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.     

Cultural heritage and archaeology materials studied by synchrotron spectroscopy and imaging

The use of synchrotron radiation techniques to study cultural heritage and archaeological materials has undergone a steep increase over the past 10–15 years. The range of materials studied is very broad and encompasses painting materials, stone, glass, ceramics, metals, cellulosic and wooden materials, and a cluster of organic-based materials, in phase with the diversity observed at archaeological sites, museums, historical buildings, etc. Main areas of investigation are: (1) the study of the alteration and corrosion processes, for which the unique non-destructive speciation capabilities of X-ray absorption have proved very beneficial, (2) the understanding of the technologies and identification of the raw materials used to produce archaeological artefacts and art objects and, to a lesser extent, (3) the investigation of current or novel stabilisation, conservation and restoration practices. In terms of the synchrotron methods used, the main focus so far has been on X-ray techniques, primarily X-ray fluorescence, absorption and diffraction, and Fourier-transform infrared spectroscopy. We review here the use of these techniques from recent works published in the field demonstrating the breadth of applications and future potential offered by third generation synchrotron techniques. New developments in imaging and advanced spectroscopy, included in the UV/visible and IR ranges, could even broaden the variety of materials studied, in particular by fostering more studies on organic and complex organic–inorganic mixtures, while new support activities at synchrotron facilities might facilitate transfer of knowledge between synchrotron specialists and users from archaeology and cultural heritage sciences.     

IR Workshop at Biozentrum Basel

A workshop took place from February 1-2, 2011, in Basel, Switzerland, organized by the infrared team of the Swiss Light Source in collaboration with that of SOLEIL. Experienced synchrotron IR users were asked to illustrate the potential of the IR method for researchers from various disciplines. The recently operational IR beamlines at SLS and SOLEIL may benefit from this event.     

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.     

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.     

Characterization of the Metrology beamline at the SOLEIL synchrotron and application to the determination of mass attenuation coefficients of Ag and Sn in the range 3.5 ≤ E ≤ 28 keV

This work presents the new Metrology beamline at the SOLEIL synchrotron facility and a first attempt to quantitative measurements of mass attenuation coefficients for Ag and Sn performed on the hard X‐ray branch. We first describe the beamline itself and the characterization performed of the unfocused monochromatic beam running mode. We performed a first experimental measurement of mass attenuation coefficients in the range 3.5 ≤ E ≤ 28 keV and we also derived the K‐absorption and L‐absorption jump ratios. The results are compared with theoretical values as well as with other experimental data and agree well with previous published values. Copyright © 2011 John Wiley & Sons, Ltd.     

Information Technology/Large-Scale Data Handling

The experience of light source users has been transformed in recent years by large increases in flux and brightness, revolutionary new optics and detectors, and automation and advanced sample environments. Beamlines are producing data at rates and volumes that challenge the capabilities of even the most experienced user groups. Meanwhile, the community of synchrotron users continues to grow in size and diversity: researchers come from physics, material science, energy and battery research, geology, biology, chemistry, art history, and more. Almost every natural science domain is being advanced through the techniques employed at these facilities, but a significant fraction of these researchers are first-time or infrequent users of a particular beamline. The combination of an expanding base of new users and increased beamline capabilities is leading to an increase in the amount of “dark data” that is not analyzed fully (or, in some cases, at all).     

VUV synchrotron radiation: a new activation technique for tandem mass spectrometry

A novel experimental technique for tandem mass spectrometry and ion spectroscopy of electrosprayed ions using vacuum‐ultraviolet (VUV) synchrotron radiation is presented. Photon activation of trapped precursor ions has been performed by coupling a commercial linear quadrupole ion trap (Thermo scientific LTQ XL), equipped with the electrosprayed ions source, to the DESIRS beamline at the SOLEIL synchrotron radiation facility. The obtained results include, for the first time on biopolymers, photodetachment spectroscopy using monochromated synchrotron radiation of multi‐charged anions and the single photon ionization of large charge‐selected polycations. The high efficiency and signal‐to‐noise ratio achieved by the present set‐up open up possibilities of using synchrotron light as a new controllable activation method in tandem mass spectrometry of biopolymers and VUV‐photon spectroscopy of large biological ions.     

