Investigation of (micro-)meteoritic materials at the new hard X-ray imaging PUMA beamline for heritage sciences

2019 ◽  
Vol 26 (6) ◽  
pp. 2033-2039 ◽  
Author(s):  
Pieter Tack ◽  
Benjamin Bazi ◽  
Bart Vekemans ◽  
Tulin Okbinoglu ◽  
Flore Van Maldeghem ◽  
...  
Keyword(s):  
Analytical Techniques ◽  
X Ray Diffraction ◽  
Contrast Imaging ◽  
X Ray ◽  
High Profile ◽  
Imaging Tool ◽  
X Ray Imaging ◽  
Synchrotron Facility ◽  
Wide Range ◽  
New Instrument

At the French synchrotron facility SOLEIL, a new X-ray imaging facility PUMA (Photons Utilisés pour les Matériaux Anciens) has been made available to scientific communities studying materials from cultural heritage. This new instrument aims to achieve 2D and 3D imaging with microscopic resolution, applying different analytical techniques including X-ray fluorescence spectroscopy (XRF), X-ray absorption spectroscopy (XAS), X-ray diffraction and phase-contrast imaging. In order to discover its capabilities a detailed analytical characterization of this beamline as an analytical and imaging tool is deemed necessary. In this work, (confocal) XRF and XAS analyses are demonstrated using the Seymchan pallasite meteorite and an Antarctic unmelted micrometeorite as case studies. The obtained spatial resolution (2 µm × 3 µm) and sensitivity (detection limits <10 p.p.m. for 1 s acquisition at 18 keV) show that PUMA is a competitive state-of-the-art beamline, providing several high-profile and high-in-demand analytical methods while maintaining applicability towards a wide range of heritage-oriented sciences.

scholarly journals Stabilising peroxyacids in niche microenvironments

2014 ◽  
Vol 70 (a1) ◽  
pp. C644-C644
Author(s):  
Dyanne Cruickshank ◽  
Chick Wilson
Keyword(s):  
Chemical Reactivity ◽  
Analytical Techniques ◽  
Direct Consequence ◽  
High Reactivity ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Wide Range ◽  
Chemically Reactive Species ◽  
Household Cleaning Products

There has been dramatic evolution in the formulation of household cleaning products over the last decade, this is mainly due to the influence of social change, regulatory pressure and the need for new less toxic, safer formulations with increased performance. Due to their high chemical reactivity, peroxides are found in a wide range of bleaching agents, they are known for their instability which is a direct consequence of their high reactivity (in turn essential for function). Stabilising such materials for implementation in a range of product types is a significant target within the domestic products industry. Supramolecular approaches are already being explored to try stabilise other chemically reactive species such as explosives [1,2] thus illustrating the feasibility of this research. The work to be presented will deal with peroxyacids that include small model compounds such as m-chloroperbenzoic acid as well as a commericially relevant bleaching agent and their inclusion in both crystalline and amorphous hosting systems. Single crystal X-ray diffraction methods are used to elucidate the ordered crystalline structures and to confirm whether or not the peroxo group is still intact within the crystalline host environments. Simple reactivity tests are used to demonstrate whether or not the amorphous host-guest complexes contain the active peroxy acid within their host cavity. Other complementary analytical techniques such as powder X-ray diffraction, differential scanning calorimetry and thermogravimetry have also been used to characterise the newly-hosted peroxyacid materials. By hosting these molecules in microenvironments it is possible to prepare formulations that are less pH sensitive, thus making their storage safer while allowing their reactivity to be controlled and tuned.

Design of the experimental stage for coherent diffraction imaging

2010 ◽  
Vol 1 (SRMS-7) ◽  
Author(s):  
Z. D. Pešić ◽  
U. H. Wagner ◽  
C. Rau
Keyword(s):  
Preliminary Design ◽  
X Ray Diffraction ◽  
Contrast Imaging ◽  
Coherent Imaging ◽  
Full Field ◽  
X Ray ◽  
Coherent Diffraction Imaging ◽  
X Ray Imaging ◽  
Diffraction Imaging ◽  
Experimental Stage

The I13 beamline of Diamond Light Source encompasses two fully independent branches devoted for coherent imaging experiments (coherent X-ray diffraction and ptychography) and X-ray imaging and tomography (full-field microscopy and in-line phase contrast imaging). This contributed paper outlines the main features of the coherence beamline and a preliminary design of the experimental station for coherent X-ray diffraction imaging.

