scholarly journals X-Ray Fluorescence Analysis of a Gold Ibex and other Artifacts from Akrotiri

2019 ◽  
Vol 11 ◽  
Author(s):  
A. G. Karydas ◽  
T. Pantazis ◽  
C. Doumas ◽  
A. Vlachopoulos ◽  
P. Nomikos ◽  
...  
Keyword(s):  
Bulk Composition ◽  
Fluorescence Analysis ◽  
Wall Painting ◽  
Inorganic Elements ◽  
X Ray ◽  
Wide Range ◽  
Soldering Technology ◽  
Excavation Area

In-situ X-ray fluorescence analysis (XRF) of ancient artifacts from the excavation area was performed using a novel X-ray instrumentation, composed of a portable silicon PIN thermoelectrically cooled X-ray detector, a miniature X-ray source, and portable data acquisition devices. The main objective of the analyses in Akrotiri was to explore the potential of the technique to provide answers to a wide range of archaeometric questions regarding the bulk composition of metal alloys, especially of gold, the characterization of corrosion products in bronze artifacts, identification of inorganic elements which are fingerprints of the minerals used in wall-painting pigments, and of the painting materials and techniques used for the decoration of clay vase surfaces. Among the analysed artifacts are a unique gold ibex, a bronze dagger and blade, various pigments from the wall paintings of room 3 in Xeste 3, decoration pigments from rosettes of faience, a bichrome jug, and other clay vases. The results of the in-situ XRF survey, primarily those of the bulk composition and soldering technology of the gold ibex, are discussed and compared with literature.

scholarly journals Applications with a brighter X-ray source and new detectors from Agilent

2014 ◽  
Vol 70 (a1) ◽  
pp. C1734-C1734
Author(s):  
Zoltan Gal ◽  
Tadeusz Skarzynski ◽  
Fraser White ◽  
Oliver Presly ◽  
Adrian Jones ◽  
...  
Keyword(s):  
Data Quality ◽  
Single Crystal ◽  
Measurement System ◽  
Single Crystal Diffraction ◽  
X Ray ◽  
Vacuum Technology ◽  
Intelligent Measurement ◽  
Wide Range

Agilent Technologies develop and supply X-ray systems for single-crystal diffraction research, including the SuperNova; a compact, highly reliable and very low maintenance instrument providing X-ray data of the highest quality; and the PX Scanner for testing and characterization of protein crystals in their original crystallization drops (in-situ). The SuperNova and PX Scanner are constantly improving, with recent enhancements including a new range of detectors using an Intelligent Measurement System. The Eos S2, Atlas S2 and Titan S2 detector range employs a smart sensitivity control of the electronic gain and is capable of instantaneously switching its binning modes thus providing unprecedented flexibility in tuning every exposure to provide the highest data quality for a wide range of experiments. We have also developed a completely new micro-focus X-ray source based on Gradient Vacuum technology, with novel filament and target designs. This novel source is an integral part of the new Agilent GV1000 X-ray diffractometer, which has been designed for applications that require even higher brightness of the X-ray beam.

The Use of Advanced Analytical Techniques for Characterization of the Chemical, Physical, and Crystallographic Nature of a Surface

1973 ◽  
Vol 31 ◽  
pp. 132-133 ◽  
Author(s):  
R. E. Herfert
Keyword(s):  
Surface Characterization ◽  
Analytical Techniques ◽  
X Ray Diffraction ◽  
Depth Of Penetration ◽  
X Ray ◽  
The Past ◽  
Transmission Electron ◽  
Scanning Electron

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.

scholarly journals In-situ characterization of highly reversible phase transformation by synchrotron X-ray Laue microdiffraction

2016 ◽  
Vol 108 (21) ◽  
pp. 211902 ◽  
Author(s):  
Xian Chen ◽  
Nobumichi Tamura ◽  
Alastair MacDowell ◽  
Richard D. James
Keyword(s):  
Phase Transformation ◽  
In Situ Characterization ◽  
X Ray ◽  
Reversible Phase ◽  
Laue Microdiffraction

scholarly journals Structural Characterization of Heterodinuclear ZnII-LnIII Complexes (Ln = Pr, Nd) with a Ring-Contracted H2valdien-Derived Schiff Base Ligand

2021 ◽  
Author(s):  
Shabana Noor ◽  
Richard Goddard ◽  
Fehmeeda Khatoon ◽  
Sarvendra Kumar ◽  
Rüdiger W. Seidel
Keyword(s):  
Molecular Structure ◽  
Schiff Base ◽  
Structural Characterization ◽  
Schiff Base Ligand ◽  
Crystal And Molecular Structure ◽  
X Ray ◽  
X Ray Crystallography ◽  
Imidazoline Ring

