Operando measurement of lattice deformation profiles of synchrotron radiation monochromator

This study presents a new method for characterizing the thermal lattice deformation of a monochromator with high precision under service conditions and first reports the operando measurements of nanoscale thermal lattice deformation on a double-crystal monochromator at different incident powers.The nanoscale thermal lattice deformation of the monochromator first crystal was obtained by analyzing the intensity of the distorted DuMond diagrams.DuMond diagrams of the 333 diffraction index,sensitive to lattice deformation,were obtained directly using a 2D detector and an analyzer crystal orthogonal to the monochromator.With increasing incident power and power density,the maximum height of the lattice deformation increased from 3.2 to 18.5 nm,and the deformation coefficient of the maximum height increased from 1.1 to 3.2 nm/W.The maximum relative standard deviation was 4.2%,and the maximum standard deviation was 0.1 nm.Based on the measured thermal deformations,the flux saturation phenomenon and critical point for the linear operation of the monochromator were predicted with increasing incident power.This study provides a simple solution to the problem of the lower precision of synchrotron radiation monochromator characterizations compared to simulations.

Small-angle X-ray scattering investigation of aging behavior of Al-Cu-Mg-Ag alloys using synchrotron radiation

The aging behavior of Al-Cu-Mg-Ag alloys with high Cu/Mg was studied by transmission electron microscopy (TEM) and small-angle X-ray scattering (SAXS) using synchrotron radiation. TEM study reveals that the major strengthening phases of the alloy after aging at 160?C for 10 h are Ω and less θ′. SAXS study shows that the scattering patterns are composed of several concentric circles at the beginning of aging process, which is replaced by the butterfly-wings scattering patterns with the increase of aging time. The butterfly-wings scattering patterns are composed of several branches. The angles between the branches are roughly equal to that between the habit planes of precipitates. The evolution of Guinier radius with aging time indicates the good coarsening resistance of the precipitates. The evolution of integrated intensity is consistent with the classical two-step precipitation process.

Polycapillary X-ray lens for the secondary focusing Beijing synchrotron radiation source

According to intensity distribution of the synchrotron radiation source focused by a toroidal mirror at the Beijing synchrotron radiation biological macromolecule station, theoretical modeling of the Beijing synchrotron radiation source is developed for capillary optics. Using this theoretical modeling, the influences of the configuration curve of the polycapillary X-ray lens on transmission efficiency and working distance are analyzed. The experimental results of the transmission efficiency and working distance at the biological macromolecule station are in good agreement with the theoretical results.

Internal Structure of Cambrian Fossil Embryo Markuelia Revealed in the Light of Synchrotron Radiation X-ray Tomographic Microscopy

In the light of Synchrotron Radiation X-ray Tomographic Microscopy （SRXTM）, the internal structure of Markuelia hunanensis is revealed. In one example, vitrification and peeling show the annuli hidden under the chorion. Sectioning and 3-D reconstruction display an intact digestive tract from the inverted introvert to the terminal anus. The inverted introvert forms a rugby cavum. The following digestive tract is rope-like coiling, parallel to the body axis, about 650 μm in length, and uniform in diameter （-80 μm）. An exquisitely preserved pipe-like structure is hidden in the middle of the rope-like structure, diameter 20--40 lam, with a length of -120 μm. We interpret this pipe-like structure as the possible epidermis of the gut and its surroundings as the possible residue of musculature, similar to that in Priapulans. The two symmetrical rod-shape structures connecting the body wall and digestive tract are interpreted as the possible retractor muscles. After comparing the well preserved Left-form and Right-form Body of Markuelia, we suggest that they may represent a dimorphism. Counted directly, one sample of Markuelia hunanensis possesses 62 annulations and the other 68.

