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1.
The Sos Furrighesos necropolis (Anela) is considered to be one of the most important funerary monuments in Sardinia. The hypogeum consists of various graves, called Domus de Janas, which are decorated with Neolithic mural paintings and sculptures. This work was undertaken in order to clarify which techniques were used in the past, through the identification of pigments and binding media. The samples, scraped off from the paint surface, were studied by using various analytical techniques in order to characterise both the pigments and the binding media. The main problems concerning the characterisation were due to the small sizes (1–5 mg) of the samples and their complex nature. As regards pigments, X-ray diffraction and scanning electron microscopy-energy dispersive X-ray spectrometry analyses were performed on the samples. These techniques are well suited to the characterisation of inorganic pigments and have led to the identification of the red pigment as haematite. In order to characterise the organic binders, the samples were analysed by a procedure based on a gas chromatography–mass spectrometry technique, which allows proteinaceous and lipidic media determination in the same sample. In most of the samples, the presence of egg was suggested.  相似文献   

2.
Optical and SEM-EDS microscopy, X-ray powder diffraction and micro FT-IR spectroscopy investigations of the funerary klinai (couches) of Tomb 1 from Amphipolis and a stone sarcophagus from ancient Tragilos—two painted monuments made by Macedonian craftsmen of the Early Hellenistic period—identified the original materials and painting technique, as well as synthetic materials used as consolidants during past restoration treatments. The original organic binders and the superficial modern coatings have been identified by micro FT-IR spectroscopy applied directly to the sampled powders or tiny fragments and to their solvent—soluble fractions. The pigments identified on the couch of Amphipolis are: red and yellow ochre, cinnabar, Madder lake, paratacamite and antlerite, carbon black, calcium carbonate, kaolin and gypsum. The identification of egg and animal glue confirms the application of tempera and secco techniques. The detection of polymers such as polydimethylsiloxane, polyvinyl acetate and alkyd resins, is related to modern restoration products. The pigments attested on the paintings of the Tragilos' sarcophagus are: red and yellow ochre, Egyptian blue, malachite, carbon black, calcium carbonate and gypsum. The absence of organic binders combined with the constant presence of calcium carbonate in all the examined samples suggests the use of lime as the binding medium in the painted decoration of the sarcophagus. The presence of Paraloid B72 is related to recent conservation treatments.  相似文献   

3.
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4.
The glazed tile decorative art was one of the widely used ornamental techniques for the monumental buildings during the Mughal period, in Pakistan. Coloured tile samples from Jahangir tomb were analyzed to know the glaze composition and to identify the colouring phases used at that time. The study was performed using light microscopy (OM), scanning electron microscopy equipped with energy dispersive X-ray analyzer (SEM-EDS), Raman spectroscopy (RS) and electron microprobe analysis (EMPA). These complementary analytical techniques allowed characterizing the samples as alkali glazes made from plant ashes. The results indicated the use of lead-tin yellow type II for yellow glazes, cobalt and copper for blue glazes, mixtures of yellow and blue glazes for the green glazes, manganese for purple glazes, and a transparent glaze layer for white glazes.  相似文献   

5.
Analysis of historic mortars including Islamic, Gothic and later ones taken from palaces, convents and mansions in Palma de Mallorca has been carried out. Scanning electron microscopy (SEM) coupled to energy dispersive X-ray spectrometer (EDX), Fourier transform infrared spectroscopy (FTIR), and X-ray diffraction (XRD) techniques were used to characterise the morphology and analytical composition of the samples analysed. Generally, covering plaster mortars presented a low percentage of small size aggregate. The reported results show that mixed and lime mortars have been used, thus, the establishment of a relationship between the type of mortar employed and its age is not feasible. In the painted mortars, polychromy has also been studied. The most common pigments to be found are natural earths.  相似文献   