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.     

Time‐resolved photoelectron spectroscopy using synchrotron radiation time structure

Synchrotron radiation time structure is becoming a common tool for studying dynamic properties of materials. The main limitation is often the wide time domain the user would like to access with pump–probe experiments. In order to perform photoelectron spectroscopy experiments over time scales from milliseconds to picoseconds it is mandatory to measure the time at which each measured photoelectron was created. For this reason the usual CCD camera‐based two‐dimensional detection of electron energy analyzers has been replaced by a new delay‐line detector adapted to the time structure of the SOLEIL synchrotron radiation source. The new two‐dimensional delay‐line detector has a time resolution of 5 ns and was installed on a Scienta SES 2002 electron energy analyzer. The first application has been to characterize the time of flight of the photoemitted electrons as a function of their kinetic energy and the selected pass energy. By repeating the experiment as a function of the available pass energy and of the kinetic energy, a complete characterization of the analyzer behaviour in the time domain has been obtained. Even for kinetic energies as low as 10 eV at 2 eV pass energy, the time spread of the detected electrons is lower than 140 ns. These results and the time structure of the SOLEIL filling modes assure the possibility of performing pump–probe photoelectron spectroscopy experiments with the time resolution given by the SOLEIL pulse width, the best performance of the beamline and of the experimental station.     

The first microbeam synchrotron X‐ray fluorescence beamline at the Siam Photon Laboratory

The first microbeam synchrotron X‐ray fluorescence (µ‐SXRF) beamline using continuous synchrotron radiation from Siam Photon Source has been constructed and commissioned as of August 2011. Utilizing an X‐ray capillary half‐lens allows synchrotron radiation from a 1.4 T bending magnet of the 1.2 GeV electron storage ring to be focused from a few millimeters‐sized beam to a micrometer‐sized beam. This beamline was originally designed for deep X‐ray lithography (DXL) and was one of the first two operational beamlines at this facility. A modification has been carried out to the beamline in order to additionally enable µ‐SXRF and synchrotron X‐ray powder diffraction (SXPD). Modifications included the installation of a new chamber housing a Si(111) crystal to extract 8 keV synchrotron radiation from the white X‐ray beam (for SXPD), a fixed aperture and three gate valves. Two end‐stations incorporating optics and detectors for µ‐SXRF and SXPD have then been installed immediately upstream of the DXL station, with the three techniques sharing available beam time. The µ‐SXRF station utilizes a polycapillary half‐lens for X‐ray focusing. This optic focuses X‐ray white beam from 5 mm × 2 mm (H × V) at the entrance of the lens down to a diameter of 100 µm FWHM measured at a sample position 22 mm (lens focal point) downstream of the lens exit. The end‐station also incorporates an XYZ motorized sample holder with 25 mm travel per axis, a 5× ZEISS microscope objective with 5 mm × 5 mm field of view coupled to a CCD camera looking to the sample, and an AMPTEK single‐element Si (PIN) solid‐state detector for fluorescence detection. A graphic user interface data acquisition program using the LabVIEW platform has also been developed in‐house to generate a series of single‐column data which are compatible with available XRF data‐processing software. Finally, to test the performance of the µ‐SXRF beamline, an elemental surface profile has been obtained for a piece of ancient pottery from the Ban Chiang archaeological site, a UNESCO heritage site. It was found that the newly constructed µ‐SXRF technique was able to clearly distinguish the distribution of different elements on the specimen.     

Versatile variable temperature insert at the DEIMOS beamline for in situ electrical transport measurements

The design and the first experiments are described of a versatile cryogenic insert used for its electrical transport capabilities. The insert is designed for the cryomagnet installed on the DEIMOS beamline at the SOLEIL synchrotron dedicated to magnetic characterizations through X‐ray absorption spectroscopy (XAS) measurements. This development was spurred by the multifunctional properties of novel materials such as multiferroics, in which, for example, the magnetic and electrical orders are intertwined and may be probed using XAS. The insert thus enables XAS to in situ probe this interplay. The implementation of redundant wiring and careful shielding also enables studies on operating electronic devices. Measurements on magnetic tunnel junctions illustrate the potential of the equipment toward XAS studies of in operando electronic devices.     

