scholarly journals Application of analytical techniques to the unveiling of the glazing technology of medieval pottery from the Belgrade Fortress

2020 ◽  
Vol 85 (10) ◽  
pp. 1329-1343
Author(s):  
Ljiljana Damjanovic-Vasilic ◽  
Vesna Bikic ◽  
Srna Stojanovic ◽  
Danica Bajuk-Bogdanovic ◽  
Djurdjija Dzodan ◽  
...  

Medieval glazed ceramics, dated to the early 15th century, excavated at the Belgrade Fortress, Serbia, were investigated by combining optical microscopy, X-ray powder diffraction (XRPD), scanning electron microscopy with energy-dispersive spectroscopy (SEM-EDS), micro-Raman spectroscopy and multivariate statistical analysis. The decoration and style of the investigated ceramics were characteristic of workshops from different areas of the medieval Serbian State: Ras, Krusevac and Belgrade/Smederevo. Comparison was made with ceramic samples from the same period excavated at the Studenica Monastery, the hitherto earliest workshop discovered, which were used as reference material for the Ras area. Ceramics from the Belgrade Fortress were covered with a transparent, lead-based glaze. The majority of the glazes were produced by application of mixture of lead oxide and quartz to the clay body, whereas only two samples were glazed by application of lead oxide by itself. The brown colours of the glaze originated from Fe-based spinel, whereas copper and iron were responsible for the colouring of the green and yellow glazes. The obtained results revealed glazing technology taken from Byzantine tradition.

2015 ◽  
Vol 69 (4) ◽  
pp. 387-393
Author(s):  
Sofija Stojanovic ◽  
Maja Gajic-Kvascev ◽  
Ljiljana Damjanovic

Russian icon painted on wooden panel analyzed in this work is interesting for art historians because there is no precise information in which workshops it was made or who the author was. Similar icons are often found in churches and monasteries in our region. In order to obtain information about materials used for creation of investigated icon two micro-analytical techniques were used: Energy-Dispersive X-Ray Fluorescence spectroscopy (EDXRF) and micro-Raman spectroscopy. Obtained results confirmed presence of following materials: lead-white, vermilion, minium, ultramarine, brown and green earth pigments and silver in combination with yellow organic varnish, which served to an iconographer for gilding. Ground layer was made of calcite. Blue pigment ultramarine was probably used for blue colour as well as for obtaining particulars hues in several parts of the paint layer. This can be important information for further research concerning particular workshop in which the icon was made. Identified materials are typical for Russian iconography of the 19th century.


ACTA IMEKO ◽  
2021 ◽  
Vol 10 (1) ◽  
pp. 234
Author(s):  
Tilde De Caro ◽  
Emma Angelini ◽  
Leila Es Sebar

<p>In this paper, a study of the corrosion products formed on archaeological bronze artefacts excavated in Tharros (Sardinia, Italy) is presented. The investigation was carried out by means of the combination of different analytical techniques, including optical microscopy, micro-Raman spectroscopy (µ-RS), scanning electron microscopy coupled with energy dispersive X-ray spectroscopy and X-ray diffraction. The artefacts under study are three bronze coins from the Phoenician–Punic period that are deeply corroded due to the chloride-rich soil of the Tharros excavation site. µ-Raman spectroscopy was chosen to investigate the corroded surfaces of the artefacts because it is a non-destructive technique, it has high spatial resolution, and it makes it possible to discriminate between polymorphs and correlate colour and chemical composition. Through µ-RS, it was possible to identify different mineralogical phases and different polymorphs, such as cuprite (Cu<sub>2</sub>O), copper trihydroxychloride [Cu<sub>2</sub>Cl(OH)<sub>3</sub>] polymorphs, hydroxy lead chloride laurionite [PbCl(OH)] and calcium carbonate polymorph aragonite. The experimental findings highlight that micro-Raman spectroscopy can be used to provide further knowledge regarding the environmental factors that may cause the degradation of archaeological bronzes in soil.</p>


Author(s):  
R. E. Herfert

Studies of the nature of a surface, either metallic or nonmetallic, in the past, have been limited to the instrumentation available for these measurements. In the past, optical microscopy, replica transmission electron microscopy, electron or X-ray diffraction and optical or X-ray spectroscopy have provided the means of surface characterization. Actually, some of these techniques are not purely surface; the depth of penetration may be a few thousands of an inch. Within the last five years, instrumentation has been made available which now makes it practical for use to study the outer few 100A of layers and characterize it completely from a chemical, physical, and crystallographic standpoint. The scanning electron microscope (SEM) provides a means of viewing the surface of a material in situ to magnifications as high as 250,000X.


Author(s):  
G. Remond ◽  
R.H. Packwood ◽  
C. Gilles ◽  
S. Chryssoulis

Merits and limitations of layered and ion implanted specimens as possible reference materials to calibrate spatially resolved analytical techniques are discussed and illustrated for the case of gold analysis in minerals by means of x-ray spectrometry with the EPMA. To overcome the random heterogeneities of minerals, thin film deposition and ion implantation may offer an original approach to the manufacture of controlled concentration/ distribution reference materials for quantification of trace elements with the same matrix as the unknown.In order to evaluate the accuracy of data obtained by EPMA we have compared measured and calculated x-ray intensities for homogeneous and heterogeneous specimens. Au Lα and Au Mα x-ray intensities were recorded at various electron beam energies, and hence at various sampling depths, for gold coated and gold implanted specimens. X-ray intensity calculations are based on the use of analytical expressions for both the depth ionization Φ (ρz) and the depth concentration C (ρz) distributions respectively.


