scholarly journals Development of a novel microfluidic device to study metal geochemistry in situ using X-ray fluorescence microprobe spectroscopy

2021 ◽  
Vol 28 (2) ◽  
pp. 461-471
Author(s):  
Michael A. Chen ◽  
Benjamin D. Kocar
Keyword(s):  
Microfluidic Device ◽  
Microfluidic System ◽  
X Rays ◽  
Thin Glass ◽  
X Ray ◽  
Wide Range ◽  
Etched Silicon ◽  
Materials Used ◽  
Energy Mapping

The study of in situ microscale biogeochemical processes represents a major challenge in the environmental sciences. The combination of microfluidic devices with X-ray fluorescence microprobe spectroscopy may address this need, but typical materials used in these devices attenuate the X-rays needed to analyze key elements of interest, such as Fe or As. In this work, a method is presented for fabricating an etched silicon microfluidic device that is sealed with a 30 µm thin glass window that is sufficiently transparent for X-ray fluorescence microprobe spectroscopy. The capabilities of these devices for X-ray microprobe spectroscopy are demonstrated using an Fe (hydr)oxide solid that is loaded with As and then infused with sulfide, on beamline 4-BM at NSLS-II, resulting in time-variant Fe precipitation reactions and As sorption. Key results include in situ X-ray fluorescence time-series maps of Fe, As and a Br flow tracer, as well as spot XANES at both the Fe K edge and As K edge. Additionally, multiple energy mapping is used to examine the spatial speciation of As over time. The results of this work clearly demonstrate the capabilities of this novel microfluidic system that can be analyzed using X-ray fluorescence microprobe spectroscopy and can be made to study a wide range of complex microscale geochemical systems.

scholarly journals Photoreduction and validation of haem–ligand intermediate states in protein crystals byin situsingle-crystal spectroscopy and diffraction

IUCrJ ◽  
2017 ◽  
Vol 4 (3) ◽  
pp. 263-270 ◽  
Author(s):  
Demet Kekilli ◽  
Tadeo Moreno-Chicano ◽  
Amanda K. Chaplin ◽  
Sam Horrell ◽  
Florian S. N. Dworkowski ◽  
...  
Keyword(s):  
Crystal Structures ◽  
Structural Data ◽  
X Rays ◽  
Solvated Electrons ◽  
X Ray ◽  
Redox States ◽  
Density Maps ◽  
Correct Assignment ◽  
Wide Range

Powerful synergies are available from the combination of multiple methods to study proteins in the crystalline form. Spectroscopies which probe the same region of the crystal from which X-ray crystal structures are determined can give insights into redox, ligand and spin states to complement the information gained from the electron-density maps. The correct assignment of crystal structures to the correct protein redox and ligand states is essential to avoid the misinterpretation of structural data. This is a particular concern for haem proteins, which can occupy a wide range of redox states and are exquisitely sensitive to becoming reduced by solvated electrons generated from interactions of X-rays with water molecules in the crystal. Here, single-crystal spectroscopic fingerprinting has been applied to investigate the laser photoreduction of ferric haem in cytochromec′. Furthermore,in situX-ray-driven generation of haem intermediates in crystals of the dye-decolourizing-type peroxidase A (DtpA) fromStreptomyces lividansis described.

scholarly journals Development of a sticker sealed microfluidic device for in situ analytical measurements using synchrotron radiation

2021 ◽  
Author(s):  
ITAMAR NECKEL ◽  
Lucas F. de Castro ◽  
Flavia Callefo ◽  
Verônica Teixeira ◽  
Angelo Gobbi ◽  
...  
Keyword(s):  
Microfluidic Device ◽  
Green Energy ◽  
X Rays ◽  
Electrical Measurements ◽  
X Ray ◽  
Electrochemical Nucleation ◽  
Synchrotron Light

