Characterisation of archaeological mortars and plasters from kyme (Turkey)

The present study focuses on the compositional characterisation of Roman, proto-Byzantine and Medieval mortars, sampled in the archaeological site of Kyme (Turkey), an Aeolian city, founded in the middle of the XI century BC by Greek populations. The mortars were studied through elemental (SEM-EDS, XRF), mineralogical (XRPD, De Astis calcimeter) and petrographic (polarised optical microscopy) analysis. The comparison between the samples allowed us to emphasise compositional differences within mortars of the same historical period.In particular, we detected the prevalent use of cocciopesto, which was used as a pozzolanic additive to create hydraulic mortars in the Roman and Byzantine period. The cocciopesto was used to improve the technological properties of an initially slaked lime. Furthermore, compositional similarities allowed us to attribute an unknown sample to the Roman period. Our study also pointed out the fact that the lower quality mortars belonged to the Medieval period. As a matter of fact, the most friable sample belonging to the Middle Ages turned out to be a mixture of clay, lime and volcanic sand.     

CHARACTERIZATION OF PLASTERS AND MORTARS AS A TOOL IN ARCHAEOLOGICAL STUDIES: THE CASE OF LARDIRAGO CASTLE IN PAVIA,NORTHERN ITALY*

Plasters and mortars from Lardirago Castle (Pavia, northern Italy) have been characterized by means of petrographical and chemical analyses in order to achieve technical and historical evidence of material production. The study focused on the oldest nucleus of the structure, where hidden plastered masonry has been discovered recently. Textural and compositional data of the binder and the aggregate fractions were collected by means of optical microscopy and electron microscopy coupled with microanalysis. These data permit the identification of building materials with similar technical and compositional characteristics, which can be related to different building phases.     

Characterisation of archaeological mortars from Pompeii (Campania,Italy) and identification of construction phases by compositional data analysis

This work describes the compositional characterisation of coccciopesto and natural pozzolanic mortars sampled in the Regio VI area of the archaeological site of Pompeii, with particular reference to the Casa di Pansa in Insula 6 and Casa 17 in Insula 2. Samples were studied by optical microscopy and analysed by XRF, SEM-EDS, LA-ICP-MS and XRPD. The XRF and SEM-EDS data, subjected to multivariate analysis (cluster analysis), identified the three main construction phases involved in building the Casa di Pansa. In addition, mineralogical and petrographic characteristics of the aggregate were determined and found to be compatible with pyroclastic deposits from the volcano Vesuvius. Study revealed C–S–H phases in the binder, due to pozzolanic hydration phemomena of hydrated lime with cocciopesto and natural pozzalana.     

Mineralogical and Mechanical Properties of Masonry and Mortars of the Lucknow Monuments Circa the 18th Century

The Lucknow monuments of the 18th century are large masonry structures built using thin burnt-clay bricks (Lakhauri) and lime-crushed brick aggregate (surkhi) mortars. Investigations were carried out to characterize the engineering properties of old masonry materials and new mortars being used for renovation work. Mechanical properties of reclaimed Lakhauri bricks were found comparable to good quality contemporary bricks of the region. Moreover, X-ray diffraction (XRD) and scanning electron microscopy–energy dispersive X-ray spectrometry (SEM-EDS) analyses indicated that mineralogical composition is not too different, except for few minerals. The lime-surkhi mortar used in old masonry work was found to be lime-rich with binder to aggregate ratio of approximately 1:2 to 3 by volume. The renovation mortar had poor hydraulic property as compared to old mortars indicated by thermal gravimetric analysis–differential thermal analysis (TGA-DTA) analyses. The compressive behavior of multi-wythe recreated Lakhauri masonry prisms was characterized with low compressive strength, low modulus, and significant deformability which result in lower stress demands imposed on the structural assemblages by various environmental forces.     

Paper 5: Historic Mortars from the Coudenberg Archaeological Site: Characterization and Source of Raw Materials

Abstract

The characterization of historic mortars by means of a concise methodology of material analyses can provide crucial information with regard to the origin of the raw materials and the ancient mortar technology. For the analysis of the historic mortars of the Coudenberg archaeological site, the methodology consists of optical and scanning electron microscopy, simultaneous thermal analysis, and an acidic treatment. These analyses were carried out on a total of seventeen samples lifted from various areas in the site, in function of the building chronology resulting from a historic built investigation. The type of binder and aggregate as well as their volumetric ratio were determined.

