Characterization of ancient building lime mortars of Anhui province,China: A multi-analytical approach

The characterization of lime mortars has become of primary importance in order to obtain information about the raw ingredients and building technology of ancient masonry structures. Five different samples from Anhui province, China, representing two types of lime mortar-based materials: joint mortars between the bricks of the city wall and lime mortar sealing a tomb coffin, were collected for analysis. Archaeological information about the samples was reported and studies into the microtextural features and mineralogical compositions of those mortars were performed via a multi-analytical approach. The joint lime mortars between the bricks of city walls, including Mingzhongdu city wall, Mingzhongdu Xihua gate foundation, Zhengyangguan city wall and She county city wall, were found to be aerial lime mortars. The lime mortar from Nanling Tieguai Song dynasty tomb was analysed and found to be a pozzolanic mortar consisting of lime, clay, sand and cocciopesto-like materials. The analytical results serve as a critical reference for the maintenance and restoration of ancient city walls in Anhui province, and as a starting point for searching for ancient Chinese pozzolanic mortars and technology for making those mortars.     

Multi‐analytical Studies of the Lime Mortars from the Yanxi Hall in the Yangxin Palace of the Palace Museum (Beijing)

For centuries, the architecture of the Palace Museum represented the highest standard of Chinese architecture. The Yangxin Palace of the Palace Museum consisted of 18 masonry buildings built using bricks, wood, roof tiles and various mortars. In 2016, a five‐year project was initiated to work on the maintenance and restoration of the Yangxin Palace buildings. The characterization of the construction materials has become of primary importance, in order to obtain information about the raw ingredients and building technology of the mortars, and the history of possible previous restorations. In this paper, 12 different samples representing three types of mortar‐based materials—namely, jointing mortars between the bricks on the wall, and surface plasters as well as mortars used on the roof—were collected for analysis from the Yanxi Hall of the Yangxin Palace. Analysis into the composition, grain‐size distribution, organic and fibre additives and testing of the mortar density and water absorption were performed. Starch, protein and plant fibres were identified in some of the samples. Brucite, mullite and ettringite were detected within most mortars on the roof, possibly originating from the furnace slag added into the raw materials for restoration purposes. The analytical results will serve as a critical reference for the maintenance and restoration of the buildings in the Yangxin Palace.     

The ancient pozzolanic mortars and concretes of <Emphasis Type="Italic">Heliocaminus</Emphasis> baths in Hadrian’s Villa (Tivoli,Italy)

The aim of this work is the physical and mineralogical-petrographic characterization of the mortars from the Baths with Heliocaminus, a special and unique architectural building in the complex of the Hadrian’s Villa in Tivoli. Thirty samples were investigated for composition and physical properties (density, porosity, water absorption, mechanical strength, particle size distribution of aggregate, etc.), representative of eight mortar groups: cubilia bedding mortar, brick bedding mortars, floor-coating and wall-coating bedding mortars, floor (rudus) and wall conglomerates (trullisatio), vault concretes, and lime plasters (arriccio). Physical parameters, together with the microscopic analysis and binder/aggregate ratio determined in three ways using image analysis (on thin sections and on specimens) and weight-data from dissolution of binder, have shown an interesting relationship between the physical-compositional characteristics and the function of mortars within the structure of the Heliocaminus baths. To identify the minerals and the reactant phases between binder and aggregate, as well as the hydraulic degree, selected samples were analyzed with x-ray powder diffraction, thermogravimetry, and differential scanning calorimetry techniques. The obtained results provide a close relation between pozzolanic characteristics and physical-mechanical properties of the mortars (i.e., punching strength index).     

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.     

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.     

Characterization of archaeological lime mortars in a Ming dynasty tomb: A multi-analytical approach

Lime mortars have played an important role in constructing ancient Chinese masonry structures, including city walls, buildings, and tombs. A tomb built with lime mortars and stones belonging a Ming high-ranking official, Xu Jie, was discovered in Huzhou City of China. Eight different samples from Xu Jie’s tomb, representing four types of lime-mortar-based materials: joint mortar between stone bricks, bedding mortar, grouting mortar, and plaster mortars were collected for analysis and comparison. The characterization of the construction materials has therefore become of primary importance. The function of each mortar was reported and studies into the micro-textural features and mineralogical compositions of those mortars were performed via a multi-analytical approach. The joint mortars were all found to be aerial lime mortars with predominately lime. The bedding mortar was found to consist of lime, soil and sand, typical of a tabia mortar. The grouting mortar was found to consist of lime and ground contact metamorphosed limestone. Analysis of plaster sample taken from the roof of the main tomb identified the presence of calcium stearate/palmitate, indicating the usage of plant-based tung oil as an additive. The analytical results will promote our understanding of Ming architectural technology and craftsmanship, and provide critical information for the conservation of Xu Jie’s tomb.     

