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Article

Organic Residue Analysis on Iron Age Ceramic Mugs (5th–1st Century BC) from Valle Camonica—UNESCO Site n. 94, Northern Italy

by
Paolo Rondini
1,
Giulia Patrizi
2,* and
Giuseppe Egidio De Benedetto
3
1
Department of Humanities, University of Pavia, 27100 Pavia, Italy
2
Department of Civil and Environmental Engineering, University of Perugia, 06125 Perugia, Italy
3
Laboratory of Analytic and Isotopic Mass Spectrometry, University of Salento, 73100 Lecce, Italy
*
Author to whom correspondence should be addressed.
Heritage 2025, 8(6), 198; https://doi.org/10.3390/heritage8060198
Submission received: 7 May 2025 / Revised: 24 May 2025 / Accepted: 26 May 2025 / Published: 29 May 2025
(This article belongs to the Section Archaeological Heritage)
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Abstract

:
The paper is dedicated to the study of organic remains in ceramic drinking vessels from protohistoric Northern Italy. These one-handled mugs are a typical item of the prealpine area, dating from the 5th to the 1st century BCE, and possibly carried high cultural value, given their presence in graves and sanctuaries as well as the presence of alphabetic inscriptions on some of them. The sampled items consist of 10 mug bases from the Iron Age sanctuary of Dos dell’Arca (Capo di Ponte, BS) and the coeval settlement of Castello di Castione della Presolana (BG). The analyses included HT-GC-MS and GC-C-IRMS analyses to identify ancient food/beverage products. The results indicate a differentiated use for the two types of mugs (“Breno” and “Dos dell’Arca” types), suggesting a possible shift in cultic habits. While both types were primarily containers for milk consumption, the earliest type was also used for consuming fermented, millet-based beverages, while the latter was covered with some oily vegetal substance before its disposal.

1. Introduction

UNESCO World Heritage Site no. 94 (“Rock Drawings in Valcamonica”, province of Brescia, Northern Italy) is known as one of the most important places in the world for prehistoric rock art. Despite its status as a relevant archaeological site, research in this area has been primarily focused on iconography, with limited consideration given to the archaeological context in which this phenomenon occurs. Material culture studies undertaken between the late 1980s and early 2000s have predominantly addressed data derived from non-systematic field activities (i.e., sporadic discoveries, preventive and rescue archaeology) or excavations conducted between the sixties and eighties, which exhibited deficiencies in both methodology and data processing. Despite these premises, typo-chronological studies [1,2,3,4] have succeeded in establishing a general chronological and cultural framework for the prealpine settlement in Lombardy from the Late Neolithic (late 5th millennium BC) to the beginning of the Roman period (around the end of the 1st century BC). A special attention has been paid to the Iron Age phase (1st millennium BC), considered as the period when the cultural alignment coincides with the ethnic formation of the so-called “Camunni”, one of the pre-roman peoples of Northern Italy, spread in the valleys of Central-Eastern Lombardy and Giudicarie, modern-day Trentino (Figure 1). Even though the majority of these studies have concentrated almost exclusively on the material culture, utilizing morphometric and typological characteristics specifically for ceramic studies, they have succeeded in attributing a specific role to a particular object, namely the single-handled mug. This role has been identified as that of a primary implement employed in both cults and funerary contexts [5] (p. 61) [2,6] and as an agent of identity [1] (pp. 116–117) [7] (pp. 274–276), without further specification of the details inherent its actual primary purpose, both in daily life and in cultic activities. This work focuses on the organic content of these vessels, aiming to provide a different level of understanding for these objects, in the hope of better comprehension of the relationship between typological differences (etic), functional articulation, and social role (emic) [8,9,10].

1.1. The Cultural Background

The Middle Iron Age (6th–5th century BC) and the Late Iron Age (4th–1st century BC) have been identified as a period of intense human occupation in Valle Camonica. During this time, there is evidence of a diffuse and structured management of land and resources, as well as trade and further contacts with other pre-Roman peoples, such as the ancient Veneti [11]. From a social perspective, already in the late 7th–early 6th centuries BC are significant as the period of initial cultural coagulation in the prealpine area of Valle Camonica, Valtellina, Valseriana, Val Borlezza, Giudicarie in modern Trentino (Figure 1), as evidenced by the development of the “Facies delle Valli Lombarde” [4,11] (pp. 326–337). This first formation, centred around the Valle Camonica, which functioned as its propulsive heart, evolved into a distinct culture during the 5th century BC and exhibited a remarkable degree of cohesion in all aspects of material culture, way of life, technology, cult, and language [6,7,12]. This archaeological culture has been referred to as “Cultura di Breno-Dos dell’Arca”, deriving from the two primary sites of Breno-Val Morina (a cemetery) and Dos dell’Arca (a sanctuary) [1]. The ethnic identification with the pre-Roman people of the “Camunni” [7,13] is evident in both Roman literary sources [13,14] and epigraphic texts, such as the Tropaeum Alpium in La Turbie, France, which celebrates Rome’s victory over the Alpine peoples [13]. The single-handled mug (Figure 2) is a particularly salient marker of this cultural group, due to its strong local character, its ubiquity throughout the group’s extensive territory, and its central role in the materials found in both cult sites and cemeteries [1].
Made of refined impasto pottery, these objects appear towards the beginning of the 5th century BC and seem to assume a central role in this culture for more than 5 centuries. Their morphological coherence is remarkable. Their main features are a sinuous profile with an outwardly enlarged foot, a wide and pronounced shoulder with a distinct vertical neck, and an outwardly folded rim. A long strip-handle links the rim to the foot. Raffaele de Marinis carried out their first typological analysis in 1989 [1], dividing this specific object into two different types. The “Breno”-type mug derives its nomenclature from the Breno-Val Morina cemetery, where it was initially unearthed as a grave good in tomb no. 1 [1,15]. Its defining characteristics include a linear and somewhat rigid profile, a clear break between the neck and the rim, and a high shoulder. The dating of the type was proposed by de Marinis between the 5th and the 4th century BC, based on closed-context finds and contextual analyses [1]. The “Dos dell’Arca”- type mug is regarded as a subsequent development of the “Breno”-type, exhibiting slightly diminished dimensions, a more pronounced morphology of the base (defined as a “trumpet-like” foot), a more rounded shoulder, and a continuous line between the neck and the rim. The temporal frame for this typology has been established as spanning from the late 3rd to the early 1st centuries BC. This determination was primarily informed by a thorough examination of the archaeological contexts, which have been deemed mostly unreliable [1] (pp. 113–115). The alternation of the two types is presented by de Marinis [1] as a typochronological evolution of the same object, without any implication of potential phases of overlap or coexistence between the two types. This paper, which presents both unpublished contextual data from excavations in the Valle Camonica and Valle Seriana area and new analyses of organic residues on ceramic mug samples, argues that the typological differentiation between the two items could have involved both a phase of coexistence and a differentiation in their function as drinking vessels. Their pervasive presence in sanctuaries and cult areas suggests that the divergent function of the two types could be related to different cult practices, thereby implying a clear cultural distinction between the selection of one or the other.

