovenia. The settlement sequence spans approximately two millennia from the 5th to the 3rd millennium calBC. The Ajdovska jama cave site lies within the catchment of the Sava River in south-eastern Slovenia. The site is well known for its burials. The human remains at the site occurred as distinct Fig. 1. A map of Slovenia showing the locations of archaeological sites investigated (adapted from National Museum of Slovenia). clusters of mainly disarticulated bones belonging to at least 31 individuals. The cave was used for burial and related ritual practices in the late 5th and early 4th millennium calBC. Moverna vas The Neolithic and Eneolithic settlement sequence at Moverna vas consists of nine settlement phases. Phases 2 to 6 were recognised as Neolithic, and phases 7 to 9 as Eneolithic (Budja 1989; 1994). Bayesian modelling (Fig. 2) shows that the sequence spans approximately two millennia, with continuous occupation from 4945-4810 calBC to 4270-4135 calBC and discontinuous occupation until 2905-2800 calBC (at 68.2% probability) with possibly centuries-long breaks in occupation (Budja 1994; Sraka 2013). The chronology is largely based on AMS 14C dates from carbonised organic residues adhering to interior pottery surfaces. Chemical analyses of these residues show that they are either charred remains of food Sample Name 14C Con- Calibrated age Calibrated age A13C Material Context Phase Lab code ventional age (BP) acc. to 68.2% prob. (calBC) acc. to 95.4% prob. (calBC) (meas. on AMS) Reference 23MV food crust 053.1 3 Poz-21396 5750±40 4450-4350 4460-4335 -24.9±0.5 Sraka 2013.App. 24MV birch bark tar 050.2 4 Poz-21398 5550±40 4540-4455 4615-4370 -20.6±0.3 Sraka 2013.App. 25MV birch bark tar 050.1 4 Poz-21399 5630±40 4715-4605 4770-4540 -24.2±0.2 Sraka 2013.App. 26MV birch bark tar 022.1 5 Poz-21400 5610±40 4940-4805 4995-4785 -24.2±0.6 Sraka 2013.App. 27MV birch bark tar 050.1 4 Poz-21401 5620±40 4495-4370 4530-4360 -20±0.4 Sraka 2013.App. 28MV birch bark tar 050.2/056 2 Poz-21402 5990±40 4490-4365 4520-4355 -22.3±0.7 Sraka 2013.App. 29MV food crust planum 7 2 Poz-21403 5800±40 4505-4370 4540-4365 -21.6±1.8 Sraka 2013.App. 151MV birch bark tar 031.4 6 Poz-21404 5670±40 4450-4350 4460-4335 -19.1±0.5 Sraka 2013.App. 152MV birch bark tar 050.2 4 Poz-21420 5550±40 4680-4545 4705-4500 -22.9±0.5 Sraka 2013.App. Tab. 1. 14C dates obtained from organic remains on pottery for Moverna vas (see also Fig. 10). Fig. 2. Moverna vas stratigraphical sequence with Bayesian statistical modelling of radiocarbon dates. (23MV, 29MV; App. 1; Tab. 1) or birch bark tar (24MV-28MV, 151MV, 152MV; App. 2; Tab. 1; Fig. 10). According to the results of chemical analyses, no freshwater reservoir effect is to be expected for these dates. Both the food crust and birch bark tar samples are considered as reliable samples with minimal inbuilt age (Hedges et al. 1992; Oinonen et al. 2010). During the continuous occupation in the 5th millennium, two related changes in 4325-4265 calBC (at 68.2% probability) have been observed. While the transition from Neolithic to Eneolithic vessel types and pottery fabrics was observed in the pottery assemblages (Tomaž 1997), the changes in settlement pattern relate to settlement fragmentation and settlement extension within the site-catchment areas, as well as in previously uninhabited areas (Budja 1995). The pottery samples selected for lipid analysis were embedded in Neolithic settlement phases 2 to 6 (c. 4945-4265 calBC) (Figs. 2, 4). The ceramic vessels of these settlement phases include various types of pot (Fig. 3.type 4, 5, 6, 8, 9), dishes with spouts (Fig. 3.type 1), pedestal dishes (Fig. 3.type 7), small pots (Fig. 3.type 3), bowls (Fig. 3.type 2), and ladles (Fig. 3.type 1O). Most of the pottery was fired in an oxidising atmosphere and well made, with burnished surfaces and red or brown slips applied to the sur- face. The vessels were made with homogenous clay fabrics and abundant quartz grain inclusions, which in some samples can even be interpreted as added temper {Tomaž 1997; 1999; Žibrat Gašparič 2008). Mala Triglavca The Neolithic and Eneolithic sequence at the Mala Triglavca rock shelter consists of 23 occupational levels, ranging from c. 5600 to 3500 calBC. The lipid analyses of the pottery assemblage, which is comprised mainly of various types of bowls, beakers, dishes and pots have been published (Soberl et al. 2008; Budja et al. 2013) and will be used here mainly in relation to other sites in the discussion. The pottery samples were taken from Neolithic occupational levels and can be linked according to their morphology and technology to the Vlaska pottery group (Barfield 1972; Žibrat Gašparič 2004). The oldest pottery fragments appear as early as 56165525 calBC. For the lipid analysis, we sampled 65 vessels from contexts that range from 5480 to 4261 calBC (68.2% probability). The results indicate an extensive mixing of ruminant and non-ruminant, and ruminant adipose and ruminant dairy fats in individual vessels. In some vessels, the presence of molluscs, crustaceans and freshwater fish was detected. Thirty per cent of the sampled pottery contained lipids characteristic of dairy fats, indicating Fig. 3. Moverna vas pottery types represented within the different settlement phases. Types 1-10 were-analysed for organic residues. See Appendix 1. that the processing of dairy products in pottery vessels was quite extensive. The use of dairy products at Mala Triglavca is embedded in the time span between 5467-5227 calBC (for details see Budja et al. 2013). Ajdovska jama Excavations in Ajdovska jama proved that the cave was an eminent site at the end of the Neolithic period, with traces of temporary human activity until the High Middle Ages. Ajdovska jama is the funerary site with the oldest excavated burials in Slovenia, and a place where the remains of the dead were worshipped. The cave is also a natural karstic phenomenon, which might have had a symbolic meaning for prehistoric people. The most typical grave goods of individual groups of burials that were excavated in the central hall and the left corridor included pottery (i.e. pot, dish, jug and ladle), jewellery (i.e. necklace or bracelet), and tools or weapons (i.e. axe, awl). The grave goods were found alongside the bodies of the deceased and prove that rituals were performed at the time of subsequent burials and visits to the cave. Food and meat were also placed beside the bodies as offerings. Analyses of plant and animal remains from the burials showed that cereals (e.g., wheat, barley and a type of bean) and the meat of domestic animals (i.e. ovicaprids, cattle) as well as wild animals (i.e. rabbit, wild boar, red deer, fox) were cooked (Horvat 1989). Additional information on diet came from the analyses of carbon (iSC) and nitrogen (15N) isotopes in collagen obtained from human and animal bones. The results show that the people of this community consumed mostly meat and plant protein coming from C3 dietary source (Ogrinc, Budja 2005; Bonsall et al. 2007). Bayesian chronological modelling of 14C dates provided by Clive Bonsall et al. (2007) shows that the burials belong to a relatively Fig. 4. Vessels from Moverna vas that were analysed for organic residues. short time interval of a few human generations from 4340-4290 to 4295-4235 calBC (at 68.2% probability). A collection of 52 pottery samples was selected for lipid residue analysis, including various types of pots, dishes, dishes with spouts, pedestalled vessels, bowls and jugs (Fig. 5). Most of the vessels were fired in an oxidising atmosphere and were made with various fine-grained quartz fabrics (Horvat 1989; Os-terc 1986). Organic residue analysis Cooking and processing organic commodities enables insoluble lipid residues to be absorbed into porous ceramic matrix and preserved for several thousand of years in the form of surface or/and absorbed residues. Cooking vessels have proved to be the most convenient for analysing organic residues due to their constant everyday use and exposure to high temperatures during cooking. However, non-culinary related vessel use can also absorb lipids when fatty commodities are stored: from the use of various sealants to reduce the permeability of the unglazed ceramic surface (resin, tar, pitch, milk and beeswax) and from the use of adhesives to repair broken ves- sels (Charters et al. 1993a; Regert, Rolando 2002; Regert 2004). When determining the functionality of pottery, numerous archaeological methods can be employed, including written and pictorial evidence, the use of archaeological contexts, information obtained via ethnographical comparisons, pollen analysis of visible organic remains, use wear analysis and the analysis of preserved contents (Orton et al. 1993; Rice 1987; Tite 2008; Skibo, Feinman 1999). Prudence Rice (1987) divided the principle functions of pottery into three categories: (i) storing dry substances; (ii) carrying liquids; and (iii) heating the contents over fire. Direct evidence for storage vessels apart from their larger size is not readily available, cooking pots offer some additional indices, i.e. carbonised visible remains adhering to outer or inner pot surfaces and signs of sooting. Chemistry offers interpretative tools for use in cases with a complete absence or selective preservation of organic and biological remains, such as osteological assemblages or plant remains; or for activities that