6.
The pigments, organic materials and techniques used on a post-Byzantine icon of St Nicholas were determined by means of several micro-analytical techniques. The icon painter covered the leather support with silver leaf about 3 μm thick to create a smooth working surface. Animal glue was used to secure the leaf to the leather, and FTIR spectroscopy has identified another layer, 30–60 μm thick, of the same material applied as a primer above the silver. Above that, a layer of lead white covering the entire surface creates a white substratum serving the same purpose as the gesso on a wood panel. The colour palette, determined by means of scanning electron microscopy and FTIR spectroscopy, is very simple. Only seven colours were identified: lead white, caput mortuum, red and yellow ochre, cinnabar, carbon black and smalt. As far as we know, this is the first time that smalt has been found on a Byzantine icon. Since smalt was chemically synthesised only after 1500 AD, it may be concluded that this icon was painted after the end of the 15th century. Beeswax was used as a protective varnish.  相似文献   

7.
A group of 51 shards of medieval polychrome glazed pottery, coming from Canosa castle archaeological site (Bari, Italy), has been investigated through surface analytical techniques, such as Scanning Electron Microscopy (SEM) with Energy Dispersive X-ray Spectroscopy (EDS) and elemental ones, such as Inductively Coupled Plasma–Optical Emission Spectroscopy (ICP–OES) and Absorption Atomic Spectroscopy (AAS) by flame and electro-thermal atomisation. The investigation was aimed at defining the elemental composition of pottery findings, identifying pigments and clarifying glaze types. The results of the analytical characterization allowed the identification of materials and technological expedients used for pottery manufacturing, highlighting original features in the production of the investigated pottery.The quantitative analysis performed on ceramic paste, glaze and painted decorations provided a significant number of results, thus enabling their effective exploitation for multivariate statistical techniques, in order to find out possible groups of pottery items with defined similarity within the samples.  相似文献   

8.
This paper reports results derived from a chemico-physical characterisation study undertaken on an important ensamble of early 20th century stained glass windows from Madrid and signed by the prestigious and well-known Maumejean Fréres company. The study is part of an on-going project of restoration and conservation carried out by the National Glass Centre Foundation (FCNV, La Granja de San Ildefonso, Segovia, Spain). The basic aim of the research was to assess their current state of conservation and to study the degree of damage suffered throughout the last century by different materials employed in their production, namely colourless and coloured glasses, grisailles, lead cames, and putties used to fix glass pieces into the lead cames. Selected samples from these materials were characterised through optical microscopy (OM), X-ray fluorescence (XRF), scanning electron microscopy (SEM), energy dispersive X-ray microanalysis (EDX), VIS spectrophotometry, and X-ray diffraction (XRD). As a general rule, most of them presented an acceptable state of conservation, without any of the known degradation phenomena of more ancient stained glasses (e.g. Medieval, Renaissance, etc.). However, some remarkable alterations were observed. Important deposits of soot and dirt particles coming from a polluted urban environment were detected, producing a slow blackening of the panels. Resulting data have been useful to design and optimise a combined conservation and restoration strategy in the recovery of this valuable legacy of early 20th century stained glass windows from Madrid.  相似文献   

9.
This work reports mainly the results of an X-ray Absorption Spectroscopy (XAS) study carried out on coloured glass tesserae from the palaeo-Christian mosaic which decorated the votive chapel of St. Prosdocimus (Padova) until its replacement with the current frescoes of Renaissance age, and which is one of the only two known mosaics in the Veneto region (Italy). The study aims at clarifying how the different local structure, oxidation state and quantity of copper influenced colour. Analysis of high-resolution Cu-K edge X-ray Absorption Near Edge Structure (XANES) and Extended X-ray Absorption Fine Structure (EXAFS) spectra showed that copper is present as cuprite (Cu2O) in orange samples and as metallic copper in red and brown ones. These phases are responsible for both the colour and opacity of the samples. In addition, Cu1+ ions linked to the oxygen atoms of the glass framework were identified in ratios of about 60% and 30% of total copper in orange and red/brown samples, respectively. In blue and green samples, copper is dispersed in the glass matrix as a mixture of Cu1+ and Cu2+ ions, and no crystalline phases are visible. In this context, the Cu1+ and Cu2+ contents in glass were also quantified thanks to suitable standards, demonstrating that, when Cu2+ is the main chromophorous ion, colour intensity is directly correlated to its content in the glass. In particular, in green and blue samples, coloured by copper, Cu2+ content varies from 26% to 56% of total copper, and the higher contents of Cu2+ are shown by more intensely coloured samples. It should be stressed here that the green colour of the analysed tesserae is given by the physical interaction of blue colour, due to Cu2+ ions, and yellow colour, due to Pb antimonates used as opacifiers.  相似文献   