1.2. The Archaeological Context: The Sites of Provenance of the Samples

The main sampling site is the namesake of the latter type, the protohistoric sanctuary of Dos dell’Arca, in the Quattro Dossi area, in Capo di Ponte (Valle Camonica, BS, Italy). An additional mug was also sourced from the “Castione della Presolana” settlement, for a comparison with a vessel of the same type and period, but different provenance context.

1.2.1. Dos dell’Arca

After the first research in 1962 [16], the new “Quattro Dossi Project” [17] has been led since 2016 by the University of Pavia—Department of Humanities, directed by P. Rondini and A. Marretta. The project is dedicated to bridging the gap between archaeological research and rock art studies through the resumption of research at the already partially excavated [16] and mentioned site of Dos dell’Arca [17,18,19], which represented the ideal location for the coexistence of both rock engravings and archaeological evidence. It was also of significant importance in the history of research, having been referenced in the literature as the eponymous site of the “Dos dell’Arca” type mug, due to the large number of individuals of this specific object that were found there [1]. Despite the site having previously been the subject of investigation, it remained, to a considerable extent, obscure, and further research was required with a methodology that had been updated. Overall, the place is a small rocky hill located in the eastern valley bottom (around 430/440 m. asl) of the middle Valle Camonica (Figure 3). It has a long timeline, with alternate phases of occupation and abandonment ranging from the Middle and Late Neolithic (late 5th–early 4th millennium BC) to the Copper Age (late 4th–3rd millennium BC) to Middle- recent Bronze Age (mid-17th–13th century BC), before reaching its peak in the 1st millennium BC. Around the middle of the 6th century BC, after a few centuries of hiatus since the previous phase of occupation, the site was intensively revisited, with the upper part, the so-called “Bastione” now being chosen for the construction of a square stone altar dedicated to some fire-related cult activities.
The construction of this structure has been dated by radiocarbon on a charred coal from its inner part (DSH11332_CH 2472 ± 36, cal BC 768–462, 2σ) and by material culture study, which is consistent with the latter part of the range indicated by the measurement. The activities surrounding the altar included the lighting of fires and the utilization of a considerable number of drinking vessels, which may have been employed for libations. The data obtained from the excavations are in accordance with the established chronology of the artefacts in question. It has been observed that the earliest “Breno” type is exclusively present in the deepest and most ancient layers of the stratigraphic sequence. As the sequence progresses, the “Dos dell’Arca” type sherds emerge. Numerous mugs were found in a fragmentary state in the various layers of residual cultic waste that accumulated downhill from the altar. Throughout the five centuries during which the “Bastione” area was utilized, these wastes amassed and filled three levels of artificial terracing (Figure 4). Over time, this resulted in the structuring and monumentalization of the western slope of the hilltop, now interpretable as a proper sacred place, or sanctuary. In addition to the mugs, the material culture from the site also includes other sporadic ceramic vessels (mainly jars in the older levels and wide pans in the more recent ones), some bronze personal ornaments (both recovered in a fragmented state and partially burnt) and some faunal remains (currently under study by F. Fapanni and U. Tecchiati, University of Milano). Furthermore, an increasing number of mugs, from the few of the “Breno” type to the greater number of the “Dos dell’Arca” type, were decorated with some alphabetical inscriptions in the local pre-Roman alphabet [20]: single letters, more rarely pairs or triads. These inscriptions provide valuable insights into the personal effort and the underlying meaning of these ceramic forms, as well as their special significance in relation to the cult practice in place.
The “Bastione” area of Dos dell’Arca was chosen as the data source for this study due to the abundance of mug remains and its cultic character. Furthermore, the site is of particular significance for the study of this vessel type, being one of the few known locations that, given its extensive chronological span, facilitates the observation of the typological evolution between the two types from a continuous perspective. In this case, we can cautiously hypothesize that the transition from one type to the other can be interpreted as gradual, with multiple indications of a phase of coexistence of both types, as they have been recovered together in the same layers. As the stratification deepens, there is a gradual shift in the percentages of both types from an initial “Breno” predominance to layers consisting exclusively of “Dos dell’Arca” types. The analysis of the organic remains in these vessels is pivotal in substantiating a definitive cultural and functional interpretation.

