Analytical investigations of adornment pieces from Susani (Timiş County, Romania

Journal of Thermal Analysis and Calorimetry https://doi.org/10.1007/s10973-020-09878-3 Analytical investigations of adornment pieces from Susani (Timiş County, Romania) Dan Vlase1,2 · Dragoș Diaconescu3 · Victor Bunoiu4 · Mădălin Bunoiu5 · Gabriela Vlase2 · Paula Sfârloagă6 · Titus Vlase2 Received: 31 October 2019 / Accepted: 23 May 2020 © Akadémiai Kiadó, Budapest, Hungary 2020 Abstract The samples originate from the funerary cache of a cremation burial mound dating from the Late Bronze Age (according to the Reinecke chronological system, Bronze D—Hallstatt A, according to absolute chronology ca. 1200 cal BC), discovered within the Susani-Grămurada de la Jupani mound (Timiș County, Romania). The pieces are sphere-shaped; however, many show signs of fire from the cremation of the buried person/persons. Together with bronze and gold pieces, they were part of composite necklaces and/or bracelets. Complementary techniques were used in the analysis: TG/DTA, FTIR, XRD, SEM and EDX to determine composition. All the techniques used in the present paper argued that the jewelry analyzed underwent a second burn at temperatures between 500 and 800 °C. Keywords Archaeological research · Thermogravimetric analysis · FTIR/UATR spectroscopy · SEM · EDX · XRD analysis · Ancient faiance · Beads · Late Bronze Age · Early Hallstatt · Cremation burial · Romanian Banat Introduction Archaeological excavations are of several different categories, depending on the intended objective and duration of the excavations. The vast majority of archaeological * Paula Sfârloagă paulasfirloaga@gmail.com * Titus Vlase titus.vlase@e-uvt.ro 1 Department of Scientific Research and Academic Creation, West University of Timisoara, Parvan Bvd. 4, Timisoara, Romania 2 Research Center for Thermal Analysis in Environmental Problems, West University of Timisoara, Pestalozzi Street 16, 300115 Timisoara, Romania 3 Banat National Museum, Str. Martin Luther nr. 4, Timisoara, Romania 4 County Directorate for Culture Timiș, Str. Episcop Augustin Pacha nr. 8, Timisoara, Romania 5 Faculty of Physics, West University of Timisoara, V. Parvan Ave., No. 4, Timisoara, Romania 6 Institute for Research and Development in Electrochemistry and Condensed Matter, P. Andronescu Str. 1, 300224 Timisoara, Romania investigations consist of rescue excavations or field surveys; however, several archaeological sites are targeted by systematic research projects aimed at investigating such sites in detail. Systematic excavations can last several years or even decades, depending on their size and complexity. One such site is Susani-Grămurada de la Jupani (eng. The mound from Jupani) mound (Timiș County, Romania). The site is located 610 m E-NE from the modern SusaniBega train stop, 1, 32 km E-NE from the Susani (orthodox) church (see Fig. 1) and 870 W-SW from the Petrom gas station near km 21 + 720 of the A1 Lugoj-Deva Highway (WGS coordinates: 45° 48′ 36.61″ N, 22° 0′ 30.10″ E). It is also 30 m north of the Glavița river’s right bank. It consists of an earthen mound, with a 42 m diameter and an elevation of 4 m, covering an area of 0.144 ha. The area around present-day Susani is well-known within archaeological literature, which mentions discoveries within a mound in the immediate vicinity of the Susani village, named Grămurada lui Ticu mound. These discoveries were considered to be a ritual place dated to Hallstatt A1–A2 [1–4]. Along these discoveries, the Grămurada de la Jupani mound was first mentioned, along with approximate measurements (4 m height and a 60 m diameter) [1]. In 2016, during a routine check by the authorities (the County Police, the Timiș County Directorate of Culture 13 Vol.:(0123456789) D. Vlase et al. Grămurada de la Jupani (no. 3) - location Grămurada de la Jupani - detail Fig. 1 Location of Grămurada de la Jupani burial mound (no. 3) and the Banat Museum), the mound was found to have been damaged by archaeological poachers, through a trench dug toward the center by mechanized means. Following this, the mound has been the subject for systematic archaeological investigations beginning in 2017, done by the West University of Timisoara, the Timiș County Directorate of Culture and the History, Ethnography and Plastic Arts Museum of Lugoj, continuing to the present day. The archaeological excavations have shown