Optimized IR synchrotron beamline design

Synchrotron infrared beamlines are powerful tools on which to perform spectroscopy on microscopic length scales but require working with large bending‐magnet source apertures in order to provide intense photon beams to the experiments. Many infrared beamlines use a single toroidal‐shaped mirror to focus the source emission which generates, for large apertures, beams with significant geometrical aberrations resulting from the shape of the source and the beamline optics. In this paper, an optical layout optimized for synchrotron infrared beamlines, that removes almost totally the geometrical aberrations of the source, is presented and analyzed. This layout is already operational on the IR beamline of the Brazilian synchrotron. An infrared beamline design based on a SOLEIL bending‐magnet source is given as an example, which could be useful for future IR beamline improvements at this facility.     

SOLEIL shining on the solution‐state structure of biomacromolecules by synchrotron X‐ray footprinting at the Metrology beamline

Synchrotron X‐ray footprinting complements the techniques commonly used to define the structure of molecules such as crystallography, small‐angle X‐ray scattering and nuclear magnetic resonance. It is remarkably useful in probing the structure and interactions of proteins with lipids, nucleic acids or with other proteins in solution, often better reflecting the in vivo state dynamics. To date, most X‐ray footprinting studies have been carried out at the National Synchrotron Light Source, USA, and at the European Synchrotron Radiation Facility in Grenoble, France. This work presents X‐ray footprinting of biomolecules performed for the first time at the X‐ray Metrology beamline at the SOLEIL synchrotron radiation source. The installation at this beamline of a stopped‐flow apparatus for sample delivery, an irradiation capillary and an automatic sample collector enabled the X‐ray footprinting study of the structure of the soluble protein factor H (FH) from the human complement system as well as of the lipid‐associated hydrophobic protein S3 oleosin from plant seed. Mass spectrometry analysis showed that the structural integrity of both proteins was not affected by the short exposition to the oxygen radicals produced during the irradiation. Irradiated molecules were subsequently analysed using high‐resolution mass spectrometry to identify and locate oxidized amino acids. Moreover, the analyses of FH in its free state and in complex with complement C3b protein have allowed us to create a map of reactive solvent‐exposed residues on the surface of FH and to observe the changes in oxidation of FH residues upon C3b binding. Studies of the solvent accessibility of the S3 oleosin show that X‐ray footprinting offers also a unique approach to studying the structure of proteins embedded within membranes or lipid bodies. All the biomolecular applications reported herein demonstrate that the Metrology beamline at SOLEIL can be successfully used for synchrotron X‐ray footprinting of biomolecules.     

Distribution of Pb and Zn in slices of human bone by synchrotron µ‐XRF

Synchrotron radiation‐induced micro x‐ray fluorescence analysis (µ‐XRF) at HASYLAB beamline L was used to determine the distribution of Pb and other trace elements in slices of human bone. Using a focused synchrotron x‐ray beam of about 15 µm in diameter it was found that Pb was mostly located at the outer border of the cortical bone in various samples. Ratios of Pb intensities of cortical and trabecular bone varied from 0.027 for hip head to 0.408 for proximal tibia. Additionally Ca, Zn and Sr distributions were simultaneously recorded. A remarkable association between Pb and Zn content could be observed. Copyright © 2004 John Wiley & Sons, Ltd.     

In situ multi‐axial loading frame to probe elastomers using X‐ray scattering

An in situ tensile–shear loading device has been designed to study elastomer crystallization using synchrotron X‐ray scattering at the Synchrotron Soleil on the DiffAbs beamline. Elastomer tape specimens of thickness 2 mm can be elongated by up to 500% in the longitudinal direction and sheared by up to 200% in the transverse direction. The device is fully automated and plugged into the TANGO control system of the beamline allowing synchronization between acquisition and loading sequences. Experimental results revealing the evolution of crystallization peaks under load are presented for several tension/shear loading sequences.     

