image/svg+xml117XIII/2/2022INTERDISCIPLINARIA ARCHAEOLOGICANATURAL SCIENCES IN ARCHAEOLOGYhomepage: http://www.iansa.euBeyond a Decoration; Mineralogical and Micro-structural Study of the Early Bronze Age “Life Cycle Jar” from Keshik Cemetery, Sistan and Balouchistan, IranYasin Sedghi1, Farahangiz Sabouhi Sani2, Nasir Eskandari3, Mohammadamin Emami4,5*1Department of Conservation, Cultural Institute of Bonyad Museum, Resalat Highway, P.O. Box : 1519611197, Tehran, Iran2Department of Conservation of Cultural Properties and Archaeometry, Art University of Isfahan, Hakim-Nezami St., P. O. Box: 1744, Isfahan, Iran3Department of Archaeology, University of Tehran, Enghelab Square, 16 Azar St., P. O. Box: 661914155, Tehran, Iran4Department of Conservation of Cultural Properties and Archaeometry, Art University of Isfahan, Hakim-Nezami St., P. O. Box: 1744, Isfahan, Iran5Institut de Recherche sur les Archéomatériaux-Centre de Recherche en Physique Appliquée à l’Archéologie (IRAMAT-CRP2A), Université Bordeaux Montaigne, University area, F-33607 PESSAC Cedex, France1. IntroductionThe construction of a reliable archaeological framework for the development of the prehistoric cultures of the Iranian Baluchistan is still an ongoing efort, following the famous survey of A. Stein in the 1930s (Lamberg-Karlovsky and Besserat, 1977; De Cardi, 1966; De Cardi, 1968; Mutin et al., 2017; Sajjadi and Casanova, 2006; Stein, 1937).This paper deals with a collection of ceramics recovered from the plundered cemetery of Keshik, in the Makran region of the Indo-Iranian Borderlands. The collection includes two typical ceramic groups. The frst group includes a high-quality, painted grey ware present in the Indo-Iranian Borderlands during late 4thmillennium and early 3rdmillennium BC (Mutin, 2013). This ceramic is labelled as Emir Grey Ware, and has been reported at sites located hundreds of kilometres apart: such as Shahi-Tump and Miri Qalat in Southwestern Pakistan, Tepe Yahya, Konar Sandal and Varamin in Kerman, Shahr-i Sokhta and Mundigak in Sistan (both Iran and Afghanistan), and at many sites in the Iranian Baluchistan such as Tepe Bampur and Khurab. The production, chemical composition, and distribution of this ceramic has been the subject of many publications (Wright, 1984; Mutin et al., 2016). The second group of ceramics includes painted buf/red wares which can be associated with the newly-defned ceramic culture Volume XIII ● Issue 2/2022 ● Pages 117–128*Corresponding author. E-mail: aminemami.ae@gmail.comARTICLE INFOArticle history:Received: 26thJanuary 2022Accepted: 20thJune 2022DOI: http://dx.doi.org/10.24916/iansa.2022.2.2Key words:Iranian PlateauAncient potteryLife Cycle JarPetrographyXRPDSEM-EDXKeshik cemeteryBronze AgeABSTRACTThe present study focuses on a unique pottery vessel, the so-called “Life Cycle Jar”, and nine other potsherds which were discovered in the Keshik cemetery, Baluchistan, south-east Iran. Samples were investigated through classical analytical methods such as thin-section petrography, X-ray powder difraction (XRPD), and scanning electron microscopy coupled with energy dispersive X-ray fuorescence (SEM-EDX) to determine the production techniques, fabric characterisation, as well as the pigments applied to decorate the surface of the Life Cycle Jar. Mineralogical and chemical investigations revealed that the pottery pieces were similar in raw materials, and produced locally. Samples show a wheel-thrown signature based on the defnite orientation of pores and structural character in their thin sections. The potter pieces were fred under oxidation processes demonstrated by the red and green colour of the matrix. The investigated pottery samples were defned as high-fred sherds (ca. 800–950°C), due to the presence of inclusions in the form of reacted calcite in rhombohedra crystal structure, and hematite within the matrix of the pottery. The microstructural characteristics of the pottery pieces showed that the manufacturing temperature was no higher than 950 °C, by pre-sintering texture. The investigations on the painted decoration on the Life Cycle Jar suggested that iron oxide and manganese oxide was used as the colourant agent in the decoration.
