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X-ray fluorescence with synchrotron radiation.

The use of synchrotron radiation for X-ray fluorescence has several advantages over the use of other conventional X-ray sources. The principles of synchrotron radiation and methods for applying synchrotron radiation to the X-ray fluorescence measurements of trace elements are discussed. The Brookhaven National Laboratory X-ray microprobe, facilities dedicated to X-ray fluorescence, and related analytical techniques are discussed. Some examples of trace element analyses in biological materials with synchrotron radiation are presented.

Electron Probe Microanalysis↗

Reveal protein molecular structural-chemical differences between two types of winterfat (forage) seeds with physiological differences in low temperature tolerance using synchrotron-based Fourier transform infrared microspectroscopy.

Winterfat (Krascheninnikovia lanata) (forage seed) is a long-lived native shrub with superior forage quality for livestock and wildlife. The objectives of this study were to use advanced synchrotron technology [S-Fourier transform infrared microspectroscopy (FTIR)] as a novel approach to reveal protein molecular structural-chemical differences in terms of protein secondary structures between the two types of winterfat (forage) seeds, which show physiological differences in low-temperature tolerances. This experiment was performed at beamline U10B at the National Synchrotron Light Source (NSLS) in Brookhaven National Laboratory (BNL), U.S. Department of Energy (NSLS-BNL, New York). The results showed that with the synchrotron analytical technique (S-FTIR), the molecular structural-chemical makeup and characteristics of the winterfat seed tissues could be imaged and revealed. The protein secondary structures differed between the large and the small seed tissues. By using the multicomponent peaks modeling method, the results show that the large seeds contained no significant differences (P > 0.05) in percentage of beta-sheet (average 37.0%) and alpha-helix (average 24.1%). However, the large seeds contained a lower (P < 0.05) percentage of beta-turns (18.1 vs 20.1%) and a lower (P < 0.05) ratio of beta-turns to alpha-helices (0.8 vs 0.9) and beta-turns to beta-sheets (0.5 vs 0.6). Our results demonstrate the potential of highly spatially resolved synchrotron-based FTIR microspectroscopy to reveal differences of structural molecular chemistry and protein secondary structures, which are associated with seed size variation and may affect germination behaviors.

Amaranthaceae↗

Objective comparison of image quality and dose between conventional and synchrotron radiation mammography.

The shape of the energy spectrum produced by an x-ray tube has a great importance in mammography. Many anode-filtration combinations have been proposed to obtain the most effective spectrum shape for the image quality-dose relationship. On the other hand, third generation synchrotrons such as the European Synchrotron Radiation Facility in Grenoble are able to produce a high flux of monoenergetic radiation. It is thus a powerful tool to study the effect of beam energy on image quality and dose in mammography. An objective method was used to evaluate image quality and dose in mammography with synchrotron radiation and to compare them to standard conventional units. It was performed systematically in the energy range of interest for mammography through the evaluation of a global image quality index and through the measurement of the mean glandular dose. Compared to conventional mammography units, synchrotron radiation shows a great improvement of the image quality-dose relationship, which is due to the beam monochromaticity and to the high intrinsic collimation of the beam, which allows the use of a slit instead of an anti-scatter grid for scatter rejection.

Dose-Response Relationship, Radiation↗

Synchrotron radiation of crystallized beams.

We study the modifications of synchrotron radiation of charges in a storage ring as they are cooled. The pair correlation lengths between the charges are manifest in the synchrotron radiation and coherence effects exist for wavelengths longer than the coherence lengths between the charges. Therefore, the synchrotron radiation can be used as a diagnostic tool to determine the state (gas, liquid, crystal) of the charged plasma in the storage ring. We show also that the total power of the synchrotron radiation is significantly reduced for crystallized beams, both coasting and bunched. This opens the possibility of accelerating particles to ultrarelativistic energies using small-sized cyclic accelerators.

Journal Article↗

Combined system of synchrotron radiation and laser for solid-state research.

Two combined systems of synchrotron radiation and laser have been constructed for solid-state research. One is a laser-induced fluorescence system to observe synchrotron radiation-induced desorption of alkali atoms from ionic crystals, which consists of a laser diode with a high repetition rate and synchrotron radiation under a single-bunch operation. The other is a system of two-photon spectroscopy, which is based on the combination of synchrotron radiation pulses with a low intensity and high repetition rate and Nd:YAG laser pulses with a high intensity and low repetition rate. The experimental systems and the preliminary results are presented in this report.