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 Principles of Different X-ray Phase-Contrast Imaging: A Review

2021 ◽  
Vol 11 (7) ◽  
pp. 2971
Author(s):  
Siwei Tao ◽  
Congxiao He ◽  
Xiang Hao ◽  
Cuifang Kuang ◽  
Xu Liu
Keyword(s):  
Biological Samples ◽  
Phase Contrast ◽  
Recent Progress ◽  
Phase Contrast Imaging ◽  
Contrast Imaging ◽  
X Ray ◽  
X Ray Imaging ◽  
Internal Structures ◽  
X Ray Absorption ◽  
Made In

Numerous advances have been made in X-ray technology in recent years. X-ray imaging plays an important role in the nondestructive exploration of the internal structures of objects. However, the contrast of X-ray absorption images remains low, especially for materials with low atomic numbers, such as biological samples. X-ray phase-contrast images have an intrinsically higher contrast than absorption images. In this review, the principles, milestones, and recent progress of X-ray phase-contrast imaging methods are demonstrated. In addition, prospective applications are presented.

scholarly journals Multidimensional Ln-Aminophthalate Photoluminescent Coordination Polymers

Materials ◽  
2021 ◽  
Vol 14 (7) ◽  
pp. 1786
Author(s):  
Carla Queirós ◽  
Chen Sun ◽  
Ana M. G. Silva ◽  
Baltazar de Castro ◽  
Juan Cabanillas-Gonzalez ◽  
...  
Keyword(s):  
Water Content ◽  
Coordination Polymers ◽  
Metal Ion ◽  
Low Cost ◽  
Microwave Assisted Synthesis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Wide Range ◽  
Ft Ir ◽  
Ft Ir Spectroscopy

The development of straightforward reproducible methods for the preparation of new photoluminescent coordination polymers (CPs) is an important goal in luminescence and chemical sensing fields. Isophthalic acid derivatives have been reported for a wide range of applications, and in addition to their relatively low cost, have encouraged its use in the preparation of novel lanthanide-based coordination polymers (LnCPs). Considering that the photoluminescent properties of these CPs are highly dependent on the existence of water molecules in the crystal structure, our research efforts are now focused on the preparation of CP with the lowest water content possible, while considering a green chemistry approach. One- and two-dimensional (1D and 2D) LnCPs were prepared from 5-aminoisophthalic acid and Sm3+/Tb3+ using hydrothermal and/or microwave-assisted synthesis. The unprecedented LnCPs were characterized by single-crystal X-ray diffraction (SCRXD), powder X-ray diffraction (PXRD), Fourier transform infrared (FT-IR) spectroscopy and scanning electron microscopy (SEM), and their photoluminescence (PL) properties were studied in the solid state, at room temperature, using the CPs as powders and encapsulated in poly(methyl methacrylate (PMMA) films, envisaging the potential preparation of devices for sensing. The materials revealed interesting PL properties that depend on the dimensionality, metal ion, co-ligand used and water content.

scholarly journals X-ray imaging of silicon die within fully packaged semiconductor devices

2021 ◽  
pp. 1-7
Author(s):  
Brian K. Tanner ◽  
Patrick J. McNally ◽  
Andreas N. Danilewsky
Keyword(s):  
Synchrotron Radiation ◽  
Feasibility Studies ◽  
Monochromatic Radiation ◽  
X Ray Diffraction ◽  
Divergent Beam ◽  
X Ray ◽  
X Ray Imaging ◽  
Setting Process ◽  
Diffraction Imaging ◽  
Lattice Planes

X-ray diffraction imaging (XRDI) (topography) measurements of silicon die warpage within fully packaged commercial quad-flat no-lead devices are described. Using synchrotron radiation, it has been shown that the tilt of the lattice planes in the Analog Devices AD9253 die initially falls, but after 100 °C, it rises again. The twist across the die wafer falls linearly with an increase in temperature. At 200 °C, the tilt varies approximately linearly with position, that is, displacement varies quadratically along the die. The warpage is approximately reversible on cooling, suggesting that it has a simple paraboloidal form prior to encapsulation; the complex tilt and twisting result from the polymer setting process. Feasibility studies are reported, which demonstrate that a divergent beam and quasi-monochromatic radiation from a sealed X-ray tube can be used to perform warpage measurements by XRDI in the laboratory. Existing tools have limitations because of the geometry of the X-ray optics, resulting in applicability only to simple warpage structures. The necessary modifications required for use in situations of complex warpage, for example, in multiple die interconnected packages are specified.

scholarly journals Analytical study of Buddha sculptures in Jingyin temple of Taiyuan, China

2021 ◽  
Vol 9 (1) ◽  
Author(s):  
Xiaojian Bai ◽  
Chen Jia ◽  
Zhigen Chen ◽  
Yuxuan Gong ◽  
Huwei Cheng ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Scanning Electron Microscopy ◽  
Analytical Study ◽  
Energy Dispersive Spectrometry ◽  
Analytical Techniques ◽  
X Ray Diffraction ◽  
Ancient China ◽  
X Ray ◽  
Unique Style ◽  
Scanning Electron

AbstractWith exquisite design and unique style, the painted sculptures of Tutang Buddha and two attendants Buddha in Jingyin Temple are precious cultural heritages of China. The sculpture of Tutang Buddha, which was carved from a mound and painted by ancient craftsmen, was rarely found in ancient China. However, due to natural and human factors, the sculptures were severely damaged. Obviously, they require urgent and appropriate protection and restoration. In this study, samples taken from the sculptures were analysed through multiple analytical techniques, including scanning electron microscopy with energy dispersive spectrometry (SEM–EDS), Raman spectroscopy, X-ray diffraction (XRD), optical microscopy (OM) and granulometry. The analysis results enable us to infer the techniques used by the craftsmen in making the sculptures and provide a reliable evidence for the conservation and future protection of these and similar sculptures.