Both binder and aggregate present distinctive features, which made it possible to identify the probable geological provenance of the raw materials. The observations are verified with available historical records regarding the construction of the main banqueting hall — the Aula Magna — and the use of raw materials such as limestone and sand for the production of lime and construction purposes.     

The Evolution of the Vitruvian Recipes over 500 Years of Floor‐Making Techniques: The Case Studies of the Domus delle Bestie Ferite and the Domus di Tito Macro (Aquileia,Italy)

The paper reports the results of a research project aimed at the characterization of the floor bedding mortars of two Roman houses in Aquileia (north‐eastern Italy), the Domus delle Bestie Ferite and the Domus di Tito Macro. Seventy floor bedding mortars of the two domus were selected and almost half were fully minero‐petrographically characterized by means of optical microscopy operated in transmitted light (OM‐TL), X‐ray powder diffraction analyses coupled with quantitative phase analysis by means of the Rietveld method (XRPD‐QPA) and scanning electron microscopy with EDS microanalysis (SEM–EDS). The results indicate an evolution of the mortar preparation techniques over time in the mosaic of both houses. The materials are compared to the traditional Roman recipes for specific construction techniques.     

The painting of the Etruscan “Tomba della Quadriga Infernale” (4th century BC), in Sarteano (Siena, Italy): technical features

This work presents the results of an investigation of the painting technique used in the Etruscan tomb “Tomba della Quadriga Infernale”. This tomb was discovered in Sarteano (Siena, Italy) in October 2003 and dated back to the second half of the 4th century BC. Red, dark red, pink, yellow, white, black, and grey colours were used in the tomb in order to create paintings, which now represent a very precious record of the Etruscan art of wall painting in a hypogeal environment. The technical features of the painting were revealed by stratigraphy using optical and electronic microscopy. The components and preparatory layers of the painted areas were characterized using Fourier transform infrared spectroscopy (FTIR), energy dispersive X-ray microanalysis (SEM-EDS), X-ray diffraction (XRD), and gas chromatography/mass spectrometry (GC/MS). XRD, SEM-EDS, and optical microscopic techniques were also used for mineralogical analysis of the rock substrate. The SEM-EDS and FTIR analyses showed that red and yellow ochre, calcite, and vegetable charcoal were used to paint the walls of the tomb: the pigments, either alone or mixed together, were utilized to produce pure colours (red, yellow, white, and black) and intermediate tonalities (pink, dark red, and grey). SEM-EDS, FTIR, and XRD highlighted that the painting was made on a preparatory layer of calcite, applied onto a levelling material made up of calcite, clay minerals, quartz, and iron oxides. GC/MS analyses revealed that egg was used as an organic binder to disperse the pigments.     

Archaeometric study of natural hydraulic mortars: the case of the Late Roman Villa dell’Oratorio (Florence,Italy)

This paper shows the results of a multidisciplinary study carried out on the mortars from the Late Roman Villa dell’Oratorio (fourth-sixth ad), an aristocratic mansion built in the lower Valdarno (Florence, Italy). Thirty-one bedding mortar and plaster samples were analysed through optical microscopy, thermogravimetric analysis, X-ray powder diffraction and scanning electron microscopy with energy-dispersive X-ray spectroscopy for determining the chemical, mineralogical and petrographic characteristics, while their main physical properties were measured by geotechnical procedures. The collected data indicates that the analysed mortars are made up of very fine to coarse river sand aggregate mixed with white to yellowish-white natural hydraulic lime binder mainly consisting of mixtures of prevailing calcite and hydraulic compounds. With regard to the origin of the raw materials, the aggregates were recognized to be selected Arno river sands, and the binders are the burning product of a local marly limestone (ex Alberese). Therefore, the mortars of the Late Roman Villa dell’Oratorio are one of the first uses of natural hydraulic lime in the lower Valdarno.     

