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.     

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.     

Qadhat—a comparative study of ancient and new lime mortar from the Marib province/Yemen

Qadhat is the name for a lime mortar in Southern Arabia. Its usage has a long tradition. This work describes physical and mineralogical properties of ancient, historical and new samples, which seem to have been produced the same way. XRD, thin sections and SEM analyses show the similarity of the material. It consists of aggregates of volcanic material that are rich in volcanic glass and lime as binder. The production process includes several hours of crushing the material, which produces fine-grained splinters of aggregates in the binder matrix and gives the mortar a high stability. A weathering test with sodium sulphate on different samples confirms that the stability of this mortar is the result of the production process.     

传统建筑泥灰类加固材料的性能研究与机理探讨

人们已经发现一些古建筑所使用的传统材料具有较好的加固作用,其耐久性、强度、与建筑本体的和谐、以及与环境的友好等方面都具有突出的优点。但是由于当时科学技术水平的限制,以及天然材料混合物本身的复杂性,这些传统材料的加固机理一直未被人们充分认识。为了利用和发展传统材料的优势并为古建筑和文物保护服务,本工作选择最具中国特色的以石灰等无机材料为基料,以糯米浆和蛋清等天然生物材料为配料的古代建筑灰浆配方和三合土配方,开展了一系列加固性能研究,并且结合现代SEM和XRD分析仪器,对一些典型的样品进行了微观结构和形貌分析。结果发现,这些古代配方具有现代复合材料的某些特点,即通过无机/有机相互协同的效应,达到了较好的加固效果;重要的是发现糯米浆具有一定的生物矿化的模板作用,即糯米浆的生物大分子对碳酸钙的结晶和生长起到了调控作用,使方解石结晶体的大小和形貌具有一定程度的有序性。本研究为传统材料进一步科学地应用于古建筑和石质文物的修复加固提供了新的思路。     

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.     

Radiocarbon Dating of Architectural Mortar: A Case Study in the Maya Region,Quintana Roo,Mexico

Abstract

The use of radiocarbon dating to analyze mortar and charcoal inclusions within mortar or plaster is a useful way to date the construction of architecture, particularly when options for other chronometric methods are limited. In the Yalahau region of northern Quintana Roo, Mexico, members of the Yalahau Regional Human Ecology Project have faced challenges in dating buildings made of large blocks of stone in the Megalithic architectural style. The Megalithic style poses serious problems for any analysis, as excavating into structures with stones weighing several tons can be dangerous, expensive, and time consuming. Additionally, there are no associated sculptures, texts with dates, or other traditionally accessible chronological markers. These factors have resulted in a reliance on a ceramic chronology despite the uncertainty of the dating of many ceramic types in this region, as well as the questionable contextual associations between recovered ceramics and architectural construction phases. Megalithic-style structures at the ancient Maya site of El Naranjal have residual mortar with charcoal inclusions left behind during the mortar-making processes that can be extracted and dated with AMS ¹⁴C methods. Several samples of mortar and charcoal were obtained from structures 1 and 10 from exposed exterior walls and an interior vault. The resulting dates confirm the date for the construction based on ceramics excavated from the same site.     

日本古代楼阁式木塔的类型学研究

日本现存8～12世纪所建造的楼阁式木塔11座,目前为止,针对这些遗构的实测和基础考察已基本完成,相应的文献研究、木结构技术研究也已经有一定的成果。不过,仍有5座塔的建造年代尚未明确,并且这些楼阁式木塔在形态上是怎样演进的——有关这方面的研究还有待深入。此文对这11座木塔的木构架进行类型学研究,在精确上述5座塔的建造年代的同时,也梳理了日本楼阁式木塔在这5个世纪里的形态演变和各个年代的形态特征。     

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.     

A Discussion on the Emergence and Development of Ancient Chinese Artificial Barium Copper Silicate Pigments from Simulation Experiments

The ancient Chinese barium copper silicate minerals mainly comprise Chinese purple (BaCuSi₂O₆) and Chinese blue (BaCuSi₄O₁₀), which were widely used from the late Warring States Period to the late Eastern Han Dynasty. In order to clarify the raw material of the pigment, a series of simulation experiments was conducted to produce Chinese purple pigment under varying mineral conditions. The minerals that we applied in the experiment were quartz as the source of silicon, malachite and copper oxide as the sources of copper, barite and witherite as the sources of barium and lead oxide as the source of lead. Simulation experiments showed that the barium copper silicate minerals and the purple pigment can be produced easily when witherite is used as the barium‐containing raw material. From the perspective of mineral resources, the birth of the ancient Chinese pigment associated with a unique barium mineral resource. The Chinese copper‐based pigments are assumed to have been developed independently and are presumably an outcome of historical developments in glazing techniques.     

