Single-crystal Raman spectroscopy and X-ray crystallography at beamline X26-C of the NSLS

Three-dimensional structures derived from X-ray diffraction of protein crystals provide a wealth of information. Features and interactions important for the function of macromolecules can be deduced and catalytic mechanisms postulated. Still, many questions can remain, for example regarding metal oxidation states and the interpretation of `mystery density', i.e. ambiguous or unknown features within the electron density maps, especially at ～2 ? resolutions typical of most macromolecular structures. Beamline X26-C at the National Synchrotron Light Source (NSLS), Brookhaven National Laboratory (BNL), provides researchers with the opportunity to not only determine the atomic structure of their samples but also to explore the electronic and vibrational characteristics of the sample before, during and after X-ray diffraction data collection. When samples are maintained under cryo-conditions, an opportunity to promote and follow photochemical reactions in situ as a function of X-ray exposure is also provided. Plans are in place to further expand the capabilities at beamline X26-C and to develop beamlines at NSLS-II, currently under construction at BNL, which will provide users access to a wide array of complementary spectroscopic methods in addition to high-quality X-ray diffraction data.     

I19, the small‐molecule single‐crystal diffraction beamline at Diamond Light Source

The dedicated small‐molecule single‐crystal X‐ray diffraction beamline (I19) at Diamond Light Source has been operational and supporting users for over three years. I19 is a high‐flux tunable‐wavelength beamline and its key details are described in this article. Much of the work performed on the beamline involves structure determination from small and weakly diffracting crystals. Other experiments that have been supported to date include structural studies at high pressure, studies of metastable species, variable‐temperature crystallography, studies involving gas exchange in porous materials and structural characterizations that require analysis of the diffuse scattering between Bragg reflections. A range of sample environments to facilitate crystallographic studies under non‐ambient conditions are available as well as a number of options for automation. An indication of the scope of the science carried out on the beamline is provided by the range of highlights selected for this paper.     

Design and performance of an X‐ray scanning microscope at the Hard X‐ray Nanoprobe beamline of NSLS‐II

A hard X‐ray scanning microscope installed at the Hard X‐ray Nanoprobe beamline of the National Synchrotron Light Source II has been designed, constructed and commissioned. The microscope relies on a compact, high stiffness, low heat dissipation approach and utilizes two types of nanofocusing optics. It is capable of imaging with ～15 nm × 15 nm spatial resolution using multilayer Laue lenses and 25 nm × 26 nm resolution using zone plates. Fluorescence, diffraction, absorption, differential phase contrast, ptychography and tomography are available as experimental techniques. The microscope is also equipped with a temperature regulation system which allows the temperature of a sample to be varied in the range between 90 K and 1000 K. The constructed instrument is open for general users and offers its capabilities to the material science, battery research and bioscience communities.     

A microfocus X‐ray fluorescence beamline at Indus‐2 synchrotron radiation facility

A microfocus X‐ray fluorescence spectroscopy beamline (BL‐16) at the Indian synchrotron radiation facility Indus‐2 has been constructed with an experimental emphasis on environmental, archaeological, biomedical and material science applications involving heavy metal speciation and their localization. The beamline offers a combination of different analytical probes, e.g. X‐ray fluorescence mapping, X‐ray microspectroscopy and total‐external‐reflection fluorescence characterization. The beamline is installed on a bending‐magnet source with a working X‐ray energy range of 4–20 keV, enabling it to excite K‐edges of all elements from S to Nb and L‐edges from Ag to U. The optics of the beamline comprises of a double‐crystal monochromator with Si(111) symmetric and asymmetric crystals and a pair of Kirkpatrick–Baez focusing mirrors. This paper describes the performance of the beamline and its capabilities with examples of measured results.     

Novel interface for cultural heritage at SOLEIL

The information that can be retrieved from the study of ancient materials and studies on their conservation rely strongly on the development and application of new techniques of physical analysis. This is particularly important at a time when global changes affecting our environment and way of life impose new stresses putting heritage preservation at risk. For this purpose, synchrotron techniques are particularly suited to the non- (or micro-) destructive characterisation of such heterogeneous materials, and a steep increase in the number of publications has been noticed recently from cultural heritage works using synchrotron radiation. In 2004, an interface dedicated to archaeology and cultural heritage was launched at the SOLEIL synchrotron to allow researchers from the international scientific community to be granted specific expertise. This interface aims at easing the access of researchers to the synchrotron, facilitating contacts, providing technical support and informing the community. The very first applications of SOLEIL beamlines in the heritage field are illustrated through works recently carried out at the first beamline of SOLEIL, LUCIA, currently located at the Swiss Light Source (SLS). The setup of the beamline is succinctly described. PACS 07.85.Qe; 87.59.-e     

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.     

