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The struggle between thermodynamics and kinetics: Phase evolution of ancient and historical ceramics
This contribution is dedicated to the memory of Professor Ursula Martius Franklin, a true pioneer of archaeometric research, who passed away at her home in Toronto on July 22, 2016, at the age of 94. Making ceramics by firing of clay is essentially a reversal of the natural weathering process of rocks. Millennia ago, potters invented simple pyrotechnologies to recombine the chemical compounds once separated by weathering in order to obtain what is more or less a rock-like product shaped and decorated according to need and preference. Whereas Nature reconsolidates clays by long-term diagenetic or metamorphic transformation processes, potters exploit a ‘short-cut’ of these processes that affects the state of equilibrium of the system being transformed thermally. This ‘short-cut’ is thought to be akin to the development of mineral-reaction textures resulting from disequilibria established during rapidly heated pyrometamorphic events (Grapes, 2006) involving contact aureoles or reactions with xenoliths. In contrast to most naturally consolidated clays, the solidified rock-like ceramic material inherits non-equilibrium and statistical states best described as ‘frozen-in’. The more or less high temperatures applied to clays during ceramic firing result in a distinct state of sintering that is dependent on the firing temperature, the duration of firing, the firing atmosphere, and the composition and grain-size distribution of the clay. Hence, the salient properties of the ceramics have to be assessed in a temperature-time-composition space. Owing to the variability of clay composition, the mineralogical processes during thermal transformation of clay minerals can be very complex, not least because most reactions occur far removed from thermodynamic equilibrium and hence are kinetically controlled; that is, they are time- and temperature-dependent. Indeed, kinetics imposes constraints on thermodynamics by retarding reaction rates because of low temperatures, large temperature gradients present in primitive pottery kilns, short reaction times, inhomogeneously distributed reaction partners, and varying redox conditions triggered, for example, by ingress of air during reducing firing cycles. In the context of ceramic technological development over time, the role and development of pottery technology within complex societies is discussed. The close relationship between pottery development and changes in life/societal organization appears to be a major driver in this endeavour. In this chapter, the phase evolution of some typical ancient and historical ceramics will be traced using ceramic phase diagrams, i.e . chemographical expressions of Goldschmidt’s mineralogical phase rule. In particular, the systems CaO–Al 2 O 3 –SiO 2 (in which most ancient low- to medium-fired ceramics can be accommodated), K 2 O–Al 2 O 3 –SiO 2 (applicable to high-fired Chinese stoneware and European hard-paste porcelain) and Na 2 O–CaO–(Al 2 O 3 )–SiO 2 (typical of some ancient Egyptian and Mesopotamian alkaline glazes and French soft-paste porcelain) are discussed.
Phase and compositional analysis of a Sèvres soft paste porcelain plate from 1781, with a review of early porcelain techniques
Paul-Louis Cyfflé’s (1724–1806) search for porcelain
Front Matter
Abstract First, a brief overview of the tasks and the historical development of archaeometry will be given. Although archaeometry is generally doing well, a few issues currently faced by this discipline will be outlined. These include: (1) funding for projects and research positions; (2) the appeal of archaeometry to a new generation of academics; (3) the standard of publications; (4) the safeguarding of and the immediate access to scientific data.
A review of the non-destructive identification of diverse geomaterials in the cultural heritage using different configurations of Raman spectroscopy
Abstract Non-destructive Raman microscopy (RM) applied to geomaterials in the cultural heritage is reviewed by means of explaining selected examples representative of the different kinds of geomaterials that can be characterized and of the different kinds of analytical configuration that can be employed. To explain the versatility and considerable analytical potential of RM that result from its unique combination of capabilities, the first sections summarize the theory and practice of the method and its advantages and disadvantages. The most modern configurations (mobile RM (MRM) and ultra-mobile RM; micro-mapping and imaging; telescopy) are described. Applications in the new age of ‘don’t move it, don’t even touch it’ archaeometry have previously been classified into 10 domains, seven of which concern geomaterials: gems; rocks; ceramics; corroded metals; coloured vitreous materials; and mineral pigments on an inorganic or organic substrate. The representative examples here include all these domains and cover the time range from Prehistoric through Egyptian, Roman, Meso-American, Medieval, Chinese, Renaissance and Mogul cultures to modern colouring of glass and a contemporaneous simulation of submarine archaeology.