Three dimensional distribution of surfactant in microspheres revealed by synchrotron radiation X-ray microcomputed tomography

This study investigated the formulation mechanism of microspheres via internal surfactant distribution. Eudragit L100 based microspheres loaded with bovine serum albumin were prepared by solid in oil in oil emulsion solvent evaporation method using acetone and liquid paraffin system containing sucrose stearate as a surfactant. The fabricated microspheres were evaluated for encapsulation efficiency, particle size, production yield, and in vitro release characteristics. The internal structures of microspheres were characterized using synchrotron radiation X-ray microcomputed tomography(SR-μCT). The enhanced contrast made the sucrose stearate distinguished from Eudragit to have its three dimensional(3D) distribution. Results indicated that the content and concentration determined the state of sucrose stearate and had significant influences on the release kinetics of protein. The dispersity of sucrose stearate was the primary factor that controlled the structure of the microspheres and further affected the encapsulation efficiency, effective drug loading, as well as in vitro release behavior. In conclusion, the 3D internal distribution of surfactant in microspheres and its effects on protein release behaviors have been revealed for the first time. The highly resolved 3D architecture provides new evidence for the deep understanding of the microsphere formation mechanism.

High pressure x-ray diffraction techniques with synchrotron radiation

This article summarizes the developments of experimental techniques for high pressure x-ray diffraction（XRD） in diamond anvil cells（DACs） using synchrotron radiation. Basic principles and experimental methods for various diffraction geometry are described, including powder diffraction, single crystal diffraction, radial diffraction, as well as coupling with laser heating system. Resolution in d-spacing of different diffraction modes is discussed. More recent progress, such as extended application of single crystal diffraction for measurements of multigrain and electron density distribution, timeresolved diffraction with dynamic DAC and development of modulated heating techniques are briefly introduced. The current status of the high pressure beamline at BSRF（Beijing Synchrotron Radiation Facility） and some results are also presented.

The Study Internal Structure of the Annual Layers in Lake Sediments Using Synchrotron Radiation with X-ray Focusing Optics

1 Introduction Annually laminated(varve)sedimentary deposits are considered as one of the most important archives,since they offer precise temporal information(years)in combination with high time resolutions.Bottom sediments of the lakes contain detailed geochemical information on

L-shell x-ray fluorescence relative intensities for elements with 62≤Z≤83 at 18 keV and 23 keV by synchrotron radiation

The relative intensities of L-subshell x-ray fluorescence(XRF)for elements with atomic numbers 62≤Z≤83 were measured at two excitation energies,18 keV and 23 keV,using a synchrotron radiation source at a beamline of the Synchrotron Light Center for Experimental Science and Applications in the Middle East(SESAME),Jordan.The experimentally measured results of the relative intensities were compared with the calculated results using the subshell fluorescence yield and the Coster-Kronig transition probabilities recommended by Campbell and the values based on the Dirac-Hartree-Slater model by Puri.The experimental and theoretical results are in agreement.In this work,L XRF relative intensities for the elements Sm,Gd,Tb,Er,Ta,W,Re,Hg,Pb and Bi at energies of 18 keV and 23 keV were measured.

Investigation of the topological shape of bovine serum albumin in solution by small-angle x-ray scattering at Beijing synchrotron radiation facility

This paper reports that at a newly constructed small-angle x-ray scattering station of Beijing Synchrotron Radia- tion Facility, the topological shape of ligand-free bovine serum albumin in solution has been investigated. An appropriate scattering curve is obtained and the calculated value of the gyration radius is 31.2~=t=0.25 ~_ （11=0.1 nm） which is co- incident with other ones＇ results. It finds that the low-resolution structure models obtained by making use of ab initio reconstruction methods are fitting the crystal structure of human serum albumin very well. All of these results perform the potential of the beamline to apply to structural biology studies. The characteristics, the defects, and the improving measures of the station in future are also discussed.

Hard X-ray in-line outline imaging for blood vessels:first generation synchrotron radiation without contrast agents in vitro

Objective: Phase-contrast X-ray imaging which reduces radiation exposure, is a promising technique for observing the inner structures of biological soft tissues without the aid of contrast agents. The present study intends to depict blood vessels of rabbits and human livers with hard X-ray in-line outline imaging without contrast agents using synchrotron radiation. Methods: All samples were fixed with formalin and sliced into 6 mm sections. The imaging experiments were performed with Fuji-IX80 films on the 4W1A light beam of the first generation synchrotron radiation in Beijing, China. The device of the experiment, which supplies a maximum light spot size of 20×10 mm was similar to that of in-line holography. The photon energy was set at 8 KeV and high quality imagines were obtained by altering the distance between the sample and the film. Results: The trees of rabbit-liver blood vessels and the curved vessels of the cirrhotic human liver were revealed on the images, where vessels < 20 μm in diameter were differentiated. Conclusion: These results show that the blood vessels of liver samples can be revealed by using hard X-ray in-line outline imaging with the first generation synchrotron radiation without contrast agents.