In situ diffuse reflectance IR spectroscopy and X‐ray absorption spectroscopy for fast catalytic processes

A new instrument for synchronous in situ investigations of catalytic materials by IR and X‐ray absorption spectroscopies was designed and built at the X18A beamline of the National Synchrotron Light Source of Brookhaven National Laboratory. It provides analytical tools for solving structural, electronic and kinetic problems in catalysis science by two complementary methods. Among the features attractive for catalysis research are the broad range of catalytically active elements that can be investigated (starting with Ni and beyond), the wide range of reaction conditions (temperatures up to 873 K, various reactive gases) and time scales (starting from tens of seconds). The results of several representative experiments that illustrate the attractive capabilities of the new set‐up are discussed.     

2009 SSRL School on X-ray Spectroscopy Techniques in Environmental and Materials Sciences: Theory and Application

More than 50 students, post-docs, and career scientists from US national laboratories, academic institutions, and the international user community participated in this four-day school, held from June 2–5, 2009, which delved deeply into theoretical and practical aspects of synchrotron X-ray spectroscopy. The fourth annual school on synchrotron techniques in environmental and materials sciences, organized by the Stanford Synchrotron Radiation Lightsource (SSRL) at the SLAC National Accelerator Laboratory, was designed to introduce new and prospective users to theoretical underpinnings and capabilities of the techniques, data collection procedures, and data analysis approaches. More advanced topics, particularly in data analysis, were also discussed to reinforce and clarify important concepts that are fundamental to data interpretation. Although the school focused principally on applications in environmental and materials sciences, diverse and cross-cutting disciplinary backgrounds were represented, from environmental remediation science and geochemistry, to heterogeneous catalysis and bioinorganic chemistry, to materials sciences and applied physics.     

Installation of a combined Raman and AFM microscope as a sample environment for nuclear resonance scattering at P01, PETRA III

A combined Raman and atomic force microscope (AFM) has been installed at beamline P01, PETRA III, DESY in Hamburg and is now available for all users of this beamline. With this unique setup nuclear resonance scattering and simultaneously performed Raman or Atomic Force Microscopy experiments are possible. Here we report on technical details of this new sample environment and on first tests with respect to the study of microstructures of spin crossover materials using ⁵⁷Fe nuclear resonance scattering.     

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.     

HAXPES beamline PES‐BL14 at the Indus‐2 synchrotron radiation source

The Hard X‐ray Photo‐Electron Spectroscopy (HAXPES) beamline (PES‐BL14), installed at the 1.5 T bending‐magnet port at the Indian synchrotron (Indus‐2), is now available to users. The beamline can be used for X‐ray photo‐emission electron spectroscopy measurements on solid samples. The PES beamline has an excitation energy range from 3 keV to 15 keV for increased bulk sensitivity. An in‐house‐developed double‐crystal monochromator [Si (111)] and a platinum‐coated X‐ray mirror are used for the beam monochromatization and manipulation, respectively. This beamline is equipped with a high‐energy (up to 15 keV) high‐resolution (meV) hemispherical analyzer with a microchannel plate and CCD detector system with SpecsLab Prodigy and CasaXPS software. Additional user facilities include a thin‐film laboratory for sample preparation and a workstation for on‐site data processing. In this article, the design details of the beamline, other facilities and some recent scientific results are described.     