10.
The preservation of early 20th century, late 19th century albumen prints is of great concern to collection managers and conservators of photographic materials. Attenuated Total Reflection Fourier Transform Infrared (ATR-FTIR) spectroscopic imaging is presented for the first time as analytical methodology for the study of albumen photographs. This paper shows the feasibility of obtaining FTIR images of samples from albumen photographs with a high spatial resolution using a Ge ATR objective coupled with an infrared microscope. The improved spatial resolution compared to FTIR images obtained by the reflection method is due to the high refractive index of the ATR crystal, which gives a high numerical aperture and hence, a higher spatial resolution. The technique reveals detailed information on the organic functional group distribution in the individual layers of embedded cross sections and is used complementary to visual microscopy and scanning electron microscopy/energy dispersed X-ray spectroscopy. The main results of the study are discussed with regard to their historical and artistic significance, and they are compared with data from historical and conservation literature.  相似文献   

11.
The present work reports on a spectroscopic study of white colour samples collected from Etruscan polychromes on terracotta from the Cerveteri area. In particular, both white-on-red potsherds of the Orientalising period and high-value polychromes of the Archaic period were considered. The white pigment, a fundamental element in this class of artworks, was not clearly identified in previous archaeological and analytical studies, although the use of kaolin was tentatively proposed. Therefore, samples from the Monte Sughereto kaolin quarry in the Cerveteri area were also studied. The results of detailed analyses carried out using micro-Raman spectroscopy, X-ray diffraction, and Fourier transform infrared spectroscopy first show that the quarry material is a high-purity kaolin containing quartz. Raman results strongly suggest that the same kind of kaolin was employed in the polychromes of the Archaic period. As to white-on red potsherds, infrared results have a key role in showing that the white pigment is a kaolin closely corresponding to the quarry material since a particular kaolin polytype (dickite) is dominant in both cases. The present work thus provides the first definitive identification of the white pigment used in Etruscan polychromes on terracotta from the Cerveteri area, and suggests that the source of kaolin might be the Monte Sughereto quarry.  相似文献   

12.
In the present work, an analytical characterization of painted plaster samples coming from ancient buildings dated back to 2nd cent. B.C., located in Licata (Sicily, Southern Italy), has been carried out. The investigation has been performed through different spectroscopic techniques: X-ray fluorescence (XRF) using an handheld energy-dispersive XRF analyzer, scanning electron microscopy equipped with an Energy Dispersive Spectrometry microanalysis detector (SEM-EDS) and Fourier transform infrared absorbance spectroscopy (FT-IR). The main goal is to identify the plaster and pigments material. In particular, the XRF investigation of surfaces is the first step for a preliminary elemental characterization. Then, through SEM-EDS measurements, a quantitative analysis of the chemical composition of the plaster and the pigmenting agents along with eventual components related to deterioration processes has been obtained. Finally, FT-IR absorbance spectra have proven to be a useful tool to investigate the molecular nature of the used materials.  相似文献   

13.
The sculptural polychromy in the Zhongshan Grottoes, sited in northwest China, has been investigated in terms of chemical composition of employed materials and pigments, state of conservation and painting technique. Raman analysis, Fourier-transform infrared analysis, analysis through energy-dispersive X-ray spectrometry coupled to scanning electron microscopy and pyrolysis coupled to gas chromatography and mass spectrometry were applied. Six analyzed samples showed silicates and kaolin as main components of the ground layers. Also lead white has been found in these layers. Minium, red-earth and mercury sulfide are the red pigments detected in the polychromy. A mixed use of malachite and atacamite has been detected in three green samples. Optical characteristics of atacamite and malachite found in the samples indicate a synthetic origin. The presence of a synthetic organic pigment such as phthalocyanine chlorinated pigment was also revealed. Ultramarine blue pigment, obtained by purification of lapis lazuli, has been detected in the blue sample. As for the binders used, fatty materials and siccative oil were found.  相似文献   