DISCO: a low‐energy multipurpose beamline at synchrotron SOLEIL

DISCO, a novel low‐energy beamline covering the spectrum range from the VUV to the visible, has received its first photons at the French synchrotron SOLEIL. In this article the DISCO design and concept of three experimental stations serving research communities in biology and chemistry are described. Emphasis has been put on high flux generation and preservation of polarization at variable energy resolutions. The three experiments include a completely new approach for microscopy and atmospheric pressure experiments as well as a `classical' synchrotron radiation circular dichroism station. Preliminary tests of the optical design and technical concept have been made. Theoretical predictions of the beam have been compared with the first images produced by the first photons originating from the large‐aperture bending‐magnet source. Results are also reported concerning the cold finger used to absorb hard X‐ray radiation in the central part of the synchrotron beam and to avoid heavy thermal load on the following optics. Wavelength selection using monochromators with different gratings for each experimental set‐up as well as beam propagation and conditioning throughout the optical system are detailed. First photons comply very well with the theoretical calculations.     

The LUCIA beamline at SOLEIL

Commissioned in May 2004 on the SLS machine, the LUCIA beamline was moved to the synchrotron SOLEIL during the summer of 2008. To take advantage of this new setting several changes to its design were introduced. Here, a review of the various improvements of the mechanics and, mostly, of the optics is given. Described in detail are the results of a new multilayer grating monochromator implemented on the Kohzu vessel already holding the two‐crystal set‐up. It consists of a grating grooved onto a multilayer (replacing the first crystal) associated to a multilayer (as a second crystal). It allows a shift of the low‐energy limit of the beamline to around 500 eV with an energy resolution and a photon flux comparable with those of the previous couples of crystals (KTP and beryl).     

DISCO synchrotron‐radiation circular‐dichroism endstation at SOLEIL

The new synchrotron‐radiation circular‐dichroism (SRCD) endstation on the UV‐visible synchrotron beamline DISCO has been commissioned at the SOLEIL synchrotron. The design has been focused on preservation of a high degree of linear polarization at high flux and moderate resolving power covering the vacuum ultraviolet to visible spectral range (125–600 nm). The beam dimensions have been set to 4 mm × 4 mm at 1 nm bandwidth for lower sample degradation. The nitrogen‐purged sample chamber fits three types of sample holders accommodating conventional round cell mounting, automated rotation of the samples, as well as a microfluidic set‐up. Automated temperature‐controlled data collection on microvolumes is now available to the biology and chemistry communities. Macromolecules including membrane proteins, soluble proteins, bio‐nanotubes, sugars, DNA and RNAs are now routinely investigated.     

Circular dichroism beamline B23 at the Diamond Light Source

Synchrotron radiation circular dichroism (SRCD) is a well established technique in structural biology. The first UV‐VIS beamline, dedicated to circular dichroism, at Diamond Light Source Ltd, a third‐generation synchrotron facility in south Oxfordshire, UK, has recently become operational and it is now available for the user community. Herein the main characteristics of the B23 SRCD beamline, the ancillary facilities available for users, and some of the recent advances achieved are summarized.     

Status of the hard X‐ray microprobe beamline ID22 of the European Synchrotron Radiation Facility

The ESRF synchrotron beamline ID22, dedicated to hard X‐ray microanalysis and consisting of the combination of X‐ray fluorescence, X‐ray absorption spectroscopy, diffraction and 2D/3D X‐ray imaging techniques, is one of the most versatile instruments in hard X‐ray microscopy science. This paper describes the present beamline characteristics, recent technical developments, as well as a few scientific examples from recent years of the beamline operation. The upgrade plans to adapt the beamline to the growing needs of the user community are briefly discussed.     

A differential pumping system to deliver windowless VUV photons at atmospheric pressure

In order to deliver VUV (vacuum ultraviolet) photons under atmospheric pressure conditions, a differential pumping system has been built on the DISCO beamline at the SOLEIL synchrotron radiation facility. The system is made of four stages and is 840 mm long. The conductance‐limiting body has been designed to allow practicable optical alignment. VUV transmission of the system was tested under air, nitrogen, argon and neon, and photons could be delivered down to 60 nm (20 eV).