Focusing high-energy x-rays by a P MMA compound x-ray lens on Beijing synchrotron radiation facility

The x-ray compound lens is a novel refractive x-ray optical device. This paper reports the authors＇ recent research on a polymethyl methacrylate （PMMA） compound x-ray lens. Firstly the designing and LIGA fabrication process for the PMMA compound x-ray lens are briefly described. Then, a method for theoretical analysis, as well as the experimental system for measurement is also introduced. Finally, the focusing spots for 8keV monochromatic x-rays by the PMMA compound x-ray lens are measured and analysed. According to the experimental results, it is concluded that the PMMA compound x-ray lens promises a good focusing performance under the high-energy x-rays.

The Significance of Solutions Obtained from Ill-Posed Systems of Linear Equations Constituted by Synchrotron Radiation Based Anomalous Small-Angle X-Ray Scattering

Synchrotron radiation based experimental techniques known as Anomalous Small-Angle X-ray Scattering (ASAXS) provide deep insight into the nanostructure of uncountable material systems in condensed matter research i.e. solid state physics, chemistry, engineering and life sciences thereby rendering the origin of the macroscopic functionalization of the various materials via correlation to its structural architecture on a nanometer length scale. The techniques constitute a system of linear equations, which can be treated by matrix theory. The study aims to analyze the significance of the solutions of the stated matrix equations by use of the so-called condition numbers first introduced by A. Turing, J. von Neumann and H. Goldstine. Special attention was given for the comparison with direct methods i.e. the Gaussian elimination method. The mathematical roots of ill-posed ASAXS equations preventing matrix inversion have been identified. In the framework of the theory of von Neumann and Goldstine the inversion of certain matrices constituted by ASAXS gradually becomes impossible caused by non-definiteness. In Turing’s theory which starts from more general prerequisites, the principal minors of the same matrices approach singularity thereby imposing large errors on inversion. In conclusion both theories recommend for extremely ill-posed ASAXS problems avoiding inversion and the use of direct methods for instance Gaussian elimination.

Characterization of metal element distributions in the rat brain following ischemic stroke by synchrotron radiation microfluorescence analysis

Ischemic stroke is one of the leading causes of death worldwide,and effective treatment strategies in the chronic phase of this disease remain insufficient.Homeostasis of metals in the brain plays an important role in maintaining normal brain function.However,the dynamic spatial distributions of iron,zinc,calcium,potassium,and copper in a rat brain following ischemic stroke and the association between structural distribution and function remain to be elucidated.In this study,we used a synchrotron radiation-based micro-X-ray fluorescence technique to image element mapping changes in special rat brain regions after ischemic stroke,showing the distribution characteristics of iron,zinc,calcium,potassium,and copper.We demonstrated,for the first time,the consistent dynamic spatial distributions of metal elements at a series of time points(3 h,4.5 h,6 h,12 h,1 d,3 d,5 d,7 d,10 d,14 d,28 d)after brain ischemia,which revealed that the homeostasis of iron,zinc,calcium,potassium,and copper in the brain was disturbed with distinctive change trends,providing clear insights in understanding the underlying pathogenesis of stroke from a novel perspective,thus laying the foundation of further developing new drug targets for stroke treatment.

Scan system for arbitrary-shaped samples at the synchrotron radiation facility

X-ray fluorescence(XRF) scan methodology is important for elemental mapping of samples at a synchrotron radiation facility. To save the experiment time and improve the experiment efficiency, one should develop an efficient XRF scan method. In this paper, a new scan mode is presented. It can map arbitrary-shaped areas withou stopping the motors. The control and data acquisition system integrates motor controlling, detector triggering, and data acquisition and storage. The system realizes the arbitrary-shaped 2D-mapping and fluorescence data acquisition synchronously. SR-XRF mapping has been performed with a standard gold mask to verify the validity of this method a beamline BL15U1 of the Shanghai Synchrotron Radiation Facility. The results show that this method reduces the tota scan time and improves the experiment efficiency.

