Methodology and Archaeometry

Organic residue analysis (ORA) is a well-established technique that has been used for over 30 years to characterise vessel content through the analysis of absorbed lipids. Here, we first describe the general principles behind the technique, from the selection of the vessels, handling of selected samples prior to analysis and the biomarker and isotopic approaches used to characterise the residues. Special attention will be given to compound-specific isotope analysis, which allows further distinction between terrestrial ruminant adipose fats, dairy fats, non-ruminant fats and even wild animals fats as well as fats from marine and freshwater sources based on the d13C signatures of the palmitic and stearic acids commonly found in archaeological residues. Complexities and limitations of the technique will also be discussed. The results obtained from ORA on vessels recovered from the Late Bronze Age cemetery and settlement of Mačkovac-Crišnjevi, in Northern Croatia will be presented. The site is located on the left bank of the Sava River, near the town of Nova Gradiška and is dated to the BrC2 to HaA1 period (Barice-Gređani group). Lipids were extracted and characterised using Gas Chromatography-Mass Spectrometry (GC-MS) and Gas Chromatography - combustion - Isotope Ratio Mass Spectrometry (GC-c-IRMS). The results obtained were found to complement faunal data, and further show the use of dairy products.

A group of Late-Copper-Age decorated cross-footed bowls from the Trieste Karst (NE Italy) and the Deschmann’s pile dwellings (Ljubljansko barje, Slovenia), has been investigated through a non-destructive approach combining X-ray computed microtomography (microCT) and Prompt gamma activation analysis (PGAA) in order to study the vessels-forming technique, to characterise their pastes and to test the hypothesis that some vessels from the Karst could have been imported. Cross-footed bowls represent one of the most characteristic vessels of the 3rd millennium BC. In the Deschmann’s pile dwellings most bowls are attributed to Ljubljansko barje variant of the Vučedol Culture, corresponding to the first phase of the site. In the Karst, only a few bowls were discovered and, despite the small number, they are heterogeneous in terms of shape and decoration. According to their typology, the Karst bowls are associated to the Vučedol Culture but often referred to as an individual type. The PGAA results, combined with the microCT data, have shown that only one bowl from the Karst might have been imported from Ljubljansko barje, while other 4 Karst vessels were most probably imported but not from central Slovenia. In more detail, K2O contents, higher than values reported from local Karst and Slovenian soils, have been recorded in two of these Italian bowls. The Karst bowls represent, according to their shape and ornamentation mainly consisting of cord impressions, a special variant of cross-footed bowls with relevant typological comparisons in Hungary, Slovakia and the Czech Republic. A possible central European origin of some Karst bowls would be in agreement with high K2O soil contents in some areas of the Czech Republic. Cross-footed bowls from the Trieste Karst might be considered as evidence of long-distance connections, movements of ideas, artefacts and/or even movements of people.

Ovens are enclosed thermal structures typical for sedentary agricultural communities in the Middle East and Europe since the Neolithic Period. At the territory of the Central Balkans and Croatia, ovens have been built and used since the beginning of the Neolithic. In the published literature regarding the Starčevo culture settlements, four different types of enclosed thermal structures have been mentioned, some of which were interpreted as ovens and others as pottery kilns. It was assumed that all of the ovens/kilns were built from the same material – mud plaster and that all of them were free-standing above-ground structures located inside the dwellings. Several building techniques were proposed for their construction. The revision of the published data and unpublished field documentation from the excavations of the site of Lepenski Vir, has shown that not all of the thermal structures were constructed from the same material, only one type was a free-standing above-ground structure and one type should not have been interpreted either as an oven or as a kiln, but as an open fire installation. Based on the building material, three different building techniques were defined, and some of the previously presumed techniques were refuted. Also, the existence of pottery kilns during the Early Neolithic Starčevo culture was questioned. In order to test these hypotheses, several oven building and usage experiments were conducted. The aim of this presentation is to show different oven building techniques applied during the Early Neolithic in this region and introduce a typology for the Starčevo culture ovens.