1.2.2. Castello di Castione della Presolana

The site is a settlement in the Valle Seriana at around 850 m.a.s.l. in the Central Prealps, in the province of Bergamo, about 30 km from Dos dell’Arca [11] (Figure 5).
Known since the 1940s, the area was sporadically explored in the 1950s by local researchers and archaeologists such as Mario Bertolone and Ferrante Rittatore Vonwiller, who documented both prehistoric remains and Roman (early imperial) burials. In 1962, Luis Monteagudo Garcìa, during his absence from Spain, directed a campaign of 26 trenches in the site, providing evidence of a pluristratified site with phases of occupation dating from the Late Neolithic, the Late Bronze Age, and the entire Iron Age (1st millennium BC). The Iron Age phase of the site is the most consistent, and since the 6th century BC testifies to the involvement of the site in the development of the “Facies delle Valli Lombarde” [11] and then, since the 5th onwards, of the “Camunian” culture (Breno-Dos dell’Arca culture [1], thus participating in the same cultural milieu as the Valle Camonica.
The recent resumption of activities on the site follows the complete study and publication of the materials recovered in the old research [11], long unpublished, and aims to identify more consistent evidence of the settlement, as well as a better understanding of its structure. The provenance of sample no. 5 is a layer (stratigraphic unit no. 1201) formed in “Room A”, a residential structure dating from the 5th century BC. The excavation was directed by P.R. for the University of Pavia, and coordinated by the “Soprintendenza Archeologia, Belle Arti e Paesaggio per le province di Bergamo e Brescia” (Dr. C. Longhi).

2. Materials and Methods

2.1. Description of Archaeological Samples

The present study sampled 10 bases of the two different mug types, “Breno” and “Dos dell’Arca”, to analyse organic residues. The artefacts were collected and stored individually during excavation and did not undergo any washing or treatment prior to laboratory sampling. Drawing and photography were completed before the sampling (Figure 6; Table 1).
The samples nn. 1-2-3-4-6-7-8 and 9 come from three layers excavated during the 2022 campaign at Dos dell’Arca (stratigraphic units nos. 2002, 2005, 2006: Figure 4): these layers were documented in the second artificial terrace downhill from the altar (sector I, trench C) and were formed by the accumulation of waste from cultic activities. The stratigraphical position of the layers and the material culture seemingly date them to the 4th century BCE. These layers were selected because they contain both “Breno type” and “Dos dell’Arca type” mugs, thus providing an example of typological diversification in the same period and context. However, two items, one for each vase type, have been selected from other places not involved in the same activities as the main sourcing area. Sample n. 10 was found at Dos dell’Arca, excavation 2022, in sector NW—trench M, in a layer of use (US 2101) dated to the late Iron Age (possibly 3rd or 2nd century BC) and not directly related to the cultic activities of sector I.
On the other hand, sample n. 5, belonging to the “Breno” type, was discovered during the 2023 excavation of the Castello di Castione della Presolana.
The following table (Table 1) provides a complete description of each finding, including the laboratory code, provenance, type of vessel, vessel description, size, vessel technology, and lipid recovery yield.

2.2. Organic Residue Analyses (ORA)

ORA was carried out at the University of Salento, Italy. Each of the ten vessels described above was analyzed to determine its content. The ceramic vessels had not been washed before analysis or undergone invasive treatment, and each sample was collected from the bottom of a single mug.
A modeling drill with an abrasive tip as the grinding tool, rinsed with dichloromethane (DCM) before use to further reduce the possibility of exogenous or cross-sample contamination, was employed to clean the vessel surfaces and remove any exogenous lipids (Layers 1 and 3). Subsequently, approximately 1 g of potsherd (Layer 2) was manually pulverized using a mortar cleaned with DCM both prior to and after ceramic crushing.
The ceramic powder collected during internal surface cleaning (Layer 1) was retained for potential further analysis. Samples taken from the external surface of the vessels (Layer 3) served as controls, as no external sediment was preserved during excavation. The characterization of the lipid compounds present was based on the analytical results obtained from Layer 2. Ceramic powders and the soil sample were stored in vials that had been heated in a furnace at 450 °C for 12 h prior to storage. All used glassware was treated in a furnace before use.

2.2.1. Extraction Protocol and Instrumentation for the Recovery of Lipid Fraction

Powdered sherds were solvent-extracted (Dichloromethane-Methanol, 2:1, v:v) by ultrasonication to target lipid compounds following established protocols [21]. An aliquot (500 µL) of the total lipid extract was trimethylsilylated using N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA, 50 μL) before analysis by HTGC and HTGC-MS.
Analyses were carried out using an Agilent Technologies 6890B GC System coupled to an Agilent Technologies 5973inert MS. Injection was performed by an Agilent Autosampler (Agilent Technologies, Palo Alto, CA, USA) on a split/splitless injector at 300 °C. Analytes were separated on Agilent J&W DB-1HT column (15 m, 0.32 mm i.d., 0.10 µm thickness). The oven temperature was ramped from 50 °C (held isothermally for 1 min) to 350 °C at 10 °C min−1 (held isothermally for 7 min). The analysis used helium as carrier gas at a constant 3.0 mL/min flow. Mass spectra were acquired using electron ionization at 70 eV. The mass range was scanned from m/z 50–600. The ion source and the transfer line temperatures were fixed at 230 °C and 300 °C, respectively. Peaks were identified by comparison of their mass spectra with the NIST mass spectral database (2014), and with authentic standards of saturated (nonanoic acid, palmitic acid, stearic acid, arachidic acid) and unsaturated fatty acids (linoleic acid, oleic acid), analyzed under the same conditions.