Ceramic findings from the archaeological site at Aiano-Torraccia di Chiusi (Siena,Italy): a multi-analytical approach

In 2005, the remains of a Roman villa, dating from the early fourth to the sixth centuries ad, were discovered at the archaeological site of Aiano-Torraccia di Chiusi (Siena, Italy). After being abandoned in the sixth century ad, the complex was occupied by a group of Ostrogothic or Lombardic artisans in the period between the sixth and the seventh centuries ad. Many ceramic remains (coarse pottery and red slip ceramics) from the first to the seventh centuries ad have been discovered on this archaeological site. These findings have been analysed using different analytical techniques (optical microscopy (OM), X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscope-energy dispersive spectroscopy (SEM-EDS), attenuated total reflection Fourier transform infrared (ATR-FTIR), and micro-Raman in order to characterize the ceramic body, the coating, the temper, and to investigate the compositional relationship between the different kinds of ceramics. The use of different techniques on the same samples yielded information at different scales. OM and SEM-EDS yielded interesting information on the coarse pottery: the analyses performed on some minerals and rock fragments suggest that stone tesserae from the Roman villa (in the form of numerous marble fragments) were used in the production of this pottery. Bulk analyses (XRD and XRF) and subsequent micro-analyses (SEM-EDS, ATR-FTIR, and micro-Raman) of the red slip pottery revealed clear chemical, mineralogical and textural differences: some ceramics (the TCC sample group) typically have a Fe-enriched coating while others (the INGR sample group) present a clear difference in grain size but no chemical or mineralogical differences between the ceramic body and the coating.     

Mineralogical analysis and provenancing of ancient ceramics using automated SEM-EDS analysis (QEMSCAN®): a pilot study on LB I pottery from Akrotiri,Thera

A wide range of existing mineralogical and geochemical methodologies such as optical microscopy, X-ray diffraction, manual scanning electron microscopy, ICP-MS and INAA have been utilised in the analysis of ancient ceramics, in attempts to elucidate patterns of regional trade and interaction. However, advances in automated scanning electron microscopy with linked energy dispersive spectrometers (SEM-EDS) have created the potential to offer a seamless combination of textural and mineralogical data based on the acquisition of energy dispersive spectra that has so far been unattainable with existing techniques. In this pilot study on pottery from the Cycladic Bronze Age site of Akrotiri (Thera), we have quantified the mineralogy of the ceramics based on automated SEM-EDS using QEMSCAN^® technology and imaged the textures of the ceramics through compositional mapping. Thirteen samples were analysed and, based upon the automated analysis, four groups of ceramic compositions are defined. These data are consistent with, but also refine, previous traditional petrographic examination of the ceramic samples, and enable the likely provenance of the raw materials used in the ceramic manufacture to be identified. This technique allows the acquisition of fully quantitative data, not only for the larger inclusions within the ceramics but also for the typically finer-grained groundmass/matrix, whilst also providing the overall texture of the ceramic.     

A Multidisciplinary Approach for the Archaeometric Study of Pozzolanic Aggregate in Roman Mortars: The Case of Villa dei Quintili (Rome,Italy)

This contribution focuses on the study of historical mortars from a Roman archaeological site known as Villa dei Quintili, a monumental villa located in the south‐eastern part of Rome (Italy). The study was carried out on 38 mortar samples, collected from several edifices within the complex. A multi‐analytical approach, including polarized optical microscopy, scanning electron microscopy coupled with energy‐dispersive system and laser ablation inductively coupled plasma mass spectrometry, was used to analyse the pozzolanic material used for the preparation of mortars. Data obtained on both major and trace elements were compared with the compositions of Pozzolana Rossa, Pozzolana Nera and Pozzolanella samples from the Alban Hills volcanic district, collected from a historic quarry nearby, as well as with literature data. The results of such a multidisciplinary approach allowed us to recognize the use of all three pozzolan types for the aggregate fraction of examined mortars from the Villa dei Quintili.     