The Neolithic pottery of Abri Pendimoun (Castellar, France): A petro-archaeometric study
Abstract Middle and Late Neolithic ceramics from Abri Pendimoun (Castellar, France) and their geological raw materials have been investigated to characterize the ceramic bodies and to determine the possible provenance of raw materials. Petrographic, mineralogical and energy-dispersive spectrometry analyses were undertaken to define the compositional parameters of sherds and to clarify the relationship between Square Mouthed Pottery-phase I (VBQ I) and Chassey Culture. The ceramic bodies were generally made from glauconite-rich layers and terra rossa, unprocessed or mixed in variable proportions. Different kinds of temper, such as carbonates and/or aplite fragments, were added to the mixtures. Although most of the analysed ceramics were produced locally, a few mixtures show the addition of exogenous rocks. Although these ceramics could be interpreted as imported, we demonstrate that local clayey materials were used at Abri Pendimoun. The hypothesis that pottery was imported can therefore be ruled out. A small amount of crushed calcite (5%) was added to some glauconitic pellet mixtures. Pots made with this mixture are normally referred to the VBQ I. This combination of mixture and shape indicates that there was an important link between the VBQ I and Chassey Cultures.
Abstract Apulia is the best-represented region in Italy as far as archaeometric analyses of Neolithic pottery are concerned. Cross-checked use of petrological (optical microscopy), mineralogical (X-ray powder diffraction) and chemical analyses (X-ray fluorescence) have been performed, in the Dipartimento Geomineralogico of Bari University, on 375 Early to Late Neolithic (from the seventh to the fourth millennium BC) pottery samples from the Tavoliere and Murge areas. A correlated analysis of 134 samples of the main clayey deposits of the two areas was also conducted. Generally local clays were used and, in some cases, the exploitation of a range of different local fabrics has been verified. In Middle Neolithic sites, the use of non-local clay, probably imported, has been also determined. Few finished pots were actually exchanged at an inter-site scale during the Neolithic. Preparation of raw materials has shown different choices followed by ancient potters. Clays are usually more or less refined and the use of mineral temper such as sand, quartz, calcite and grog has been found. The maximum temperature reached during firing is usually between 600–700 and 850 °C. For some Middle Neolithic fine painted pottery higher temperatures have been suggested (between 850 and 1050 °C), revealing a better firing control and the use of kilns.
Late La Tène pottery from western Switzerland: One regional or several local workshops?
Abstract A total of 203 pieces of fine ceramic and four clays from seven sites of western Switzerland (Bern, Genève, Grotte du Four, La Tène, Marin, Saint-Triphon-Massongex and Yverdon) were studied chemically and mineralogically to determine if there was local production at each site and if trade links existed between the sites. Firing wasters from Bern and the region of Genève indicate local ceramic production. The sherds are often contaminated with secondary phosphorus and, in the case of Bern, copper. Most of the fine ceramic is CaO-poor, contrasting with the CaO-rich clays. Based on the chromium and nickel concentrations, it can be subdivided into two distinct groups. The majority of the sherd populations from Genève, Saint-Triphon and Massongex, as well as a few specimens from Bern, La Tène and Yverdon, have high Cr and Ni values. The remaining sherds have low Cr and Ni concentrations. The analyses show that: (1) the fine ceramic from each of the seven sites forms an often inhomogeneous and widely dispersed group, distinct from the others; consequently, it is most probably a local or regional product; (2) ceramic import is probable for one piece from Grotte du Four (provenance Yverdon); (3) the Late La Tène fine ceramic was manufactured mainly from silicate or silicate-carbonate, fat to lean clays.
Characterization of Maltese pottery of the Late Neolithic, Bronze Age and Punic Period by neutron activation analysis
Abstract A set of 41 samples from Tas-Silg, Malta, has been analysed by neutron activation. It contained nine ware groups formed by visual examination covering the Late Neolithic, Bronze Age and Punic Periods ( c . 3000–218 bc ). Despite this diversity and long time range, seven of these ware groups, including the ‘Thermi Ware’, all have a similar chemical composition and, therefore, have been made from the same clay. This points most probably to a local origin. One group from the Punic Period, containing only Bricky Red cooking ware, is chemically separate and represents a second distinct pattern probably assignable to a local production. Five amphora sherds also from the Punic Period, and consisting of a micaceous fabric, all have different chemical characteristics and are probably imports from overseas production sites of unknown location.
Cobalt blue painted pottery from 18th Dynasty Egypt
Abstract Cobalt blue painted pottery was produced in New Kingdom Egypt, with the heyday for its production being from about 1400 bc to 1200 bc . Previous scientific examination has established that the cobalt blue pigment was a CoAl-spinel, which it was suggested was produced from cobaltiferous alums from the Western Desert of Egypt. In the present paper, quantitative analyses of a range of cobalt blue painted pottery have confirmed the Western Desert as the source of the cobalt blue pigment but suggested that the cobaltiferous alums used for the pottery differed in composition from those used in the production of contemporary cobalt blue glass. The pottery bodies were produced using either non-calcareous Nile silt or calcareous clay. Before being painted, the Nile silt bodies were first coated with pale firing calcareous clay slip to which gypsum had probably been added.
