DETERMINATION OF PIGMENTS AND BINDERS IN POMPEIAN WALL PAINTINGS USING SYNCHROTRON RADIATION – HIGH‐RESOLUTION X‐RAY POWDER DIFFRACTION AND CONVENTIONAL SPECTROSCOPY – CHROMATOGRAPHY

The employment of synchrotron techniques complemented by conventional laboratory systems has allowed us to deepen and improve our knowledge of Roman wall painting procedures. The palette identified in wall paintings from Pompeii and Herculaneum from the second century bc includes goethite, hematite, cinnabar, glauconite, Egyptian blue, and other components such as calcite and aragonite. Proof of the use of organic binders is provided by FTIR and PY–GC/MS. Therefore, the possibility of the use of ‘a secco’ techniques cannot be ruled out. Pigments in wall paintings are usually found in small percentages and conventional X‐ray diffractometers do not detect them. Synchrotron radiation – high‐resolution X‐ray powder diffraction has allowed identification with only a few micrograms of sample.     

SCIENTIFIC INVESTIGATIONS OF ANTIQUE LACQUERS FROM A 17TH‐CENTURY JAPANESE ORNAMENTAL CABINET

A recent restoration of a 17th‐century Japanese lacquer cabinet revealed various later treatments over the original black coating to maintain and preserve the high gloss of the oriental cabinet over the course of time and to meet changing tastes. The comprehensive investigation on a series of coating samples was executed by means of two hyphenated techniques: gas chromatography – mass spectrometry (GC–MS) and pyrolysis combined with GC–MS (Py‐GC–MS). The results showed that the original lacquer is based on urushi and linseed oil, while the past interventions are composed of sandarac, shellac and dammar. Additional microscopic studies proved the multi‐layer structure of the lacquer and the use of different pigments.     

The 9th‐Century‐AD Belitung Wreck,Indonesia: analysis of a resin lump

The 9th‐century‐AD Belitung wreck was discovered in 1998 in the Java Sea. Construction techniques rapidly confirmed that it was unlike any known Chinese or Southeast Asian vessel. The uncertainty about its origins was resolved in 2008 by timber identifications: it was constructed in the Middle East (probably Oman or Yemen). This paper, on the characterization of a dammar resin lump collected in the vicinity of the wreck, supplies additional evidence confirming the probable re‐stitching of the vessel somewhere in Asia. © 2010 The Authors     

A MULTI‐ANALYTICAL APPROACH FOR THE CHARACTERIZATION OF COMMODITIES IN A CERAMIC JAR FROM ANTINOE (EGYPT)*

This paper describes a multi‐analytical chemical study performed on the original, almost totally conserved, content of a small ceramic jar from the Antinoe archaeological site (fifth to seventh centuries ad, Roman Egypt) and now belonging to the archaeological collection of the Istituto Papirologico ‘Girolamo Vitelli’ (Florence, Italy). Scanning electron microscopy with an energy‐dispersive X‐ray spectrometer (SEM–EDX), Fourier transformed infrared spectroscopy (FTIR) and X‐ray diffraction (XRD) were all used to characterize the inorganic components of the archaeological material. The organic substances were analysed using FTIR, direct exposure mass spectrometry (DE–MS) and gas chromatography – mass spectrometry (GC–MS). The inorganic component essentially consisted of halite (NaCl). Among the NaCl crystals, lamellar elements were identified. They were chemically characterized by carbonato‐apatite and showed a concentric morphology typical of the scales of small fish. The most prevalent organic constituents of the sample were monocarboxylic acids, α,ω‐dicarboxylic acids, and cholesterol and its oxidation products. The organic material composition was consistent with the occurrence of lipids of animal origin. In addition, diterpenes related to pine pitch were also identified. The overall results suggest that the material recovered in the small ceramic jar found in Antinoe is a residue of fish‐based pickles such as garum, muria, allex and liquamen, which were commonly used in Roman times.     