image/svg+xmlIANSA 2022 ● XIII/2 ● 117–128Yasin Sedghi, Farahangiz Sabouhi Sani, Nasir Eskandari, Mohammadamin Emami: Beyond a Decoration; Mineralogical and Micro-structural Study of the Early Bronze Age “Life Cycle Jar” from Keshik Cemetery, Sistan and Balouchistan, Iran118of the Halilrud basin, ca. 3000 BC, the so-called “Varamin Culture”. The masterpiece Life Cycle Jar (LCJ) falls in the latter group. Thanks to the discovery of Keshik, Nikshahr is the most Eastern infuential extension of the Varamin ceramic tradition. They were already recorded at sites across the Halilrud basin such as Varamin in the Jiroft plain, and Tepe Yahya in the Soghan valley (Eskandari et al., 2020; Eskandari et al., 2021a; Eskandari et al., 2021b).South Makran is an important archaeological zone, where more archaeological studies have been undertaken in its periphery, and excavations are still going ahead (Lorentz et al., 2020). The site is located in the southeaster part of Hamun Basin and Jaz Murian, the East-West connective highway in southern Iran (Figure 1). Stein (1937) described the Keshik territory in his survey from Ghasr-e Ghand to Nikshahr; however; the Keshik cemetery was not discussed in detail. The cemetery of Keshik will be discussed in the broader archaeological context of Indo-Iranian Borderlands in order to visualise the cross-regional interactions during the late 4th-early 3rdmillennium BC (Stein, 1937). Based on recent studies, this type of pottery was demonstrated as the earliest dark-grey pottery, which had been obviously an essential type during the Early Bronze Age in the south east of Iran (Mutin, 2013; Mutin and Lamberg-Karlovsky, 2013). This study will also focus on the characterisation and the fabrication of the Life Cycle Jar amongst other pieces. This pottery has been classifed as a typical fabrication of Jiroft, showing that the production of the vessels was very cautiously followed with much attention to elaborate decoration (Eskandari et al.,2021a).This paper will also explore the ceramic collection of the Keshik cemetery by using mineralogical and micro-structural analyses such as thin-section petrography, XRPD (X-ray powder difraction) and SEM-EDX (Scanning electron microscopy with coupled energy dispersive X-ray fuorescence).2. Context of Recovery2.1 Keshik cemeteryThe prehistoric Keshik cemetery is located 8 km northeast of Nikshahr, 2 km southwest of the village of Keshik, and northeast of the Keshik River Basin and its dam (Kheir-Abad Dam) (Figure 2). In 2012, the site was uncovered during the construction of a water canal. Later, Heydari et al. (2015) discovered a large Bronze Age cemetery during subsequent excavations at Keshik. The ceramics used in this study were obtained from the surface of the cemetery’s plundered graves. Though the exact context of the ceramics is unclear, due to the nature of the site and the context of the recovery, it is evident that they served as burial goods. Haidari’s excavation at this site was able to document 26 graves, which appeared to be of a catacomb type that were architecturally the same but varied in size. Lengths varied between 180 and 420 cm, with the width approximately 120 cm, and the heights between 110 and 130 cm. It seems that this cemetery has accommodated graves from later periods.The cemetery is chronologically considered as a newly-discovered ancient site that enables the cultural exchange that occurred in south east of Iran to be described (Eskandari et al., 2020). Based on the recovered burial fnds, particularly those forming the focus of the current research, this cemetery dates back to the late 4th- early 3rdmillennium BC (3300–2900 BC). This dating is supported by new radiocarbon dates from the site of Varamin in the Jiroft plain (Eskandari et al., 2021). During the Proto-Elamite level of Tepe Yahya (Yahya IVC), Varamin period ceramics are comparable with the painted buf/red wares of Keshik. In addition, the fne painted grey wares of Keshik cemetery (Emir Grey wares – recently named Late Shahi Tump) are already contextualised in many sites in Kech-Makran – such as Shahi Tump IIIA (Mutin, 2016), Shahr-i Sokhta period I in Sistan, Tepe Yahya IVC (Mutin, 2013) and Varamin (Eskandari et al., 2020) in Figure 1.Location of the Keshik cemetery in relation to other south-eastern sites.