Microstructures of Building Materials from Huaca De La Luna,Peru

ABSTRACT

The microstructures of building materials from the archaeological complex of Huaca de la Luna on the northern coast of Peru is assessed for the first time by a multiscale approach. The multiscale microstructural characterization used laboratory techniques including optical microscopy, scanning electron microscopy, X-ray microtomography, and both gas and powder pycnometry. Optical microscopy revealed the presence of organic matter and shell fragments and X-ray microtomography showed differences in the sizes and connectivity of pores. The BET (N₂ gas adsorption) specific surface areas showed greater presence of clayey matrix in the mortars. No significant differences among mortars and brick fragments mineralogy were detected by X-ray diffraction, so the larger amount of fine binding matrix in the mortars suggests that they were produced blending raw material with different grain sizes. The aim of this study is to provide data that can be used for a better understanding of the Moche culture, its construction techniques, and to support conservation strategies of the archaeological heritage.     

Wall Paintings from the Roman Emona (Ljubljana,Slovenia): Characterization of Mortar Layers and Pigments

This study concerns the investigation of mortar layers and pigments of wall paintings from the Roman town of Emona (Ljubljana, Slovenia). Fragments of wall paintings consist of up to three preserved mortar layers. The mineralogical–petrographic compositions of the mortars were determined by means of optical microscopy and FT–IR spectroscopy. The investigated samples were divided into several groups based on similar thicknesses of the mortar layer, the binder colour and the composition of an aggregate. Furthermore, the results of mercury intrusion porosimetry showed that mortar layers consisting of carbonate grains exhibited lower porosity with respect to layers with mainly silicate grains, which is attributed to the angular shapes of carbonate aggregate. This is in accordance with the drilling resistance measurement system test (DRMS), confirming that layers with angular carbonate grains are harder than those with addition of rounded silicate ones, due to the good packing effect. The wall paintings were mainly executed using the fresco technique, while for some details secco was used. The identified pigments were red and yellow ochre, green earth, Egyptian blue, carbon black and lime white; all of them belonged to the so‐called austere pigment, which is quite common in Roman wall paintings.     

Materials Characteristics of Roman and Arabic Mortars and Stuccoes from the Patio De Banderas in the Real Alcazar of Seville (Spain)

This study discusses the materials and traditional knowledge used in the manufacture and application of lime mortars and stuccoes by Romans and Arabs in Seville (southern Iberian Peninsula). All of the samples studied contain calcite as a binder, combined with aggregates based on river sand from the filling materials of the Guadalquivir River's depression, located in the vicinity of the Real Alcazar Palace in Seville, Spain, where the artefacts were discovered. The Romans used high‐quality production technology, as evidenced by the careful selection of raw materials as well as by the adequate binder‐to‐aggregate ratio and the elevated homogeneity of the mortars and stuccoes. The suitable distribution of aggregates resulted in higher density values for Roman fragments than for Arabic ones. Results derived from Arabic samples suggest a decline in technology manufacture over time. This work provides useful information, particularly regarding the Roman and Arabic periods in the Iberian Peninsula. The analytical techniques employed in this study were X‐ray diffraction (XRD), X‐ray fluorescence (XRF)—using conventional and portable systems, scanning electron microscopy (SEM), petrographic microscopy, differential thermal analysis/thermogravimetry (DTA/TG), particle‐size analysis and mercury intrusion porosimetry.     

法门寺地宫出土唐髹漆平脱秘色瓷碗髹漆工艺初探

在1987年的法门寺地宫考古发掘中,出土一对髹漆平脱秘色瓷碗,是秘色瓷与金银工艺、髹漆工艺完美结合的珍贵文物。为了对其髹漆工艺进行了探讨,本研究利用显微观察、扫描电镜能谱分析和红外光谱分析等方法,对髹漆残块、银扣残块样品进行检测分析。在此基础上,提出了其髹漆工艺的流程。研究结果可为文物保护修复、科学技术史和艺术史研究提供可靠参考。     

Technology of Medieval Mortars: An Investigation into the Use of Organic Additives

This work proposes a multi‐analytical approach to determine the additives in historical mortars, the use of which is widely described in bibliographical sources, but has rarely been reported in the literature. A protocol to thoroughly analyse mortars was created (optical microscopy, X‐ray diffraction, infrared spectroscopy, thermal analyses and gas chromatography – mass spectrometry). These techniques, which had already been carried out on samples from various sites from the Roman to the modern era, determined that additives had only been used in the mortars from the internal masonry at our sampling site: the medieval military shipyard of Amalfi (Italy). The investigations yielded information on the production technology, and FT–IR and GC–MS revealed a saccharide material‐based additive in the mortars, of plant origin. The FT–IR spectra suggested the presence of a natural gum, which has been used since ancient times to strengthen the cohesion properties of mortars and their resistance to tensile stress.     