Development of an experimental set‐up for low‐temperature spectroscopic studies of matrix‐isolated molecules and molecular ices using synchrotron radiation

An experimental set‐up for studying photophysics and photochemistry of molecules in an inert gas medium (matrix‐isolated) and in the ice phase at low temperatures has been developed and commissioned at the Photophysics beamline, Indus‐1 synchrotron radiation source. This end‐station uses an in‐house‐developed closed‐cycle cryostat for achieving cryo‐temperatures (～10 K). Synchrotron radiation from the Photophysics beamline is used as the source of UV–VUV photons and the system is equipped with a Fourier transform infrared spectrometer for characterization of the molecular species formed at low temperature. Various individual components of the end‐station like closed‐cycle cryostat, experimental chamber, gas mixing and deposition systems are tested to ascertain that the desired performance criteria are satisfied. The performance of the composite system after integration with the Photophysics beamline is evaluated by recording IR and UV–VUV photoabsorption spectra of sulfur dioxide at low temperatures (10 K), both in the ice phase as well as isolated in argon matrices. Results obtained are in good agreement with earlier literature, thus validating the satisfactory performance of the system. As an off‐shoot of the study, the VUV absorption spectrum of matrix‐isolated SO₂ in argon matrix up to 10.2 eV is reported here for the first time. This experimental end‐station will provide new opportunities to study photon‐induced reactions in molecules of environmental, astrochemical and industrial importance. Details of the design, development and initial experimental results obtained are presented.     

High‐performance X‐ray detectors for the new powder diffraction beamline I11 at Diamond

The design and performance characterization of a new light‐weight and compact X‐ray scintillation detector is presented. The detectors are intended for use on the new I11 powder diffraction beamline at the third‐generation Diamond synchrotron facility where X‐ray beams of high photon brightness are generated by insertion devices. The performance characteristics of these detection units were measured first using a radioactive source (efficiency of detection and background count rate) and then synchrotron X‐rays (peak stability, light yield linearity and response consistency). Here, the results obtained from these tests are reported, and the suitability of the design for the Diamond powder beamline is demonstrated by presenting diffraction data obtained from a silicon powder standard using a prototype multicrystal analyser stage.     

Synchrotron X‐ray footprinting on tour

Synchrotron footprinting is a valuable technique in structural biology for understanding macromolecular solution‐state structure and dynamics of proteins and nucleic acids. Although an extremely powerful tool, there is currently only a single facility in the USA, the X28C beamline at the National Synchrotron Light Source (NSLS), dedicated to providing infrastructure, technology development and support for these studies. The high flux density of the focused white beam and variety of specialized exposure environments available at X28C enables footprinting of highly complex biological systems; however, it is likely that a significant fraction of interesting experiments could be performed at unspecialized facilities. In an effort to investigate the viability of a beamline‐flexible footprinting program, a standard sample was taken on tour around the nation to be exposed at several US synchrotrons. This work describes how a relatively simple and transportable apparatus can allow beamlines at the NSLS, CHESS, APS and ALS to be used for synchrotron footprinting in a general user mode that can provide useful results.     

The impact of infrared synchrotron radiation in biology: Past,present and future

The Synchrotron Radiation Center (SRC) at the University of Wisconsin-Madison was shut down permanently in March 2014. It began operation in 1968 as the world's first dedicated synchrotron radiation user facility. This revolutionary idea of using synchrotron radiation for broad support of science and technology proved a resounding success, and it subsequently led to worldwide development of ever more powerful light sources for R&;D in many major scientific and technical areas. With upgrades and groundbreaking initiatives, SRC remained a cutting-edge and cost-effective facility to the end. SRC filled an important niche for tough experiments that were not possible at the newer facilities, given their beam time constraints. The world of IR, VUV, and soft X-ray research has been diminished by its loss, but its closing was necessitated by higher priorities at the US NSF.     

A new optical scheme for large‐extraction small‐aberration vacuum‐ultraviolet synchrotron radiation beamlines

Vacuum‐ultraviolet radiation delivered by bending‐magnet sources is used at numerous synchrotron radiation facilities worldwide. As bending‐magnet radiation is inherently much less collimated compared with undulator sources, the generation of high‐quality intense bending‐magnet vacuum‐ultraviolet photon beams is extremely demanding in terms of the optical layout due to the necessary larger collection apertures. In this article, an optimized optical layout which takes into account both the optical and electron beam properties is proposed. This layout delivers an improved beam emittance of over one order of magnitude compared with existing vacuum‐ultraviolet bending‐magnet beamlines that, up to now, do not take into account electron beam effects. The arrangement is made of two dedicated mirrors, a cylindrical and a cone‐shaped one, that focus independently both the horizontal and the vertical emission of a bending‐magnet source, respectively, and has been already successfully applied in the construction of the infrared beamline at the Brazilian synchrotron. Using this scheme, two vacuum‐ultraviolet beamline designs based on a SOLEIL synchrotron bending‐magnet source are proposed and analysed. They would be useful for future upgrades to the DISCO beamline at SOLEIL and could be readily implemented at other synchrotron radiation facilities.     

