Characterization of dyes in ancient textiles from Yingpan,Xinjiang

In this paper we analyzed the natural dyes in well-preserved, ancient textiles from Yingpan, an important archaeological site on the Silk Road, using high-performance liquid chromatography with diode array and mass spectrometric detection. Dyes were removed from textile fibers using a soft extraction method (pyridine, water and oxalic acid). Two species of madder-type plants, Rubia tinctorum and Rubia cordifolia were identified as the dye sources in red and brown samples. We also were able to detect unusual flavonoid glycosides in yellow and green woolen yarns, although we have not been able to pinpoint with certainty a specific plant that may have been used to produce this dye(s). On the other hand, we found that yellow and green silk threads had been colored with protoberberine-type dyes, probably obtained from species of cork tree, Phellodendron spp., and/or other protoberberine producing plant. We propose that the textile dyes found at Yingpan reflect a merging of Eastern and Western practices and technologies during the 800-year period (206 BCE–618 CE) encompassing the early years of the Silk Road.     

Non-destructive in situ analysis of polychromy on ancient Cypriot sculptures

The study focuses on the characterization of polychromy on limestone sculptures from Cyprus, attributed to the Cypro-Archaic—end of the Hellenistic periods. Polychromy components were identified by integrating digital microscopy, imaging under ultraviolet (UV) light, visible-induced luminescence (VIL), X-ray fluorescence spectroscopy (XRF) and fibre optics reflectance spectroscopy (FORS). Data acquisition was performed directly in exhibition rooms at the Cyprus Museum (Nicosia) and the Paphos District Archaeological Museum (Paphos). Among the identified materials, there are iron-containing (red, yellow, green) and copper-containing (green and blue) pigments. The precision of pigment identification by non-destructive techniques is discussed, and specific pigment names are proposed: red iron oxide, yellow iron oxide-hydroxide, green earth and Egyptian blue. Interesting results were obtained by VIL, which allowed identifying traces of Egyptian blue otherwise undetectable with the naked eye. Complementary, this study discusses advantages and problems of combined and separate use of portable XRF and FORS, raising the question of their complementarity and interchangeability for the purposes of pigment identification.     

Coloration and Fabric Structure of Selected Polychrome Textiles from the Seip Mound Group

Abstract

Selected yellow and brown colored textiles from the Hopewellian Seip Mound group were examined visually and photographed. In some cases, the yarns are colorant saturated and the colored patterns are nearly identical on both sides of the textiles. In addition to the use of several colors, fringe and possibly leather are used as decorations. Particulate material shed from these fabrics, or small samples strategically removed based on the results of the forensic photography, were examined with optical microscopy, revealing that the fabrics are made of dyed rabbit hair and bast fibers. Energy dispersive spectroscopy (EDS) of a subset of the samples indicates that there is no significant difference in elemental composition between the different colors. However, the high carbon and copper content are signs of mineralization of the fibers. These textiles reflect multifaceted textile construction methods with elaborate decoration techniques as well as the use of complex dye technology.     

山普拉墓群出土毛织品上蓝色染料的分析研究

本文采用薄层色谱法、红外光谱法、高效液相色谱法、质谱及快原子轰击质谱法的分析测试手段,通过综合比照认定毛织品上的蓝色染料的主要成分应是靛蓝素,染色过程中可能采用了复染与套染工艺     

A Technological Study of the Elamite Polychrome Glazed Bricks at Susa,South‐Western Iran

This study investigated the technological features of the Neo‐Elamite glazed bricks discovered at the Acropolis of Susa, south‐western Iran, by conducting micro‐Raman spectroscopy, differential thermal analysis/thermogravimetry (DTA/TG), X‐ray diffraction (XRD) and scanning electron microscopy–energy‐dispersive X‐ray spectroscopy (SEM–EDS). The results showed that calcium antimonate white and lead antimonate yellow were used as opacifiers in the white, yellow and green glazes, and that green and turquoise glazes were achieved using copper. Coloured glazes were separated by a Si‐rich brown glaze to prevent them from running together during firing. The glazed bricks most probably were not fired at temperatures higher than 900°C.     