image/svg+xmlIANSA 2022 ● XIII/2 ● 117–128Yasin Sedghi, Farahangiz Sabouhi Sani, Nasir Eskandari, Mohammadamin Emami: Beyond a Decoration; Mineralogical and Micro-structural Study of the Early Bronze Age “Life Cycle Jar” from Keshik Cemetery, Sistan and Balouchistan, Iran119Kerman, and at the early periods of Tepe Bampur (de Cardi 1966) in the Bampur valley.All the graves are primarily constructed from stone, with additional buried objects – such as items of metal, stone, and pottery – found inside the graves. Among the discovered artefacts, a big pottery stirrup jar, in a buf to reddish paste colour with unique goat motifs on the surface, has been discovered. Due to the narrative nature of the periodically moving motifs on the surface of the jar, this kind of jar was described as a “Life Cycle Jar” (Figure 3). The motifs represent diferent life stages of a goat from birth to maturity. Most of the patterns used for decorating the pottery have been realised by geometrical shapes, ornamentation and specifc symbols (Heydari et al., 2015; Sajjadi et al., 2008). The geometrical patterns are observed on the red and buf pottery vessels, especially on the glasses, cups and carafes, Figure 2.Geographical map of the Keshik cemetery and its location connection to the village of Keshik, the River Keshik and the Kheir-Abad Dam (picture top left is a destroyed grave in the cemetery).Figure 3.The Life Cycle Jar recovered from the Keshik cemetery.
image/svg+xmlIANSA 2022 ● XIII/2 ● 117–128Yasin Sedghi, Farahangiz Sabouhi Sani, Nasir Eskandari, Mohammadamin Emami: Beyond a Decoration; Mineralogical and Micro-structural Study of the Early Bronze Age “Life Cycle Jar” from Keshik Cemetery, Sistan and Balouchistan, Iran120whereas the natural plant and animal patterns are only seen on the grey pottery (Sajjadi et al., 2008). The plant patterns and motifs clearly represent date palms and ears of wheat. The natural patterns are the symbols of mountains. For instance, the patterns of the life cycle (a broken cross) are the sun, and waves. The animal patterns include domestic animals such as goats (comb-like and realistic). The goat was the symbol of a blessing in life and living in Ancient Persia (Sajjadi et al., 2008). It represents frstly the rolling terrain of Baluchistan and secondly the grazing of goats (where there must be water and plants). Keshik style pottery is also remarkable for its painted natural surroundings (Sedghi and Razani, 2020).2.2 Geological setting of Keshik cemeteryGeologically, Nikshahr is located in the Makran zone. It is a mountainous area with narrow valleys which were formed due to enormous geological and orogenic formations. The valleys are passageways of seasonal and permanent rivers that make up suitable and fertile agricultural lands (Berberian et al., 1982; Wright, 1984). According to geological studies, the Keshik cemetery is located in an area of short foothill fans and terrace deposits at the boundary of a Rig unit. The Rig unit has a harmonious sequence of layered sandstone and shale with not an insignifcant amount of siltstone (Owliaieet al., 2006).The surveyed area was characterised by the existence of sandstone, shale and conglomerate associated with tuf and basaltic lava (Mousivand et al., 2018). The geological setting correlates with the availability of rich metallic resources and a fuvial clay deposit (Mousivand et al., 2018). Geologically, the outcrops of this area are defned as Ophiolite-hosted deposits. The outcrops are Eocene andesite host rocks. Various alteration zones such as propyritic, sericitic and argilitic are common. In certain parts, potassic and silicic zones are also observed. Magmatic actions during the Early-Middle-Late Eocene age in the Bazman sub-zone has also been observed in other parts of the Kerman. However, acid magmatic products such as agglomerates, breccia and tufs are not signifcant. Based on the geological survey in the feld, the soil from the region around the Keshik cemetery consists of fragments of sandstone and shale as a conglomerate structure. The geological setting confrmed an homogeneous sequence of layered sandstone and shale with a little siltstone, lichen and conglomerate (Falcon, 1974; Owliaie et al., 2006).3. Materials and Methods3.1 SamplesNine sherds of Bronze Age pottery explored during the 2012 excavation of the Keshik cemetery (Heydari et al., 2015), and the unique Life Cycle Jar (Figure 4, No. 10) were chosen for the technological study. Five of the selected pottery sherds are light red in colour with the remaining fve items being light grey in colour. Valuable painted grey ware was present in the Indo-Iranian borders through the late 4thmillennium, and early 3rdmillennium BC (Figure 4, No. 9). Regarding the surface as well as macroscopic features, it is worth noting that the pottery sherds were sampled from painted vessels in the form of large bowls and jars. The walls of the bowls Figure 4.Investigated samples from the Keshik cemetery.