that the mound has an anthropic character, being a cremation burial ground barrow [5]. After 3 years of archaeological excavations, it can be stated that the earthen mound named as Grămurada de la Jupani was erected/built up, based on 14C data, at ca. 1430–1340 cal BC (σ value) or 1380 cal BC (μ value). From the larger historic-chronological perspective this time span corresponds to the C2 phase of the Bronze Age, in Paul Reinecke’s chronology [6]. During this particular chronological horizon the fashion of burial mounds was quite common in Central Europe. This phenomenon, belonging to the Middle Bronze Age, is named by the archaeologists as Tumulus Culture (germ. Hügelgräberkultur). The Bronze Age burial mounds from Romanian Banat, where also the modern Susani village is situated, can be considered as an eastern periphery of this archaeological culture/cultural vogue. Thus, Grămurada de la Jupani is a funerary monument built up by populations belonging to the final stage of the Middle Bronze Age, exhibiting the pottery style labeled as Balta Sărată, an archaeological culture representative for the Middle and Late Bronze Age from the hilly part of the Romanian Banat. All the burials identified so far from this stage of the barrow are of cremation type. Later, the populations belonging to the end of the Bronze Age (Bronze D) and/or the beginning of Iron Age (Hallstatt periode, phase A1), characterized by the pottery style named as Susani-Bobda, were reusing the mound from Susani, arranging into the central area of the existing barrow a secondary cremation grave. This custom, to arrange secondary 13 graves into the tumuli is reaching its decline, but is still present, in the 13th century cal BC, being connected to the Bronze D phase [7]. This event is happening in Susani at ca. 1300–1180 cal BC (σ value) or 1240 cal BC (μ value). This secondary grave, labeled as feature C.11/2018, belongs to this cultural horizon, anchored previously, from the absolute chronological perspective, around 1150-1050 cal BC [8]. The samples originate from feature C.11, which has been a secondary cremation burial, discovered within the Grămurada de la Jupani mound during the 2018 campaign. The beads were found in the two ash layers of feature C.11/2018. The C.11/2018 feature contained, besides the analyzed beads, bronze arrow tips, pottery shards, bronze and gold jewelry, calcinated human and animal bones. The manner in which the finds were places indicated they were part of the funerary inventory of the deceased individual/ individuals [9]. The presence, into the deposition from feature C.11 of the remains of a not cremated large herbivore mammal bones, allowed a 14C analysis, with indicated a calibrated value dating the feature at ca. 1200 cal BC (1240 cal BC, μ value), slightly earlier than it was traditionally chronological framed [8]. Materials and methods From the multitude of available techniques frequently used in analyzing archaeological artifacts [10, 11], the most easily available is FTIR spectroscopy, used as an initial a method of determining composition, most helpful in identifying the organic components within analyzed samples [12–15]. X-ray diffraction is certainly one of the most suitable analytical tools for mineral characterization and determination of the composition of crystallographic phases that can thus be linked to the provenance of the material analyzed [16–19]. In order to understand the combustion process adopted and the combustion temperature used to obtain the Analytical investigations of adornment pieces from Susani (Timiş County, Romania) material, it is necessary to investigate very carefully the characteristic features of the material transformation to heating and to follow the decomposition steps. Thermal analysis is a suitable tool for analyzing ancient ceramics, which allows the control of the combustion process and the recording of variations due to the simultaneous thermal process TG/DTG/DTA (HF) [20]. Thermal analysis in combination with FTIR and XRD provides information for estimating the original combustion temperature of the material and finding out the type of material [21], while also allowing a relatively clear image of the various phases of the firing process [22–26]. This study also makes use of a scanning electron microscope with energy-dispersive X-ray detection (SEM–EDX), in order to analyze the main element