Journal Article↗

Synchrotron radiation direct photo-etching of polymers and crystals for micromachining.

Synchrotron radiation etching of polymers and optical crystals which are transparent throughout the spectral range from visible to ultraviolet has been carried out without using any chemicals, successfully creating high-aspect-ratio microstructures for micromachining. A detailed study of the etching rates by varying the synchrotron beam current, sample temperature, beam size and aspect ratio showed that this synchrotron radiation process is essentially different from laser ablation, while an in situ mass spectrometric analysis of gaseous etching products showed that the dissociation mechanism involved with the synchrotron radiation processing, even with heating, is completely different from the thermal dissociation of the laser ablation.

Journal Article↗

Relationship between spatial coherence of synchrotron radiation and emittance.

Analytical calculation of the first-order spatial coherence for the Gaussian beam and the exact numerical calculation for synchrotron radiation are compared in this paper. The approximation of regarding synchrotron radiation as a Gaussian beam is often used to investigate the brightness, the flux and some qualitative properties. Calculations show that synchrotron radiation does not have as high coherence as the Gaussian beam because of the beam profile, the phases of the wave and the polarization. If one can measure the beam size and the spatial coherence of synchrotron radiation, it is possible to determine the total photon beam emittance without any knowledge of the Twiss parameters of the ring.

Journal Article↗

Ultrahigh-vacuum reaction apparatus to study synchrotron-radiation-stimulated processes.

An ultrahigh-vacuum reaction apparatus to study synchrotron-radiation-stimulated processes has been constructed and placed on beamline 4B of the synchrotron radiation storage ring (UVSOR) at the Institute for Molecular Science. The apparatus is designed so that multiple synchrotron radiation processes such as etching and chemical vapour deposition can be carried out successively without breaking the high vacuum. It is equipped with IR reflection absorption spectroscopy (IRRAS) apparatus and reflective high-energy electron diffraction (RHEED) apparatus for in situ observations. The basic parameters of the apparatus including etching and deposition rates have been measured. IRRAS using buried metal layer substrates has been confirmed to be a very useful method of analyzing the reaction mechanisms of the synchrotron-radiation-stimulated processes.

Journal Article↗

Deconvoluting ultrafast structural dynamics: temporal resolution beyond the pulse length of synchrotron radiation.

100 picosecond X-ray snapshots visualizing the structural dynamics of macromolecular systems are now routinely available at synchrotron sources. A wealth of fundamental processes in photochemistry, condensed matter physics and biology, however, occur on considerably faster time scales. Standard experimental protocols at synchrotron sources cannot provide structural information with faster temporal resolution as these are limited by the duration of the electron bunch within the synchrotron ring. By walking the timing of femtosecond laser photolysis through a (much longer) X-ray pulse in steps of a few picoseconds, structural information on ultrafast dynamics may be retrieved from a set of X-ray scattering images, initially through deconvolution and subsequently through refinement. This experimental protocol promises immediate improvements in the temporal resolution available at synchrotron sources, facilitating the study of a number of rapid complex photochemical processes. Combined with techniques which reshape the X-ray probe pulse, the accessible temporal domain could further be extended to near-picosecond resolution.

Journal Article↗

New trend of cardiac imaging--intravenous coronary arteriography by synchrotron radiation.

Synchrotron radiation is a broadspectrum intense X-ray beam. Selected X-ray wavelength was obtained by Bragg reflex. That is a monochromatic beam, which has a high spatial resolution, and has a K-edge discontinuity in attenuation coefficient, which, by energy subtraction, contributes to improve time resolution. An attempt to apply this method to intravenous coronary arteriography was performed in 7 anesthetized dogs. The beam was obtained by synchrotron radiation from accumulation ring, was reflected by silicon crystal, and was detected by 7 inch image intensifier system. Two-dimensional real time images were recorded on video tape. Phantom experiment was also performed. In dogs, coronary arteries were clearly distinguished by synchrotron radiation, especially at real time by video system. Phantom experiment suggested that coronary arteries could be visualized even over the visualized left ventricle. In conclusion, synchrotron radiation using two-dimensional real time images is expected to be useful in intravenous coronary arteriography in man.

Animals↗

Hydroxyl radical probe of the surface of lysozyme by synchrotron radiolysis and mass spectrometry.