image/svg+xmlIANSA 2022 ● XIII/2 ● 117–128Yasin Sedghi, Farahangiz Sabouhi Sani, Nasir Eskandari, Mohammadamin Emami: Beyond a Decoration; Mineralogical and Micro-structural Study of the Early Bronze Age “Life Cycle Jar” from Keshik Cemetery, Sistan and Balouchistan, Iran121are thinner, whereas the jars have a thicker wall. They show a mostly diferent colour hue along the section, since they were possibly exposed to a diferent fring condition. The thickness of the samples varied between 1.7 to 3.5 cm (Figure 4, and Table 1). Sample number 9 is classifed as a very important ceramic shape, since the intercultural variety of the pottery can be refected in the stratigraphic contexts of the Early Bronze Age of the region, and has been classifed as a shape typical for the Varamin Culture (Eskandari et al., 2020).3.2 MethodsThe characterisation of the samples of pottery and their mineralogical chemical content were performed by a number of diferent methods. Petrographic and petrological studies were performed using 30 µm sections using a Polarizing Microscope®-James Swift Model (Burton et al., 2019; Quinn and Burton, 2009). Observations were carried out using plane polarised light (PPL), as well as crossed polarised light (XPL), in order to identify the mineralogical constituents. In order to qualitatively detect the presence/absence of minute crystalline phases within the samples, XRPD was applied. Samples were prepared with 0.5 g of homogenised powder that was taken from the sherds. Samples were analysed on a Bruker-D8 Difractometer®(Canada) with a 40 KV, 30 mA copper (Cu) X-ray producing tube lamp. X-ray powder difraction (XRPD) was achieved on the samples (2θ = 10°–60°). Quantitative measurements were obtained by determining the crystallographic character via the ICSD database for each crystalline phase, which had been applied for interpreting the XRPD patterns in X’Pert HighScore Plus®-2008 ver. (2.2.c) (Burton et al., 2019; Emami, 2020; Eramo, 2020; Quinn and Burton, 2009).A scanning electron microscope coupled with an energy-dispersive X-rap fuorescence detector (SEM-EDX) from TESCAN MIRA3 FEG-SEM®was used to analyse the microstructure and chemical composition of the samples. The device is equipped with Fielmann feld emission and operates in both high and low vacuum. The resolution is defned to 1 nm and its magnifcation is 1 µm by applying 30 KV voltage. In addition, the device is equipped with an EDX INCAx-Sight (UK) that is capable of qualitative and quantitative analysis for micro chemical composition. The analysis was conducted at the Central Laboratory of Sahand University of Technology, Tabriz, Iran.4. Results and Discussion4.1 Petrology and Petrography of the samplesFor the outcomes of this research, we frst consider interpretation of the results about the Life Cycle Jar, followed by the results achieved from other pottery samples. The Life Cycle Jar exhibits a grain size in micritic quality. The colour of the matrix is brownish-red which is achievable during an oxidative fring régime, and the additives were characterised mostly as quartz, calcite and secondary iron accumulation (Figure 5). Quartz, feldspars and plagioclases are the common additives within the matrix. Quartz is the main mineral within the sample matrix, presenting as fne grains distributed in the micritic matrix. Quartz grains were shown to have had crucial and careful processing, since they have a very comparable grain size. This efect is not visible in the plagioclases and alkali-feldspars, which had defnitely been crushed and added to the raw clayey paste materials (Peterson and Betancourt, 2009). Despite quartz being the leading phase within the matrix, some other key minerals such as, rock