composition of the clay matrix using, a useful preliminary method [27–29]. The samples (Fig. 2) were taken from beads, with the primary focus of determining the materials used. The pieces are sphere-shaped; however, many show signs of fire from the cremation of the buried person/persons. Together with bronze and gold pieces, they were most likely part of composite necklaces and/or bracelets. Complementary techniques were used in the analysis, namely TG/DTA, FTIR, XRD, SEM and EDX to determine composition. Also the techniques were used to confirm the pieces were indeed burned during cremation. Thermogravimetric analysis Thermal stability was determined using a PerkinElmer TG/DTA diamond in dynamic air atmosphere (synthetic air 5.0 Linde Gas with flow rate 100 ml min−1) using open ceramic crucibles. The thermogravimetric study followed the main decomposition stages that are associated in the case of ceramics of decomposition processes that can bring additional data and arguments related to the composition of that material as well as information related to the processing temperature of the ceramic material studied. FTIR/UATR spectroscopy data were collected using a PerkinElmer SPECTRUM 100 device and employing the Universal Attenuated Total Reflectance (UATR) technique. Regarding data collection, the monitoring was made after 8 consecutive recordings at a resolution of 4 cm−1 on the spectral range 4000–650 cm−1. SEM/EDX investigations were performed on a Fei Inspect S electron microscope, at 15 and 20 kV, in order to determine the elements in the composition of the materials. For the identification of the crystalline phases X’Pert HighScore Plus software was used. The X-ray powder diffraction (XRD) measurements were performed using a PANalytical diffractometer, with Cu-Kα radiations (λ = 0.15406 nm) in a 2θ range from 10° to 90°, with a scan rate of 2°/min in order to confirm the crystal structure of the studied materials. Results and discussion Thermoanalytical analysis In the thermoanalytical study (Fig. 3) performed in the synthetic air atmosphere, the main stages of decomposition and their analysis were explained in accordance with the other techniques used to explain the type of material analyzed and its composition. Mass losses at 22–250 °C temperature ranges are associated with the processes of water loss (drying—loss of crystallization water) in the temperature range of 250–550 °C are attributed to dehydroxylation processes and between Fig. 2 Analyzed samples 13 D. Vlase et al. 1.5 100 2.0 95 1.0 1.5 90 TG B1 85 0.0 – 0.5 Mass/% Derivative mass/% xmin–1 0.5 1.0 B2 B3 DTG 80 0.5 75 0.0 – 1.0 70 – 1.5 65 – 2.0 60 Norm.HF 30 100 200 300 400 500 600 700 800 Normalized heat flow endo down/Wxg–1 Fig. 3 TG/HF for beads samples B1, B2, B3 – 0.5 – 1.0 900 Temperature/°C 550–700 °C the processes of decomposition of carbonate compounds are observed [30]. In the case of the thermoanalytical analysis carried out on sample B1, we can see the presence of three decomposition processes. The first process takes place in the range 45–236.9 °C with a mass loss of 10.26% being the process with the highest mass loss. In the range 240–574 °C, there is a continuous process of loss of mass (3%) without being observed a little clear on the HF curve. The last stage of visible mass loss on the thermoanalytic curves occurs in the range 574–780 °C with a loss of 1.1% of the sample mass. Over 800 °C no decomposition processes are observed. The last decomposition process is accompanied by an endothermic process with a maximum at 700 °C. The total mass loss in the range 25–900 °C in the case of sample B1 is 15.6%. In the case of sample B2, a thermal behavior similar to the previous sample is observed, namely the presence of three hardly separable stages, namely: one in the range 45–294 °C with a mass loss of 3.75% of the mass of the sample much smaller than in the case of the sample previous. The decomposition process is accompanied by an exothermic process with a maximum at 105 °C. The second process takes place in the range 295–470 °C with a loss of 0.73% of the sample mass having a maximum observable on the DTG curve at 380 °C. The last stage of decomposition observable on the TG curve occurs through several overlapping processes. The mass loss above 500 °C is 0.84% of the sample mass. The decomposition ends at 730 °C when a total loss of 6.5% is observed. The