A new approach is reported that combines synchrotron radiolysis and mass spectrometry to probe the surface of proteins. Hydroxyl radicals produced upon the radiolysis of protein solutions with synchrotron light for several milliseconds result in the reaction of amino acid side chains. This results in the formation of stable oxidation products where the level of oxidation at the reactive residues is influenced by the accessibility of their side chains to the bulk solvent. The aromatic and sulfur-containing residues have been found to react preferentially in accord with previous peptide studies. The sites of oxidation have been determined by tandem mass spectrometry. The rate of oxidation at these reactive markers has been measured for each of the proteolytic peptides as a function of exposure time based on the relative proportion of modified and unmodified peptide ions detected by mass spectrometry. Oxidation rates have been found to correlate closely with a theoretical measure of the accessibility of residue side chains to the bulk solvent in the native protein structure. The synchrotron-based approach is able to distinguish the relative accessibility of the tryptophan residue side chains of lysozyme at positions 62 and 123 from each other and all other tryptophan residues based on their rates of oxidation.

Amino Acid Sequence↗

Synchrotron radiation in radiology: novel X-ray sources.

X-rays, the key ingredient of radiology, are still primarily produced with the mechanism discovered by Röntgen over one century ago. A different approach, however, is becoming increasingly important: the use of synchrotron sources based on fast-moving electrons and on their relativistic properties. We discuss the elements of this new strategy, its practical implementation, and some new types of synchrotron sources under development. The present and potential impact on radiology of different classes of synchrotron sources is briefly and realistically analyzed.

Humans↗

Visualizing rhizosphere chemistry of legumes with mid-infrared synchrotron radiation.

A bright synchrotron light source operated by the Lawrence Berkeley National Laboratory served as an external source for infrared (IR) microscopy of plant root microcosms. Mid-IR light from synchrotrons is 2-3 orders of magnitude brighter than conventional sources, providing contrast based on the chemical information in the reflected signal at a spatial resolution near the diffraction-limit of 3-10 microm. In an experiment using plant root microcosms fitted with zinc selenide IR-transmissive windows (50 mm x 20 mm x 1 mm), we describe chemical differences and similarities within the root zone of mung bean (Vigna radiata L.), grown with or without phosphorus, and revealed by reflectance spectromicroscopy. Comparative root and root-exudate profiles are described in sand/silt culture over the wavelength range of 2.5 to 16 pm (4.000 to 650 cm(-1) ) in the mid-IR. the spectral region most useful for the analytical identification of small organic molecules. Root epidermal tissue of plants grown with low phosphorus showed a greater lipid contribution and less lignin than nutrient-sufficient plants. In the zone 200 microm from the root axis, control plants were enriched with simple sugars and monomeric lignin precursors. In low-phosphorus plants, the rhizosphere possessed IR signatures from protein and sugars. Individual soil minerals could be easily discriminated from biological material. Synchrotron IR spectromicroscopy, therefore, complements existing root imaging techniques.

Fabaceae↗

Quantification of crystallinity in substantially amorphous materials by synchrotron X-ray powder diffractometry.

PURPOSE: The aim of this study was to develop a highly sensitive powder X-ray diffraction (XRD) technique for quantification of crystallinity in substantially amorphous pharmaceuticals, utilizing synchrotron radiation and a 2-D area detector. METHODS: Diffraction data were acquired at the European Synchrotron Radiation Facility (France) using a 2-D charge-coupled device detector. The crystallization of amorphous sucrose was monitored in situ, isothermally at several temperatures in the range of 90 to 160 degrees C. An algorithm was developed for separation of the crystalline and amorphous intensities from the total diffraction pattern. RESULTS: The synchrotron XRD technique allowed powder diffraction patterns to be recorded with a time resolution of 40 ms. The gradual crystallization of sucrose is analogous to a series of physical mixtures with increasing content of the crystalline component. The in situ crystallization approach circumvented the problem of inhomogeneity in mixing--a potentially serious issue at extreme mixture compositions. The estimated limit of detection of crystalline sucrose in an amorphous matrix was 0.2% w/w, a considerable improvement over the reported value of approximately 1% w/w with a conventional XRD. CONCLUSION: High-intensity XRD can discern subtle changes in the lattice order of materials. The first evidence of crystallization can serve as an indicator of the potential physical instability of the product.