fragments, biotite, and low amounts of calcite, have also been considered. These kinds of mineral assemblies are typical for such a volcanic area present around the region (Quinn and Day, 2007; Riederer, 2004). Calcite appears as secondary phases, and grogs are not visible within the fabric of the Life Cycle Jar. However; the optical character of the sample and anisotropic efect of the matrix (matrix bi-refringence), provide the reason for thinking it had a high fring temperature during its manufacture that probably reached over 950°C (Gliozzo, 2020; Maggetti et al., 2011).The textures in the other 9 potteries are described as microcrystalline additives (micritic in size) within a clayey fabric. As shown in Table 2, the mineralogical compositions Table 1.Investigated Pottery sherds from the Keshik cemetery; Sample 10 is the Life Cycle Jar.SampleType of vesselShred typeDecorationInteriorColour pasteExterior1JarBodyPaintedLight redLight greyLight red 2BowlEdgePaintedLight greyLight greyPink 3JarEdgePaintedLight greyLight greyLight grey 4JarEdgePaintedLight redLight redLight red 5JarEdgePaintedLight greyLight greyLight red 6JarBodyPaintedLight redLight redLight red 7JarBodyPaintedLight brownLight greyLight grey 8JarEdgePaintedLight redLight redLight red 9BowlFull bowlBroken crossLight greyLight greyLight grey10 (LCJ)JarFull jarLife cycleBufLight greyBuf
image/svg+xmlIANSA 2022 ● XIII/2 ● 117–128Yasin Sedghi, Farahangiz Sabouhi Sani, Nasir Eskandari, Mohammadamin Emami: Beyond a Decoration; Mineralogical and Micro-structural Study of the Early Bronze Age “Life Cycle Jar” from Keshik Cemetery, Sistan and Balouchistan, Iran122were characterised by means of the occurrences of quartz in phenocrystals, calcite as secondary polycrystals, and the accumulation of iron oxides (seldom grog as well) (Figure 6). Polycrystalline quartz are shown as the efect of transformation processes (Riederer, 2004). Colloidal iron particles in the form of a non-uniform to dark-red accumulation are the other minerals which were observed in microscopic images (Riccardi et al., 1999b). The iron-rich matrix can be interpreted – despite the oxidative atmosphere – by means of the iron-rich clay. The optical character of the samples and anisotropic efect is indicative of a high temperature régime during manufacturing (Riccardi et al., 1999a). These mineralogical constituents are mostly epigenic, and have reacted and decomposed to produce newly-formed crystals. The secondary calcite occurred over time due to the post-burial conditions (Fabbri et al., 2014; Maritan, 2020). According to the local geology, the soil of the region (southeast of Iran) has been classifed as calcareous soil. However; the low amount of calcium oxide suggests a fring temperature more than 850°C and lower than 1000°C for these samples. The colour of the matrices varied from red to green depending on the fring condition from oxidation to reduction (Fabbri et al., 2014; Feathers, 1989). Grog or reused ceramic sherds were not a common constituent in the majority of samples. Grog is the crushed sherds of pottery which is re-added to pottery paste as a fller and acts as a modifer of a clay’s characteristics (Maritan, 2004; Mason and Cooper, 1999). The red matrix suggests that Figure 5.Photomicrographs of the Life Cycle Jar (A & B), depicting tiny grains of quartz, colloidal irons, and secondary calcite. Image A is in PPL mode and Image B is in XPL mode. Qtz: Quartz, Cc: Calcite, Fe: Colloidal Iron Accumulation.Figure 6.Photomicrographs of the other nine samples studied. A) Sample 1 in XPL, B) Sample 2 in XPL, C) Sample 3 in XPL, D) Sample 4 in XPL, E) Sample 5 in PPL, F) Sample 6 in PPL, G) Sample 7 in XPL, H) Sample 8 in XPL, I) Sample 9 in XPL.