AbstractSynthesis and structural characterization of two heterodinuclear ZnII-LnIII complexes with the formula [ZnLn(HL)(µ-OAc)(NO3)2(H2O)x(MeOH)1-x]NO3 · n H2O · n MeOH [Ln = Pr (1), Nd (2)] and the crystal and molecular structure of [ZnNd(HL)(µ-OAc)(NO3)2(H2O)] [ZnNd(HL)(OAc)(NO3)2(H2O)](NO3)2 · n H2O · n MeOH (3) are reported. The asymmetrical compartmental ligand (E)-2-(1-(2-((2-hydroxy-3-methoxybenzylidene)amino)-ethyl)imidazolidin-2-yl)-6-methoxyphenol (H2L) is formed from N1,N3-bis(3-methoxysalicylidene)diethylenetriamine (H2valdien) through intramolecular aminal formation, resulting in a peripheral imidazoline ring. The structures of 1–3 were revealed by X-ray crystallography. The smaller ZnII ion occupies the inner N2O2 compartment of the ligand, whereas the larger and more oxophilic LnIII ions are found in the outer O2O2’ site. Graphic Abstract Synthesis and structural characterization of two heterodinuclear ZnII-LnIII complexes (Ln = Pr, Nd) bearing an asymmetrical compartmental ligand formed in situ from N1,N3-bis(3-methoxysalicylidene)diethylenetriamine (H2valdien) through intramolecular aminal formation are reported.

Reference-free, depth-dependent characterization of nanolayers and gradient systems with advanced grazing incidence X-ray fluorescence analysis

2015 ◽  
Vol 212 (3) ◽  
pp. 523-528 ◽  
Author(s):  
Philipp Hönicke ◽  
Blanka Detlefs ◽  
Matthias Müller ◽  
Erik Darlatt ◽  
Emmanuel Nolot ◽  
...  
Keyword(s):  
Fluorescence Analysis ◽  
Grazing Incidence ◽  
X Ray ◽  
Gradient Systems

In situsmall-angle X-ray scattering characterization of X-ray-induced local heating

2014 ◽  
Vol 47 (6) ◽  
pp. 2078-2080 ◽  
Author(s):  
Monika Witala ◽  
Jun Han ◽  
Andreas Menzel ◽  
Kim Nygård
Keyword(s):  
Local Heating ◽  
Liquid Mixtures ◽  
Glass Capillary ◽  
Sample Container ◽  
X Ray ◽  
X Ray Scattering ◽  
Synchrotron Light ◽  
Ray Scattering

It is shown that small-angle X-ray scattering from binary liquid mixtures close to the critical point of demixing can be used forin situcharacterization of beam-induced heating of liquid samples. For demonstration purposes, the proposed approach is applied on a well studied critical mixture of water and 2,6-lutidine. Given a typical incident X-ray flux at a third-generation synchrotron light source and using a 1.5 mm-diameter glass capillary as sample container, a beam-induced local temperature increase of 0.45 ± 0.10 K is observed.

Anin situatomic force microscope for normal-incidence nanofocus X-ray experiments

2016 ◽  
Vol 23 (5) ◽  
pp. 1110-1117 ◽  
Author(s):  
M. V. Vitorino ◽  
Y. Fuchs ◽  
T. Dane ◽  
M. S. Rodrigues ◽  
M. Rosenthal ◽  
...  
Keyword(s):  
Thin Film ◽  
Atomic Force Microscope ◽  
High Speed ◽  
Normal Incidence ◽  
Organic Thin Film ◽  
X Ray ◽  
Atomic Force ◽  
Synchrotron Beamlines

A compact high-speed X-ray atomic force microscope has been developed forin situuse in normal-incidence X-ray experiments on synchrotron beamlines, allowing for simultaneous characterization of samples in direct space with nanometric lateral resolution while employing nanofocused X-ray beams. In the present work the instrument is used to observe radiation damage effects produced by an intense X-ray nanobeam on a semiconducting organic thin film. The formation of micrometric holes induced by the beam occurring on a timescale of seconds is characterized.

scholarly journals Synchrotron radiation microbeam X-ray fluorescence analysis of zinc concentration in remineralized enamel in situ

2009 ◽  
Vol 54 (5) ◽  
pp. 420-423 ◽  
Author(s):  
Tsunenori Matsunaga ◽  
Hidetaka Ishizaki ◽  
Shuji Tanabe ◽  
Yoshihiko Hayashi
Keyword(s):  
Synchrotron Radiation ◽  
Zinc Concentration ◽  
Fluorescence Analysis ◽  
X Ray

scholarly journals Characterization of Ti/SnO2 Interface by X-ray Photoelectron Spectroscopy

