Archaeometric analysis of ceramic production in Tiwanaku state (c.500–1000 ce): An exploratory study

The chemical and mineralogical characterization of seven ceramic fragments produced within Tiwanaku state (c.500–1000 ce ) is reported. The instrumental techniques used included X‐ray elemental and mineralogical chemical analysis, Raman spectroscopy, and scanning and light microscopy. The results indicate there are several clay types, although they show similarities, such as the use of a plant‐based temper. The red colour of the decoration is hematite, and manganese oxides such as jacobsite are present in the black. The white colour is a mixture of gypsum and clay, and the orange is a mixture of hematite and clay. The use of colours, the quality of the clays and the temperatures reached during pottery firing point to expertise in ceramic production and to complex decision‐making processes. The multi‐elemental archaeometric approach documented here could become an important tool to shed a light on ancient ceramic technology and the internal variance of Tiwanaku pottery.     

The Pyramids—Cement or Stone?

Several samples of pyramids from Giza were obtained. The samples were analysed by scanning electron microscopy, electron diffraction by X-rays, powder X-ray diffraction, inductively coupled plasmography, Fourier-transform infrared spectroscopy and other techniques. Some scientists who have recently studied the pyramids have suggested that the pyramids were poured into place, stone by stone. The prevailing theory among Egyptologists is, of course, that the pyramids were built from blocks of natural stone. All of the results obtained during this study directly support the concept that the pyramids are made of limestone and are not cementitious in nature.     

X-ray fluorescence analysis of late Roman and Sassanian silver plate

About 200 analyses have been made on late Roman and Sassanian silver objects using energy-dispersive X-ray fluorescence. This has shown that the main feature of the composition of the silver throughout the period and across the geographical area studied was towards high fineness (average silver percentage about 95%). Compositional differences are found between Roman and Sassanian silversmiths' products for the elements copper and lead. Much of the material analysed came from hoards, and using a statistical technique on the analytical data (Discriminant Analysis) broad compositional differences between hoards were found to emerge. The use of different compositions of silver for different joined parts of a single object are discussed.     

拉曼光谱在纸质文物研究中的应用

纸张的老化程度一直是纸质文物保护中的重要研究方面,以往多采用目测法和经验来推断纸张的老化程度。纸张物理强度、聚合度等能表征老化状态的理化性能测试由于需要大量的样品而无法用于文物检测。近年来随着显微共聚焦拉曼光谱、近红外傅里叶变换拉曼光谱、表面增强拉曼光谱等技术的发展,作为一种原位、无损、微区的分析方法,拉曼光谱被越来越多地应用到了纸质文物的相关分析研究中,为纸质文物的保护修复提供科学依据。结合国内外文献,对拉曼光谱在纸张老化、碳黑颜料以及其他颜料上的应用和研究现状进行了梳理归纳。随着拉曼光谱应用的不断深入,以及与其他分析技术、化学计量学等的结合,未来将在纸质文物研究中发挥更多的作用。     

Can the Raman spectrum of anatase in artwork and archaeology be used for dating purposes? Identification by Raman microscopy of anatase in decorative coatings on Neolithic (Yangshao) pottery from Henan,China

Scanning electron microscopy/energy dispersive X-ray analysis has earlier shown that the white background layer (slip) on painted pottery sherds (Yangshao culture, Henan, China, 4200 BC) is composed of kaolinitic clay containing titanium in the assumed form of TiO₂ at just 1 wt%. The same samples of white slip have now been studied by Raman microscopy, revealing bands characteristic of anatase, but none from the majority species, the matrix of kaolinitic clay. These results highlight the extraordinarily intense Raman scattering from even trace amounts of anatase and thus the need to recognise that, although the colours of archaeological artefacts are almost always determined by the nature of the matrix, the Raman spectrum may be determined by a highly scattering trace component such as anatase. The significance of anatase as a potential date-marker pigment on works of art and archaeological artefacts is discussed.     