The remains of cape Stoba shipwreck lies on the seabed near Mljet island at the depth between 21 and 28 m. The wreck-site is evidenced by a cargo of amphorae and glass dated back to the 10th-11th century AD. Five amphoras, located in the cargo part of the ship, as well as the small ceramic vessel which had to be placed in the ship’s kitchen, were found filled with sand and closed with a wooden stopper and resin. The aim of this study is a characterization of the sand which could help in the determination of its purpose. Sand samples from amphorae and vessel, as well as from the sea bottom, were investigated. Mineralogical content was determined using X-ray diffraction and grain size distribution by wet sieving. From fine sand magnetic fraction is separated. All granulometric and magnetic fractions were examined by binocular magnifier. All sand samples are marine sediment of carbonate composition. Sand grains are mainly skeletons of the Mollusca, Corals, Foraminifera, Sponges and Echinoderms. This investigation has neglected the archaeological assumption that sand was used as a raw material for glass manufacture. One of the assumptions is that sand could serve as dishwash as it was found in a small ceramic vessel inside the kitchen as well. But, the composition of sand is not suitable for this purpose. It is not possible that sand from the sea bottom entered in amphorae through a small hole at the center of the cap as the coarser grain size were found. Additionally, the depth at which the amphorae were found is below the base of the waves, and the sea currents in this area are not strong enough to produce a significant suspension of seabed material. This sand could serve as a ballast, although archaeologists have not encountered such a case so far.

The fact that vessels as well potter’s wheels and spindle whorls in Chalcolithic and Early Bronze Age I were made selectively from basaltic rocks shows that this raw material played a major role for tool production as well as for craft specialization during these periods. These items obviously had a great value for the communities in the southern Levant, facing increasing social and economic changes. The petrological definition of the raw material of the archaeologic finds, as well as the determination of the sources of basaltic rocks that were used for these tools, enables not only the mapping of the distribution of these items across the landscape and over time but also tracking possible trade routes and exchange mechanisms. The value of basaltic rock tools as carriers for information is essential. In contrast to many other raw materials, the petrological characteristics of a basaltic tool correspond directly to the characteristics of its source. To achieve more information about trade/ exchange systems, a geochemical database of the basaltic raw material is currently created to enable a geochemical affiliation of the archaeologic finds to their sources. For this reason, over 500 basaltic rock samples were collected in Israel and geochemically analyzed over the past years. The evaluation of the major and trace element analytical data supported by cluster analyses show that single basaltic rock deposits can be distinguished from each other as well as from other sources outside the borders of modern Israel. This permits an exact tracking of the origin of the archaeologic finds. This presentation will give an overview of the geological background data as well as present a case study of a Chalcolithic and Early Bronze Age I assemblage in order to demonstrate the approach of the provenance determinations.

The Cycladic island of Naxos, Greece is long renowned for its geology, and the range of lithic resources used in antiquity, not least marble, chert and emery. The latter raw material is particularly rare, with few sources in the larger region, and globally more generally. While its use as an abrasive from the later Neolithic to modern times is relatively well established, this paper focuses on its previously undocumented use as a resource for the production of flaked stone tools. Emery consists mainly of blue corundum and is mixed with magnetic iron ore creating the rough granular abrasive stone. It is one of the hardest materials to knap being graded 6-9 on Mohs scale depending on the source. Here we detail the first evidence for an assemblage of flaked stone implements, knapping debris and hammerstones of emery stone from Stelida on the northwest coast of Naxos, a chert source and stone tool workshop (located at least 5km distant from the nearest emery outcrops) whose exploitation spanned ~9000 to ≥200,000 years ago. In the presentation we discuss the techno-typological characteristics of emery assemblage, discuss its distribution across the site and its potential chronological range of use, before then considering the exploitation of this material within the context of hominin and early human mobility on Naxos, and Palaeolithic behavioural studies more generally.

In all scientific fields, the external validity of the studies is an indispensable condition to generalize the results. So, validation and cross-population studies are always of paramount importance. Although researchers are encouraged to provide and publish their raw data, it is still more exception than a rule. Also, many earlier studies contain valuable data, but it is not possible to access them. Recent anthropological studies provided a novel approach that employs algorithms used to recreate data from descriptive statistics. Using the assumption that skeletal metric data from a homogenous sample follow the normal distribution, they provided raw data and constructed metapopulation data. Although that approach showed promising results, it was not tested in detail if the original sample and simulated sample differed. This study aimed to examine differences between the original and simulated sample on seven femoral measurements. For the original sample, we used those of male and female skeletons from Ancient Salona for which we computed descriptive statistics. Using this data and package ‘truncnorm’ in R, we created a simulated sample. We statistically compared distributions of those samples and descriptive data. In both samples, we tested the accuracy of univariate discriminant functions for sex estimation on femoral measurements developed in previous research for various ancient and modern populations. For all variables, both for males and females, there were no statistically significant differences. Also, in most of the cases, discriminant functions for sex estimation for the previous study showed minor variation in accuracy when they were applied to the original and simulated sample. Therefore, the employed approach could be of great importance in anthropological population studies but also studies from the forensic context for validation and development of methods for the estimation of biological profile. It could also be utilized for archaeometric studies of materials whose measurements follow normal distributions.