2D X-ray diffraction and molecular modelling of the crystalline structure of polyesters under uniaxial stress

2021 ◽  
pp. 096739112199822
Author(s):  
Ahmed I Abou-Kandil ◽  
Gerhard Goldbeck
Keyword(s):  
Crystalline Structure ◽  
Molecular Modelling ◽  
Three Dimensional ◽  
Uniaxial Stress ◽  
X Ray Diffraction ◽  
X Ray ◽  
Wide Range ◽  
Modelling Techniques ◽  
Diffraction Patterns

Studying the crystalline structure of uniaxially and biaxially drawn polyesters is of great importance due to their wide range of applications. In this study, we shed some light on the behaviour of PET and PEN under uniaxial stress using experimental and molecular modelling techniques. Comparing experiment with modelling provides insights into polymer crystallisation with extended chains. Experimental x-ray diffraction patterns are reproduced by means of models of chains sliding along the c-axis leading to some loss of three-dimensional order, i.e. moving away from the condition of perfect register of the fully extended chains in triclinic crystals of both PET and PEN. This will help us understand the mechanism of polymer crystallisation under uniaxial stress and the appearance of mesophases in some cases as discussed herein.

X-ray imaging with ultra-small-angle X-ray scattering as a contrast mechanism

2004 ◽  
Vol 37 (5) ◽  
pp. 757-765 ◽  
Author(s):  
L. E. Levine ◽  
G. G. Long
Keyword(s):  
Small Angle ◽  
Imaging Technique ◽  
Three Dimensional ◽  
Sample Volume ◽  
Contrast Imaging ◽  
X Ray ◽  
X Ray Scattering ◽  
X Ray Imaging ◽  
Contrast Mechanism ◽  
Ray Scattering

A new transmission X-ray imaging technique using ultra-small-angle X-ray scattering (USAXS) as a contrast mechanism is described. USAXS imaging can sometimes provide contrast in cases where radiography and phase-contrast imaging are unsuccessful. Images produced at different scattering vectors highlight different microstructural features within the same sample volume. When used in conjunction with USAXS scans, USAXS imaging provides substantial quantitative and qualitative three-dimensional information on the sizes, shapes and spatial arrangements of the scattering objects. The imaging technique is demonstrated on metal and biological samples.

scholarly journals Assay and physicochemical characterization of the antiparasitic albendazole

2012 ◽  
Vol 48 (2) ◽  
pp. 281-290 ◽  
Author(s):  
Noely Camila Tavares Cavalcanti ◽  
Giovana Damasceno Sousa ◽  
Maria Alice Maciel Tabosa ◽  
José Lamartine Soares Sobrinho ◽  
Leila Bastos Leal ◽  
...  
Keyword(s):  
Physicochemical Characterization ◽  
Analytical Techniques ◽  
Assay Method ◽  
Active Pharmaceutical Ingredients ◽  
X Ray Diffraction ◽  
Melting Points ◽  
X Ray ◽  
Pharmaceutical Ingredients ◽  
Complementary Techniques

The aim of this study was to characterize three batches of albendazole by pharmacopeial and complementary analytical techniques in order to establish more detailed specifications for the development of pharmaceutical forms. The ABZ01, ABZ02, and ABZ03 batches had melting points of 208 ºC, 208 ºC, and 209 ºC, respectively. X-ray diffraction revealed that all three batches showed crystalline behavior and the absence of polymorphism. Scanning electron microscopy showed that all the samples were crystals of different sizes with a strong tendency to aggregate. The samples were insoluble in water (5.07, 4.27, and 4.52 mg mL-1, respectively) and very slightly soluble in 0.1 M HCl (55.10, 56.90, and 61.70 mg mL-1, respectively) and additionally showed purities within the range specified by the Brazilian Pharmacopoeia 5th edition (F. Bras. V; 98% to 102%). The pharmacopeial assay method was not reproducible and some changes were necessary. The method was validated and showed to be selective, specific, linear, robust, precise, and accurate. From this characterization, we concluded that pharmacopeial techniques alone are not able to detect subtle differences in active pharmaceutical ingredients; therefore, the use of other complementary techniques is required to ensure strict quality control in the pharmaceutical industry.

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