Hydraulic structures of the Roman Mithraeum house in Augusta emerita, Spain

This paper deals with some of the hydraulic structures of Augusta Emerita (Mérida, Spain), specifically those found in the Mithraeum House. In particular, we describe and characterise the hydraulic mortars and coatings of the viridarium water channel. The recipient of the channel was covered with two hydraulic mortars and a finishing coating. Hydrated lime was used as binder. Calcite grains with different morphology have been observed in the mortars studied. The siliceous aggregate was composed of quartz, mica and feldspars. Ceramic fragments, which were added to the mortar to improve its hydraulic properties, were composed of quartz, mica, iron oxides, anorthite and an amorphous phase; aluminium-iron silicates were used as raw materials for their manufacture. We discuss the interactions between the hydrated lime and the surface of the ceramics in the mortars.     

Chemical and mineralogical characterization of historic mortars from the Santa Eulalia de Bóveda temple,NW Spain

Bulk samples of mortars from the Santa Eulalia de Bóveda temple (NW Spain) have been characterized from a chemical and mineralogical point of view, with the aims of contributing technological and provenance inferences, and evaluating possible correlations with the various identified stages along historical periods of construction.     

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.     

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.     

Calcareous nannofossils in medieval mortar and mortar‐based materials: A powerful tool for provenance analysis

Calcareous nannofossils—very small‐scaled marine microfossils—occur in many archaeological materials. Foremost, these include limestones used in masonry, material which has not experienced significant modification by humans. Poorly documented are nannofossils in mortars, because the burning process of quicklime requires the heating of the raw material to > 800°C. Here we focus on calcareous nannofossils in mortar and mortar‐based samples of four medieval buildings in northern Germany. The study documents the presence of nannofossils in historic mortars. It supplies evidence for the provenance of the mortars used, thereby introducing a new tool for mortar provenance studies.     

Mortars in context: An integrated study of mortars and plasters from the so-called Ginnasio in Solunto (Sicily,Italy)

This paper presents a multipronged scientific study of mortars and plasters of the so-called Ginnasio in the Hellenistic–Roman city of Solunto (Sicily, Italy). A selection of 16 well-contextualized samples was collected to represent different functions and building phases of this private house. The results show that a variety of locally available raw materials was used as aggregates and to produce binders. The diversity of raw materials’ sources and production techniques identified in this study reveals the advanced technological knowledge of the builders of Solunto, indicating a complex relationship between the settlement's cityscape and its surrounding landscape.     

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.     

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.     

EFFECTS OF MILLING: A POSSIBLE FACTOR INFLUENCING THE DURABILITY OF HISTORICAL MORTARS

In their literary texts, some classical Roman authors such as Gaius Plinius Secundus and Marcus Vitruvius Pollio stress the importance of milling when preparing mortars. Following these indications, this work describes the effects of milling between lime (calcium hydroxide) and clay brick powder before and after the addition of water. Starting and resulting materials were investigated by XRPD, SEM/EDS, differential scanning calorimetry and thermogravimetry (DSC/TC), colorimetry, densimetry and porosimetry. Prolonged milling changes the mineralogy of the starting materials and increases their reactivity. The final lime pastes, starting from materials milled for varying periods of time, had different mineralogical and physical characteristics. These results may help to clarify the reasons for the marked differences in durability of some historical mortars.     

Analytical Investigations of Traditional Masonry Mortars from Ancient City Walls Built during Ming and Qing Dynasties in China

With the development of China’s economy, the protection and conservation of ancient buildings were put on the agenda. However, the current understandings on Chinese traditional mortars are limited and rarely reported in the literature. In this article, the authors investigate seven ancient city wall sites built during the Ming and Qing dynasties (1368–1841 AD) in situ, and subsequently the laboratory analysis were carried out on the collected mortar samples. The characterizations of mortar samples were performed using digital microscopy, scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), simultaneous thermal analysis (TG-DSC), as well as wet chemical analysis. The analytical results show that pure lime mortar was widely used in construction during the Ming and Qing dynasties, and it was also a common practice adding sticky rice soup into slaked lime to form sticky-rice lime mortar during preparations. This organic-inorganic composite material could effectively improve mechanical strength of the lime mortar. Moreover, it was first found that the sticky-rice lime mortar sample from Kaifeng ancient city wall contained very fine quartz aggregates, with an approximate binder/aggregate ratio of 1:1. The appearance of this type of mortar probably indicates a great development of Chinese traditional mortars during the mid-19th century.     