Abstract The Iron Age ceramic technology used in the manufacture of functional pottery from Galilee was studied. Applied methods included petrography, X-ray diffraction, infrared spectroscopy and chemical analyses. The results demonstrate that the potters in biblical times had knowledge of raw materials and manufacturing technologies, enabling them to select suitable ones, according to their advantages, for the manufacture of cooking pots, storage jars and tableware vessels. The paper describes the petrography of the pottery, the composition of the ceramic matrix, the firing temperature, the tempering of the cooking pots, the processes that allow consolidation of the ceramic and the origin of the pottery. The results are placed in an archaeological context.
Abstract Late Archaic to Early Woodland (4500–3000 years bp ) Stallings Island Culture fibre-tempered plainware pottery is found from northern North Carolina to NW Florida and is often separated into two temper groups (Stalling and Orange series) based upon fibre type. Thirty-four sherds were studied to determine textural or mineralogical characteristics to assist in form and type separation. This study finds that only a few of the sherds were dominated by fibre. The fibre is visible as secondary porosity (voids) with some carbonized remains and exhibits specific shape and orientation at different locations within the sherd. Only two sherds had carbonized stem fragments that allowed identification of the Spanish moss ( Tillandsia usnedoides ). The remainder of the Crescent site plainware pottery has such low (to no) fibre contents as to be indistinguishable from similar age sand-tempered Thorn’s Creek wares. The identity and textural features of the fine-grained aplastic minerals (quartz, feldspar, biotite and opaque minerals) in the paste are similar in both fibre- and non-fibre-tempered sherds, and this suggests that the materials used are consistent with sediment extraction from a fluvial coastal plain or estuarine setting. These observations indicate that the degree of fibre incorporation in these sherds may be related to the specific clay source (or manufacturing location) or represent examples of an evolving pottery manufacturing process within the Stallings Island Culture.
Abstract In this paper we present bulk X-ray fluorescence-X-ray diffraction (XRF/XRD) and microanalytical scanning electron microscope-electron microprobe analysis (SEM-EMPA) data on historical bricks from Medieval or Renaissance buildings of Ferrara (NE Italy) to provide insights into the nature and provenance of the raw material as well as clues on the sintering techniques. Chemical data indicate that the starting materials were obtained by mixing high Cr-Ni clay and subordinate sand (both quarried from the Po river alluvial deposits) with the possible introduction of a Na-rich flux component. Thin-section observation, XRD and micro-analytical data indicate the presence of key accessory phases such as pyroxene, amphibole, epidote and rare olivine in the pre-fired mineral assemblage, confirming the utilization of the Po river sediments. Recognition of neo-formation firing phases (e.g. melilite, wollastonite), together with composition of micas, amphiboles and interstitial glasses, indicate kiln temperatures between c . 800 and 1000 °C. This provides guidelines for making new compatible and durable bricks to be utilized for restoration, and contributes to the preservation of historical masonry.
Abstract Gökeyüp cooking pottery is a particular type of pottery produced according to ancient craft tradition in western Turkey. It is made by mixing 75 wt% of local red and green smectitic clays with 25 wt% of local gneissic temper. Both temper and tempered objects are rich in MgO, as can be seen from XRF analyses. The vessels are coated with a sheet-silicate enriched layer, corresponding to the <2 mm sieved fraction of the crushed gneissic temper. The pottery is fired for 45 min using the bonfire technique. Apart from the dehydroxylation of the smectites, no clear mineralogical difference can be observed between the unfired and fired products. The reduction factor FeO/FeO tot reveals no significant oxidizing or reducing firing conditions. As evidenced by SEM-EDS analyses, there is no chemical difference between the unfired and externally fired micas of the coating. The golden colouring is therefore due to the oxidation of the biotites during firing.
Chemical and mineralogical investigations of majolicas (16th–19th centuries) from Laterza, southern Italy
Abstract Laterza (southern Italy) was the most important town for the manufacture of Apulian majolica ceramic from the 16th century until the end of the 18th century. The Laterza majolicas have previously been subjected to only preliminary analyses. This study extends the archaeometric knowledge of the Laterza productions with mineralogical, petrographical and chemical characterizations of ceramic body, glazed coating and pigments of the majolica. A number of 16th to 19th century pottery and tile fragments of majolica have been studied and compared with clay from local and surrounding deposits. Analyses were carried out by optical microscope, scanning electron microscope, energy-dispersive spectrometry, X-ray powder diffraction, X-ray fluorescence and inductively coupled plasma. A purification process of the raw material is suggested and for some fragments, doubtfully attributed to Laterza, a different place of manufacture. Slip (‘ingobbio’) was never found under the glaze. Si, Pb and Sn are confirmed as the principal elements in the tin-glazed coatings. The differences in the glaze opacity were attributed to different manufacturing techniques and not simply the quantity of tin. The orange–yellow colour is due to a Sb–Pb compound; black to Ni with a lower amount of Co, Fe and Sb; blue to Co, As, Fe and Ni; and Mn is the pigment of the violet–brown.