14.
The present research is an attempt to create a link among different disciplines and to confirm stratigraphic observations through chemical analyses. It involved detailed colorimetric examination and in-depth chemical-physical study of the samples taken from the historical centre of Genoa, which enabled connections to be made among many data. This led to the creation of an analytical method that is applicable to various geographical sites. Examinations involved several experimental techniques: X-ray diffractometry, scanning electron microscopy, optical microscopy and infrared spectroscopy; the data were compared with those from the stratigraphic examination. A detailed investigation of the Ligurian climate, including data kindly supplied by the Environment Department of the Provincia di Genova, allowed us to explain the presence of particular chemical substances and suggested how they might have been formed.  相似文献   

15.
In recent years, plastics are designated as a source of indoor pollution and particular attention has thus been devoted to the identification of emitting low molecular weight compounds. Headspace-solid phase microextraction-gas chromatography coupled with mass spectrometry (HS-SPME-GC/MS) has been already successfully applied for screening emissions from synthetic materials. This analytical tool being also non-invasive, it has been already successfully applied in the field of cultural heritage science for the identification of volatile organic compounds (VOCs) emitted from various museum objects made of natural materials. In this research, we aimed at assessing the use of HS-SPME-GC/MS as an in situ non-invasive analytical tool for a better knowledge of the volatile organic compounds emitted by plastics in collections. The possibility of characterizing plastics based on their emission signatures was also evaluated. Twelve new standard plastic samples, belonging to seven main polymer families widely present in museum collections as well as three naturally aged museum objects, were investigated. In this paper, we provide a survey of the VOCs emitted, and the use of HS-SPME-GC/MS for identifying volatile marker compounds, degradation products, additives, and monomer residues of the plastic synthesis is evaluated. More than 200 different VOCs were identified from the new standard samples. Two categories of VOCs were distinguished: “non-specific” and “specific” ones. We showed that based on the “specific” VOCs, it was possible to identify the nature of the polymeric matrix itself or at least to unambiguously distinguish a plastic by family. Emissions from the museum objects were then characterised, and main volatile degradation compounds considered as degradation markers of the natural deterioration of polymeric matrices, were identified. This identification procedure could be further exploited for the characterization of VOCs emitted by objects made of multiple synthetic polymers. Complementary to other techniques, this analytical tool is an interesting way to assess the risk for the objects stored in the vicinity of emitting plastics.  相似文献   

16.
This study presents characterizations of weathering forms of the same oolitic limestone from four quarries and eight monuments exposed on various environmental conditions focusing on the waterproofing effect of endolithic organic matter. Patinas were analyzed by X-ray diffraction (XRD), scanning electron microscopy with energy dispersive X-ray spectrometry (SEM-EDX), capillarity coefficient through weathered and unweathered sides, gypsum content and porous network morphology by epoxy resin molding. Study of weathering forms on old quarries indicates that lichens colonization (Verrucaria nigrescens and Caloplaca aurantia) can fill the superficial porous network with a dense network of lichenised fungal hyphae. Capillary coefficient measurement on natural and calcinated samples showed that endolithic organic matter can waterproof the stone and could act as a sulfate contamination barrier. Similar endolithic organic layer due to ancient lichens growth are found on some antique monuments of the Nîmes downtown and could explain their well-preserved state, unlike decayed 19th century churches that were never colonized by lichens.  相似文献   