are archaeologically difficult to trace, such as beekeeping. The primary focus of lipid research in the past 20 years has been to identify various biomar- Fig. 5. Vessels from Ajdovska jama that were analysed for organic residues. kers connected to specific domestic activities and ancient diets, and above all, identifying landmark transitions in ancient economies. These transitions include examples such as horse domestication (Outram et al. 2009), the earliest dairying practices in Europe, the Near East and Africa (Copley et al. 2005c; Craig et al. 2005; Evershed et al. 2008b; Dunne et al. 2012; Salque et al. 2013; Cramp et al. 2014);, the chronologically and typologically diverse importance of pig exploitation (Mukherjee et al. 2007) and the evidence of geographical dependence on marine food sources (Copley et al. 2004b; Hansel et al. 2004; Evershed et al. 2008d; Craig et al. 2011; Cramp et al. 2014; Cramp, Evershed 2014). The components of the lipid extracts of such residues can be identified and quantified by solvent extraction and a combination of analytical techniques that can achieve molecular level resolution, i.e. high temperature-gas chromatography (HTGC), GC/mass spectrometry (GC/MS; Evershed et al. 1990) and GC-combustion-isotope ratio MS (GC-C-IRMS; Evershed et al. 1994; 1999). Furthermore, modern cooking experiments have helped to understand the accumulation of lipids caused by different cooking practices, vessel use and preservation. If we take into consideration that an average concentration of preserved lipids in archaeological pottery is around IGG^g g-1, it is quite clear that only 1% or less of the original concentration survives post-depositional degradation (Evershed 2008). The initial lipid absorption also depends on the lipid content of processed food (animal vs. plant products) and modes of food preparation or storage. Variations in long-term lipid preservation can also occur due to differences in fabric types. Animal fats are by far the most common class of residue identi- fied from archaeological pottery with compound-specific stable carbon isotope analysis, allowing the identification of different animal fats, e.g., ruminant and non-ruminant adipose fats and dairy fats (Dudd, Evershed 1998), as well as the identification of the mixing of commodities (Charters et al. 1995; Ever-shed et al. 1999). Materials and methods Lipid analyses were performed with established protocols that are described in detail in earlier publications (Evershed et al. 1990; Charters et al. 1993b). The identification of individual compounds was based upon eluting order, a comparison of retention times to standards and by comparing the mass spectra with known fragmentation patters and NIST spectra library. In summary, after cleaning the potsherd surface, a 2g fragment was ground to a fine powder and extracted using a mixture of chloroform and methanol (2:1 v/v). An aliquot of the obtained total lipid extract (TLE) was trimethylsilylated and analysed directly by HTGC. Structure elucidation and molecular identification was achieved by GC-MS and HTGC-MS analyses. Fatty acid methyl esters were prepared by saponification of a TLE aliquot with BF3/methanol to enable compound-specific stable isotopic determination by GC-C-IRMS. The addition of an internal standard of known concentration (n-tetratriacontane, 1mg mL-i) enabled the calculation of extracted lipid concentration. The discussion of recovery rates refers to the proportional number of pottery extracts with an appreciable preserved li-pid concentration (>5^g g-1), which was determined as the lowest acceptable lipid concentration that can be reliably attributed to and interpreted as remnants of ancient food processing rather than modern contamination (Evershed et al. 1999; Evershed 2008a). Visible surface residues were scraped from the ceramic surface with a clean scalpel, ground to a fine powder and extracted as described above; again an internal standard was added for lipid quantification. A total of 179 potsherds and visible residues were selected for organic residue analysis: 52 samples from Ajdovska jama, 36 samples from Mala Triglavca and 91 samples from Moverna vas site. Potsherds were selected to represent different occupational phases and human activities at each site. Visible residues were sampled and analysed separately. To avoid duplication, where visible residues were present they were labelled with the number 1, while the originating potsherd extract was labelled with the number 2. Results Neolithic and Eneolithic pottery from Ajdovska jama, Mala Triglavca and Moverna vas showed a very good lipid preservation, with an overall 53.6% of potsherds analysed yielding an appreciable lipid concentration. The preservation of lipids in pottery is heavily influenced by the alterations that may occur during vessel use or due to post-burial conditions in the soil, as well as the use of ceramic vessels during their lifetime (Evershed et al. 1999; Ever-shed 2008a). These factors could explain the variations observed in average lipid concentrations and recovery rates between sites: the pottery assemblage from Mala Triglavca yielded the least TLE extracts, with appreciable lipid concentrations (30.6%), followed by 48% of pottery from Ajdovska jama yielding lipids, while 65.9% of the analysed pottery from the Moverna vas site showed preserved organic residues. This trend is also repeated in observed median lipid concentrations from potsherd extracts as well as lipid concentration ranges. For a better demonstration of different concentration ranges, these are plotted as box-and-whiskers plots in Figure 5. Since, generally, only lipid concentrations higher than 5^g g-1 are considered as appreciable and can therefore be interpreted as archaeological, lipid concentrations below this threshold were ignored in the following comparisons (see Fig. 6 and Tab. 2). The observed lipid concentration ranges are considerably narrower in the ceramic assemblages of Mala Triglavca and Ajdovska jama than those from Moverna vas. Since the latter site was a fully developed, permanent settlement, in contrast to the occasionally used rock shelter and burial cave, higher li-pid concentrations could indicate frequent daily use of ceramic vessels resulting in an accumulation of residues. The organic residues in the investigated pottery showed compound distributions typical of animal fats and plant material degraded to various degrees. The parent triacylgycerols (TAGs) present in fresh adipose fats and plant oils quickly degrade into their constituent fatty acids, with the palmitic (C16:o) and stearic (C18:o) fatty acids persisting in highest abundance, and with minor contributions from shorter chain saturated fatty acid components. Many vessels yielded only free fatty acids, indicating that complete hydrolysis of the precursor TAG components had taken place. Two gas chromatograms representing differing degrees of degradation and compounds most commonly identified in the Neoli- thic and Eneolithic residues analysed can be seen in Figure 7. Fatty acids are usually present in the greatest abundance in archaeological lipid extracts with even rather than odd carbon number preference, dominated by palmitic (C16:0) and stearic (C18:0) fatty acids. While animal fats generally display a greater abundance of stearic acid, the plant derived lipids show a predominance of palmitic acid (Dudd 1999; Copley et al. 2005a; Romanus et al. 2007). The presence of odd carbon number free fatty acids (e.g., C15:0, C17:0, C19:0) together with their iso- and anteiso-bran-ched variations may indicate ruminant animal sources, as these compounds are biosynthesised by the bacteria living in the rumen (Mottram et al. 1999; Evershed et al. 2002). Despite their predominance, the C16:0 and C18:0 fatty acids possess only limited biomarker potential. Broad groups of commodities can be alluded to only by investigating the C16:0 vs. C18:0 fatty acid ratio (P/S ratio). Previous investigations of P/S ratios in modern reference materials have provided some additional proxies; however, interpretations of these have to be applied with great caution and only in combination with other data, i.e. TAG distributions and 5i3C values. Calculated P/S ratios for pottery extracts from investigated sites are shown in Figure 8. Previous studies have reported a P/S ratio <1.3 as indicative of ruminant adipose fats; a P/S ratio of approx. 