Abstract Shedding synchrotron light on microfluidic systems, exploring several contrasts in situ operando at the nanoscale, like X-ray fluorescence, diffraction, luminescence, and absorption, has the potential to reveal new properties and functionalities of materials across diverse areas, such as green energy, photonics, and nanomedicine. In this work, we present the micro-fabrication and characterization of a multifunctional polyester/glass sealed microfluidic device well-suited to combine with analytical X-ray techniques. The device consists of smooth microchannels patterned on glass, where three gold electrodes are deposited into the channels to serve in situ electrochemistry analysis or standard electrical measurements. It has been efficiently sealed through an ultraviolet-sensitive sticker-like layer based on a polyester film, and The burst pressure determined by pumping water through the microchannel(up to 0.22 MPa). Overall, the device has demonstrated exquisite chemical resistance to organic solvents, and its efficiency in the presence of biological samples (proteins) is remarkable. The device potentialities, and its high transparency to X-rays, have been demonstrated by taking advantage of the X-ray nanoprobe Carnaúba/Sirius/LNLS, by obtaining 2D X-ray nanofluorescence maps on the microchannel filled with water and after an electrochemical nucleation reaction. To wrap up, the microfluidic device characterized here has the potential to be employed in standard laboratory experiments as well as in situ and in vivo analytical experiments using a wide electromagnetic window, from infrared to X-rays, which could serve experiments in many branches of science.

Cladding Thickness of Fuel Elements by X-Rays

1958 ◽  
Vol 2 ◽  
pp. 275-281
Author(s):  
Beverley James Lowe ◽  
Payson D. Sierer ◽  
Robert B. Ogilvie
Keyword(s):  
304 Stainless Steel ◽  
X Rays ◽  
X Ray ◽  
Uranium Fuel ◽  
Wide Range ◽  
Materials Used ◽  
Fuel Elements ◽  
Destructive Measurement ◽  
Non Destructive ◽  
Cladding Material

AbstractThe paper is based on a feasibility study to determine the suitability of various techniques for the non-destructive measurement of cladding thickness on uranium fuel elements. The techniques studied were: 1—the attentuation of the characteristic X-ray fluorescence from the uranium base metal by the cladding material, and 2—Compton scattering of X-rays from the cladding surface. The cladding materials used in the investigation were aluminum, 304 stainless steel and zirconium, providing a wide range of both atomic number and density.

scholarly journals Development of a sticker sealed microfluidic device for in situ analytical measurements using synchrotron radiation

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Itamar T. Neckel ◽  
Lucas F. de Castro ◽  
Flavia Callefo ◽  
Verônica C. Teixeira ◽  
Angelo L. Gobbi ◽  
...  
Keyword(s):  
Microfluidic Device ◽  
Green Energy ◽  
X Rays ◽  
Electrical Measurements ◽  
X Ray ◽  
Electrochemical Nucleation ◽  
Synchrotron Light

AbstractShedding synchrotron light on microfluidic systems, exploring several contrasts in situ/operando at the nanoscale, like X-ray fluorescence, diffraction, luminescence, and absorption, has the potential to reveal new properties and functionalities of materials across diverse areas, such as green energy, photonics, and nanomedicine. In this work, we present the micro-fabrication and characterization of a multifunctional polyester/glass sealed microfluidic device well-suited to combine with analytical X-ray techniques. The device consists of smooth microchannels patterned on glass, where three gold electrodes are deposited into the channels to serve in situ electrochemistry analysis or standard electrical measurements. It has been efficiently sealed through an ultraviolet-sensitive sticker-like layer based on a polyester film, and The burst pressure determined by pumping water through the microchannel(up to 0.22 MPa). Overall, the device has demonstrated exquisite chemical resistance to organic solvents, and its efficiency in the presence of biological samples (proteins) is remarkable. The device potentialities, and its high transparency to X-rays, have been demonstrated by taking advantage of the X-ray nanoprobe Carnaúba/Sirius/LNLS, by obtaining 2D X-ray nanofluorescence maps on the microchannel filled with water and after an electrochemical nucleation reaction. To wrap up, the microfluidic device characterized here has the potential to be employed in standard laboratory experiments as well as in in situ and in vivo analytical experiments using a wide electromagnetic window, from infrared to X-rays, which could serve experiments in many branches of science.