The La Tène cemetery at Veliko Polje is situated on an elongated ridge close to Zvonimirovo in northern Croatia. In the beginning, it was excavated as a medieval cemetery of the Bijelo Brdo group, but during the research, numerous incineration Middle La Téne graves were unearthed, leading to continuous and systematic research of this particular Late Iron Age necropolis. These graves can be dated to a range from the end of the 3rd century BC to the first half of the 2nd century BC (LT C2). Based on the typological characteristics of the grave finds, this cemetery at Veliko Polje in Zvonimirovo can be ascribed to the Taurisci community, or more accurately to the distribution of the Mokronog group. The funerary ritual of this La Téne cemetery seems to have been quite well organized, because in most of the cases the graves were shaped as rectangular or oval pits, sometimes even containing wooden coffins or other funerary containers made of organic material, and the buried human remains were always incinerated. An important feature for this cemetery are the grave goods, ranging from ceramic vessels with food and drink as funerary gifts to weapons and toiletry accessories in warrior graves or knives and ceramic spindle-whorls in female graves, all accompanied regularly by typical male or female costume attire, such as fibulae, belts, jewelry, etc. Thanks to the fact that many of these finds were made of iron, several textile and other organic fragments were preserved in its corrosion and were eligible for further investigation after the conservation of the objects. The analysis consisted of determining the weave type of the fragments, noticing the thread spin direction and measuring the thread diameter. The remains were analyzed primarily by viewing with the naked eye, but some finer details such as thread diameter and patterning were determined with the help of digital microscopy. In this paper, preliminary results of the analysis of textile remains from four graves will be presented, along with their explanation and possible interpretation.

Remains of an early medieval iron production workshop were excavated at the Virje – Volarski breg site, located in the Podravina region (NW), a lowland area dominated by the alluvial plain of the Drava river. Current archaeological research has confirmed that iron ore processing has been present in this region in the 5th century (Virje-Sušine site), 7th century (Hlebine-Velike Hlebine site) and 8/9th century (Virje - Volarski breg and Sušine site). At the Virje-Volarski breg site several samples of iron ore were collected, analyzed and compared to ore samples from other iron production sites in the region as well as local bog iron ores collected as surface finds during an archaeological survey. Remains of four bloomery furnaces at the site had an in situ residue of iron production slag formed during the smelting process. Samples of different types of smelting slag (furnace slag, furnace bottom slag, tapped slag) were analyzed in order to define consistency or change in the smelting procedure during individual smelts. The aim of the study is also to define in what way and to what extent does the mineralogical and chemical composition of ores and smelting waste reflect the choice of resources and steps in the iron production procedures at the Virje – Volarski breg site. X-ray powder diffraction (XRD) was used to determine mineralogical composition of slag and bog iron ore samples. Detailed geochemical characterization of samples was performed using inductively coupled plasma mass spectroscopy (ICP-MS).

Mortar can be absolutely dated by physical methods of radioactive carbon decay (radiocarbon), optically stimulated luminescence (OSL) or by electronic paramagnetic resonance spectroscopy (EPR). However, to this day, there is no consensus on the method or on the unique way of sample preparation that would always provide the true date. The most used method is radiocarbon dating of pyrogenic carbonate created simultaneously with the mortar sample. However, the problem of extracting the pure pyrogenic fraction without carbonates originating from unburned limestone used for mortar production can often give too old dates. In order to find the most reliable method of mortar dating, the Mortar Dating Inter-comparison Study was conducted (MODIS, Hajdas et al. 2017; Hayen et al. 2017). Four mortar samples were distributed to seven radiocarbon and one OSL laboratory. The dates provided by mortar dating were compared by 14C dates obtained from charcoal associated with the production of mortars. For two samples laboratories provided dates similar to the consensus value, and one sample was found to be too heterogeneous for dating. For one sample all the laboratories provided too young dates, implying that the mortar was re-burned, so the analyzed pyrogenic carbonates actually pointed to the last time the construction was on fire, not to the actual building of the construction. The new mortar dating inter-comparison is in progress (MODIS 2). Three mortar samples have been distributed among 12 radiocarbon laboratories. The Zagreb Radiocarbon Laboratory is also included in MODIS 2, after being recognized for the mortar dating of the Skopje Aqueduct (Sironić et al. 2019). The most promising methods for extraction of pyrogenic carbonate form mortars applied in the MODIS will be presented.