2.2-2.9 and 4.9 indicative of dairy fats or non-ruminant adipose fats, while a P/S ratio between 4.0 and 9.4 has been reported for commercial olive oils (Dudd 1999; Copley et al. 2005a; Romanus et al. 2007). P/S ratios calculated for TLEs of Slovenian pottery (Fig. 8) show a large proportion of 53 lipid extracts (68%) falling below the 1.3 mark, indicative of ruminant adipose fat; 24 extracts (31%) displaying the range 1.3-4.0, attributed to either rumi- Labels Ajdovska Mala Moverna jama Triglavca vas Min 5.02 5.53 5.25 Qi 8.26 10.81 18.03 Median 32.45 21.93 118.18 Q3 79.25 65.95 503.45 Max 557.13 173.35 3308.10 IQR 70.99 55.14 485.42 Upper Outliers 3 1 7 Tab. 2. Details of absorbed lipid concentration ranges in analysed pottery. Fig. 6. Box-and-whiskerplots showing the range of preserved appreciable lipid concentrations in pottery from Ajdovska jama, Mala Triglavca and Mo-verna vas. Only concentrations higher than >5vgg-1 were used. nant dairy or non-ruminant adipose fats; only 1 extract (1%) displays a P/S ratio higher than 4.0, indicative of olive/plant oils. The presence of ruminant-derived lipids has also been confirmed by observed distributions of odd carbon number saturated fatty acids with their branched iso- and anteiso- homologues (C15:0, C15:0br, C17:0, C17:0br), biosynthesised by the bacteria living in the rumen (Dudd et al. 1998; Mottram et al. 1999; Vlaemnick et al. 2006). These branched fatty acid biomarkers were found in ten potsherd extracts: 08MT, 18MT, 75MT, 87MT, 23MV-2, 98MV, 134MV, 149MV, 153MV and 154MV. Apart from C16:0 and C18:0 fatty acids, a series of saturated long-chain fatty acids (LCFA) with a carbon number range between C20 and C30 has also been identified in fifteen potsherd extracts, representing 8% of the total assemblage: 03AJ, 37AJ, 69AJ, 70AJ, 18MT, 29MV-2, 91MV, 99MV, 102MV, 111MV, 114MV, 121MV, 147MV, 149MV AND 154MV. Such a series of LCFA has previously been associated with two potential sources, depending on the accompanying compounds. If found in combination with isopre-noid fatty acids such as phytanic or pristanic acid, 4,8,12-trimethyltridecanoic acid or w-(o-alkylphenyl)-alkanoic acids, preserved lipids are most likely derived from marine organisms (Copley et al. 2004b; Fig. 7. Partial HTGC profile of the trimethylsilylated total lipid extract from potsherds 18MT (Mala Triglavca) and 110MV (Moverna vas) illustrating the contrasting distribution of compounds characteristic of partially and fully degraded animal fat. Key: FAX:Y are saturated free fatty acids of carbon length x and degree of unsaturation y. IS is the added internal standard; MAGs are monoacylglycerols; DAGs are diacyl-glycerols; TAGs are triacylglycerols. Hansel et al. 2004; Evershed et al. 2008c). LCFA extracted from Slovenian Neolithic and Eneolithic pottery, however, occur in high frequency together with long-chain n-alcohols of C22 to C32 even-carbon number series and analogous odd-carbon number n-alkane series of C23 to C33 chain length, which are more characteristic of degraded plant waxes (Tulloch 1976; Bianchi 1995). Mid-chain ketones have been identified in six residues derived from five body sherds and one rim sherd (02AJ, 04AJ, 72AJ, 29MV-2, 91MV, and 133MV), most frequently displaying a narrow distribution with C29, C31, C33 and C35 homologues. These bio-marker compounds are known to form by the condensation of fatty acids, involving decarboxylation and dehydration reactions occurring at high temperatures, typically in excess of 300°C (Evershed et al. 1995; Raven et al. 1997). The carbon chain length of ketones previously found in pottery extracts usu- ally ranges between C27 and C35, which reflects the length of the precursor fatty acids. These compounds have also been reported as components of the epicuticu-lar leaf waxes of higher plants (Tulloch 1976; Kolattukudy et al. 1976). However, the presence of unsaturated keto-nes was identified in two lipid extracts (02AJ and 72AJ), suggesting the unsatu-rated fatty acid precursors common in plant oils. A similar series of ketones was also reported to be formed during vigorous pyrolysis at temperatures reaching 800°C (Raven et al. 1997). Waxes Beeswax recovered from archaeological contexts can undergo various degrees of alteration; however, four major groups of compounds provide biomarkers for its presence: (i) long-chain alcohols (C24 to C32); (ii) odd-carbon number n-alka-nes (C25 to C33); (iii) a series of palmitic wax esters (C40 to C54); and (iv) hydroxy palmitic wax esters (C42 to C54). Similarly, plant waxes contain a mixture of compounds, including odd-carbon number n-alkanes (C21 to C37), monoesters ranging in chain length from C32 to C64 and long-chain alcohols with a chain length range between C22 to C34 (Tulloch 1976; Heron et al. 1994; Mills, White 1994; Charters et al. 1995; Regert et al. 2001). A relatively large proportion of preserved lipid residues (27%) showed traces of wax esters with chain lengths of C40 to C48, together with even-carbon number long chain alcohols (C22-C32) and odd-carbon number straight chain alkanes (C23-A33), which could either derive from diagenetically altered beeswax or degraded epicuticular plant waxes (Fig. 9). Wax esters in these potsherd extracts were predominantly found together with free fatty acids and their acylglycerol moities, suggesting that the vessels were used to process both leafy plants and animal products; whether they were processed simultaneously or separately cannot be elucidated from this data. Interestingly, a beeswax residue was identified in cup extract 125MV without any contributions from animal fats or plant waxes. A further seven potsherd extracts from three vessels (25MV, 26MV and 28MV) contained birch-bark tar biomarkers in conjunction with wax esters, indicating mixing of commodities. Recent experimental work reported by Dana Millson (2011) and Merryn Dineley (2000; 2011) has addressed the question of applying beeswax as a sealant, concluding that, although it is an effective waterproofing agent, it is not appropriate for use on cooking pots, causing the pot fabric to spall and flake off. Based on this, as honey would have been the earliest available natural sweetener, the beeswax residues identified in archaeological pottery could be interpreted as the remains of food processing that involved the addition of honey. Birch bark tar An unusual set of triterpenoid compounds was identified in 16 potsherd extracts from Moverna vas, representing seven vessels (24MV, 25MV, 26MV, 27MV, 28MV, 151MV and 152 MV) which had visible residues present on either the interior or exterior surface (Fig. 1G). Visible residues are a common find on archaeological pottery, and routinely used for radiocarbon dating. It has been previously assumed/assessed that the exposed nature and structure of visible residues are usually not a good medium for preserving organic molecules (Evershed et al. 1992; Evershed 2008). It was possible to assess this variation, because visible residues were sampled and extracted separately. Lipid concentration values differ quite significantly, with values for visible residues averaging at 1537.G4^g g-1, while absorbed residues displayed an average lipid concentration of 25.5^g g-1. The two sets of residues were also diffe- rentiated by the biomarkers extracted: visible residues showed the presence of lupa-2,2G(29)-dien-28-ol, allobetul-2-ene, lupenone, lupeol, betulone and betu-lin, which are characteristic of birch-bark tar. While betulin and lupeol are the predominant biomarkers present in birch-bark tar, other compounds are formed by degradation reactions, particularly the heating processes needed to produce the pitch. In particular, betulin is partly transformed into lupa-2,2G(29)-dien-28-ol by dehydration, whereas lupeol leads to the formation of a triterpenoid hydrocarbon identified as lupa-2,2-(29)-diene (Charters et al. 1993; Pollard, Heron 1996; Regert, Rolando 2002; Regert et al. 2003a: 2003b). Triacylglycerols Triacylglycerols, as the most abundant components of fresh animal fats and plant oils, can be useful indicators of lipid preservation and the extent of degradation. A comparison of TAG distributions with those of modern reference fats has shown that specific distributions can be linked to different lipid sources and enable the preliminary differentiation of their origins from the two major classes of domestic animals (ruminant and non-ruminant/porcine) and between ruminant dairy and adipose fats. Ruminant animals show a characteristic distribution of TAGs, with carbon numbers ranging from C44 to C54 with a maximum concentration at C52, whereas non-ruminant animals display a slightly shorter distribution with carbon numbers between C46 and C54 with a low concentration at C46 and C54 and a maximum again at C52. Dairy fats show the widest TAG distribution, with carbon numbers ranging from C42 to C54, usually with two maxima at C5G and C52 (Evershed et al. 1997; Dudd, Evershed 1998; Mottram et al. 1999). Triacylglycerol remains (including samples with only trace amounts preserved) were identified in thirty pottery lipid extracts, representing 17% of the total assemblage investigated. Quantifiable TAG distributions as detected in lipid extracts from Slovenian potsherds are represented in Figure 11. Fig. 8. Histograms representing the relative abundance ratios of palmitic (C16:0) vs. stearic (C18.0) fatty acid as detected in analysed potsherds. The dotted lines (set at 1.3 and 4) represent criteria as reported in the literature and used to separate ruminant adipose fats from non-ruminant, ruminant dairy fats and plant oils (Dudd 1999; Copley et al. 2005a; Romanus et al. 2007). TAG distributions detected in potsherd extracts seem to be predominantly derived from ruminant adipose fats, with only 5 extracts (18MT, 79MT, 159MT, 96MV, 143MV) possibly deriving from ruminant dairy Fig. 9. Partial gas chromatograms of the trimethylsilylated TLEs from pottery showing the various biomarkers detected: 116MV epicuticular waxes residue; 69AJ a mixture of beeswax and plant residue; 26-2MV mixture of birch bark tar and plant residue. Key: FAx:y are fatty acids where x is the carbon chain length and y is the degree of unsaturation; OHx are long-chain alcohols of carbon chain length x; Ax are aliphatic alkanes of carbon chain length x; Wx are wax esters with carbon chain length x; IS is internal standard; * are plasticisers. tion