2.2.2. Extraction Protocol and Instrumentation for the Recovery of Short-Chain Carboxylic Compounds

To target short-chain carboxylic compounds (insoluble in organic solvents or entrapped in the ceramic matrix), BF3/BuOH/cyclohexane treatment with extraction in dichloromethane [22] was used. Analyses were conducted using a Bruker SCION-456G coupled to a triple quadrupole mass spectrometer, Bruker SCION-TQ (Bruker Daltonics, Fremont, CA, USA). Analytes were separated on DB5-MS column (30 m, 0.25 mm i.d., 0.25 µm thickness). The analysis was carried out using helium as carrier gas at a constant flow of 1.2 mL/min. The oven temperature was ramped from 60 °C (held isothermally for 2 min) to 320 °C at 10 °C min−1 (held isothermally for 6 min). Mass spectra were acquired using electron ionization at 70 eV. The ion source and the transfer line temperatures were fixed at 230 °C and 280 °C, respectively.

2.2.3. GC-C-IRMS Analyses

An aliquot (250 µL) of the TLE of six selected vessels (1, 2, 4, 6, 7, 9) was used for GC-C-IRMS analysis. It was treated with an acidified methanol solution (H2SO4–MeOH 2% v/v) and heated at 70 °C for 1 h while mixing every 5 min. After cooling, 1 mL of H2O was added to the solution, and the free fatty acid fraction was extracted with hexane (3 × 1 mL). Then, the hexane extracts were combined and evaporated to dryness under a gentle nitrogen stream and re-dissolved in 70 µL of hexane. GC-C-IRMS analyses were performed on an Agilent Technologies 7890A gas chromatograph coupled to an Isoprime 100 stable isotope mass spectrometer using the Isoprime GC5 interface (IsoPrime Ltd., Cheadle Hulme, UK). The separation was performed on a DB1-HT column (15 m, id 0.320 mm, film thickness 0.1 μm) with the following temperature program: 80 °C (2 min), increased by 5 °C min−1 up to 300 °C (14 min). He gas (99.9995% purity) was used as carrier gas at a flow rate of 1 mL min−1. The injection was performed in split mode 1:2 into a split/splitless injector at 250 °C. The CuO-packed combustion tube was operated at 850 °C, while the chromatograph/furnace interface was operated at 350 °C. The ionization energy of the mass spectrometer was set at 80 eV, and the isotopes 44, 45, and 46 were recorded. The certified reference materials used for calibration were n-undecane (δ13C: −26.11‰, Chiron C0414.11-150-CY) and n-pentadecane (δ13C: −30.22‰, Chiron C0418.15-150-CY). Each sample was analyzed three times.

3. Results

The results obtained from ORA analysis demonstrate a remarkable degree of preservation of organic residues, in all cases exceeding 5 µg/g [23,24]. HTGC-MS analysis facilitated the identification of several families of molecules, including triacylglycerols, diacylglycerols, monoacylglycerols, fatty acids, n-alcohols, miliacin, bacteriohopanoids, diterpenoid compounds, and heated markers (Table S1). These could originate from various organic products such as animal fats, vegetable oils, millet, fermented by-products, and Pinaceae resins, and may represent the actual residues of the vessels’ contents.
All the internal pottery surfaces (L2) contained diterpenoid compounds, including methyl dehydroabietate, dehydroabietic acid, and 7-oxodehydroabietic acid [25,26,27], suggesting that a Pinaceae tar had been used to line the pot. Additionally, pimaric acid and isopimaric acid were identified in two samples, namely vessels 1 and 6; their presence is characteristic of a Pinus origin [28].
The occurrence of cholesterol and its degradation products (cholestanol and cholestan-3-ol), not found in the external layer (L3) analyzed as controls, together with linear saturated fatty acids ranging from C7:0 to C28:0 and branched C15:0 and C17:0 fatty acids, suggests the presence of animal fats in all potteries.
Their presence, along with the predominance of anteiso- over iso-branched C15:0 and C17:0, further supports the hypothesis of ruminant fat, as these can result from the activity of bacteria in the rumen [29,30,31]. In vessel 6, the presence of even-numbered saturated TAGs, comprising 44 (trace), 46, 48, 50, 52, and 54 (trace) carbon atoms, is also noted, along with traces of odd-numbered TAGs, particularly T49, T51, and T53. Their restricted profile, dominated by T52, suggests the presence of ruminant adipose fats, possibly also a degraded dairy product. This hypothesis is further supported by the values of palmitic and stearic acids obtained through the GC-C-IRMS analysis (Table 2 and Figure 7).
Samples 1, 2, 3, 4, and 5 show the presence of miliacin, a diagnostic triterpenoid marker which suggests the presence of Panicum miliaceum (common millet) [32,33] and its use in this site. In addition, in these samples a series of compounds characterized by a base peak at m/z 191 and molecular ions (M+.) 398 (C29H50) and 412 (C30H52), and occasionally 426 (C31H54), 440 (C32H56), 454 (C33H58), and 468 (C34H60), corresponding to hopanes, were identified (Figure 8). Although ubiquitous compounds present in the environment, they can also indicate the presence of different substances such as bitumen [34] or fermented alcoholic beverages [35]. In particular, the latter could result from bacterial activity, specifically from Zymomonas mobilis. Hopanoid biomarkers of this bacterium could occur due to sugar fermentation from plant by-products such as palm, beer, and a wide range of other plant sap and fruit-derived beverages [36].
The presence of these compounds in association with cereals, in this case, miliacin, could suggest a beverage produced from their fermentation, such as millet beer. Moreover, the absence of these compounds on the external surfaces of the vessels allows us to exclude their presence as exogenous contaminations and interpret them as the actual content of the vessels.
The methyl ester of palmitic and stearic acids and long-chain ketones (K29 to K37, K33 having the highest abundance, followed by K35 and K31) were also identified in sample 4. These compounds are known to be formed when fatty substances are exposed to high temperatures [37]. Still, they can also result from prolonged low heating of animal fat or plant oil in ceramics at less than 100 °C, probably catalyzed by metal salts in the pottery fabric, as revealed by recent experiments [38].
Some samples also contain plant residues, probably from oilseeds: the presence of β-sitosterol and, in some cases, its degradation products campesterol, stigmasterol and stigmastanol [39], unsaturated fatty acids, mainly 16:1 and 18:1, a palmitic/stearic acid ratio greater than 1.5, and an amount of oleic acid greater than that of stearic acid [40] suggest this hypothesis for samples 6, 7, 8, 9, and 10.