THE ANALYSIS OF DYESTUFFS FROM FIRST‐ TO SECOND‐CENTURY TEXTILE ARTEFACTS FOUND IN THE MARTRES‐DE‐VEYRE (FRANCE) EXCAVATIONS*

A series of Gallo‐Roman clothes and miscellaneous textile fragments from the first and second centuries from the Martres‐de‐Veyre necropolis (Puy‐de‐Dôme, France) was investigated. The objects studied were excavated between 1851 and 1923, during successive rounds of archaeological work. Since that time, they have been conserved in the Barguin Museum at Clermont‐Ferrand. The target of our research was dye identification, as it gives very interesting and useful information regarding the ancient technology. This approach has until now not been considered to be relevant and, unfortunately, is not systematic. The analysis was carried out by high‐performance liquid chromatography with photodiode array detection (HPLC–PDA). The small samples (threads up to 0.6 mg, less than 1 cm long) of coloured textile fibres were submitted to this technique. In one case, X‐ray fluorescence (XRF) analysis was applied. According to the analysis, the dyeing sources proposed are the Rubiaceae family for red, a luteolin ‘base’ for yellow, ellagitannins for brown and indigo for blue colours. Several samples did not seem to contain any dye. We point out possible factors for the partial dye source determination: instrumental limits, sample size, low dyestuff content in analysed samples and the dyes’ decomposition during ageing. Some improvements of dye analysis in archaeological samples by separation techniques based on recent analytical instrumentation and combined approaches are proposed.     

周一汉毛织品的染色工艺探讨

为探讨1985年新疆且末县扎洪鲁克墓群和洛浦山普拉墓群出土的一批周一汉毛染织品的染色工艺,用能量色散x射线荧光仪和色度仪对这批毛染织品分别进行了元素分析和反射光谱的测定。结果表明,这批毛染品均使用植物染料染色,分别采用四种染色工艺：直接染色、媒染染色、复染染色和套染染色。其中,蓝色毛织品为直接染色;红色毛织品采用了媒染、复染工艺,绿色毛织品由蓝色与黄色套染而成。进一步的研究表明,红色毛织品是用铝盐作媒染剂染色而成,铝盐含量与毛织品的色度呈相关性。说明能量色散X射线荧光分析仪和色度仪的使用是分析古代毛染品染色工艺的有效手段。     

IDENTIFICATION AND DIFFERENTIATION OF OPAQUE CHINESE OVERGLAZE YELLOW ENAMELS BY RAMAN SPECTROSCOPY AND SUPPORTING TECHNIQUES*

Using Raman spectroscopy, energy-dispersive X-ray fluorescence and X-ray diffraction, the Pb–Sn–Sb triple oxide yellow and lead–tin yellow have been identified on two pieces of cloisonné enamel (Falangcai) porcelains. Lead–tin yellow and lead antimonate yellow have been identified on famille rose porcelains manufactured before and after 1911, respectively. The replacement of the Pb–Sn–Sb triple oxide yellow by lead–tin yellow and that of the lead–tin yellow by lead antimonate yellow are discussed.     

Raman Spectroscopic Analysis of Ancient Egyptian Pigments

The application of FT‐Raman spectroscopy and visible Raman microscopy to the non‐destructive analysis of pigment specimens excavated from Tell el Amarna by Flinders Petrie in the 1890s has provided information about the chemical composition of the materials used by XVIIIth Dynasty artists in the New Kingdom at the time of King Akhenaten, c. 1340 bc. Comparison of the Raman spectra of the samples labelled ‘red and yellow ochre’ with documented, archival material from geological collections provided a clear indication of the materials used in the iron(III) oxide/hydroxide system, including α‐hematite, goethite, maghemite, magnetite and lepidocrocite. The yellow–orange specimen labelled ‘realgar’ proved to be a mixture of realgar and pararealgar; since the specimen had been sheltered from light since its excavation, this could indicate that the ancient Egyptian artists recognized the colour variation and may have used this to effect in their decorations. A specimen of yellow ochre contained goethite, α‐FeO.OH, with particles of crystalline, highly ordered graphite; in contrast, the red ochre specimens contained amorphous carbon particles.     

Identification of colourants in icons of the Cretan School of iconography using Raman spectroscopy and liquid chromatography

The stratigraphies of twenty five (25) samples removed from twenty (20) icons of the Cretan School of iconography are studied using Optical Microscopy and micro-Raman spectroscopy. The objects are dated in 15th–17th c. and belong to the collection of the Benaki Museum, Athens, Greece. Cinnabar, red ochre, minium, yellow ochre, azurite, malachite, lapis lazuli, lead white, carbon black, and indigo are identified in the cross-sections of the icon samples using Raman spectroscopy.     