Abstract Islamic and Hispano-Moresque glazes from the 10th to 15th centuries found in various archaeological sites, most of them workshops, are studied to show the technical evolution of the medieval glazing process. The technology seems to show a simplification: the early Islamic glazes were applied on prefired bodies and after fritting a lead–silica mixture, whereas for the later Islamic productions the raw materials for the lead glazes were not fritted and they were applied over unfired bodies. The same simplified technology was used in the Hispano-Moresque workshops. In the Islamic workshops lead glazes were coloured by adding elements (Fe, Cu, Mn), whereas the múdejar technology simplified the process by using only one recipe to produce pots of different colour. This was achieved by applying the glaze in a different manner (on one side of the pot to obtain yellow or on both sides to obtain green), or using different pastes (already used to produce pottery for different uses). Finally, there are differences between Islamic and Hispano-Moresque tin glazes related to the crystal size of the opacifier (tin oxide crystals), which should indicate some technological differences in temperature, glaze composition and the process to obtain the frits because of the high dependence between viscosity, temperature and crystal nucleation and growth.
Archaeometric analyses of game counters from Pompeii
Abstract Among the glass finds of the Pompeii excavations, numerous objects of opaque and transparent glassy material of different colours were recovered and classified as game counters. The main aims of this work were to characterize these samples so as to identify the materials used as colorants and opacifying agents, and subsequently to deduce the technology used for their production. The results of the chemical and mineralogical analyses obtained for game counters were also compared with those obtained for transparent and opaque glass artefacts. The chemical analyses were carried out, using only 300 mg of sample, by both wavelength-dispersive electron microprobe and X-ray fluorescence analysis. The crystalline phases present in the opaque glass were identified using both an automatic X-ray powder diffractometer and a Gandolfi camera. Secondary and backscattered electron images were obtained to study the distribution and morphology of the opacifier particles, and qualitative chemical analyses were obtained with an energy-dispersive system. All the game counters analysed can be classified as silica–soda–lime glass. Two calcium antimonates (CaSb 2 O 6 and Ca 2 Sb 2 O 7 ) were identified in the opaque white, green and blue glass, and Pb 2 Sb 2 O 7 particles were detected in the opaque yellow glass. Particles of metallic copper were detected by both energy-dispersive system and X-ray powder diffraction. These results support the hypothesis that transparent game counters were obtained by remelting of fragments of common transparent artefacts. In contrast, opaque finds were probably produced using the glassy paste employed in the production of mosaic tesserae.
Pre-industrial glassmaking in the Swiss Jura: the refractory earth for the glassworks of Derrière Sairoche (ct. Bern, 1699–1714)
Abstract Fragments of the melting furnace and several crucibles of the glassworks of Derrière Sairoche are compared with local raw materials. Principal component analysis (PCA) based on the chemical composition and on the grain-size distribution of the archaeological and natural materials demonstrates that the analysed samples were made from the same raw material and that local clayey sands (Hupper, Sidérolithique) were exploited. Availability in situ of good raw materials made tempering unnecessary. Their high melting point ( c . 1600 °C) allowed good performance in service conditions at temperatures up to 1500 °C. Moreover, because of low Fe 2 O 3tot concentrations, batch-glass contamination was avoided.
Glass production in Late Antiquity and the Early Islamic period: a geochemical perspective
Abstract First millennium AD glass production was divided between a relatively small number of workshops that made raw glass and a large number of secondary workshops that fabricated vessels. Glass compositions reflect the primary glassmaking source. For most of the period, Egyptian mineral soda was fused with lime-bearing siliceous sand to produce soda–lime–silica glass. The location of the Belus glassmaking sand, which is known from the classical literature, is located on that part of the Levantine coast where iron contents are lowest. 87 Sr/ 86 Sr of primary glass from workshops in the Levantine region is close to that of modern seawater, and confirms the use of beach sand, which contained shell. Heavy mineral assemblages of Levantine beach sands are dominated by hornblende, hence the primary glasses are characterized by very similar trace element signatures. Glasses believed on archaeological grounds to have been made in other regions, for example in inland Egypt, may have higher 87 Sr/ 86 Sr, reflecting terrigenous sources of lime, and have different trace element signatures. Compositional data for glasses from as far away as Britain suggest origins of the glass material in the Eastern Mediterranean. Recycling of old glass may be recognized by the presence of elevated transition metals. The use of plant ash as a flux became dominant practice in the ninth century and preliminary data for plant ash glasses from the early Islamic world indicate that primary production centres may be separated using strontium and oxygen isotopes as well as by major and trace elements.