Energy‐dispersive X‐ray absorption spectroscopy at LNLS: investigation on strongly correlated metal oxides

An energy‐dispersive X‐ray absorption spectroscopy beamline mainly dedicated to X‐ray magnetic circular dichroism (XMCD) and material science under extreme conditions has been implemented in a bending‐magnet port at the Brazilian Synchrotron Light Laboratory. Here the beamline technical characteristics are described, including the most important aspects of the mechanics, optical elements and detection set‐up. The beamline performance is then illustrated through two case studies on strongly correlated transition metal oxides: an XMCD insight into the modifications of the magnetic properties of Cr‐doped manganites and the structural deformation in nickel perovskites under high applied pressure.     

WIFIP: a web‐based user interface for automated synchrotron beamlines

The beamline control software, through the associated graphical user interface (GUI), is the user access point to the experiment, interacting with synchrotron beamline components and providing automated routines. FIP, the French beamline for the Investigation of Proteins, is a highly automatized macromolecular crystallography (MX) beamline at the European Synchrotron Radiation Facility. On such a beamline, a significant number of users choose to control their experiment remotely. This is often performed with a limited bandwidth and from a large choice of computers and operating systems. Furthermore, this has to be possible in a rapidly evolving experimental environment, where new developments have to be easily integrated. To face these challenges, a light, platform‐independent, control software and associated GUI are required. Here, WIFIP, a web‐based user interface developed at FIP, is described. Further than being the present FIP control interface, WIFIP is also a proof of concept for future MX control software.     

Simultaneous measurement of X‐ray diffraction and ferroelectric polarization data as a function of applied electric field and frequency

The characteristics of a new ferroelectric measurement system at the European Synchrotron Radiation Facility are presented. The electric‐field‐induced phase transitions of Pb(Mg_1/3Nb_2/3)O₃–xPbTiO₃ are determined viain situ measurements of electric polarization within the synchrotron diffraction beamline. Real‐time data collection methods on single‐crystal samples are employed as a function of frequency to determine the microstructural origin of piezoelectric effects within these materials, probing the dynamic ferroelectric response.     

SUT‐NANOTEC‐SLRI beamline for X‐ray absorption spectroscopy

The SUT‐NANOTEC‐SLRI beamline was constructed in 2012 as the flagship of the SUT‐NANOTEC‐SLRI Joint Research Facility for Synchrotron Utilization, co‐established by Suranaree University of Technology (SUT), National Nanotechnology Center (NANOTEC) and Synchrotron Light Research Institute (SLRI). It is an intermediate‐energy X‐ray absorption spectroscopy (XAS) beamline at SLRI. The beamline delivers an unfocused monochromatic X‐ray beam of tunable photon energy (1.25–10 keV). The maximum normal incident beam size is 13 mm (width) × 1 mm (height) with a photon flux of 3 × 10⁸ to 2 × 10¹⁰ photons s^?1 (100 mA)^?1 varying across photon energies. Details of the beamline and XAS instrumentation are described. To demonstrate the beamline performance, K‐edge XANES spectra of MgO, Al₂O₃, S₈, FeS, FeSO₄, Cu, Cu₂O and CuO, and EXAFS spectra of Cu and CuO are presented.     