In Situ Synchrotron Radiation Research in Materials Science

MRS Bulletin ◽  
1999 ◽  
Vol 24 (1) ◽  
pp. 13-20 ◽  
Author(s):  
Pedro A. Montano ◽  
Hiroyuki Oyanagi
Keyword(s):  
Synchrotron Radiation ◽  
Materials Science ◽  
X Rays ◽  
X Ray ◽  
Curved Trajectories ◽  
Wide Range ◽  
Materials Research ◽  
Novel Processing ◽  
Characterization Of Materials

X-rays have found a wide range of applications in chemistry, physics, and materials engineering since their discovery in 1895 by W. Roentgen. The materials science community uses x-ray-based techniques extensively for characterization of materials. In the 1970s a new tunable source of x-rays from the radiation produced by synchrotron accelerators emerged. Synchrotron radiation (SR) is an intense and forward-focused beam of radiation that is emitted when the path of an electron traveling at almost the speed of light is bent by a magnetic field. Figure 1 illustrates the evolution of radiation intensity provided by various x-ray sources. In situ SR techniques provide real-time observation of atomic arrangements with high spatial sensitivity and precision, which are important features not only in fundamental materials research, but also in the development of novel processing techniques and in the search for new exotic materials. A major advantage of SR is that it covers a wide range of wavelengths continuously from infrared to gamma rays. This feature is attractive since a wealth of detailed information on the electronic and structural properties of materials can be obtained by optimizing the wavelength of the radiation.Since the establishment of “first generation” facilities in the early 1970s, the x-ray emittance from synchrotron storage rings, where electrons traveling at almost relativistic speed s are constrained by magnetic fields to follow curved trajectories, has shown dramatic improvements. See Table I for an extensive list of SR facilities presentiy in use throughout the world.

In Situ Testing and X Rays Radiation Effects of Pt/Bi3.15Nd0.85Ti3O12/Pt Ferroelectric Capacitors

2013 ◽  
Vol 712-715 ◽  
pp. 293-297
Author(s):  
Li Li
Keyword(s):  
Radiation Effects ◽  
Hysteresis Loops ◽  
Electrical Performance ◽  
Hysteresis Curve ◽  
X Rays ◽  
Shanghai Synchrotron Radiation Facility ◽  
X Ray ◽  
In The Beginning ◽  
Ferroelectric Capacitors

Pt/Bi3.15Nd0.85Ti3O12(BNT)/Pt ferroelectric capacitors were monitored using in situ X-ray irradiation with 10 keV at BL14B1 beamline (Shanghai Synchrotron Radiation Facility). BL14B1 combined with a ferroelectric analyzer enabled measurements in situ of electrical performance. The hysteresis curve (PE) of distortion depended on the polarization during irradiation, but the diffracted intensities of the (117) peak did not change in the beginning. ThePEcurve had a negligible change from 2.09×109Gy to 4.45×109Gy. Finally, bothPrandPr+very rapidly increased, but the intensities of (117) decreased. The hysteresis loops were remarkably deformed at the maximum total dose of 4.87×109Gy.

Applications of High-Resolution Powder X-Ray Diffraction

2007 ◽  
Vol 130 ◽  
pp. 7-14 ◽  
Author(s):  
Andrew N. Fitch
Keyword(s):  
High Resolution ◽  
Synchrotron Radiation ◽  
Powder Diffraction ◽  
X Rays ◽  
X Ray Diffraction ◽  
Crystalline Materials ◽  
X Ray ◽  
Structural Characterisation ◽  
Pdf Analysis

The highly-collimated, intense X-rays produced by a synchrotron radiation source can be harnessed to build high-resolution powder diffraction instruments with a wide variety of applications. The general advantages of using synchrotron radiation for powder diffraction are discussed and illustrated with reference to the structural characterisation of crystalline materials, atomic PDF analysis, in-situ and high-throughput studies where the structure is evolving between successive scans, and the measurement of residual strain in engineering components.

scholarly journals The XXL Survey

2018 ◽  
Vol 620 ◽  
pp. A18 ◽  
Author(s):  
C. H. A. Logan ◽  
B. J. Maughan ◽  
M. N. Bremer ◽  
P. Giles ◽  
M. Birkinshaw ◽  
...  
Keyword(s):  
Angular Resolution ◽  
False Positive Rate ◽  
High Sensitivity ◽  
Point Sources ◽  
Selection Function ◽  
X Rays ◽  
Cluster Emission ◽  
X Ray ◽  
Wide Range ◽  
Function Modelling