image/svg+xmlIANSA 2022 ● XIII/2 ● 117–128Yasin Sedghi, Farahangiz Sabouhi Sani, Nasir Eskandari, Mohammadamin Emami: Beyond a Decoration; Mineralogical and Micro-structural Study of the Early Bronze Age “Life Cycle Jar” from Keshik Cemetery, Sistan and Balouchistan, Iran123the pottery pieces were fred in a well-oxidised atmosphere and the green matrix suggests the fring was in a reducing atmosphere (Maritan et al., 2006). The estimated temperature of the manufacturing process did not exceed 950°C because of the absence of a fused structure in the clayey matrices and as round pores were visible (Maniatis et al., 1983). The soil used during the pottery manufacture was chiefy processed, so that a few pores remained within the texture of the fnished pottery. The macro-textures of the pottery pieces present the same grain-size, homogeneous scattering of the grains, and a stretching of pores, which is indicative of a wheel-made production technique. A thin layer of slip was observed on the surface of the pottery, and were mainly composed of diferent oxides of iron and manganese. Consequently, based on all these similarities between the pottery sherds and the geological setting of the region, the Life Cycle Jar, and other pottery sherds were possibly made with local raw materials.4.2 Crystalline Phase Composition (XRPD)According to the XPRD difractogram (Figure 7), the refned and calculated crystalline phases in the Life Cycle Jar are quartz, calcite, diopside and anorthite (which are also detectable in all ten pottery pieces). The measured crystalline phases, such as pyroxene and anorthite, might confrm the high-temperature fring process of around 950°C (Maggetti, 2001; Maggetti et al., 2011). Difractograms 3, 7, 8 and 9 (XRPD difractograms in Figure 8) were related to the pottery characterised by a grey or dark-grey colour, and difractograms 1, 2, 4, 5 and 6 were related to the pottery with a buf, light red colour. Difractogram 10 belongs to the Life Cycle Jar. The most remarkable phases in the pottery pieces are quartz, which originated from very fne sandy inclusions. Calcite is observed in all samples, having reacted through fring and decomposed to form new crystals. Calcite does not show sharp peaks and appeared around 2θ=31° with wide Table 2.Sample Petrographic data. (+: mostly visible, ±: sometimes detectable, –: not detectable).SampleQuartzphenocrystsQuartzpolycrystallinePlagioclaseFe-oxideCalciteGrogBi-refringenceand fabricationTexture1++–+––RedFine 2++–+––GreenFine 3++–+–±GreenFine 4++–++–RedCoarse 5++–++±GreenFine 6++–+––RedFine 7++±+––GreenFine 8++–+–±GreenFine 9++–+––RedFine10 (LCJ)++±++–RedFineFigure 7. Difractogram of XRPD spectrums for the Life Cycle Jar pottery.
image/svg+xmlIANSA 2022 ● XIII/2 ● 117–128Yasin Sedghi, Farahangiz Sabouhi Sani, Nasir Eskandari, Mohammadamin Emami: Beyond a Decoration; Mineralogical and Micro-structural Study of the Early Bronze Age “Life Cycle Jar” from Keshik Cemetery, Sistan and Balouchistan, Iran124FWHM (full width at half maximum). The intensity peak of calcite at a very low ratio demonstrated occurrences of a not-well-defned crystal structure of calcite in comparison to the quartz, due to the fne micritic grain size of calcite (Nodari et al., 2004; Noghani and Emami, 2014). This is similar in all samples, and describes the fring strategy which was routinely practiced by the potters. Hematite iron phases were also detected in all pottery pieces and are considered to be secondary oxidation phases. The secondary characteristics of hematite are caused due to their accumulation within the matrix.4.3 Micro-chemical and structural investigation through SEM-EDXThe clays that were used to make the Life Cycle Jar cannot be identifed as calcareous due to the amount of CaO constituents, which does not exceed 6 w% as measured by the SEM-EDX (Maniatis, 2009; Maniatis and Tite, 1981). The low amount of carbonate is due to the decomposition of calcium carbonate to other minerals through high-temperature reactions. The micro-structure of the Life Cycle Jar was mostly shown to have a sintered body, but did not have a well-vitrifed structure due to the absence of glassy flaments within the Figure 8. Discriminating between difractogram of XRPD spectrums for light red core and grey core pottery pieces to the Life Cycle Jar pottery.Figure 9. Secondary Electron Microscopic image of the body of the Life Cycle Jar (Sample 10); Image A with 1000× zoom, Image B with 2000× zoom, and Image C with 3500× zoom.