of compounds with lower carbon numbers, and thus come to resemble the narrower distribution seen in ruminant adipose fat TAGs distribution (Dudd, Evershed 1998; Aillaud 2001). Conclusions from TAG distributions have to be drawn with caution and serve only as preliminary results, complemented with compound-specific carbon isotope ratio measurements. Compound-specific stable carbon isotope analysis Compound-specific stable carbon isotope values (8i3C) were obtained for the palmitic (C16:0) and stearic (C18:0) fatty acid methyl ester derivatives (FAMEs) from 52 Neolithic and Eneo-lithic potsherd residues with sufficient lipid concentrations. In order to elucidate the origin of preserved lipids accurately, archaeological 8i3C values were compared with modern reference fats from animals reared on isotopically similar diets to those of animals in prehistory. To eliminate any isotopic variations occurring in animals through differences in dietary intake or environmental factors, the difference between 8i3C18:0 -813C16:0 values (Ai3C) is plotted in Figure 12. Ai3C values ranging from -3.3 to -6.3^ indicate ruminant dairy fats; values from 1.0 to 2.8^ represent ruminant adipose fats, while values from -0.7 to + 1.9^ indicate porcine adipose fats (Dudd, Evershed 1998; Evershed et al. 2008; Craig et al. 2011; Dunne et al. 2012; Salque et al. 2013). residues and with no TAG distribution indicating the presence of porcine fats. However, laboratory experiments have shown that TAG distributions can be skewed by degradation occurring during use or postdeposition, causing the wide TAG distribution characteristic of fresh ruminant dairy fat to become considerably narrowed due to the preferential degrada- Distributions of stable carbon isoto-pic values of lipids preserved in Neolithic and Eneolithic pottery show differences between individual archaeological sites: the residues recovered from Ajdovska jama pottery were predominantly of ruminant adipose (5 extracts) and ruminant dairy origin (4 extracts), while those from the Moverna vas pottery assemblage were mainly of ruminant adipose origin (17 extracts). The ubiquitous presence of dairy lipid residues in vessels from Mala Triglavca has already been reported, with 63% and 17% of vessels being used to process or store dairy products, respectively (Šoberl et al. 2008; Budja et al. 2013). The lowest occurrences were of porcine derived lipids, being found on only one potsherd from Ajdovska jama and three potsherds from Moverna vas. The mixing of various commodities throughout the life of vessels can also be seen by 5i3C values plotting close to, or between, the ranges of modern reference fats. It has been assumed that the pottery extracts with minor concentrations of leaf waxes or beeswax components present still reflect the isoto-pic signature of predominant fatty acids present in the residues. Discussion Pottery use in different contexts Pottery has been traditionally regarded as a passive bearer of culture; however, with the rise of contextual archaeology, pottery has come to be seen more as an active factor, brought about by human agency and used in the construction of social identity (Boast 2002; Gibson 2002). Ceramic vessels could be used for many primary functions, such as the preparation, storage and cooking of food, brewing, tanning, dairying, dyeing, fulling, textile washing, transporting and salt preparation. Whatever pottery was used for, it was an important artefact, as demonstrated by its appearance at domestic sites, as well as within ritually structured deposits. Pottery deposited in funerary settings could consist of previously used vessels or one made deliberately for that purpose. Fig. 10. Potsherds from Moverna vas with visible residues, remnants of birch bark tar application or production. Although pottery is very robust and able to survive, it is also very sensitive and responsive to cultural, social, economic and ideological changes. These can be mirrored in a variety of ways: decoration, design, typology, modes of use and deposition. Ajdovska jama The ceramic vessels recovered from the Ajdovska jama site formed part of Neolithic burial rituals, acting as grave goods or simply containers for food offerings. Lipid preservation in ceramic vessels was good, with almost half of the potsherds (48%) yielding an appreciable amount of organic residue. The variety of animal remains deposited with the burials is well reflected in preserved fatty acid composition and isotopic signatures, indicating that ceramic vessels predominantly contained ruminant animal products (meat and dairy), while only one vessel showed the presence of porcine fat. The presence of mid-chain ketones in three pots (02AJ, 04AJ, 72AJ), formed by the condensation of precursor fatty acids at high temperatures in the presence of clay, suggests these vessels were used as cooking pots (Fig. 5). The extraction of uncommon unsaturated mid-chain homologues in 02AJ pot could be the result of processing plant material which contains high concentrations of unsaturated fatty acids. This was also suggested by the extracted organic residues, which in combination with the excavated plant remains (burnt, scattered cereal grains and pulses), show a high contribution of a plant-based diet, with approx. 25% of vessels containing some plant biomarkers. A mixed diet of plants and animals was also attested in bulk stable isotopic determinations (5i3C and 5i5N) of collagen extracted from osteo-logical remains recovered from the burials (Ogrinc, Budja 2005; Bonsall et al. 2007). However, enriched 5i3C values of palmitic acid extracted from lipid residues in ceramics (Fig. 12) could indicate a C4 or marine component in the animal-based diet, as they are strongly diet-dependent (Copley et al. 2003). Since a marine dietary contribution seems unlikely in the case of Ajdovska jama, enriched 5i3C16:0 values could have been introduced via animals eating plants from a waterlogged environment (Salque et al. 2012). This observed difference between Ajdovska jama, Mala Triglavca and Moverna vas isotopic values Fig. 11. Histograms showing triacylglycerol (TAG) distributions detected in pottery lipid extracts from Ajdovska jama, Mala Triglavca and Moverna vas. TX denotes the number of acyl carbon atoms in individual TAGs, grey bars represent TAGs identified in modern adipose and dairy fats while those in white are usually found only in dairy fats. was also confirmed statistically with a two-tailed student's T-test which returned probability values of 0.003 and 0.016. Mala Triglavca Rock-shelters such as Mala Triglavca were used as gathering places for Mesolithic populations, and some could have been subsequently transformed into shelters and pens for domestic animals during the Neolithic. An analysis of herd structure and mortality on faunal remains (sex and age of animals) can be used to produce 'kill-off curves' in order to distinguish between meat or dairy animal exploitation (Payne 1973). Kill-off curves from Neolithic sites in the Northern Adriatic region have been interpreted in two ways: while Preston Miracle, Staso Forenbaher and Laura Pugsley believe herds of domestic animals were kept predominantly for dairying, Dimitrij Mlekuž suggests simple, non-optimised animal husbandry (Miracle, Forenbaher 2005; Miracle, Pugsley, 2006; Mlekuž 2005; 2006; Bonsall et al. 2013; Rowley-Conwy et al. 2013). AJDOVSKA JAMA MALATRIGLAVCA Predominantly a. .Q. ■a ro Increasing C4 diet and/or marine component Aj68 o" -3 -5 ■ -30 •20 16:0 ' J MOVERNA VAS 3 Predominantly Increasing C4 diet and/or w -| ^ Cjdiet marine component s D) Q> ix 0 ' 1 Q. MV121* ,MV124 MV109« ...................AiM^liij,, ,,, ..................."W11V ■' " ■ ~ (/> - — -1 c 2 -1 ^ ' _ -5 ^ plant bio ma liters biomarktrs 1 plant «viaxblomartters -30 ■20 16:0 ^ J CO O ber aliphatic alkanes, even carbon number long-chain alcohols and wax esters were detected in three potsherds (08MT, 13MT, 79MT), indicating a degree of mixed commodities (meat as well as vegetables) being processed within these vessels. Moverna vas The Neo-Eneolithic settlement of Moverna vas had fully developed animal husbandry with agriculture, as well as diverse pottery production. The complexity of this settlement was mirrored perfectly in the lipid biomarkers extracted from the ceramic vessels. The 99 potsherds analysed covered a diverse vessel typology, from large cooking and storage pots to small 'drinking' cups and highly specialised pedestal dishes. Intensive use of ceramic vessels in food preparation and storage is reflected in the highest lipid concentration range (Fig. 6) and the presence of mid-chain ketones identified in three potsherds (29MV-2, 91MV, 133MV) (Fig. 4). Extensive mixing of commodities (meat and plants) is apparent from extracted lipid biomarkers, in which not only free fatty acids were identified together with their parent acylglycerol moieties, but also a suite of other compounds, i.e. aliphatic alkanes, long-chain fatty acids, long-chain alcohols, triterpenoids and wax esters. In the absence of faunal remains, compound specific stable isotope analysis of palmitic and stea-ric fatty acid enabled us to approximately reconstruct animal husbandry practices. While 5i3C values for C16:0 and C18:0 extracted from ceramic vessels found at Ajdovska jama and Mala Triglavca sites showed the ubiquitous presence of ruminant meat and dairy products, the potsherds from