以糯米灰浆为代表的中国传统有机-无机复合灰浆研究进展和新发现

在中国数千年的建筑实践中,已发现许多具有中国特色的创造,其中以糯米灰浆为代表的中国传统有机-无机复合灰浆就是其中的一类。本文综述了自2007年以来相关研究的进展,包括：针对传统灰浆中有机残留物的化学检测和免疫分析技术的创新发展;全国252处古建筑遗址的1149个灰浆样品的检测结果及解读;糯米灰浆和桐油灰浆等传统胶凝材料固化作用机理及效果的实验验证;糯米灰浆研究成果对世界的影响及在世界复合材料历史上的地位;最近在新石器时代“白灰面”中新发现的有机添加物及相关溯源;传统糯米灰浆的改良研究及在文物保护工程中的应用情况等。这一系列的探索性研究不仅可为古建筑保护提供材料和技术,也为弘扬中华文明提供了鲜活的案例。     

Combined In-Situ and Laboratory Minor Destructive Testing of Historical Mortars

ABSTRACT

Mortar is of all masonry components the most difficult to be experimentally characterized in heritage buildings. This article investigates the possibility of combining different in-situ and laboratory minor destructive testing (MDT) techniques to assess the strength of mortar in historical brickwork. Lime mortar and clay brick walls were built in the laboratory and then tested in order to derive empirical correlation rules among three different MDT techniques: double punch test (DPT), helix pull-out test (HPT), and pin penetration test (PPT). The outcomes of this activity were used eventually to assess the mortar properties of an important historical heritage structure, Casa Puig i Cadafalch, located near Barcelona. The research is intended to promote the use of MDT in studies and conservation works on built cultural heritage by providing criteria for the evaluation of the strength of existing mortar with respectful sampling and testing techniques.     

Material Characterization and Micro-Modeling of a Historic Brick Masonry Pillar

A masonry pillar composed of solid clay bricks, cement mortar and infill is extracted from a historical structure and tested in concentric compression. It is subjected to cyclic and monotonic loads up to compressive failure.

In parallel, samples are extracted from the pillar and are subjected to destructive tests. Non-destructive tests are performed on the pillar, as well. The properties of the constituent materials are critically examined and their role in the maximum load reached and the failure mode obtained are discussed.

Finally, a finite element micro-model of the pillar is used for the simulation of the pillar test. The influence of the existing damage on the pillar is investigated using the model, resulting in a fair approximation of the global Young’s modulus, maximum load and the failure mode.

Highlights

●?A brick masonry pillar extracted from a historical building is tested in compression.

●?Material samples extracted from the pillar are characterized by mechanical tests.

●?A finite element micro-model of the pillar is used for the simulation of the compressive test.

●?The effect of damage on the compressive strength of the pillar is numerically investigated.     

First ancient bovine DNA evidence from India: difficult but not impossible

Ancient DNA isolation from the tropical countries has been shown to be very difficult in the past. Here for the first time we have been successful in isolating ancient DNA from Indian cattle samples. We were able to obtain DNA and sequence the partial mitochondrial D-loop in 3 of the 15 bovine fossil samples ranging in age from 2000 BC to 1000 AD, and were able to further identify the most recent sample as being of Bos indicus origin. Our results on ancient DNA extraction from India will encourage other researchers in this field to carry out further studies of ancient DNA from Indian bovine samples. Our results represent the first successful extraction and amplification of bovine ancient DNA from India, and thus may pave the road for a better understanding of demographic and historical processes of cattle domestication that has taken place in this region.     

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.     

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.     