Context. The XMM-XXL survey has used observations from the XMM-Newton observatory to detect clusters of galaxies over a wide range in mass and redshift. The moderate PSF (FWHM ~ 6″ on-axis) of XMM-Newton means that point sources within or projected onto a cluster may not be separated from the cluster emission, leading to enhanced luminosities and affecting the selection function of the cluster survey. Aims. We present the results of short Chandra observations of 21 galaxy clusters and cluster candidates at redshifts z > 1 detected in the XMM-XXL survey in X-rays or selected in the optical and infra-red. Methods. With the superior angular resolution of Chandra, we investigate whether there are any point sources within the cluster region that were not detected by the XMM-XXL analysis pipeline, and whether any point sources were misclassified as distant clusters. Results. Of the 14 X-ray selected clusters, 9 are free from significant point source contamination, either having no previously unresolved sources detected by Chandra or with less than about 10% of the reported XXL cluster flux being resolved into point sources. Of the other five sources, one is significantly contaminated by previously unresolved AGN, and four appear to be AGN misclassified as clusters. All but one of these cases are in the subset of less secure X-ray selected cluster detections and the false positive rate is consistent with that expected from the XXL selection function modelling. We also considered a further seven optically selected cluster candidates associated with faint XXL sources that were not classed as clusters. Of these, three were shown to be AGN by Chandra, one is a cluster whose XXL survey flux was highly contaminated by unresolved AGN, while three appear to be uncontaminated clusters. By decontaminating and vetting these distant clusters, we provide a pure sample of clusters at redshift z > 1 for deeper follow-up observations, and demonstrate the utility of using Chandra snapshots to test for AGN in surveys with high sensitivity but poor angular resolution.

A multi-length-scale USAXS/SAXS facility: 10–50 keV small-angle X-ray scattering instrument

2013 ◽  
Vol 46 (5) ◽  
pp. 1508-1512 ◽  
Author(s):  
Byron Freelon ◽  
Kamlesh Suthar ◽  
Jan Ilavsky
Keyword(s):  
Small Angle ◽  
Soft Matter ◽  
High Energy ◽  
X Rays ◽  
X Ray ◽  
X Ray Scattering ◽  
Wide Range ◽  
And Performance ◽  
New Facility ◽  
Ray Scattering

Coupling small-angle X-ray scattering (SAXS) and ultra-small-angle X-ray scattering (USAXS) provides a powerful system of techniques for determining the structural organization of nanostructured materials that exhibit a wide range of characteristic length scales. A new facility that combines high-energy (HE) SAXS and USAXS has been developed at the Advanced Photon Source (APS). The application of X-rays across a range of energies, from 10 to 50 keV, offers opportunities to probe structural behavior at the nano- and microscale. An X-ray setup that can characterize both soft matter or hard matter and high-Zsamples in the solid or solution forms is described. Recent upgrades to the Sector 15ID beamline allow an extension of the X-ray energy range and improved beam intensity. The function and performance of the dedicated USAXS/HE-SAXS ChemMatCARS-APS facility is described.

scholarly journals In situ damage assessment using synchrotron X-rays in materials loaded by a Hopkinson bar

2014 ◽  
Vol 372 (2015) ◽  
pp. 20130191 ◽  
Author(s):  
Weinong W. Chen ◽  
Matthew C. Hudspeth ◽  
Ben Claus ◽  
Niranjan D. Parab ◽  
John T. Black ◽  
...  
Keyword(s):  
High Speed ◽  
Particle Interaction ◽  
Tensile Failure ◽  
High Rate ◽  
X Rays ◽  
Contrast Imaging ◽  
X Ray ◽  
Damage Initiation ◽  
Dynamic Experiments

Split Hopkinson or Kolsky bars are common high-rate characterization tools for dynamic mechanical behaviour of materials. Stress–strain responses averaged over specimen volume are obtained as a function of strain rate. Specimen deformation histories can be monitored by high-speed imaging on the surface. It has not been possible to track the damage initiation and evolution during the dynamic deformation inside specimens except for a few transparent materials. In this study, we integrated Hopkinson compression/tension bars with high-speed X-ray imaging capabilities. The damage history in a dynamically deforming specimen was monitored in situ using synchrotron radiation via X-ray phase contrast imaging. The effectiveness of the novel union between these two powerful techniques, which opens a new angle for data acquisition in dynamic experiments, is demonstrated by a series of dynamic experiments on a variety of material systems, including particle interaction in granular materials, glass impact cracking, single crystal silicon tensile failure and ligament–bone junction damage.

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