Author(s):  
Karen A. Katrinak ◽  
James R. Anderson ◽  
Peter R. Buseck

Aerosol samples were collected in Phoenix, Arizona on eleven dates between July 1989 and April 1990. Elemental compositions were determined for approximately 1000 particles per sample using an electron microprobe with an energy-dispersive x-ray spectrometer. Fine-fraction samples (particle cut size of 1 to 2 μm) were analyzed for each date; coarse-fraction samples were also analyzed for four of the dates.The data were reduced using multivariate statistical methods. Cluster analysis was first used to define 35 particle types. 81% of all fine-fraction particles and 84% of the coarse-fraction particles were assigned to these types, which include mineral, metal-rich, sulfur-rich, and salt categories. "Zero-count" particles, consisting entirely of elements lighter than Na, constitute an additional category and dominate the fine fraction, reflecting the importance of anthropogenic air pollutants such as those emitted by motor vehicles. Si- and Ca-rich mineral particles dominate the coarse fraction and are also numerous in the fine fraction.


2019 ◽  
Author(s):  
Paul Pearce ◽  
Gaurav Assat ◽  
Antonella Iadecola ◽  
François Fauth ◽  
Rémi Dedryvère ◽  
...  

The recent discovery of anionic redox as a means to increase the energy density of transition metal oxide positive electrodes is now a well established approach in the Li-ion battery field. However, the science behind this new phenomenon pertaining to various Li-rich materials is still debated. Thus, it is of paramount importance to develop a robust set of analytical techniques to address this issue. Herein, we use a suite of synchrotron-based X-ray spectroscopies as well as diffraction techniques to thoroughly characterize the different redox processes taking place in a model Li-rich compound, the tridimentional hyperhoneycomb β-Li2IrO3. We clearly establish that the reversible removal of Li+ from this compound is associated to a previously described reductive coupling mechanism and the formation of the M-(O-O) and M-(O-O)* states. We further show that the respective contributions to these states determine the spectroscopic response for both Ir L3-edge X-ray absorption spectroscopy (XAS) and X-ray photoemissions spectroscopy (XPS). Although the high covalency and the robust tridimentional structure of this compound enable a high degree of reversibile delithiation, we found that pushing the limits of this charge compensation mechanism has significant effects on the local as well as average structure, leading to electrochemical instability over cycling and voltage decay. Overall, this work highlights the practical limits to which anionic redox can be exploited and sheds some light on the nature of the oxidized species formed in certain lithium-rich compounds.<br>


2019 ◽  
Author(s):  
Paul Pearce ◽  
Gaurav Assat ◽  
Antonella Iadecola ◽  
François Fauth ◽  
Rémi Dedryvère ◽  
...  

The recent discovery of anionic redox as a means to increase the energy density of transition metal oxide positive electrodes is now a well established approach in the Li-ion battery field. However, the science behind this new phenomenon pertaining to various Li-rich materials is still debated. Thus, it is of paramount importance to develop a robust set of analytical techniques to address this issue. Herein, we use a suite of synchrotron-based X-ray spectroscopies as well as diffraction techniques to thoroughly characterize the different redox processes taking place in a model Li-rich compound, the tridimentional hyperhoneycomb β-Li2IrO3. We clearly establish that the reversible removal of Li+ from this compound is associated to a previously described reductive coupling mechanism and the formation of the M-(O-O) and M-(O-O)* states. We further show that the respective contributions to these states determine the spectroscopic response for both Ir L3-edge X-ray absorption spectroscopy (XAS) and X-ray photoemissions spectroscopy (XPS). Although the high covalency and the robust tridimentional structure of this compound enable a high degree of reversibile delithiation, we found that pushing the limits of this charge compensation mechanism has significant effects on the local as well as average structure, leading to electrochemical instability over cycling and voltage decay. Overall, this work highlights the practical limits to which anionic redox can be exploited and sheds some light on the nature of the oxidized species formed in certain lithium-rich compounds.<br>


2018 ◽  
Author(s):  
Zoltán Kis ◽  
Katalin Gméling ◽  
Tímea Kocsis ◽  
János Osán ◽  
Mihály András Pocsai ◽  
...  

We present precise analysis of major and trace elements of the humic acid. We used three different element analytical techniques in our investigations as prompt-gamma activation analysis (PGAA), neutron activation analysis (NAA) and X-ray fluorescence (XRF) analysis was carried out. We identified 42 elements in our sample.


Author(s):  
Deepak Goyal

Abstract Next generation assembly/package development challenges are primarily increased interconnect complexity and density with ever shorter development time. The results of this trend present some distinct challenges for the analytical tools/techniques to support this technical roadmap. The key challenge in the analytical tools/techniques is the development of non-destructive imaging for improved time to information. This paper will present the key drivers for the non-destructive imaging, results of literature search and evaluation of key analytical techniques currently available. Based on these studies requirements of a 3D imaging capability will be discussed. Critical breakthroughs required for development of such a capability are also summarized.


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