Moverna vas settlement contained predominantly ruminant and porcine adipose lipids (Fig. 12). Only seven potsherds revealed the presence of milk residues (23-2MV, 91MV, 93MV, 96MV, 99MV, 102MV, 150MV) (Fig. 4). An elusive association of porcine products with prehistoric pottery has been observed in the past, especially in British Neolithic pottery (Mukher-jee et al. 2007) as well as two recently investigated Slovenian Neolithic pottery assemblages from Ma-harski prekop and Resnikov prekop. While porcine derived lipids were detected in extracted residues at Resnikov prekop, the same class of foodstuff was completely absent from Maharski prekop (Ogrinc et al. 2012; Mlekuž et al. 2012; 2013). The discrepancy in preserved porcine lipids and faunal statistics may be the result of alternative ways of preparing porcine meat that did not necessarily involve pottery, but perhaps spit-roasting, as suggested by Umberto Albarella and Dale Serjeantson (2002). Pottery use within typology The ubiquity of pottery finds in all archaeological sites shows indirectly that this was a commodity produced en masse and used daily, not simply made for display or burials. From the perspective of pottery typology, it is only assumed which vessels were used for storing and/or cooking food. Investigations of British Neolithic and Bronze Age pottery revealed correlations between specific commodity groups and three main differential criteria: (a) pottery size/rim diameter; (b) pottery typology, and (c) various household activities (Copley et al. 2005c; 2005d). Similarly, biomarkers for a specific commodity, dairy products in this case, were detected in Neolithic ceramic sieves in Europe, which were in turn interpreted as cheese strainers (Salque et al. 2013). Lipid residue analyses of pottery from Ajdovska jama, Mala Triglavca and Moverna vas have shown some correlations between lipid concentrations and pottery typology (Figs. 4, 5 and 13), while only two correlations between specific commodities and vessel types have been observed. Mid-chain ke-tones, which are used as biomarkers for exposure to high temperature (cooking), were observed in only three vessel types, all characterised either by larger volumes or openness of rims: pots, bowls and dishes. Pots and pedestal dishes were also unique ceramic types associated with birch-bark tar biomarkers. Rice (1987) divided the principle functions of pottery into three categories: (i) storing dry substances; (ii) carrying liquids; and (iii) heating contents over fire. The investigation of potsherd samples taken from different parts along the profile of the same ceramic vessel compared to laboratory cooking simulation experiments has shown correlations between concentrations of absorbed lipids, their spatial distribution and different modes of pottery use. The hydrophobic nature of lipids and their lower density results in the highest lipid concentrations to be absorbed near the top of the vessel, where the original water line would have been (Charters et al. 1997). Other lipid distributions observed in the bases of vessels are thought to indicate an analogous preparation of food, namely roasting, or the application of surface sealing treatments (Charters et al. 1993b; 1997). The average lipid concentration profiles in Figure 13 were divided into rim, body and base sherds to assess potential variations in distinguishing pottery use. Investigated pottery from Ajdovska jama, Mala Triglavca and Moverna vas shows distinct differences in vessel use: while average lipid concentration in cups peaks in the upper parts of the vessels, suggesting preferential absorption of immobilised li-pids, an opposite concentration distribution was observed for pots and jugs, where the highest concentration in the lower vessel parts could indicate 'dry' cooking. Average lipid concentration poses an interesting question as well; accepting that lipid accumulation correlates with the longevity of vessel's use, it is clear from Figure 13 that pedestal dishes, small cups and Fig. 13. Diagrams showing the mean concentration of extracted lipids according to ceramic typology and potsherd location. pots with the highest preserved lipid concentrations (935, 269 and 237^g g-1, namely) were probably used regularly to process or store fatty foodstuffs over an extended period. On the other hand, bowls, jugs and dishes were perhaps used only as storage vessels for less fatty commodities, or were perhaps dedicated serving vessels. An estimate of the longevity of cooking pots in regular use ranges between three months, one year and even longer periods of two to ten years (Foster 1960; David 1972; DeBoer 1974; Rice 1987; Longacre 1991). Birch-bark tar - a multi-purpose widespread prehistoric commodity Similar to beeswax, resins have also been shown to have had various potential applications in prehistory: as adhesives (Charters et al. 1993a; Regert et al. 2003b), for medicinal use (Lucquin et al. 2006; Evans, Heron 1993), as a waterproofing agent (Ever-shed et al. 1985; Robinson et al. 1987; Romanus et al. 2009) in pitch and tar production (Eerkens et al. 2002) or perhaps in wine production (McGovern et al. 2009). The presence of birch-bark tar has been widely reported from various prehistoric archaeological contexts, where it was mainly used as hafting adhesive on arrowheads or as a material used to repair broken ceramic vessels as early as the Neolithic (Pollard, Heron 1996; Regert, Rolando 2002; Regert et al. 2003b; Regert 2004; Lucquin et al. 2006). Birch-bark tar is sometimes also found as free lumps in sediment or in the form of visible residues on the exterior or interior surfaces of ceramic vessels (Charters et al. 1993; Bosquet et al. 2001; Urem-Kotsou et al. 2002; Regert et al. 2003; Lucquin et al. 2006). Birch-bark tar was only identified as a visible organic residue on pottery from Moverna vas, where it was linked specifically to pedestal dishes and pots. Pedestal dishes have been previously reported together with this natural product from Neolithic funerary contexts in Brittany (Lucquin et al. 2006), where the authors interpreted these vessels as 'incense burners' or portable hearths. As the smell of burning tar is quite unpleasant, it has been suggested that it might have been used to mask strong odours, such as decomposing bodies in funerary contexts (ibid.). This theory could explain the find of a small, black, amorphous lump of tar within the burial sediments in Ajdovska jama, where burial rituals were similar to those described above (Šercelj, Culiberg 1984). The presence of this natural substance has also been reported from the Urnfield culture cemetery at the Slovenian Academy of Sciences and Arts in Ljubljana (Pus 1976; Hadzi, Cvek 1976; Hadzi, Orel 1978) and the Neolithic pile dwelling site at Maharski prekop (Hadži, Orel 1978). The availability of birch trees in prehistory has also been confirmed by pali-nological analysis of contemporary regional sediments, where a decline has been recorded after 6400 cal BP with the increase of 'anthropogenic indicators' (Andrič 2007). Conclusions The organic residue analysis of the Neolithic and Eneolithic pottery from Ajdovska jama, Mala Triglavca and Moverna vas showed very good lipid preservation, enabling us to reconstruct the past pottery use and address potential contextual differences. The choice of three sites with very diverse archaeological contexts has proven to be justified, as the vessels retained varying lipid concentrations, probably depending on their originating contexts. Pottery from Mala Triglavca rock shelter yielded the lowest lipid recovery (30.6%) as well as the lowest lipid concentration range, which together with the absence of mid-chain ketones identified might suggest less intense food processing, without heating, or a faster turnover in pottery use. Lipid biomarkers confirm the archaeozoological data, i.e. the presence of domesticated ovicaprids, which were exploited for both meat and dairy products, occasionally mixed with plant-based foods as indicated by biomarkers. The Ajdovska jama pottery that played a part in prehistoric funerary rituals proved to retain 48% of vessels with identifiable lipid residues. Identified bio-markers reflect the animal remains that were deposited with the deceased, suggesting a mixed plant and animal based diet. The compound specific stable isotopic analysis of primary fatty acids suggests that the lipids derive from ruminant animals (meat and dairy) and one porcine fat residue, most likely a remnant of wild boar. A high occurrence of plant biomarkers (25% of the pottery assemblage) in conjunction with recovered palaeobotanical remains suggests that a large proportion of the cave visitors' diet or food offerings were plant based. The highest lipid recovery rate (65.9%) as well as the broadest lipid concentration range of Moverna vas settlement pottery can be interpreted as an indication that prehistoric ceramic vessels were used frequently to process or store foodstuff of animal as well as vegetable origin. The complexity of biomar-kers in ceramic vessels mirrors perfectly the complexity of a fully developed Neolithic and Eneolithic settlement economy. Ceramic vessels were used to process animal products (ruminant and porcine adipose fats) and plant-based foodstuffs, as well as more rare commodities such as beeswax (perhaps indicating the presence of honey) and birch-bark tar. Pots and pedestal dishes were unique ceramic types associated with birch-bark tar biomarkers, which were identified only on pottery from Moverna vas. Other prehistoric finds of birch-bark tar from Slovenian archaeological sites include a lump of tar in sediment from Ajdovska jama, and occurrences with pottery have been reported from other Neolithic and Bronze Age sites in Slovenia. The analysis of pottery typology and lipid residues showed that some vessels types can be linked to specific foodstuffs or food preparation techniques. Mid-chain ketones, biomarkers for exposure to high temperature, were observed only in vessel types of larger volume or openness of rim (i.e. pots, bowls and dishes). 