Petrochemical Identification and Insights on Chronological Employment of the Volcanic Aggregates Used in Ancient Roman Mortars

Through the assistance of trace element and petrographic analyses on 14 samples of mortar aggregates from Roman monuments, including the Porticus Aemilia, the Temple of Concordia, the Temple of the Dioscuri, Temple B and other structures of the Area Sacra di Largo Argentina, and the Villa di Livia, we establish the source area and we investigate the chronological employment of the volcanic materials used in ancient Rome's masonry. In contrast to previous inferences, the petrochemical data presented here show that systematic exploitation of the local ‘Pozzolane Rosse’ pyroclastic deposit has occurred since the early development of concrete masonry, at the beginning of the second century bc , through the early Imperial age. Subsequently, exploitation was extended to the overlying Pozzolane Nere and Pozzolanelle deposits. Only during the early phase of development of the concrete masonry in Rome, volcaniclastic sediments outcropping near the construction sites were mixed with the sieved remains of the tuff employed as the coarse aggregate, to produce the fine aggregate. The results of the study on the investigated monuments suggest the possibility of establishing the chronological identification of three different types of mortars, as a function of the composition of the volcanic material employed in the fine aggregate, which, when implemented by future studies, may contribute to the dating of monuments and archaeological structures.     

Historical mortars dating from OSL signals of fine grain fraction enriched in quartz

In the last years the mortar dating through Optically Stimulated Luminescence (OSL) techniques has become a viable support for chronological estimations (date of construction or restoration episodes) of historical buildings. However, the dating of mortar has still open issues mainly regarding the assessment of the bleaching degree of quartz, the analysis of the OSL processes for this type of samples and the need to do appropriate tests for the most correct evaluation of the equivalent dose. This paper discusses the results obtained by OSL dating (blue diode stimulation) on the polymineral fine grain phase, enriched in quartz, extracted from lime mortar samples collected from different sites. Thermal transfer effects, through the behaviour of Equivalent Dose (ED) and recovery tests, degree and time of bleaching were studied. For each mortar sample the adjacent brick was collected; in some cases, sampling of the bricks bracketing a mortar layer was a possibility, thus obtaining a direct comparison with the standard thermoluminescence (TL) dating on the bricks. The results obtained show, for this set of samples, the possibility of dating the mortars through the use of the fine grain fraction provided of a suitable chemical-physical preparation procedure and the verification of the bleaching conditions.     

A Multidisciplinary Approach to the Study of Archaeological Mortars from the Town of Ammaia in the Roman Province of Lusitania (Portugal)

The Roman town of Ammaia (in Marvão Region) is considered one of the most important recent findings of the Roman presence in Portuguese territory. It was settled in Republican times and abandoned in the seventh century. In this research, 17 masonry mortars and renders from the West Tower (South Gate), the residential area near the West Tower, the macellum, the peristylium, the public bath building, the podium of the temple and the portico of the forum were analysed. The methodology of chemical, mineralogical and microstructural characterization has involved several complementary techniques, including stereomicroscopy, X‐ray diffraction, thermal analysis and scanning electron microscopy coupled with energy‐dispersive X‐ray spectroscopy. The results indicate that the mortars from the beginning of the town's edification were mainly composed of soil (clays). Later, during the main Roman building period, mortars were composed using a calcitic binder and the mortar composition varied according to their use and function. The samples from a period subsequent to the Roman occupation are based on a dolomitic binder. From the present study, relevant information has been acquired about the technological evolution of Roman construction in Ammaia, the historical context of the archaeological structures and guidelines for the conservation and restoration of mortars.     

Chemical and Microscopic Study of Masonry Mortar in Ancient Pagodas in East China

Ancient mortars played a crucial role in the construction of historical architectures due to their physical and chemical compatibility with traditional building materials such as stones and bricks. Therefore, the analysis and optimization of the ancient mortar formula are significant in the restoration and preservation of historical sites. In this work, 20 mortar samples selected from five ancient stone pagodas in Zhejiang Province, China, were analyzed. The results showed that mud, lime-soil mortar, lime-sand mortar, and lime-gypsum mortar were used as binders in these pagodas. The Ca(OH)₂/aggregate ratio ranging from 0.3 to 2.7 was usually used to prepare lime mortar. Protein and polysaccharide were also found in some samples.