image/svg+xmlIANSA 2022 ● XIII/2 ● 117–128Yasin Sedghi, Farahangiz Sabouhi Sani, Nasir Eskandari, Mohammadamin Emami: Beyond a Decoration; Mineralogical and Micro-structural Study of the Early Bronze Age “Life Cycle Jar” from Keshik Cemetery, Sistan and Balouchistan, Iran125micro-structure of the matrix (Figure 9) (Daghmehchi et al., 2017; İssi et al., 2011). The microstructures show that the samples possess very few pores as a factor for the occurrence of an essential sintering texture (Maggetti et al., 2011; Maniatis and Tite, 1981; Maggetti, 1982). This issue has also been explored during the interpretation of pottery pieces via petrographical observation. The presence or absence of pores in the fred-clay matrix depends on several diverse factors such as crystalline phase abundance, appearance of organic materials and fring conditions (İssi et al., 2011). In contrast to the Life Cycle Jar, the other samples show a typical essential vitrifcation texture and visible micro-structure that allow the estimation of fring to be around 950°C, due to the smooth surface and porosity in the texture of the matrix (Figure 10) (Maniatis and Tite, 1978; Maniatis and Tite, 1981). EDX elemental analysis (Table 3) shows that high amounts of silicon oxide contribute to the composition of the clayey raw materials (kaolinite and/or illite). The alkaline oxides of calcium and manganese can be originated because of the carbonates such as calcite and dolomite (Daghmehchi et al., 2018; Rathossi and Pontikes, 2010a; Rathossi and Pontikes, 2010b). The amount of magnesium oxide in 9 other samples compared to the Life Cycle Jar is higher than that of calcium oxide. A considerable amount of iron oxide is seen inside the pottery’s texture as the remains from the high-iron-content clayey raw materials (Aloupi-Siotis, 2020; Papachristodoulou et al., 2006). The presence of high-iron constituents may suggest the use of clay resources with a magmatic origin (Owliaie et al., 2006).Micro-chemical analysis of the colourant decoration on the surfaces of the Life Cycle Jar is given in Table 4. The most common compounds in the Life Jar colours (Sample 10) consisted of Fe2O3(62.98 w%) and MnO (21.11 w%), with lower amounts of CaO (5.12 w%) and Al2O3(5.09 w%) (Table 4). Iron oxides were mainly used as pigments that are naturally available in various forms from throughout the world (Attaelmanan, 2014; Maggetti et al., 2009). The colour range of iron oxide pigments starts from dark-yellow to red, and brown, depending on the mineral’s hydration and particle size (Okrush and Matthes, 2010). Whereas the hydration of iron oxides such as Fe2O3causes colour changes from purple–red towards auburn red hues. Hydrated iron oxide such as Fe2O3.nH2O has been shown to produce colour changes ranging from warm red to yellow (Aloupi-Siotis, 2020; Berthier et al., 2006). Iron oxides are strongly resistant to acidic, alkaline (poor to medium) conditions and UV as well. Much research evidence has demonstrated that many prehistoric communities used iron-oxide pigments for Figure 10. Secondary Electron Microscopic image from the body of selected Sample 9 (A with 1000× magnifcation), 8(B with 2000× magnifcation) and 7(C with 3500× magnifcation).Table 3.Chemical composition of shreds using EDX point analysis (w%).SampleSiO2Al2O3Fe2O3CaONa2OK2OMgOMnOP2O5PbO157.718.13.340.144.463.58.40.520.440.11249.3722.522.840.379.092.76.780.710.530.42338.6517.3614.610.063.310.310.662.090.830.21430.515.421.990.84.552.030.520.360.020.44547.8417.8216.851.980.050.479.450.590.750.02647.939.788.050.60.221.755.710.80.30.02748.9523.343.561.894.583.589.540.150.510.68849.3623.633.661.956.343.619.490.150.670.71950.321.628.12.254.812.147.350.960.810.31