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Sample # CHEM Sample # ARCH Site code SF # SE/rel. depth Sector/quadrant Description 01AJ 1 Ajdovska ama 1982 129a 42 LH\tunnel 1 body of a pot, bucket- shaped 02AJ 2 Ajdovska ama 1982 684 43 CDV\XXII, group 4 body of a pot 03AJ 3 Ajdovska ama 1982 567\2 43 CDV\XXII, group 4 body of a dish 04AJ 4 Ajdovska ama 1982 660 (2519) 43 CDV\XVI, group 4 body of a pot 05AJ 5 Ajdovska ama 1982 682 43 CDV\XVI, group 4 body of a dish 06AJ 6 Ajdovska ama 1982 146 44 LH\tunnel 1 body of a pot 07AJ 7 Ajdovska ama 1982 43 43 LH\tunnel 2 body of a pot 31AJ 8 Ajdovska ama 1976 208 43 LH\group 6 body of a pedestal dish 32AJ 9 Ajdovska ama 1982 70 \ DH\33 body with base of a dish, black residue on exterior 33AJ 10 Ajdovska ama 1986\87 633 43 CDV\XVIa, group 4 body of a pedestal dish, modern glue residue 34AJ 11 Ajdovska ama 1986 640 42 CDV\XXII upper body of a pedestal dish 35AJ 12 Ajdovska ama 1967 262 43 LH\group 6 base of a pedestal dish, traces of a red slip on exterior 36AJ 13 Ajdovska ama 1967 284 43 LH\group 6 body of a dish 37AJ 14 Ajdovska ama 1988 730 43 CDV\XXIVa, group 4 base with body of a spouted dish, yellowish residue perhaps on interior 38AJ 15 Ajdovska ama 1986 577 43 CDV\XVI, XIIa, group 4 rim of a spouted dish, black residue on interior, shiny surface - perhaps con-solidant? 39AJ 16 Ajdovska ama 1986 576 42 CDV\ XXIX\XXVIII< XXVIII rim of a dish, modern glue residue 40AJ 17 Ajdovska ama 1967 274 42 LH body of a spouted dish, modern glue present 41AJ 18 Ajdovska ama 1985-87 575 43 CDV\XXII,XXIIa, XXIX, group 4 rim of a dish 42AJ 19 Ajdovska ama 1985\86 635 43 CDV\XXIIa, group 4 rim of a bowl, modern glue present 43AJ 20 Ajdovska ama 1986 574 42 CDV\XVI rim of a dish, unusual surface - organic residue, limescale or consolidant? 44AJ 21 Ajdovska ama 1967 273 43 LH\group 6 body of a spouted dish 45AJ 22 Ajdovska ama 1967 245 42 LH body of a spouted dish , modern glue present 46AJ 23 Ajdovska ama 1982 122 42 LH\tunnel 1 rim of a dish with an applique decoration 47AJ 24 Ajdovska ama 1982 119 44 LH\group 1 body of a dish, ribbed decoration 48AJ 25 Ajdovska ama 1986 584 42 CDV\XXIX body of a bowl (by fireplace SE56), ribbed decoration 49AJ 26 Ajdovska ama 1985 583 43 CDV\XXII, group 4 rim of a bowl 50AJ 27 Ajdovska ama 1986 586 \ CDV\ X\IX,XV,XXIX body of a ribbed dish 51AJ 28 Ajdovska ama 1982\83 109 42 LH\tunnel 1 body of a spouted dish 52AJ 30 Ajdovska ama 1982 126 42 LH\tunnel 1 body of a bowl, bucket-shaped 53AJ 32 Ajdovska ama 1967 258 43 LH\group 6 body with base of a spouted bowl 54AJ 33 Ajdovska ama 1985 440 43 CDV\XVI,XXII, group 4 rim of a jug 55AJ 34 Ajdovska ama 1967 267 43 LH\group 6 body of a jug with a horizontal rib and incised decoration 56AJ 35 Ajdovska ama 1967 206 43 LH\group 6 base of a jug 57AJ 36 Ajdovska ama 1967 257 43 LH\group 6 body of a jug 58AJ-1 29 Ajdovska ama 1987 739 44 CDV\XXII,XXIIa,XVIa body of a pot, burnt residue on interior and exterior 58AJ-2 29 Ajdovska ama 1987 739 44 CDV\XXII,XXIIa,XVIa body of a pot, burnt residue on interior and exterior 59AJ 31 Ajdovska ama 1984 116 42 LH\tunnel 1 body of a pot, bucket-shaped 60AJ 37 Ajdovska ama 1985-87 743 43 CDV\XXII,XXIIa,XVI, group 4 rim of a pot with incised decoration Sample # CHEM Sample # ARCH Site code SF # SE/rel. depth Sector/quadrant Description 61AJ 38 Ajdovska jama 1986/87 756 43 CDV/XXIIa, group 4 two rims of a pot - one with a horizontal rib, one with criss-cross incisions 62AJ 39 Ajdovska jama 1985 737 43 CDV/XXII, group 4 body of a pot with horizontal incisions and a base of the handle (similar in Moverna vas assemblage) 63AJ 40 Ajdovska jama 1982 120 44 LH/group 1 three body fragments of a pot with a zoomorphic head 64AJ 41 Ajdovska jama 1984 385 83 CDV/XVIII rim with body of a pot 65AJ 42 Ajdovska jama 1987 641 43 CDV/XXIIa, group 4 body of a pot 66AJ 43 Ajdovska jama 1985 564 43 CDV/XXII, XVI, group 4 rim of a pot with vertical incisions 67AJ 44 Ajdovska jama 1985/86 455 43 CDV/XVI,XXII,XXIIa, group 4 base of a pot, painted decoration 68AJ 45 Ajdovska jama 1982 125 44 LH/group 1 body of a pot 69AJ 46 Ajdovska jama 1982 107 42 LH/tunnel 1 body of a pot 70AJ 47 Ajdovska jama 1967/82 670 44 LH/group 1 body of a large pot (pythos) 71AJ 48 Ajdovska jama 1982 198 43 LH/group 2 body of a pot 72AJ 49 Ajdovska jama 1985-87 606 44 CDV/XXII,XVI, group 3 body of a pot, red slip on exterior, burnt interior 73AJ 50 Ajdovska jama 1982 129 43 LH/tunnel 1 body of a pot, bucket-shaped 74AJ 51 Ajdovska jama 703 > CDV/22 body of a pot, ribbed decoration 8MT / Mala Triglavca 2006 PN1690 55 A/L92/a body, unwashed, undefined type 9MT / Mala Triglavca 2006 PN1722 55 A/L92/a body, unwashed, undefined type 10MT / Mala Triglavca 2006 PN1697 55 A/K93/c body, undefined type 11MT / Mala Triglavca 2006 PN1752 55 A/K91/c body, undefined type 12MT / Mala Triglavca 2006 PN1694 55 A/L93/a body, undefined type 13MT / Mala Triglavca 2006 PN1714 55 A/K92/c rim, undefined type 14MT / Mala Triglavca 2006 PN1748 55 A/L91/a body, undefined type 15MT / Mala Triglavca 2006 PN1561 47 A/L91/d body, undefined type 16MT / Mala Triglavca 2006 PN1680 55 A/L92/d body, undefined type 17MT / Mala Triglavca 2006 PN1644 47/51 A/L90/a body, undefined type 18MT / Mala Triglavca 2006 PN1829 61 A/L91/a body, undefined type 75MT 78 Mala Triglavca R043 2.90-3.05m 5,6,7 perforated rim, undefined type 76MT 81 Mala Triglavca R044 2.90-3.05m 5,6,6 base with body, burnt interior, undefined type 77MT 85 Mala Triglavca R045 2.90-3.05m 5,6,7 body of a pot 78MT 86 Mala Triglavca R046 2.90-3.05m 5,6,7 body of a bowl, incised decoration 79MT 101 Mala Triglavca R052 2.90-3.05m 5,6,7 body of a bowl, polished exterior 80MT 103 Mala Triglavca R054 2.90-3.05m 5,6,7 rim and body (two fragments), incised decoration, undefined type 81MT 112 Mala Triglavca R060 2.90-3.05m 5,6,7 body of a bowl, burnt interior 82MT 140 Mala Triglavca R076 2.90-3.05m 5,6,7 base with body, undefined type 83MT 169 Mala Triglavca R097 2.70-3.00m 4 body of a dish 84MT 335 Mala Triglavca R178 2.70-2.90m 3 base with body, undefined type 85MT 377 Mala Triglavca R187 2.60-2.75m 5,6,7 rim with body (two fragments) of a bowl 86MT 440 Mala Triglavca R208 2.50-2.70m 4 rim with body, traces of a black slip, undefined type 87MT 459 Mala Triglavca R214 2.50-2.70m 4 body of a cup, modern glue residue 88MT 503 Mala Triglavca R230 2.60-2.80m 3 rim with body, burnt interior, undefined type 89MT 512 Mala Triglavca R236 2.30-2.50m 4 rim with body (two fragments), undefined type 156MT 20 Mala Triglavca 1984 R016 3.05-3.25m 5 undefined type 157MT 27 Mala Triglavca 1984 R021 3.05-3.25m 5 pot 158MT 36 Mala Triglavca 1984 R024 3.05-3.25m 5,6,7 bowl 159MT 40 Mala Triglavca 1984 R027 3.05-3.25m 5,6,7 bowl 160MT 59 Mala Triglavca 1984 R034 3.05-3.25m 5,6,7 bowl 161MT 99 Mala Triglavca 1984 R050 2.90-3.05m 5,6,7 ladle 162MT 159 Mala Triglavca 1981 R090 2.70-3.00m 4 bowl 163MT 222 Mala Triglavca 1981 R123/124 2.70-3.00m 4 handle fragment Sample Sample Site code SF # SE/rel. Sector/quadrant Description # CHEM # ARCH depth 164MT 238 Mala Triglavca 1981 R133 2.70-3.00m 4 cup 165MT 239 Mala Triglavca 1981 R134 2.70-3.00m 4 bowl 166MT 442 Mala Triglavca 1981 R210 2.50-2.70m 4 pot 23MV-1 / Moverna vas 1988 1238 053.1 5/13 visible black, charred residue, inside 23MV-2 / Moverna vas 1988 1238 053.1 5/13 small bowl 24MV-1 / Moverna vas 1988 2478 050.2 4/3 visible black, charred residue, inside 24MV-2 / Moverna vas 1988 2478 050.2 4/3 base with body of a pot, organic residue on interior 25MV-1A / Moverna vas 1988 / 050.1 6/1-116 visible black, compact residue, inside 25MV-1B / Moverna vas 1988 / 050.1 6/1-116 visible brown, compact residue, inside 25MV-2 / Moverna vas 1988 / 050.1 6/1-116 base with body of a pot, organic residue on interior 26MV-1 / Moverna vas 1988 / 022.1 4/15 dark brown, compact residue, inside 26MV-2 / Moverna vas 1988 / 022.1 4/15 base with body of a pot, organic residue on interior 27MV-1A / Moverna vas 1988 6 050.1 5/6 black, compact residue, inside - only spots 27MV-1B / Moverna vas 1988 6 050.1 5/6 black, compact residue on section 27MV-1C / Moverna vas 1988 6 050.1 5/6 black, compact residue outside - only spots 27MV-2 / Moverna vas 1988 6 050.1 5/6 foot of a pedestal dish with red slip, organic residue on the foot 28MV-1A / Moverna vas 1988 5 050.2 5/10 black, compact residue, inside - only spots 28MV-1B / Moverna vas 1988 5 050.2 5/10 black, compact residue on section 28MV-1C / Moverna vas 1988 5 050.2 5/10 black, compact residue outside - only spots 28MV-2 / Moverna vas 1988 5 050.2 5/10 foot of a pedestal dish with red slip, organic residue on the foot 29MV-1A / Moverna vas 1984 212 323-332cm 2/1-8/7, N-profile pale brown residue on various parts, mixed with black residue - possibly soil, outside "black, compact residue in form of a lump, 29MV-1B / Moverna vas 1984 212 323-332cm 2/1-8/7, N-profile located just below the rim and running over the rib; looks charred and visible fibres, outside" 29MV-2 / Moverna vas 1984 212 323-332cm 2/1-8/7, N-profile rim of a biconical cup, organic residue on exterior 30MV-1 / Moverna vas 1984 / / 2/9/7, T8-7/7 white, compact residue in spots, inside 30MV-2 / Moverna vas 1984 / / 2/9/7, T8-7/7 base of a miniature bottle with incised decoration, whiteish residue on interior 90MV 1 Moverna vas 1988 R6 056.3 5/7 body of a spouted dish, type 1 91MV 2 Moverna vas 1988 R17 056 4/11 body of spouted dish (two fragments), type 1, burnt interior 92MV 3 Moverna vas 1988 R 174 056.3 3/10-14 rim with body of a spouted dish, type 1, impressed and combed decoration 93MV 4 Moverna vas 1988 R176 056.3 3/7 body of a spouted dish, type 1, applique decoration on exterior 94MV 5 Moverna vas 1988 R226 056.1 6/13 body of a spouted dish, type 1 95MV 6 Moverna vas 1988 R 467 050.2 > body of a spouted dish, type 1, horizontal rib and combed decoration 96MV 7 Moverna vas 1988 R8 056.2 3/13 body of a bowl with red slip, traces of residue on exterior, type 2 97MV 8 Moverna vas 1988 R19 056.2 4/3 body of a bowl (two fragments), type 2 98MV 9 Moverna vas 1988 R23 056.3 5/6 rim of a bowl (two fragments), type 2 99MV 10 Moverna vas 1988 R27 056.3 5/10 body of a bowl, type 2 100MV 11 Moverna vas 1988 R36 056.2 3/7 rim with body ofa bowl (three fragments), type 2 101MV 12 Moverna vas 1988 R179 056.2 3/5,9 body of a bowl, type 2 102MV > Moverna vas 1988 1 056.3 3/7 rim of a bowl, type 2 103MV 13 Moverna vas 1988 R20 056.3 4/13 body of a small pot with red slip, type 3 104MV 14 Moverna vas 1988 R239 056.3 5/13 body of a small pot (two fragments), type 3 105MV 15 Moverna vas 1988 sample 99 050.1-2 3/7 body of a small pot (three fragments), type 3, horizontal rib Sample Sample Site code SF # SE\rel. Sector\ Description # CHEM # ARCH depth quadrant 106MV 16 Moverna vas 1988 sample 103 056.2 3/14 body of a small pot (three fragments), type 3 horizontal rib 107MV 17 Moverna vas 1988 sample 104 056.2 3/9 body of a small pot with red slip, type 3 108MV 18 Moverna vas 1988 sample 105 056.2 3/3 base of a small pot with red slip, type 3 109MV 19 Moverna vas 1988 sample 106 056.2 3/3 body of a small pot, horizontal rib, type 3 ncMV 20 Moverna vas 1988 sample 107 056.2 3/6 rim with body of a small pot with red slip, type 3 mMV 21 Moverna vas 1988 sample 108 056.2 3/6 base of a small pot with red slip, type 3 naMV 22 Moverna vas 1988 sample 109 056.2 3/8 rim of a small pot with red slip, type 3 HbMV 23 Moverna vas 1988 sample 110 056.2 3/2 whole profile of a small pot with red slip, type 3 n4MV 24 Moverna vas 1988 sample 111 056.2 3/2 base of a small pot, type 3 nsMV 25 Moverna vas 1988 sample 112 056.2 3/7 body of a small pot with red slip, type 3 n6MV 26 Moverna vas 1988 sample 113 056.2 3/1-16 body of a small pot with fragmented handle, type 3 n7MV 27 Moverna vas 1988 sample 114 056.2 3/14 body of a small pot with red slip (two fragments), horizontal rib, type 3 nSMV 28 Moverna vas 1988 sample 115 056.2 3/14 body of a small pot with red slip, type 3 n9MV 29 Moverna vas 1988 sample 116 056.2 3/14 body of a small pot with red slip, horizontal rib, type 3 120MV 30 Moverna vas 1988 sample 117 056.2 3/14 body of a small pot with red slip, type 3 121MV 31 Moverna vas 1988 sample 118 056.2 3/14 body of a small pot, incides decoration on interior, type 3 122MV 32 Moverna vas 1988 sample 119 056.2 > rim and base of a small pot with grey slip, type 3 123MV 33 Moverna vas 1988 sample 120 056.2 3/15 body of a small pot with red slip, type 3 124MV 34 Moverna vas 1988 sample 121 056.2 3/5 body and base of a small pot with red slip, type 3 125MV 35 Moverna vas 1988 sample 132 056.3 5/5 body of a small pot, horizontal rib, type 3 126MV 36 Moverna vas 1988 sample 133 056.3 5/5 rim of a small pot with red slip, type 3 127MV 37 Moverna vas 1988 sample 134 056.3 5/10 body of a small pot with red slip, type 3 128MV 38 Moverna vas 1988 sample 183 056.2 4/7.3/3 body of a pot (two fragments), type 4 129MV 39 Moverna vas 1988 sample 225 056.3 3/12 body of a pot (two fragments), type 4 130MV 40 Moverna vas 1988 sample 102 056.3 5/11 body of a pot, type 5, combed decoration on exterior 131MV-1 41 Moverna vas 1988 sample 128 056.2 3/5 brown visible residue on exterior 131MV-2 41 Moverna vas 1988 sample 128 056.2 3/5 body of a pot, type 5, horizontal rib and combed decoration on exterior, organic residue on exterior 132MV 42 Moverna vas 1988 R38 056.3 3/7 body of a pot, type 5, 133MV 43 Moverna vas 1988 R130 056.2 3/3 rim of a pot, type 5, 134MV 44 Moverna vas 1988 R131 056.2 3/3 rim and body of a pot, type 5, horizontal rib and combed decoration on exterior 135MV 45 Moverna vas 1988 R181 056.3 5/1 body of a pot (two fragments), type 5, combed decoration on exterior 136MV 46 Moverna vas 1984 R222 1/8/7 1/5-8 body of a pot, type 5, incised decoration on exterior 137MV 47 Moverna vas 1984 R 262 2/5/7 2/9 body of a pot (two fragments), type 5, impressed and combed decoration on exterior 138MV 48 Moverna vas 1988 R212 050.1 5/11 body of a pot (three fragments), type 6 139MV 49 Moverna vas 1988 sample 101 056.3 3/14 body of a pot, type 6, horizontal rib and combed decoration on exterior 140MV 50 Moverna vas 1988 R8 056.3 3/10 body of a pedestal dish with red slip, type 7 141MV 51 Moverna vas 1988 R122 056.2 3/2 rim of a pedestal dish with red slip, type 7 142MV 52 Moverna vas 1988 R124 056.2 3/11 base with foot of a pedestal dish, type 7, red slip 143MV 53 Moverna vas 1988 R127 056.2 3/5 rim and body of a pedestal dish, type 7, red slip 144MV 54 Moverna vas 1988 R224 056.3 3/5 base with foot of a pedestal dish, type 7, red slip 145MV 55 Moverna vas 1988 R264 050.1.2 3/3 body of a pedestal dish, type 7, red slip 146MV 56 Moverna vas 1984 R56 1/8/7 1/5-6 base and foot of a pedestal dish, type 7, red slip 147MV 57 Moverna vas 1988 sample 100 056.2 3/7 base and foot of a pedestal dish, type 7, red slip 148MV 58 Moverna vas 1988 sample 123 056.2 3/2 rim and body of a pedestal dish (two fragments), type 7, red slip 149MV 59 Moverna vas 1988 sample 125 056.2 3/10 rim and body of a pedestal dish (two fragments), type 7, red slip 150MV 60 Moverna vas 1988 sample 126 056.2 3/5 rim of a pedestal dish, type 7, red slip 151MV-1 61 Moverna vas 1988 sample 135 031.4 6/12 black, compact residue, inside Sample Sample Site code SF # SE/rel. Sector/ Description # CHEM # ARCH depth quadrant 151MV-2 61 Moverna vas 1988 sample 135 031.4 6\12 body of a pedestal dish, type 7, red slip, organic residue on interior 152MV-1 62 Moverna vas 1988 sample 136 050.2 5\3 black, compact visible residue, covering interior surface uniformly 152MV-2 62 Moverna vas 1988 sample 136 050.2 5\3 body of a pedestal dish, type 7, red slip, organic residue on interior 153MV 63 Moverna vas 1988 R232 022 5\11 body of a pot, horizontal rib and incised decoration, type 8 154MV 64 Moverna vas 1984 R115 1\8\7 1\0-5 body of a pot (two fragments), combed decoration, type 9 155MV 65 Moverna vas 1988 sample 129 056.2 3\5 rim of a ladle, type 10 App. 2. Summary of lipid residue analysis and their interpretations Sample Vessel Biomarkers detected Lipid P/S 513C,6:O 613C,8:O Interpretation # CHEM part concentration ratio [%o] [%o] [^g g-1] 01AJ body / 2.38 / / / n/a 02AJ body FA14, FA16, FA17, FA18, K29-K35, K33:1, K35:1 198.63 1.19 -25.26 -27.88 mixed animal fat, plant residue, cooking 03AJ body FA14, FA16, FA17, FA18, FA20-FA28; OH24-OH34; A27-A31, traces of WE 83.19 0.46 -26.44 -29.27 ruminant adipose fat, plant residue, waxes 04AJ body FA14, FA15, FA16, FA17, FA18, K27-K35 161.18 1.15 -25.45 -31.25 ruminant dairy fat, cooking 05AJ body / 0 / / n/a 06AJ body / 11.86 1.35 / / n/a 07AJ body FA14, FA16, FA18, OH24-OH32 7.9 1.10 / / plant residue 31AJ body / 4.43 / / n/a 32AJ body / 0 / / n/a 33AJ body / 2.16 / / n/a 34AJ body / 0 / / n/a 35AJ base FA16, A25-A31; OH24-OH32, traces of WE 12.94 / / plant residue 36AJ body / 2.66 / / n/a 37AJ body FA16, FA22-34; A25-A33; OH22-OH34, WE 99.93 3.30 / / plant residue, waxes 38AJ rim / 0 / / n/a 39AJ rim / 2.73 / / n/a 40AJ body / 3.97 / / n/a 41AJ rim / 2.79 / / n/a 42AJ rim / 3.89 / / n/a 43AJ rim / 0 / / n/a 44AJ body FA14, FA16, FA17,FA 18, DAGs, TAGs 80.45 0.59 -25.71 -28.99 mixed ruminant fat 45AJ rim / 1.08 / / n/a 46AJ rim / 0 / / n/a 47AJ body / 4.03 / / n/a 48AJ body FA14, FA16, FA18:1, FA18, FA20 7.05 3.40 -22.41 -27.40 ruminant dairy fat, plant residue 49AJ rim FA16, FA18, FA20 48 2.32 -25.91 -24.88 porcine fat 50AJ body / 5.15 / / n/a 51AJ body / 0 / / n/a 52AJ body / 0 / / n/a 53AJ body / 4.16 / / n/a 54AJ rim / 1.76 / / n/a 55AJ body / 7.34 / / n/a 56AJ body / 6.72 / / n/a 57AJ base A25-A33, OH24-OH34, FA22-FA30 267.04 / / plant residue, waxes 58AJ-1 body / 0 / / n/a 58AJ-2 body / 0 / / n/a 59AJ body / 4.66 / / n/a 60AJ rim FA14, FA16, FA18 21.96 2.27 -23.25 -28.47 ruminant dairy fat, plant residue 61AJ rim FA16, FA17, FA18, FA20, MAGs, DAGs, TAGs 47.46 0.65 -25.15 -29.05 ruminant dairy fat FA14, FA16, FA17, FA18, 62AJ body MAGs, A27-A33, OH24-OH32, DAGs, WE, TAGs 73.65 1.09 / / animal fat, waxes 63AJ body / 0 / / n/a 64AJ rim FA16, FA18 9.36 1.85 -23.29 -24.24 ruminant adipose fat 65AJ body FA16, FA18, DAGs, traces TAGs 13.37 2.64 / / mixed animal fat 66AJ rim / 0 / / n/a 67AJ base / 5.02 / / n/a Sample