4. Discussion and Conclusions

The new data obtained from organic residue analyses allow for reflection on various aspects (Figure 9).
The first issue is the presence of diterpenoid compounds related to Pinaceae resins in all vessels and their potential role in sealing the inner portion of the mugs. This interpretation is technically sound, as demonstrated by studying the composition of the mugs’ material [41]. These analyses revealed a high presence of mica in the mixture of illitic clays, along with an estimated low firing temperature of approximately 450–500 °C. This is attributed to unburned organic substances in the ceramic mixture. Consequently, the artefacts were not fully sealed and exhibited high porosity. To ensure functionality as drinking vessels, it is hypothesized that internal treatment by lining with a different substance might have proved successful. The use of pine resins for waterproofing ceramic vessels is a widely attested practice since the Neolithic [42,43]. The Pinaceae resins identified in all the sampled mugs are also compatible with the site’s specific anthracological presence. Botanical data from the Iron Age layers of Dos dell’Arca (Rottoli and Castiglioni, in progress) confirm the absolute percentages (close to 90%) of Picea excelsa (European spruce) in the site, with a specific focus on the selection of wood used as fuel for the altar area. Picea excelsa is a tree species that cannot be sourced near the site due to its altitudinal preferences. This necessitates the specific selection and sourcing of wood from uphill locations.
A further commonality between the two mug types is the presence of ruminant fats. The δ13C values of palmitic and stearic acids obtained from the GC-C-IRMS analysis allow for more specific data interpretation: samples n. 1, 2 and 4 should have contained dairy products, while the isotopic signatures from findings n. 6, 7 and 9, confirm a mixture of animal (ruminant adipose and dairy) and vegetal fats, with oilseeds more prominent in 7 and 9 [44]. In addition, the finding of the vessels suggests that the mugs were utilized as containers for the consumption of cow’s milk [45], as they are not appropriate for milk processing activities such as boiling or separation. These hypotheses are also supported by archeozoological studies: the presence of bovines in the faunal record of the Iron Age Valle Camonica [46] and in the two sites from which the samples were taken (Fapanni, Tecchiati, in progress) supports this data interpretation. To attempt an interpretation of these data at a cultural level is challenging without extending the sampling and analysis to other contexts. Whilst there is a broad consensus that the consumption of milk is predominantly associated with childhood diets [47], the possibility that the mugs from the “Camunian” region were personal items, as seems suggested by the alphabetical inscriptions, utilized by individuals from an early age initially for milk consumption and subsequently for other purposes in adulthood (see below) could be hypothesized. However, albeit intriguing, this interpretation remains speculative without extending the sampling and analysis to a broader set of contexts and ultimately needs to be further tested and verified.
After providing commentary on the common features of the two ceramic types, the subsequent discussion will focus on the distinctive aspects of the organic remains, as evidenced by the analyses (Figure 9). The “Breno”-type vessels, dated from the 5th century BC to at least the whole of the 4th century BC [1], were used, aside from the milk, to consume fermented, millet-based beverages. While the presence of common millet has been recorded in Northern Italy since the Middle Bronze Age [48], its use as a cereal base for producing and consuming fermented, cereal-based alcoholic beverages also has parallels in the early Iron Age Northern Italian Villanovan site of Verucchio [49,50]. Furthermore, we are aware of the existence and use of liquid produced from the fermentation of barley [51] in the western part of the Golasecca culture area. The SEM analysis of the sediment contained in a whole drinking vessel found in grave 11 at the burial site of Pombia-Paù (NO), dating from the first half of the 6th century BCE, attests to both the existence of such products and their special role in society, given the funerary context.
Even though assigning a specific role to beer as a cultural agent has historically been primarily undertaken within the context of the “Celtic” world [52], including the Hallstatt phase [53], the increasing availability of data on the utilization of fermented, cereal- based alcoholic beverages in Northern Italy [54] complicates the established paradigm. It is imperative that the equation “beer = celts” be approached with caution, even without delving into the archaeological significance of the term ‘Celtic’ [55,56]. This caution remains as long as a more extensive and robust database concerning traditional and region-specific beverages associated with social practices has not been established. Notwithstanding, the data presented in this paper confirms that, at least during the 5th and 4th centuries BC in Valle Camonica -and culturally adjacent areas, as substantiated by sample n. 5 from Castione della Presolana- millet beer was consumed in a specific and special ceramic vessel, the “Breno”-type mug, in both domestic and cultic environments. Evidence of this kind is highly relevant from a cultural perspective, as it provides a strong and arguably exclusive functional characterization of a ceramic object, imbued with cultural significance, potentially even to the level of an identity marker [4,7,12]. The distinction in using this specific type of mug from the other, the “Dos dell’ Arca”-type mug, is one of the most surprising aspects that emerges from the analysis presented here. Even with the common “base use” as a vessel for milk consumption still standing, the absolute absence of millet beer in all the “Dos dell’ Arca”-type mugs suggests a different use for a different object. All the more significant is the fact that we analyzed several objects from the same stratigraphical contexts, and therefore most probably from the possible phase of coexistence of the two ceramic shapes, as well as objects from “type- exclusive” contexts such as Castione della Presolana—US 1201 (dated to the 5th century BCE and exclusively characterized by “Breno”-type) and Dos dell’ Arca- trench M US 2101 (dated to the late Iron Age by the exclusive presence of “Dos dell’ Arca”-type objects). As demonstrated, the functional distinction is evident, yet the utilization of the latter type is less immediate. Aside from traces of milk, the Dos dell’Arca mugs contain plant residues, most likely from oilseeds. Evidence of this was found in both the inner and outer ceramic layers, indicating that the “oily” absorption was likely achieved through immersing the mug in a larger container. The purpose of collecting the oily substance remains unclear: was it intended for use as fuel for the (votive) fire, or was its purpose merely symbolic, to establish contact between the content and the object, i.e., the mug itself? Further research is required to determine the provenance and natural characterization of these oilseeds.
As we have established, the analysis of the organic residues on the ceramic sherds leads to several points for discussion. The primary and most evident distinction between the two cup shapes is that they serve different purposes, indicative of their typological difference. This is pertinent at both archaeological and methodological levels, as it substantiates that even within a designated “object type”, such as the handled drinking vessel, the most minute variations in shape, morphology, or size employed to differentiate between types are not merely an “etic” distinction but also influence its perceived meaning and consequently its utilization in antiquity, thereby acquiring an “emic” value [57]. Moreover, the specific relation between these artefacts and their content facilitates a deeper comprehension of their unique perception within the original societal context. Each artefact is assigned a discrete function. Furthermore, these mugs hold significant importance. They are the most important objects in cultic practices, as demonstrated by the following evidence: their abundance at sacred sites, their presence in graves as grave goods, and their decoration with alphabetical letters. The transition from using millet beer in the early stages to later substituting it with oil substances, when considered in the context of the prevailing cult practices in the region, may also signify a shift in cultic practices and a cultural evolution, worthy of further investigation.
The evidence presented in this paper offers a novel perspective on cultural, chronological, and cultic practices in the Middle-Late Iron Age Valle Camonica and the broader Prealpine region of Lombardy. The analyses demonstrate a substantial degree of coherence in the data and notable robustness of the indicators. Nevertheless, the responses furnished by this study engender novel inquiries, the resolution of which necessitates subsequent research. For instance, increasing the number of analyzed samples of the two shapes is imperative with new sampling from disparate sites. Further samples will be collected in the forthcoming excavation campaigns that will take place in the Castello di Castione della Presolana settlement, as well as in other fieldwork opportunities. Other analyses, such as use–wear observations, will also be performed to gain a better understanding of the function and use of these objects. In addition, it would be pertinent to undertake testing for organic residues on other pottery shapes, including drinking vessels from the preceding stage, such as the “Castione”-type cup (late 7th–6th century BCE), and from the subsequent stage, such as the “Lovere”-type mug (1st century BCE–1st century AD). These latter mug types appear to assume the function attributed initially to the “Dos dell’Arca”-type vessel and to accompany it into the early Roman phase of the territory. In conclusion, new ORA analyses should also be performed on ceramic vessels that are not directly related to drinking. This will establish whether other products were produced and consumed in the “Camunian” area during the Iron Age. Finally, when a richer set of data is made available, new comparative observations will be established with similar data from other cultural contexts to build a stronger foundation for cultural interpretation.

Supplementary Materials

The following supporting information can be downloaded at: https://www.mdpi.com/article/10.3390/heritage8060198/s1, Table S1. List of vessels analyzed using ORA, along with relevant information about each vessel’s provenance, typology, and description, the sampled vessel part, lipid yield, molecular compounds present, GC-C-IRMS results, and their final interpretation. Lipid quantification is reported as µg of lipid per g of sherd. Cx:y = fatty acid with x carbon atoms and y representing the number of unsaturations; Cx:ybr = branched fatty acid; Ax = n-alcohols; Kx = ketones; MAG = monoglycerides; DAG = diglycerides; TAG = triglycerides; BH = bacteriohopanoids; tr = traces. (P.R., G.P.).