thermal decomposition of sample B3 in the range 30–900 °C shows a total mass loss of 9.88% loss that occurs in three separable stages on the TG curve. The first process in the range 45–250 °C with a loss of 6.38% and a maximum 13 at 110 °C. The second process that takes place in the range 250–580 °C leads to a mass loss of 1.88%, the last process leads to a loss of 0.62%. All the analyzed samples have a drying stage which ends at 45 °C. In the case of thermogravimetric analysis performed on samples B1, B2 and B3 the presence of three similar stages of decomposition in samples B2 and B3 was found in the range 30–900 °C. The thermal effect accompanying decomposition in the 600–900 °C range for sample B1 is accompanied by a more exothermic process. The exothermic thermal effect of the decomposition processes in the range 600–900 °C decreases in the order B1 > B3 > B2. The loss of water (moisture and crystallization water) has a higher mass in the case of sustained B1 sample followed by B3 and then B2. Regarding the loss of mass in the range 250–580 °C it can be observed that the highest mass of dehydroxylation processes is present in the case of sample B1 followed by sample B3. The amount of carbonate compounds decreases in the samples analyzed in the order B1 > B2 > B3. FTIR-UATR spectra FTIR spectroscopy is considered to be an important tool to analyze the clay minerals and mineral transformation due to thermal effects. Infrared spectra of archaeological artifacts reveal the type of clay and temperature of firing [31]. The FTIR spectra were obtained (Fig. 4) for all samples before and after thermodegradation at 900 °C in 4000–650 cm−1 spectral region. The FTIR spectra of samples showed a very small difference between samples B1, B2 and B3, as it is self-evident, considering that it comes from the same material but from different layers. This shows us that the ornament was not Analytical investigations of adornment pieces from Susani (Timiş County, Romania) 103.0 104.5 100 100 B2 B2_900 95 95 B1 B3_900 90 B1_900 B3 85 85 T/% T/% 90 80 75 80 70 75 65 70 68.0 4000.0 60.0 4000.0 3000 2000 1500 1000 3500 3000 650.0 2500 2000 1500 1000 650.0 Wavenumber/cm–1 Wavenumber/cm–1 (b) FTIR spectra of the all samples heat (a) FTIR spectra of the all samples B1,B2,B3 treated at 900 0C: B1,B2,B3. Fig. 4 a FTIR spectra of the all samples B1, B2, B3. b FTIR spectra of the all samples heat treated at 900 °C: B1, B2, B3 appear at 1636 cm−1 and at 1300 cm−1. B3 sample contains montmorillonite, illite and small. In the case of sample B2 the additional presence of the quartz is observed. In the case of sample B1, the presence of montmorillonite with Cu- and Fe-based pigments is observed. FTIR spectra of the samples heat treated at 900 °C are identical with only peaks in the range 1034–1000 cm−1 (Si–O stretch band), the symmetrical stretching at 800 and 780 cm−1 and the bending mode symmetrical and asymmetric Si–O at 695 cm−1. Some studies [32] have stated that the presence of the band at 915 cm−1 is due to Al–OH vibrations in the structure of the octahedral sheet, which begins to disappear at 500 °C. This band is not present in the studied samples, this is an indication that all the samples were burned above 500 °C. Intensity/a.u. obtained from different materials placed on different statures. Thus in the case of sample B1, B3 and weaker in the case of sample B2 has vibrations present in the 3350–3370 cm−1 region (humidity or KAl2[AlSi3O10](OH)2—rehydrating compounds), bands in the range 1630–1640 cm−1 (bending vibrations of the OH group) and the peaks in the range 1034–1000 cm−1 (Si–O stretch band, sharp peaks) the symmetrical stretching at 800 and 780 cm−1 and the bending mode symmetrical and asymmetric Si–O at 695 cm−1 [31]. The spectral analysis performed using the Nicolet database (Euclidean Search Hit List), compared the FTIR spectra and led to the conclusion that in all samples montmorillonite, halloysite, Quartz, Illite and Dickite could be present. Considering all minerals are minerals of aluminosilicate clay mineral, the individual montmorillonite clay crystals are not closely linked, so that the water can intervene, causing the clay to swell. The content of montmorillonite water is variable and increases greatly in volume when it absorbs water. Chemically, it is calcium magnesium sodium hydrate (Na, Ca)0.33 (Al, Mg)2(Si4O10) (OH)2·nH2O. Potassium, iron, and