Vessel Biomarkers detected Lipid P/S 613CI6:O 513Ci8:O Interpretation # CHEM part concentration ratio [%o] [%o] [Mg g-1] 68AJ body FA16, FA18>1, FA18, traces WE 11.39 2.96 -25.91 -26.47 porcine fat, plant residue 69AJ body FA14, FA15, FA16, FA17, FA18, A25-A33, OH24-OH32, FA22-FA32, WE, DWE 557.13 2.20 / / plant residue, waxes 70AJ body FA14, FA16, FA18, A25-A33, OH24-OH34, FA22-FA30, WE, traces DWE 75.66 1.85 / / plant residue, waxes 71AJ body FA16, FA18>1, FA18, OH, DAGs, TAGs 42.94 0.82 -29.11 -31.78 ruminant adipose fat, plant residue 72AJ body FA16, FA18, K29-K35, K33>1, K35>1 47.37 0.80 -27.59 -30.08 mixed ruminant fat, plant residue, cooking 73AJ body / 1.46 / / n/a 74AJ body / 0 / / n/a 08MT body FA14, FA15br, FA15, FA16, FA17br, FA17, FA18>1, FA18, MAGs, DAGs, TAGs, traces of WE 173.35 0.99 -26.51 -29.91 ruminant dairy fat, plant residue 09MT body traces of FA16 & FA18, K31-K35 1.9 / / n/a nMT body traces of FA16 & FA18, K31-K35 0.81 / / n/a 12MT body / 0.42 / / n/a 13MT rim FA16, FA18, MAGs, DAGs, TAGs, traces of WE, A and OH 11.56 0.63 -26.68 -28.85 ruminant adipose fat, plant residue 14MT body / 0.24 / / n/a 15MT body / 0 / / n/a 16MT body / 0 / / n/a 17MT body / 1.01 / / n/a 18MT body FA14, FA15br, FA15, FA16, FA17br, FA17, FA18>1, FA18, FA20-FA24, MAGs, DAGs, TAGs 88.09 0.75 -27.68 -33.26 ruminant dairy fat 75MT rim FA14, FA15, FA16>1, FA16, FA17, FA17br, FA18>1, FA18, FA20, MAGs, DAGs, TAGs 90.54 0.64 -28.96 -31.52 ruminant adipose fat 76MT base / 2.92 / / n/a 77MT body / 0 / / n/a 78MT body / 2.58 / / n/a 79MT body FA14, FA16, FA17, FA18>1, FA18, FA20, traces of A & OH, DAGs, TAGs 27.23 1.24 -27.80 -32.91 ruminant dairy fat, plant residue 80MT rim / 3.45 / / n/a 81MT body / 1.34 / / n/a 82MT base / 0 / / n/a 83MT body / 3.12 / / n/a 84MT base / 1.1 / / n/a 85MT rim / 1.34 / / n/a 86MT rim / 1.38 / / n/a FA14, FA16, FA17br, FA17, FA18>1, FA18, FA20, ruminant dairy fat, plant 87MT body MAGs, traces of A & OH, traces of DAGs & TAGs 21.93 1.05 -27.35 -32.18 residue 88MT rim FA14, FA16, FA18, FA20 9.93 2.56 -26.97 -31.91 ruminant dairy fat 89MT rim / 0 / / n/a 156MT rim FA16, FA18>1, FA18, traces of MAGs & DAGs 10.06 2.27 / / n/a 157MT rim / 4.06 / / n/a 158MT rim / 0.98 / / n/a 159MT rim FA16, FA18, MAGs, DAGs, TAGs 12.65 1.32 / / mixed animal fat 16oMT complete FA16, FA18, traces of MAGs, DAGs & TAGs 5.53 3.46 / / n/a 161MT rim FA16, FA18>1, FA18, MAGs, traces of DAGs 43.81 1.11 -29.38 -33.95 ruminant dairy fat 162MT n/a / 2.77 / / n/a 163MT body FA16, FA18 4.02 / / n/a 164MT rim FA16, FA18 2.47 / / n/a 165MT rim / 1.53 / / n/a 166MT rim / 4.67 / / n/a 23MV-1 rim FA16, FA18, traces OH 361.4 0.30 / / animal fat 23MV-2 rim FA14, FA16, FA17br, FA17, FA18, FA20, OH24-OH34, A29-A35, WE 434.99 0.25 -26.99 -30.46 mixed fat, waxes 24MV-1 base pitch markers 1789.97 / / birch bark tar Sample Vessel Biomarkers detected Lipid P/S 513C,6:O 513C,8:O Interpretation # CHEM part concentration ratio [%o] [%o] [M€ g-1] 24MV-2 base traces of pitch markers 0.77 \ \ n\a 25MV-1A base pitch markers, traces of WE 720.94 \ \ birch bark tar, waxes 25MV-1B base pitch markers, traces of WE 911.02 \ \ birch bark tar, waxes 25MV-2 base pitch markers, traces of WE 31.06 \ \ birch bark tar, waxes 26MV-1 base pitch markers 1539.77 \ \ birch bark tar 26MV-2 base FA10, FA12, FA14, FA16, FA18, pitch markers, WE 24.3 1.48 \ \ birch bark tar, waxes 27MV-1A base FA16, FA18, pitch markers 3308.1 1.33 \ \ birch bark tar 27MV-1B base FA16, FA18, pitch markers 118.18 1.34 \ \ birch bark tar 27MV-1C base FA16, FA17, FA18>1, FA18, pitch markers 740.32 1.71 \ \ birch bark tar, plant residue 27MV-2 base \ 0 \ \ n\a 28MV-1A base FA16, FA18, pitch markers, WE 3056.3 1.32 \ \ birch bark tar, plant residue, waxes 28MV-1B base FA16, FA18, pitch markers, WE 542.58 1.30 \ \ birch bark tar, plant residue, waxes 28MV-1C base FA16, FA18, pitch markers, WE 1261.79 1.68 \ \ birch bark tar, plant residue, waxes 28MV-2 base FA16, A, OH, traces of WE 5.25 \ \ plant residue 29MV-1A rim \ 18.03 \ \ n\a 29MV-1B rim FA16>1, FA16, FA18>1, FA18 8.06 1.89 \ \ plant residue 29MV-2 rim FA14, FA16>1, FA16, FA17, FA18>1, FA18, FA20-FA24, K31-K35 27.57 1.02 \ \ mixed animal and plant residue, cooking 30MV-1 base \ 0 \ \ n\a 30MV-2 base FA16, MAG16, DAG32, TAG54 17.69 \ \ plant residue 90MV body \ 0 \ \ n\a 91MV body FA16, FA17, FA18-FA24, K29-K35 156.62 0.31 -27.53 -31.65 ruminant dairy fat, cooking 92MV rim FA14, FA16, FA18, FA20, MAGs, traces of DAGs and TAGs 29.41 1.02 -27.75 -30.35 mixed ruminant fat 93MV body FA14, FA16, FA17, FA18>1, FA18, MAGs, DAGs, TAGs 119.17 0.77 -27.92 -31.36 mixed ruminant fat 94MV body FA16, FA18, FA20 15.2 0.57 -28.41 -30.89 ruminant adipose fat 95MV body FA16, FA18, MAGs, traces of DAGs and TAGs 5.5 1.19 -26.65 -28.90 mixed animal fat 96MV body FA14, FA16, FA18, FA20, MAGs, DAGs, TAGs 9.51 0.81 -27.18 -31.09 dairy fat 97MV body FA16,FA18 10.52 0.92 \ \ mixed animal fat 98MV rim FA12, FA14, FA16, FA17br, FA17, FA18, MAGs, traces of A & OH, DAGs, traces of WE, TAGs 57.85 0.69 -28.62 -30.75 ruminant adipose fat, plant residue, waxes 99MV body FA16, FA18, A25-A33, OH24-OH34, FA24-FA32, WE, DWE 429.65 6.20 -26.09 -29.62 dairy fat, plant residue, waxes 100MV rim FA16, FA18, A25-A31, MAGs, OH24-OH34, DAGs, WE, DWE 449.81 0.57 -27.47 -29.44 ruminant adipose fat, waxes 101MV body \ 0 \ \ n\a 102MV rim traces of FA16 & FA18, A25-A33, OH24-OH34, FA24-FA34, WE, DWE 399.78 2.86 -26.20 -33.48 plant residue, waxes 103MV body FA16, FA18, MAGs, traces of A&OH, DAGs, traces of WE 4.27 \ \ plant residue 104MV body FA14, FA16, FA17, FA18 214.36 0.65 -27.66 -30.22 ruminant adipose fat 105MV body \ 0 \ \ n\a 106MV body FA16, FA18, traces of A&OH 4.51 2.15 \ \ plant residue 107MV body FA16, FA18 29.38 0.67 -26.68 -28.39 mixed animal fat 108MV base \ 0 \ \ n\a 109MV body FA16, FA17, FA18 126.6 0.90 -26.14 -26.19 porcine fat n0MV rim FA16, DA17, FA18>1, FA18, FA20 1219.85 1.17 -24.90 -24.96 porcine fat mMV base FA12, FA14, FA16, FA17, FA18>1, FA18, MAG16, A27-A33, OH24-OH34, FA24-FA28, WE 177.63 2.47 -25.40 -25.73 porcine fat, plant residue, waxes n2MV rim traces of A&OH, traces of DAGs, WE 5.22 \ \ plant residue n3MV rim traces of FAi6 & FAi8, A23-A33, OH24-OH34, WE 47.2 -26.36 -27.85 plant residue, waxes n4MV base FAi6, FAi8, A23-A33, OH22-OH34, FA24-FA30, WE 94.85 2.89 \ \ plant residue, waxes Sample Vessel Biomarkers detected Lipid P/S 613C,6:O 613C,8:O Interpretation # CHEM part concentration ratio [%o] [%o] [Mg g-1] 115MV body \ 0 \ \ n\a 116MV body FA16, FA18, A23-A33, OH22-OH34, FA26, WE 145.68 3.24 -26.68 -28.75 plant residue, waxes 117MV body \ 0 \ \ n\a 118MV body \ 0 \ \ n\a 119MV body \ 0 \ \ n\a 120MV body FA16, FA17, FA18>1, FA18, FA20 197.58 0.81 -25.18 -25.15 porcine fat 121MV body A25-A33, OH24-OH34, FA24-FA32, WE 970.81 -26.89 -26.03 porcine fat, plant residue, waxes 122MV body traces of FA16 & FA18 2.18 \ \ n\a 123MV body \ 0 \ \ n\a 124MV body FA14, FA16, FA17, FA18>1, FA18, FA20 503.45 1.65 -24.24 -23.99 porcine fat 125MV body A23-A31, OH24-OH32, traces of WE 12.57 \ \ waxes 126MV rim traces of A&OH 1.4 \ \ n\a 127MV body traces of A&OH 1.74 \ \ n\a 128MV body \ 0 \ \ n\a 129MV body \ 1.07 \ \ n\a 130MV body \ 0 \ \ n\a 131MV-1 body \ 0 \ \ n\a 131MV-2 body \ 0 \ \ n\a 132MV body FA16, FA17, FA18 13.45 0.60 -26.57 -29.84 mixed ruminant fat 133MV rim FA14, FA16, FA17br, FA17, FA18, K 17.61 0.88 \ \ mixed animal fat, cooking 134MV rim FA14, FA16, FA17br, FA17, FA18, MAGs, OH22-OH32, A29-A31, DAGs, WE, TAGs 289.58 0.54 -28.35 -29.94 ruminant adipose fat, plant residue, waxes 135MV body FA16, FA17, FA18, MAGs, traces of DAGs & TAGs 47.71 1.41 -27.47 -26.99 porcine fat 136MV body \ 1.06 \ \ n\a 137MV body FA14, FA16, FA18 14.27 0.46 -28.64 -31.15 ruminant adipose fat 138MV body \ 0 \ \ n\a 139MV body \ 0 \ \ n\a 140MV body FA16, FA18, traces of A&OH< traces of DAGs&WE 4.14 1.12 \ \ mixed residue 141MV rim \ 0 \ \ n\a 142MV base \ 0 \ \ n\a 143MV rim FA16, FA18, MAGs, OH22-OH32, A27-A33, DAGs, TAGs 6.17 0.91 -27.66 -30.71 ruminant adipose fat, plant residue 144MV base FA16, FA18, FA20 9.76 1.45 -26.38 -29.28 ruminant adipose fat 145MV body traces of FA16 & FA18, A27-A31, OH22-OH32, traces of DAGs, WE & TAGs 6.82 \ \ mixed residue 146MV base \ 0 \ \ n\a 147MV base FA12, FA14, FA15, FA16, FA17, FA18>1, FA18, FA20-FA30, MAGs, A25-A33, OH22-OH32, DAGs, WE 37.61 0.53 \ \ mixed animal and plant residue, waxes 148MV rim \ 0 \ \ n\a 149MV rim FA14, FA16, FA17br, FA17, FA18, FA20-FA26, MAGs, A23-A33, OH22-OH32, DAGs, traces of TAGs 20.49 0.76 -26.71 -29.22 ruminant adipose fat, plant residue 150MV rim FA16, FA17, FA18, MAGs, A27-A33, OH24-OH32, DAGs, traces of TAGs 9.63 0.73 -27.42 -30.82 ruminant fat, plant residue 151MV-1 body traces of FA16 & FA18, pitch markers 2918.51 \ \ birch bark tar 151MV-2 body FA16, FA18, pitch markers 91.85 0.44 \ \ animal fat, birch bark tar 152MV-1 body traces of FA16 & FA18, pitch markers, traces of TAGs 2818.76 0.91 \ \ mixed animal fat, birch bark tar 152MV-2 body \ 0 \ \ n\a 153MV body FA14, FA15, FA16, FA17br, FA17, FA18>1, FA18, FA20, MAGs, DAGs, traces of TAGs 55.01 0.76 -27.70 -29.97 ruminant adipose fat 154MV body FA14, FA15br, FA15, FA16, FA17br, FA17, FA18, FA20-FA28, MAGs, A23-A33, 607.11 0.29 -27.96 -31.10 ruminant fat, plant residue, waxes OH22-OH32, traces of DAGs & TAGs, WE 155MV rim FA14, FA16, FA17, FA18>1, FA18, traces of DAGs & TAGs 7.15 0.56 -29.17 -31.37 ruminant adipose fat