Fast X‐ray microfluorescence imaging with submicrometer‐resolution integrating a Maia detector at beamline P06 at PETRA III

The high brilliance of third‐generation synchrotron sources increases the demand for faster detectors to utilize the available flux. The Maia detector is an advanced imaging scheme for energy‐dispersive detection realising dwell times per image‐pixel as low as 50 µs and count rates higher than 10 × 10⁶ s^?1. In this article the integration of such a Maia detector in the Microprobe setup of beamline P06 at the storage ring PETRA III at the Deutsches Elektronen‐Synchrotron (DESY) in Hamburg, Germany, is described. The analytical performance of the complete system in terms of rate‐dependent energy resolution, scanning‐speed‐dependent spatial resolution and lower limits of detection is characterized. The potential of the Maia‐based setup is demonstrated by key applications from materials science and chemistry, as well as environmental science with geological applications and biological questions that have been investigated at the P06 beamline.     

Performance of the infrared microspectroscopy station at SSRF

At the third generation synchrotron light source Shanghai Synchrotron Radiation Facility (SSRF), the first infrared beamline BL01B has been successfully constructed. The infrared beamline collects both bending magnet and edge radiation. A brief introduction of the infrared beamline design has been given in this article. The infrared microspectroscopy station is equipped with a Nicolet 6700 FTIR spectrometer and a Nicolet Continuum Microscope. The flux at the entrance of the FTIR spectrometer, the intensity profile, the signal to noise ratio (SNR) with different apertures, and the focused spot size of the infrared microspectroscopy station have been measured. The performances with synchrotron radiation infrared source and internal globar source have been compared. The results indicate that the infrared microspectroscopy station at SSRF has the ability of analysis samples in a small area with diffraction limited spatial resolution.     

Performance calculations of the X‐ray powder diffraction beamline at NSLS‐II

The X‐ray Powder Diffraction (XPD) beamline at the National Synchrotron Light Source II is a multi‐purpose high‐energy X‐ray diffraction beamline with high throughput and high resolution. The beamline uses a sagittally bent double‐Laue crystal monochromator to provide X‐rays over a large energy range (30–70 keV). In this paper the optical design and the calculated performance of the XPD beamline are presented. The damping wiggler source is simulated by the SRW code and a filter system is designed to optimize the photon flux as well as to reduce the heat load on the first optics. The final beamline performance under two operation modes is simulated using the SHADOW program. For the first time a multi‐lamellar model is introduced and implemented in the ray tracing of the bent Laue crystal monochromator. The optimization and the optical properties of the vertical focusing mirror are also discussed. Finally, the instrumental resolution function of the XPD beamline is described in an analytical method.     

Fabrication and testing of a newly designed slit system for depth‐resolved X‐ray diffraction measurements

A new system of slits called `spiderweb slits' have been developed for depth‐resolved powder or polycrystalline X‐ray diffraction measurements. The slits act on diffracted X‐rays to select a particular gauge volume of sample, while absorbing diffracted X‐rays from outside of this volume. Although the slit geometry is to some extent similar to that of previously developed conical slits or spiral slits, this new design has advantages over the previous ones in use for complex heterogeneous materials and in situ and operando diffraction measurements. For example, the slits can measure a majority of any diffraction cone for any polycrystalline material, over a continuous range of diffraction angles, and work for X‐ray energies of tens to hundreds of kiloelectronvolts. The design is generated and optimized using ray‐tracing simulations, and fabricated through laser micromachining. The first prototype was successfully tested at the X17A beamline at the National Synchrotron Light Source, and shows similar performance to simulations, demonstrating gauge volume selection for standard powders, for all diffraction peaks over angles of 2–10°. A similar, but improved, design will be implemented at the X‐ray Powder Diffraction beamline at the National Synchrotron Light Source II.     

The high‐resolution diffraction beamline P08 at PETRA III

The new third‐generation synchrotron radiation source PETRA III located at the Deutsches Elektronen‐Synchrotron DESY in Hamburg, Germany, has been operational since the second half of 2009. PETRA III is designed to deliver hard X‐ray beams with very high brilliance. As one of the first beamlines of PETRA III the high‐resolution diffraction beamline P08 is fully operational. P08 is specialized in X‐ray scattering and diffraction experiments on solids and liquids where extreme high resolution in reciprocal space is required. The resolving power results in the high‐quality PETRA III beam and unique optical elements such as a large‐offset monochromator and beryllium lens changers. A high‐precision six‐circle diffractometer for solid samples and a specially designed liquid diffractometer are installed in the experimental hutch. Regular users have been accepted since summer 2010.