other cations are common substitutes, and the exact ratio of cations varies by source [15]. In the case of the FTIR study of the analyzed samples, the presence of peaks characteristic of SiO2 groups in the range of 1000–1040 cm−1 more strongly evidenced in case of sample B3 is found for all samples. The FTIR spectra of sample B3 differs from specimen B1, B2 and B2 glass samples by lacking bands ranging from 3000 to 3500 cm−1 characteristic of water (humidity and crystallization water). In the case of sample B3, two more clearly visible bands 800 600 400 200 0 800 600 400 200 0 1500 B1 B2 B3 1000 500 0 20 30 40 50 60 70 2θ /° Fig. 5 XRD analysis of the all samples 13 D. Vlase et al. Fig. 6 Distribution of different element in sample B1 Table 1 Elemental composition Element mass% at% C O Mg Al Si P Ca Fe Cu Total 8.93 49.89 0.43 2.76 31.08 0.60 2.34 2.34 1.94 100.00 14.21 59.59 0.34 1.96 21.15 0.37 1.12 0.69 0.58 100.00 Fig. 7 EDAX results for sample B1 RX analysis XRD analysis—showed weak peaks (Fig. 5) in the case of sample B3 and weaker in the case of sample B1, at 27 (Quartz) 29 (Calcit), 34 (Hematit), 39 (Quatrz), 52, 65, 66° (2 Theta) which indicates the presence of poorly crystallized silicoaluminates and SiO2. The peaks are better represented in the case of sample B3 because this sample is from the inside of the ornament and we can say that the decomposition is slightly weaker than in the case of the other samples. The XRD analysis argued that the analyzed samples were heat treated because the calcite appears very poorly represented which argues the heat treatment above 800 °C. The presence of very poorly represented phyllosilicates indicates Si O Fe Al Mg C Cu Fe Cu 1.00 13 Ca Ca P 2.00 3.00 4.00 Fe 5.00 6.00 Fe Cu 7.00 8.00 Cu 9.00 10.00 11.00 12.00 13.00 keV Analytical investigations of adornment pieces from Susani (Timiş County, Romania) a heat treatment of over 500 °C. We can conclude that XRD analysis reveals a thermally degraded material [33]. SEM/EDX analysis Distributions of different elements in sample B1 are presented in Fig. 6. The distribution of the component elements of the studied material is represented in Fig. 6. From this analysis it can be observed that the component elements of the material (sample B1) present a uniform distribution of the elements. The EDX analysis of the sample shows the presence of the elements in concentrations according to Table 1 and Fig. 7. The presence in high concentration of Si is observed, which argues the presence of SiO2 (according with X-ray diffraction analysis). There are also metals such as Al, Ca, Fe, Mg and Cu which explain the color of the composition and the color of some areas of the samples. The results of the analysis indicate the nature of the beads. The study was conducted to establish said nature, as a preliminary archaeological analysis proved insufficient to determine what type of adornment these beads constitute. As such, based on these results, a clear direction was ascertained in order to establish what they are exactly, beyond an initial assessment classing them as ritualistic. The obtained results are consistent with data established by the existing literature regarding certain funerary accessories in the late Bronze Age and Iron Age. Specifically, the results indicate that the ornaments share many similarities with so-called Bronze Age “faience” beads, in regard to composition (the presence of quartz, silica and copper oxide) and manufacturing [34–36]. As such, there is a high probability that the beads were funerary accessories that suffered secondary thermal treatment during the incineration of the defunct. The results are also confirmed by parallel analysis conducted by Robin Quataert from the University of Buffalo/State University of New York (NY, USA), on the calcinated bone fragments found within the burial mound, which arrived at similar conclusions [37]. The determination of the ornaments’ nature as faience is especially illuminating, considering the only other such case extensively documented in Romania [38]. Conclusions The samples of ancient artifacts were characterized by FTIR, TG/DTG/DTA, SEM–EDX and XRD analyses. Ancient pottery has long been studied by thermal analysis. Considering the analyzed samples, we tried to establish the type of material and check their degradation degree. 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