Author Contributions

Conceptualization, P.R. and G.P.; Sample artefact collection: P.R. Methodology: P.R., G.P. and G.E.D.B.; Sampling and ORA Analyses: G.P. and G.E.D.B. Writing, reviewing and editing in Section 1, Section 1.1, Section 1.2, Section 1.2.1, Section 1.2.2, Section 2, Section 2.1 and Section 4 by P.R. Writing, reviewing and editing in Section 2.2, Section 2.2.1, Section 2.2.2, Section 2.2.3 and Section 3 by G.P. Reviewing and editing on Section 4 by G.P. Reviewing and editing on Section 2.2, Section 2.2.1, Section 2.2.2, Section 2.2.3, Section 3 and Section 4 by G.E.D.B. Supervision by G.E.D.B. All authors have read and agreed to the published version of the manuscript.

Funding

Fieldwork on the two sites where archaeological samples were collected is funded by the University of Pavia—Department of Humanities, Pavia, Italy (“Cofinanziamento di Ateneo per attività di ricerca sul campo in ambito umanistico—anni 2022–2023”); ORA Analyses were funded by the Laboratory of Analytical and Isotopic Mass Spectrometry, University of Salento, Lecce, Italy. The University of Perugia funds post-doctoral fellowship (G.P.).

Data Availability Statement

All the relevant data supporting this research are available within the paper.

Conflicts of Interest

The authors declare no conflicts of interest.