17.
The identification and localization of the proteinaceous binders are essential issues in studies of painting materials and techniques, for further proposing valid restoration and conservation treatments of the painted or polychrome works of art. The challenge for analytical chemists and conservation scientists is the availability of methods able to simultaneously identify and map the presence of the binders in the multilayered structure of a sample and the possibility to use a very low amount of sample from the studied art object (considering also the criteria of minimum sampling). These methods should be fast, reproducible in different artefacts and in case of mixture of protein-based binders with other non-proteinaceous constituents (oils, resins, waxes, gums etc.) and also economical (both in terms of materials and time consume). In this context, the present paper proposes an innovative protocol of investigation using two complementary techniques – Matrix-Assisted Laser Desorption/Ionisation – Time of Flight Mass Spectrometry (MALDI-TOF MS) and staining tests (one visible and one fluorescent stain) assisted by Optical Microscopy (OM) on cross-section of samples – for the simultaneous identification and mapping of protein – and oil-based binders in paint materials. The novelty is based on the use of MALDI-TOF MS on cross-sections of paints together with a fluorescent stain for protein identification and mapping (mainly used in the area of proteomics) complementing the use of a traditional visible stain for oil-based material identification. The protocol was successfully applied on several samples taken from a Czech medieval polychrome sculpture, entitled “The Mourning of Jesus Christ” (16th century) belonging to the Moravian Gallery (Brno).  相似文献   

18.
Very often traces of paint and pigment have been found on medieval sculpture. Presently, little is known about the effects of laser radiation on polychromy. It is important to protect and preserve these traces during any cleaning or restoration process. The absorption properties of polychrome materials are likely to be different from those of the underlying stone or substrate and as a result special care must be taken to avoid any damaging or discolouring phenomena associated with laser cleaning. Spectroscopic methods (XPS, AES, reflectance spectroscopy) together with optical microscopy, digital photography and X-ray diffraction analysis have been used in a series of experiments on simulated samples of common medieval pigments (vermilion, red and white lead and ochres in linseed oil) on limestone plates, in order to study the reaction of these materials to infrared laser radiation.  相似文献   

19.
In this study, the dyes present in five 17th- to 18th-century textiles from the National Museum of Art of Romania, three religious embroideries and two brocaded velvets, are characterized and discussed, together with earlier results on textiles from Romanian collections obtained by the same research group. Dye analyses were performed using two methods: the well-established liquid chromatography-diode array detection (LC–DAD) and a recently developed liquid chromatography-mass spectrometry (LC–MS) analytical protocol. The examination of very small historical samples by both techniques allows a better insight in the advantages and limitations of the two approaches to real analyses to be obtained. LC–MS data interpretation is based entirely on the results accumulated for dye standards. Electrospray ionization (ESI) was used in the negative ion mode and an ion trap served as mass analyzer. Both single stage (MS) and tandem (MS/MS) mass spectrometric approaches were considered. The dyes and natural sources identified by both analytical techniques are discussed in the historical context of the textiles, with respect to earlier results collected for similar Romanian objects. The study showed that the dye sources found in the 17th- and 18th-century Romanian velvets and embroideries were produced using a wide variety of dye sources, suggesting influences from Europe as well as from Asia Minor. Dye sources imported from New World have been also detected. The range of biological sources is in very good correspondence with earlier results obtained from textiles in the Romanian Collections. LC-MS (single stage and tandem MS) approaches have been demonstrated to be valuable tools for dye identification in small-scaled samples from historical textile objects only if sufficient knowledge on the dyes and their biological sources is first accumulated within experiments performed on standard dyes and standard dyed fibers.  相似文献   

20.
Optical microscopy, cross-section and fragment Micro-FTIR spectroscopic techniques along with microchemical tests were used for the identification of pigments in two different samples of an icon. Representing the Last Judgement, and painted by the Greek master Ioannis from the village of Kapesovo in the year 1771, the kneeling desk icon under investigation is a noteworthy contribution to the study of materials in post-Byzantine visual arts. The main components found in the ground layer of both samples were gypsum, beeswax and a proteinaceous material. Cinnabar, Prussian blue and cerussite were identified on the paint layers. The binding medium on the paint layers was weddelite. The materials used in the painting and ground layers were characterized in order to clarify the painting technique. Proteinaceous materials have been identified as binders for the pigments, indicating a tempera painting technique.  相似文献   

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