Crystallization↗

Solute crystallization in frozen systems-use of synchrotron radiation to improve sensitivity.

PURPOSE: To demonstrate the sensitivity of low temperature synchrotron X-ray diffractometry (SXRD) for detecting solute crystallization in frozen sodium phosphate buffer solutions. To determine the effect of annealing on solute crystallization in frozen solutions. MATERIALS AND METHODS: Sodium phosphate buffer solutions, at initial buffer concentrations ranging from 1 to 100 mM (pH 7.4) were cooled to -50 degrees C. The crystallization of disodium hydrogen phosphate dodecahydrate (Na(2)HPO(4) *12H(2)O) was monitored using a laboratory as well as a synchrotron source. At selected concentrations, the effect of annealing (at -20 degrees C) was investigated. RESULTS: With the laboratory source, solute crystallization, based on the appearance of one diagnostic peak with a d-spacing of 5.4 A, was evident only when the initial buffer concentration was at least 50 mM. In contrast, using SXRD, crystallization was detected at initial buffer concentrations down to 1 mM. In addition, the use of a high-resolution 2D detector enabled the visualization of numerous diffraction rings of the crystalline solute. At both 10 and 100 mM buffer concentration, there was no increase in solute crystallization due to annealing. CONCLUSION: By using synchrotron radiation, solute crystallization was detected with substantially increased sensitivity, making the technique useful for freeze-drying cycles of practical and commercial importance. Since numerous peaks of the crystalline solute appeared, the technique has potential utility in complex, multi-component systems.

Buffers↗

Synchrotron X-ray studies of lipids and membranes: a critique.

This review gives a description of techniques, suitable for the study of lipid dispersions and unorientated membranes, that are available at synchrotron facilities to determine either the kinetics of transitional phenomena in the time after a temperature or pressure jump is initiated, or the phases present while a sample undergoes a phase transition. Included in this description is information about synchrotron X-ray sources, sample holders and temperature controllers, detection systems, as well as data reduction. Examples involving lipid dispersions are provided to illustrate the application of these methods using synchrotron radiation.

Kinetics↗

Chemical imaging of biological tissue with synchrotron infrared light.

Fourier transform infrared micro-spectroscopy (FTIRM) and imaging (FTIRI) have become valuable techniques for examining the chemical makeup of biological materials by probing their vibrational motions on a microscopic scale. Synchrotron infrared (S-IR) light is an ideal source for FTIRM and FTIRI due to the combination of its high brightness (i.e., flux density), also called brilliance, and broadband nature. Through a 10-microm pinhole, the brightness of a synchrotron source is 100-1000 times higher than a conventional thermal (globar) source. Accordingly, the improvement in spatial resolution and in spectral quality to the diffraction limit has led to a plethora of applications that is just being realized. In this review, we describe the development of synchrotron-based FTIRM, illustrate its advantages in many applications to biological systems, and propose some potential future directions for the technique.

Chemical Phenomena↗

Synchrotron microradiography study on acute lung injury of mouse caused by PM(2.5) aerosols.

In order to investigate FeSO(4), ZnSO(4) (the two of main metal compositions of Shanghai PM(2.5) (particle matter with those aerodynamical diameter <2.5 microm)) effects on acute lung injury, six solutions contained PM(2.5) aerosol particles, FeSO(4), ZnSO(4) and their mixtures were instilled intratracheally into mouse lungs for experiment. By 2 days after instillation, the live mice were checked in vivo by synchrotron refractive index microradiography. In addition after extracted and examined by dissection, the right lobes of lung were fixed by formalin, then imaged by synchrotron microradiography again. Corresponding parts of those lung tissues were embedded in paraffin for histopathologic study. The synchrotron X-ray microradiographs of live mouse lung showed different lung texture changes after instilled with different toxic solutions. Hemorrhage points in lung were observed more from those mice instilled by FeSO(4) contained toxin solutions groups. Bronchial epithelial hyperplasia can be observed in ZnSO(4) contained solution-instilled groups from histopathologic analysis. It was found that the acute lung injury of mice caused by solution of PM(2.5)+FeSO(4)+ZnSO(4) was more serious than other toxin solutions. Results suggested that FeSO(4) mainly induced hemorrhage and ZnSO(4) mainly induced inflammation and bronchiolar epithelial hyperplasia in the early toxicological effects of PM(2.5).

Aerosols↗