唐武惠妃墓出土疑似胶结材料的分析研究

为了确定武惠妃墓室内发现的黑色多孔块状物质是否为绘制壁画时使用的胶结材料,联合使用显微镜观察、SEM-EDS、Raman、FTIR和GC-FID多种分析方法对该物质进行了显微结构观察、元素组成及物质组成分析。结果表明,该物质虽已炭化,但内部仍可见一些较新鲜的胶料残留,其成分为动物胶,并在其中发现了少量红色朱砂颜料残留。通过古文献记载和以往研究成果讨论了结果的可靠性。该研究不仅丰富了唐代墓葬壁画绘制技艺的考古学研究,更可为后期文物保护材料和工艺的选择提供借鉴。     

A Pigment Characterization Approach to Selection of Dating Methods and Interpretation of Rock Art: The Case of the Mikinak Site,Lake Wapizagonke,Quebec, Canada

Dating is perhaps the most frequently asked question in rock art studies, but still one of the most difficult to answer. However, chronology is vital in order to understand and interpret rock art sites. Unfortunately, attempts at dating the Mikinak site, at Lake Wapizagonke, Quebec, Canada were unsuccessful. But a multi‐instrumental protocol applied to characterize paintings shows that at least three different paint recipes were employed to create the site. These may reflect three different phases of paintings, and that at least three different artists contributed to the production of this site.     

利用激光拉曼对宋代官窑青瓷样品釉烧温度的研究

本文利用激光拉曼光谱仪和能量色散X-射线荧光光谱仪对21件取自故宫博物院院藏宋代官窑完整器及42件取自杭州老虎洞官窑窑址的青瓷样品表面釉层进行了测量与分析。通过计算瓷釉样品拉曼光谱中位于500cm-1附近宽带与位于1000cm-1附近宽带的面积比值(Ip值)及利用EDXRF分析样品的元素成分,讨论了这些样品的主要助熔剂成分Ca O、K2O含量与Ip值之间的关系,并通过对成分具有两类典型官窑瓷器釉料特征且在不同烧成温度下烧制的模拟釉块进行拉曼分析,对宋官窑青瓷样品的釉烧温度进行了讨论。     

山东危山西汉墓出土陶器彩绘颜料研究

为研究山东危山西汉墓出土彩绘陶器颜料成分,采用偏光显微镜、显微拉曼光谱仪和扫描电子显微镜-能谱仪进行了分析。研究结果显示,危山汉墓陶器彩绘颜料有朱砂、铅丹、中国紫(汉紫BaCuSi2O6)、铁红、铁黑、白土等。中国紫颜料首次在山东省的发现,扩大了该颜料的使用区域,具有重要的考古学意义。另外,还在紫色颜料中分析出了BaCu2Si2O7蓝色晶体,这是继中国蓝中国紫之后的又一重大发现。     

Freezing and melting behaviors of H2O‐NaCl‐CaCl2 solutions in fused silica capillaries and glass‐sandwiched films: implications for fluid inclusion studies

Fluid inclusions of the H₂O‐NaCl‐CaCl₂ system are notorious for their metastable behavior during cooling and heating processes, which can render microthermometric measurement impossible or difficult and interpretation of the results ambiguous. This study addresses these problems through detailed microscopic examination of synthetic solutions during cooling and warming runs, development of methods to enhance nucleation of hydrates, and comparison of microthermometric results with different degrees of metastability with values predicted for stable conditions. Synthetic H₂O‐NaCl‐CaCl₂ solutions with different NaCl/(NaCl + CaCl₂) ratios were prepared and loaded in fused silica capillaries and glass‐sandwiched films for microthermometric studies; pure solutions were used with the capillaries to simulate fluid inclusions, whereas alumina powder was added in the solutions to facilitate ice and hydrate crystallization in the sandwiched samples. The phase changes observed and the microthermometric data obtained in this study have led to the following conclusions that have important implications for fluid inclusion studies: (i) most H₂O‐NaCl‐CaCl₂ inclusions that appear to be completely frozen in the first cooling run to ?185°C actually contain large amounts of residual solution, as also reported in some previous studies; (ii) inability of H₂O‐NaCl‐CaCl₂ inclusions to freeze completely may be related to their composition (low NaCl/(NaCl + CaCl₂) ratios) and lack of solid particles; (iii) crystallization of hydrates, which is important for cryogenic Raman spectroscopic studies of fluid inclusion composition, can be greatly enhanced by finding an optimum combination of cooling and warming rates and temperatures; and (iv) even if an inclusion is not completely frozen, the melting temperatures of hydrohalite and ice are still valid for estimating the fluid composition.