Scanning Analysis of REE in Bastnaesite with Synchrotron Radiation X－Ray Fluorescence Microprobe

The content of REE(La.Ce.Pr.Nd.Sm) in bastnaesite was measured by synchrotron radiation X-ray fluorescence microprobe.Scanning analysis makes use of excitation of the REE K lines between 33 and 50 keV.SR white beam from a Wiggler source at the Beijing Electron Positron Collider(BEPC) of the National Laboratory,in order to excite the REE.The bastnaesite from the same mineral area was powdered to particle size≤300 mesh.It was then divided into two parts.One portion was used to be determined by XRF after depositing with oxalate and transforming into oxide.The other was pressed into disk without any binder as the reference sample.The weight and the diamieter of the disk were 15 g and 26 mm respectively.

Biological effects of synchrotron radiation on crops

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Development of a soft X-ray microprobe for single cell radiobiology

An X-ray microprobe for radiobiological studies was developed which deliver precise doses of radiation to the selected individual cells.The facility used synchrotron radiation as soft X-ray source.A zone plate combining with a pinhole produced a fine probe from bending magnet for single cell irradiating with defined doses.The diameter of microprobe at the target position was about 2 μm by scanning a knife-edge with an AXUV photo diode.The fluxes of soft X-rays at 516.7 eV(2.4 nm) were about 5.4×104 photons/s.100mA measured with the photo diode.The absorbed dose rate for typical yeast cells was about 11.34 Gy/s with the storage current of 100 mA.A preliminary experiment for yeast cells irradiation has shown that the microprobe had a definite biological effect for radiobiological investigations.The soft X-ray microprobe at "water window" region has provided a useful tool for single cell irradiating damage and a capability of individually irradiating a certain numbers of cells each time.

Performance of the merged APPLE-Knot undulator for soft x-ray beamline in medium energy ring

APPLE-Knot undulator can effectively solve the on-axis heat load problem and is proven to perform well in VUV beamline and soft x-ray beamline in high energy storage ring. However, for soft x-ray beamline in a medium energy ring,whether the APPLE-Knot undulator excels the APPLE undulator is still a question. Here, a merged APPLE-Knot undulator is studied to generate soft x-ray in a medium energy ring. Its advantages and problems are discussed. Though the on-axis heat load of the APPLE-Knot undulator is lower in linear polarization modes compared to the APPLE undulator, its flux is lower. The APPLE-Knot undulator shows no advantage when only fundamental harmonic is needed. However, in circular polarization mode, the APPLE-Knot undulator shows the ability to cover a broader energy range which can remedy the notable shortcoming of the APPLE undulator.

Small Angle X-Ray Scattering Imaging of Soft Tissue by Using Laue Diffraction Optical System

We performed a feasibility study of Small angle X-ray scattering imaging under the condition of X-ray bright field imaging by Laue crystal diffraction optics of X-ray dark-field imaging that works as an angular analysis. Collagen in chicken tibia containing abundant soft fibrous tissue was chosen as a specimen. In traditional Small angle X-ray scattering optical system, we can derive the structure information of sample by calculating q value which is available from a scattering pattern. Thus it is usually necessary to conduct a 2D scan in order to obtain scattering image. In this paper it is described by a method by which not only small angle X-ray scattering imaging is available directly but also bright-field imaging and dark-field imaging can be obtained at the same time. As the first step, the feasibility of the imaging method should be confirmed by taking pictures of the samples with known periodic length. The preliminary test showed that the collgan’s lattice spacing d is 65.1 nm that was also taken photos by scanning electron microscopy. By rotating Laue angular analyzer by 112 arcseconds small angle X-ray scattering image appeared in bright-field.

Multilayer polarization elements and their applications to polarimetric studies in vacuum ultraviolet and soft X-ray regions

Multilayer polarization elements and their applications to polarimetric studies in 20～400 eV region are mainly reviewed. General principle of selecting material combinations to get high linear polarizance multilayers of reflection type is given with practical examples,with periodic or non-periodic layer structures depending on the usage. Transmission type is introduced as linear polarizer and phase shifter. Their applications include polarization diagnosis of laboratory optical systems and synchrotron radiation beamlines of linear and circular polarization,magnetic rotation experiments such as Faraday rotation and magnetic Kerr rotation on magnetic films and multilayers,and ellipsometry to measure optical constants of thin films precisely. Polarization analysis of soft X-ray fluorescence using multilayer-coated grating is also mentioned. Finally this review is summarized with outlook of further developments.