Characterization of dyestuffs in ancient textiles from Xinjiang

Extraordinarily well-preserved organic remains from mortuary and settlement sites, including mummified bodies, are scattered along the outer, oasis-laden rim of the Tarim Basin in Xinjiang Province, China, ranging in date from about 1400 BC to the late first millennium BC. Specimens of textile finds from Chärchän, dated at about 1000 BC were selected for dye analysis using newly developed protocols employing high performance liquid chromatography with spectrophotometric and mass spectrometric detection. A single blue (from an indigo plant), a red (from madder, a Rubia species) and two yellow dyes were detected, although the exact plant source for none of them could be identified with certainty. This research offers new insights in the interpretation of textile finds from prehistoric Xinjiang, and more generally, of early Bronze Age Eurasia.     

SCIENTIFIC ANALYSIS OF SEVENTH‐CENTURY GLASS FRAGMENTS FROM THE CRYPTA BALBI IN ROME*

Inductively coupled plasma emission spectroscopy, reflectance spectroscopy and X‐ray diffraction were used to study seventh‐century AD glass fragments from the Crypta Balbi in Rome. All the samples were found to be silica‐soda‐lime glasses. Iron determines the colour of blue‐green, green and yellow‐green transparent glasses; chemical composition suggests deliberate addition of iron and/or manganese in about half the samples. Copper was found as the main colourant in red, pale blue and blue‐green opaque fragments; elemental copper acts as an opacifier in red glass, and calcium antimonate in white, pale blue and blue‐green glasses. Detection of antimony in transparent fragments suggests recycling of opaque mosaic tesserae.     

PIGMENTS AND PLASTERS FROM THE ROMAN SETTLEMENT OF THAMUSIDA (RABAT,MOROCCO)

A total of 22 samples were taken both from plasters still in situ and from collapsed material recovered by French, Italian and Moroccan teams at the Roman settlement of Thamusida (Rabat, Morocco). The sample characterization was obtained using optical microscopy, scanning electron microscopy, image analysis and Raman micro‐spectroscopy. Plaster aggregate was made using a mixture of sands and clays that outcrop nearby, while lime was probably produced using the local limestone crust, as was further verified for the mortars. The plasters from the bath complexes (public buildings) and the Temple à trois cellae (sacred building) were very poorly made, while those from areas VII and XX (private buildings) indicated the involvement of more expert masons. The pigments used were cinnabar, red ochre, yellow ochre, Egyptian blue, green earth, chalk white and carbon black. The overall manufacture was of low quality, and hence perfectly comparable to that observed in other Roman Provinces. With respect to Italy and to other Mediterranean Roman sites, Thamusida fits well within an aesthetic and technical koinè that differentiates sites of the Italian peninsula from those in the Provinces.     

CHARACTERIZATION OF PLASTERS FROM PTOLEMAIC BATHS: NEW EXCAVATIONS NEAR THE KARNAK TEMPLE COMPLEX,UPPER EGYPT*

The aim of the present work is to characterize plasters from Ptolemaic baths recently discovered in front of the Karnak temple complex, by the excavations of an Egyptian–French team. The characterization was carried out by means of optical microscopy (OM), scanning electron microscopy (SEM) equipped with an energy‐dispersive X‐ray detector (EDS), X‐ray diffraction analysis (XRD) and Fourier transform infrared spectroscopy (FT–IR). The results allowed the identification of the chemical composition and structure of these plasters. In addition, samples of red, yellow, black and white pigments were examined and identified. The results helped in providing an image concerning some materials used during the Ptolemaic era in ancient Egypt.     

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.     

Weaving value: Selling carpets in the liminal space of Istanbul's Grand Bazaar

All around the world, places of trade are typically conceived as places of deceit, if not outright danger: the plight of the carpet seller in Istanbul might be likened to that of the used car salesman in the West, for instance. But Istanbul’s Grand Bazaar is a particularly well-known centre of (perceived) deceit – the home of the trickster par excellence – and carpet sellers are the iconic bearers of this reputation. As a threshold of thresholds, the bazaar is a global crossroads, where a huge diversity of cultures and histories intersect, and carpets are objects that express this perhaps the most magnificently.     