Evidence for Migration Influx into the Ancient Greek Colony of Metaponto: A Population Genetics Approach Using Dental Nonmetric Traits

Ancient Greek colonies were founded by Greek seafarers all along the Mediterranean coast as early as the eighth century bc . Despite extensive archaeological and historical research, the population structure of the inhabitants of Greek colonies and their relationship to indigenous populations are still debated. Here, we perform a biodistance analysis to reconstruct migration and gene flow between the ancient Greek colony of Metaponto (southern Italy) and indigenous groups in the surrounding hinterland (900–250 bc ). We collected dental nonmetric trait data of 355 human skeletons from the indigenous Italic sites of Santa Maria d'Anglona, Incoronata and Passo di Giacobbe. This data set is compared with an urban and rural sample of the Greek colony of Metaponto comprising 351 individual dentitions. The R‐matrix approach is used to estimate inter‐population relationships and F _ST. The resulting kinship coefficients indicate that the three indigenous groups exhibit greater similarity to each other and possess lesser similarity to the two Metapontian samples. Interestingly, the two samples of Metaponto are least similar to each other, although they are geographically very close. The F _ST estimates confirm this pattern and reveal greater biological variation between the two nearby Metaponto samples (F _ST = 0.0603) than between the three geographically fairly distant indigenous groups (F _ST = 0.0389). We conclude that the Greek colony of Metaponto included large numbers of people with diverse geographical origins, whereas the indigenous Italic communities of the surrounding hinterland exhibited high levels of homogeneity and cohesion. Copyright © 2016 John Wiley & Sons, Ltd.     

High-performance enrichment of casein and ovalbumin in wall painting with immunomagnetic beads

The detection of trace binding medium in wall paintings is usually challenging due to the aging and degradation of proteinaceous binding medium in a long time. Therefore, immunomagnetic beads (IMBs) with specific enrichment ability for casein and ovalbumin were prepared, and then the beads were applied for capturing target proteinaceous binding medium from ancient Chinese wall paintings. After optimization of experimental conditions, the enrichment performance of magnetic beads was confirmed by enzyme-linked immunosorbent assay (ELISA) and sodium dodecyl sulfate polyacrylamide gel electrophoresis (SDS-PAGE). In this experiment, archaeological wall painting samples were used to verify the accuracy of the construction enrichment method. The results showed that the OD_450nm value of archaeological samples containing binding medium has increased to varying degrees after IMBs enrichment, effectively avoiding the occurrence of false negative results, indicating that the IMBs enrichment method developed in this work could be successfully applied for enriching ovalbumin and casein binding medium from ancient wall paintings for subsequently immunoassay detection.     

Analysis of Byzantine mortars from the Negev Desert,Israel, and subsequent environmental and economic implications

Mortar of different types and compositions was widely known and used in the ancient world, and became widespread throughout the Roman and Byzantine Empires. In many cases lime was used in it as a binder and for better plasticity. This paper discusses two mortar samples from a building in the Negev Highlands, Israel, their analysis under scanning electron microscope (SEM) and with X-ray diffraction (XRD), and the environmental implications in terms of energy consumption in the production process of lime in the Byzantine period.     

Multi-Isotope Investigations for Scientific Characterisation and Provenance Implication of Banded Travertines from Tripolis Antique City (Denizli–Turkey)

The coloured stones used in buildings and monuments were an indicator of power and wealth during the ancient times. In this study, Tripolis city samples have been compared with Tripolis quarry samples in order to recognise the provenance of the banded travertine blocks in the ancient city. The banded travertine samples have similar mineral compositions and mainly consist of calcite with minor amounts of dolomite, aragonite, clay and iron oxide minerals. These results are also supported by CRS studies. Calcite is in the form of needle-shaped crystals ranging between 0.163–1.418?mm (in city) and 0.303–1.270?mm (in quarry). Tripolis banded travertine samples show the similar compositional spread in terms of major oxide, trace elements. δ¹³C_V-PDB values of banded travertines range from 1.93 to 5.25‰ (in city) and 2.99 to 3.99‰ (in quarry), δ¹⁸O_V-PDB values change between (?16.93)–(?10.08) ‰ and (?15.93)–(?13.01)‰, respectively. The U–Th radiometric ages are determined between ～267 and 9?ka in Tripolis city samples and ～350 and 2?ka in Tripolis quarry samples. The minero-petrographic, geochemical, C–O and U–Th isotope results fairly matched with each other. It seems highly probable that the banded travertines in Tripolis city were extracted from the Tripolis quarry, which is located at the northeast of the antique city with a distance of 3?km.