ANALYSIS OF NASRID POLYCHROME CARPENTRY AT THE HALL OF THE MEXUAR PALACE,ALHAMBRA COMPLEX (GRANADA,SPAIN), COMBINING MICROSCOPIC,CHROMATOGRAPHIC AND SPECTROSCOPIC METHODS*†

The pigments, binders and execution techniques used by the Nasrids (1238–1492) to polychrome carpentry in the Hall of the Mexuar Palace at the Alhambra (Granada, Spain) were studied using optical microscopy, scanning electron microscopy with EDX analysis, selective staining techniques and gas chromatography – mass spectrometry. This pioneering investigation presents the first results of a research project devoted to filling gaps in the knowledge of Nasrid art, traditionally approached by stylistic studies. Moreover, it is essential for the polychromy conservation of the studied artworks, and will help to clarify historical and painting uncertainties in the Alhambra monument. The palette consists of a limited range of colours: white (lead‐base pigment), red (cinnabar and red lead), blue (lapis lazuli), black (carbon‐based) and false gold (golden tin). Tempera grassa was the painting technique identified. Two types of grounds were used: (i) gypsum in calligraphy decoration for the false gold technique, and (ii) synthetic minium in geometric drawings in carpentry. Organic insulating layers of linseed oil were used between paint strata. Artists applied synthetic minium to protect the wood (Juglans regia and conifer) against attack by xylophages. To lighten the surface darkened by this ground layer, powdered tin was added to achieve a metallic lustre.     

木材中挥发性有机酸的SPMEGC/MS分析研究

采用木材制作的藏展空间,木材释放出的挥发性有机酸,在一定的温湿度条件下,会对文物造成不良的影响,因此需要建立一套对木材挥发性有机酸测定的方法.为此,采用固相微萃取(SPME)样品预处理技术,分离富集木材中的挥发性有机物,结合气相色谱-质谱(GC/MS)联用技术对木材中挥发性有机酸进行半定量分析,研究了9种木材中挥发性有机酸的挥发量和分布规律.结果表明,不同木材有机酸的挥发量差别较大.实验结果可为博物馆在装修和储藏中对材料的筛选提供科学依据.     

博物馆藏展材料评估筛选的薄膜试片测试法

为改善Oddy测试法实验周期长,依靠目测判断腐蚀程度的状况研究建立了一种薄膜试片测试法,研发薄膜试片、设计成套测试容器与夹具、改变测试条件并结合数码采集腐蚀图像和对腐蚀图像数字化分析等简化藏展材料评估筛选实验操作、缩短测试时间和提高结果分级判别能力.另外,固相微萃取和气质联用仪(SPME-GC/MS)被用于表征藏展材料在挥发和降解过程中所释放的污染物成分,佐证其对银、铜和铅金属文物的潜在危害.新建薄膜试片测试法表明,14d的测试周期不仅大大缩短了测试时间,简化了操作,而且薄膜试片的使用也有利于克服人为分级的主观判断性,为数字化分级打下坚实基础.     

STUDY OF ROMAN ANCHOR FROM THE DEAD SEA SHORE*

A wooden Roman anchor was discovered at the retreating shore of the Dead Sea, north of Ein Gedi. The anchor's wood material was coated by a thick veneer of aragonite and gypsum crusts. The wood was dated by radiocarbon to the early Roman time in the Levant. Lead isotope analyses carried out on the Pb–Fe–Cu anchor material (remains of the anchor's metal parts) yielded ratios that indicate origin of the metal in Italian ores (maybe Tuscan). For the wooden part of the anchor a local tree was used.     

Subsistence practices and pottery use in Neolithic Jordan: molecular and isotopic evidence

This paper presents direct evidence of subsistence practices and pottery use at a Late Neolithic site at al-Basatîn, northern Jordan. Measurable concentrations of C_16:0 and C_18:0 were recovered from 8 of 10 archaeological pottery fragments through use of a microwave-assisted silica gel and aminopropyl solvent protocol developed for the isolation and concentration of free fatty acids in marine sediments. Subsequent isotopic analysis of the surviving C_16:0 and C_18:0 saturated fatty acids revealed ∂¹³C ratios consistent with those of adipose fats of ruminant and non-ruminant animals pastured on lands adjacent to the Jordan Valley. The high recovery of diagnostic compounds from the al-Basatîn material is discussed in context of a wider examination of the initial development and use of pottery in the Fertile Crescent, and the emerging debate concerning the efficacy of stable carbon isotope values in characterizing organic residues embedded in pottery fragments recovered from the earliest ceramic horizons in the Middle East and Europe.     

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.