Metallurgical study on some Sasanian silver coins in Sistan Museum

Elemental analyses and microstructural studies of historical metal artifacts provide researchers with invaluable and priceless information about metal extraction technology and the procedure of creating artifacts. In addition, the information is helpful for knowing about the metallurgical processes of the artifacts. This study was conducted by a microscopic examination and elemental analyses of seven Sasanian silver coins preserved in the Sistan Anthropology Museum, Iran. For the purpose of this study, three methods were employed: first, the proton induced X-ray emission microanalysis (micro-PIXE), to determine the main and trace elements of the coins; second, scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDS), to perform elemental analysis to identify impurities of the metal; and third, microstructural analysis of the coins which was carried out with an optical microscope (OM). The elemental analyses identified Ca, Cu, Ag, Au, and Pb in the coins. The high quantity of Ag in samples validated the application of advanced and accurate cupellation technology for refining silver and separating impurities from raw ore. The gold concentration in the coins indicated the use of non-galena ore for silver extraction. Additionally, the microstructural analyses of samples pointed to the application of thermo-mechanical processes on coins.     

Characterization of lime carbonates in plasters from Teotihuacan,Mexico: preliminary results of cathodoluminescence and carbon isotope analyses

This study characterizes the degree of calcination of lime in lime plaster samples from Teotihuacan, the capital of a regional state in prehispanic Central Mexico. Lime plaster production consists of multiple steps, from the firing of raw materials to the mixing of lime and aggregate and the final application. While previous studies have focused on the compositional variability, specifically the recipe of lime plasters and mortars, the characterization of lime itself has not been sufficiently addressed. In this study, cathodoluminescence analysis coupled with petrographic and image analyses were employed to examine the degree of calcination of lime. The results of cathodoluminescence petrography were further examined through stable carbon isotope and ¹⁴C measurements. It appeared that the results of cathodoluminescence analysis are consistent with those of other analytical methods and that there are diachronic changes in the degree of calcination of lime among lime plaster samples. This implies changes in the organization of lime production, specifically the consistency in the control of firing temperature.     

SEM-EDS characterization of western Mediterranean obsidians and the Neolithic site of A Fuata (Corsica)

During the Neolithic, obsidians of the Monte Arci (Sardinia) volcanic complex were by far more used in the northern Tyrrhenian area than those of the three other source-islands (Lipari, Palmarola, Pantelleria) in the western Mediterranean. It is shown that merely determinations of content for six major elements with a scanning electron microscope by energy dispersion spectrometry (SEM-EDS) are sufficient to distinguish the four types of Monte Arci obsidians. Because of the compositional similarities between these obsidian types, a multivariate analysis is recommended in provenance studies. Although SEM-EDS, electron microprobe-wavelength dispersion spectrometry (EMP-WDS) and particle induced X-ray emission (PIXE) give essentially concordant results in the determination of these six element contents, subtle technique-related biases prevent the combination of SEM-EDS, EMP-WDS and PIXE data on source samples for provenance purposes. An SEM-EDS test-study reveals the first occurrence of obsidians of Lipari for the A Fuata Middle to Late Neolithic site of NW Corsica (north of Sardinia), in addition to the usual Monte Arci obsidians. Similar to EMP-WDS, the SEM-EDS technique requires only millimeter-sized fragments.     

Roman double-layered crucibles from Autun/France: a petrological and geochemical approach

Eighteen double-layered crucible fragments found in an archaeological excavation site of the Lycée militaire (Autun/France), which dates to the Gallo-Roman period, were analysed with a series of classical mineralogical techniques in order to obtain knowledge about the raw materials of the individual layers. This work focuses on the usage of the crucibles as well as technical aspects of their production. The crucible fragments were studied by using petrographical (optical microscopy), elemental (SEM-EDS, EMPA, XRF-WDS) and mineralogical (XRD) techniques.