Nanomaterials ◽  
2022 ◽  
Vol 12 (2) ◽  
pp. 202
Author(s):  
Miranda Martinez ◽  
Anil R. Chourasia
Keyword(s):  
Photoelectron Spectroscopy ◽  
Room Temperature ◽  
Chemical Interaction ◽  
Photoelectron Spectra ◽  
X Ray ◽  
Increasing Trend ◽  
Substrate Temperatures ◽  
Beam Technique

The Ti/SnO2 interface has been investigated in situ via the technique of x-ray photoelectron spectroscopy. Thin films (in the range from 0.3 to 1.1 nm) of titanium were deposited on SnO2 substrates via the e-beam technique. The deposition was carried out at two different substrate temperatures, namely room temperature and 200 °C. The photoelectron spectra of tin and titanium in the samples were found to exhibit significant differences upon comparison with the corresponding elemental and the oxide spectra. These changes result from chemical interaction between SnO2 and the titanium overlayer at the interface. The SnO2 was observed to be reduced to elemental tin while the titanium overlayer was observed to become oxidized. Complete reduction of SnO2 to elemental tin did not occur even for the lowest thickness of the titanium overlayer. The interfaces in both the types of the samples were observed to consist of elemental Sn, SnO2, elemental titanium, TiO2, and Ti-suboxide. The relative percentages of the constituents at the interface have been estimated by curve fitting the spectral data with the corresponding elemental and the oxide spectra. In the 200 °C samples, thermal diffusion of the titanium overlayer was observed. This resulted in the complete oxidation of the titanium overlayer to TiO2 upto a thickness of 0.9 nm of the overlayer. Elemental titanium resulting from the unreacted overlayer was observed to be more in the room temperature samples. The room temperature samples showed variation around 20% for the Ti-suboxide while an increasing trend was observed in the 200 °C samples.

scholarly journals In situ X-ray Diffraction Investigation of the Crystallisation of Perfluorinated Ce(IV)-based Metal-Organic Frameworks with UiO-66 and MIL-140 architectures

2020 ◽  
Author(s):  
Stephen Shearan ◽  
Jannick Jacobsen ◽  
Ferdinando Costantino ◽  
Roberto D’Amato ◽  
Dmitri Novikov ◽  
...  
Keyword(s):  
Crystal Growth ◽  
Metal Organic Frameworks ◽  
Building Blocks ◽  
Nucleation And Growth ◽  
X Ray Diffraction ◽  
X Ray ◽  
Rate Determining Step ◽  
Wide Range ◽  
Metal Organic

We report on the results of a thorough <i>in situ</i> synchrotron powder X-ray diffraction study of the crystallisation in aqueous medium of two recently discovered perfluorinated Ce(IV)-based metal-organic frameworks (MOFs), analogues of the already well investigated Zr(IV)-based UiO-66 and MIL-140A, namely, F4_UiO-66(Ce) and F4_MIL-140A(Ce). The two MOFs were originally obtained in pure form in similar conditions, using ammonium cerium nitrate and tetrafluoroterephthalic acid as building blocks, and small variations of the reaction parameters were found to yield mixed phases. Here, we investigate the crystallisation of these compounds <i>in situ</i> in a wide range of conditions, varying parameters such as temperature, amount of the protonation modulator nitric acid (HNO<sub>3</sub>) and amount of the coordination modulator acetic acid (AcOH). When only HNO<sub>3</sub> is present in the reaction environment, F4_MIL-140A(Ce) is obtained as a pure phase. Heating preferentially accelerates nucleation, which becomes rate determining below 57 °C, whereas the modulator influences nucleation and crystal growth to a similar extent. Upon addition of AcOH to the system, alongside HNO<sub>3</sub>, mixed-phased products, consisting of F4_MIL-140A(Ce) and F4_UiO-66(Ce), are obtained. In these conditions, F4_UiO-66(Ce) is always formed faster and no interconversion between the two phases occurs. In the case of F4_UiO-66(Ce), crystal growth is always the rate determining step. An increase in the amount of HNO<sub>3</sub> slows down both nucleation and growth rates for F4_MIL-140A(Ce), whereas nucleation is mainly affected for F4_UiO-66(Ce). In addition, a higher amount HNO<sub>3</sub> favours the formation of F4_MIL-140A(Ce). Similarly, increasing the amount of AcOH leads to slowing down of the nucleation and growth rate, but favours the formation of F4_UiO-66(Ce). The pure F4_UiO-66(Ce) phase could also be obtained when using larger amounts of AcOH in the presence of minimal HNO<sub>3</sub>. Based on these <i>in situ</i> results, a new optimised route to achieving a pure, high quality F4_MIL-140A(Ce) phase in mild conditions (60 °C, 1 h) is also identified.

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