XDS: a flexible beamline for X‐ray diffraction and spectroscopy at the Brazilian synchrotron

The majority of the beamlines at the Brazilian Synchrotron Light Source Laboratory (LNLS) use radiation produced in the storage‐ring bending magnets and are therefore currently limited in the flux that can be used in the harder part of the X‐ray spectrum (above ～10 keV). A 4 T superconducting multipolar wiggler (SCW) was recently installed at LNLS in order to improve the photon flux above 10 keV and fulfill the demands set by the materials science community. A new multi‐purpose beamline was then installed at the LNLS using the SCW as a photon source. The XDS is a flexible beamline operating in the energy range between 5 and 30 keV, designed to perform experiments using absorption, diffraction and scattering techniques. Most of the work performed at the XDS beamline concentrates on X‐ray absorption spectroscopy at energies above 18 keV and high‐resolution diffraction experiments. More recently, new setups and photon‐hungry experiments such as total X‐ray scattering, X‐ray diffraction under high pressures, resonant X‐ray emission spectroscopy, among others, have started to become routine at XDS. Here, the XDS beamline characteristics, performance and a few new experimental possibilities are described.     

X-ray Nanoprobe Beamline and Pioneering Electron Microscopy Facility Come into Focus

An exciting new hub for cutting-edge materials and life science research is well on its way to being built at Diamond. The new building, which is under construction next to the Imaging and Coherence beamline (I13), will house the X-ray Nanoprobe beamline (I14) along with the Electron Bio-imaging Centre (eBIC) and the Electron Microscopy Centre for physical sciences.     

Structure of crystalline and amorphous Ge probed by X-ray absorption and diffraction techniques

Results of experiments dedicated to the study of the structure under high pressure of amorphous Ge (a-Ge) and crystalline Ge (c-Ge) are reported. Energy-dispersive X-ray diffraction measurements of c-Ge have been collected at the DW11A beamline (DCI, LURE) using a heatable diamond anvil cell as pressure device up to 500?K. The a-Ge measurements have been performed at the ESRF, using the advanced set-up available at the BM29 beamline, which allows the simultaneous collection of X-ray absorption spectroscopy data and diffraction patterns used to monitor pressure and crystallization of a sample in a Paris–Edinburgh large-volume cell. The new structural data allowed us to obtain a reliable determination of the lattice parameters as a function of pressure and temperature in c-Ge and of the first-neighbor distance distribution in a-Ge.     

European research platform IPANEMA at the SOLEIL synchrotron for ancient and historical materials

IPANEMA, a research platform devoted to ancient and historical materials (archaeology, cultural heritage, palaeontology and past environments), is currently being set up at the synchrotron facility SOLEIL (Saint‐Aubin, France; SOLEIL opened to users in January 2008). The new platform is open to French, European and international users. The activities of the platform are centred on two main fields: increased support to synchrotron projects on ancient materials and methodological research. The IPANEMA team currently occupies temporary premises at SOLEIL, but the platform comprises construction of a new building that will comply with conservation and environmental standards and of a hard X‐ray imaging beamline today in its conceptual design phase, named PUMA. Since 2008, the team has supported synchrotron works at SOLEIL and at European synchrotron facilities on a range of topics including pigment degradation in paintings, composition of musical instrument varnishes, and provenancing of medieval archaeological ferrous artefacts. Once the platform is fully operational, user support will primarily take place within medium‐term research projects for `hosted' scientists, PhDs and post‐docs. IPANEMA methodological research is focused on advanced two‐dimensional/three‐dimensional imaging and spectroscopy and statistical image analysis, both optimized for ancient materials.     

Energy-dispersive X-ray diffraction beamline at Indus-2 synchrotron source

An energy-dispersive X-ray diffraction beamline has been designed, developed and commissioned at BL-11 bending magnet port of the Indian synchrotron source, Indus-2. The performance of this beamline has been benchmarked by measuring diffraction patterns from various elemental metals and standard inorganic powdered samples. A few recent high-pressure investigations are presented to demonstrate the capabilities of the beamline.     

RixsToolBox: software for the analysis of soft X‐ray RIXS data acquired with 2D detectors

A software with a graphical user interface has been developed with the aim of facilitating the data analysis for users of a new resonant inelastic X‐ray scattering (RIXS) spectrometer installed at the ESRF beamline ID32. The software is organized in modules covering all relevant steps in the data reduction from a stack of several hundred two‐dimensional CCD images to a single RIXS spectrum. It utilizes both full charge integration and single‐photon centroiding to cope with high‐flux and high‐resolution requirements. Additional modules for further data analysis and the extraction of instrumental parameters are available. The software has been in routine use for about a year now and in that time many additional features have been incorporated. It now meets the users' need for an easy‐to‐use data analysis tool that allows looking at and understanding data as it is acquired and thus steering users' experiments more efficiently.