image/svg+xmlIANSA 2022 ● XIII/2 ● 117–128Yasin Sedghi, Farahangiz Sabouhi Sani, Nasir Eskandari, Mohammadamin Emami: Beyond a Decoration; Mineralogical and Micro-structural Study of the Early Bronze Age “Life Cycle Jar” from Keshik Cemetery, Sistan and Balouchistan, Iran126ornamenting their ceramics (Noll, 1999). Manganese oxides are important compounds in this group of pigments, ranging from yellowish-brown to black. Manganese oxide originates mostly from minerals such as pyrolusite and ramsdellite (MnO2), and were used for ornamenting prehistoric pottery (Molina et al., 2014). Hence, iron oxide and manganese oxide were the frst and second choices for potters to produce black pigments. Accordingly, iron oxide (hematite and/or magnetite) and a little manganese oxide are the colour bases of the painted decoration of this pottery. A mixture of two pigments with iron-oxide bases produces a colour characterised by a dark brown to black appearance (De Benedetto et al., 2002; de Faria and Lopes, 2007).5. ConclusionThe unique Life Cycle Jar and the nine other pottery pieces from the Keshik cemetery were studied in order to determine their chemistry and micro-structure and thus help to interpret their possible provenance. The present study has recognised efective similarities in the applied inclusions and fring condition, and as others such as the vitrifed- or pre-sintered texture within the pottery pieces. Based on chemical and phase analysis of the pottery pieces, the raw materials have a mostly common working style, same geological origin and the same kind of additives used during production. The soil of the Keshik cemetery was shown to contain fragmented sandstone, shale and conglomerate. The pottery pieces contained rounded-grain quartz which was shown to be fuvial in origin, and not the result of crushing. This suggests that the potters might have used the fuvial as well as re-depository soils of the Keshik riverbank to make the pottery. Additionally, the additives were well dispersed in the various textures. The geological setting, in association with the cluster analysis of the pottery pieces, and their manufacture, suggest that the pottery pieces were local in origin. XRPD analysis confrms that the Life Cycle Jar was made with the Figure 11.Microscopic image relating to the surface decoration of the Life Cycle Jar (Sample 10). The mineral grains of colourants are evident in the decoration on the surface as very tiny, and sporadic mineral grains, which are observed so much on the crust of the pottery.Table 4. Chemical composition of painted Life Cycle Jar (sample 10) using EDX point analysis (w%).ElementsAl2O3Fe2O3CaONa2OK2OMgOMnOP2O5PbO10 LCJ5.0962.985.120.361.230.8821.110.070.83
image/svg+xmlIANSA 2022 ● XIII/2 ● 117–128Yasin Sedghi, Farahangiz Sabouhi Sani, Nasir Eskandari, Mohammadamin Emami: Beyond a Decoration; Mineralogical and Micro-structural Study of the Early Bronze Age “Life Cycle Jar” from Keshik Cemetery, Sistan and Balouchistan, Iran127same raw materials and manufacturing techniques as the other investigated ceramic pieces.The pottery pieces are classifed as high-temperature pottery with an estimated fring temperature of 850°C–950°C. The fring regime may have been under oxidative and reduced conditions due to the red-orange and green matrix, and rehabilitation under reduction conditions (grey pottery pieces). Furthermore, the matrix colour of the several red and dark green pottery pieces shows that the fring temperature was about 950°C. According to the analysis of the pigments applied as decoration lines on the surface of the painted Life Cycle Jar, the pigments had to be composed of iron oxide-based minerals for the red-orange colour (such as goethite and hematite), and a favourable manganese oxide (pyrolusite and ramsdellite) to produce the brown-black colour.AcknowledgmentsThe authors are grateful for permission granted by the Research Centre of Archaeology, Iranian Cultural Heritage Organisation, for the survey and sampling from the Keshik cemetery. Advice and support from Professor Rémy Chapoulie and other colleagues from the IRAMAT Institute (Institut de Recherche sur les Archéomatériaux-Centre de Recherche en Physique Appliquée à l’Archéologie) is gratefully acknowledged. We are grateful for comments from two anonymous reviewers; any remaining errors are our own.ReferencesALOUPI-SIOTIS, E., 2020. Ceramic technology: how to characterise black Fe-based glass-ceramic coatings. 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