FTIR imaging and HPLC reveal ancient painting and dyeing techniques of molluskan purple

Fourier transform infrared spectroscopy and imaging coupled to optical microscopy, scanning electron microscopy coupled to energy dispersive x-ray spectroscopy and high-performance liquid chromatography (HPLC) coupled to diode-array detection are used to investigate two samples removed from a painted decoration of a burial kline and a textile fragment, both found in Koru tumulus (fifth century BCE) in Daskyleion. Tyrian purple and kaolinite were identified in both samples, thus suggesting that the aluminosilicate compound had an important role in the applied painting and dyeing processes. The textile fragment is composed of undyed cotton and silk yarns dyed with the molluskan dye. The relative compositions of the molluskan materials used in the two archaeological objects are similar and comparable with the corresponding composition measured for a purple sample originated from Murex trunculus mollusks according to the HPLC results. This result is supported by principal component analysis (PCA) which, furthermore, takes into account the relative compositions of the extracts of the three Mediterranean mollusks, published in previous reports.     

北京市石景山区一清代墓葬出土纺织品染料与染色方法综合研究

清代的染色技术无论在染料的选择、染色方法,还是在获得颜色的数量上均达到我国古代天然染料染色的最高峰。文献和传世品研究极大推进了对清代纺织品染色技术的了解,但对清代考古纺织品染料的分析研究尚无结果发表。在此,对北京市石景山区2006年出土清代墓葬中纺织品的染料和染色方法进行了研究。化学分析使用超高效液相色谱法,首次将我国考古染料结合历史文献、传世纺织品颜色及染料组成详细比对,检测出苏木、黄檗、含鞣花酸染料(疑为橡斗)及蓝草四种染料。大多数样品上鉴定出一到两种染料,少数样品可能由三种或更多染料染成。相同的染料组合可以通过不同用量获得深浅不同的颜色。研究第一次对同一墓葬出土不同织物的染色方法进行比较,发现同种染料可以用于染不同类型、质地和用途的织物。这套纺织品所用的染料和染色方法与文献记载和传世样品都相符合。这一研究也是针对清代考古出土纺织品染料展开的首次成功的分析鉴定,补充了传世纺织品和染色历史文献,是清代染色史的重要部分。     

Identification of Pigments in Hellenistic and Roman Funeral Figurines

Microsamples removed from funeral figurines, which were found in two Hellenistic (third to second centuries bc ) and two Roman (first to second centuries ac ) tombs in the centre of Thessaloniki, Greece, are investigated following a multi‐analytical approach. Polarized light microscopy (PLM), X‐ray fluorescence (XRF) spectroscopy, micro‐Raman spectroscopy and high‐performance liquid chromatography coupled with a diode array detector (HPLC–DAD) are employed to identify both inorganic and organic pigments. PLM is useful to reveal the combinations of the colourants, which are identified as follows. Red ochre, cinnabar, yellow ochre, Egyptian blue, carbon black, calcite, dolomite and quartz are identified using XRF and Raman spectroscopy. HPLC–DAD is used to identify the organic colourants, which are rarely detected in painted objects of the Hellenistic and Roman period. In particular, cochineal and madder are found in six samples extracted from Hellenistic figurines. This is the first study describing the unequivocal identification of cochineal in Hellenistic objects. Furthermore, madder is identified in one sample dated to the Roman period. Madder lakes detected in the samples contain high amounts of purpurin; alizarin is either not detected or detected in trace amounts.     

古代染料及其分析检测技术

纺织品考古具有百年历史,但纺织品科技考古是一个新兴的研究领域。其中,古代染料的分析检测可以提供天然染料的来源、相关染色方法,甚至纺织品文物的生产地点和时间等重要信息,从而为古代文物的修复和保护提供科学依据,且有助于了解古代纺织服饰的色彩文化。古代染料按颜色分可分为红色系染料、蓝色系染料和黄色系染料等,其中:红色系染料中植物染料较为常见的有红花、苏木和茜草等,动物染料主要有南美胭脂虫、克玫兹胭脂虫和紫胶虫等；蓝色系染料一般为靛青,主要从含靛植物中获得,中国历史上使用的含靛植物主要有马蓝、木蓝、蓼蓝和菘蓝；黄色系染料主要包括黄栌、槐米、黄檗和姜黄等。目前,用于古代染料分析检测的方法主要有光纤反射光谱(FORS)、荧光光谱(FS)、高效液相色谱-质谱联用(HPLC-MS)和表面增强拉曼光谱(SERS)技术等,这些方法具有各自特点,为纺织品文物上天然染料的研究提供了科学支持。