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Figure 1. The area under consideration, with evidence of the diffusion area of the ceramic shapes in question (red shading) and the two sampling sites (yellow star symbols): A. Capo di Ponte (BS), Dos dell’Arca; B. Castione della Presolana (BG), Castello (map: P.R.).
Figure 1. The area under consideration, with evidence of the diffusion area of the ceramic shapes in question (red shading) and the two sampling sites (yellow star symbols): A. Capo di Ponte (BS), Dos dell’Arca; B. Castione della Presolana (BG), Castello (map: P.R.).
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Figure 2. The “Breno”-type mug (left) and the “Dos dell’Arca”-type mug (right): objects found at the site of Dos dell’Arca, Capo di Ponte (BS), excavations 2018–2023 (reconstructive drawings: P.R.).
Figure 2. The “Breno”-type mug (left) and the “Dos dell’Arca”-type mug (right): objects found at the site of Dos dell’Arca, Capo di Ponte (BS), excavations 2018–2023 (reconstructive drawings: P.R.).
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Figure 3. Dos dell’Arca, Capo di Ponte (BS): general plan of the site with structures subdivided by chronological phase. Evidenced in color blue, the “Bastione” area (LIDAR-based map: P.R.).
Figure 3. Dos dell’Arca, Capo di Ponte (BS): general plan of the site with structures subdivided by chronological phase. Evidenced in color blue, the “Bastione” area (LIDAR-based map: P.R.).
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Figure 4. Dos dell’Arca, Capo di Ponte (BS): plan of the Sector I (Bastione)—Trench C, excavation 2022, with some layers (2002, 2005) of waste accumulation from cult activities from which some of the samples were taken (GIS plan: P.R.).
Figure 4. Dos dell’Arca, Capo di Ponte (BS): plan of the Sector I (Bastione)—Trench C, excavation 2022, with some layers (2002, 2005) of waste accumulation from cult activities from which some of the samples were taken (GIS plan: P.R.).
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Figure 5. Photograph and positioning of the Castello, Castione della Presolana (BG) site (Photo: S. Fazzi; Map: P.R.).
Figure 5. Photograph and positioning of the Castello, Castione della Presolana (BG) site (Photo: S. Fazzi; Map: P.R.).
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Figure 6. The sampled artefacts. (A): bases of “Breno”-type mug (nn. 1–5); (B): bases of “Dos dell’Arca”-type mugs (nn. 6–10) (drawings: P.R.).
Figure 6. The sampled artefacts. (A): bases of “Breno”-type mug (nn. 1–5); (B): bases of “Dos dell’Arca”-type mugs (nn. 6–10) (drawings: P.R.).
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Figure 7. Plots of the Δ13C values for archaeological animal fat residues in the analyzed potteries. (G.E.D.B.).
Figure 7. Plots of the Δ13C values for archaeological animal fat residues in the analyzed potteries. (G.E.D.B.).
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Figure 8. Partial Total Ion Chromatogram (TIC) showing the molecular constituents present in sample 1. Cx:y = fatty acid with x carbon atoms and y representing the number of unsaturations, DHA = dehydroabietic, BH = bacteriohopanoid, MAG = monoglycerides, DAG = diglycerides, * = presence of isomers. The inset shows the GC-MS selected ion monitoring (m/z 191) showing the hopane distribution and their respective mass spectra (insets (A–C)) (drawings: G.P.).
Figure 8. Partial Total Ion Chromatogram (TIC) showing the molecular constituents present in sample 1. Cx:y = fatty acid with x carbon atoms and y representing the number of unsaturations, DHA = dehydroabietic, BH = bacteriohopanoid, MAG = monoglycerides, DAG = diglycerides, * = presence of isomers. The inset shows the GC-MS selected ion monitoring (m/z 191) showing the hopane distribution and their respective mass spectra (insets (A–C)) (drawings: G.P.).
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Figure 9. Schematic view of the ORA results; different colors represent the various substances individuated within the vessels. (G.P., P.R.).
Figure 9. Schematic view of the ORA results; different colors represent the various substances individuated within the vessels. (G.P., P.R.).
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Table 1. List of vessels recovered and analyzed using ORA, together with relevant information on the technology and typology of each vessel, their description, the part of the vessel sampled, and the lipid yield. Lipid quantification is reported as µg of lipid per g of sherd (P.R., G.P.).
Table 1. List of vessels recovered and analyzed using ORA, together with relevant information on the technology and typology of each vessel, their description, the part of the vessel sampled, and the lipid yield. Lipid quantification is reported as µg of lipid per g of sherd (P.R., G.P.).
Lab CodeProvenanceType DescriptionSizeVessel Techology Part of the Vessel SampledTLE (µg/g)
1Capo di Ponte (BS), Dos dell’Arca, Sector I, Trench C, US 2005Breno-TypeBase and low wall of “Breno”-type mug, with red paint on the exterior side. Diameter 8.5 cm, height 3.3 cm.Fine ware, yellowish brown.Inner base of the vessel (L2)475
2Capo di Ponte (BS), Dos dell’Arca, Sector I, Trench C, US 2005—RR 56Breno-TypeBase and low wall of “Breno”-type mug.Diameter 8 cm, height 2.3 cm.Fine ware, light brown.Inner base of the vessel (L2)508
3Capo di Ponte (BS), Dos dell’Arca, Sector I, Trench C, US 2005, RR 55Breno-TypeBase and low wall of “Breno”-type mug.Diameter 9 cm, height 2.5 cm.Fine ware, light brown with darker fire marks.Inner base of the vessel (L2)143
4Capo di Ponte (BS), Dos dell’Arca, Sector I, Trench C, US 2006Breno-TypeBase and low wall “Breno”-type mug.Diameter 9 cm, height 2.2 cm.Fine ware, light brown.Inner base of the vessel (L2)736
5Castione della Presolana (BG), Castello, Sector NW, Trench 2-2023, US 1201Breno-TypeBase and low-wall of “Breno”-type mug, with a concave base with a circular central cavity. It has a white encrustation on the inside.Diameter 7 cm, height 4 cm.Fine ware, light brown, with traces of red paint on the bottom. Inner base of the vessel (L2)56
6Capo di Ponte (BS), Dos dell’Arca, Sector I, Trench C, US 2002Dos dell’Arca- TypeBase and short wall of a “Dos dell’Arca”-type mug.Diameter 7.4 cm, height 8 cm.Fine ware with mica, dark brown.Inner base of the vessel (L2)1549
7Capo di Ponte (BS), Dos dell’Arca, Sector I, Trench C, US 2005, RR 50Dos dell’Arca- TypeBase and short wall with handle attachment for a “Dos dell’Arca”-type mug.Diameter 9 cm, height 2.9 cm.Fine ware with mica, reddish brown.Inner base of the vessel (L2)177
8Capo di Ponte (BS), Dos dell’Arca, Sector I, Trench C, US 2006Dos dell’Arca-TypeBase and short wall of a “Dos dell’Arca”-type mug with incised line over the low border.Diameter 8.8 cm, height 1.2 cm.Fine ware with mica, greyish brown.Inner base of the vessel (L2)69
9Capo di Ponte (BS), Dos dell’Arca, Sector I, Trench C, US 2005Dos dell’Arca-TypeBase and short wall of a “Dos dell’Arca” type mug with two incised lines on the wall (possibly part of an inscription) and a continuous vertical hole drilled between the wall and the bottom, possibly for repair.Diameter 9.2 cm, height, 2.5 cm.Fine ware with mica, dark gray.Inner base of the vessel (L2)70
10Capo di Ponte (BS), Dos dell’Arca, Sector NW, Trench M, US 2101, RR 57. Dos dell’Arca-TypeBase and short wall of a “Dos dell’Arca”-type mug, with incised line over the low border.Diameter 8.1 cm, height 2.4 cm.Fine ware with mica, light reddish brown.Inner base of the vessel (L2)64
Table 2. δ13C values of C16:0 fatty acid and Δ13C values preserved in each pottery analyzed. (G.E.D.B.).
Table 2. δ13C values of C16:0 fatty acid and Δ13C values preserved in each pottery analyzed. (G.E.D.B.).
Samples δ13C16:0 Δ13C
(‰ VPDB) (‰ VPDB)
1−26.49−4.26
2−27.84−3.2
4−27.02−3.41
6−27.32−1.75
7−30.17−0.4
9−29.56−0.81
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Rondini, P.; Patrizi, G.; De Benedetto, G.E. Organic Residue Analysis on Iron Age Ceramic Mugs (5th–1st Century BC) from Valle Camonica—UNESCO Site n. 94, Northern Italy. Heritage 2025, 8, 198. https://doi.org/10.3390/heritage8060198

AMA Style

Rondini P, Patrizi G, De Benedetto GE. Organic Residue Analysis on Iron Age Ceramic Mugs (5th–1st Century BC) from Valle Camonica—UNESCO Site n. 94, Northern Italy. Heritage. 2025; 8(6):198. https://doi.org/10.3390/heritage8060198

Chicago/Turabian Style

Rondini, Paolo, Giulia Patrizi, and Giuseppe Egidio De Benedetto. 2025. "Organic Residue Analysis on Iron Age Ceramic Mugs (5th–1st Century BC) from Valle Camonica—UNESCO Site n. 94, Northern Italy" Heritage 8, no. 6: 198. https://doi.org/10.3390/heritage8060198

APA Style

Rondini, P., Patrizi, G., & De Benedetto, G. E. (2025). Organic Residue Analysis on Iron Age Ceramic Mugs (5th–1st Century BC) from Valle Camonica—UNESCO Site n. 94, Northern Italy. Heritage, 8(6), 198. https://doi.org/10.3390/heritage8060198

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